Split (1)

train · 558k rows

file_name stringlengths 11 11	content stringlengths 1.16k 56.6M
1100693.cif	#------------------------------------------------------------------------------ #$Date: 2018-08-16 00:31:59 +0300 (Thu, 16 Aug 2018) $ #$Revision: 209732 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/10/06/1100693.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100693 loop_ _publ_author_name 'Dias, H. V. Rasika' 'Diyabalanage, Himashinie V. K.' 'Gamage, Chammi S. Palehepitiya' _publ_section_title ; Neutral Cu~4~N~12~ and Ag~4~N~12~ metallacycles with a para-cyclophane framework assembled from copper(I) and silver(I) pyrazolates and pyridazine. ; _journal_coden_ASTM CHCOFS _journal_issue 12 _journal_name_full ; Chemical Communications (Cambridge, United Kingdom) ; _journal_page_first 1619 _journal_page_last 1621 _journal_paper_doi 10.1039/b418306a _journal_year 2005 _chemical_formula_sum 'C28 H12 Cu4 F24 N12' _chemical_formula_weight 613.33 _chemical_name_common ((3,5-(CF3)2PzCu)4(C4H4N2)2) _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 105.928(2) _cell_angle_beta 109.526(2) _cell_angle_gamma 96.780(2) _cell_formula_units_Z 1 _cell_length_a 9.3177(10) _cell_length_b 10.0414(11) _cell_length_c 11.7532(13) _cell_measurement_temperature 100(2) _cell_volume 969.56(18) _diffrn_ambient_temperature 100(2) _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0159 _diffrn_reflns_av_sigmaI/netI 0.0268 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 6176 _diffrn_reflns_theta_max 26.00 _diffrn_reflns_theta_min 1.95 _exptl_absorpt_coefficient_mu 2.323 _exptl_absorpt_correction_type none _exptl_absorpt_process_details SADABS _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 2.101 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 596 _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.25 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 307 _refine_ls_number_reflns 3685 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.054 _refine_ls_R_factor_all 0.0312 _refine_ls_R_factor_gt 0.0302 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0473P)^2^+0.8518P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0815 _refine_ls_wR_factor_ref 0.0824 _reflns_number_gt 3577 _reflns_number_total 3685 _reflns_threshold_expression >2sigma(I) _cod_duplicate_entry 7100785 _cod_depositor_comments ; Adding additional information after consulting the original publication and the supplementary material. Antanas Vaitkus, 2018-08-16 The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_sg_symbol_H-M P-1 _cod_database_code 1100693 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 1.48831(3) 0.58016(3) 0.69656(3) 0.01609(10) Uani 1 1 d . . . Cu2 Cu 1.74735(3) 0.57984(3) 0.60677(3) 0.01716(10) Uani 1 1 d . . . C1 C 1.9589(3) 0.7166(3) 0.8787(3) 0.0253(6) Uani 1 1 d . . . H1A H 2.0419 0.7113 0.8491 0.030 Uiso 1 1 calc R . . C2 C 1.9964(3) 0.7793(3) 1.0090(3) 0.0292(6) Uani 1 1 d . . . H2A H 2.1022 0.8163 1.0676 0.035 Uiso 1 1 calc R . . C3 C 1.8754(4) 0.7861(3) 1.0498(2) 0.0263(6) Uani 1 1 d . . . H3A H 1.8942 0.8281 1.1379 0.032 Uiso 1 1 calc R . . C4 C 1.7242(3) 0.7294(3) 0.9583(2) 0.0220(5) Uani 1 1 d . . . H4A H 1.6391 0.7329 0.9856 0.026 Uiso 1 1 calc R . . C13 C 1.2668(3) 0.7766(3) 0.6645(2) 0.0191(5) Uani 1 1 d . . . C16 C 1.3391(3) 0.8632(3) 0.8036(3) 0.0236(6) Uani 1 1 d . . . C23 C 1.6728(3) 0.8375(3) 0.5240(2) 0.0196(5) Uani 1 1 d . . . C26 C 1.7653(3) 0.9418(3) 0.6536(3) 0.0217(5) Uani 1 1 d . . . C33 C 1.4708(3) 0.2695(2) 0.6774(2) 0.0189(5) Uani 1 1 d . . . C34 C 1.4035(3) 0.1345(3) 0.5866(2) 0.0212(5) Uani 1 1 d . . . H34A H 1.4086 0.0448 0.5979 0.025 Uiso 1 1 calc R . . C36 C 1.5652(3) 0.3082(3) 0.8155(3) 0.0230(5) Uani 1 1 d . . . C43 C 1.8835(3) 0.3235(3) 0.5343(2) 0.0184(5) Uani 1 1 d . . . C44 C 1.8629(3) 0.2110(3) 0.4277(2) 0.0205(5) Uani 1 1 d . . . H44A H 1.9235 0.1418 0.4199 0.025 Uiso 1 1 calc R . . C46 C 2.0097(3) 0.3675(3) 0.6644(3) 0.0222(5) Uani 1 1 d . . . N1 N 1.6933(2) 0.6704(2) 0.83405(19) 0.0160(4) Uani 1 1 d . . . N2 N 1.8127(2) 0.6633(2) 0.79316(19) 0.0180(4) Uani 1 1 d . . . N11 N 1.3212(2) 0.6646(2) 0.61741(19) 0.0161(4) Uani 1 1 d . . . N21 N 1.6545(2) 0.6963(2) 0.50202(19) 0.0174(4) Uani 1 1 d . . . N31 N 1.4356(2) 0.3701(2) 0.62418(19) 0.0170(4) Uani 1 1 d . . . N41 N 1.7734(2) 0.3988(2) 0.50779(19) 0.0164(4) Uani 1 1 d . . . F16C F 1.49266(18) 0.91530(16) 0.84762(15) 0.0272(4) Uani 1 1 d . . . F16B F 1.3208(2) 0.7869(2) 0.87776(16) 0.0442(5) Uani 1 1 d . . . F16A F 1.2741(2) 0.9730(2) 0.82937(18) 0.0518(6) Uani 1 1 d . . . F26C F 1.91246(19) 0.92585(18) 0.70353(16) 0.0345(4) Uani 1 1 d . . . F26B F 1.7034(2) 0.93330(17) 0.73985(15) 0.0291(4) Uani 1 1 d . . . F26A F 1.7771(2) 1.07537(16) 0.65309(17) 0.0377(4) Uani 1 1 d . . . F36A F 1.71399(19) 0.37813(18) 0.85046(15) 0.0301(4) Uani 1 1 d . . . F36B F 1.5071(2) 0.39468(19) 0.88919(15) 0.0338(4) Uani 1 1 d . . . F36C F 1.5746(3) 0.19374(17) 0.85162(16) 0.0419(5) Uani 1 1 d . . . F46C F 1.95507(18) 0.37558(16) 0.75779(14) 0.0245(3) Uani 1 1 d . . . F46B F 2.10246(19) 0.49586(17) 0.69736(16) 0.0311(4) Uani 1 1 d . . . F46A F 2.1020(2) 0.27448(19) 0.67094(16) 0.0325(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01628(17) 0.01461(16) 0.01437(16) 0.00110(12) 0.00583(12) 0.00181(11) Cu2 0.01675(17) 0.01729(16) 0.01445(16) 0.00102(12) 0.00608(13) 0.00314(12) C1 0.0163(13) 0.0275(13) 0.0223(13) 0.0005(11) 0.0021(11) 0.0045(10) C2 0.0215(14) 0.0274(13) 0.0240(14) -0.0007(11) -0.0019(11) 0.0067(11) C3 0.0366(16) 0.0207(12) 0.0159(12) 0.0017(10) 0.0057(11) 0.0102(11) C4 0.0276(14) 0.0187(12) 0.0173(12) 0.0034(10) 0.0077(11) 0.0049(10) C13 0.0208(13) 0.0172(11) 0.0220(12) 0.0050(10) 0.0132(11) 0.0031(9) C16 0.0219(13) 0.0239(13) 0.0235(13) 0.0011(11) 0.0125(11) 0.0047(10) C23 0.0214(13) 0.0162(11) 0.0224(13) 0.0027(10) 0.0134(11) 0.0027(10) C26 0.0226(13) 0.0169(11) 0.0245(13) 0.0016(10) 0.0127(11) 0.0022(10) C33 0.0212(13) 0.0166(11) 0.0215(12) 0.0055(10) 0.0120(10) 0.0047(9) C34 0.0269(14) 0.0156(11) 0.0241(13) 0.0056(10) 0.0142(11) 0.0045(10) C36 0.0292(14) 0.0200(12) 0.0239(13) 0.0090(10) 0.0134(11) 0.0070(10) C43 0.0200(12) 0.0192(11) 0.0213(12) 0.0090(10) 0.0125(10) 0.0046(10) C44 0.0205(13) 0.0196(12) 0.0252(13) 0.0069(10) 0.0136(11) 0.0059(10) C46 0.0220(13) 0.0262(13) 0.0246(13) 0.0108(11) 0.0138(11) 0.0091(10) N1 0.0178(10) 0.0123(9) 0.0151(9) 0.0020(7) 0.0055(8) 0.0020(8) N2 0.0184(10) 0.0169(9) 0.0175(10) 0.0027(8) 0.0075(8) 0.0048(8) N11 0.0170(10) 0.0156(9) 0.0160(10) 0.0041(8) 0.0079(8) 0.0028(8) N21 0.0174(10) 0.0163(9) 0.0160(10) 0.0015(8) 0.0068(8) 0.0031(8) N31 0.0178(10) 0.0155(9) 0.0152(10) 0.0017(8) 0.0066(8) 0.0025(8) N41 0.0164(10) 0.0172(9) 0.0165(10) 0.0045(8) 0.0086(8) 0.0027(8) F16C 0.0216(8) 0.0240(8) 0.0274(8) -0.0018(6) 0.0097(7) -0.0021(6) F16B 0.0500(12) 0.0503(11) 0.0195(8) 0.0029(8) 0.0147(8) -0.0182(9) F16A 0.0442(12) 0.0492(11) 0.0374(10) -0.0167(9) 0.0043(9) 0.0299(9) F26C 0.0196(8) 0.0372(9) 0.0294(9) -0.0086(7) 0.0054(7) 0.0027(7) F26B 0.0327(9) 0.0273(8) 0.0225(8) -0.0029(6) 0.0164(7) -0.0012(7) F26A 0.0575(12) 0.0128(7) 0.0323(9) 0.0008(6) 0.0136(9) -0.0032(7) F36A 0.0240(8) 0.0375(9) 0.0253(8) 0.0105(7) 0.0058(7) 0.0056(7) F36B 0.0372(10) 0.0446(10) 0.0200(8) 0.0041(7) 0.0156(7) 0.0136(8) F36C 0.0664(13) 0.0250(8) 0.0277(9) 0.0150(7) 0.0070(9) 0.0050(8) F46C 0.0260(8) 0.0309(8) 0.0201(7) 0.0100(6) 0.0117(6) 0.0077(6) F46B 0.0253(9) 0.0337(9) 0.0295(8) 0.0127(7) 0.0064(7) -0.0040(7) F46A 0.0297(9) 0.0420(9) 0.0309(9) 0.0144(7) 0.0120(7) 0.0213(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N11 1.945(2) . ? Cu1 N1 1.951(2) . ? Cu1 N31 1.976(2) . ? Cu1 Cu2 2.9398(5) . ? Cu2 N41 1.962(2) . ? Cu2 N2 1.963(2) . ? Cu2 N21 1.987(2) . ? C1 N2 1.331(3) . ? C1 C2 1.387(4) . ? C1 H1A 0.9500 . ? C2 C3 1.367(4) . ? C2 H2A 0.9500 . ? C3 C4 1.389(4) . ? C3 H3A 0.9500 . ? C4 N1 1.331(3) . ? C4 H4A 0.9500 . ? C13 N11 1.345(3) . ? C13 C44 1.373(4) 2_866 ? C13 C16 1.493(4) . ? C16 F16A 1.331(3) . ? C16 F16C 1.330(3) . ? C16 F16B 1.346(3) . ? C23 N21 1.348(3) . ? C23 C34 1.380(4) 2_866 ? C23 C26 1.481(3) . ? C26 F26A 1.335(3) . ? C26 F26B 1.340(3) . ? C26 F26C 1.347(3) . ? C33 N31 1.345(3) . ? C33 C34 1.388(3) . ? C33 C36 1.476(4) . ? C34 C23 1.380(4) 2_866 ? C34 H34A 0.9500 . ? C36 F36C 1.332(3) . ? C36 F36B 1.345(3) . ? C36 F36A 1.348(3) . ? C43 N41 1.349(3) . ? C43 C44 1.376(3) . ? C43 C46 1.490(4) . ? C44 C13 1.373(4) 2_866 ? C44 H44A 0.9500 . ? C46 F46B 1.340(3) . ? C46 F46C 1.344(3) . ? C46 F46A 1.342(3) . ? N1 N2 1.353(3) . ? N11 N41 1.354(3) 2_866 ? N21 N31 1.357(3) 2_866 ? N31 N21 1.357(3) 2_866 ? N41 N11 1.354(3) 2_866 ?
1100694.cif	#------------------------------------------------------------------------------ #$Date: 2018-08-16 00:31:59 +0300 (Thu, 16 Aug 2018) $ #$Revision: 209732 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/10/06/1100694.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100694 loop_ _publ_author_name 'Dias, H. V. Rasika' 'Diyabalanage, Himashinie V. K.' 'Gamage, Chammi S. Palehepitiya' _publ_section_title ; Neutral Cu~4~N~12~ and Ag~4~N~12~ metallacycles with a para-cyclophane framework assembled from copper(I) and silver(I) pyrazolates and pyridazine. ; _journal_coden_ASTM CHCOFS _journal_issue 12 _journal_name_full ; Chemical Communications (Cambridge, United Kingdom) ; _journal_page_first 1619 _journal_page_last 1621 _journal_paper_doi 10.1039/b418306a _journal_year 2005 _chemical_formula_sum 'C28 H12 Ag4 F24 N12' _chemical_formula_weight 1403.98 _chemical_name_common ((3,5-(CF3)2PzAg)4(C4H4N2)2) _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 104.477(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 18.142(2) _cell_length_b 22.807(3) _cell_length_c 10.0462(12) _cell_measurement_temperature 101(2) _cell_volume 4024.7(8) _diffrn_ambient_temperature 101(2) _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0245 _diffrn_reflns_av_sigmaI/netI 0.0247 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 22956 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_min 1.16 _exptl_absorpt_coefficient_mu 2.071 _exptl_absorpt_correction_type none _exptl_absorpt_process_details SADABS _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 2.317 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 2672 _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.28 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 613 _refine_ls_number_reflns 6991 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.085 _refine_ls_R_factor_all 0.0329 _refine_ls_R_factor_gt 0.0298 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0430P)^2^+7.1648P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0769 _refine_ls_wR_factor_ref 0.0788 _reflns_number_gt 6417 _reflns_number_total 6991 _reflns_threshold_expression >2sigma(I) _cod_duplicate_entry 7100786 _cod_depositor_comments ; Adding additional information after consulting the original publication and the supplementary material. Antanas Vaitkus, 2018-08-16 The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_sg_symbol_H-M P2(1)/c _cod_database_code 1100694 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag -0.484990(15) 0.580908(12) -0.16061(3) 0.02020(9) Uani 1 1 d . . . Ag2 Ag -0.355622(15) 0.487372(11) 0.08503(3) 0.01909(8) Uani 1 1 d . . . Ag4 Ag 0.136167(15) 0.534027(12) 0.05640(3) 0.02055(9) Uani 1 1 d . . . Ag3 Ag 0.031861(15) 0.403682(12) -0.09653(3) 0.02235(9) Uani 1 1 d . . . N1 N -0.45080(17) 0.44253(13) -0.0946(3) 0.0198(7) Uani 1 1 d . . . N4 N 0.03127(17) 0.54491(13) -0.1472(3) 0.0210(7) Uani 1 1 d . . . F27C F -0.19608(13) 0.42831(11) 0.1890(2) 0.0316(5) Uani 1 1 d . . . N12 N -0.33496(17) 0.58055(12) 0.0694(3) 0.0171(6) Uani 1 1 d . . . F37C F 0.32889(14) 0.50461(11) 0.2287(3) 0.0372(6) Uani 1 1 d . . . F17C F -0.39302(13) 0.72328(10) -0.1980(2) 0.0310(5) Uani 1 1 d . . . N2 N -0.49667(17) 0.47738(14) -0.1883(3) 0.0209(7) Uani 1 1 d . . . F36C F 0.14058(15) 0.28839(11) -0.0852(3) 0.0412(6) Uani 1 1 d . . . N22 N -0.60130(17) 0.60398(13) -0.2794(3) 0.0207(7) Uani 1 1 d . . . F17B F -0.47837(13) 0.72037(11) -0.0842(3) 0.0347(6) Uani 1 1 d . . . F47C F -0.31224(14) 0.29796(12) -0.1645(3) 0.0442(7) Uani 1 1 d . . . F27B F -0.16086(13) 0.44356(11) 0.4064(3) 0.0346(6) Uani 1 1 d . . . N31 N 0.17780(17) 0.44712(13) 0.1133(3) 0.0191(6) Uani 1 1 d . . . N32 N 0.14218(17) 0.39917(13) 0.0476(3) 0.0202(7) Uani 1 1 d . . . N21 N -0.33689(16) 0.41670(13) 0.2408(3) 0.0185(6) Uani 1 1 d . . . F16C F -0.25364(15) 0.56219(13) 0.3620(3) 0.0457(7) Uani 1 1 d . . . N3 N -0.00313(18) 0.49610(14) -0.2062(3) 0.0236(7) Uani 1 1 d . . . F46C F -0.08371(16) 0.25189(14) -0.4298(3) 0.0522(8) Uani 1 1 d . . . F47B F -0.28821(14) 0.38799(11) -0.1006(3) 0.0455(7) Uani 1 1 d . . . F47A F -0.24376(14) 0.31819(13) 0.0352(3) 0.0427(6) Uani 1 1 d . . . F17A F -0.37783(16) 0.77272(10) -0.0106(3) 0.0423(7) Uani 1 1 d . . . F37B F 0.25684(15) 0.50683(12) 0.3669(3) 0.0459(7) Uani 1 1 d . . . F27A F -0.15305(13) 0.35731(10) 0.3272(3) 0.0415(7) Uani 1 1 d . . . F46B F 0.00192(15) 0.31733(11) -0.3537(3) 0.0454(7) Uani 1 1 d . . . F37A F 0.34554(16) 0.44245(12) 0.3929(3) 0.0508(8) Uani 1 1 d . . . C33 C 0.1830(2) 0.35215(16) 0.1036(4) 0.0243(8) Uani 1 1 d . . . N42 N -0.07790(17) 0.35866(13) -0.1745(3) 0.0218(7) Uani 1 1 d . . . N11 N -0.38346(16) 0.61596(13) -0.0222(3) 0.0170(6) Uani 1 1 d . . . C14 C -0.3007(2) 0.67410(16) 0.1241(4) 0.0230(8) Uani 1 1 d . . . H14A H -0.2747 0.7077 0.1684 0.028 Uiso 1 1 calc R . . F16B F -0.18073(14) 0.55219(11) 0.2285(3) 0.0391(6) Uani 1 1 d . . . C44 C -0.1695(2) 0.29041(16) -0.2358(4) 0.0225(8) Uani 1 1 d . . . H44A H -0.1974 0.2568 -0.2758 0.027 Uiso 1 1 calc R . . C13 C -0.2855(2) 0.61598(16) 0.1559(4) 0.0209(8) Uani 1 1 d . . . C34 C 0.2452(2) 0.36825(17) 0.2068(4) 0.0249(8) Uani 1 1 d . . . H34A H 0.2828 0.3437 0.2627 0.030 Uiso 1 1 calc R . . C3 C -0.5478(2) 0.45355(17) -0.2913(4) 0.0227(8) Uani 1 1 d . . . H3A H -0.5793 0.4788 -0.3569 0.027 Uiso 1 1 calc R . . C6 C -0.4581(2) 0.38438(16) -0.1076(4) 0.0214(8) Uani 1 1 d . . . H6A H -0.4255 0.3602 -0.0412 0.026 Uiso 1 1 calc R . . C25 C -0.2753(2) 0.39136(15) 0.3225(4) 0.0191(7) Uani 1 1 d . . . C15 C -0.3627(2) 0.67170(15) 0.0119(4) 0.0193(8) Uani 1 1 d . . . C23 C -0.6266(2) 0.64162(17) -0.3839(4) 0.0241(8) Uani 1 1 d . . . C24 C -0.2951(2) 0.35379(17) 0.4160(4) 0.0249(8) Uani 1 1 d . . . H24A H -0.2628 0.3306 0.4852 0.030 Uiso 1 1 calc R . . F16A F -0.17869(18) 0.63239(11) 0.3364(3) 0.0637(10) Uani 1 1 d . . . C17 C -0.4026(2) 0.72130(16) -0.0701(4) 0.0257(9) Uani 1 1 d . . . F36B F 0.21539(18) 0.25380(11) 0.0951(3) 0.0564(8) Uani 1 1 d . . . C47 C -0.2587(2) 0.33453(17) -0.0982(4) 0.0271(9) Uani 1 1 d . . . C27 C -0.1966(2) 0.40516(16) 0.3107(4) 0.0232(8) Uani 1 1 d . . . C4 C -0.5577(2) 0.39325(18) -0.3082(4) 0.0271(9) Uani 1 1 d . . . H4A H -0.5954 0.3774 -0.3827 0.033 Uiso 1 1 calc R . . F36A F 0.0978(2) 0.27435(14) 0.0898(4) 0.0741(11) Uani 1 1 d . . . C37 C 0.2921(2) 0.47035(18) 0.2980(4) 0.0267(9) Uani 1 1 d . . . F46A F -0.00306(15) 0.23905(11) -0.2390(3) 0.0432(7) Uani 1 1 d . . . N41 N -0.13538(17) 0.37386(13) -0.1164(3) 0.0214(7) Uani 1 1 d . . . F26C F -0.55387(19) 0.72683(13) -0.3879(4) 0.0611(9) Uani 1 1 d . . . F26B F -0.50540(16) 0.64727(14) -0.4293(3) 0.0564(8) Uani 1 1 d . . . C35 C 0.2397(2) 0.42848(17) 0.2093(4) 0.0215(8) Uani 1 1 d . . . C45 C -0.1898(2) 0.33250(15) -0.1539(4) 0.0202(8) Uani 1 1 d . . . F26A F -0.59938(19) 0.6831(2) -0.5776(3) 0.0833(13) Uani 1 1 d . . . C43 C -0.0986(2) 0.30890(15) -0.2458(4) 0.0217(8) Uani 1 1 d . . . C46 C -0.0459(2) 0.27988(17) -0.3178(4) 0.0294(9) Uani 1 1 d . . . C9 C 0.0116(2) 0.59631(17) -0.2101(4) 0.0268(9) Uani 1 1 d . . . H9A H 0.0360 0.6308 -0.1677 0.032 Uiso 1 1 calc R . . C5 C -0.5115(2) 0.35778(17) -0.2140(4) 0.0254(8) Uani 1 1 d . . . H5A H -0.5155 0.3163 -0.2209 0.030 Uiso 1 1 calc R . . C12 C -0.0551(3) 0.49944(19) -0.3240(5) 0.0357(10) Uani 1 1 d . . . H12A H -0.0788 0.4643 -0.3639 0.043 Uiso 1 1 calc R . . C26 C -0.5728(2) 0.6739(2) -0.4473(4) 0.0330(10) Uani 1 1 d . . . C10 C -0.0423(3) 0.60173(19) -0.3333(5) 0.0380(11) Uani 1 1 d . . . H10A H -0.0549 0.6389 -0.3754 0.046 Uiso 1 1 calc R . . C11 C -0.0768(3) 0.5519(2) -0.3924(5) 0.0468(13) Uani 1 1 d . . . H11A H -0.1144 0.5530 -0.4774 0.056 Uiso 1 1 calc R . . C36 C 0.1585(3) 0.29229(18) 0.0530(5) 0.0355(10) Uani 1 1 d . . . C16 C -0.2254(2) 0.59090(16) 0.2702(4) 0.0274(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.01652(15) 0.02391(16) 0.02004(16) 0.00148(11) 0.00433(12) -0.00076(10) Ag2 0.01941(15) 0.01561(14) 0.02282(16) 0.00377(10) 0.00634(12) -0.00007(10) Ag4 0.02069(16) 0.01687(15) 0.02489(17) -0.00089(11) 0.00723(12) 0.00167(10) Ag3 0.01750(15) 0.02436(16) 0.02543(17) -0.00371(12) 0.00580(12) -0.00099(11) N1 0.0166(15) 0.0215(16) 0.0229(17) 0.0002(13) 0.0079(13) -0.0006(12) N4 0.0201(16) 0.0181(15) 0.0246(18) -0.0003(13) 0.0049(14) -0.0012(12) F27C 0.0244(12) 0.0431(14) 0.0292(13) 0.0045(11) 0.0101(10) -0.0048(10) N12 0.0163(15) 0.0164(15) 0.0180(16) 0.0024(12) 0.0029(13) 0.0009(11) F37C 0.0352(14) 0.0426(14) 0.0337(14) 0.0014(11) 0.0083(12) -0.0154(11) F17C 0.0362(13) 0.0319(12) 0.0279(13) 0.0122(10) 0.0137(11) 0.0093(10) N2 0.0186(16) 0.0250(16) 0.0195(17) 0.0002(13) 0.0055(14) 0.0012(13) F36C 0.0414(15) 0.0301(13) 0.0484(17) -0.0076(12) 0.0045(13) -0.0055(11) N22 0.0200(16) 0.0198(15) 0.0228(17) 0.0036(13) 0.0062(14) -0.0002(12) F17B 0.0290(13) 0.0354(13) 0.0418(15) 0.0114(11) 0.0128(11) 0.0148(10) F47C 0.0300(14) 0.0565(17) 0.0482(17) -0.0149(13) 0.0138(12) -0.0232(12) F27B 0.0292(13) 0.0383(14) 0.0325(14) -0.0048(11) 0.0003(11) -0.0110(11) N31 0.0181(15) 0.0191(15) 0.0209(17) 0.0013(13) 0.0063(13) 0.0012(12) N32 0.0189(16) 0.0211(16) 0.0211(17) 0.0014(13) 0.0062(14) 0.0004(12) N21 0.0159(15) 0.0182(15) 0.0212(17) 0.0038(12) 0.0043(13) -0.0005(12) F16C 0.0405(15) 0.0691(19) 0.0283(14) 0.0231(13) 0.0104(12) 0.0124(13) N3 0.0220(16) 0.0210(16) 0.0261(19) -0.0019(13) 0.0026(15) -0.0016(13) F46C 0.0428(16) 0.0681(19) 0.0453(17) -0.0337(15) 0.0105(14) -0.0001(14) F47B 0.0330(14) 0.0328(14) 0.079(2) 0.0133(13) 0.0299(14) 0.0101(11) F47A 0.0421(15) 0.0572(17) 0.0322(15) 0.0063(12) 0.0155(12) 0.0029(12) F17A 0.0585(17) 0.0152(11) 0.0447(16) 0.0015(11) -0.0028(14) 0.0037(11) F37B 0.0439(16) 0.0529(17) 0.0443(17) -0.0237(13) 0.0172(13) -0.0070(13) F27A 0.0216(12) 0.0295(13) 0.074(2) 0.0061(13) 0.0131(13) 0.0065(10) F46B 0.0508(16) 0.0330(14) 0.0658(19) -0.0092(13) 0.0394(15) -0.0023(12) F37A 0.0441(16) 0.0456(16) 0.0448(17) 0.0075(13) -0.0223(14) -0.0024(13) C33 0.023(2) 0.0224(19) 0.029(2) 0.0047(16) 0.0081(17) -0.0006(15) N42 0.0187(16) 0.0199(15) 0.0270(18) -0.0026(13) 0.0061(14) 0.0006(12) N11 0.0149(15) 0.0190(15) 0.0180(16) 0.0018(12) 0.0058(13) 0.0003(12) C14 0.026(2) 0.0174(18) 0.026(2) -0.0026(15) 0.0069(17) -0.0027(15) F16B 0.0333(14) 0.0456(15) 0.0387(15) 0.0132(12) 0.0094(12) 0.0162(12) C44 0.023(2) 0.0194(18) 0.023(2) -0.0009(15) 0.0013(16) -0.0030(15) C13 0.0218(19) 0.0207(18) 0.020(2) 0.0023(15) 0.0042(16) -0.0002(15) C34 0.024(2) 0.025(2) 0.026(2) 0.0089(16) 0.0075(17) 0.0061(16) C3 0.0203(19) 0.027(2) 0.021(2) -0.0021(16) 0.0041(16) 0.0020(15) C6 0.0191(18) 0.0195(18) 0.028(2) 0.0034(15) 0.0108(17) 0.0025(14) C25 0.0197(19) 0.0170(17) 0.0188(19) -0.0002(14) 0.0017(15) 0.0004(14) C15 0.0188(18) 0.0184(18) 0.023(2) 0.0036(15) 0.0089(16) 0.0015(14) C23 0.027(2) 0.026(2) 0.020(2) 0.0042(16) 0.0060(17) -0.0024(16) C24 0.024(2) 0.029(2) 0.021(2) 0.0064(16) 0.0026(17) 0.0018(16) F16A 0.067(2) 0.0262(14) 0.068(2) 0.0020(14) -0.0407(17) -0.0075(13) C17 0.032(2) 0.0186(19) 0.028(2) 0.0033(16) 0.0097(18) 0.0023(16) F36B 0.067(2) 0.0246(14) 0.067(2) 0.0045(13) -0.0021(17) 0.0084(13) C47 0.024(2) 0.026(2) 0.029(2) 0.0007(17) 0.0049(18) -0.0007(16) C27 0.0177(19) 0.0227(19) 0.026(2) 0.0008(16) 0.0007(17) 0.0005(15) C4 0.027(2) 0.029(2) 0.025(2) -0.0102(17) 0.0066(18) -0.0034(16) F36A 0.088(2) 0.0509(18) 0.107(3) -0.0169(19) 0.068(2) -0.0408(18) C37 0.025(2) 0.032(2) 0.022(2) 0.0027(17) 0.0030(17) 0.0025(16) F46A 0.0426(15) 0.0339(14) 0.0558(18) -0.0006(12) 0.0174(13) 0.0177(12) N41 0.0188(16) 0.0207(16) 0.0252(18) -0.0024(13) 0.0062(14) 0.0016(12) F26C 0.070(2) 0.0481(18) 0.077(2) -0.0018(16) 0.0403(19) -0.0244(16) F26B 0.0447(17) 0.067(2) 0.069(2) 0.0208(16) 0.0356(16) 0.0024(14) C35 0.0202(19) 0.0275(19) 0.019(2) 0.0039(15) 0.0088(16) 0.0013(15) C45 0.0173(18) 0.0175(17) 0.023(2) 0.0013(15) 0.0006(16) -0.0005(14) F26A 0.057(2) 0.151(4) 0.0361(18) 0.041(2) 0.0007(15) -0.043(2) C43 0.0236(19) 0.0150(17) 0.025(2) -0.0020(15) 0.0037(16) 0.0028(14) C46 0.030(2) 0.025(2) 0.035(2) -0.0095(18) 0.0094(19) -0.0040(17) C9 0.026(2) 0.025(2) 0.030(2) 0.0055(17) 0.0089(18) -0.0007(16) C5 0.026(2) 0.0206(19) 0.032(2) -0.0059(16) 0.0115(18) -0.0024(15) C12 0.039(3) 0.030(2) 0.032(3) -0.0027(19) -0.003(2) -0.0075(19) C26 0.033(2) 0.041(3) 0.026(2) 0.0113(19) 0.0104(19) -0.0032(19) C10 0.038(3) 0.030(2) 0.039(3) 0.0121(19) -0.003(2) 0.0005(19) C11 0.052(3) 0.038(3) 0.034(3) 0.007(2) -0.018(2) -0.005(2) C36 0.035(2) 0.022(2) 0.048(3) 0.0087(19) 0.006(2) 0.0004(18) C16 0.030(2) 0.0180(19) 0.030(2) 0.0003(16) -0.0011(19) -0.0044(16) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N11 2.165(3) . ? Ag1 N22 2.212(3) . ? Ag1 N2 2.381(3) . ? Ag2 N12 2.170(3) . ? Ag2 N21 2.213(3) . ? Ag2 N1 2.393(3) . ? Ag4 N31 2.147(3) . ? Ag4 N41 2.186(3) 3_565 ? Ag4 N4 2.433(3) . ? Ag3 N32 2.160(3) . ? Ag3 N42 2.203(3) . ? Ag3 N3 2.389(3) . ? N1 C6 1.336(5) . ? N1 N2 1.348(4) . ? N4 C9 1.337(5) . ? N4 N3 1.340(4) . ? F27C C27 1.335(5) . ? N12 C13 1.351(5) . ? N12 N11 1.367(4) . ? F37C C37 1.332(5) . ? F17C C17 1.340(5) . ? N2 C3 1.322(5) . ? F36C C36 1.347(5) . ? N22 C23 1.345(5) . ? N22 N21 1.359(4) 3_465 ? F17B C17 1.346(5) . ? F47C C47 1.326(5) . ? F27B C27 1.341(5) . ? N31 C35 1.353(5) . ? N31 N32 1.355(4) . ? N32 C33 1.344(5) . ? N21 C25 1.341(5) . ? N21 N22 1.359(4) 3_465 ? F16C C16 1.334(5) . ? N3 C12 1.318(6) . ? F46C C46 1.326(5) . ? F47B C47 1.329(5) . ? F47A C47 1.352(5) . ? F17A C17 1.341(5) . ? F37B C37 1.342(5) . ? F27A C27 1.333(4) . ? F46B C46 1.330(5) . ? F37A C37 1.339(5) . ? C33 C34 1.378(6) . ? C33 C36 1.485(6) . ? N42 C43 1.344(5) . ? N42 N41 1.361(4) . ? N11 C15 1.345(5) . ? C14 C13 1.375(5) . ? C14 C15 1.381(5) . ? F16B C16 1.335(5) . ? C44 C45 1.373(5) . ? C44 C43 1.382(5) . ? C13 C16 1.485(6) . ? C34 C35 1.378(5) . ? C3 C4 1.392(6) . ? C6 C5 1.389(6) . ? C25 C24 1.383(5) . ? C25 C27 1.496(5) . ? C15 C17 1.478(5) . ? C23 C24 1.380(5) 3_465 ? C23 C26 1.488(5) . ? C24 C23 1.380(5) 3_465 ? F16A C16 1.332(5) . ? F36B C36 1.340(5) . ? C47 C45 1.492(5) . ? C4 C5 1.363(6) . ? F36A C36 1.313(5) . ? C37 C35 1.478(6) . ? F46A C46 1.338(5) . ? N41 C45 1.349(5) . ? N41 Ag4 2.186(3) 3_565 ? F26C C26 1.352(5) . ? F26B C26 1.336(5) . ? F26A C26 1.294(5) . ? C43 C46 1.490(5) . ? C9 C10 1.378(6) . ? C12 C11 1.387(6) . ? C10 C11 1.361(7) . ?
1100695.cif	#------------------------------------------------------------------------------ #$Date: 2018-08-16 00:31:59 +0300 (Thu, 16 Aug 2018) $ #$Revision: 209732 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/10/06/1100695.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100695 loop_ _publ_author_name 'Dias, H. V. Rasika' 'Diyabalanage, Himashinie V. K.' 'Gamage, Chammi S. Palehepitiya' _publ_section_title ; Neutral Cu~4~N~12~ and Ag~4~N~12~ metallacycles with a para-cyclophane framework assembled from copper(I) and silver(I) pyrazolates and pyridazine. ; _journal_coden_ASTM CHCOFS _journal_issue 12 _journal_name_full ; Chemical Communications (Cambridge, United Kingdom) ; _journal_page_first 1619 _journal_page_last 1621 _journal_paper_doi 10.1039/b418306a _journal_year 2005 _chemical_formula_sum 'C28 H13 Cl2 Cu3 F18 N8' _chemical_formula_weight 1064.98 _chemical_name_common ((3,5-(CF3)2PzCu)3(C12H8N2)) _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 99.060(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 9.2674(14) _cell_length_b 15.769(2) _cell_length_c 23.946(4) _cell_measurement_reflns_used 7362 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 28.34 _cell_measurement_theta_min 2.51 _cell_volume 3455.7(9) _diffrn_ambient_temperature 100(2) _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0442 _diffrn_reflns_av_sigmaI/netI 0.0392 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_number 27148 _diffrn_reflns_theta_max 26.00 _diffrn_reflns_theta_min 1.72 _exptl_absorpt_coefficient_mu 2.119 _exptl_absorpt_correction_type none _exptl_absorpt_process_details SADABS _exptl_crystal_colour 'dark orange' _exptl_crystal_density_diffrn 2.047 _exptl_crystal_density_meas 0 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plates _exptl_crystal_F_000 2080 _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.03 _refine_ls_extinction_coef 0.00000(17) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.190 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 533 _refine_ls_number_reflns 6798 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.190 _refine_ls_R_factor_all 0.0665 _refine_ls_R_factor_gt 0.0554 _refine_ls_shift/su_max 3.997 _refine_ls_shift/su_mean 0.008 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0496P)^2^+16.3200P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1397 _refine_ls_wR_factor_ref 0.1444 _reflns_number_gt 5712 _reflns_number_total 6798 _reflns_threshold_expression >2sigma(I) _cod_duplicate_entry 7100787 _cod_depositor_comments ; Adding additional information after consulting the original publication and the supplementary material. Antanas Vaitkus, 2018-08-16 The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_sg_symbol_H-M P2(1)/n _cod_database_code 1100695 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.40401(7) 0.12369(4) 0.22880(3) 0.02177(17) Uani 1 1 d . . . Cu2 Cu 0.36570(6) 0.13439(4) 0.35200(3) 0.02058(17) Uani 1 1 d . . . Cu3 Cu 0.16688(6) 0.24935(4) 0.26406(3) 0.02003(17) Uani 1 1 d . . . F11 F -0.1445(4) 0.3148(2) 0.28720(15) 0.0364(8) Uani 1 1 d . . . N2 N 0.5641(5) 0.1210(3) 0.33834(18) 0.0203(9) Uani 1 1 d . . . F18 F 0.0307(4) 0.3987(2) 0.19542(14) 0.0344(8) Uani 1 1 d . . . F12 F -0.1672(4) 0.3791(3) 0.36478(16) 0.0440(9) Uani 1 1 d . . . F5 F 0.6796(4) 0.2003(2) 0.45054(14) 0.0397(9) Uani 1 1 d . . . N1 N 0.5814(4) 0.1178(3) 0.28343(18) 0.0187(9) Uani 1 1 d . . . N3 N 0.2237(5) 0.2078(3) 0.37945(18) 0.0203(9) Uani 1 1 d . . . F10 F -0.0122(4) 0.4233(2) 0.31297(17) 0.0411(9) Uani 1 1 d . . . C26 C 0.1424(6) -0.0077(4) 0.3855(2) 0.0242(11) Uani 1 1 d . . . H26 H 0.2076 0.0298 0.4080 0.029 Uiso 1 1 calc R . . N4 N 0.1353(5) 0.2522(3) 0.33911(18) 0.0208(9) Uani 1 1 d . . . F16 F -0.0102(4) 0.4068(2) 0.10494(16) 0.0459(10) Uani 1 1 d . . . F6 F 0.6380(4) 0.0680(2) 0.45534(15) 0.0444(9) Uani 1 1 d . . . F8 F 0.1901(6) 0.1148(3) 0.49507(17) 0.0576(12) Uani 1 1 d . . . F9 F 0.2507(5) 0.2360(3) 0.52704(15) 0.0482(10) Uani 1 1 d . . . F4 F 0.8578(4) 0.1136(3) 0.45510(16) 0.0531(11) Uani 1 1 d . . . N6 N 0.3020(4) 0.1983(3) 0.17194(18) 0.0209(9) Uani 1 1 d . . . N8 N 0.2447(4) 0.0362(3) 0.30468(18) 0.0186(9) Uani 1 1 d . . . N5 N 0.1966(4) 0.2488(3) 0.18887(18) 0.0208(9) Uani 1 1 d . . . F17 F -0.1143(3) 0.3102(2) 0.14751(18) 0.0436(10) Uani 1 1 d . . . N7 N 0.2554(4) 0.0322(3) 0.25164(18) 0.0188(9) Uani 1 1 d . . . C23 C -0.0445(6) -0.1217(4) 0.3202(2) 0.0273(12) Uani 1 1 d . . . H23 H -0.1077 -0.1614 0.2989 0.033 Uiso 1 1 calc R . . C8 C 0.0419(6) 0.2969(4) 0.3653(2) 0.0268(12) Uani 1 1 d . . . F2 F 0.7362(5) 0.1734(3) 0.19335(18) 0.0610(13) Uani 1 1 d . . . C17 C 0.1954(6) -0.0268(4) 0.1593(2) 0.0260(12) Uani 1 1 d . . . H17 H 0.2598 0.0127 0.1461 0.031 Uiso 1 1 calc R . . C27 C 0.1477(5) -0.0172(3) 0.3274(2) 0.0201(10) Uani 1 1 d . . . F3 F 0.9280(3) 0.1132(3) 0.23523(16) 0.0402(9) Uani 1 1 d . . . C16 C 0.1752(5) -0.0263(3) 0.2160(2) 0.0200(10) Uani 1 1 d . . . C20 C 0.0029(6) -0.1424(4) 0.1972(2) 0.0258(12) Uani 1 1 d . . . H20 H -0.0627 -0.1819 0.2096 0.031 Uiso 1 1 calc R . . C18 C 0.1207(6) -0.0850(4) 0.1230(2) 0.0266(12) Uani 1 1 d . . . H18 H 0.1341 -0.0861 0.0844 0.032 Uiso 1 1 calc R . . C15 C 0.4041(6) 0.1702(4) 0.0846(2) 0.0294(13) Uani 1 1 d . . . C7 C 0.0673(6) 0.2836(4) 0.4225(2) 0.0271(12) Uani 1 1 d . . . H7 H 0.0176 0.3073 0.4506 0.033 Uiso 1 1 calc R . . C3 C 0.6995(6) 0.1183(3) 0.3700(2) 0.0227(11) Uani 1 1 d . . . C12 C 0.1989(6) 0.2762(4) 0.0970(2) 0.0255(12) Uani 1 1 d . . . H12 H 0.1772 0.2995 0.0600 0.031 Uiso 1 1 calc R . . F1 F 0.7471(5) 0.0397(3) 0.19815(18) 0.0598(13) Uani 1 1 d . . . C13 C 0.3020(6) 0.2150(4) 0.1170(2) 0.0231(11) Uani 1 1 d . . . C2 C 0.8042(6) 0.1134(4) 0.3357(2) 0.0260(12) Uani 1 1 d . . . H2 H 0.9072 0.1113 0.3468 0.031 Uiso 1 1 calc R . . C25 C 0.0411(6) -0.0535(4) 0.4091(2) 0.0265(12) Uani 1 1 d . . . H25 H 0.0355 -0.0473 0.4481 0.032 Uiso 1 1 calc R . . C11 C 0.1361(6) 0.2949(3) 0.1437(2) 0.0227(11) Uani 1 1 d . . . C14 C 0.0102(6) 0.3525(4) 0.1480(2) 0.0279(12) Uani 1 1 d . . . F13 F 0.4279(5) 0.0901(3) 0.10024(19) 0.0544(11) Uani 1 1 d . . . C19 C 0.0246(6) -0.1430(4) 0.1424(2) 0.0289(12) Uani 1 1 d . . . H19 H -0.0258 -0.1831 0.1169 0.035 Uiso 1 1 calc R . . C5 C 0.7163(6) 0.1245(4) 0.4324(2) 0.0276(12) Uani 1 1 d . . . C21 C 0.0772(5) -0.0831(3) 0.2362(2) 0.0201(11) Uani 1 1 d . . . C22 C 0.0584(5) -0.0759(3) 0.2940(2) 0.0209(11) Uani 1 1 d . . . C1 C 0.7275(5) 0.1124(3) 0.2818(2) 0.0206(11) Uani 1 1 d . . . C24 C -0.0532(6) -0.1089(4) 0.3760(2) 0.0279(12) Uani 1 1 d . . . H24 H -0.1251 -0.1385 0.3926 0.033 Uiso 1 1 calc R . . F14 F 0.5371(4) 0.2036(3) 0.0921(2) 0.0711(16) Uani 1 1 d . . . F7 F 0.3933(5) 0.1677(5) 0.48124(17) 0.086(2) Uani 1 1 d . . . F15 F 0.3581(6) 0.1710(4) 0.03063(17) 0.0796(18) Uani 1 1 d . . . C6 C 0.1842(6) 0.2268(4) 0.4294(2) 0.0230(11) Uani 1 1 d . . . C4 C 0.7821(6) 0.1103(4) 0.2275(2) 0.0250(12) Uani 1 1 d . . . C10 C -0.0707(6) 0.3539(4) 0.3329(3) 0.0277(12) Uani 1 1 d . . . C9 C 0.2572(6) 0.1864(4) 0.4830(2) 0.0300(13) Uani 1 1 d . . . Cl1 Cl 0.99165(18) 0.10232(12) 0.04221(8) 0.0468(4) Uani 1 1 d . . . Cl2 Cl 0.69847(19) 0.03011(13) 0.01966(9) 0.0547(5) Uani 1 1 d . . . C28 C 0.8361(8) 0.0728(5) 0.0716(3) 0.0434(16) Uani 1 1 d . . . H28A H 0.7972 0.1231 0.0890 0.052 Uiso 1 1 calc R . . H28B H 0.8643 0.0301 0.1016 0.052 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0145(3) 0.0307(4) 0.0197(3) 0.0004(3) 0.0014(2) 0.0040(3) Cu2 0.0132(3) 0.0284(4) 0.0203(3) 0.0011(3) 0.0035(2) 0.0022(2) Cu3 0.0141(3) 0.0259(3) 0.0200(3) 0.0005(3) 0.0023(2) 0.0002(2) F11 0.0268(18) 0.040(2) 0.038(2) -0.0013(16) -0.0103(15) 0.0034(15) N2 0.016(2) 0.023(2) 0.021(2) 0.0008(18) -0.0012(17) 0.0007(17) F18 0.0319(18) 0.0354(19) 0.0349(19) -0.0065(15) 0.0028(15) 0.0064(15) F12 0.0248(18) 0.062(3) 0.046(2) -0.0034(19) 0.0087(16) 0.0189(17) F5 0.049(2) 0.040(2) 0.0289(19) -0.0091(16) 0.0012(16) 0.0003(17) N1 0.0125(19) 0.023(2) 0.022(2) -0.0034(17) 0.0058(16) 0.0013(16) N3 0.017(2) 0.026(2) 0.017(2) -0.0002(18) 0.0014(17) -0.0010(17) F10 0.0229(17) 0.0331(19) 0.065(3) 0.0094(18) -0.0003(17) 0.0040(14) C26 0.018(3) 0.027(3) 0.028(3) 0.003(2) 0.004(2) 0.001(2) N4 0.016(2) 0.025(2) 0.020(2) -0.0005(18) 0.0009(17) -0.0006(17) F16 0.052(2) 0.045(2) 0.040(2) 0.0162(18) 0.0051(18) 0.0239(19) F6 0.057(2) 0.047(2) 0.0293(19) 0.0047(17) 0.0076(17) -0.0135(19) F8 0.087(3) 0.043(2) 0.036(2) 0.0058(18) -0.010(2) -0.008(2) F9 0.073(3) 0.047(2) 0.0237(18) -0.0070(16) 0.0037(18) -0.009(2) F4 0.0224(18) 0.101(3) 0.032(2) 0.001(2) -0.0080(15) 0.016(2) N6 0.0118(19) 0.029(2) 0.023(2) 0.0037(19) 0.0040(17) 0.0005(17) N8 0.0105(19) 0.024(2) 0.022(2) 0.0021(18) 0.0038(16) 0.0015(16) N5 0.013(2) 0.026(2) 0.022(2) 0.0013(19) 0.0012(17) -0.0025(17) F17 0.0129(16) 0.045(2) 0.071(3) -0.0104(19) -0.0003(16) 0.0009(15) N7 0.0102(19) 0.023(2) 0.023(2) -0.0004(18) 0.0023(16) 0.0014(16) C23 0.015(2) 0.031(3) 0.036(3) 0.001(2) 0.003(2) -0.001(2) C8 0.014(2) 0.035(3) 0.032(3) -0.003(2) 0.005(2) 0.001(2) F2 0.060(3) 0.083(3) 0.048(2) 0.033(2) 0.032(2) 0.038(2) C17 0.016(2) 0.032(3) 0.029(3) 0.001(2) 0.000(2) 0.004(2) C27 0.012(2) 0.023(3) 0.025(3) 0.000(2) 0.0024(19) -0.0002(19) F3 0.0165(16) 0.062(2) 0.045(2) -0.0054(18) 0.0119(15) -0.0042(16) C16 0.012(2) 0.026(3) 0.021(3) 0.000(2) -0.0018(19) 0.003(2) C20 0.015(2) 0.028(3) 0.034(3) -0.004(2) 0.003(2) -0.001(2) C18 0.020(3) 0.033(3) 0.027(3) -0.006(2) 0.002(2) 0.006(2) C15 0.029(3) 0.037(3) 0.026(3) 0.004(2) 0.013(2) 0.000(2) C7 0.017(3) 0.035(3) 0.029(3) -0.007(2) 0.004(2) 0.001(2) C3 0.017(2) 0.026(3) 0.023(3) -0.002(2) -0.003(2) -0.001(2) C12 0.022(3) 0.034(3) 0.020(3) 0.003(2) -0.001(2) -0.005(2) F1 0.062(3) 0.073(3) 0.053(3) -0.039(2) 0.036(2) -0.044(2) C13 0.020(3) 0.028(3) 0.022(3) 0.003(2) 0.004(2) -0.003(2) C2 0.014(2) 0.030(3) 0.032(3) 0.001(2) -0.001(2) 0.002(2) C25 0.021(3) 0.032(3) 0.028(3) 0.005(2) 0.009(2) 0.002(2) C11 0.020(3) 0.022(3) 0.024(3) 0.002(2) -0.002(2) -0.005(2) C14 0.026(3) 0.030(3) 0.026(3) 0.001(2) 0.000(2) -0.001(2) F13 0.064(3) 0.039(2) 0.072(3) 0.007(2) 0.046(2) 0.008(2) C19 0.021(3) 0.032(3) 0.031(3) -0.007(2) -0.006(2) 0.003(2) C5 0.017(3) 0.036(3) 0.028(3) 0.002(2) -0.001(2) 0.006(2) C21 0.010(2) 0.019(2) 0.029(3) 0.000(2) -0.003(2) 0.0049(19) C22 0.010(2) 0.023(3) 0.030(3) 0.003(2) 0.003(2) 0.0012(19) C1 0.012(2) 0.023(3) 0.027(3) 0.000(2) 0.002(2) -0.0008(19) C24 0.015(2) 0.033(3) 0.036(3) 0.009(2) 0.006(2) 0.001(2) F14 0.030(2) 0.064(3) 0.128(4) -0.044(3) 0.040(3) -0.016(2) F7 0.032(2) 0.196(6) 0.034(2) 0.034(3) 0.0115(18) 0.049(3) F15 0.080(3) 0.136(5) 0.025(2) 0.005(3) 0.013(2) 0.066(3) C6 0.016(2) 0.029(3) 0.024(3) -0.004(2) 0.005(2) -0.001(2) C4 0.014(2) 0.031(3) 0.031(3) -0.002(2) 0.007(2) 0.000(2) C10 0.014(2) 0.033(3) 0.037(3) -0.003(3) 0.005(2) 0.002(2) C9 0.022(3) 0.049(4) 0.019(3) -0.002(3) 0.006(2) 0.003(3) Cl1 0.0363(9) 0.0473(10) 0.0532(10) -0.0021(8) -0.0037(7) -0.0025(7) Cl2 0.0362(9) 0.0635(12) 0.0673(12) -0.0124(10) 0.0171(8) -0.0095(8) C28 0.041(4) 0.055(4) 0.035(4) 0.002(3) 0.007(3) 0.013(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N6 1.930(4) . ? Cu1 N1 1.936(4) . ? Cu1 N7 2.125(4) . ? Cu1 Cu2 3.0311(10) . ? Cu2 N2 1.929(4) . ? Cu2 N3 1.943(4) . ? Cu2 N8 2.130(4) . ? Cu3 N5 1.864(4) . ? Cu3 N4 1.866(4) . ? F11 C10 1.344(7) . ? N2 N1 1.351(6) . ? N2 C3 1.361(6) . ? F18 C14 1.338(7) . ? F12 C10 1.326(6) . ? F5 C5 1.333(7) . ? N1 C1 1.363(6) . ? N3 C6 1.339(7) . ? N3 N4 1.359(6) . ? F10 C10 1.342(7) . ? C26 C25 1.374(8) . ? C26 C27 1.409(7) . ? C26 H26 0.9500 . ? N4 C8 1.345(7) . ? F16 C14 1.330(7) . ? F6 C5 1.323(7) . ? F8 C9 1.341(8) . ? F9 C9 1.322(7) . ? F4 C5 1.349(6) . ? N6 C13 1.342(7) . ? N6 N5 1.371(6) . ? N8 N7 1.291(6) . ? N8 C27 1.402(6) . ? N5 C11 1.350(7) . ? F17 C14 1.331(7) . ? N7 C16 1.390(7) . ? C23 C24 1.365(8) . ? C23 C22 1.418(7) . ? C23 H23 0.9500 . ? C8 C7 1.369(8) . ? C8 C10 1.499(8) . ? F2 C4 1.316(7) . ? C17 C18 1.375(8) . ? C17 C16 1.401(8) . ? C17 H17 0.9500 . ? C27 C22 1.405(7) . ? F3 C4 1.336(6) . ? C16 C21 1.413(7) . ? C20 C19 1.359(8) . ? C20 C21 1.420(7) . ? C20 H20 0.9500 . ? C18 C19 1.406(8) . ? C18 H18 0.9500 . ? C15 F15 1.295(7) . ? C15 F13 1.326(7) . ? C15 F14 1.327(7) . ? C15 C13 1.492(8) . ? C7 C6 1.395(8) . ? C7 H7 0.9500 . ? C3 C2 1.370(8) . ? C3 C5 1.480(8) . ? C12 C11 1.371(8) . ? C12 C13 1.390(8) . ? C12 H12 0.9500 . ? F1 C4 1.327(7) . ? C2 C1 1.372(8) . ? C2 H2 0.9500 . ? C25 C24 1.393(8) . ? C25 H25 0.9500 . ? C11 C14 1.495(8) . ? C19 H19 0.9500 . ? C21 C22 1.428(8) . ? C1 C4 1.469(7) . ? C24 H24 0.9500 . ? F7 C9 1.303(7) . ? C6 C9 1.496(8) . ? Cl1 C28 1.763(7) . ? Cl2 C28 1.768(7) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ?
1100696.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100696.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100696 _chemical_formula_sum 'C12 H12 Cu I N2 S' _chemical_formula_weight 406.74 _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 110.1120(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 8.0239(5) _cell_length_b 18.7101(11) _cell_length_c 9.5160(6) _cell_measurement_reflns_used ? _cell_measurement_temperature 293(2) _cell_measurement_theta_max ? _cell_measurement_theta_min ? _cell_volume 1341.50(14) _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0389 _diffrn_reflns_av_sigmaI/netI 0.0233 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 17040 _diffrn_reflns_theta_full 26.42 _diffrn_reflns_theta_max 26.42 _diffrn_reflns_theta_min 2.18 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _exptl_absorpt_coefficient_mu 4.063 _exptl_absorpt_correction_T_max ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_crystal_colour red _exptl_crystal_density_diffrn 2.014 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description hexagonal _exptl_crystal_F_000 784 _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _refine_diff_density_max 1.197 _refine_diff_density_min -0.803 _refine_diff_density_rms 0.140 _refine_ls_extinction_coef 0.0050(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 155 _refine_ls_number_reflns 2747 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.052 _refine_ls_R_factor_all 0.0313 _refine_ls_R_factor_gt 0.0276 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0430P)^2^+1.1676P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0698 _refine_ls_wR_factor_ref 0.0715 _reflns_number_gt 2514 _reflns_number_total 2747 _reflns_threshold_expression >2sigma(I) _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_sg_symbol_H-M P2(1)/c _cod_database_code 1100696 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2103(4) 0.87490(18) 0.9903(4) 0.0298(7) Uani 1 1 d . . . H1 H 0.2003 0.9147 0.9294 0.036 Uiso 1 1 calc R . . C2 C 0.0615(5) 0.8345(2) 0.9710(4) 0.0355(8) Uani 1 1 d . . . H2 H -0.0462 0.8465 0.8982 0.043 Uiso 1 1 calc R . . C3 C 0.0752(5) 0.7758(2) 1.0619(5) 0.0442(10) Uani 1 1 d . . . H3 H -0.0238 0.7477 1.0523 0.053 Uiso 1 1 calc R . . C4 C 0.2375(5) 0.75931(19) 1.1671(5) 0.0388(9) Uani 1 1 d . . . H4 H 0.2485 0.7201 1.2296 0.047 Uiso 1 1 calc R . . C5 C 0.3849(4) 0.80132(17) 1.1798(4) 0.0251(6) Uani 1 1 d . . . C6 C 0.5645(4) 0.78286(17) 1.2915(4) 0.0280(7) Uani 1 1 d . . . H6A H 0.6554 0.8016 1.2558 0.034 Uiso 1 1 calc R . . H6B H 0.5769 0.7313 1.2972 0.034 Uiso 1 1 calc R . . C7 C 0.6609(4) 0.90951(17) 1.4586(4) 0.0262(7) Uani 1 1 d . . . H7A H 0.5637 0.9324 1.3809 0.031 Uiso 1 1 calc R . . H7B H 0.6776 0.9346 1.5516 0.031 Uiso 1 1 calc R . . C8 C 0.8264(4) 0.91612(16) 1.4204(3) 0.0209(6) Uani 1 1 d . . . C9 C 0.9938(5) 0.90717(18) 1.5284(3) 0.0281(7) Uani 1 1 d . . . H9 H 1.0043 0.8980 1.6272 0.034 Uiso 1 1 calc R . . C10 C 1.1444(5) 0.91184(19) 1.4895(4) 0.0318(7) Uani 1 1 d . . . H10 H 1.2566 0.9058 1.5610 0.038 Uiso 1 1 calc R . . C11 C 1.1246(4) 0.92564(18) 1.3423(4) 0.0302(7) Uani 1 1 d . . . H11 H 1.2233 0.9288 1.3126 0.036 Uiso 1 1 calc R . . C12 C 0.9555(4) 0.93468(16) 1.2396(4) 0.0251(7) Uani 1 1 d . . . H12 H 0.9431 0.9450 1.1410 0.030 Uiso 1 1 calc R . . N1 N 0.3710(3) 0.86001(14) 1.0932(3) 0.0250(6) Uani 1 1 d . . . N2 N 0.8070(3) 0.92925(13) 1.2762(3) 0.0212(5) Uani 1 1 d . . . S1 S 0.60152(11) 0.81763(5) 1.47782(9) 0.0301(2) Uani 1 1 d . . . Cu1 Cu 0.56510(5) 0.93529(2) 1.11316(4) 0.02746(13) Uani 1 1 d . . . I1 I 0.59662(3) 0.940236(10) 0.84663(2) 0.02321(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0249(17) 0.0335(17) 0.0295(17) -0.0023(14) 0.0075(14) -0.0011(13) C2 0.0222(17) 0.038(2) 0.041(2) -0.0110(15) 0.0039(15) 0.0005(14) C3 0.030(2) 0.035(2) 0.066(3) -0.0092(19) 0.0151(19) -0.0122(15) C4 0.034(2) 0.0270(18) 0.055(2) 0.0001(16) 0.0162(18) -0.0095(15) C5 0.0275(16) 0.0208(15) 0.0315(16) -0.0026(12) 0.0160(14) -0.0023(12) C6 0.0280(17) 0.0223(15) 0.0356(18) 0.0010(13) 0.0134(14) 0.0016(12) C7 0.0298(17) 0.0279(16) 0.0224(15) 0.0013(13) 0.0108(13) 0.0031(13) C8 0.0243(15) 0.0185(13) 0.0197(14) -0.0006(11) 0.0072(12) 0.0010(11) C9 0.0321(18) 0.0289(17) 0.0183(15) -0.0002(13) 0.0023(13) -0.0019(14) C10 0.0213(16) 0.0291(17) 0.0363(19) -0.0004(14) -0.0013(14) -0.0010(13) C11 0.0202(16) 0.0315(17) 0.039(2) -0.0039(14) 0.0108(15) -0.0005(13) C12 0.0226(16) 0.0301(17) 0.0245(16) -0.0020(12) 0.0106(13) -0.0002(12) N1 0.0225(13) 0.0267(14) 0.0266(13) -0.0022(11) 0.0095(11) -0.0017(10) N2 0.0175(12) 0.0259(13) 0.0188(12) -0.0014(10) 0.0047(10) 0.0000(10) S1 0.0320(4) 0.0331(4) 0.0272(4) 0.0078(3) 0.0126(4) -0.0016(3) Cu1 0.0208(2) 0.0385(3) 0.0218(2) 0.00086(16) 0.00569(17) -0.00376(16) I1 0.02612(15) 0.02651(14) 0.01745(13) 0.00135(7) 0.00808(9) 0.00499(7) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 123.6(3) . . ? C1 C2 C3 118.5(3) . . ? C4 C3 C2 119.1(3) . . ? C3 C4 C5 120.0(4) . . ? N1 C5 C4 121.0(3) . . ? N1 C5 C6 118.3(3) . . ? C4 C5 C6 120.7(3) . . ? C5 C6 S1 113.7(2) . . ? C8 C7 S1 112.9(2) . . ? N2 C8 C9 121.2(3) . . ? N2 C8 C7 117.4(3) . . ? C9 C8 C7 121.4(3) . . ? C10 C9 C8 120.3(3) . . ? C11 C10 C9 118.5(3) . . ? C10 C11 C12 118.9(3) . . ? N2 C12 C11 123.0(3) . . ? C1 N1 C5 117.8(3) . . ? C1 N1 Cu1 115.4(2) . . ? C5 N1 Cu1 126.6(2) . . ? C8 N2 C12 118.1(3) . . ? C8 N2 Cu1 122.2(2) . . ? C12 N2 Cu1 119.6(2) . . ? C7 S1 C6 101.65(15) . . ? N2 Cu1 N1 121.79(11) . . ? N2 Cu1 I1 110.78(8) . . ? N1 Cu1 I1 104.76(7) . . ? N2 Cu1 I1 108.25(7) . 3_677 ? N1 Cu1 I1 102.33(7) . 3_677 ? I1 Cu1 I1 108.028(14) . 3_677 ? Cu1 I1 Cu1 71.972(14) . 3_677 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.353(4) . ? C1 C2 1.370(5) . ? C2 C3 1.380(6) . ? C3 C4 1.377(6) . ? C4 C5 1.391(5) . ? C5 N1 1.354(4) . ? C5 C6 1.507(5) . ? C6 S1 1.815(3) . ? C7 C8 1.498(4) . ? C7 S1 1.810(3) . ? C8 N2 1.349(4) . ? C8 C9 1.393(4) . ? C9 C10 1.383(5) . ? C10 C11 1.379(5) . ? C11 C12 1.383(5) . ? C12 N2 1.355(4) . ? N1 Cu1 2.060(3) . ? N2 Cu1 2.029(3) . ? Cu1 I1 2.6357(5) . ? Cu1 I1 2.7560(5) 3_677 ? I1 Cu1 2.7560(5) 3_677 ?
1100697.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100697.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100697 _chemical_formula_sum 'C13 H14 Cu2 I2 N2 S' _chemical_formula_weight 611.20 _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.000(5) _cell_angle_beta 100.080(5) _cell_angle_gamma 90.000(5) _cell_formula_units_Z 4 _cell_length_a 10.354(5) _cell_length_b 16.245(5) _cell_length_c 10.528(5) _cell_measurement_reflns_used ? _cell_measurement_temperature 293(2) _cell_measurement_theta_max ? _cell_measurement_theta_min ? _cell_volume 1743.5(13) _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.987 _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.0251 _diffrn_reflns_av_sigmaI/netI 0.0177 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 21993 _diffrn_reflns_theta_full 26.36 _diffrn_reflns_theta_max 26.36 _diffrn_reflns_theta_min 2.33 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _exptl_absorpt_coefficient_mu 6.091 _exptl_absorpt_correction_T_max ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_crystal_colour pale-yellow _exptl_crystal_density_diffrn 2.329 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 1144 _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.09 _refine_diff_density_max 3.151 _refine_diff_density_min -1.887 _refine_diff_density_rms 0.148 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 182 _refine_ls_number_reflns 3508 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.036 _refine_ls_R_factor_all 0.0445 _refine_ls_R_factor_gt 0.0370 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0607P)^2^+5.8100P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1016 _refine_ls_wR_factor_ref 0.1050 _reflns_number_gt 2967 _reflns_number_total 3508 _reflns_threshold_expression >2sigma(I) _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_sg_symbol_H-M P2(1)/n _cod_database_code 1100697 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3085(6) 0.1299(5) 0.1562(7) 0.0545(18) Uani 1 1 d . . . H1 H 0.3067 0.1844 0.1831 0.065 Uiso 1 1 calc R . . C2 C 0.3416(7) 0.1125(7) 0.0367(8) 0.067(2) Uani 1 1 d . . . H2 H 0.3614 0.1548 -0.0163 0.080 Uiso 1 1 calc R . . C3 C 0.3445(7) 0.0330(7) -0.0018(7) 0.070(3) Uani 1 1 d . . . H3 H 0.3662 0.0210 -0.0819 0.084 Uiso 1 1 calc R . . C4 C 0.3158(6) -0.0309(6) 0.0763(6) 0.0549(19) Uani 1 1 d . . . H4 H 0.3184 -0.0855 0.0505 0.066 Uiso 1 1 calc R . . C5 C 0.2827(5) -0.0098(4) 0.1950(5) 0.0353(12) Uani 1 1 d . . . C6 C 0.2526(6) -0.0747(4) 0.2873(6) 0.0380(13) Uani 1 1 d . . . H6A H 0.3286 -0.0821 0.3546 0.046 Uiso 1 1 calc R . . H6B H 0.2362 -0.1265 0.2414 0.046 Uiso 1 1 calc R . . C7 C -0.0182(6) -0.0517(4) 0.2196(6) 0.0371(13) Uani 1 1 d . . . H7A H -0.0987 -0.0310 0.2429 0.045 Uiso 1 1 calc R . . H7B H 0.0053 -0.0160 0.1533 0.045 Uiso 1 1 calc R . . C8 C -0.0404(5) -0.1384(3) 0.1668(5) 0.0325(11) Uani 1 1 d . . . C9 C 0.0030(6) -0.1621(4) 0.0549(6) 0.0426(14) Uani 1 1 d . . . H9 H 0.0437 -0.1245 0.0083 0.051 Uiso 1 1 calc R . . C10 C -0.0155(8) -0.2434(5) 0.0135(6) 0.0556(18) Uani 1 1 d . . . H10 H 0.0132 -0.2610 -0.0609 0.067 Uiso 1 1 calc R . . C11 C -0.0773(7) -0.2977(4) 0.0849(6) 0.0490(16) Uani 1 1 d . . . H11 H -0.0904 -0.3522 0.0586 0.059 Uiso 1 1 calc R . . C12 C -0.1191(6) -0.2709(4) 0.1946(6) 0.0393(13) Uani 1 1 d . . . C13 C -0.1865(8) -0.3278(4) 0.2735(8) 0.0599(19) Uani 1 1 d . . . H13A H -0.1394 -0.3288 0.3605 0.090 Uiso 1 1 calc R . . H13B H -0.1889 -0.3822 0.2376 0.090 Uiso 1 1 calc R . . H13C H -0.2744 -0.3088 0.2729 0.090 Uiso 1 1 calc R . . N1 N 0.2790(5) 0.0691(3) 0.2342(5) 0.0367(11) Uani 1 1 d . . . N2 N -0.0995(4) -0.1920(3) 0.2362(4) 0.0315(10) Uani 1 1 d . . . S1 S 0.11217(16) -0.04951(10) 0.36092(14) 0.0398(3) Uani 1 1 d . . . Cu1 Cu 0.20016(8) 0.08802(5) 0.39735(7) 0.0413(2) Uani 1 1 d . . . Cu2 Cu -0.15727(7) -0.15795(4) 0.39963(7) 0.03892(19) Uani 1 1 d . . . I1 I -0.35896(4) -0.06111(2) 0.38049(4) 0.03757(13) Uani 1 1 d . . . I2 I -0.05997(5) -0.22081(3) 0.61951(4) 0.05549(16) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.035(3) 0.067(5) 0.061(4) 0.030(4) 0.009(3) -0.004(3) C2 0.033(3) 0.112(7) 0.056(4) 0.043(5) 0.011(3) 0.000(4) C3 0.036(4) 0.143(9) 0.035(4) 0.018(5) 0.015(3) 0.017(5) C4 0.039(3) 0.090(6) 0.035(3) -0.008(3) 0.006(3) 0.020(4) C5 0.024(2) 0.050(4) 0.032(3) -0.001(2) 0.005(2) 0.008(2) C6 0.038(3) 0.040(3) 0.034(3) -0.001(2) 0.000(2) 0.004(2) C7 0.036(3) 0.039(3) 0.039(3) 0.002(2) 0.014(2) -0.001(2) C8 0.029(3) 0.036(3) 0.031(3) -0.002(2) 0.003(2) 0.005(2) C9 0.047(3) 0.050(4) 0.033(3) 0.005(3) 0.012(3) 0.002(3) C10 0.079(5) 0.060(4) 0.031(3) -0.011(3) 0.017(3) 0.009(4) C11 0.065(4) 0.043(4) 0.037(3) -0.015(3) 0.003(3) 0.000(3) C12 0.042(3) 0.038(3) 0.036(3) -0.003(2) 0.001(2) 0.001(3) C13 0.070(5) 0.048(4) 0.061(5) -0.010(3) 0.012(4) -0.009(4) N1 0.029(2) 0.051(3) 0.031(2) 0.008(2) 0.0078(18) 0.000(2) N2 0.031(2) 0.035(2) 0.027(2) -0.0069(19) 0.0026(17) -0.0002(19) S1 0.0535(9) 0.0392(8) 0.0295(7) -0.0032(6) 0.0149(6) -0.0123(6) Cu1 0.0507(4) 0.0402(4) 0.0360(4) -0.0068(3) 0.0159(3) -0.0016(3) Cu2 0.0496(4) 0.0371(4) 0.0332(4) -0.0029(3) 0.0160(3) 0.0030(3) I1 0.0393(2) 0.0400(2) 0.0347(2) 0.00312(15) 0.01010(15) 0.00531(16) I2 0.0733(3) 0.0557(3) 0.0385(2) 0.00691(19) 0.0125(2) 0.0241(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 121.2(8) . . ? C3 C2 C1 119.1(7) . . ? C2 C3 C4 121.1(7) . . ? C3 C4 C5 117.3(8) . . ? N1 C5 C4 122.2(6) . . ? N1 C5 C6 116.6(5) . . ? C4 C5 C6 121.2(6) . . ? C5 C6 S1 113.0(4) . . ? C8 C7 S1 111.1(4) . . ? N2 C8 C9 121.7(5) . . ? N2 C8 C7 117.0(5) . . ? C9 C8 C7 121.2(5) . . ? C8 C9 C10 118.8(6) . . ? C11 C10 C9 119.0(6) . . ? C12 C11 C10 119.8(6) . . ? N2 C12 C11 121.3(6) . . ? N2 C12 C13 117.5(5) . . ? C11 C12 C13 121.2(6) . . ? C5 N1 C1 119.0(6) . . ? C5 N1 Cu1 115.9(4) . . ? C1 N1 Cu1 124.4(5) . . ? C8 N2 C12 119.3(5) . . ? C8 N2 Cu2 121.4(4) . . ? C12 N2 Cu2 119.3(4) . . ? C6 S1 C7 100.4(3) . . ? C6 S1 Cu1 88.2(2) . . ? C7 S1 Cu1 110.6(2) . . ? N1 Cu1 S1 85.57(15) . . ? N1 Cu1 Cu2 158.53(15) . 3_556 ? S1 Cu1 Cu2 115.62(5) . 3_556 ? N1 Cu1 I2 111.60(14) . 3_556 ? S1 Cu1 I2 124.61(6) . 3_556 ? Cu2 Cu1 I2 60.27(3) 3_556 3_556 ? N1 Cu1 I1 116.00(14) . 3_556 ? S1 Cu1 I1 98.40(5) . 3_556 ? Cu2 Cu1 I1 60.09(4) 3_556 3_556 ? I2 Cu1 I1 116.87(3) 3_556 3_556 ? N2 Cu2 Cu1 167.68(14) . 3_556 ? N2 Cu2 I2 122.50(14) . . ? Cu1 Cu2 I2 61.05(4) 3_556 . ? N2 Cu2 I1 117.36(13) . . ? Cu1 Cu2 I1 62.28(3) 3_556 . ? I2 Cu2 I1 119.63(3) . . ? Cu2 I1 Cu1 57.62(3) . 3_556 ? Cu2 I2 Cu1 58.69(3) . 3_556 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.353(8) . ? C1 C2 1.390(11) . ? C2 C3 1.355(13) . ? C3 C4 1.388(12) . ? C4 C5 1.395(8) . ? C5 N1 1.349(8) . ? C5 C6 1.504(8) . ? C6 S1 1.810(6) . ? C7 C8 1.517(8) . ? C7 S1 1.826(6) . ? C8 N2 1.350(7) . ? C8 C9 1.387(8) . ? C9 C10 1.393(10) . ? C10 C11 1.387(10) . ? C11 C12 1.372(9) . ? C12 N2 1.360(7) . ? C12 C13 1.494(10) . ? N1 Cu1 2.050(5) . ? N2 Cu2 1.995(5) . ? S1 Cu1 2.4179(18) . ? Cu1 Cu2 2.5275(13) 3_556 ? Cu1 I2 2.5887(11) 3_556 ? Cu1 I1 2.6493(13) 3_556 ? Cu2 Cu1 2.5275(14) 3_556 ? Cu2 I2 2.5690(13) . ? Cu2 I1 2.5941(12) . ? I1 Cu1 2.6493(13) 3_556 ? I2 Cu1 2.5887(11) 3_556 ?
1100698.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100698.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100698 _chemical_formula_sum 'C14 H16 Cu2 I2 N2 S' _chemical_formula_weight 625.23 _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 105.338(5) _cell_angle_beta 102.112(5) _cell_angle_gamma 102.073(5) _cell_formula_units_Z 2 _cell_length_a 9.351(5) _cell_length_b 10.314(5) _cell_length_c 10.441(5) _cell_measurement_reflns_used 3680 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 26.40 _cell_measurement_theta_min 2.11 _cell_volume 911.3(8) _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.984 _diffrn_measured_fraction_theta_max 0.984 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.0196 _diffrn_reflns_av_sigmaI/netI 0.0203 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 11726 _diffrn_reflns_theta_full 26.40 _diffrn_reflns_theta_max 26.40 _diffrn_reflns_theta_min 2.11 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _exptl_absorpt_coefficient_mu 5.829 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.8685 _exptl_absorpt_correction_type none _exptl_absorpt_process_details 'SADABS (Sheldrick 1996)' _exptl_crystal_colour 'light green' _exptl_crystal_density_diffrn 2.278 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description rectangular _exptl_crystal_F_000 588 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.09 _refine_diff_density_max 1.310 _refine_diff_density_min -0.941 _refine_diff_density_rms 0.128 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 182 _refine_ls_number_reflns 3680 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.045 _refine_ls_R_factor_all 0.0325 _refine_ls_R_factor_gt 0.0274 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0469P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0699 _refine_ls_wR_factor_ref 0.0713 _reflns_number_gt 3187 _reflns_number_total 3680 _reflns_threshold_expression >2sigma(I) _cod_original_sg_symbol_H-M P-1 _cod_database_code 1100698 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.0088(5) 0.3863(4) 1.2715(4) 0.0344(9) Uani 1 1 d . . . C2 C 1.0728(5) 0.2749(5) 1.2630(5) 0.0477(11) Uani 1 1 d . . . H2 H 1.1756 0.2909 1.3057 0.057 Uiso 1 1 calc R . . C3 C 0.9833(6) 0.1433(5) 1.1917(5) 0.0522(12) Uani 1 1 d . . . H3 H 1.0247 0.0680 1.1841 0.063 Uiso 1 1 calc R . . C4 C 0.8283(5) 0.1203(4) 1.1294(5) 0.0432(10) Uani 1 1 d . . . H4 H 0.7651 0.0299 1.0821 0.052 Uiso 1 1 calc R . . C5 C 0.7709(4) 0.2345(4) 1.1393(4) 0.0281(8) Uani 1 1 d . . . C6 C 0.6059(4) 0.2190(4) 1.0767(4) 0.0297(8) Uani 1 1 d . . . H6A H 0.5562 0.2360 1.1498 0.036 Uiso 1 1 calc R . . H6B H 0.5573 0.1237 1.0155 0.036 Uiso 1 1 calc R . . C7 C 0.6677(4) 0.2712(4) 0.8470(4) 0.0282(8) Uani 1 1 d . . . H7A H 0.6752 0.3320 0.7905 0.034 Uiso 1 1 calc R . . H7B H 0.7700 0.2707 0.8901 0.034 Uiso 1 1 calc R . . C8 C 0.5768(4) 0.1255(4) 0.7567(4) 0.0273(8) Uani 1 1 d . . . C9 C 0.6460(5) 0.0208(4) 0.7267(4) 0.0375(9) Uani 1 1 d . . . H9 H 0.7502 0.0384 0.7644 0.045 Uiso 1 1 calc R . . C10 C 0.5584(5) -0.1122(4) 0.6391(4) 0.0442(11) Uani 1 1 d . . . H10 H 0.6024 -0.1852 0.6187 0.053 Uiso 1 1 calc R . . C11 C 0.4042(5) -0.1330(4) 0.5831(4) 0.0418(10) Uani 1 1 d . . . H11 H 0.3439 -0.2205 0.5229 0.050 Uiso 1 1 calc R . . C12 C 0.3398(5) -0.0242(4) 0.6166(4) 0.0342(9) Uani 1 1 d . . . C13 C 0.1764(5) -0.0394(5) 0.5524(5) 0.0553(13) Uani 1 1 d . . . H13A H 0.1302 -0.0051 0.6235 0.083 Uiso 1 1 calc R . . H13B H 0.1244 -0.1365 0.5031 0.083 Uiso 1 1 calc R . . H13C H 0.1694 0.0134 0.4894 0.083 Uiso 1 1 calc R . . C14 C 1.1017(5) 0.5321(5) 1.3536(5) 0.0561(13) Uani 1 1 d . . . H14A H 1.0939 0.5912 1.2967 0.084 Uiso 1 1 calc R . . H14B H 1.2063 0.5336 1.3855 0.084 Uiso 1 1 calc R . . H14C H 1.0648 0.5656 1.4317 0.084 Uiso 1 1 calc R . . N1 N 0.8614(3) 0.3668(3) 1.2079(3) 0.0271(7) Uiso 1 1 d . . . N2 N 0.4241(3) 0.1034(3) 0.7048(3) 0.0260(6) Uiso 1 1 d . . . S1 S 0.58042(10) 0.33910(9) 0.98004(9) 0.02489(19) Uani 1 1 d . . . Cu1 Cu 0.33751(5) 0.26378(5) 0.77776(5) 0.03205(13) Uani 1 1 d . . . Cu2 Cu 0.76565(5) 0.52310(4) 1.18388(5) 0.02905(12) Uani 1 1 d . . . I1 I 0.10799(3) 0.26304(3) 0.87876(3) 0.03472(9) Uani 1 1 d . . . I2 I 0.40978(3) 0.44687(3) 0.64871(3) 0.03398(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.033(2) 0.036(2) 0.035(2) 0.0133(18) 0.0052(18) 0.0130(17) C2 0.038(3) 0.053(3) 0.056(3) 0.023(2) 0.003(2) 0.025(2) C3 0.056(3) 0.043(3) 0.071(3) 0.026(2) 0.016(3) 0.033(2) C4 0.056(3) 0.028(2) 0.050(3) 0.0154(19) 0.017(2) 0.017(2) C5 0.037(2) 0.0243(18) 0.0286(19) 0.0148(16) 0.0120(17) 0.0103(16) C6 0.034(2) 0.0208(17) 0.035(2) 0.0086(16) 0.0139(17) 0.0046(15) C7 0.0234(19) 0.0309(19) 0.032(2) 0.0102(16) 0.0103(16) 0.0078(15) C8 0.031(2) 0.0321(19) 0.0252(18) 0.0112(15) 0.0141(16) 0.0131(16) C9 0.037(2) 0.044(2) 0.037(2) 0.0119(19) 0.0114(19) 0.0239(19) C10 0.059(3) 0.037(2) 0.042(2) 0.0066(19) 0.017(2) 0.030(2) C11 0.061(3) 0.0212(19) 0.036(2) -0.0022(17) 0.016(2) 0.0101(19) C12 0.038(2) 0.031(2) 0.027(2) 0.0056(16) 0.0075(17) 0.0008(17) C13 0.050(3) 0.057(3) 0.047(3) 0.003(2) 0.009(2) 0.012(2) C14 0.044(3) 0.053(3) 0.066(3) 0.022(3) 0.004(2) 0.011(2) S1 0.0210(4) 0.0227(4) 0.0280(5) 0.0042(4) 0.0053(4) 0.0067(3) Cu1 0.0280(3) 0.0265(2) 0.0462(3) 0.0107(2) 0.0162(2) 0.01274(19) Cu2 0.0279(2) 0.0217(2) 0.0384(3) 0.00840(19) 0.0097(2) 0.01007(18) I1 0.02670(15) 0.02939(14) 0.05539(19) 0.01735(12) 0.02060(12) 0.00925(10) I2 0.04596(17) 0.03530(15) 0.03155(15) 0.01517(11) 0.02025(12) 0.01896(12) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 121.8(4) . . ? N1 C1 C14 117.4(3) . . ? C2 C1 C14 120.8(4) . . ? C3 C2 C1 119.0(4) . . ? C2 C3 C4 120.0(4) . . ? C5 C4 C3 118.7(4) . . ? N1 C5 C4 121.4(4) . . ? N1 C5 C6 116.5(3) . . ? C4 C5 C6 122.1(3) . . ? C5 C6 S1 112.3(2) . . ? C8 C7 S1 111.3(2) . . ? N2 C8 C9 122.1(3) . . ? N2 C8 C7 116.9(3) . . ? C9 C8 C7 121.0(4) . . ? C8 C9 C10 119.3(4) . . ? C11 C10 C9 118.5(4) . . ? C12 C11 C10 120.1(4) . . ? N2 C12 C11 121.3(4) . . ? N2 C12 C13 116.7(4) . . ? C11 C12 C13 122.0(4) . . ? C1 N1 C5 119.0(3) . . ? C1 N1 Cu2 124.9(2) . . ? C5 N1 Cu2 115.6(2) . . ? C12 N2 C8 118.7(3) . . ? C12 N2 Cu1 124.5(3) . . ? C8 N2 Cu1 116.6(2) . . ? C7 S1 C6 98.15(17) . . ? C7 S1 Cu2 112.52(13) . . ? C6 S1 Cu2 86.38(13) . . ? C7 S1 Cu1 84.49(13) . . ? C6 S1 Cu1 117.57(12) . . ? Cu2 S1 Cu1 149.22(4) . . ? N2 Cu1 Cu2 166.27(9) . 2_667 ? N2 Cu1 S1 82.47(9) . . ? Cu2 Cu1 S1 104.12(4) 2_667 . ? N2 Cu1 I1 129.45(8) . . ? Cu2 Cu1 I1 60.50(2) 2_667 . ? S1 Cu1 I1 108.14(5) . . ? N2 Cu1 I2 106.26(9) . . ? Cu2 Cu1 I2 60.96(3) 2_667 . ? S1 Cu1 I2 100.88(4) . . ? I1 Cu1 I2 119.03(2) . . ? N1 Cu2 S1 84.82(9) . . ? N1 Cu2 Cu1 165.08(9) . 2_667 ? S1 Cu2 Cu1 106.51(4) . 2_667 ? N1 Cu2 I1 125.08(9) . 2_667 ? S1 Cu2 I1 111.83(4) . 2_667 ? Cu1 Cu2 I1 60.35(4) 2_667 2_667 ? N1 Cu2 I2 107.87(9) . 2_667 ? S1 Cu2 I2 99.30(4) . 2_667 ? Cu1 Cu2 I2 61.41(2) 2_667 2_667 ? I1 Cu2 I2 119.32(3) 2_667 2_667 ? Cu1 I1 Cu2 59.15(2) . 2_667 ? Cu2 I2 Cu1 57.63(2) 2_667 . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.346(5) . ? C1 C2 1.394(5) . ? C1 C14 1.487(6) . ? C2 C3 1.351(6) . ? C3 C4 1.400(6) . ? C4 C5 1.381(5) . ? C5 N1 1.355(4) . ? C5 C6 1.501(5) . ? C6 S1 1.815(4) . ? C7 C8 1.500(5) . ? C7 S1 1.813(4) . ? C8 N2 1.364(5) . ? C8 C9 1.371(5) . ? C9 C10 1.393(6) . ? C10 C11 1.384(6) . ? C11 C12 1.381(6) . ? C12 N2 1.349(5) . ? C12 C13 1.491(6) . ? N1 Cu2 2.046(3) . ? N2 Cu1 2.031(3) . ? S1 Cu2 2.4643(12) . ? S1 Cu1 2.5699(14) . ? Cu1 Cu2 2.5506(12) 2_667 ? Cu1 I1 2.5818(12) . ? Cu1 I2 2.6519(10) . ? Cu2 Cu1 2.5506(12) 2_667 ? Cu2 I1 2.5857(11) 2_667 ? Cu2 I2 2.6404(11) 2_667 ? I1 Cu2 2.5857(11) 2_667 ? I2 Cu2 2.6404(11) 2_667 ?
1100699.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100699.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100699 _chemical_formula_sum 'C12 H12 Cl2 Cu N2 O S' _chemical_formula_weight 366.76 _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 94.728(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 8.077(2) _cell_length_b 13.919(4) _cell_length_c 12.956(3) _cell_measurement_reflns_used 2951 _cell_measurement_temperature 170(2) _cell_measurement_theta_max 26.44 _cell_measurement_theta_min 2.15 _cell_volume 1451.6(6) _diffrn_ambient_temperature 170(2) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0434 _diffrn_reflns_av_sigmaI/netI 0.0295 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 18180 _diffrn_reflns_theta_full 26.44 _diffrn_reflns_theta_max 26.44 _diffrn_reflns_theta_min 2.15 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _exptl_absorpt_coefficient_mu 2.008 _exptl_absorpt_correction_T_max 0.786 _exptl_absorpt_correction_T_min 0.642 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Sheldrick 1996)' _exptl_crystal_colour green _exptl_crystal_density_diffrn 1.678 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 740 _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.12 _refine_diff_density_max 0.601 _refine_diff_density_min -0.417 _refine_diff_density_rms 0.086 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 172 _refine_ls_number_reflns 2951 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.099 _refine_ls_R_factor_all 0.0520 _refine_ls_R_factor_gt 0.0374 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0290P)^2^+2.5926P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0783 _refine_ls_wR_factor_ref 0.0829 _reflns_number_gt 2413 _reflns_number_total 2951 _reflns_threshold_expression >2sigma(I) _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_sg_symbol_H-M P2(1)/n _cod_database_code 1100699 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.07976(5) 0.68010(3) 0.79637(3) 0.01955(12) Uani 1 1 d . . . Cl2 Cl 0.20355(10) 0.59031(6) 0.93013(6) 0.02379(18) Uani 1 1 d . . . Cl1 Cl -0.02825(11) 0.55329(7) 0.67591(7) 0.0342(2) Uani 1 1 d . . . S1 S -0.00518(10) 0.82769(6) 0.71419(6) 0.02591(19) Uani 1 1 d . . . N1 N 0.2898(3) 0.70652(19) 0.7285(2) 0.0219(6) Uani 1 1 d . . . N2 N -0.1289(3) 0.69885(18) 0.8672(2) 0.0207(6) Uani 1 1 d . . . C1 C 0.3950(4) 0.6356(3) 0.7081(3) 0.0307(8) Uani 1 1 d . . . H1 H 0.3731 0.5723 0.7308 0.037 Uiso 1 1 calc R . . C2 C 0.5337(4) 0.6516(3) 0.6551(3) 0.0343(9) Uani 1 1 d . . . H2 H 0.6055 0.6000 0.6412 0.041 Uiso 1 1 calc R . . C3 C 0.5670(4) 0.7435(3) 0.6226(3) 0.0308(8) Uani 1 1 d . . . H3 H 0.6616 0.7558 0.5857 0.037 Uiso 1 1 calc R . . C4 C 0.4608(4) 0.8176(3) 0.6445(3) 0.0275(7) Uani 1 1 d . . . H4 H 0.4820 0.8815 0.6235 0.033 Uiso 1 1 calc R . . C5 C 0.3224(4) 0.7967(2) 0.6977(2) 0.0215(7) Uani 1 1 d . . . C6 C 0.2054(4) 0.8746(2) 0.7258(3) 0.0291(8) Uani 1 1 d . . . H6A H 0.2137 0.9303 0.6788 0.035 Uiso 1 1 calc R . . H6B H 0.2351 0.8965 0.7976 0.035 Uiso 1 1 calc R . . C7 C -0.0968(4) 0.8698(2) 0.8305(3) 0.0270(7) Uani 1 1 d . . . H7A H -0.0083 0.8907 0.8831 0.032 Uiso 1 1 calc R . . H7B H -0.1712 0.9250 0.8134 0.032 Uiso 1 1 calc R . . C8 C -0.1941(4) 0.7876(2) 0.8722(2) 0.0214(7) Uani 1 1 d . . . C9 C -0.3437(4) 0.8031(2) 0.9149(3) 0.0260(7) Uani 1 1 d . . . H9 H -0.3874 0.8662 0.9190 0.031 Uiso 1 1 calc R . . C10 C -0.4286(4) 0.7254(3) 0.9513(3) 0.0296(8) Uani 1 1 d . . . H10 H -0.5324 0.7345 0.9795 0.036 Uiso 1 1 calc R . . C11 C -0.3607(4) 0.6341(3) 0.9465(3) 0.0283(8) Uani 1 1 d . . . H11 H -0.4166 0.5800 0.9718 0.034 Uiso 1 1 calc R . . C12 C -0.2107(4) 0.6232(2) 0.9043(3) 0.0258(7) Uani 1 1 d . . . H12 H -0.1635 0.5609 0.9011 0.031 Uiso 1 1 calc R . . O1 O 0.2637(4) 0.9534(3) 0.9629(2) 0.0679(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0177(2) 0.0182(2) 0.0236(2) 0.00181(16) 0.00660(14) 0.00046(16) Cl2 0.0219(4) 0.0246(4) 0.0254(4) 0.0037(3) 0.0052(3) 0.0026(3) Cl1 0.0295(5) 0.0357(5) 0.0375(5) -0.0153(4) 0.0038(4) -0.0028(4) S1 0.0254(4) 0.0265(4) 0.0264(4) 0.0043(3) 0.0053(3) 0.0029(4) N1 0.0202(14) 0.0216(14) 0.0245(14) 0.0018(11) 0.0047(11) -0.0006(11) N2 0.0179(13) 0.0209(14) 0.0235(14) 0.0015(11) 0.0034(11) 0.0007(11) C1 0.0282(19) 0.0246(18) 0.041(2) 0.0090(16) 0.0123(16) 0.0048(15) C2 0.0284(19) 0.034(2) 0.042(2) 0.0052(17) 0.0161(16) 0.0096(16) C3 0.0213(17) 0.046(2) 0.0265(18) 0.0077(16) 0.0086(14) 0.0002(16) C4 0.0245(17) 0.0298(18) 0.0284(18) 0.0072(15) 0.0042(14) -0.0063(15) C5 0.0177(16) 0.0252(17) 0.0212(16) 0.0025(13) -0.0007(13) -0.0029(13) C6 0.0274(19) 0.0223(17) 0.039(2) 0.0014(15) 0.0115(15) -0.0030(14) C7 0.0293(19) 0.0233(17) 0.0297(19) -0.0016(14) 0.0091(15) 0.0018(14) C8 0.0205(16) 0.0234(16) 0.0201(16) 0.0004(13) 0.0009(13) 0.0001(13) C9 0.0246(17) 0.0252(17) 0.0287(18) -0.0009(14) 0.0057(14) 0.0051(14) C10 0.0171(16) 0.041(2) 0.0308(19) -0.0003(16) 0.0043(14) 0.0010(15) C11 0.0226(18) 0.0315(19) 0.0317(19) 0.0068(15) 0.0067(14) -0.0026(15) C12 0.0253(18) 0.0232(17) 0.0293(18) 0.0047(14) 0.0041(14) -0.0009(14) O1 0.055(2) 0.106(3) 0.0420(18) 0.0015(19) 0.0007(15) -0.036(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cu1 N1 161.92(11) . . ? N2 Cu1 Cl2 93.20(8) . . ? N1 Cu1 Cl2 95.69(8) . . ? N2 Cu1 S1 82.55(8) . . ? N1 Cu1 S1 82.49(8) . . ? Cl2 Cu1 S1 153.54(3) . . ? N2 Cu1 Cl1 96.66(8) . . ? N1 Cu1 Cl1 96.97(8) . . ? Cl2 Cu1 Cl1 101.37(4) . . ? S1 Cu1 Cl1 105.06(4) . . ? C6 S1 C7 104.86(17) . . ? C6 S1 Cu1 92.30(12) . . ? C7 S1 Cu1 91.66(11) . . ? C1 N1 C5 118.9(3) . . ? C1 N1 Cu1 121.5(2) . . ? C5 N1 Cu1 119.5(2) . . ? C8 N2 C12 119.5(3) . . ? C8 N2 Cu1 119.3(2) . . ? C12 N2 Cu1 121.1(2) . . ? N1 C1 C2 122.1(3) . . ? C1 C2 C3 119.2(3) . . ? C2 C3 C4 119.2(3) . . ? C3 C4 C5 118.8(3) . . ? N1 C5 C4 121.7(3) . . ? N1 C5 C6 117.3(3) . . ? C4 C5 C6 121.0(3) . . ? C5 C6 S1 108.9(2) . . ? C8 C7 S1 108.0(2) . . ? N2 C8 C9 121.3(3) . . ? N2 C8 C7 117.4(3) . . ? C9 C8 C7 121.3(3) . . ? C10 C9 C8 119.2(3) . . ? C9 C10 C11 119.4(3) . . ? C12 C11 C10 118.8(3) . . ? N2 C12 C11 121.8(3) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N2 2.001(3) . ? Cu1 N1 2.008(3) . ? Cu1 Cl2 2.2977(9) . ? Cu1 S1 2.3883(10) . ? Cu1 Cl1 2.4673(10) . ? S1 C6 1.817(3) . ? S1 C7 1.829(3) . ? N1 C1 1.343(4) . ? N1 C5 1.349(4) . ? N2 C8 1.346(4) . ? N2 C12 1.352(4) . ? C1 C2 1.379(5) . ? C2 C3 1.380(5) . ? C3 C4 1.386(5) . ? C4 C5 1.392(4) . ? C5 C6 1.503(5) . ? C7 C8 1.513(4) . ? C8 C9 1.386(4) . ? C9 C10 1.384(5) . ? C10 C11 1.388(5) . ? C11 C12 1.378(5) . ?
1100700.cif	#------------------------------------------------------------------------------ #$Date: 2016-03-16 11:15:42 +0200 (Wed, 16 Mar 2016) $ #$Revision: 178221 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100700.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100700 loop_ _publ_author_name 'Caradoc-Davies, Paula L.' 'Hanton, Lyall R.' 'Lee, Kitty' _publ_section_title ; Extension of a \p-stacked N~2~S ligand to form bi- and tri-nuclear silver(I) complexes ; _journal_coden_ASTM CHCOFS _journal_issue 9 _journal_name_full ; Chemical Communications (Cambridge, United Kingdom) ; _journal_page_first 783 _journal_page_last 784 _journal_paper_doi 10.1039/a910342m _journal_year 2000 _chemical_formula_sum 'C12 H12 Ag F6 N2 P S' _chemical_formula_weight 469.14 _space_group_IT_number 13 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yac' _symmetry_space_group_name_H-M 'P 1 2/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 103.063(4) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 13.657(4) _cell_length_b 8.278(3) _cell_length_c 14.071(4) _cell_measurement_reflns_used 8192 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 26.50 _cell_measurement_theta_min 2.36 _cell_volume 1549.7(8) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'Bruker SHELXTL' _diffrn_ambient_temperature 173(2) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0320 _diffrn_reflns_av_sigmaI/netI 0.0207 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 19328 _diffrn_reflns_theta_full 26.50 _diffrn_reflns_theta_max 26.50 _diffrn_reflns_theta_min 2.36 _diffrn_standards_decay_% 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.599 _exptl_absorpt_correction_T_max 0.8387 _exptl_absorpt_correction_T_min 0.5627 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Sheldrick 1996)' _exptl_crystal_colour gold _exptl_crystal_density_diffrn 2.011 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 920 _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.61 _exptl_crystal_size_min 0.11 _refine_diff_density_max 0.906 _refine_diff_density_min -1.112 _refine_diff_density_rms 0.138 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 208 _refine_ls_number_reflns 3176 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.060 _refine_ls_R_factor_all 0.0426 _refine_ls_R_factor_gt 0.0353 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0521P)^2^+2.5837P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0899 _refine_ls_wR_factor_ref 0.0940 _reflns_number_gt 2720 _reflns_number_total 3176 _reflns_threshold_expression >2sigma(I) _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_sg_symbol_H-M P2/n _cod_database_code 1100700 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.716973(19) 0.88094(4) 0.346590(19) 0.03500(12) Uani 1 1 d . . . S1 S 0.61044(7) 0.64585(10) 0.25348(6) 0.02902(19) Uani 1 1 d . . . P1 P 0.75202(7) 0.47423(11) -0.03813(7) 0.0279(2) Uani 1 1 d . . . F11 F 0.7244(5) 0.5149(7) -0.1474(2) 0.141(2) Uani 1 1 d . . . F12 F 0.8645(2) 0.4542(4) -0.0415(4) 0.1084(17) Uani 1 1 d . . . F13 F 0.7791(4) 0.4340(4) 0.0746(2) 0.0985(14) Uani 1 1 d . . . F14 F 0.6390(2) 0.4947(4) -0.0320(3) 0.0879(13) Uani 1 1 d . . . F15 F 0.77129(18) 0.6624(3) -0.0129(2) 0.0448(6) Uani 1 1 d . . . F16 F 0.7319(2) 0.2863(3) -0.0602(3) 0.0640(8) Uani 1 1 d . . . N1 N 0.5625(2) 0.9514(4) 0.3658(2) 0.0280(6) Uani 1 1 d . . . N2 N 0.6345(2) 0.9927(3) 0.1340(2) 0.0251(6) Uani 1 1 d . . . C1 C 0.5423(3) 1.1022(5) 0.3903(3) 0.0368(8) Uani 1 1 d . . . H1 H 0.5968 1.1755 0.4094 0.044 Uiso 1 1 calc R . . C2 C 0.4470(3) 1.1565(6) 0.3891(3) 0.0466(10) Uani 1 1 d . . . H2 H 0.4357 1.2644 0.4070 0.056 Uiso 1 1 calc R . . C3 C 0.3680(3) 1.0497(6) 0.3610(3) 0.0466(10) Uani 1 1 d . . . H3 H 0.3010 1.0831 0.3593 0.056 Uiso 1 1 calc R . . C4 C 0.3874(3) 0.8945(5) 0.3357(3) 0.0390(9) Uani 1 1 d . . . H4 H 0.3339 0.8197 0.3166 0.047 Uiso 1 1 calc R . . C5 C 0.4855(3) 0.8474(4) 0.3380(2) 0.0277(7) Uani 1 1 d . . . C6 C 0.5075(3) 0.6761(4) 0.3135(3) 0.0324(8) Uani 1 1 d . . . H6A H 0.4458 0.6306 0.2710 0.039 Uiso 1 1 calc R . . H6B H 0.5218 0.6127 0.3747 0.039 Uiso 1 1 calc R . . C7 C 0.5593(3) 0.7260(4) 0.1315(2) 0.0280(7) Uani 1 1 d . . . H7A H 0.6033 0.6918 0.0881 0.034 Uiso 1 1 calc R . . H7B H 0.4922 0.6776 0.1060 0.034 Uiso 1 1 calc R . . C8 C 0.5493(2) 0.9061(4) 0.1269(2) 0.0224(6) Uani 1 1 d . . . C9 C 0.4572(2) 0.9799(4) 0.1176(2) 0.0269(7) Uani 1 1 d . . . H9 H 0.3980 0.9167 0.1107 0.032 Uiso 1 1 calc R . . C10 C 0.4517(3) 1.1466(5) 0.1185(3) 0.0346(8) Uani 1 1 d . . . H10 H 0.3889 1.1995 0.1130 0.042 Uiso 1 1 calc R . . C11 C 0.5388(3) 1.2344(4) 0.1275(3) 0.0355(8) Uani 1 1 d . . . H11 H 0.5371 1.3491 0.1290 0.043 Uiso 1 1 calc R . . C12 C 0.6280(3) 1.1547(4) 0.1343(3) 0.0317(8) Uani 1 1 d . . . H12 H 0.6876 1.2163 0.1394 0.038 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.01986(16) 0.0543(2) 0.03006(16) 0.00241(12) 0.00400(11) -0.00358(11) S1 0.0340(5) 0.0223(4) 0.0298(4) 0.0027(3) 0.0051(3) 0.0026(3) P1 0.0244(4) 0.0261(4) 0.0348(5) -0.0062(4) 0.0099(4) -0.0025(3) F11 0.257(7) 0.127(4) 0.0286(17) -0.0031(19) 0.014(3) -0.064(4) F12 0.0478(18) 0.0556(19) 0.241(5) -0.042(3) 0.073(3) -0.0141(15) F13 0.161(4) 0.073(2) 0.0492(18) 0.0136(16) -0.003(2) -0.046(2) F14 0.0314(14) 0.0541(17) 0.182(4) -0.036(2) 0.0319(19) -0.0058(12) F15 0.0444(13) 0.0259(11) 0.0657(16) -0.0040(11) 0.0159(12) -0.0046(10) F16 0.0498(15) 0.0361(13) 0.114(2) -0.0341(15) 0.0359(16) -0.0134(11) N1 0.0256(14) 0.0327(15) 0.0266(14) -0.0015(12) 0.0079(11) -0.0006(12) N2 0.0218(13) 0.0294(14) 0.0239(13) 0.0032(11) 0.0046(11) -0.0032(11) C1 0.040(2) 0.037(2) 0.0358(19) -0.0074(16) 0.0124(16) -0.0027(16) C2 0.051(3) 0.048(2) 0.045(2) -0.0027(19) 0.019(2) 0.015(2) C3 0.034(2) 0.067(3) 0.044(2) 0.006(2) 0.0194(18) 0.015(2) C4 0.0238(18) 0.059(3) 0.0357(19) 0.0062(18) 0.0090(15) -0.0040(16) C5 0.0255(17) 0.0348(18) 0.0233(15) 0.0038(13) 0.0067(13) -0.0025(14) C6 0.0321(19) 0.0328(18) 0.0339(18) 0.0024(15) 0.0105(15) -0.0066(15) C7 0.0327(18) 0.0246(16) 0.0247(16) -0.0031(13) 0.0025(13) -0.0028(13) C8 0.0243(16) 0.0243(16) 0.0175(14) 0.0007(12) 0.0024(12) -0.0026(12) C9 0.0207(16) 0.0333(18) 0.0261(16) 0.0060(14) 0.0038(13) -0.0010(13) C10 0.0337(19) 0.038(2) 0.0322(18) 0.0049(15) 0.0071(15) 0.0119(16) C11 0.047(2) 0.0230(16) 0.0359(19) 0.0031(14) 0.0074(16) 0.0035(15) C12 0.0350(19) 0.0277(17) 0.0307(17) 0.0032(14) 0.0040(15) -0.0105(14) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ag1 N1 137.61(11) 2_655 . ? N2 Ag1 S1 140.92(7) 2_655 . ? N1 Ag1 S1 79.77(8) . . ? N2 Ag1 Ag1 70.08(7) 2_655 2_655 ? N1 Ag1 Ag1 125.29(7) . 2_655 ? S1 Ag1 Ag1 78.20(3) . 2_655 ? C6 S1 C7 102.43(17) . . ? C6 S1 Ag1 93.82(12) . . ? C7 S1 Ag1 104.68(11) . . ? F11 P1 F12 90.8(3) . . ? F11 P1 F14 90.5(3) . . ? F12 P1 F14 178.6(3) . . ? F11 P1 F13 179.2(3) . . ? F12 P1 F13 90.0(3) . . ? F14 P1 F13 88.7(2) . . ? F11 P1 F16 91.5(2) . . ? F12 P1 F16 91.03(16) . . ? F14 P1 F16 89.30(15) . . ? F13 P1 F16 88.89(19) . . ? F11 P1 F15 90.0(2) . . ? F12 P1 F15 89.81(15) . . ? F14 P1 F15 89.83(15) . . ? F13 P1 F15 89.58(17) . . ? F16 P1 F15 178.26(16) . . ? C1 N1 C5 118.6(3) . . ? C1 N1 Ag1 121.5(2) . . ? C5 N1 Ag1 119.2(2) . . ? C12 N2 C8 118.3(3) . . ? C12 N2 Ag1 118.7(2) . 2_655 ? C8 N2 Ag1 122.9(2) . 2_655 ? N1 C1 C2 123.4(4) . . ? C1 C2 C3 118.1(4) . . ? C4 C3 C2 119.2(4) . . ? C3 C4 C5 119.9(4) . . ? N1 C5 C4 120.8(3) . . ? N1 C5 C6 119.1(3) . . ? C4 C5 C6 120.0(3) . . ? C5 C6 S1 116.9(2) . . ? C8 C7 S1 114.5(2) . . ? N2 C8 C9 121.6(3) . . ? N2 C8 C7 117.2(3) . . ? C9 C8 C7 121.2(3) . . ? C8 C9 C10 119.5(3) . . ? C11 C10 C9 118.7(3) . . ? C12 C11 C10 119.3(3) . . ? N2 C12 C11 122.6(3) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N2 2.190(3) 2_655 ? Ag1 N1 2.263(3) . ? Ag1 S1 2.5997(11) . ? Ag1 Ag1 3.0515(10) 2_655 ? S1 C6 1.814(4) . ? S1 C7 1.825(3) . ? P1 F11 1.535(3) . ? P1 F12 1.557(3) . ? P1 F14 1.575(3) . ? P1 F13 1.580(3) . ? P1 F16 1.598(3) . ? P1 F15 1.606(2) . ? N1 C1 1.340(5) . ? N1 C5 1.347(5) . ? N2 C12 1.344(5) . ? N2 C8 1.350(4) . ? N2 Ag1 2.190(3) 2_655 ? C1 C2 1.373(6) . ? C2 C3 1.382(7) . ? C3 C4 1.375(6) . ? C4 C5 1.389(5) . ? C5 C6 1.505(5) . ? C7 C8 1.497(4) . ? C8 C9 1.378(5) . ? C9 C10 1.382(5) . ? C10 C11 1.375(6) . ? C11 C12 1.370(5) . ?
1100701.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100701.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100701 _chemical_formula_sum 'C24 H24 Ag2 N6 O6 S2' _chemical_formula_weight 772.35 _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.000(5) _cell_angle_beta 108.144(5) _cell_angle_gamma 90.000(5) _cell_formula_units_Z 4 _cell_length_a 13.277(5) _cell_length_b 15.822(5) _cell_length_c 14.031(5) _cell_measurement_reflns_used 5731 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 26.35 _cell_measurement_theta_min 2.06 _cell_volume 2800.9(17) _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.969 _diffrn_measured_fraction_theta_max 0.969 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.1632 _diffrn_reflns_av_sigmaI/netI 0.4216 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 20290 _diffrn_reflns_theta_full 26.35 _diffrn_reflns_theta_max 26.35 _diffrn_reflns_theta_min 2.06 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _exptl_absorpt_coefficient_mu 1.598 _exptl_absorpt_correction_T_max 0.8523 _exptl_absorpt_correction_T_min 0.7366 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Sheldrick 1996)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.832 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 1536 _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.10 _refine_diff_density_max 9.069 _refine_diff_density_min -3.616 _refine_diff_density_rms 0.876 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.291 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 363 _refine_ls_number_reflns 5731 _refine_ls_number_restraints 216 _refine_ls_restrained_S_all 1.269 _refine_ls_R_factor_all 0.3282 _refine_ls_R_factor_gt 0.1869 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.5071 _refine_ls_wR_factor_ref 0.5275 _reflns_number_gt 1631 _reflns_number_total 5731 _reflns_threshold_expression >2sigma(I) _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_sg_symbol_H-M P2(1)/c _cod_database_code 1100701 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.725(3) 0.586(2) 0.145(3) 0.040(9) Uani 1 1 d U . . H1 H 0.6731 0.6259 0.1457 0.048 Uiso 1 1 calc R . . C2 C 0.823(3) 0.617(2) 0.150(2) 0.037(9) Uani 1 1 d U . . H2 H 0.8339 0.6751 0.1447 0.044 Uiso 1 1 calc R . . C3 C 0.900(3) 0.563(2) 0.164(2) 0.029(8) Uani 1 1 d U . . H3 H 0.9688 0.5814 0.1736 0.035 Uiso 1 1 calc R . . C4 C 0.879(2) 0.480(2) 0.163(2) 0.022(7) Uani 1 1 d U . . H4 H 0.9328 0.4406 0.1691 0.027 Uiso 1 1 calc R . . C5 C 0.778(3) 0.454(2) 0.154(2) 0.027(8) Uani 1 1 d U . . C6 C 0.748(3) 0.360(2) 0.151(3) 0.043(10) Uani 1 1 d U . . H6A H 0.8124 0.3268 0.1729 0.052 Uiso 1 1 calc R . . H6B H 0.7116 0.3447 0.0816 0.052 Uiso 1 1 calc R . . C7 C 0.742(3) 0.359(2) 0.353(2) 0.038(9) Uani 1 1 d U . . H7A H 0.7095 0.3326 0.3984 0.046 Uiso 1 1 calc R . . H7B H 0.8124 0.3341 0.3668 0.046 Uiso 1 1 calc R . . C8 C 0.755(2) 0.4500(18) 0.376(2) 0.016(7) Uani 1 1 d U . . C9 C 0.854(3) 0.487(2) 0.394(2) 0.037(9) Uani 1 1 d U . . H9 H 0.9122 0.4539 0.3951 0.044 Uiso 1 1 calc R . . C10 C 0.867(3) 0.571(2) 0.412(3) 0.047(10) Uani 1 1 d U . . H10 H 0.9308 0.5991 0.4176 0.056 Uiso 1 1 calc R . . C11 C 0.775(3) 0.615(2) 0.419(2) 0.037(9) Uani 1 1 d U . . H11 H 0.7785 0.6716 0.4368 0.044 Uiso 1 1 calc R . . C12 C 0.682(3) 0.570(2) 0.401(2) 0.035(9) Uani 1 1 d U . . H12 H 0.6235 0.6009 0.4036 0.042 Uiso 1 1 calc R . . C13 C 0.346(3) 0.571(2) 0.393(2) 0.036(9) Uani 1 1 d U . . H13 H 0.4061 0.6040 0.4165 0.043 Uiso 1 1 calc R . . C14 C 0.252(3) 0.606(2) 0.385(2) 0.033(9) Uani 1 1 d U . . H14 H 0.2470 0.6632 0.3957 0.040 Uiso 1 1 calc R . . C15 C 0.164(3) 0.556(2) 0.363(2) 0.039(9) Uani 1 1 d U . . H15 H 0.0987 0.5793 0.3608 0.046 Uiso 1 1 calc R . . C16 C 0.170(3) 0.475(2) 0.343(2) 0.036(9) Uani 1 1 d U . . H16 H 0.1095 0.4422 0.3294 0.043 Uiso 1 1 calc R . . C17 C 0.268(3) 0.437(2) 0.342(3) 0.043(10) Uani 1 1 d U . . C18 C 0.281(2) 0.347(2) 0.317(2) 0.031(8) Uani 1 1 d U . . H18A H 0.2130 0.3265 0.2747 0.037 Uiso 1 1 calc R . . H18B H 0.2986 0.3145 0.3788 0.037 Uiso 1 1 calc R . . C19 C 0.314(3) 0.356(2) 0.131(2) 0.037(9) Uani 1 1 d U . . H19A H 0.3579 0.3398 0.0899 0.044 Uiso 1 1 calc R . . H19B H 0.2472 0.3261 0.1047 0.044 Uiso 1 1 calc R . . C20 C 0.290(3) 0.455(2) 0.115(3) 0.048(11) Uani 1 1 d U . . C21 C 0.189(3) 0.484(2) 0.100(2) 0.034(9) Uani 1 1 d U . . H21 H 0.1325 0.4469 0.0927 0.040 Uiso 1 1 calc R . . C2A C 0.177(3) 0.564(3) 0.097(3) 0.054(11) Uani 1 1 d U . . H22 H 0.1091 0.5847 0.0857 0.065 Uiso 1 1 calc R . . C23 C 0.257(3) 0.621(2) 0.108(2) 0.038(9) Uani 1 1 d U . . H23 H 0.2451 0.6792 0.1065 0.045 Uiso 1 1 calc R . . C24 C 0.357(3) 0.587(2) 0.121(2) 0.040(9) Uani 1 1 d U . . H24 H 0.4135 0.6232 0.1246 0.048 Uiso 1 1 calc R . . N1 N 0.696(2) 0.5074(17) 0.1385(18) 0.028(7) Uani 1 1 d U . . N2 N 0.666(2) 0.4887(18) 0.3786(19) 0.032(7) Uani 1 1 d U . . N3 N 0.357(2) 0.491(2) 0.367(2) 0.047(9) Uani 1 1 d U . . N4 N 0.374(2) 0.5044(17) 0.1275(19) 0.026(6) Uani 1 1 d U . . S3 S 0.6649(8) 0.3307(6) 0.2252(7) 0.040(3) Uani 1 1 d . . . S4 S 0.3773(7) 0.3199(6) 0.2557(7) 0.039(2) Uani 1 1 d . . . Ag1 Ag 0.5146(2) 0.43279(19) 0.3525(2) 0.0409(10) Uani 1 1 d . . . Ag2 Ag 0.5382(2) 0.4571(2) 0.1491(2) 0.0447(10) Uani 1 1 d . . . O23 O 0.449(2) 0.2811(16) 0.5258(19) 0.056(8) Uani 1 1 d U . . O22 O 0.506(2) 0.1592(17) 0.4982(17) 0.049(7) Uani 1 1 d U . . O21 O 0.5743(18) 0.2684(15) 0.4606(18) 0.047(7) Uani 1 1 d U . . N22 N 0.511(2) 0.2373(19) 0.4977(19) 0.031(7) Uani 1 1 d U . . N11 N 0.004(2) 0.274(2) 0.071(2) 0.045(8) Uani 1 1 d U . . O11 O 0.050(3) 0.298(2) 0.163(2) 0.092(11) Uani 1 1 d U . . O12 O 0.049(2) 0.2955(16) 0.009(2) 0.058(8) Uani 1 1 d U . . O13 O -0.074(2) 0.2260(17) 0.0530(19) 0.059(8) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.038(12) 0.043(13) 0.042(12) -0.002(9) 0.015(9) 0.003(9) C2 0.036(12) 0.037(13) 0.036(12) -0.002(9) 0.007(9) -0.002(9) C3 0.029(11) 0.027(12) 0.031(11) 0.001(8) 0.009(9) 0.000(9) C4 0.019(10) 0.024(11) 0.025(11) -0.005(8) 0.010(8) -0.002(8) C5 0.029(11) 0.024(12) 0.024(11) -0.004(8) 0.004(8) -0.003(9) C6 0.042(13) 0.044(13) 0.046(13) 0.007(9) 0.017(9) -0.005(9) C7 0.037(12) 0.039(13) 0.041(12) 0.006(9) 0.016(9) -0.001(9) C8 0.019(10) 0.018(11) 0.013(9) -0.010(8) 0.008(8) -0.001(8) C9 0.036(12) 0.039(13) 0.034(12) 0.004(9) 0.009(9) -0.002(9) C10 0.048(13) 0.047(14) 0.044(13) 0.000(9) 0.013(9) 0.000(9) C11 0.039(12) 0.032(12) 0.035(12) 0.004(9) 0.005(9) -0.003(9) C12 0.040(12) 0.035(12) 0.031(11) 0.013(9) 0.010(9) 0.000(9) C13 0.036(12) 0.031(12) 0.040(12) 0.000(9) 0.009(9) -0.002(9) C14 0.036(12) 0.035(12) 0.032(11) -0.004(9) 0.014(9) 0.001(9) C15 0.037(12) 0.038(13) 0.040(12) -0.002(9) 0.013(9) 0.002(9) C16 0.031(12) 0.038(13) 0.039(12) -0.001(9) 0.009(9) -0.002(9) C17 0.041(12) 0.048(13) 0.044(12) -0.002(9) 0.020(9) -0.004(9) C18 0.031(11) 0.032(12) 0.027(11) 0.006(8) 0.006(9) -0.005(9) C19 0.037(12) 0.036(13) 0.037(12) 0.006(9) 0.012(9) -0.004(9) C20 0.045(13) 0.048(14) 0.052(13) 0.000(9) 0.014(9) -0.002(9) C21 0.034(12) 0.036(12) 0.031(11) 0.006(9) 0.009(9) -0.005(9) C2A 0.055(14) 0.053(14) 0.054(14) -0.003(9) 0.017(9) 0.004(9) C23 0.039(12) 0.034(13) 0.038(12) -0.003(9) 0.009(9) 0.004(9) C24 0.044(12) 0.037(13) 0.040(12) -0.002(9) 0.016(9) -0.003(9) N1 0.029(10) 0.031(11) 0.023(10) 0.003(8) 0.007(8) -0.005(8) N2 0.034(10) 0.034(11) 0.032(10) 0.000(8) 0.019(8) 0.003(8) N3 0.043(11) 0.046(12) 0.050(12) -0.007(9) 0.012(9) 0.001(9) N4 0.023(10) 0.026(10) 0.031(10) 0.010(8) 0.010(8) 0.000(8) S3 0.045(6) 0.040(7) 0.040(6) 0.000(5) 0.018(5) -0.012(5) S4 0.034(6) 0.040(7) 0.041(6) 0.004(5) 0.008(5) -0.004(5) Ag1 0.0208(15) 0.063(2) 0.0423(17) -0.0061(16) 0.0144(13) 0.0034(15) Ag2 0.0226(16) 0.066(2) 0.0431(18) -0.0112(16) 0.0072(13) 0.0058(15) O23 0.057(14) 0.051(15) 0.066(14) -0.007(11) 0.026(12) 0.022(12) O22 0.059(14) 0.058(15) 0.036(12) -0.002(11) 0.023(11) -0.006(12) O21 0.047(13) 0.046(14) 0.058(14) -0.002(11) 0.030(11) -0.019(11) N22 0.034(10) 0.027(11) 0.033(10) 0.004(8) 0.014(8) -0.003(8) N11 0.044(11) 0.049(12) 0.041(11) -0.005(9) 0.014(9) 0.001(9) O11 0.082(17) 0.114(19) 0.087(17) -0.014(14) 0.038(14) -0.014(14) O12 0.053(14) 0.057(15) 0.065(14) 0.019(12) 0.018(12) -0.015(12) O13 0.052(14) 0.059(15) 0.072(15) -0.015(12) 0.030(12) -0.018(12) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 127(3) . . ? C3 C2 C1 117(4) . . ? C2 C3 C4 120(3) . . ? C3 C4 C5 119(3) . . ? N1 C5 C4 123(3) . . ? N1 C5 C6 114(3) . . ? C4 C5 C6 123(3) . . ? C5 C6 S3 116(2) . . ? C8 C7 S3 116(2) . . ? N2 C8 C9 126(3) . . ? N2 C8 C7 115(3) . . ? C9 C8 C7 119(3) . . ? C10 C9 C8 121(3) . . ? C9 C10 C11 115(4) . . ? C12 C11 C10 119(3) . . ? N2 C12 C11 128(3) . . ? N3 C13 C14 123(3) . . ? C13 C14 C15 120(4) . . ? C16 C15 C14 120(3) . . ? C15 C16 C17 122(3) . . ? N3 C17 C16 116(3) . . ? N3 C17 C18 119(3) . . ? C16 C17 C18 125(3) . . ? C17 C18 S4 120(2) . . ? C20 C19 S4 117(2) . . ? N4 C20 C21 125(4) . . ? N4 C20 C19 116(3) . . ? C21 C20 C19 119(3) . . ? C2A C21 C20 116(4) . . ? C21 C2A C23 125(4) . . ? C2A C23 C24 115(4) . . ? N4 C24 C23 122(3) . . ? C1 N1 C5 113(3) . . ? C1 N1 Ag2 126(2) . . ? C5 N1 Ag2 119(2) . . ? C12 N2 C8 112(3) . . ? C12 N2 Ag1 121(2) . . ? C8 N2 Ag1 127(2) . . ? C13 N3 C17 119(3) . . ? C13 N3 Ag1 125(2) . . ? C17 N3 Ag1 116(2) . . ? C24 N4 C20 117(3) . . ? C24 N4 Ag2 119(2) . . ? C20 N4 Ag2 124(2) . . ? C6 S3 C7 104.4(16) . . ? C6 S3 Ag2 89.9(12) . . ? C7 S3 Ag2 108.1(12) . . ? C19 S4 C18 101.9(16) . . ? C19 S4 Ag1 109.3(12) . . ? C18 S4 Ag1 94.3(11) . . ? N2 Ag1 N3 130.0(11) . . ? N2 Ag1 S4 147.7(7) . . ? N3 Ag1 S4 79.5(8) . . ? N2 Ag1 Ag2 74.7(7) . . ? N3 Ag1 Ag2 113.2(7) . . ? S4 Ag1 Ag2 81.7(2) . . ? N4 Ag2 N1 138.4(10) . . ? N4 Ag2 S3 142.0(7) . . ? N1 Ag2 S3 78.9(7) . . ? N4 Ag2 Ag1 77.6(6) . . ? N1 Ag2 Ag1 118.5(6) . . ? S3 Ag2 Ag1 76.0(2) . . ? O21 N22 O23 122(3) . . ? O21 N22 O22 117(3) . . ? O23 N22 O22 121(3) . . ? O13 N11 O12 125(3) . . ? O13 N11 O11 120(3) . . ? O12 N11 O11 115(3) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.30(4) . ? C1 C2 1.37(4) . ? C2 C3 1.31(4) . ? C3 C4 1.34(4) . ? C4 C5 1.37(4) . ? C5 N1 1.35(4) . ? C5 C6 1.53(4) . ? C6 S3 1.80(3) . ? C7 C8 1.48(4) . ? C7 S3 1.82(3) . ? C8 N2 1.33(4) . ? C8 C9 1.39(4) . ? C9 C10 1.36(5) . ? C10 C11 1.43(5) . ? C11 C12 1.37(4) . ? C12 N2 1.33(4) . ? C13 N3 1.33(4) . ? C13 C14 1.33(4) . ? C14 C15 1.36(4) . ? C15 C16 1.31(4) . ? C16 C17 1.43(5) . ? C17 N3 1.41(4) . ? C17 C18 1.50(5) . ? C18 S4 1.79(3) . ? C19 C20 1.60(5) . ? C19 S4 1.79(3) . ? C20 N4 1.33(4) . ? C20 C21 1.37(5) . ? C21 C2A 1.28(4) . ? C2A C23 1.37(5) . ? C23 C24 1.40(4) . ? C24 N4 1.33(4) . ? N1 Ag2 2.29(3) . ? N2 Ag1 2.13(3) . ? N3 Ag1 2.35(3) . ? N4 Ag2 2.23(3) . ? S3 Ag2 2.617(10) . ? S4 Ag1 2.611(10) . ? Ag1 Ag2 2.991(4) . ? O23 N22 1.24(3) . ? O22 N22 1.24(3) . ? O21 N22 1.22(3) . ? N11 O13 1.24(3) . ? N11 O12 1.25(3) . ? N11 O11 1.30(4) . ?
1100702.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100702.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100702 _chemical_formula_sum 'C18 H18 Ag Cl N4 O4 S2' _chemical_formula_weight 561.80 _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 66.954(5) _cell_angle_beta 80.260(5) _cell_angle_gamma 73.600(5) _cell_formula_units_Z 2 _cell_length_a 8.371(5) _cell_length_b 10.844(5) _cell_length_c 13.407(5) _cell_measurement_reflns_used 4302 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 26.45 _cell_measurement_theta_min 2.15 _cell_volume 1072.0(9) _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.972 _diffrn_measured_fraction_theta_max 0.972 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.0274 _diffrn_reflns_av_sigmaI/netI 0.0174 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 13364 _diffrn_reflns_theta_full 26.45 _diffrn_reflns_theta_max 26.45 _diffrn_reflns_theta_min 2.15 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _exptl_absorpt_coefficient_mu 1.293 _exptl_absorpt_correction_T_max 0.7622 _exptl_absorpt_correction_T_min 0.5003 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (sheldrick 1996)' _exptl_crystal_colour pale-yellow _exptl_crystal_density_diffrn 1.741 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description irregular-block _exptl_crystal_F_000 564 _exptl_crystal_size_max 0.84 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.21 _refine_diff_density_max 0.634 _refine_diff_density_min -0.819 _refine_diff_density_rms 0.080 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 294 _refine_ls_number_reflns 4302 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.046 _refine_ls_R_factor_all 0.0331 _refine_ls_R_factor_gt 0.0310 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0528P)^2^+0.7913P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0851 _refine_ls_wR_factor_ref 0.0865 _reflns_number_gt 3983 _reflns_number_total 4302 _reflns_threshold_expression >2sigma(I) _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_sg_symbol_H-M P-1 _cod_database_code 1100702 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.05356(2) 0.80167(2) 0.306790(15) 0.04381(9) Uani 1 1 d . . . Cl1 Cl 0.43093(7) 1.19224(7) 0.19462(5) 0.03960(15) Uani 1 1 d . . . O11 O 0.2576(4) 1.2029(6) 0.1881(4) 0.1363(19) Uani 1 1 d . . . O12 O 0.4449(7) 1.2256(5) 0.2833(3) 0.0939(15) Uani 0.844(6) 1 d P . . O13 O 0.5055(5) 1.0428(4) 0.2280(3) 0.0778(11) Uani 0.844(6) 1 d P . . O14 O 0.5033(5) 1.2668(4) 0.0958(3) 0.0869(13) Uani 0.844(6) 1 d P . . O21 O 0.404(3) 1.1069(19) 0.1636(18) 0.073(6) Uani 0.156(6) 1 d P . . O22 O 0.310(3) 1.284(2) 0.226(3) 0.110(12) Uani 0.156(6) 1 d P . . O23 O 0.596(4) 1.154(3) 0.232(2) 0.118(9) Uiso 0.156(6) 1 d P . . S1 S -0.21172(7) 0.75228(6) 0.44071(5) 0.03230(14) Uani 1 1 d . . . S2 S 0.35235(7) 0.74892(7) 0.20844(5) 0.03720(15) Uani 1 1 d . . . N1 N 0.1732(2) 0.6277(2) 0.50164(17) 0.0315(4) Uani 1 1 d . . . N2 N 0.0118(2) 0.95421(19) 0.41412(16) 0.0315(4) Uani 1 1 d . . . N3 N 0.0288(3) 0.6446(2) 0.20838(18) 0.0366(5) Uani 1 1 d . . . N4 N 0.0172(3) 0.9597(2) 0.11120(16) 0.0340(4) Uani 1 1 d . . . C1 C 0.3271(3) 0.6356(3) 0.5116(2) 0.0359(5) Uani 1 1 d . . . H1 H 0.4101 0.6244 0.4580 0.043 Uiso 1 1 calc R . . C2 C 0.3688(3) 0.6594(3) 0.5969(2) 0.0393(6) Uani 1 1 d . . . H2 H 0.4771 0.6636 0.6004 0.047 Uiso 1 1 calc R . . C3 C 0.2463(4) 0.6769(3) 0.6770(2) 0.0426(6) Uani 1 1 d . . . H3 H 0.2702 0.6938 0.7351 0.051 Uiso 1 1 calc R . . C4 C 0.0866(3) 0.6684(3) 0.6684(2) 0.0358(5) Uani 1 1 d . . . H4 H 0.0020 0.6789 0.7213 0.043 Uiso 1 1 calc R . . C5 C 0.0544(3) 0.6440(2) 0.57978(18) 0.0274(4) Uani 1 1 d . . . C6 C -0.1184(3) 0.6339(2) 0.5674(2) 0.0320(5) Uani 1 1 d . . . H6A H -0.1924 0.6504 0.6272 0.038 Uiso 1 1 calc R . . H6B H -0.1114 0.5404 0.5737 0.038 Uiso 1 1 calc R . . C7 C -0.2715(3) 0.9141(3) 0.4633(2) 0.0353(5) Uani 1 1 d . . . H7A H -0.3275 0.9856 0.4008 0.042 Uiso 1 1 calc R . . H7B H -0.3508 0.9053 0.5260 0.042 Uiso 1 1 calc R . . C8 C -0.1272(3) 0.9591(2) 0.48163(19) 0.0304(5) Uani 1 1 d . . . C9 C 0.1368(3) 0.9952(2) 0.4332(2) 0.0320(5) Uani 1 1 d . . . H9 H 0.2339 0.9930 0.3878 0.038 Uiso 1 1 calc R . . C10 C -0.1252(3) 0.6606(3) 0.1814(2) 0.0426(6) Uani 1 1 d . . . H10 H -0.2138 0.6672 0.2327 0.051 Uiso 1 1 calc R . . C11 C -0.1594(4) 0.6679(3) 0.0820(3) 0.0494(7) Uani 1 1 d . . . H11 H -0.2683 0.6805 0.0663 0.059 Uiso 1 1 calc R . . C12 C -0.0282(5) 0.6562(4) 0.0065(3) 0.0626(9) Uani 1 1 d . . . H12 H -0.0470 0.6612 -0.0616 0.075 Uiso 1 1 calc R . . C13 C 0.1325(4) 0.6366(3) 0.0333(2) 0.0507(7) Uani 1 1 d . . . H13 H 0.2230 0.6262 -0.0161 0.061 Uiso 1 1 calc R . . C14 C 0.1568(3) 0.6328(2) 0.1341(2) 0.0338(5) Uani 1 1 d . . . C15 C 0.3299(3) 0.6152(3) 0.1658(2) 0.0407(6) Uani 1 1 d . . . H15A H 0.4089 0.6123 0.1044 0.049 Uiso 1 1 calc R . . H15B H 0.3596 0.5269 0.2246 0.049 Uiso 1 1 calc R . . C16 C 0.3241(3) 0.8990(3) 0.0841(2) 0.0370(5) Uani 1 1 d . . . H16A H 0.3506 0.9735 0.0959 0.044 Uiso 1 1 calc R . . H16B H 0.4040 0.8776 0.0283 0.044 Uiso 1 1 calc R . . C17 C 0.1518(3) 0.9506(2) 0.04141(19) 0.0304(5) Uani 1 1 d . . . C18 C -0.1332(3) 1.0092(2) 0.06900(19) 0.0348(5) Uani 1 1 d . . . H18 H -0.2284 1.0167 0.1154 0.042 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.03737(13) 0.07352(17) 0.02544(12) -0.02329(10) 0.00675(8) -0.01811(10) Cl1 0.0323(3) 0.0612(4) 0.0290(3) -0.0236(3) 0.0005(2) -0.0078(3) O11 0.0536(18) 0.215(5) 0.102(3) -0.020(3) -0.0216(19) -0.019(3) O12 0.126(4) 0.131(3) 0.065(2) -0.064(2) 0.012(2) -0.061(3) O13 0.076(2) 0.068(2) 0.083(3) -0.0320(18) 0.014(2) -0.0129(17) O14 0.095(3) 0.089(2) 0.0503(18) -0.0132(16) 0.0416(17) -0.0271(19) O21 0.086(13) 0.064(11) 0.112(15) -0.070(12) 0.009(11) -0.036(10) O22 0.097(17) 0.110(16) 0.17(3) -0.121(19) 0.097(18) -0.052(14) S1 0.0258(3) 0.0461(3) 0.0311(3) -0.0194(2) 0.0004(2) -0.0114(2) S2 0.0281(3) 0.0574(4) 0.0253(3) -0.0107(3) -0.0023(2) -0.0149(3) N1 0.0275(9) 0.0326(10) 0.0316(10) -0.0127(8) -0.0018(8) -0.0018(7) N2 0.0312(10) 0.0272(9) 0.0308(10) -0.0096(8) 0.0062(8) -0.0051(8) N3 0.0325(10) 0.0402(11) 0.0347(11) -0.0092(9) -0.0023(8) -0.0112(9) N4 0.0368(11) 0.0336(10) 0.0262(9) -0.0098(8) 0.0063(8) -0.0066(8) C1 0.0255(11) 0.0389(12) 0.0381(13) -0.0132(10) -0.0009(10) -0.0015(9) C2 0.0305(12) 0.0434(13) 0.0403(14) -0.0091(11) -0.0091(10) -0.0081(10) C3 0.0497(15) 0.0485(14) 0.0334(13) -0.0139(11) -0.0098(11) -0.0145(12) C4 0.0393(13) 0.0391(12) 0.0282(12) -0.0121(10) 0.0029(10) -0.0115(10) C5 0.0280(11) 0.0231(10) 0.0280(11) -0.0074(8) -0.0007(8) -0.0048(8) C6 0.0306(11) 0.0314(11) 0.0326(12) -0.0105(9) 0.0040(9) -0.0105(9) C7 0.0241(11) 0.0372(12) 0.0400(13) -0.0141(10) 0.0005(9) -0.0020(9) C8 0.0273(11) 0.0232(10) 0.0333(12) -0.0073(9) 0.0029(9) -0.0022(8) C9 0.0286(11) 0.0272(10) 0.0354(12) -0.0118(9) 0.0088(9) -0.0054(9) C10 0.0349(13) 0.0405(13) 0.0503(16) -0.0105(12) -0.0062(11) -0.0128(11) C11 0.0515(16) 0.0427(14) 0.0584(18) -0.0122(13) -0.0225(14) -0.0157(12) C12 0.087(3) 0.068(2) 0.0440(17) -0.0202(15) -0.0195(17) -0.0266(19) C13 0.0618(18) 0.0545(17) 0.0402(15) -0.0217(13) 0.0030(13) -0.0180(14) C14 0.0389(13) 0.0253(10) 0.0338(12) -0.0062(9) -0.0013(10) -0.0095(9) C15 0.0322(12) 0.0376(13) 0.0433(14) -0.0081(11) 0.0010(11) -0.0064(10) C16 0.0337(12) 0.0420(13) 0.0344(13) -0.0103(10) 0.0064(10) -0.0181(10) C17 0.0342(12) 0.0244(10) 0.0300(11) -0.0086(9) 0.0052(9) -0.0091(9) C18 0.0351(12) 0.0344(12) 0.0270(11) -0.0089(9) 0.0087(9) -0.0061(9) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ag1 N4 106.47(7) . . ? N2 Ag1 N3 167.51(7) . . ? N4 Ag1 N3 75.20(7) . . ? N2 Ag1 S2 116.73(5) . . ? N4 Ag1 S2 75.80(5) . . ? N3 Ag1 S2 75.75(5) . . ? N2 Ag1 S1 75.13(5) . . ? N4 Ag1 S1 119.92(6) . . ? N3 Ag1 S1 93.21(5) . . ? S2 Ag1 S1 158.33(3) . . ? O21 Cl1 O22 124.1(15) . . ? O21 Cl1 O14 96.2(10) . . ? O22 Cl1 O14 106.8(11) . . ? O21 Cl1 O12 146.9(11) . . ? O22 Cl1 O12 57.7(15) . . ? O14 Cl1 O12 115.4(3) . . ? O21 Cl1 O11 65.2(10) . . ? O22 Cl1 O11 59.0(12) . . ? O14 Cl1 O11 112.1(3) . . ? O12 Cl1 O11 108.1(3) . . ? O21 Cl1 O23 113.0(16) . . ? O22 Cl1 O23 119.2(18) . . ? O14 Cl1 O23 84.6(12) . . ? O12 Cl1 O23 63.5(12) . . ? O11 Cl1 O23 163.3(12) . . ? O21 Cl1 O13 50.7(11) . . ? O22 Cl1 O13 141.1(11) . . ? O14 Cl1 O13 112.0(2) . . ? O12 Cl1 O13 104.8(3) . . ? O11 Cl1 O13 103.4(3) . . ? O23 Cl1 O13 67.1(11) . . ? O22 O11 Cl1 57.3(9) . . ? O22 O11 O21 107.9(12) . . ? Cl1 O11 O21 50.7(6) . . ? O22 O12 Cl1 59.1(7) . . ? O22 O12 O23 116.6(13) . . ? Cl1 O12 O23 59.5(11) . . ? O21 O13 Cl1 54.2(6) . . ? O21 O13 O23 105.3(13) . . ? Cl1 O13 O23 55.4(10) . . ? O13 O21 Cl1 75.1(11) . . ? O13 O21 O11 120.1(14) . . ? Cl1 O21 O11 64.1(7) . . ? O12 O22 Cl1 63.2(12) . . ? O12 O22 O11 116.7(16) . . ? Cl1 O22 O11 63.7(7) . . ? Cl1 O23 O12 57.0(11) . . ? Cl1 O23 O13 57.4(11) . . ? O12 O23 O13 94.3(16) . . ? C7 S1 C6 101.34(12) . . ? C7 S1 Ag1 97.09(8) . . ? C6 S1 Ag1 102.32(8) . . ? C16 S2 C15 102.19(13) . . ? C16 S2 Ag1 98.93(9) . . ? C15 S2 Ag1 99.52(9) . . ? C5 N1 C1 117.5(2) . . ? C9 N2 C8 116.9(2) . . ? C9 N2 Ag1 123.08(15) . . ? C8 N2 Ag1 116.81(16) . . ? C10 N3 C14 117.7(2) . . ? C10 N3 Ag1 115.66(18) . . ? C14 N3 Ag1 112.32(16) . . ? C17 N4 C18 116.9(2) . . ? C17 N4 Ag1 116.56(16) . . ? C18 N4 Ag1 121.75(15) . . ? N1 C1 C2 123.8(2) . . ? C1 C2 C3 118.7(2) . . ? C2 C3 C4 118.4(2) . . ? C3 C4 C5 119.5(2) . . ? N1 C5 C4 122.2(2) . . ? N1 C5 C6 116.6(2) . . ? C4 C5 C6 121.1(2) . . ? C5 C6 S1 115.61(16) . . ? C8 C7 S1 114.19(16) . . ? N2 C8 C9 120.3(2) . 2_576 ? N2 C8 C7 118.8(2) . . ? C9 C8 C7 120.8(2) 2_576 . ? N2 C9 C8 122.7(2) . 2_576 ? N3 C10 C11 123.8(3) . . ? C12 C11 C10 118.2(3) . . ? C11 C12 C13 119.1(3) . . ? C14 C13 C12 119.3(3) . . ? N3 C14 C13 121.9(3) . . ? N3 C14 C15 116.9(2) . . ? C13 C14 C15 121.2(3) . . ? C14 C15 S2 115.20(18) . . ? C17 C16 S2 116.11(16) . . ? N4 C17 C18 120.5(2) . 2_575 ? N4 C17 C16 119.1(2) . . ? C18 C17 C16 120.4(2) 2_575 . ? N4 C18 C17 122.6(2) . 2_575 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N2 2.509(2) . ? Ag1 N4 2.523(2) . ? Ag1 N3 2.596(2) . ? Ag1 S2 2.6436(14) . ? Ag1 S1 2.6480(12) . ? Cl1 O21 1.237(12) . ? Cl1 O22 1.348(16) . ? Cl1 O14 1.393(3) . ? Cl1 O12 1.403(3) . ? Cl1 O11 1.437(4) . ? Cl1 O23 1.44(3) . ? Cl1 O13 1.474(4) . ? O11 O22 1.37(2) . ? O11 O21 1.451(19) . ? O12 O22 1.33(3) . ? O12 O23 1.50(3) . ? O13 O21 1.18(2) . ? O13 O23 1.61(3) . ? S1 C7 1.814(3) . ? S1 C6 1.822(3) . ? S2 C16 1.810(3) . ? S2 C15 1.818(3) . ? N1 C5 1.346(3) . ? N1 C1 1.347(3) . ? N2 C9 1.342(3) . ? N2 C8 1.350(3) . ? N3 C10 1.344(3) . ? N3 C14 1.348(3) . ? N4 C17 1.345(3) . ? N4 C18 1.347(3) . ? C1 C2 1.384(4) . ? C2 C3 1.385(4) . ? C3 C4 1.393(4) . ? C4 C5 1.396(3) . ? C5 C6 1.522(3) . ? C7 C8 1.511(3) . ? C8 C9 1.395(3) 2_576 ? C9 C8 1.395(3) 2_576 ? C10 C11 1.378(4) . ? C11 C12 1.376(5) . ? C12 C13 1.388(5) . ? C13 C14 1.383(4) . ? C14 C15 1.519(4) . ? C16 C17 1.514(4) . ? C17 C18 1.393(3) 2_575 ? C18 C17 1.393(3) 2_575 ?
1100703.cif	#------------------------------------------------------------------------------ #$Date: 2016-03-29 03:17:44 +0300 (Tue, 29 Mar 2016) $ #$Revision: 180573 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100703.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100703 loop_ _publ_author_name 'Caradoc-Davies, Paula L.' 'Hanton, Lyall R.' 'Henderson, William' _publ_section_title ; Coordination polymers and isomerism; a study using silver(I) and a \p-stacked ligand ; _journal_coden_ASTM JCSDAA _journal_issue 19 _journal_name_full ; Journal of the Chemical Society, Dalton Transactions ; _journal_page_first 2749 _journal_page_last 2755 _journal_paper_doi 10.1039/b104284j _journal_year 2001 _chemical_formula_sum 'C36 H36 Ag4 N12 O13 S4' _chemical_formula_weight 1404.49 _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 100.182(5) _cell_angle_beta 92.571(5) _cell_angle_gamma 115.658(5) _cell_formula_units_Z 2 _cell_length_a 11.445(5) _cell_length_b 13.146(5) _cell_length_c 17.529(5) _cell_measurement_reflns_used 8192 _cell_measurement_temperature 163(2) _cell_measurement_theta_max 26.45 _cell_measurement_theta_min 1.98 _cell_volume 2317.8(15) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'Bruker SHELXTL' _diffrn_ambient_temperature 163(2) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.980 _diffrn_measured_fraction_theta_max 0.980 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.0366 _diffrn_reflns_av_sigmaI/netI 0.0461 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 30447 _diffrn_reflns_theta_full 26.45 _diffrn_reflns_theta_max 26.45 _diffrn_reflns_theta_min 1.98 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _exptl_absorpt_coefficient_mu 1.921 _exptl_absorpt_correction_T_max 0.7941 _exptl_absorpt_correction_T_min 0.6506 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (sheldrick 1996)' _exptl_crystal_colour pale-yellow _exptl_crystal_density_diffrn 2.012 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description wedge _exptl_crystal_F_000 1384 _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _refine_diff_density_max 1.311 _refine_diff_density_min -0.564 _refine_diff_density_rms 0.102 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.951 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 682 _refine_ls_number_reflns 9379 _refine_ls_number_restraints 60 _refine_ls_restrained_S_all 0.959 _refine_ls_R_factor_all 0.0659 _refine_ls_R_factor_gt 0.0390 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0625P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0979 _refine_ls_wR_factor_ref 0.1061 _reflns_number_gt 6229 _reflns_number_total 9379 _reflns_threshold_expression >2sigma(I) _cod_data_source_file b104284j.txt _cod_data_source_block '[Ag2(L)](NO3)2' _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_sg_symbol_H-M P-1 _cod_database_code 1100703 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.9425(5) 0.9197(4) 1.0410(3) 0.0418(12) Uani 1 1 d . . . H1 H 1.9046 0.8647 1.0708 0.050 Uiso 1 1 calc R . . C2 C 1.9338(5) 0.9882(4) 0.9304(3) 0.0386(11) Uani 1 1 d . . . C3 C 1.8644(5) 0.9806(4) 0.8532(3) 0.0441(12) Uani 1 1 d . . . H3A H 1.9297 1.0219 0.8221 0.053 Uiso 1 1 calc R . . H3B H 1.8107 1.0205 0.8630 0.053 Uiso 1 1 calc R . . C4 C 1.8813(5) 0.7904(5) 0.7590(3) 0.0528(14) Uani 1 1 d . . . H4A H 1.8364 0.7217 0.7175 0.063 Uiso 1 1 calc R . . H4B H 1.9436 0.8505 0.7362 0.063 Uiso 1 1 calc R . . C5 C 1.9556(5) 0.7643(4) 0.8195(3) 0.0467(13) Uani 1 1 d . . . C6 C 2.0849(5) 0.8419(5) 0.8504(4) 0.0579(15) Uani 1 1 d . . . H6 H 2.1276 0.9093 0.8323 0.069 Uiso 1 1 calc R . . C7 C 2.1490(6) 0.8178(6) 0.9081(4) 0.0677(17) Uani 1 1 d . . . H7 H 2.2341 0.8699 0.9304 0.081 Uiso 1 1 calc R . . C8 C 2.0844(6) 0.7148(6) 0.9321(4) 0.0655(17) Uani 1 1 d . . . H8 H 2.1262 0.6953 0.9696 0.079 Uiso 1 1 calc R . . C9 C 1.9562(6) 0.6415(5) 0.8990(3) 0.0603(15) Uani 1 1 d . . . H9 H 1.9125 0.5732 0.9161 0.072 Uiso 1 1 calc R . . C10 C 1.6315(6) 0.3290(5) 0.8952(4) 0.0561(15) Uani 1 1 d . . . H10 H 1.7206 0.3728 0.9124 0.067 Uiso 1 1 calc R . . C11 C 1.5651(6) 0.2274(5) 0.9216(4) 0.0581(15) Uani 1 1 d . . . H11 H 1.6088 0.2041 0.9554 0.070 Uiso 1 1 calc R . . C12 C 1.4347(7) 0.1632(5) 0.8966(4) 0.0651(17) Uani 1 1 d . . . H12 H 1.3875 0.0958 0.9140 0.078 Uiso 1 1 calc R . . C13 C 1.3721(6) 0.1990(5) 0.8449(3) 0.0569(15) Uani 1 1 d . . . H13 H 1.2836 0.1549 0.8260 0.068 Uiso 1 1 calc R . . C14 C 1.4454(5) 0.3031(4) 0.8218(3) 0.0448(12) Uani 1 1 d . . . C15 C 1.3793(5) 0.3434(5) 0.7665(3) 0.0547(14) Uani 1 1 d . . . H15A H 1.2867 0.3095 0.7714 0.066 Uiso 1 1 calc R . . H15B H 1.3874 0.3126 0.7135 0.066 Uiso 1 1 calc R . . C16 C 1.3753(4) 0.5315(4) 0.8683(3) 0.0403(12) Uani 1 1 d . . . H16A H 1.3874 0.6106 0.8769 0.048 Uiso 1 1 calc R . . H16B H 1.2821 0.4812 0.8623 0.048 Uiso 1 1 calc R . . C17 C 1.4406(4) 0.5168(4) 0.9386(3) 0.0316(10) Uani 1 1 d . . . C18 C 1.6240(4) 0.5768(4) 1.0265(3) 0.0336(10) Uani 1 1 d . . . H18 H 1.7107 0.6282 1.0459 0.040 Uiso 1 1 calc R . . C19 C 1.0885(5) 0.4766(5) 0.7364(3) 0.0497(13) Uani 1 1 d . . . H19 H 1.0345 0.4604 0.7752 0.060 Uiso 1 1 calc R . . C20 C 1.1582(6) 0.5896(5) 0.7310(3) 0.0573(15) Uani 1 1 d . . . H20 H 1.1520 0.6484 0.7661 0.069 Uiso 1 1 calc R . . C21 C 1.2382(6) 0.6158(5) 0.6728(3) 0.0574(15) Uani 1 1 d . . . H21 H 1.2876 0.6920 0.6689 0.069 Uiso 1 1 calc R . . C22 C 1.2422(5) 0.5268(5) 0.6217(3) 0.0484(13) Uani 1 1 d . . . H22 H 1.2936 0.5418 0.5816 0.058 Uiso 1 1 calc R . . C23 C 1.1693(5) 0.4132(4) 0.6294(3) 0.0431(12) Uani 1 1 d . . . C24 C 1.1740(5) 0.3134(5) 0.5741(3) 0.0506(14) Uani 1 1 d . . . H24A H 1.2050 0.2730 0.6046 0.061 Uiso 1 1 calc R . . H24B H 1.2380 0.3446 0.5395 0.061 Uiso 1 1 calc R . . C26 C 1.0114(5) 0.2871(4) 0.4409(3) 0.0471(13) Uani 1 1 d . . . H26A H 1.0880 0.3047 0.4142 0.057 Uiso 1 1 calc R . . H26B H 0.9352 0.2369 0.4026 0.057 Uiso 1 1 calc R . . C27 C 1.0032(5) 0.3989(4) 0.4721(3) 0.0374(11) Uani 1 1 d . . . C28 C 1.0767(4) 0.4980(4) 0.4447(3) 0.0380(11) Uani 1 1 d . . . H28 H 1.1296 0.4945 0.4066 0.046 Uiso 1 1 calc R . . C30 C 0.5375(5) 0.1722(4) 0.6367(3) 0.0428(12) Uani 1 1 d . . . H30A H 0.4687 0.1375 0.6678 0.051 Uiso 1 1 calc R . . H30B H 0.5256 0.2340 0.6201 0.051 Uiso 1 1 calc R . . C31 C 0.5198(4) 0.0815(4) 0.5644(3) 0.0348(11) Uani 1 1 d . . . C32 C 0.3993(4) -0.0116(4) 0.5385(3) 0.0383(11) Uani 1 1 d . . . H32 H 0.3300 -0.0181 0.5663 0.046 Uiso 1 1 calc R . . C33 C 0.6772(5) 0.1135(4) 0.7410(3) 0.0481(13) Uani 1 1 d . . . H33A H 0.7462 0.1414 0.7847 0.058 Uiso 1 1 calc R . . H33B H 0.5943 0.0838 0.7615 0.058 Uiso 1 1 calc R . . C34 C 0.6838(5) 0.0157(4) 0.6850(3) 0.0416(12) Uani 1 1 d . . . C35 C 0.5757(5) -0.0878(4) 0.6588(3) 0.0508(14) Uani 1 1 d . . . H35 H 0.4973 -0.1010 0.6782 0.061 Uiso 1 1 calc R . . C36 C 0.5832(6) -0.1726(5) 0.6035(4) 0.0610(16) Uani 1 1 d . . . H36 H 0.5097 -0.2426 0.5840 0.073 Uiso 1 1 calc R . . C37 C 0.7023(6) -0.1514(5) 0.5777(4) 0.0614(16) Uani 1 1 d . . . H37 H 0.7104 -0.2070 0.5405 0.074 Uiso 1 1 calc R . . C38 C 0.8084(6) -0.0470(5) 0.6080(3) 0.0522(14) Uani 1 1 d . . . H38 H 0.8885 -0.0329 0.5907 0.063 Uiso 1 1 calc R . . N1 N 1.8773(4) 0.9077(3) 0.9727(2) 0.0412(10) Uani 1 1 d . A . N2 N 1.8929(4) 0.6641(4) 0.8442(3) 0.0479(11) Uani 1 1 d . . . N3 N 1.5741(4) 0.3668(3) 0.8463(2) 0.0435(10) Uani 1 1 d . . . N4 N 1.5654(3) 0.5952(3) 0.9660(2) 0.0314(8) Uani 1 1 d . A . N5 N 1.0951(4) 0.3886(3) 0.6878(2) 0.0425(10) Uani 1 1 d . . . N6 N 0.9272(3) 0.4014(3) 0.5278(2) 0.0361(9) Uani 1 1 d . . . N7 N 0.6216(4) 0.0930(3) 0.5254(2) 0.0357(9) Uani 1 1 d . . . N8 N 0.8004(4) 0.0355(3) 0.6616(2) 0.0442(10) Uani 1 1 d . . . N11 N 1.1466(4) 0.0426(4) 0.6740(3) 0.0501(11) Uani 1 1 d . . . N22 N 1.0266(4) 0.3369(4) 0.8842(2) 0.0482(11) Uani 1 1 d . . . O1 O 1.3261(10) 0.8896(10) 0.7321(6) 0.238(5) Uani 1 1 d . . . O11 O 1.1684(6) 0.0836(5) 0.6163(3) 0.1039(18) Uani 1 1 d . . . O12 O 1.1803(5) -0.0350(4) 0.6797(3) 0.0902(15) Uani 1 1 d . . . O13 O 1.0915(4) 0.0726(4) 0.7267(3) 0.0652(11) Uani 1 1 d . . . O21 O 0.9158(4) 0.3207(4) 0.8610(3) 0.0793(13) Uani 1 1 d . . . O22 O 1.0930(4) 0.4208(4) 0.9395(2) 0.0719(12) Uani 1 1 d . . . O23 O 1.0769(4) 0.2753(3) 0.8501(2) 0.0522(9) Uani 1 1 d . . . S1 S 1.76179(13) 0.83662(11) 0.79572(7) 0.0461(3) Uani 1 1 d . A . S2 S 1.43788(12) 0.49912(12) 0.77818(7) 0.0454(3) Uani 1 1 d . . . S3 S 1.02077(12) 0.20883(11) 0.51456(8) 0.0443(3) Uani 1 1 d . . . S4 S 0.69292(13) 0.23502(10) 0.69870(7) 0.0435(3) Uani 1 1 d . . . Ag1 Ag 1.67000(4) 0.74931(3) 0.91325(2) 0.04681(12) Uani 1 1 d . . . Ag2 Ag 1.68025(4) 0.54303(3) 0.80581(2) 0.04963(13) Uani 1 1 d . A . Ag3 Ag 0.82935(4) 0.24007(3) 0.58320(2) 0.04955(13) Uani 1 1 d . . . Ag4 Ag 0.98390(4) 0.20406(3) 0.70546(2) 0.05070(13) Uani 1 1 d . . . N33 N 1.5259(19) 0.9044(16) 0.9085(14) 0.068(4) Uani 0.52(2) 1 d PU A 1 O31 O 1.459(2) 0.7937(19) 0.8559(16) 0.156(10) Uani 0.52(2) 1 d PU A 1 O32 O 1.492(2) 0.9600(17) 0.8815(17) 0.178(10) Uani 0.52(2) 1 d PU A 1 O33 O 1.6142(14) 0.9141(17) 0.9426(8) 0.104(6) Uani 0.52(2) 1 d PU A 1 N331 N 1.4988(16) 0.8824(14) 0.8735(11) 0.044(5) Uani 0.48(2) 1 d PU A 2 O331 O 1.488(2) 0.807(2) 0.9016(14) 0.110(9) Uani 0.48(2) 1 d P A 2 O332 O 1.435(2) 0.915(2) 0.8389(12) 0.121(9) Uani 0.48(2) 1 d P A 2 O333 O 1.6133(18) 0.9776(15) 0.9083(19) 0.174(12) Uani 0.48(2) 1 d P A 2 N44 N 1.6018(3) 0.4636(2) 0.59450(17) 0.0069(6) Uiso 1 1 d D . . O41 O 1.6949(8) 0.5142(8) 0.6565(4) 0.062(2) Uani 0.653(8) 1 d PDU B 3 O42 O 1.4846(5) 0.4006(5) 0.6034(4) 0.065(2) Uani 0.653(8) 1 d PD B 3 O43 O 1.6188(9) 0.5535(7) 0.5556(5) 0.096(3) Uani 0.653(8) 1 d PDU B 3 O441 O 1.6298(10) 0.3910(9) 0.5354(5) 0.062(4) Uani 0.347(8) 1 d PD B 4 O442 O 1.6609(18) 0.5649(15) 0.6003(10) 0.186(11) Uani 0.347(8) 1 d PDU B 4 O443 O 1.6768(14) 0.4636(11) 0.6633(7) 0.044(4) Uani 0.347(8) 1 d PDU A 4 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.050(3) 0.027(3) 0.037(3) 0.012(2) 0.009(2) 0.006(2) C2 0.041(3) 0.026(2) 0.039(3) 0.009(2) 0.008(2) 0.005(2) C3 0.046(3) 0.036(3) 0.042(3) 0.015(2) 0.004(2) 0.008(2) C4 0.060(3) 0.041(3) 0.038(3) 0.012(2) 0.016(3) 0.002(3) C5 0.045(3) 0.044(3) 0.042(3) 0.007(2) 0.014(2) 0.012(2) C6 0.047(3) 0.046(3) 0.065(4) 0.013(3) 0.018(3) 0.005(3) C7 0.042(3) 0.067(4) 0.073(4) 0.003(3) 0.007(3) 0.011(3) C8 0.047(3) 0.073(4) 0.068(4) 0.019(3) 0.004(3) 0.018(3) C9 0.061(4) 0.056(4) 0.059(4) 0.025(3) 0.010(3) 0.018(3) C10 0.050(3) 0.052(4) 0.077(4) 0.016(3) 0.019(3) 0.030(3) C11 0.071(4) 0.040(3) 0.071(4) 0.017(3) 0.014(3) 0.030(3) C12 0.093(5) 0.029(3) 0.066(4) 0.013(3) 0.027(4) 0.019(3) C13 0.057(3) 0.039(3) 0.054(3) -0.002(3) 0.010(3) 0.007(3) C14 0.054(3) 0.036(3) 0.036(3) 0.000(2) 0.013(2) 0.015(2) C15 0.054(3) 0.046(3) 0.044(3) 0.004(3) 0.001(3) 0.007(3) C16 0.035(3) 0.043(3) 0.042(3) 0.019(2) 0.004(2) 0.013(2) C17 0.030(2) 0.029(2) 0.033(2) 0.0046(19) 0.0060(19) 0.0113(19) C18 0.026(2) 0.029(2) 0.037(3) 0.006(2) 0.0062(19) 0.0054(19) C19 0.053(3) 0.045(3) 0.037(3) 0.006(2) 0.001(2) 0.011(3) C20 0.070(4) 0.038(3) 0.051(3) -0.002(3) -0.009(3) 0.018(3) C21 0.058(4) 0.035(3) 0.061(4) 0.012(3) -0.006(3) 0.005(3) C22 0.037(3) 0.046(3) 0.050(3) 0.021(3) 0.000(2) 0.004(2) C23 0.036(3) 0.043(3) 0.041(3) 0.011(2) -0.005(2) 0.009(2) C24 0.037(3) 0.054(3) 0.052(3) 0.015(3) 0.007(2) 0.011(2) C26 0.062(3) 0.037(3) 0.035(3) 0.004(2) 0.009(2) 0.016(3) C27 0.042(3) 0.039(3) 0.027(2) 0.009(2) 0.006(2) 0.013(2) C28 0.036(3) 0.043(3) 0.033(3) 0.012(2) 0.012(2) 0.015(2) C30 0.048(3) 0.038(3) 0.040(3) 0.002(2) 0.011(2) 0.019(2) C31 0.034(2) 0.032(3) 0.040(3) 0.012(2) 0.008(2) 0.015(2) C32 0.034(2) 0.041(3) 0.040(3) 0.008(2) 0.010(2) 0.017(2) C33 0.049(3) 0.046(3) 0.040(3) 0.016(2) 0.007(2) 0.011(2) C34 0.046(3) 0.030(3) 0.041(3) 0.015(2) 0.000(2) 0.007(2) C35 0.047(3) 0.040(3) 0.057(3) 0.020(3) 0.005(3) 0.009(2) C36 0.065(4) 0.031(3) 0.066(4) 0.010(3) -0.006(3) 0.003(3) C37 0.071(4) 0.035(3) 0.067(4) -0.002(3) -0.001(3) 0.019(3) C38 0.058(3) 0.042(3) 0.052(3) 0.008(3) 0.008(3) 0.020(3) N1 0.041(2) 0.031(2) 0.037(2) 0.0122(18) 0.0041(18) 0.0022(18) N2 0.038(2) 0.045(3) 0.049(3) 0.015(2) 0.008(2) 0.006(2) N3 0.042(2) 0.036(2) 0.052(3) 0.010(2) 0.017(2) 0.016(2) N4 0.0279(19) 0.029(2) 0.032(2) 0.0073(16) 0.0087(16) 0.0072(16) N5 0.043(2) 0.037(2) 0.035(2) 0.0080(19) -0.0015(19) 0.0082(19) N6 0.031(2) 0.039(2) 0.033(2) 0.0119(18) 0.0053(17) 0.0081(17) N7 0.034(2) 0.031(2) 0.037(2) 0.0031(18) 0.0050(17) 0.0108(17) N8 0.047(3) 0.030(2) 0.046(2) 0.011(2) 0.000(2) 0.0088(19) N11 0.048(3) 0.031(2) 0.056(3) 0.008(2) 0.003(2) 0.004(2) N22 0.037(2) 0.060(3) 0.038(2) 0.018(2) 0.007(2) 0.010(2) O1 0.202(10) 0.278(13) 0.233(11) -0.002(9) 0.042(8) 0.129(10) O11 0.157(5) 0.090(4) 0.070(3) 0.041(3) 0.040(3) 0.050(4) O12 0.124(4) 0.071(3) 0.085(3) 0.010(3) 0.021(3) 0.053(3) O13 0.051(2) 0.070(3) 0.068(3) 0.005(2) 0.017(2) 0.025(2) O21 0.039(2) 0.098(4) 0.086(3) 0.015(3) -0.001(2) 0.021(2) O22 0.060(3) 0.088(3) 0.049(2) -0.008(2) 0.002(2) 0.025(2) O23 0.064(2) 0.047(2) 0.046(2) 0.0148(18) 0.0144(19) 0.023(2) S1 0.0467(7) 0.0388(7) 0.0387(7) 0.0139(6) 0.0003(6) 0.0048(6) S2 0.0436(7) 0.0491(8) 0.0346(7) 0.0143(6) 0.0019(5) 0.0111(6) S3 0.0459(7) 0.0324(7) 0.0467(7) 0.0074(6) 0.0061(6) 0.0111(6) S4 0.0492(7) 0.0310(7) 0.0374(7) 0.0024(5) 0.0055(6) 0.0081(6) Ag1 0.0451(2) 0.0344(2) 0.0472(2) 0.01484(18) 0.00901(18) 0.00294(17) Ag2 0.0450(2) 0.0429(2) 0.0482(2) 0.01152(19) 0.01456(18) 0.00673(18) Ag3 0.0381(2) 0.0439(2) 0.0486(2) 0.01869(19) 0.00614(18) -0.00128(17) Ag4 0.0485(2) 0.0376(2) 0.0499(3) 0.01352(18) 0.00248(19) 0.00350(18) N33 0.064(8) 0.068(10) 0.078(11) 0.044(7) 0.019(8) 0.023(8) O31 0.173(15) 0.057(9) 0.20(2) 0.032(11) -0.005(13) 0.015(9) O32 0.22(2) 0.103(11) 0.22(2) 0.000(12) -0.077(17) 0.105(13) O33 0.105(9) 0.127(15) 0.109(10) 0.030(8) 0.022(7) 0.077(10) N331 0.048(6) 0.037(6) 0.057(6) 0.019(4) 0.014(4) 0.023(4) O331 0.122(16) 0.085(14) 0.17(2) 0.091(15) 0.096(15) 0.059(13) O332 0.148(16) 0.19(2) 0.124(15) 0.107(15) 0.083(13) 0.134(16) O333 0.104(12) 0.091(11) 0.37(3) 0.091(16) 0.099(16) 0.063(10) O41 0.066(5) 0.070(6) 0.060(5) 0.029(4) 0.040(4) 0.031(4) O42 0.048(4) 0.051(4) 0.083(5) 0.014(3) -0.024(3) 0.015(3) O43 0.112(7) 0.082(5) 0.068(5) 0.052(5) 0.021(5) 0.004(5) O441 0.052(7) 0.053(7) 0.038(6) -0.001(5) -0.015(5) -0.010(5) O442 0.23(2) 0.40(3) 0.047(10) 0.003(17) -0.012(13) 0.27(2) O443 0.051(5) 0.046(5) 0.034(5) 0.013(4) 0.003(4) 0.021(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 122.4(4) . 2_977 ? N1 C2 C1 119.7(4) . 2_977 ? N1 C2 C3 120.5(4) . . ? C1 C2 C3 119.8(4) 2_977 . ? C2 C3 S1 116.3(3) . . ? C5 C4 S1 114.8(4) . . ? N2 C5 C6 120.8(5) . . ? N2 C5 C4 118.3(4) . . ? C6 C5 C4 120.9(5) . . ? C7 C6 C5 119.6(5) . . ? C6 C7 C8 118.9(5) . . ? C9 C8 C7 118.6(6) . . ? N2 C9 C8 123.1(6) . . ? N3 C10 C11 123.7(5) . . ? C12 C11 C10 118.2(6) . . ? C11 C12 C13 119.7(5) . . ? C12 C13 C14 118.6(5) . . ? N3 C14 C13 122.0(5) . . ? N3 C14 C15 118.7(5) . . ? C13 C14 C15 119.3(5) . . ? C14 C15 S2 117.4(4) . . ? C17 C16 S2 113.3(3) . . ? N4 C17 C18 121.0(4) . 2_867 ? N4 C17 C16 117.8(4) . . ? C18 C17 C16 121.2(4) 2_867 . ? N4 C18 C17 122.4(4) . 2_867 ? N5 C19 C20 122.5(5) . . ? C19 C20 C21 119.7(5) . . ? C22 C21 C20 118.1(5) . . ? C21 C22 C23 120.1(5) . . ? N5 C23 C22 121.4(5) . . ? N5 C23 C24 117.7(4) . . ? C22 C23 C24 120.9(5) . . ? C23 C24 S3 116.1(4) . . ? C27 C26 S3 114.9(3) . . ? N6 C27 C28 120.7(4) . . ? N6 C27 C26 118.9(4) . . ? C28 C27 C26 120.4(4) . . ? N6 C28 C27 121.6(4) 2_766 . ? C31 C30 S4 116.1(3) . . ? N7 C31 C32 120.1(4) . . ? N7 C31 C30 119.9(4) . . ? C32 C31 C30 120.0(4) . . ? N7 C32 C31 122.2(4) 2_656 . ? C34 C33 S4 114.7(3) . . ? N8 C34 C35 121.7(5) . . ? N8 C34 C33 116.9(4) . . ? C35 C34 C33 121.4(5) . . ? C34 C35 C36 119.8(5) . . ? C35 C36 C37 118.6(5) . . ? C38 C37 C36 119.0(6) . . ? N8 C38 C37 122.2(5) . . ? C1 N1 C2 117.9(4) . . ? C1 N1 Ag1 126.0(3) . . ? C2 N1 Ag1 116.0(3) . . ? C9 N2 C5 118.9(5) . . ? C9 N2 Ag2 117.8(4) . . ? C5 N2 Ag2 123.0(3) . . ? C10 N3 C14 117.8(5) . . ? C10 N3 Ag2 124.7(4) . . ? C14 N3 Ag2 117.4(3) . . ? C18 N4 C17 116.6(4) . . ? C18 N4 Ag1 121.6(3) . . ? C17 N4 Ag1 121.8(3) . . ? C19 N5 C23 118.0(4) . . ? C19 N5 Ag4 120.1(3) . . ? C23 N5 Ag4 121.9(3) . . ? C27 N6 C28 117.8(4) . 2_766 ? C27 N6 Ag3 118.9(3) . . ? C28 N6 Ag3 122.9(3) 2_766 . ? C32 N7 C31 117.7(4) 2_656 . ? C32 N7 Ag3 124.2(3) 2_656 . ? C31 N7 Ag3 117.6(3) . . ? C38 N8 C34 118.6(4) . . ? C38 N8 Ag4 118.1(4) . . ? C34 N8 Ag4 123.2(3) . . ? O11 N11 O13 123.3(5) . . ? O11 N11 O12 117.9(6) . . ? O13 N11 O12 118.8(5) . . ? O21 N22 O22 118.5(5) . . ? O21 N22 O23 121.3(5) . . ? O22 N22 O23 120.1(4) . . ? N11 O13 Ag4 119.5(4) . . ? N22 O23 Ag4 109.9(3) . . ? C3 S1 C4 102.4(2) . . ? C3 S1 Ag1 95.31(16) . . ? C4 S1 Ag1 111.59(17) . . ? C16 S2 C15 100.4(2) . . ? C16 S2 Ag2 111.03(15) . . ? C15 S2 Ag2 93.41(19) . . ? C26 S3 C24 100.6(3) . . ? C26 S3 Ag3 91.73(18) . . ? C24 S3 Ag3 106.51(18) . . ? C30 S4 C33 100.7(2) . . ? C30 S4 Ag3 94.77(16) . . ? C33 S4 Ag3 107.84(18) . . ? N4 Ag1 N1 122.99(13) . . ? N4 Ag1 O33 118.9(4) . . ? N1 Ag1 O33 77.7(4) . . ? N4 Ag1 O331 97.9(4) . . ? N1 Ag1 O331 113.6(6) . . ? O33 Ag1 O331 35.9(6) . . ? N4 Ag1 S1 150.59(10) . . ? N1 Ag1 S1 77.66(10) . . ? O33 Ag1 S1 83.8(4) . . ? O331 Ag1 S1 90.7(4) . . ? N4 Ag1 Ag2 73.37(10) . . ? N1 Ag1 Ag2 116.28(10) . . ? O33 Ag1 Ag2 154.1(3) . . ? O331 Ag1 Ag2 124.9(6) . . ? S1 Ag1 Ag2 78.62(4) . . ? N2 Ag2 N3 122.62(15) . . ? N2 Ag2 O443 102.4(4) . . ? N3 Ag2 O443 98.9(3) . . ? N2 Ag2 S2 152.56(12) . . ? N3 Ag2 S2 78.50(11) . . ? O443 Ag2 S2 90.0(3) . . ? N2 Ag2 Ag1 77.69(12) . . ? N3 Ag2 Ag1 114.12(10) . . ? O443 Ag2 Ag1 140.9(3) . . ? S2 Ag2 Ag1 77.36(4) . . ? N6 Ag3 N7 118.97(13) . . ? N6 Ag3 S4 123.14(10) . . ? N7 Ag3 S4 78.34(10) . . ? N6 Ag3 S3 76.47(10) . . ? N7 Ag3 S3 111.27(10) . . ? S4 Ag3 S3 152.00(5) . . ? N6 Ag3 Ag4 119.70(9) . . ? N7 Ag3 Ag4 120.45(10) . . ? S4 Ag3 Ag4 78.56(4) . . ? S3 Ag3 Ag4 73.96(4) . . ? N8 Ag4 N5 143.40(14) . . ? N8 Ag4 O23 121.21(13) . . ? N5 Ag4 O23 89.58(13) . . ? N8 Ag4 O13 84.57(14) . . ? N5 Ag4 O13 124.45(14) . . ? O23 Ag4 O13 76.94(13) . . ? N8 Ag4 Ag3 72.48(10) . . ? N5 Ag4 Ag3 70.94(10) . . ? O23 Ag4 Ag3 142.11(9) . . ? O13 Ag4 Ag3 140.89(10) . . ? O33 N33 O32 138(3) . . ? O33 N33 O31 112(2) . . ? O32 N33 O31 103(2) . . ? N33 O33 Ag1 116.6(18) . . ? O331 N331 O332 141(2) . . ? O331 N331 O333 109(2) . . ? O332 N331 O333 107.8(17) . . ? N331 O331 Ag1 121.3(14) . . ? O442 N44 O42 131.5(10) . . ? O442 N44 O41 67.7(8) . . ? O42 N44 O41 119.8(5) . . ? O442 N44 O43 37.1(8) . . ? O42 N44 O43 115.2(5) . . ? O41 N44 O43 104.5(5) . . ? O442 N44 O441 117.2(10) . . ? O42 N44 O441 103.7(5) . . ? O41 N44 O441 112.6(6) . . ? O43 N44 O441 99.2(6) . . ? O442 N44 O443 93.9(9) . . ? O42 N44 O443 102.9(7) . . ? O41 N44 O443 26.2(5) . . ? O43 N44 O443 130.5(6) . . ? O441 N44 O443 101.0(7) . . ? N44 O443 Ag2 129.8(9) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.329(6) . ? C1 C2 1.399(6) 2_977 ? C2 N1 1.348(6) . ? C2 C1 1.399(6) 2_977 ? C2 C3 1.502(6) . ? C3 S1 1.809(5) . ? C4 C5 1.505(7) . ? C4 S1 1.821(6) . ? C5 N2 1.360(6) . ? C5 C6 1.396(7) . ? C6 C7 1.381(8) . ? C7 C8 1.386(9) . ? C8 C9 1.385(8) . ? C9 N2 1.328(7) . ? C10 N3 1.340(7) . ? C10 C11 1.395(8) . ? C11 C12 1.361(8) . ? C12 C13 1.394(8) . ? C13 C14 1.404(7) . ? C14 N3 1.343(6) . ? C14 C15 1.503(8) . ? C15 S2 1.825(6) . ? C16 C17 1.498(6) . ? C16 S2 1.821(5) . ? C17 N4 1.350(5) . ? C17 C18 1.398(6) 2_867 ? C18 N4 1.341(5) . ? C18 C17 1.398(6) 2_867 ? C19 N5 1.342(7) . ? C19 C20 1.372(7) . ? C20 C21 1.390(8) . ? C21 C22 1.361(8) . ? C22 C23 1.396(7) . ? C23 N5 1.352(6) . ? C23 C24 1.510(7) . ? C24 S3 1.816(5) . ? C26 C27 1.519(7) . ? C26 S3 1.813(5) . ? C27 N6 1.344(6) . ? C27 C28 1.394(6) . ? C28 N6 1.345(6) 2_766 ? C30 C31 1.517(6) . ? C30 S4 1.807(5) . ? C31 N7 1.343(6) . ? C31 C32 1.375(6) . ? C32 N7 1.336(6) 2_656 ? C33 C34 1.506(7) . ? C33 S4 1.821(5) . ? C34 N8 1.343(6) . ? C34 C35 1.365(7) . ? C35 C36 1.377(8) . ? C36 C37 1.383(8) . ? C37 C38 1.371(7) . ? C38 N8 1.343(7) . ? N1 Ag1 2.405(4) . ? N2 Ag2 2.242(4) . ? N3 Ag2 2.359(4) . ? N4 Ag1 2.248(4) . ? N5 Ag4 2.287(4) . ? N6 C28 1.345(6) 2_766 ? N6 Ag3 2.337(4) . ? N7 C32 1.336(6) 2_656 ? N7 Ag3 2.352(4) . ? N8 Ag4 2.266(4) . ? N11 O11 1.214(6) . ? N11 O13 1.243(6) . ? N11 O12 1.255(6) . ? N22 O21 1.228(5) . ? N22 O22 1.250(5) . ? N22 O23 1.268(6) . ? O13 Ag4 2.583(4) . ? O23 Ag4 2.548(4) . ? S1 Ag1 2.5790(14) . ? S2 Ag2 2.5799(18) . ? S3 Ag3 2.6939(17) . ? S4 Ag3 2.6043(15) . ? Ag1 O33 2.490(17) . ? Ag1 O331 2.52(2) . ? Ag1 Ag2 3.0666(11) . ? Ag2 O443 2.523(13) . ? Ag3 Ag4 2.9477(9) . ? N33 O33 1.10(2) . ? N33 O32 1.13(3) . ? N33 O31 1.43(4) . ? N331 O331 1.15(3) . ? N331 O332 1.181(18) . ? N331 O333 1.38(3) . ? N44 O442 1.187(17) . ? N44 O42 1.269(6) . ? N44 O41 1.337(8) . ? N44 O43 1.413(8) . ? N44 O441 1.425(11) . ? N44 O443 1.449(11) . ?
1100704.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-24 15:32:01 +0200 (Wed, 24 Feb 2016) $ #$Revision: 176868 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100704.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100704 loop_ _publ_author_name 'Caradoc-Davies, Paula L.' 'Hanton, Lyall R.' _publ_section_title ; Formation of a Single-Stranded Silver(I) Helical Coordination Polymer Containing \p-Stacked Planar Chiral N~4~S~2~ Ligands ; _journal_issue 12 _journal_name_full ; Chemical Communications (Cambridge, United Kingdom) ; _journal_page_first 1098 _journal_page_last 1099 _journal_paper_doi 10.1039/b101875m _journal_year 2001 _chemical_formula_sum 'C20 H22 Ag2 Cl2 N4 O8 S2' _chemical_formula_weight 797.18 _space_group_IT_number 179 _symmetry_cell_setting hexagonal _symmetry_space_group_name_Hall 'P 65 2 (0 0 1)' _symmetry_space_group_name_H-M 'P 65 2 2' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_formula_units_Z 6 _cell_length_a 9.182(2) _cell_length_b 9.182(2) _cell_length_c 52.480(18) _cell_measurement_reflns_used 2623 _cell_measurement_temperature 163(2) _cell_measurement_theta_max 26.33 _cell_measurement_theta_min 2.33 _cell_volume 3831.7(19) _diffrn_ambient_temperature 163(2) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0455 _diffrn_reflns_av_sigmaI/netI 0.0156 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 65 _diffrn_reflns_limit_l_min -65 _diffrn_reflns_number 49638 _diffrn_reflns_theta_full 26.33 _diffrn_reflns_theta_max 26.33 _diffrn_reflns_theta_min 2.33 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _exptl_absorpt_coefficient_mu 1.961 _exptl_absorpt_correction_T_max 0.7109 _exptl_absorpt_correction_T_min 0.5877 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (sheldrick 1996)' _exptl_crystal_colour pale-orange _exptl_crystal_density_diffrn 2.073 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 2364 _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _refine_diff_density_max 0.499 _refine_diff_density_min -0.885 _refine_diff_density_rms 0.112 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.05(7) _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.177 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 173 _refine_ls_number_reflns 2623 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.177 _refine_ls_R_factor_all 0.0434 _refine_ls_R_factor_gt 0.0420 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0144P)^2^+25.3451P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0887 _refine_ls_wR_factor_ref 0.0893 _reflns_number_gt 2553 _reflns_number_total 2623 _reflns_threshold_expression >2sigma(I) _cod_data_source_file b101875m.txt _cod_data_source_block '[Ag2(L)](ClO4)2' _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Hexagonal' changed to 'hexagonal' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_sg_symbol_H-M P6(5)22 _cod_database_code 1100704 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' '-x, -y, z+1/2' 'y, -x+y, z+1/6' 'x-y, x, z+5/6' 'y, x, -z+2/3' 'x-y, -y, -z' '-x, -x+y, -z+1/3' '-y, -x, -z+1/6' '-x+y, y, -z+1/2' 'x, x-y, -z+5/6' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.56519(7) 0.71190(7) 0.943653(9) 0.02747(13) Uani 1 1 d . . . S1 S 0.3416(2) 0.8043(2) 0.94645(3) 0.0276(3) Uani 1 1 d . . . Cl1 Cl 0.3218(2) 0.3549(2) 0.98048(3) 0.0328(4) Uani 1 1 d . . . O11 O 0.4988(9) 0.4336(10) 0.97691(17) 0.090(3) Uani 1 1 d . . . O12 O 0.2710(10) 0.4622(8) 0.96920(14) 0.081(2) Uani 1 1 d . . . O13 O 0.2887(10) 0.3417(10) 1.00650(10) 0.078(2) Uani 1 1 d . . . O14 O 0.2414(10) 0.1950(9) 0.96869(16) 0.091(2) Uani 1 1 d . . . N1 N 0.6954(6) 0.6208(6) 0.91766(9) 0.0237(11) Uani 1 1 d . . . N2 N 0.6424(7) 0.8765(8) 0.98137(10) 0.0338(13) Uani 1 1 d . . . C1 C 0.8651(9) 0.6982(9) 0.91749(11) 0.0292(14) Uani 1 1 d . . . C2 C 0.9507(9) 0.6532(10) 0.90060(12) 0.0374(17) Uani 1 1 d . . . H2 H 1.0702 0.7116 0.9005 0.045 Uiso 1 1 calc R . . C3 C 0.8607(10) 0.5217(10) 0.88380(13) 0.0398(18) Uani 1 1 d . . . H3 H 0.9177 0.4903 0.8718 0.048 Uiso 1 1 calc R . . C4 C 0.6861(10) 0.4363(10) 0.88466(12) 0.0374(16) Uani 1 1 d . . . H4 H 0.6213 0.3418 0.8740 0.045 Uiso 1 1 calc R . . C5 C 0.6092(9) 0.4929(8) 0.90150(11) 0.0281(14) Uani 1 1 d . . . C6 C 0.4208(9) 1.0079(10) 0.93117(13) 0.0352(15) Uani 1 1 d . . . H6A H 0.3833 0.9898 0.9132 0.042 Uiso 1 1 calc R . . H6B H 0.3706 1.0687 0.9397 0.042 Uiso 1 1 calc R . . C7 C 0.3697(8) 0.8631(9) 0.97974(11) 0.0295(15) Uani 1 1 d . . . H7A H 0.3303 0.9446 0.9824 0.035 Uiso 1 1 calc R . . H7B H 0.2957 0.7617 0.9899 0.035 Uiso 1 1 calc R . . C8 C 0.5469(8) 0.9396(8) 0.99035(10) 0.0230(13) Uani 1 1 d . . . C9 C 0.7954(10) 0.9366(12) 0.99107(13) 0.045(2) Uani 1 1 d . . . H9 H 0.8628 0.8909 0.9856 0.054 Uiso 1 1 calc R . . C10 C 0.9584(8) 0.8372(9) 0.93660(13) 0.0362(16) Uani 1 1 d . . . H10A H 0.8993 0.9004 0.9389 0.054 Uiso 1 1 calc R . . H10B H 1.0726 0.9129 0.9304 0.054 Uiso 1 1 calc R . . H10C H 0.9638 0.7885 0.9529 0.054 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0269(3) 0.0302(3) 0.0271(2) -0.0063(2) 0.0021(2) 0.0157(2) S1 0.0196(7) 0.0368(9) 0.0262(7) -0.0102(7) -0.0042(6) 0.0139(7) Cl1 0.0391(9) 0.0346(9) 0.0308(8) 0.0025(7) 0.0018(7) 0.0229(8) O11 0.056(5) 0.078(5) 0.143(7) 0.019(5) 0.031(5) 0.039(4) O12 0.096(6) 0.054(4) 0.104(5) -0.005(4) -0.051(5) 0.046(4) O13 0.085(5) 0.094(6) 0.038(3) 0.003(3) 0.012(3) 0.032(5) O14 0.095(6) 0.053(4) 0.120(6) -0.039(4) -0.006(5) 0.033(4) N1 0.027(3) 0.021(3) 0.023(2) 0.001(2) 0.001(2) 0.013(2) N2 0.034(3) 0.047(4) 0.029(3) -0.011(3) -0.006(2) 0.028(3) C1 0.030(3) 0.037(4) 0.026(3) 0.008(3) 0.003(3) 0.021(3) C2 0.031(4) 0.056(5) 0.034(3) 0.000(3) -0.001(3) 0.029(3) C3 0.052(5) 0.059(5) 0.030(3) 0.002(3) 0.006(3) 0.044(4) C4 0.049(4) 0.043(4) 0.028(3) -0.007(3) -0.011(3) 0.028(4) C5 0.038(4) 0.026(3) 0.024(3) 0.003(2) 0.002(3) 0.018(3) C6 0.036(4) 0.044(4) 0.038(3) -0.007(3) -0.004(3) 0.029(4) C7 0.022(3) 0.042(4) 0.019(3) -0.008(3) -0.002(2) 0.012(3) C8 0.020(3) 0.032(3) 0.017(3) 0.003(2) -0.002(2) 0.014(3) C9 0.041(4) 0.086(7) 0.032(3) -0.016(4) -0.004(3) 0.049(4) C10 0.027(4) 0.038(4) 0.045(4) -0.008(3) 0.000(3) 0.017(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N2 134.6(2) . . ? N1 Ag1 S1 144.91(13) . . ? N2 Ag1 S1 77.14(14) . . ? N1 Ag1 Ag1 73.29(13) . 12_566 ? N2 Ag1 Ag1 123.71(15) . 12_566 ? S1 Ag1 Ag1 75.50(4) . 12_566 ? C7 S1 C6 101.3(3) . . ? C7 S1 Ag1 97.7(2) . . ? C6 S1 Ag1 109.7(2) . . ? O13 Cl1 O14 111.2(5) . . ? O13 Cl1 O12 109.7(5) . . ? O14 Cl1 O12 111.0(5) . . ? O13 Cl1 O11 108.5(5) . . ? O14 Cl1 O11 109.9(5) . . ? O12 Cl1 O11 106.4(5) . . ? C5 N1 C1 118.5(5) . . ? C5 N1 Ag1 121.5(4) . . ? C1 N1 Ag1 120.0(4) . . ? C9 N2 C8 117.8(6) . . ? C9 N2 Ag1 120.1(4) . . ? C8 N2 Ag1 120.7(4) . . ? N1 C1 C2 121.8(7) . . ? N1 C1 C10 117.3(5) . . ? C2 C1 C10 120.9(6) . . ? C1 C2 C3 119.3(7) . . ? C2 C3 C4 119.2(6) . . ? C5 C4 C3 118.0(7) . . ? N1 C5 C4 123.0(7) . . ? N1 C5 C6 116.4(6) . 12_566 ? C4 C5 C6 120.6(6) . 12_566 ? C5 C6 S1 114.0(5) 12_566 . ? C8 C7 S1 116.9(4) . . ? N2 C8 C8 120.5(3) . 8_677 ? N2 C8 C7 116.6(5) . . ? C8 C8 C7 122.8(3) 8_677 . ? N2 C9 C9 121.7(4) . 8_677 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.234(5) . ? Ag1 N2 2.374(5) . ? Ag1 S1 2.5882(18) . ? Ag1 Ag1 3.1158(13) 12_566 ? S1 C7 1.809(6) . ? S1 C6 1.818(8) . ? Cl1 O13 1.391(6) . ? Cl1 O14 1.414(7) . ? Cl1 O12 1.414(6) . ? Cl1 O11 1.423(7) . ? N1 C5 1.340(8) . ? N1 C1 1.351(8) . ? N2 C9 1.327(9) . ? N2 C8 1.355(8) . ? C1 C2 1.378(9) . ? C1 C10 1.508(9) . ? C2 C3 1.386(11) . ? C3 C4 1.390(11) . ? C4 C5 1.384(9) . ? C5 C6 1.505(10) 12_566 ? C6 C5 1.505(10) 12_566 ? C7 C8 1.519(8) . ? C8 C8 1.396(12) 8_677 ? C9 C9 1.377(15) 8_677 ?
1100705.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100705.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100705 _chemical_formula_sum 'C18 H18 Cu2 I2 N4 S2' _chemical_formula_weight 735.36 _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 91.4210(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 10.0330(10) _cell_length_b 8.7293(8) _cell_length_c 12.3735(11) _cell_measurement_reflns_used 2085 _cell_measurement_temperature 158(2) _cell_measurement_theta_max 26.38 _cell_measurement_theta_min 2.65 _cell_volume 1083.35(18) _diffrn_ambient_temperature 158(2) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.941 _diffrn_measured_fraction_theta_max 0.941 _diffrn_measurement_device_type 'Siemans SMART CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0218 _diffrn_reflns_av_sigmaI/netI 0.0176 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_number 7329 _diffrn_reflns_theta_full 26.38 _diffrn_reflns_theta_max 26.38 _diffrn_reflns_theta_min 2.65 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _exptl_absorpt_coefficient_mu 5.018 _exptl_absorpt_correction_T_max 0.4711 _exptl_absorpt_correction_T_min 0.3689 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Sheldrick 1996)' _exptl_crystal_colour red _exptl_crystal_density_diffrn 2.254 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description triangular _exptl_crystal_F_000 700 _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _refine_diff_density_max 0.930 _refine_diff_density_min -0.823 _refine_diff_density_rms 0.109 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 127 _refine_ls_number_reflns 2085 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.073 _refine_ls_R_factor_all 0.0313 _refine_ls_R_factor_gt 0.0290 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0346P)^2^+2.8776P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0709 _refine_ls_wR_factor_ref 0.0729 _reflns_number_gt 1950 _reflns_number_total 2085 _reflns_threshold_expression >2sigma(I) _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_sg_symbol_H-M P2(1)/n _cod_database_code 1100705 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I1 I 0.40888(3) -0.00254(3) 0.83354(2) 0.03390(11) Uani 1 1 d . . . Cu1 Cu 0.40857(5) 0.11584(6) 1.03237(4) 0.03417(14) Uani 1 1 d . . . S1 S 0.13477(10) 0.44576(13) 1.08726(9) 0.0371(2) Uani 1 1 d . . . N1 N 0.2214(3) 0.0592(4) 1.0890(3) 0.0303(7) Uani 1 1 d . . . N2 N 0.4608(3) 0.3482(4) 1.0177(2) 0.0287(7) Uani 1 1 d . . . C1 C 0.1711(4) -0.0785(5) 1.0638(3) 0.0367(9) Uani 1 1 d . . . H1 H 0.2174 -0.1385 1.0153 0.044 Uiso 1 1 calc R . . C2 C 0.0553(4) -0.1377(5) 1.1048(3) 0.0377(9) Uani 1 1 d . . . H2 H 0.0254 -0.2348 1.0851 0.045 Uiso 1 1 calc R . . C3 C -0.0148(4) -0.0486(6) 1.1758(4) 0.0397(10) Uani 1 1 d . . . H3 H -0.0931 -0.0845 1.2055 0.048 Uiso 1 1 calc R . . C4 C 0.0333(4) 0.0941(5) 1.2017(3) 0.0359(9) Uani 1 1 d . . . H4 H -0.0129 0.1564 1.2488 0.043 Uiso 1 1 calc R . . C5 C 0.1522(4) 0.1461(5) 1.1573(3) 0.0298(8) Uani 1 1 d . . . C6 C 0.2028(4) 0.3040(5) 1.1815(3) 0.0342(8) Uani 1 1 d . . . H6A H 0.2993 0.3044 1.1780 0.041 Uiso 1 1 calc R . . H6B H 0.1792 0.3320 1.2544 0.041 Uiso 1 1 calc R . . C7 C 0.2301(4) 0.4071(5) 0.9654(3) 0.0335(8) Uani 1 1 d . . . H7A H 0.2256 0.2986 0.9487 0.040 Uiso 1 1 calc R . . H7B H 0.1909 0.4629 0.9048 0.040 Uiso 1 1 calc R . . C8 C 0.3727(4) 0.4536(5) 0.9811(3) 0.0292(8) Uani 1 1 d . . . C9 C 0.5862(4) 0.3962(4) 1.0365(3) 0.0311(8) Uani 1 1 d . . . H9 H 0.6487 0.3258 1.0626 0.037 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.03232(17) 0.03871(18) 0.03077(16) 0.00327(10) 0.00320(11) -0.00041(10) Cu1 0.0288(3) 0.0311(3) 0.0429(3) 0.0009(2) 0.0057(2) -0.0004(2) S1 0.0303(5) 0.0317(5) 0.0496(6) -0.0001(5) 0.0063(4) 0.0025(4) N1 0.0271(16) 0.0290(17) 0.0348(16) -0.0017(14) 0.0033(13) 0.0017(14) N2 0.0280(16) 0.0261(16) 0.0321(16) -0.0018(13) 0.0044(12) -0.0010(13) C1 0.034(2) 0.034(2) 0.042(2) -0.0013(18) 0.0054(17) 0.0027(18) C2 0.035(2) 0.031(2) 0.047(2) 0.0022(18) -0.0033(17) -0.0036(17) C3 0.029(2) 0.045(2) 0.045(2) 0.010(2) 0.0017(17) -0.0062(19) C4 0.030(2) 0.043(2) 0.035(2) -0.0011(18) 0.0074(16) 0.0011(18) C5 0.0279(19) 0.033(2) 0.0281(17) 0.0034(16) -0.0005(14) -0.0005(16) C6 0.032(2) 0.038(2) 0.0318(19) -0.0054(17) 0.0025(15) -0.0014(17) C7 0.029(2) 0.035(2) 0.036(2) 0.0045(17) -0.0009(15) -0.0025(17) C8 0.0279(19) 0.030(2) 0.0293(18) -0.0026(16) 0.0027(14) -0.0004(16) C9 0.0306(19) 0.0272(19) 0.0356(19) 0.0022(16) 0.0023(15) 0.0041(16) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cu1 I1 Cu1 65.244(19) 3_657 . ? N1 Cu1 N2 119.17(13) . . ? N1 Cu1 I1 108.55(9) . 3_657 ? N2 Cu1 I1 104.22(9) . 3_657 ? N1 Cu1 I1 103.89(9) . . ? N2 Cu1 I1 106.71(9) . . ? I1 Cu1 I1 114.756(19) 3_657 . ? N1 Cu1 Cu1 121.14(10) . 3_657 ? N2 Cu1 Cu1 119.66(9) . 3_657 ? I1 Cu1 Cu1 57.973(19) 3_657 3_657 ? I1 Cu1 Cu1 56.783(18) . 3_657 ? C6 S1 C7 101.88(19) . . ? C1 N1 C5 117.2(3) . . ? C1 N1 Cu1 118.3(3) . . ? C5 N1 Cu1 124.3(3) . . ? C9 N2 C8 116.7(3) . . ? C9 N2 Cu1 121.4(3) . . ? C8 N2 Cu1 121.7(3) . . ? N1 C1 C2 124.6(4) . . ? C3 C2 C1 118.1(4) . . ? C4 C3 C2 118.6(4) . . ? C3 C4 C5 120.1(4) . . ? N1 C5 C4 121.5(4) . . ? N1 C5 C6 117.9(3) . . ? C4 C5 C6 120.6(4) . . ? C5 C6 S1 112.2(3) . . ? C8 C7 S1 111.1(3) . . ? N2 C8 C9 120.1(3) . 3_667 ? N2 C8 C7 118.4(4) . . ? C9 C8 C7 121.4(4) 3_667 . ? N2 C9 C8 123.1(4) . 3_667 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag I1 Cu1 2.6334(6) 3_657 ? I1 Cu1 2.6686(6) . ? Cu1 N1 2.080(3) . ? Cu1 N2 2.104(3) . ? Cu1 I1 2.6334(6) 3_657 ? Cu1 Cu1 2.8584(10) 3_657 ? S1 C6 1.821(4) . ? S1 C7 1.837(4) . ? N1 C1 1.337(6) . ? N1 C5 1.343(5) . ? N2 C9 1.341(5) . ? N2 C8 1.347(5) . ? C1 C2 1.380(6) . ? C2 C3 1.379(7) . ? C3 C4 1.371(7) . ? C4 C5 1.400(5) . ? C5 C6 1.497(6) . ? C7 C8 1.495(5) . ? C8 C9 1.393(6) 3_667 ? C9 C8 1.393(6) 3_667 ?
1100706.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100706.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100706 loop_ _publ_author_name 'Ling-I Hung' 'Sue-Lein Wang' 'Chia-Yi Chen' 'Bor-Chen Chang' 'Kwang-Hwa Lii' _publ_section_title ; Rb3In(H2O)Si5O13: A Novel Indium Silicate with a CdSO4-Topological-Type Structure ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 2992 _journal_page_last 2994 _journal_paper_doi 10.1021/ic048296n _journal_volume 44 _journal_year 2005 _chemical_formula_moiety Rb3In(H2O)Si5O13 _chemical_formula_sum 'H2 In O14 Rb3 Si5' _chemical_formula_weight 737.70 _chemical_name_systematic ; ? ; _space_group_IT_number 9 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall 'C -2yc' _symmetry_space_group_name_H-M 'C 1 c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 102.3000(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 9.0697(5) _cell_length_b 11.5456(6) _cell_length_c 13.9266(8) _cell_measurement_temperature 298(2) _cell_volume 1424.85(14) _computing_molecular_graphics Diamond _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 298(2) _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Bruker APEX CCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_sigmaI/netI 0.0248 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 4937 _diffrn_reflns_theta_full 28.31 _diffrn_reflns_theta_max 28.31 _diffrn_reflns_theta_min 2.90 _exptl_absorpt_coefficient_mu 12.334 _exptl_absorpt_correction_T_max 0.966 _exptl_absorpt_correction_T_min 0.514 _exptl_absorpt_correction_type 'empirical based on symmetry equivalents' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 3.439 _exptl_crystal_density_method 'not measured' _exptl_crystal_description tablet _exptl_crystal_F_000 1376 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.851 _refine_diff_density_min -0.887 _refine_diff_density_rms 0.147 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00 _refine_ls_extinction_coef 0.00277(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 209 _refine_ls_number_reflns 2551 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 1.044 _refine_ls_R_factor_all 0.0211 _refine_ls_R_factor_gt 0.0209 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0391P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0521 _refine_ls_wR_factor_ref 0.0522 _reflns_number_gt 2524 _reflns_number_total 2551 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic048296nsi20050225_115014.cif _cod_data_source_block rbin2m _cod_database_code 1100706 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rb1 Rb 0.92365(6) -0.22627(4) 0.05771(4) 0.02439(12) Uani 1 1 d . . . Rb2 Rb 0.95896(6) -0.22257(4) 0.53158(4) 0.02380(12) Uani 1 1 d . . . Rb3 Rb 0.89786(6) 0.00220(4) 0.29430(4) 0.02414(12) Uani 1 1 d . . . In1 In 0.64939(4) 0.25154(2) 0.32074(3) 0.00969(8) Uani 1 1 d . . . Si1 Si 1.26463(13) 0.17414(9) 0.27674(8) 0.0093(2) Uani 1 1 d . . . Si2 Si 0.50425(13) -0.17531(9) 0.29957(9) 0.0108(2) Uani 1 1 d . . . Si3 Si 0.61613(14) -0.00296(9) 0.46604(9) 0.0106(2) Uani 1 1 d . . . Si4 Si 1.24883(13) -0.04806(9) 0.16567(8) 0.0097(2) Uani 1 1 d . . . Si5 Si 1.26707(13) 0.00153(9) 0.45685(9) 0.0097(2) Uani 1 1 d . . . O1 O 1.2579(4) 0.0927(2) 0.1796(2) 0.0141(6) Uani 1 1 d . . . O2 O 1.1098(4) 0.2481(2) 0.2434(3) 0.0147(6) Uani 1 1 d . . . O3 O 1.4090(4) 0.2549(2) 0.3021(3) 0.0147(8) Uani 1 1 d . . . O4 O 1.2402(4) 0.0943(3) 0.3677(2) 0.0191(7) Uani 1 1 d . . . O5 O 0.3916(5) -0.2515(2) 0.3457(3) 0.0165(8) Uani 1 1 d . . . O6 O 0.6223(4) -0.0979(3) 0.3795(3) 0.0199(7) Uani 1 1 d . . . O7 O 0.4200(4) -0.0911(3) 0.2118(3) 0.0217(7) Uani 1 1 d . . . O8 O 0.7374(4) -0.0453(3) 0.5637(3) 0.0211(7) Uani 1 1 d . . . O9 O 0.6563(4) 0.1232(3) 0.4355(3) 0.0170(7) Uani 1 1 d . . . O10 O 0.4485(4) -0.0170(3) 0.4917(3) 0.0174(6) Uani 1 1 d . . . O11 O 1.1263(4) -0.1109(3) 0.2125(2) 0.0132(6) Uani 1 1 d . . . O12 O 1.2152(4) -0.0705(3) 0.0470(2) 0.0150(6) Uani 1 1 d . . . O13 O 1.1718(4) -0.1147(3) 0.4317(2) 0.0140(7) Uani 1 1 d . . . O14 O 0.6318(4) 0.1264(3) 0.2062(3) 0.0179(7) Uani 1 1 d . . . H2 H 0.6184 0.1209 0.1433 0.050 Uiso 1 1 d . . . H1 H 0.5832 0.0729 0.2174 0.050 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rb1 0.0249(3) 0.0243(2) 0.0203(3) -0.00178(19) -0.00366(18) -0.00198(19) Rb2 0.0266(3) 0.0250(2) 0.0223(2) -0.00036(18) 0.0107(2) 0.0006(2) Rb3 0.0207(2) 0.0167(2) 0.0348(3) 0.00114(19) 0.0056(2) 0.00499(14) In1 0.00966(14) 0.00969(11) 0.01014(14) 0.00011(9) 0.00307(9) -0.00036(9) Si1 0.0098(5) 0.0084(5) 0.0107(5) 0.0003(4) 0.0041(4) 0.0006(4) Si2 0.0097(5) 0.0105(4) 0.0128(5) 0.0003(4) 0.0039(4) 0.0016(4) Si3 0.0112(6) 0.0097(5) 0.0113(5) -0.0002(4) 0.0033(4) -0.0007(4) Si4 0.0114(5) 0.0090(5) 0.0097(5) 0.0007(4) 0.0043(4) 0.0009(4) Si5 0.0108(6) 0.0095(5) 0.0095(5) -0.0003(3) 0.0036(4) -0.0004(4) O1 0.0181(15) 0.0116(13) 0.0136(15) -0.0010(11) 0.0054(12) -0.0008(12) O2 0.0135(17) 0.0171(14) 0.0134(16) -0.0019(11) 0.0025(13) 0.0053(11) O3 0.0105(19) 0.0137(18) 0.021(2) -0.0025(12) 0.0058(15) -0.0024(10) O4 0.0237(18) 0.0202(15) 0.0146(16) 0.0040(12) 0.0065(13) -0.0022(13) O5 0.0124(19) 0.0157(19) 0.0214(19) 0.0029(11) 0.0037(14) 0.0006(11) O6 0.0189(17) 0.0202(15) 0.0224(16) -0.0096(13) 0.0087(14) -0.0046(13) O7 0.0124(16) 0.0265(16) 0.0266(18) 0.0124(14) 0.0050(13) 0.0055(13) O8 0.0159(17) 0.0303(18) 0.0171(16) 0.0060(14) 0.0037(13) 0.0038(14) O9 0.0210(18) 0.0134(15) 0.0167(16) 0.0059(13) 0.0041(14) -0.0033(13) O10 0.0100(15) 0.0240(15) 0.0192(16) 0.0002(12) 0.0054(12) 0.0009(12) O11 0.0109(15) 0.0139(14) 0.0155(15) 0.0012(12) 0.0041(12) 0.0003(12) O12 0.0230(16) 0.0132(14) 0.0100(15) -0.0009(10) 0.0066(12) -0.0027(12) O13 0.0181(18) 0.0120(15) 0.0132(15) -0.0021(12) 0.0064(13) -0.0020(13) O14 0.0206(18) 0.0173(16) 0.0166(16) -0.0029(13) 0.0055(14) -0.0024(14) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O11 Rb1 O9 125.13(8) . 2_554 ? O11 Rb1 O5 135.77(10) . 4_544 ? O9 Rb1 O5 63.38(10) 2_554 4_544 ? O11 Rb1 O14 62.33(12) . 3_545 ? O9 Rb1 O14 163.11(11) 2_554 3_545 ? O5 Rb1 O14 123.93(9) 4_544 3_545 ? O11 Rb1 O10 126.21(10) . 4_544 ? O9 Rb1 O10 108.66(10) 2_554 4_544 ? O5 Rb1 O10 67.45(9) 4_544 4_544 ? O14 Rb1 O10 65.93(10) 3_545 4_544 ? O11 Rb1 O13 165.22(10) . 4_444 ? O9 Rb1 O13 59.85(11) 2_554 4_444 ? O5 Rb1 O13 58.77(9) 4_544 4_444 ? O14 Rb1 O13 109.06(8) 3_545 4_444 ? O10 Rb1 O13 51.23(9) 4_544 4_444 ? O11 Rb1 O12 51.03(8) . . ? O9 Rb1 O12 109.54(10) 2_554 . ? O5 Rb1 O12 84.74(9) 4_544 . ? O14 Rb1 O12 86.93(9) 3_545 . ? O10 Rb1 O12 113.81(9) 4_544 . ? O13 Rb1 O12 143.29(8) 4_444 . ? O11 Rb1 O1 101.60(8) . 3_445 ? O9 Rb1 O1 98.52(9) 2_554 3_445 ? O5 Rb1 O1 120.92(9) 4_544 3_445 ? O14 Rb1 O1 64.59(9) 3_545 3_445 ? O10 Rb1 O1 67.34(8) 4_544 3_445 ? O13 Rb1 O1 63.66(8) 4_444 3_445 ? O12 Rb1 O1 148.84(8) . 3_445 ? O11 Rb1 O3 55.65(9) . 3_445 ? O9 Rb1 O3 113.72(9) 2_554 3_445 ? O5 Rb1 O3 168.35(10) 4_544 3_445 ? O14 Rb1 O3 55.66(9) 3_545 3_445 ? O10 Rb1 O3 104.55(8) 4_544 3_445 ? O13 Rb1 O3 109.70(8) 4_444 3_445 ? O12 Rb1 O3 106.59(8) . 3_445 ? O1 Rb1 O3 47.48(8) 3_445 3_445 ? O11 Rb1 O8 78.68(9) . 2_554 ? O9 Rb1 O8 46.67(9) 2_554 2_554 ? O5 Rb1 O8 98.94(9) 4_544 2_554 ? O14 Rb1 O8 135.26(9) 3_545 2_554 ? O10 Rb1 O8 154.65(9) 4_544 2_554 ? O13 Rb1 O8 103.54(8) 4_444 2_554 ? O12 Rb1 O8 84.72(8) . 2_554 ? O1 Rb1 O8 106.16(8) 3_445 2_554 ? O3 Rb1 O8 85.08(8) 3_445 2_554 ? O11 Rb1 Si5 146.78(7) . 4_444 ? O9 Rb1 Si5 85.60(7) 2_554 4_444 ? O5 Rb1 Si5 65.52(6) 4_544 4_444 ? O14 Rb1 Si5 84.70(7) 3_545 4_444 ? O10 Rb1 Si5 26.48(7) 4_544 4_444 ? O13 Rb1 Si5 25.90(6) 4_444 4_444 ? O12 Rb1 Si5 136.48(6) . 4_444 ? O1 Rb1 Si5 56.97(5) 3_445 4_444 ? O3 Rb1 Si5 103.44(5) 3_445 4_444 ? O8 Rb1 Si5 128.93(6) 2_554 4_444 ? O11 Rb1 Si4 24.40(7) . . ? O9 Rb1 Si4 120.74(8) 2_554 . ? O5 Rb1 Si4 111.38(7) 4_544 . ? O14 Rb1 Si4 72.67(7) 3_545 . ? O10 Rb1 Si4 123.60(7) 4_544 . ? O13 Rb1 Si4 169.52(6) 4_444 . ? O12 Rb1 Si4 26.63(5) . . ? O1 Rb1 Si4 124.75(6) 3_445 . ? O3 Rb1 Si4 80.00(6) 3_445 . ? O8 Rb1 Si4 80.79(6) 2_554 . ? Si5 Rb1 Si4 150.07(3) 4_444 . ? O13 Rb2 O8 108.56(9) . . ? O13 Rb2 O2 107.75(10) . 2 ? O8 Rb2 O2 95.82(9) . 2 ? O13 Rb2 O9 61.52(11) . 3_545 ? O8 Rb2 O9 162.59(9) . 3_545 ? O2 Rb2 O9 100.87(10) 2 3_545 ? O13 Rb2 O3 60.84(9) . 3_445 ? O8 Rb2 O3 104.77(9) . 3_445 ? O2 Rb2 O3 158.74(10) 2 3_445 ? O9 Rb2 O3 58.20(10) 3_545 3_445 ? O13 Rb2 O12 150.52(8) . 4_445 ? O8 Rb2 O12 90.27(9) . 4_445 ? O2 Rb2 O12 92.10(8) 2 4_445 ? O9 Rb2 O12 94.04(8) 3_545 4_445 ? O3 Rb2 O12 93.03(8) 3_445 4_445 ? O13 Rb2 O7 144.83(9) . 4_545 ? O8 Rb2 O7 98.38(8) . 4_545 ? O2 Rb2 O7 45.83(8) 2 4_545 ? O9 Rb2 O7 96.82(8) 3_545 4_545 ? O3 Rb2 O7 133.40(8) 3_445 4_545 ? O12 Rb2 O7 46.53(8) 4_445 4_545 ? O13 Rb2 O1 64.65(8) . 2 ? O8 Rb2 O1 94.76(9) . 2 ? O2 Rb2 O1 45.92(8) 2 2 ? O9 Rb2 O1 93.28(9) 3_545 2 ? O3 Rb2 O1 125.40(8) 3_445 2 ? O12 Rb2 O1 137.99(7) 4_445 2 ? O7 Rb2 O1 91.53(8) 4_545 2 ? O13 Rb2 O4 107.30(8) . 3_445 ? O8 Rb2 O4 102.24(10) . 3_445 ? O2 Rb2 O4 132.55(8) 2 3_445 ? O9 Rb2 O4 69.82(9) 3_545 3_445 ? O3 Rb2 O4 48.09(8) 3_445 3_445 ? O12 Rb2 O4 44.99(7) 4_445 3_445 ? O7 Rb2 O4 87.96(8) 4_545 3_445 ? O1 Rb2 O4 162.89(8) 2 3_445 ? O13 Rb2 O10 110.25(9) . 3_545 ? O8 Rb2 O10 135.15(9) . 3_545 ? O2 Rb2 O10 93.03(8) 2 3_545 ? O9 Rb2 O10 49.23(8) 3_545 3_545 ? O3 Rb2 O10 76.17(8) 3_445 3_545 ? O12 Rb2 O10 45.45(8) 4_445 3_545 ? O7 Rb2 O10 59.18(8) 4_545 3_545 ? O1 Rb2 O10 121.75(8) 2 3_545 ? O4 Rb2 O10 44.72(8) 3_445 3_545 ? O13 Rb2 O6 96.53(9) . . ? O8 Rb2 O6 45.63(9) . . ? O2 Rb2 O6 140.11(9) 2 . ? O9 Rb2 O6 118.62(8) 3_545 . ? O3 Rb2 O6 61.14(9) 3_445 . ? O12 Rb2 O6 80.36(8) 4_445 . ? O7 Rb2 O6 118.58(8) 4_545 . ? O1 Rb2 O6 130.22(7) 2 . ? O4 Rb2 O6 63.81(8) 3_445 . ? O10 Rb2 O6 107.90(8) 3_545 . ? O13 Rb2 Si5 124.20(7) . 3_445 ? O8 Rb2 Si5 110.22(8) . 3_445 ? O2 Rb2 Si5 106.49(6) 2 3_445 ? O9 Rb2 Si5 69.75(7) 3_545 3_445 ? O3 Rb2 Si5 71.50(6) 3_445 3_445 ? O12 Rb2 Si5 26.50(5) 4_445 3_445 ? O7 Rb2 Si5 62.63(6) 4_545 3_445 ? O1 Rb2 Si5 145.71(5) 2 3_445 ? O4 Rb2 Si5 26.06(6) 3_445 3_445 ? O10 Rb2 Si5 26.20(6) 3_545 3_445 ? O6 Rb2 Si5 83.66(6) . 3_445 ? O14 Rb3 O3 122.59(11) . 3_445 ? O14 Rb3 O11 132.21(11) . . ? O3 Rb3 O11 62.62(10) 3_445 . ? O14 Rb3 O5 63.85(12) . 3 ? O3 Rb3 O5 163.86(13) 3_445 3 ? O11 Rb3 O5 126.03(10) . 3 ? O14 Rb3 O13 167.82(10) . . ? O3 Rb3 O13 61.64(11) 3_445 . ? O11 Rb3 O13 59.87(8) . . ? O5 Rb3 O13 108.98(10) 3 . ? O14 Rb3 O6 71.64(10) . . ? O3 Rb3 O6 69.47(10) 3_445 . ? O11 Rb3 O6 131.83(9) . . ? O5 Rb3 O6 101.65(9) 3 . ? O13 Rb3 O6 101.54(9) . . ? O14 Rb3 O4 129.68(10) . . ? O3 Rb3 O4 107.01(10) 3_445 . ? O11 Rb3 O4 63.33(9) . . ? O5 Rb3 O4 70.83(10) 3 . ? O13 Rb3 O4 50.17(8) . . ? O6 Rb3 O4 140.70(9) . . ? O14 Rb3 O8 48.82(9) . 2_554 ? O3 Rb3 O8 101.21(11) 3_445 2_554 ? O11 Rb3 O8 83.55(9) . 2_554 ? O5 Rb3 O8 93.69(11) 3 2_554 ? O13 Rb3 O8 143.35(9) . 2_554 ? O6 Rb3 O8 101.53(9) . 2_554 ? O4 Rb3 O8 117.18(8) . 2_554 ? O14 Rb3 O9 58.10(8) . . ? O3 Rb3 O9 113.27(10) 3_445 . ? O11 Rb3 O9 169.68(10) . . ? O5 Rb3 O9 55.55(9) 3 . ? O13 Rb3 O9 109.82(9) . . ? O6 Rb3 O9 46.37(8) . . ? O4 Rb3 O9 111.22(9) . . ? O8 Rb3 O9 106.73(8) 2_554 . ? O14 Rb3 O2 87.54(9) . . ? O3 Rb3 O2 141.53(9) 3_445 . ? O11 Rb3 O2 79.59(9) . . ? O5 Rb3 O2 47.15(9) 3 . ? O13 Rb3 O2 94.22(9) . . ? O6 Rb3 O2 148.57(8) . . ? O4 Rb3 O2 44.17(8) . . ? O8 Rb3 O2 80.23(8) 2_554 . ? O9 Rb3 O2 102.69(8) . . ? O14 Rb3 Si5 148.85(8) . . ? O3 Rb3 Si5 87.34(9) 3_445 . ? O11 Rb3 Si5 66.36(7) . . ? O5 Rb3 Si5 85.00(9) 3 . ? O13 Rb3 Si5 25.99(6) . . ? O6 Rb3 Si5 117.28(7) . . ? O4 Rb3 Si5 26.55(6) . . ? O8 Rb3 Si5 140.66(6) 2_554 . ? O9 Rb3 Si5 104.70(6) . . ? O2 Rb3 Si5 70.22(6) . . ? O14 Rb3 In1 153.48(8) . 3_545 ? O3 Rb3 In1 35.81(8) 3_445 3_545 ? O11 Rb3 In1 36.39(7) . 3_545 ? O5 Rb3 In1 141.85(9) 3 3_545 ? O13 Rb3 In1 36.19(6) . 3_545 ? O6 Rb3 In1 101.34(6) . 3_545 ? O4 Rb3 In1 72.05(6) . 3_545 ? O8 Rb3 In1 110.93(6) 2_554 3_545 ? O9 Rb3 In1 134.87(6) . 3_545 ? O2 Rb3 In1 107.31(5) . 3_545 ? Si5 Rb3 In1 57.38(2) . 3_545 ? O14 Rb3 H2 14.6 . . ? O3 Rb3 H2 117.7 3_445 . ? O11 Rb3 H2 117.7 . . ? O5 Rb3 H2 72.2 3 . ? O13 Rb3 H2 177.6 . . ? O6 Rb3 H2 80.1 . . ? O4 Rb3 H2 129.3 . . ? O8 Rb3 H2 34.2 2_554 . ? O9 Rb3 H2 72.6 . . ? O2 Rb3 H2 85.1 . . ? Si5 Rb3 H2 154.2 . . ? In1 Rb3 H2 141.9 3_545 . ? O14 Rb3 H1 15.6 . . ? O3 Rb3 H1 108.3 3_445 . ? O11 Rb3 H1 134.9 . . ? O5 Rb3 H1 75.7 3 . ? O13 Rb3 H1 158.8 . . ? O6 Rb3 H1 57.4 . . ? O4 Rb3 H1 144.6 . . ? O8 Rb3 H1 53.6 2_554 . ? O9 Rb3 H1 54.8 . . ? O2 Rb3 H1 103.2 . . ? Si5 Rb3 H1 157.6 . . ? In1 Rb3 H1 142.4 3_545 . ? H2 Rb3 H1 23.1 . . ? O14 In1 O3 90.55(14) . 1_455 ? O14 In1 O5 91.22(14) . 3 ? O3 In1 O5 177.69(18) 1_455 3 ? O14 In1 O13 176.81(14) . 3_455 ? O3 In1 O13 90.68(13) 1_455 3_455 ? O5 In1 O13 87.63(13) 3 3_455 ? O14 In1 O11 89.74(15) . 3_455 ? O3 In1 O11 87.58(13) 1_455 3_455 ? O5 In1 O11 93.91(13) 3 3_455 ? O13 In1 O11 87.37(10) 3_455 3_455 ? O14 In1 O9 94.24(11) . . ? O3 In1 O9 88.30(14) 1_455 . ? O5 In1 O9 90.08(13) 3 . ? O13 In1 O9 88.74(15) 3_455 . ? O11 In1 O9 174.30(14) 3_455 . ? O14 In1 Rb3 121.01(10) . 3_455 ? O3 In1 Rb3 51.37(8) 1_455 3_455 ? O5 In1 Rb3 128.57(8) 3 3_455 ? O13 In1 Rb3 57.88(9) 3_455 3_455 ? O11 In1 Rb3 52.00(9) 3_455 3_455 ? O9 In1 Rb3 122.31(10) . 3_455 ? O14 In1 Rb1 122.91(10) . 2 ? O3 In1 Rb1 125.71(11) 1_455 2 ? O5 In1 Rb1 52.00(11) 3 2 ? O13 In1 Rb1 58.38(9) 3_455 2 ? O11 In1 Rb1 128.69(9) 3_455 2 ? O9 In1 Rb1 51.72(10) . 2 ? Rb3 In1 Rb1 116.059(15) 3_455 2 ? O14 In1 Rb3 49.66(10) . . ? O3 In1 Rb3 128.64(8) 1_455 . ? O5 In1 Rb3 51.99(8) 3 . ? O13 In1 Rb3 131.00(9) 3_455 . ? O11 In1 Rb3 117.93(9) 3_455 . ? O9 In1 Rb3 67.76(10) . . ? Rb3 In1 Rb3 168.67(2) 3_455 . ? Rb1 In1 Rb3 73.791(14) 2 . ? O14 In1 Rb2 132.15(9) . 3_455 ? O3 In1 Rb2 57.46(11) 1_455 3_455 ? O5 In1 Rb2 120.23(11) 3 3_455 ? O13 In1 Rb2 50.80(8) 3_455 3_455 ? O11 In1 Rb2 119.81(9) 3_455 3_455 ? O9 In1 Rb2 54.53(10) . 3_455 ? Rb3 In1 Rb2 68.366(13) 3_455 3_455 ? Rb1 In1 Rb2 68.848(14) 2 3_455 ? Rb3 In1 Rb2 122.182(15) . 3_455 ? O14 In1 Rb1 52.14(10) . 3_455 ? O3 In1 Rb1 63.71(11) 1_455 3_455 ? O5 In1 Rb1 118.59(11) 3 3_455 ? O13 In1 Rb1 126.08(9) 3_455 3_455 ? O11 In1 Rb1 47.87(9) 3_455 3_455 ? O9 In1 Rb1 132.84(10) . 3_455 ? Rb3 In1 Rb1 69.721(14) 3_455 3_455 ? Rb1 In1 Rb1 170.536(19) 2 3_455 ? Rb3 In1 Rb1 99.774(14) . 3_455 ? Rb2 In1 Rb1 120.601(15) 3_455 3_455 ? O3 Si1 O4 113.8(2) . . ? O3 Si1 O2 112.18(17) . . ? O4 Si1 O2 105.60(19) . . ? O3 Si1 O1 113.93(19) . . ? O4 Si1 O1 109.42(17) . . ? O2 Si1 O1 100.82(18) . . ? O3 Si1 Rb2 53.87(15) . 3 ? O4 Si1 Rb2 64.01(13) . 3 ? O2 Si1 Rb2 107.61(13) . 3 ? O1 Si1 Rb2 151.56(13) . 3 ? O3 Si1 Rb1 64.31(15) . 3 ? O4 Si1 Rb1 159.07(13) . 3 ? O2 Si1 Rb1 93.67(13) . 3 ? O1 Si1 Rb1 57.77(11) . 3 ? Rb2 Si1 Rb1 118.18(3) 3 3 ? O3 Si1 Rb3 162.61(15) . . ? O4 Si1 Rb3 53.47(13) . . ? O2 Si1 Rb3 65.87(12) . . ? O1 Si1 Rb3 83.02(12) . . ? Rb2 Si1 Rb3 109.32(3) 3 . ? Rb1 Si1 Rb3 132.16(3) 3 . ? O3 Si1 Rb2 120.25(15) . 2_554 ? O4 Si1 Rb2 124.66(14) . 2_554 ? O2 Si1 Rb2 43.47(12) . 2_554 ? O1 Si1 Rb2 58.11(12) . 2_554 ? Rb2 Si1 Rb2 149.56(3) 3 2_554 ? Rb1 Si1 Rb2 65.30(2) 3 2_554 ? Rb3 Si1 Rb2 71.19(2) . 2_554 ? O3 Si1 Rb3 36.71(12) . 3 ? O4 Si1 Rb3 125.85(13) . 3 ? O2 Si1 Rb3 75.48(12) . 3 ? O1 Si1 Rb3 123.77(11) . 3 ? Rb2 Si1 Rb3 64.44(2) 3 3 ? Rb1 Si1 Rb3 66.41(2) 3 3 ? Rb3 Si1 Rb3 136.87(3) . 3 ? Rb2 Si1 Rb3 93.82(3) 2_554 3 ? O5 Si2 O7 113.5(2) . . ? O5 Si2 O2 113.01(16) . 3_445 ? O7 Si2 O2 101.27(19) . 3_445 ? O5 Si2 O6 114.3(2) . . ? O7 Si2 O6 108.69(19) . . ? O2 Si2 O6 104.97(19) 3_445 . ? O5 Si2 Rb3 44.68(12) . 3_445 ? O7 Si2 Rb3 119.40(14) . 3_445 ? O2 Si2 Rb3 68.53(12) 3_445 3_445 ? O6 Si2 Rb3 131.88(13) . 3_445 ? O5 Si2 Rb2 106.16(16) . 4_444 ? O7 Si2 Rb2 61.11(14) . 4_444 ? O2 Si2 Rb2 46.99(13) 3_445 4_444 ? O6 Si2 Rb2 138.24(13) . 4_444 ? Rb3 Si2 Rb2 73.17(2) 3_445 4_444 ? O5 Si2 Rb1 38.50(16) . 4_445 ? O7 Si2 Rb1 134.78(13) . 4_445 ? O2 Si2 Rb1 121.35(13) 3_445 4_445 ? O6 Si2 Rb1 76.17(12) . 4_445 ? Rb3 Si2 Rb1 69.35(2) 3_445 4_445 ? Rb2 Si2 Rb1 141.72(3) 4_444 4_445 ? O5 Si2 Rb3 156.50(17) . . ? O7 Si2 Rb3 87.66(13) . . ? O2 Si2 Rb3 70.17(12) 3_445 . ? O6 Si2 Rb3 45.44(12) . . ? Rb3 Si2 Rb3 134.01(3) 3_445 . ? Rb2 Si2 Rb3 92.80(3) 4_444 . ? Rb1 Si2 Rb3 118.88(3) 4_445 . ? O9 Si3 O8 110.3(2) . . ? O9 Si3 O6 111.85(18) . . ? O8 Si3 O6 106.85(19) . . ? O9 Si3 O10 115.26(19) . . ? O8 Si3 O10 106.25(19) . . ? O6 Si3 O10 105.80(18) . . ? O9 Si3 Rb2 52.29(13) . 3_455 ? O8 Si3 Rb2 106.34(14) . 3_455 ? O6 Si3 Rb2 146.68(14) . 3_455 ? O10 Si3 Rb2 67.20(12) . 3_455 ? O9 Si3 Rb3 66.26(14) . . ? O8 Si3 Rb3 95.94(13) . . ? O6 Si3 Rb3 54.77(12) . . ? O10 Si3 Rb3 154.62(14) . . ? Rb2 Si3 Rb3 118.49(3) 3_455 . ? O9 Si3 Rb1 42.76(14) . 2 ? O8 Si3 Rb1 67.57(13) . 2 ? O6 Si3 Rb1 124.51(13) . 2 ? O10 Si3 Rb1 129.26(13) . 2 ? Rb2 Si3 Rb1 67.08(2) 3_455 2 ? Rb3 Si3 Rb1 70.54(2) . 2 ? O9 Si3 Rb1 164.83(15) . 4_445 ? O8 Si3 Rb1 75.97(13) . 4_445 ? O6 Si3 Rb1 78.09(12) . 4_445 ? O10 Si3 Rb1 49.75(12) . 4_445 ? Rb2 Si3 Rb1 113.10(3) 3_455 4_445 ? Rb3 Si3 Rb1 127.87(3) . 4_445 ? Rb1 Si3 Rb1 141.16(4) 2 4_445 ? O9 Si3 Rb2 115.87(15) . . ? O8 Si3 Rb2 42.26(13) . . ? O6 Si3 Rb2 66.02(13) . . ? O10 Si3 Rb2 127.13(13) . . ? Rb2 Si3 Rb2 145.17(4) 3_455 . ? Rb3 Si3 Rb2 64.01(2) . . ? Rb1 Si3 Rb2 83.47(3) 2 . ? Rb1 Si3 Rb2 78.29(2) 4_445 . ? O11 Si4 O7 113.15(18) . 1_655 ? O11 Si4 O12 110.36(18) . . ? O7 Si4 O12 107.90(19) 1_655 . ? O11 Si4 O1 115.42(17) . . ? O7 Si4 O1 103.70(18) 1_655 . ? O12 Si4 O1 105.71(16) . . ? O11 Si4 Rb1 48.16(13) . . ? O7 Si4 Rb1 127.63(14) 1_655 . ? O12 Si4 Rb1 62.21(12) . . ? O1 Si4 Rb1 128.67(13) . . ? O11 Si4 Rb2 109.85(13) . 4_544 ? O7 Si4 Rb2 57.76(14) 1_655 4_544 ? O12 Si4 Rb2 54.69(12) . 4_544 ? O1 Si4 Rb2 134.70(11) . 4_544 ? Rb1 Si4 Rb2 81.74(2) . 4_544 ? O11 Si4 Rb3 35.66(13) . . ? O7 Si4 Rb3 130.48(13) 1_655 . ? O12 Si4 Rb3 118.61(13) . . ? O1 Si4 Rb3 80.12(11) . . ? Rb1 Si4 Rb3 67.48(2) . . ? Rb2 Si4 Rb3 144.60(3) 4_544 . ? O13 Si5 O4 113.75(19) . . ? O13 Si5 O10 114.91(18) . 1_655 ? O4 Si5 O10 107.04(18) . 1_655 ? O13 Si5 O12 110.29(18) . 2 ? O4 Si5 O12 104.21(17) . 2 ? O10 Si5 O12 105.80(18) 1_655 2 ? O13 Si5 Rb3 58.57(13) . . ? O4 Si5 Rb3 63.32(13) . . ? O10 Si5 Rb3 158.20(13) 1_655 . ? O12 Si5 Rb3 95.73(13) 2 . ? O13 Si5 Rb1 59.89(13) . 4_545 ? O4 Si5 Rb1 148.96(13) . 4_545 ? O10 Si5 Rb1 58.90(12) 1_655 4_545 ? O12 Si5 Rb1 106.31(12) 2 4_545 ? Rb3 Si5 Rb1 118.44(3) . 4_545 ? O13 Si5 Rb2 173.92(13) . 3 ? O4 Si5 Rb2 68.16(13) . 3 ? O10 Si5 Rb2 68.99(12) 1_655 3 ? O12 Si5 Rb2 63.72(12) 2 3 ? Rb3 Si5 Rb2 119.65(3) . 3 ? Rb1 Si5 Rb2 121.72(4) 4_545 3 ? O13 Si5 Rb2 32.65(12) . . ? O4 Si5 Rb2 127.80(14) . . ? O10 Si5 Rb2 122.79(12) 1_655 . ? O12 Si5 Rb2 77.86(12) 2 . ? Rb3 Si5 Rb2 64.57(2) . . ? Rb1 Si5 Rb2 65.30(2) 4_545 . ? Rb2 Si5 Rb2 141.49(3) 3 . ? Si4 O1 Si1 131.26(19) . . ? Si4 O1 Rb1 126.38(14) . 3 ? Si1 O1 Rb1 97.03(13) . 3 ? Si4 O1 Rb2 110.74(15) . 2_554 ? Si1 O1 Rb2 97.64(13) . 2_554 ? Rb1 O1 Rb2 78.31(7) 3 2_554 ? Si2 O2 Si1 135.4(2) 3 . ? Si2 O2 Rb2 109.65(17) 3 2_554 ? Si1 O2 Rb2 114.60(16) . 2_554 ? Si2 O2 Rb3 86.56(14) 3 . ? Si1 O2 Rb3 89.70(12) . . ? Rb2 O2 Rb3 88.00(8) 2_554 . ? Si1 O3 In1 142.03(18) . 1_655 ? Si1 O3 Rb3 123.95(19) . 3 ? In1 O3 Rb3 92.82(11) 1_655 3 ? Si1 O3 Rb2 102.09(17) . 3 ? In1 O3 Rb2 87.47(13) 1_655 3 ? Rb3 O3 Rb2 87.26(9) 3 3 ? Si1 O3 Rb1 91.18(17) . 3 ? In1 O3 Rb1 82.40(11) 1_655 3 ? Rb3 O3 Rb1 84.69(9) 3 3 ? Rb2 O3 Rb1 166.72(12) 3 3 ? Si5 O4 Si1 162.5(3) . . ? Si5 O4 Rb3 90.13(14) . . ? Si1 O4 Rb3 102.81(16) . . ? Si5 O4 Rb2 85.77(14) . 3 ? Si1 O4 Rb2 90.78(14) . 3 ? Rb3 O4 Rb2 142.72(11) . 3 ? Si2 O5 In1 130.6(2) . 3_445 ? Si2 O5 Rb1 121.7(2) . 4_445 ? In1 O5 Rb1 92.48(13) 3_445 4_445 ? Si2 O5 Rb3 113.03(17) . 3_445 ? In1 O5 Rb3 92.77(12) 3_445 3_445 ? Rb1 O5 Rb3 99.13(10) 4_445 3_445 ? Si3 O6 Si2 138.2(2) . . ? Si3 O6 Rb3 100.53(14) . . ? Si2 O6 Rb3 113.20(15) . . ? Si3 O6 Rb2 89.57(14) . . ? Si2 O6 Rb2 121.90(15) . . ? Rb3 O6 Rb2 74.50(7) . . ? Si2 O7 Si4 137.6(2) . 1_455 ? Si2 O7 Rb2 94.08(15) . 4_444 ? Si4 O7 Rb2 98.23(16) 1_455 4_444 ? Si3 O8 Rb2 116.04(17) . . ? Si3 O8 Rb3 148.56(19) . 2 ? Rb2 O8 Rb3 94.54(10) . 2 ? Si3 O8 Rb1 87.45(14) . 2 ? Rb2 O8 Rb1 105.26(10) . 2 ? Rb3 O8 Rb1 77.03(8) 2 2 ? Si3 O9 In1 148.7(2) . . ? Si3 O9 Rb1 115.55(18) . 2 ? In1 O9 Rb1 92.36(12) . 2 ? Si3 O9 Rb2 103.33(16) . 3_455 ? In1 O9 Rb2 89.80(12) . 3_455 ? Rb1 O9 Rb2 89.89(10) 2 3_455 ? Si3 O9 Rb3 89.52(15) . . ? In1 O9 Rb3 77.53(10) . . ? Rb1 O9 Rb3 87.07(9) 2 . ? Rb2 O9 Rb3 166.83(12) 3_455 . ? Si5 O10 Si3 147.8(2) 1_455 . ? Si5 O10 Rb1 94.62(14) 1_455 4_445 ? Si3 O10 Rb1 106.61(15) . 4_445 ? Si5 O10 Rb2 84.81(12) 1_455 3_455 ? Si3 O10 Rb2 86.72(13) . 3_455 ? Rb1 O10 Rb2 152.90(12) 4_445 3_455 ? Si4 O11 In1 130.6(2) . 3_545 ? Si4 O11 Rb1 107.44(16) . . ? In1 O11 Rb1 97.73(12) 3_545 . ? Si4 O11 Rb3 125.71(18) . . ? In1 O11 Rb3 91.60(11) 3_545 . ? Rb1 O11 Rb3 96.24(10) . . ? Si4 O12 Si5 132.4(2) . 2_554 ? Si4 O12 Rb1 91.16(12) . . ? Si5 O12 Rb1 132.68(17) 2_554 . ? Si4 O12 Rb2 101.41(15) . 4_544 ? Si5 O12 Rb2 89.78(13) 2_554 4_544 ? Rb1 O12 Rb2 99.61(8) . 4_544 ? Si5 O13 In1 136.21(19) . 3_545 ? Si5 O13 Rb2 130.05(17) . . ? In1 O13 Rb2 93.74(11) 3_545 . ? Si5 O13 Rb3 95.44(15) . . ? In1 O13 Rb3 85.92(11) 3_545 . ? Rb2 O13 Rb3 87.43(9) . . ? Si5 O13 Rb1 94.21(15) . 4_545 ? In1 O13 Rb1 85.90(10) 3_545 4_545 ? Rb2 O13 Rb1 87.72(9) . 4_545 ? Rb3 O13 Rb1 170.20(12) . 4_545 ? In1 O14 Rb3 95.57(13) . . ? In1 O14 Rb1 93.85(13) . 3_455 ? Rb3 O14 Rb1 158.30(13) . 3_455 ? In1 O14 H2 141.5 . . ? Rb3 O14 H2 108.9 . . ? Rb1 O14 H2 53.9 3_455 . ? In1 O14 H1 109.6 . . ? Rb3 O14 H1 88.7 . . ? Rb1 O14 H1 106.4 3_455 . ? H2 O14 H1 100.3 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rb1 O11 2.848(4) . ? Rb1 O9 2.904(4) 2_554 ? Rb1 O5 2.916(4) 4_544 ? Rb1 O14 3.011(4) 3_545 ? Rb1 O10 3.126(3) 4_544 ? Rb1 O13 3.156(4) 4_444 ? Rb1 O12 3.227(3) . ? Rb1 O1 3.255(3) 3_445 ? Rb1 O3 3.442(4) 3_445 ? Rb1 O8 3.571(4) 2_554 ? Rb1 Si5 3.6387(12) 4_444 ? Rb1 Si4 3.6473(12) . ? Rb2 O13 2.891(3) . ? Rb2 O8 2.968(4) . ? Rb2 O2 2.990(4) 2 ? Rb2 O9 3.031(4) 3_545 ? Rb2 O3 3.141(4) 3_445 ? Rb2 O12 3.293(3) 4_445 ? Rb2 O7 3.381(4) 4_545 ? Rb2 O1 3.386(3) 2 ? Rb2 O4 3.418(3) 3_445 ? Rb2 O10 3.442(3) 3_545 ? Rb2 O6 3.623(4) . ? Rb2 Si5 3.6726(12) 3_445 ? Rb3 O14 2.850(4) . ? Rb3 O3 2.859(3) 3_445 ? Rb3 O11 2.881(3) . ? Rb3 O5 2.936(3) 3 ? Rb3 O13 3.103(4) . ? Rb3 O6 3.202(3) . ? Rb3 O4 3.235(4) . ? Rb3 O8 3.269(4) 2_554 ? Rb3 O9 3.528(4) . ? Rb3 O2 3.583(3) . ? Rb3 Si5 3.6205(14) . ? Rb3 In1 3.6548(6) 3_545 ? Rb3 H2 3.2332 . ? Rb3 H1 2.9420 . ? In1 O14 2.133(3) . ? In1 O3 2.141(4) 1_455 ? In1 O5 2.150(4) 3 ? In1 O13 2.164(3) 3_455 ? In1 O11 2.169(3) 3_455 ? In1 O9 2.171(3) . ? In1 Rb3 3.6548(6) 3_455 ? In1 Rb1 3.6968(6) 2 ? In1 Rb2 3.7222(6) 3_455 ? In1 Rb1 3.8053(6) 3_455 ? Si1 O3 1.584(4) . ? Si1 O4 1.620(3) . ? Si1 O2 1.624(3) . ? Si1 O1 1.638(3) . ? Si1 Rb2 3.8025(13) 3 ? Si1 Rb1 3.8185(12) 3 ? Si1 Rb2 3.9526(13) 2_554 ? Si1 Rb3 3.9674(12) 3 ? Si2 O5 1.584(4) . ? Si2 O7 1.620(3) . ? Si2 O2 1.622(3) 3_445 ? Si2 O6 1.636(4) . ? Si2 Rb3 3.8431(12) 3_445 ? Si2 Rb2 3.8516(13) 4_444 ? Si2 Rb1 3.9836(13) 4_445 ? Si3 O9 1.581(3) . ? Si3 O8 1.632(4) . ? Si3 O6 1.638(3) . ? Si3 O10 1.642(4) . ? Si3 Rb2 3.7282(12) 3_455 ? Si3 Rb1 3.8596(13) 2 ? Si3 Rb1 3.9243(12) 4_445 ? Si4 O11 1.579(3) . ? Si4 O7 1.626(3) 1_655 ? Si4 O12 1.635(3) . ? Si4 O1 1.637(3) . ? Si4 Rb2 3.9559(12) 4_544 ? Si5 O13 1.594(3) . ? Si5 O4 1.618(3) . ? Si5 O10 1.628(4) 1_655 ? Si5 O12 1.639(3) 2 ? Si5 Rb1 3.6387(12) 4_545 ? Si5 Rb2 3.6726(12) 3 ? O1 Rb1 3.255(3) 3 ? O1 Rb2 3.386(3) 2_554 ? O2 Si2 1.622(3) 3 ? O2 Rb2 2.990(4) 2_554 ? O3 In1 2.141(4) 1_655 ? O3 Rb3 2.859(3) 3 ? O3 Rb2 3.141(4) 3 ? O3 Rb1 3.442(4) 3 ? O4 Rb2 3.418(3) 3 ? O5 In1 2.150(4) 3_445 ? O5 Rb1 2.916(4) 4_445 ? O5 Rb3 2.936(3) 3_445 ? O7 Si4 1.626(3) 1_455 ? O7 Rb2 3.381(4) 4_444 ? O8 Rb3 3.269(4) 2 ? O8 Rb1 3.571(4) 2 ? O9 Rb1 2.904(4) 2 ? O9 Rb2 3.031(4) 3_455 ? O10 Si5 1.628(4) 1_455 ? O10 Rb1 3.126(3) 4_445 ? O10 Rb2 3.442(3) 3_455 ? O11 In1 2.169(3) 3_545 ? O12 Si5 1.639(3) 2_554 ? O12 Rb2 3.293(3) 4_544 ? O13 In1 2.164(3) 3_545 ? O13 Rb1 3.156(4) 4_545 ? O14 Rb1 3.011(4) 3_455 ? O14 H2 0.8603 . ? O14 H1 0.7933 . ?
1100707.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100707.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100707 loop_ _publ_author_name 'Jay R. Stork' 'Daniel Rios' 'David Pham' 'Vincent Bicocca' 'Marilyn M. Olmstead' 'Alan L. Balch' _publ_section_title ; Metal-Metal Interactions in Platinum(II)/Gold(I) or Platinum(II)/Silver(I) Salts Containing Planar Cations and Linear Anions ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3466 _journal_page_last 3472 _journal_paper_doi 10.1021/ic048333a _journal_volume 44 _journal_year 2005 _chemical_formula_moiety 'C12 H32 N8 Pt, 2(C2 Au N2)' _chemical_formula_sum 'C16 H32 Au2 N12 Pt' _chemical_formula_weight 981.56 _chemical_name_common '[Pt(C(NHCH3)2)4] 2[Au(CN)2]' _chemical_name_systematic ; ? ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 107.047(15) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 8.919(5) _cell_length_b 15.424(7) _cell_length_c 10.074(5) _cell_measurement_reflns_used 893 _cell_measurement_temperature 90(2) _cell_measurement_theta_max 28.236 _cell_measurement_theta_min 2.728 _cell_volume 1325.0(12) _computing_cell_refinement SAINT _computing_data_collection 'SMART 5.054 (Bruker, 2003)' _computing_data_reduction 'SAINT 6.45A (Bruker, 2003)' _computing_molecular_graphics 'SHELXTL 5.1, XP (Sheldrick, 1994)' _computing_publication_material 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 90(2) _diffrn_detector_area_resol_mean 8.3 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0392 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 2684 _diffrn_reflns_theta_full 26.36 _diffrn_reflns_theta_max 26.36 _diffrn_reflns_theta_min 2.64 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 16.338 _exptl_absorpt_correction_T_max 0.5610 _exptl_absorpt_correction_T_min 0.1677 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS 2.10 (Sheldrick, 2004)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 2.460 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needles _exptl_crystal_F_000 896 _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _refine_diff_density_max 5.092 _refine_diff_density_min -3.642 _refine_diff_density_rms 0.483 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 141 _refine_ls_number_reflns 2684 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.061 _refine_ls_R_factor_all 0.0577 _refine_ls_R_factor_gt 0.0527 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1094P)^2^+0.4633P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1338 _refine_ls_wR_factor_ref 0.1408 _reflns_number_gt 2324 _reflns_number_total 2684 _reflns_threshold_expression I>2\s(I) _cod_data_source_file ic048333asi20041124_041657_1.cif _cod_data_source_block dp32-1 _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. '_exptl_absorpt_correction_type' value 'Multi-scan' changed to 'multi-scan' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_cell_volume 1325.0(11) _cod_original_sg_symbol_H-M 'P 1 21/n 1 ' _cod_database_code 1100707 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.26469(3) 0.166678(17) 0.68845(3) 0.01884(18) Uani 1 1 d . . . N1 N -0.0933(9) 0.1889(4) 0.5304(8) 0.0242(15) Uani 1 1 d . . . N2 N 0.6241(9) 0.1404(5) 0.8265(8) 0.0268(16) Uani 1 1 d . . . C1 C 0.0382(10) 0.1814(5) 0.5902(9) 0.0174(16) Uani 1 1 d . . . C2 C 0.4946(10) 0.1509(5) 0.7793(9) 0.0209(17) Uani 1 1 d . . . Pt1 Pt 0.5000 0.5000 0.5000 0.01214(18) Uani 1 2 d S . . N3 N 0.7253(8) 0.3524(4) 0.5171(7) 0.0185(14) Uani 1 1 d . . . H3A H 0.7465 0.2973 0.5090 0.022 Uiso 1 1 calc R . . N4 N 0.4686(8) 0.3144(4) 0.4356(7) 0.0167(13) Uani 1 1 d . . . H4A H 0.3692 0.3296 0.4139 0.020 Uiso 1 1 calc R . . N5 N 0.6932(7) 0.5110(4) 0.7905(7) 0.0184(14) Uani 1 1 d . . . H5A H 0.7509 0.5406 0.7490 0.022 Uiso 1 1 calc R . . N6 N 0.4684(7) 0.4365(4) 0.7727(7) 0.0189(13) Uani 1 1 d . . . H6A H 0.5093 0.4244 0.8613 0.023 Uiso 1 1 calc R . . C3 C 0.5768(9) 0.3758(5) 0.4819(8) 0.0181(16) Uani 1 1 d . . . C4 C 0.5565(9) 0.4812(4) 0.7101(8) 0.0152(15) Uani 1 1 d . . . C5 C 0.8571(9) 0.4118(4) 0.5685(8) 0.0201(16) Uani 1 1 d . . . H5B H 0.9414 0.3961 0.5289 0.030 Uiso 1 1 calc R . . H5C H 0.8957 0.4081 0.6700 0.030 Uiso 1 1 calc R . . H5D H 0.8226 0.4713 0.5412 0.030 Uiso 1 1 calc R . . C6 C 0.5053(8) 0.2239(5) 0.4187(8) 0.0199(16) Uiso 1 1 d . . . H6B H 0.4078 0.1905 0.3867 0.030 Uiso 1 1 calc R . . H6C H 0.5695 0.2007 0.5079 0.030 Uiso 1 1 calc R . . H6D H 0.5635 0.2194 0.3501 0.030 Uiso 1 1 calc R . . C7 C 0.7559(10) 0.4999(5) 0.9374(8) 0.0219(17) Uani 1 1 d . . . H7A H 0.8589 0.5279 0.9696 0.033 Uiso 1 1 calc R . . H7B H 0.7670 0.4379 0.9594 0.033 Uiso 1 1 calc R . . H7C H 0.6849 0.5263 0.9840 0.033 Uiso 1 1 calc R . . C8 C 0.3115(9) 0.4065(5) 0.7058(8) 0.0210(16) Uani 1 1 d . . . H8A H 0.2766 0.3691 0.7696 0.032 Uiso 1 1 calc R . . H8B H 0.3101 0.3736 0.6222 0.032 Uiso 1 1 calc R . . H8C H 0.2408 0.4564 0.6800 0.032 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.0212(3) 0.0168(3) 0.0210(3) -0.00224(11) 0.01011(17) 0.00383(10) N1 0.032(4) 0.013(3) 0.028(4) 0.000(3) 0.009(3) 0.001(3) N2 0.030(4) 0.026(3) 0.027(4) -0.004(3) 0.013(3) 0.002(3) C1 0.021(4) 0.012(3) 0.022(4) -0.001(3) 0.010(3) 0.003(3) C2 0.019(4) 0.022(4) 0.023(4) 0.004(3) 0.009(3) 0.007(3) Pt1 0.0171(3) 0.0073(3) 0.0157(3) 0.00069(14) 0.01055(18) -0.00016(13) N3 0.023(3) 0.010(3) 0.027(4) -0.002(3) 0.015(3) 0.001(2) N4 0.019(3) 0.010(3) 0.024(3) -0.002(3) 0.013(3) -0.001(2) N5 0.023(4) 0.017(3) 0.018(3) 0.001(3) 0.010(3) -0.004(3) N6 0.027(3) 0.012(3) 0.019(3) 0.006(3) 0.010(3) -0.001(3) C3 0.028(4) 0.018(4) 0.014(4) -0.001(3) 0.014(3) -0.010(3) C4 0.025(4) 0.003(3) 0.022(4) 0.001(3) 0.014(3) 0.005(3) C5 0.023(4) 0.012(3) 0.032(5) -0.004(3) 0.018(3) -0.002(3) C7 0.024(4) 0.021(4) 0.019(4) 0.000(3) 0.004(3) 0.003(3) C8 0.025(4) 0.014(4) 0.028(4) 0.005(3) 0.014(3) -0.003(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Au1 C2 177.4(3) . . ? N1 C1 Au1 178.4(7) . . ? N2 C2 Au1 177.6(8) . . ? C4 Pt1 C4 180.000(1) 3_666 . ? C4 Pt1 C3 88.4(3) 3_666 3_666 ? C4 Pt1 C3 91.6(3) . 3_666 ? C4 Pt1 C3 91.6(3) 3_666 . ? C4 Pt1 C3 88.4(3) . . ? C3 Pt1 C3 180.000(1) 3_666 . ? C3 N3 C5 124.4(6) . . ? C3 N3 H3A 117.8 . . ? C5 N3 H3A 117.8 . . ? C3 N4 C6 123.8(7) . . ? C3 N4 H4A 118.1 . . ? C6 N4 H4A 118.1 . . ? C4 N5 C7 126.7(7) . . ? C4 N5 H5A 116.6 . . ? C7 N5 H5A 116.6 . . ? C4 N6 C8 124.8(7) . . ? C4 N6 H6A 117.6 . . ? C8 N6 H6A 117.6 . . ? N3 C3 N4 117.9(7) . . ? N3 C3 Pt1 124.4(5) . . ? N4 C3 Pt1 117.7(6) . . ? N5 C4 N6 116.9(7) . . ? N5 C4 Pt1 118.9(5) . . ? N6 C4 Pt1 124.1(6) . . ? N3 C5 H5B 109.5 . . ? N3 C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N3 C5 H5D 109.5 . . ? H5B C5 H5D 109.5 . . ? H5C C5 H5D 109.5 . . ? N4 C6 H6B 109.5 . . ? N4 C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N4 C6 H6D 109.5 . . ? H6B C6 H6D 109.5 . . ? H6C C6 H6D 109.5 . . ? N5 C7 H7A 109.5 . . ? N5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N6 C8 H8A 109.5 . . ? N6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 C1 1.985(8) . ? Au1 C2 2.000(8) . ? N1 C1 1.156(11) . ? N2 C2 1.124(11) . ? Pt1 C4 2.048(8) 3_666 ? Pt1 C4 2.048(8) . ? Pt1 C3 2.061(8) 3_666 ? Pt1 C3 2.061(8) . ? N3 C3 1.317(10) . ? N3 C5 1.461(9) . ? N3 H3A 0.8800 . ? N4 C3 1.335(10) . ? N4 C6 1.456(9) . ? N4 H4A 0.8800 . ? N5 C4 1.333(10) . ? N5 C7 1.431(11) . ? N5 H5A 0.8800 . ? N6 C4 1.334(9) . ? N6 C8 1.440(9) . ? N6 H6A 0.8800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C5 H5D 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C6 H6D 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3A N1 0.88 2.17 2.979(10) 152.8 1_655 N4 H4A N2 0.88 2.15 3.025(10) 170.4 4_565 N5 H5A N2 0.88 2.16 3.025(10) 165.7 2_656 loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 Au1 C1 N1 24(30) . . . . ? C1 Au1 C2 N2 -25(24) . . . . ? C5 N3 C3 N4 179.6(7) . . . . ? C5 N3 C3 Pt1 -2.7(11) . . . . ? C6 N4 C3 N3 -1.5(11) . . . . ? C6 N4 C3 Pt1 -179.4(6) . . . . ? C4 Pt1 C3 N3 105.8(7) 3_666 . . . ? C4 Pt1 C3 N3 -74.2(7) . . . . ? C3 Pt1 C3 N3 -154(100) 3_666 . . . ? C4 Pt1 C3 N4 -76.4(6) 3_666 . . . ? C4 Pt1 C3 N4 103.6(6) . . . . ? C3 Pt1 C3 N4 24(100) 3_666 . . . ? C7 N5 C4 N6 0.2(11) . . . . ? C7 N5 C4 Pt1 -176.3(6) . . . . ? C8 N6 C4 N5 173.7(7) . . . . ? C8 N6 C4 Pt1 -10.0(10) . . . . ? C4 Pt1 C4 N5 145(100) 3_666 . . . ? C3 Pt1 C4 N5 -82.1(6) 3_666 . . . ? C3 Pt1 C4 N5 97.9(6) . . . . ? C4 Pt1 C4 N6 -31(100) 3_666 . . . ? C3 Pt1 C4 N6 101.6(6) 3_666 . . . ? C3 Pt1 C4 N6 -78.4(6) . . . . ?
1100708.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100708.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100708 loop_ _publ_author_name 'Jay R. Stork' 'Daniel Rios' 'David Pham' 'Vincent Bicocca' 'Marilyn M. Olmstead' 'Alan L. Balch' _publ_section_title ; Metal-Metal Interactions in Platinum(II)/Gold(I) or Platinum(II)/Silver(I) Salts Containing Planar Cations and Linear Anions ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3466 _journal_page_last 3472 _journal_paper_doi 10.1021/ic048333a _journal_volume 44 _journal_year 2005 _chemical_formula_moiety 'C12 H32 N8 Pt, C2 Ag2 N4, C2 Ag N2' _chemical_formula_sum 'C16 H32 Ag3 N14 Pt' _chemical_formula_weight 939.26 _chemical_name_common ; [Pt(C(NHCH~3~)~2~)~4~][Ag(CN)~2~][Ag~2~(CN)~3~] ; _chemical_name_systematic ; ? ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 86.480(2) _cell_angle_beta 74.549(2) _cell_angle_gamma 89.270(3) _cell_formula_units_Z 1 _cell_length_a 8.3863(5) _cell_length_b 8.4243(5) _cell_length_c 10.8888(7) _cell_measurement_reflns_used 1002 _cell_measurement_temperature 90(2) _cell_measurement_theta_max 31.0215 _cell_measurement_theta_min 2.4235 _cell_volume 740.07(8) _computing_cell_refinement SAINT _computing_data_collection 'SMART 5.054 (Bruker, 2003)' _computing_data_reduction 'SAINT 6.45A (Bruker, 2003)' _computing_molecular_graphics 'SHELXTL 5.1, XP (Sheldrick, 1994)' _computing_publication_material 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 90(2) _diffrn_detector_area_resol_mean 8.3 _diffrn_measured_fraction_theta_full 0.962 _diffrn_measured_fraction_theta_max 0.962 _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0276 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 2600 _diffrn_reflns_theta_full 25.34 _diffrn_reflns_theta_max 25.34 _diffrn_reflns_theta_min 1.94 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 6.696 _exptl_absorpt_correction_T_max 0.6164 _exptl_absorpt_correction_T_min 0.3205 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS 2.10 (Sheldrick, 2004)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 2.107 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 445 _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.08 _refine_diff_density_max 1.222 _refine_diff_density_min -0.802 _refine_diff_density_rms 0.134 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.904 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 170 _refine_ls_number_reflns 2600 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.904 _refine_ls_R_factor_all 0.0283 _refine_ls_R_factor_gt 0.0236 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0442P)^2^+1.5374P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0580 _refine_ls_wR_factor_ref 0.0625 _reflns_number_gt 2361 _reflns_number_total 2600 _reflns_threshold_expression I>2\s(I) _cod_data_source_file ic048333asi20041124_041657_2.cif _cod_data_source_block dp33-1 _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. '_exptl_absorpt_correction_type' value 'Multi-scan' changed to 'multi-scan' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_sg_symbol_H-M 'P -1 ' _cod_database_code 1100708 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.00373(5) 0.29266(5) 0.39602(4) 0.02455(12) Uani 1 1 d . . . N/C1 N 0.0029(6) 0.0641(6) 0.4775(4) 0.0304(11) Uani 1 1 d . . . N2 N -0.0453(6) 0.6293(5) 0.2585(4) 0.0280(10) Uani 1 1 d . . . C2 C -0.0310(6) 0.5104(6) 0.3122(5) 0.0206(10) Uani 1 1 d . . . Pt1 Pt 0.0000 0.0000 0.0000 0.01126(9) Uani 1 2 d S . . N4 N 0.2553(5) -0.1902(5) -0.1777(4) 0.0189(9) Uani 1 1 d . . . H4A H 0.3319 -0.2006 -0.2498 0.023 Uiso 1 1 calc R . . N5 N 0.2206(5) 0.0574(5) -0.2578(3) 0.0167(8) Uani 1 1 d . . . H5A H 0.1754 0.1520 -0.2461 0.020 Uiso 1 1 calc R . . N6 N 0.2048(5) -0.1046(5) 0.1701(4) 0.0184(9) Uani 1 1 d . . . H6A H 0.1434 -0.1900 0.1755 0.022 Uiso 1 1 calc R . . N7 N 0.2690(5) 0.1483(5) 0.0923(4) 0.0182(9) Uani 1 1 d . . . H7A H 0.3436 0.1443 0.1359 0.022 Uiso 1 1 calc R . . C4 C 0.2244(7) -0.3256(6) -0.0840(5) 0.0216(11) Uani 1 1 d . . . H4D H 0.2698 -0.4222 -0.1260 0.032 Uiso 0.50 1 calc PR A 1 H4C H 0.1049 -0.3388 -0.0470 0.032 Uiso 0.50 1 calc PR A 1 H4B H 0.2776 -0.3068 -0.0163 0.032 Uiso 0.50 1 calc PR A 1 H4X H 0.1520 -0.2927 -0.0032 0.032 Uiso 0.50 1 d PR A 2 H4Y H 0.3295 -0.3640 -0.0704 0.032 Uiso 0.50 1 d PR A 2 H4Z H 0.1707 -0.4111 -0.1156 0.032 Uiso 0.50 1 d PR A 2 C5 C 0.3379(6) 0.0338(6) -0.3808(4) 0.0203(10) Uani 1 1 d . . . H5D H 0.3463 0.1315 -0.4359 0.030 Uiso 1 1 calc R . . H5C H 0.2996 -0.0536 -0.4213 0.030 Uiso 1 1 calc R . . H5B H 0.4468 0.0076 -0.3680 0.030 Uiso 1 1 calc R . . C6 C 0.3290(6) -0.1108(6) 0.2420(5) 0.0237(11) Uani 1 1 d . . . H6D H 0.3287 -0.2169 0.2843 0.036 Uiso 1 1 calc R . . H6C H 0.3032 -0.0312 0.3064 0.036 Uiso 1 1 calc R . . H6B H 0.4384 -0.0885 0.1837 0.036 Uiso 1 1 calc R . . C7 C 0.2537(7) 0.2957(6) 0.0187(5) 0.0229(11) Uani 1 1 d . . . H7D H 0.3597 0.3526 -0.0050 0.034 Uiso 0.50 1 calc PR B 1 H7C H 0.1683 0.3625 0.0704 0.034 Uiso 0.50 1 calc PR B 1 H7B H 0.2227 0.2710 -0.0587 0.034 Uiso 0.50 1 calc PR B 1 H7X H 0.164(15) 0.276(15) -0.024(11) 0.034 Uiso 0.50 1 d P C 2 H7Y H 0.362(15) 0.329(14) -0.052(11) 0.034 Uiso 0.50 1 d P D 2 H7Z H 0.238(15) 0.409(15) 0.074(11) 0.034 Uiso 0.50 1 d P E 2 C8 C 0.1763(6) -0.0531(5) -0.1616(4) 0.0139(9) Uani 1 1 d . . . C9 C 0.1764(6) 0.0191(6) 0.0971(4) 0.0154(10) Uani 1 1 d . . . Ag2 Ag 0.5000 0.5000 0.5000 0.02479(15) Uani 1 2 d S . . N3 N 0.3831(5) 0.3006(5) 0.2991(4) 0.0240(10) Uani 1 1 d . . . C3 C 0.4221(6) 0.3762(6) 0.3694(5) 0.0218(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0297(2) 0.0156(2) 0.0289(2) 0.00790(16) -0.01089(18) 0.00047(17) N/C1 0.034(3) 0.024(2) 0.036(3) 0.006(2) -0.015(2) -0.001(2) N2 0.035(3) 0.018(3) 0.033(2) 0.004(2) -0.012(2) 0.000(2) C2 0.021(3) 0.017(3) 0.024(2) 0.001(2) -0.007(2) -0.002(2) Pt1 0.01463(14) 0.00980(14) 0.00988(13) 0.00059(9) -0.00445(9) 0.00016(9) N4 0.023(2) 0.018(2) 0.0127(18) 0.0008(16) -0.0011(16) 0.0052(18) N5 0.017(2) 0.017(2) 0.0128(18) 0.0042(16) 0.0003(16) -0.0003(17) N6 0.023(2) 0.017(2) 0.019(2) 0.0033(16) -0.0125(17) -0.0060(17) N7 0.023(2) 0.016(2) 0.019(2) 0.0007(16) -0.0106(17) -0.0007(17) C4 0.031(3) 0.011(2) 0.023(2) -0.0015(19) -0.008(2) 0.003(2) C5 0.017(2) 0.027(3) 0.015(2) 0.002(2) -0.0029(19) 0.001(2) C6 0.027(3) 0.024(3) 0.023(2) 0.000(2) -0.014(2) 0.003(2) C7 0.026(3) 0.015(3) 0.027(3) 0.002(2) -0.007(2) -0.005(2) C8 0.015(2) 0.014(2) 0.013(2) -0.0021(18) -0.0043(18) 0.0010(19) C9 0.017(2) 0.014(2) 0.014(2) -0.0025(18) -0.0014(18) 0.0030(19) Ag2 0.0345(3) 0.0212(3) 0.0225(3) -0.0067(2) -0.0129(2) -0.0011(2) N3 0.024(2) 0.026(2) 0.024(2) -0.0079(19) -0.0089(19) 0.0008(19) C3 0.021(3) 0.022(3) 0.022(2) -0.004(2) -0.004(2) 0.000(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Ag1 N/C1 171.08(19) . . ? N/C1 N/C1 Ag1 177.7(6) 2_556 . ? N2 C2 Ag1 176.0(5) . . ? C8 Pt1 C8 180.0(3) 2 . ? C8 Pt1 C9 91.02(17) 2 2 ? C8 Pt1 C9 88.98(17) . 2 ? C8 Pt1 C9 88.98(17) 2 . ? C8 Pt1 C9 91.02(17) . . ? C9 Pt1 C9 180.00(19) 2 . ? C8 N4 C4 124.5(4) . . ? C8 N4 H4A 117.7 . . ? C4 N4 H4A 117.7 . . ? C8 N5 C5 125.3(4) . . ? C8 N5 H5A 117.4 . . ? C5 N5 H5A 117.4 . . ? C9 N6 C6 125.6(4) . . ? C9 N6 H6A 117.2 . . ? C6 N6 H6A 117.2 . . ? C9 N7 C7 123.8(4) . . ? C9 N7 H7A 118.1 . . ? C7 N7 H7A 118.1 . . ? N4 C4 H4D 109.5 . . ? N4 C4 H4C 109.5 . . ? N4 C4 H4B 109.5 . . ? N4 C4 H4X 109.5 . . ? N4 C4 H4Y 109.5 . . ? H4X C4 H4Y 109.5 . . ? N4 C4 H4Z 109.5 . . ? H4X C4 H4Z 109.5 . . ? H4Y C4 H4Z 109.5 . . ? N5 C5 H5D 109.5 . . ? N5 C5 H5C 109.5 . . ? H5D C5 H5C 109.5 . . ? N5 C5 H5B 109.5 . . ? H5D C5 H5B 109.5 . . ? H5C C5 H5B 109.5 . . ? N6 C6 H6D 109.5 . . ? N6 C6 H6C 109.5 . . ? H6D C6 H6C 109.5 . . ? N6 C6 H6B 109.5 . . ? H6D C6 H6B 109.5 . . ? H6C C6 H6B 109.5 . . ? N7 C7 H7D 109.5 . . ? N7 C7 H7C 109.5 . . ? N7 C7 H7B 109.5 . . ? N7 C7 H7X 106(7) . . ? H7D C7 H7X 135.8 . . ? H7C C7 H7X 81.9 . . ? H7B C7 H7X 31.7 . . ? N7 C7 H7Y 114(7) . . ? H7D C7 H7Y 31.8 . . ? H7C C7 H7Y 129.7 . . ? H7B C7 H7Y 78.8 . . ? H7X C7 H7Y 108(9) . . ? N7 C7 H7Z 116(6) . . ? H7D C7 H7Z 71.7 . . ? H7C C7 H7Z 38.7 . . ? H7B C7 H7Z 131.4 . . ? H7X C7 H7Z 115(9) . . ? H7Y C7 H7Z 98(9) . . ? N4 C8 N5 116.2(4) . . ? N4 C8 Pt1 124.5(3) . . ? N5 C8 Pt1 119.3(3) . . ? N6 C9 N7 116.1(4) . . ? N6 C9 Pt1 119.2(3) . . ? N7 C9 Pt1 124.7(3) . . ? C3 Ag2 C3 180.0(2) . 2_666 ? N3 C3 Ag2 176.3(5) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 C2 2.051(5) . ? Ag1 N/C1 2.070(4) . ? N/C1 N/C1 1.154(9) 2_556 ? N2 C2 1.150(6) . ? Pt1 C8 2.043(4) 2 ? Pt1 C8 2.043(4) . ? Pt1 C9 2.048(5) 2 ? Pt1 C9 2.048(5) . ? N4 C8 1.322(6) . ? N4 C4 1.460(6) . ? N4 H4A 0.8800 . ? N5 C8 1.336(6) . ? N5 C5 1.458(6) . ? N5 H5A 0.8800 . ? N6 C9 1.329(6) . ? N6 C6 1.459(6) . ? N6 H6A 0.8800 . ? N7 C9 1.336(6) . ? N7 C7 1.459(6) . ? N7 H7A 0.8800 . ? C4 H4D 0.9800 . ? C4 H4C 0.9800 . ? C4 H4B 0.9800 . ? C4 H4X 0.9801 . ? C4 H4Y 0.9801 . ? C4 H4Z 0.9800 . ? C5 H5D 0.9800 . ? C5 H5C 0.9800 . ? C5 H5B 0.9800 . ? C6 H6D 0.9800 . ? C6 H6C 0.9800 . ? C6 H6B 0.9800 . ? C7 H7D 0.9800 . ? C7 H7C 0.9800 . ? C7 H7B 0.9800 . ? C7 H7X 1.01(12) . ? C7 H7Y 1.05(12) . ? C7 H7Z 1.15(13) . ? Ag2 C3 2.056(5) . ? Ag2 C3 2.056(5) 2_666 ? N3 C3 1.140(6) . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N4 H4A N3 0.88 2.46 3.123(6) 132.9 2_655 N5 H5A N2 0.88 2.15 3.006(6) 165.8 2_565 N6 H6A N2 0.88 2.18 3.021(6) 159.0 1_545 N7 H7A N3 0.88 2.37 3.028(5) 131.8 . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 Ag1 N/C1 N/C1 -3(17) . . . 2_556 ? N/C1 Ag1 C2 N2 -96(6) . . . . ? C4 N4 C8 N5 -179.8(4) . . . . ? C4 N4 C8 Pt1 2.1(6) . . . . ? C5 N5 C8 N4 5.1(7) . . . . ? C5 N5 C8 Pt1 -176.7(3) . . . . ? C8 Pt1 C8 N4 -87(100) 2 . . . ? C9 Pt1 C8 N4 -107.1(4) 2 . . . ? C9 Pt1 C8 N4 72.9(4) . . . . ? C8 Pt1 C8 N5 95(100) 2 . . . ? C9 Pt1 C8 N5 74.8(4) 2 . . . ? C9 Pt1 C8 N5 -105.2(4) . . . . ? C6 N6 C9 N7 -1.2(7) . . . . ? C6 N6 C9 Pt1 178.2(4) . . . . ? C7 N7 C9 N6 -179.1(4) . . . . ? C7 N7 C9 Pt1 1.6(7) . . . . ? C8 Pt1 C9 N6 83.1(4) 2 . . . ? C8 Pt1 C9 N6 -96.9(4) . . . . ? C9 Pt1 C9 N6 -44(100) 2 . . . ? C8 Pt1 C9 N7 -97.6(4) 2 . . . ? C8 Pt1 C9 N7 82.4(4) . . . . ? C9 Pt1 C9 N7 135(100) 2 . . . ? C3 Ag2 C3 N3 8(100) 2_666 . . . ?
1100709.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100709.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100709 loop_ _publ_author_name 'Jay R. Stork' 'Daniel Rios' 'David Pham' 'Vincent Bicocca' 'Marilyn M. Olmstead' 'Alan L. Balch' _publ_section_title ; Metal-Metal Interactions in Platinum(II)/Gold(I) or Platinum(II)/Silver(I) Salts Containing Planar Cations and Linear Anions ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3466 _journal_page_last 3472 _journal_paper_doi 10.1021/ic048333a _journal_volume 44 _journal_year 2005 _chemical_formula_moiety 'C20 H16 N4 Pt, 2(C2 Au N2)' _chemical_formula_sum 'C24 H16 Au2 N8 Pt' _chemical_formula_weight 1005.47 _chemical_name_common '[Pt(bpy)~2~][Au(CN)~2~]~2~' _chemical_name_systematic ; ? ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 75.077(2) _cell_angle_beta 77.247(5) _cell_angle_gamma 79.743(6) _cell_formula_units_Z 1 _cell_length_a 7.0515(13) _cell_length_b 9.2481(14) _cell_length_c 9.2728(18) _cell_measurement_reflns_used 914 _cell_measurement_temperature 90(2) _cell_measurement_theta_max 30.5 _cell_measurement_theta_min 2.87 _cell_volume 565.16(17) _computing_cell_refinement SAINT _computing_data_collection 'SMART 5.054 (Bruker, 2003)' _computing_data_reduction 'SAINT 6.45A (Bruker, 2003)' _computing_molecular_graphics 'SHELXTL 5.1 (Sheldrick, 1994)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _diffrn_ambient_temperature 90(2) _diffrn_detector_area_resol_mean 8.3 _diffrn_measured_fraction_theta_full 0.978 _diffrn_measured_fraction_theta_max 0.978 _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0373 _diffrn_reflns_av_sigmaI/netI 0.0255 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 8943 _diffrn_reflns_theta_full 25.33 _diffrn_reflns_theta_max 25.33 _diffrn_reflns_theta_min 2.31 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 19.152 _exptl_absorpt_correction_T_max 0.72644 _exptl_absorpt_correction_T_min 0.04045 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'TWINABS (Sheldrick, 2002)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 2.954 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 452 _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.02 _refine_diff_density_max 2.713 _refine_diff_density_min -1.730 _refine_diff_density_rms 0.307 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 151 _refine_ls_number_reflns 2401 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.047 _refine_ls_R_factor_all 0.0387 _refine_ls_R_factor_gt 0.0354 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0720P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0903 _refine_ls_wR_factor_ref 0.0921 _reflns_number_gt 2225 _reflns_number_total 2401 _reflns_threshold_expression I>2\s(I) _cod_data_source_file ic048333asi20041124_041657_3.cif _cod_data_source_block jrs57-1 _cod_database_code 1100709 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.5000 0.5000 0.5000 0.00839(15) Uani 1 2 d S . . C1 C 0.7496(13) 0.2181(11) 0.4223(11) 0.014(2) Uani 1 1 d . . . H1 H 0.7385 0.1767 0.5283 0.017 Uiso 1 1 calc R . . C2 C 0.8418(14) 0.1273(12) 0.3226(11) 0.017(2) Uani 1 1 d . . . H2 H 0.8949 0.0260 0.3597 0.020 Uiso 1 1 calc R . . C3 C 0.8551(14) 0.1864(11) 0.1688(10) 0.014(2) Uani 1 1 d . . . H3 H 0.9082 0.1245 0.0985 0.017 Uiso 1 1 calc R . . C4 C 0.7897(14) 0.3383(12) 0.1185(11) 0.017(2) Uani 1 1 d . . . H4 H 0.8043 0.3819 0.0126 0.021 Uiso 1 1 calc R . . C5 C 0.7031(12) 0.4265(11) 0.2218(10) 0.0113(19) Uani 1 1 d . . . C6 C 0.6577(14) 0.5892(11) 0.1849(11) 0.015(2) Uiso 1 1 d . . . C7 C 0.6994(13) 0.6803(11) 0.0415(11) 0.014(2) Uani 1 1 d . . . H7 H 0.7416 0.6366 -0.0442 0.017 Uiso 1 1 calc R . . C8 C 0.6802(14) 0.8316(12) 0.0230(11) 0.016(2) Uani 1 1 d . . . H8 H 0.7018 0.8946 -0.0763 0.020 Uiso 1 1 calc R . . C9 C 0.6300(13) 0.8942(12) 0.1467(11) 0.015(2) Uani 1 1 d . . . H9 H 0.6241 1.0000 0.1344 0.018 Uiso 1 1 calc R . . C10 C 0.5880(13) 0.8024(11) 0.2893(11) 0.014(2) Uani 1 1 d . . . H10 H 0.5528 0.8451 0.3759 0.017 Uiso 1 1 calc R . . N1 N 0.6761(11) 0.3612(9) 0.3746(8) 0.0111(16) Uani 1 1 d . . . N2 N 0.5964(10) 0.6533(9) 0.3068(8) 0.0101(16) Uiso 1 1 d . . . Au1 Au 0.83233(5) 0.52210(4) 0.67213(4) 0.01418(15) Uani 1 1 d . . . C11 C 0.7529(14) 0.7438(11) 0.6381(11) 0.014(2) Uani 1 1 d . . . C12 C 0.8878(14) 0.2998(11) 0.7375(12) 0.015(2) Uani 1 1 d . . . N3 N 0.6915(13) 0.8679(11) 0.6293(10) 0.024(2) Uani 1 1 d . . . N4 N 0.9038(14) 0.1722(11) 0.7858(10) 0.026(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0081(2) 0.0110(3) 0.0064(2) -0.0037(2) 0.00022(18) -0.0015(2) C1 0.012(5) 0.013(5) 0.016(5) -0.002(4) 0.001(4) -0.005(4) C2 0.016(5) 0.018(5) 0.021(5) -0.016(4) -0.005(4) 0.002(4) C3 0.019(5) 0.012(5) 0.014(5) -0.010(4) 0.006(4) -0.008(4) C4 0.014(5) 0.029(6) 0.014(5) -0.009(4) -0.003(4) -0.008(4) C5 0.004(4) 0.012(5) 0.018(5) -0.002(4) -0.005(4) 0.000(4) C7 0.010(5) 0.020(6) 0.012(5) -0.006(4) -0.001(4) 0.001(4) C8 0.013(5) 0.016(5) 0.017(5) 0.002(4) -0.003(4) -0.001(4) C9 0.009(5) 0.015(5) 0.020(5) -0.001(4) -0.003(4) -0.002(4) C10 0.009(4) 0.015(5) 0.019(5) -0.005(4) 0.001(4) -0.007(4) N1 0.008(4) 0.018(4) 0.010(4) -0.007(3) 0.003(3) -0.008(3) Au1 0.0129(2) 0.0186(2) 0.0126(2) -0.00512(16) -0.00320(14) -0.00269(16) C11 0.015(5) 0.014(6) 0.016(5) 0.000(4) -0.008(4) -0.006(4) C12 0.011(5) 0.011(5) 0.028(5) -0.010(4) -0.008(4) 0.001(4) N3 0.024(5) 0.029(6) 0.019(5) 0.001(4) -0.002(4) -0.012(4) N4 0.027(5) 0.030(6) 0.019(5) -0.011(4) -0.002(4) 0.003(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pt1 N1 180.000(1) 2_666 . ? N1 Pt1 N2 79.3(3) 2_666 2_666 ? N1 Pt1 N2 100.7(3) . 2_666 ? N1 Pt1 N2 100.7(3) 2_666 . ? N1 Pt1 N2 79.3(3) . . ? N2 Pt1 N2 180.0(4) 2_666 . ? N1 Pt1 Au1 86.0(2) 2_666 . ? N1 Pt1 Au1 94.0(2) . . ? N2 Pt1 Au1 85.1(2) 2_666 . ? N2 Pt1 Au1 94.9(2) . . ? N1 Pt1 Au1 94.0(2) 2_666 2_666 ? N1 Pt1 Au1 86.0(2) . 2_666 ? N2 Pt1 Au1 94.9(2) 2_666 2_666 ? N2 Pt1 Au1 85.1(2) . 2_666 ? Au1 Pt1 Au1 180.0 . 2_666 ? N1 C1 C2 122.3(9) . . ? N1 C1 H1 118.8 . . ? C2 C1 H1 118.9 . . ? C3 C2 C1 118.9(10) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C2 C3 C4 118.8(9) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? C5 C4 C3 120.4(9) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? N1 C5 C4 119.4(9) . . ? N1 C5 C6 114.8(8) . . ? C4 C5 C6 125.4(9) . . ? N2 C6 C7 119.4(9) . . ? N2 C6 C5 114.9(8) . . ? C7 C6 C5 124.9(9) . . ? C8 C7 C6 120.1(9) . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C7 C8 C9 120.1(9) . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C8 C9 C10 119.3(10) . . ? C8 C9 H9 120.3 . . ? C10 C9 H9 120.3 . . ? N2 C10 C9 120.4(9) . . ? N2 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C1 N1 C5 119.8(8) . . ? C1 N1 Pt1 127.9(6) . . ? C5 N1 Pt1 112.1(6) . . ? C10 N2 C6 120.5(8) . . ? C10 N2 Pt1 127.4(6) . . ? C6 N2 Pt1 111.9(6) . . ? C12 Au1 C11 171.3(4) . . ? C12 Au1 Pt1 92.4(3) . . ? C11 Au1 Pt1 89.1(3) . . ? C12 Au1 Au1 85.2(3) . 2_766 ? C11 Au1 Au1 103.5(3) . 2_766 ? Pt1 Au1 Au1 85.599(19) . 2_766 ? N3 C11 Au1 173.2(9) . . ? N4 C12 Au1 173.4(9) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 N1 2.026(7) 2_666 ? Pt1 N1 2.026(7) . ? Pt1 N2 2.044(7) 2_666 ? Pt1 N2 2.044(8) . ? Pt1 Au1 3.1735(6) . ? Pt1 Au1 3.1735(6) 2_666 ? C1 N1 1.331(12) . ? C1 C2 1.387(13) . ? C1 H1 0.9500 . ? C2 C3 1.378(14) . ? C2 H2 0.9500 . ? C3 C4 1.389(14) . ? C3 H3 0.9500 . ? C4 C5 1.387(13) . ? C4 H4 0.9500 . ? C5 N1 1.374(11) . ? C5 C6 1.448(14) . ? C6 N2 1.362(12) . ? C6 C7 1.379(13) . ? C7 C8 1.350(14) . ? C7 H7 0.9500 . ? C8 C9 1.366(14) . ? C8 H8 0.9500 . ? C9 C10 1.377(13) . ? C9 H9 0.9500 . ? C10 N2 1.338(11) . ? C10 H10 0.9500 . ? Au1 C12 1.980(10) . ? Au1 C11 1.988(10) . ? Au1 Au1 3.5978(9) 2_766 ? C11 N3 1.141(13) . ? C12 N4 1.145(13) . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -1.1(14) . . . . ? C1 C2 C3 C4 5.0(14) . . . . ? C2 C3 C4 C5 -3.3(14) . . . . ? C3 C4 C5 N1 -2.4(13) . . . . ? C3 C4 C5 C6 169.7(9) . . . . ? N1 C5 C6 N2 0.5(12) . . . . ? C4 C5 C6 N2 -171.9(8) . . . . ? N1 C5 C6 C7 170.4(9) . . . . ? C4 C5 C6 C7 -2.0(16) . . . . ? N2 C6 C7 C8 0.3(14) . . . . ? C5 C6 C7 C8 -169.2(9) . . . . ? C6 C7 C8 C9 3.6(14) . . . . ? C7 C8 C9 C10 -3.8(14) . . . . ? C8 C9 C10 N2 0.1(13) . . . . ? C2 C1 N1 C5 -4.8(14) . . . . ? C2 C1 N1 Pt1 169.2(7) . . . . ? C4 C5 N1 C1 6.4(13) . . . . ? C6 C5 N1 C1 -166.5(8) . . . . ? C4 C5 N1 Pt1 -168.4(7) . . . . ? C6 C5 N1 Pt1 18.7(10) . . . . ? N1 Pt1 N1 C1 158(100) 2_666 . . . ? N2 Pt1 N1 C1 -16.7(8) 2_666 . . . ? N2 Pt1 N1 C1 163.3(8) . . . . ? Au1 Pt1 N1 C1 69.0(8) . . . . ? Au1 Pt1 N1 C1 -111.0(8) 2_666 . . . ? N1 Pt1 N1 C5 -27(100) 2_666 . . . ? N2 Pt1 N1 C5 157.6(6) 2_666 . . . ? N2 Pt1 N1 C5 -22.4(6) . . . . ? Au1 Pt1 N1 C5 -116.6(6) . . . . ? Au1 Pt1 N1 C5 63.4(6) 2_666 . . . ? C9 C10 N2 C6 3.9(13) . . . . ? C9 C10 N2 Pt1 -169.5(7) . . . . ? C7 C6 N2 C10 -4.1(13) . . . . ? C5 C6 N2 C10 166.5(8) . . . . ? C7 C6 N2 Pt1 170.3(7) . . . . ? C5 C6 N2 Pt1 -19.2(10) . . . . ? N1 Pt1 N2 C10 16.5(8) 2_666 . . . ? N1 Pt1 N2 C10 -163.5(8) . . . . ? N2 Pt1 N2 C10 152(100) 2_666 . . . ? Au1 Pt1 N2 C10 -70.3(7) . . . . ? Au1 Pt1 N2 C10 109.7(7) 2_666 . . . ? N1 Pt1 N2 C6 -157.4(6) 2_666 . . . ? N1 Pt1 N2 C6 22.6(6) . . . . ? N2 Pt1 N2 C6 -21(100) 2_666 . . . ? Au1 Pt1 N2 C6 115.8(6) . . . . ? Au1 Pt1 N2 C6 -64.2(6) 2_666 . . . ? N1 Pt1 Au1 C12 126.3(4) 2_666 . . . ? N1 Pt1 Au1 C12 -53.7(4) . . . . ? N2 Pt1 Au1 C12 46.7(4) 2_666 . . . ? N2 Pt1 Au1 C12 -133.3(4) . . . . ? Au1 Pt1 Au1 C12 143(100) 2_666 . . . ? N1 Pt1 Au1 C11 -45.1(4) 2_666 . . . ? N1 Pt1 Au1 C11 134.9(4) . . . . ? N2 Pt1 Au1 C11 -124.7(4) 2_666 . . . ? N2 Pt1 Au1 C11 55.3(4) . . . . ? Au1 Pt1 Au1 C11 -29(100) 2_666 . . . ? N1 Pt1 Au1 Au1 -148.8(2) 2_666 . . 2_766 ? N1 Pt1 Au1 Au1 31.2(2) . . . 2_766 ? N2 Pt1 Au1 Au1 131.6(2) 2_666 . . 2_766 ? N2 Pt1 Au1 Au1 -48.4(2) . . . 2_766 ? Au1 Pt1 Au1 Au1 -132(100) 2_666 . . 2_766 ? C12 Au1 C11 N3 -26(9) . . . . ? Pt1 Au1 C11 N3 74(7) . . . . ? Au1 Au1 C11 N3 159(7) 2_766 . . . ? C11 Au1 C12 N4 22(9) . . . . ? Pt1 Au1 C12 N4 -78(8) . . . . ? Au1 Au1 C12 N4 -163(8) 2_766 . . . ?
1100710.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100710.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100710 loop_ _publ_author_name 'Jay R. Stork' 'Daniel Rios' 'David Pham' 'Vincent Bicocca' 'Marilyn M. Olmstead' 'Alan L. Balch' _publ_section_title ; Metal-Metal Interactions in Platinum(II)/Gold(I) or Platinum(II)/Silver(I) Salts Containing Planar Cations and Linear Anions ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3466 _journal_page_last 3472 _journal_paper_doi 10.1021/ic048333a _journal_volume 44 _journal_year 2005 _chemical_formula_moiety 'C4 H16 N4 Pt, 2(C2 Au N2)' _chemical_formula_sum 'C8 H16 Au2 N8 Pt' _chemical_formula_weight 813.31 _chemical_name_common '[Pt(en)~2~][Au(CN)~2~]~2~' _chemical_name_systematic ; ? ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 88.311(2) _cell_angle_beta 79.576(2) _cell_angle_gamma 74.306(2) _cell_formula_units_Z 1 _cell_length_a 6.3598(6) _cell_length_b 6.9603(7) _cell_length_c 9.0333(9) _cell_measurement_reflns_used 778 _cell_measurement_temperature 90(2) _cell_measurement_theta_max 30.4 _cell_measurement_theta_min 3.04 _cell_volume 378.53(6) _computing_cell_refinement SAINT _computing_data_collection 'SMART 5.054 (Bruker, 2003)' _computing_data_reduction 'SAINT 6.45A (Bruker, 2003)' _computing_molecular_graphics 'SHELXTL 5.1 (Sheldrick, 1994)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _diffrn_ambient_temperature 90(2) _diffrn_detector_area_resol_mean 8.3 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0320 _diffrn_reflns_av_sigmaI/netI 0.0349 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 5170 _diffrn_reflns_theta_full 28.27 _diffrn_reflns_theta_max 28.27 _diffrn_reflns_theta_min 2.29 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 28.547 _exptl_absorpt_correction_T_max 0.38862 _exptl_absorpt_correction_T_min 0.04242 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS 2.10 (Sheldrick, 2004)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 3.568 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 356 _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _refine_diff_density_max 1.373 _refine_diff_density_min -3.061 _refine_diff_density_rms 0.288 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 91 _refine_ls_number_reflns 1864 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.062 _refine_ls_R_factor_all 0.0205 _refine_ls_R_factor_gt 0.0205 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0235P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0501 _refine_ls_wR_factor_ref 0.0501 _reflns_number_gt 1862 _reflns_number_total 1864 _reflns_threshold_expression I>2\s(I) _cod_data_source_file ic048333asi20041124_041657_4.cif _cod_data_source_block jrs65-2 _cod_database_code 1100710 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.5000 0.5000 0.5000 0.00631(7) Uani 1 2 d S . . C1 C 0.4562(8) 0.6791(6) 0.2066(5) 0.0130(9) Uani 1 1 d . . . H1A H 0.4841 0.7855 0.1368 0.016 Uiso 1 1 calc R . . H1B H 0.3184 0.6488 0.1906 0.016 Uiso 1 1 calc R . . C2 C 0.6493(8) 0.4943(7) 0.1779(5) 0.0121(9) Uani 1 1 d . . . H2A H 0.6609 0.4362 0.0771 0.015 Uiso 1 1 calc R . . H2B H 0.7898 0.5277 0.1824 0.015 Uiso 1 1 calc R . . N1 N 0.4330(6) 0.7453(5) 0.3653(4) 0.0094(7) Uani 1 1 d . . . H1C H 0.2909 0.8233 0.3983 0.011 Uiso 1 1 calc R . . H1D H 0.5299 0.8207 0.3709 0.011 Uiso 1 1 calc R . . N2 N 0.6073(6) 0.3490(5) 0.2974(4) 0.0107(7) Uani 1 1 d . . . H2C H 0.7357 0.2497 0.3003 0.013 Uiso 1 1 calc R . . H2D H 0.5013 0.2913 0.2770 0.013 Uiso 1 1 calc R . . Au1 Au 0.0000 0.5000 0.5000 0.00945(7) Uani 1 2 d S . . C3 C 0.0977(8) 0.2226(7) 0.5720(5) 0.0120(9) Uani 1 1 d . . . N3 N 0.1646(7) 0.0635(6) 0.6129(5) 0.0155(8) Uani 1 1 d . . . Au2 Au 0.0000 0.0000 0.0000 0.01069(7) Uani 1 2 d S . . C4 C 0.1658(8) 0.1475(7) 0.0988(5) 0.0148(9) Uani 1 1 d . . . N4 N 0.2642(8) 0.2282(7) 0.1589(5) 0.0204(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.00663(12) 0.00628(11) 0.00626(12) 0.00043(8) -0.00157(9) -0.00187(8) C1 0.017(2) 0.0095(19) 0.011(2) 0.0018(16) -0.0006(18) -0.0015(17) C2 0.012(2) 0.016(2) 0.008(2) 0.0039(17) -0.0015(17) -0.0037(17) N1 0.0087(17) 0.0084(16) 0.0112(19) 0.0016(14) -0.0018(15) -0.0025(14) N2 0.0123(18) 0.0092(16) 0.0098(18) 0.0013(14) -0.0040(15) -0.0004(14) Au1 0.00812(12) 0.00805(12) 0.01251(13) 0.00159(9) -0.00266(9) -0.00236(9) C3 0.010(2) 0.016(2) 0.011(2) -0.0012(17) 0.0002(18) -0.0054(17) N3 0.016(2) 0.0115(18) 0.019(2) 0.0000(15) -0.0028(17) -0.0034(15) Au2 0.01029(13) 0.01054(12) 0.01106(13) -0.00110(9) -0.00263(9) -0.00191(9) C4 0.016(2) 0.013(2) 0.014(2) -0.0015(17) -0.0027(19) -0.0009(18) N4 0.020(2) 0.021(2) 0.020(2) -0.0021(17) -0.0032(18) -0.0071(18) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Pt1 N2 180.00(11) . 2_666 ? N2 Pt1 N1 82.99(15) . . ? N2 Pt1 N1 97.01(15) 2_666 . ? N2 Pt1 N1 97.01(15) . 2_666 ? N2 Pt1 N1 82.99(15) 2_666 2_666 ? N1 Pt1 N1 180.000(1) . 2_666 ? N2 Pt1 Au1 88.12(11) . 1_655 ? N2 Pt1 Au1 91.88(11) 2_666 1_655 ? N1 Pt1 Au1 95.14(10) . 1_655 ? N1 Pt1 Au1 84.86(10) 2_666 1_655 ? N2 Pt1 Au1 91.88(11) . . ? N2 Pt1 Au1 88.12(11) 2_666 . ? N1 Pt1 Au1 84.86(10) . . ? N1 Pt1 Au1 95.14(10) 2_666 . ? Au1 Pt1 Au1 180.0 1_655 . ? N1 C1 C2 107.4(4) . . ? N1 C1 H1A 110.2 . . ? C2 C1 H1A 110.2 . . ? N1 C1 H1B 110.2 . . ? C2 C1 H1B 110.2 . . ? H1A C1 H1B 108.5 . . ? N2 C2 C1 107.2(4) . . ? N2 C2 H2A 110.3 . . ? C1 C2 H2A 110.3 . . ? N2 C2 H2B 110.3 . . ? C1 C2 H2B 110.3 . . ? H2A C2 H2B 108.5 . . ? C1 N1 Pt1 109.8(3) . . ? C1 N1 H1C 109.7 . . ? Pt1 N1 H1C 109.7 . . ? C1 N1 H1D 109.7 . . ? Pt1 N1 H1D 109.7 . . ? H1C N1 H1D 108.2 . . ? C2 N2 Pt1 108.3(3) . . ? C2 N2 H2C 110.0 . . ? Pt1 N2 H2C 110.0 . . ? C2 N2 H2D 110.0 . . ? Pt1 N2 H2D 110.0 . . ? H2C N2 H2D 108.4 . . ? C3 Au1 C3 180.0(3) . 2_566 ? C3 Au1 Pt1 83.74(13) . . ? C3 Au1 Pt1 96.26(13) 2_566 . ? C3 Au1 Pt1 96.26(13) . 1_455 ? C3 Au1 Pt1 83.74(13) 2_566 1_455 ? Pt1 Au1 Pt1 180.0 . 1_455 ? C3 Au1 N4 77.87(15) . . ? C3 Au1 N4 102.13(15) 2_566 . ? Pt1 Au1 N4 80.11(7) . . ? Pt1 Au1 N4 99.89(7) 1_455 . ? N3 C3 Au1 176.6(4) . . ? C4 Au2 C4 180.0(3) 2 . ? C4 Au2 N3 75.58(16) 2 1_554 ? C4 Au2 N3 104.42(16) . 1_554 ? N4 C4 Au2 177.9(4) . . ? C4 N4 Au1 119.4(4) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 N2 2.048(4) . ? Pt1 N2 2.048(4) 2_666 ? Pt1 N1 2.061(4) . ? Pt1 N1 2.061(4) 2_666 ? Pt1 Au1 3.1799(3) 1_655 ? Pt1 Au1 3.1799(3) . ? C1 N1 1.489(6) . ? C1 C2 1.510(6) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 N2 1.495(6) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? N1 H1C 0.9200 . ? N1 H1D 0.9200 . ? N2 H2C 0.9200 . ? N2 H2D 0.9200 . ? Au1 C3 1.990(5) . ? Au1 C3 1.990(5) 2_566 ? Au1 Pt1 3.1799(3) 1_455 ? Au1 N4 3.556(4) . ? C3 N3 1.150(6) . ? Au2 C4 1.986(5) 2 ? Au2 C4 1.986(5) . ? Au2 N3 3.515(4) 1_554 ? C4 N4 1.154(6) . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1C N3 0.92 2.47 3.112(6) 127.1 1_565 N1 H1D N3 0.92 2.32 3.225(5) 166.2 2_666 N2 H2C N3 0.92 2.26 3.007(5) 138.1 2_656 N2 H2D N4 0.92 2.14 3.013(6) 158.4 . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 N2 53.8(4) . . . . ? C2 C1 N1 Pt1 -37.3(4) . . . . ? N2 Pt1 N1 C1 10.4(3) . . . . ? N2 Pt1 N1 C1 -169.6(3) 2_666 . . . ? N1 Pt1 N1 C1 -124(100) 2_666 . . . ? Au1 Pt1 N1 C1 97.9(3) 1_655 . . . ? Au1 Pt1 N1 C1 -82.1(3) . . . . ? C1 C2 N2 Pt1 -44.4(4) . . . . ? N2 Pt1 N2 C2 80(100) 2_666 . . . ? N1 Pt1 N2 C2 18.9(3) . . . . ? N1 Pt1 N2 C2 -161.1(3) 2_666 . . . ? Au1 Pt1 N2 C2 -76.6(3) 1_655 . . . ? Au1 Pt1 N2 C2 103.4(3) . . . . ? N2 Pt1 Au1 C3 80.43(17) . . . . ? N2 Pt1 Au1 C3 -99.57(17) 2_666 . . . ? N1 Pt1 Au1 C3 163.22(18) . . . . ? N1 Pt1 Au1 C3 -16.78(18) 2_666 . . . ? Au1 Pt1 Au1 C3 0.0 1_655 . . . ? N2 Pt1 Au1 C3 -99.57(17) . . . 2_566 ? N2 Pt1 Au1 C3 80.43(17) 2_666 . . 2_566 ? N1 Pt1 Au1 C3 -16.78(18) . . . 2_566 ? N1 Pt1 Au1 C3 163.22(18) 2_666 . . 2_566 ? Au1 Pt1 Au1 C3 0.0 1_655 . . 2_566 ? N2 Pt1 Au1 Pt1 0.0 . . . 1_455 ? N2 Pt1 Au1 Pt1 0.0 2_666 . . 1_455 ? N1 Pt1 Au1 Pt1 0.0 . . . 1_455 ? N1 Pt1 Au1 Pt1 0.0 2_666 . . 1_455 ? Au1 Pt1 Au1 Pt1 0.0 1_655 . . 1_455 ? N2 Pt1 Au1 N4 1.70(12) . . . . ? N2 Pt1 Au1 N4 -178.30(12) 2_666 . . . ? N1 Pt1 Au1 N4 84.49(13) . . . . ? N1 Pt1 Au1 N4 -95.51(13) 2_666 . . . ? Au1 Pt1 Au1 N4 0.0 1_655 . . . ? C3 Au1 C3 N3 75(100) 2_566 . . . ? Pt1 Au1 C3 N3 -3(7) . . . . ? Pt1 Au1 C3 N3 177(7) 1_455 . . . ? N4 Au1 C3 N3 78(7) . . . . ? C4 Au2 C4 N4 7(70) 2 . . . ? N3 Au2 C4 N4 -132(12) 1_554 . . . ? Au2 C4 N4 Au1 -87(12) . . . . ? C3 Au1 N4 C4 83.5(4) . . . . ? C3 Au1 N4 C4 -96.5(4) 2_566 . . . ? Pt1 Au1 N4 C4 169.1(4) . . . . ? Pt1 Au1 N4 C4 -10.9(4) 1_455 . . . ?
1100711.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100711.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100711 loop_ _publ_author_name 'Jay R. Stork' 'Daniel Rios' 'David Pham' 'Vincent Bicocca' 'Marilyn M. Olmstead' 'Alan L. Balch' _publ_section_title ; Metal-Metal Interactions in Platinum(II)/Gold(I) or Platinum(II)/Silver(I) Salts Containing Planar Cations and Linear Anions ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3466 _journal_page_last 3472 _journal_paper_doi 10.1021/ic048333a _journal_volume 44 _journal_year 2005 _chemical_formula_moiety 'C4 H16 N4 Pt, 2(C2 Ag N2)' _chemical_formula_sum 'C8 H16 Ag2 N8 Pt' _chemical_formula_weight 635.12 _chemical_name_common '[Pt(en)~2~][Ag(CN)~2~]~2~' _chemical_name_systematic ; ? ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 89.0260(10) _cell_angle_beta 79.6310(10) _cell_angle_gamma 73.7160(10) _cell_formula_units_Z 1 _cell_length_a 6.3899(4) _cell_length_b 6.9793(5) _cell_length_c 8.9383(6) _cell_measurement_reflns_used 1022 _cell_measurement_temperature 90(2) _cell_measurement_theta_max 30.5 _cell_measurement_theta_min 3.73 _cell_volume 376.15(4) _computing_cell_refinement SAINT _computing_data_collection 'SMART 5.054 (Bruker, 2003)' _computing_data_reduction 'SAINT 6.45A (Bruker, 2003)' _computing_molecular_graphics 'SHELXTL 5.1 (Sheldrick, 1994)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _diffrn_ambient_temperature 90(2) _diffrn_detector_area_resol_mean 8.3 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0158 _diffrn_reflns_av_sigmaI/netI 0.0168 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 5148 _diffrn_reflns_theta_full 28.27 _diffrn_reflns_theta_max 28.27 _diffrn_reflns_theta_min 3.04 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 11.851 _exptl_absorpt_correction_T_max 0.49946 _exptl_absorpt_correction_T_min 0.07528 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS 2.10 (Sheldrick, 2004)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 2.804 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 292 _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.07 _refine_diff_density_max 1.102 _refine_diff_density_min -1.422 _refine_diff_density_rms 0.145 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 91 _refine_ls_number_reflns 1851 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.056 _refine_ls_R_factor_all 0.0151 _refine_ls_R_factor_gt 0.0151 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0257P)^2^+0.1966P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0391 _refine_ls_wR_factor_ref 0.0391 _reflns_number_gt 1850 _reflns_number_total 1851 _reflns_threshold_expression I>2\s(I) _cod_data_source_file ic048333asi20041124_041657_5.cif _cod_data_source_block jrs67 _cod_database_code 1100711 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.5000 0.5000 0.5000 0.00713(5) Uani 1 2 d S . . C1 C 0.4548(5) 0.6887(4) 0.2083(3) 0.0122(5) Uani 1 1 d . . . H1A H 0.4824 0.7970 0.1415 0.015 Uiso 1 1 calc R . . H1B H 0.3184 0.6601 0.1895 0.015 Uiso 1 1 calc R . . C2 C 0.6495(5) 0.5034(4) 0.1755(3) 0.0123(5) Uani 1 1 d . . . H2A H 0.6628 0.4485 0.0717 0.015 Uiso 1 1 calc R . . H2B H 0.7888 0.5355 0.1826 0.015 Uiso 1 1 calc R . . N1 N 0.4289(4) 0.7500(3) 0.3717(3) 0.0103(4) Uani 1 1 d . . . H1C H 0.2860 0.8267 0.4064 0.012 Uiso 1 1 calc R . . H1D H 0.5233 0.8256 0.3810 0.012 Uiso 1 1 calc R . . N2 N 0.6081(4) 0.3557(3) 0.2907(3) 0.0105(4) Uani 1 1 d . . . H2C H 0.7365 0.2548 0.2913 0.013 Uiso 1 1 calc R . . H2D H 0.5026 0.3003 0.2675 0.013 Uiso 1 1 calc R . . Ag1 Ag 0.0000 0.5000 0.5000 0.01431(7) Uani 1 2 d S . . C3 C 0.0949(5) 0.2180(4) 0.5864(3) 0.0145(5) Uani 1 1 d . . . N3 N 0.1621(4) 0.0638(4) 0.6337(3) 0.0162(5) Uani 1 1 d . . . Ag2 Ag 0.0000 0.0000 0.0000 0.01406(7) Uani 1 2 d S . . C4 C 0.1621(5) 0.1635(4) 0.1035(3) 0.0143(5) Uani 1 1 d . . . N4 N 0.2524(5) 0.2493(4) 0.1655(3) 0.0197(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.00725(7) 0.00657(7) 0.00791(8) 0.00043(4) -0.00224(5) -0.00199(5) C1 0.0133(13) 0.0131(12) 0.0090(12) 0.0008(9) -0.0028(10) -0.0010(10) C2 0.0130(13) 0.0106(12) 0.0111(12) 0.0010(9) -0.0008(10) -0.0004(10) N1 0.0115(11) 0.0091(10) 0.0103(11) 0.0009(8) -0.0030(9) -0.0025(8) N2 0.0116(11) 0.0076(10) 0.0115(11) 0.0000(8) -0.0021(9) -0.0013(8) Ag1 0.01235(15) 0.01122(14) 0.02146(16) 0.00635(11) -0.00698(12) -0.00458(11) C3 0.0105(13) 0.0140(13) 0.0186(14) 0.0005(10) -0.0013(10) -0.0039(10) N3 0.0142(12) 0.0140(11) 0.0202(12) 0.0020(9) -0.0029(10) -0.0037(9) Ag2 0.01254(15) 0.01230(14) 0.01794(15) -0.00244(11) -0.00472(11) -0.00308(11) C4 0.0127(13) 0.0126(12) 0.0168(13) 0.0020(10) -0.0024(10) -0.0024(10) N4 0.0193(13) 0.0221(13) 0.0206(13) 0.0009(10) -0.0058(10) -0.0092(10) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Pt1 N2 180.00(7) 2_666 . ? N2 Pt1 N1 97.01(9) 2_666 . ? N2 Pt1 N1 82.99(9) . . ? N2 Pt1 N1 82.99(9) 2_666 2_666 ? N2 Pt1 N1 97.01(9) . 2_666 ? N1 Pt1 N1 180.0 . 2_666 ? N2 Pt1 Ag1 92.00(7) 2_666 1_655 ? N2 Pt1 Ag1 88.00(7) . 1_655 ? N1 Pt1 Ag1 94.77(7) . 1_655 ? N1 Pt1 Ag1 85.23(7) 2_666 1_655 ? N2 Pt1 Ag1 88.00(7) 2_666 . ? N2 Pt1 Ag1 92.00(7) . . ? N1 Pt1 Ag1 85.23(7) . . ? N1 Pt1 Ag1 94.77(7) 2_666 . ? Ag1 Pt1 Ag1 180.0 1_655 . ? N1 C1 C2 107.4(2) . . ? N1 C1 H1A 110.2 . . ? C2 C1 H1A 110.2 . . ? N1 C1 H1B 110.2 . . ? C2 C1 H1B 110.2 . . ? H1A C1 H1B 108.5 . . ? N2 C2 C1 107.2(2) . . ? N2 C2 H2A 110.3 . . ? C1 C2 H2A 110.3 . . ? N2 C2 H2B 110.3 . . ? C1 C2 H2B 110.3 . . ? H2A C2 H2B 108.5 . . ? C1 N1 Pt1 109.70(16) . . ? C1 N1 H1C 109.7 . . ? Pt1 N1 H1C 109.7 . . ? C1 N1 H1D 109.7 . . ? Pt1 N1 H1D 109.7 . . ? H1C N1 H1D 108.2 . . ? C2 N2 Pt1 108.44(16) . . ? C2 N2 H2C 110.0 . . ? Pt1 N2 H2C 110.0 . . ? C2 N2 H2D 110.0 . . ? Pt1 N2 H2D 110.0 . . ? H2C N2 H2D 108.4 . . ? C3 Ag1 C3 180.0 . 2_566 ? C3 Ag1 Pt1 84.64(8) . . ? C3 Ag1 Pt1 95.36(8) 2_566 . ? C3 Ag1 Pt1 95.36(8) . 1_455 ? C3 Ag1 Pt1 84.64(8) 2_566 1_455 ? Pt1 Ag1 Pt1 180.0 . 1_455 ? C3 Ag1 N4 82.63(9) . . ? C3 Ag1 N4 97.37(9) 2_566 . ? Pt1 Ag1 N4 80.06(5) . . ? Pt1 Ag1 N4 99.94(5) 1_455 . ? N3 C3 Ag1 175.1(3) . . ? C3 N3 Ag2 66.4(2) . 1_554 ? C4 Ag2 C4 180.00(11) 2 . ? N4 C4 Ag2 177.4(3) . . ? C4 N4 Ag1 120.7(2) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 N2 2.049(2) 2_666 ? Pt1 N2 2.049(2) . ? Pt1 N1 2.060(2) . ? Pt1 N1 2.060(2) 2_666 ? Pt1 Ag1 3.1949(2) 1_655 ? Pt1 Ag1 3.1950(2) . ? C1 N1 1.496(3) . ? C1 C2 1.512(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 N2 1.487(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? N1 H1C 0.9200 . ? N1 H1D 0.9200 . ? N2 H2C 0.9200 . ? N2 H2D 0.9200 . ? Ag1 C3 2.070(3) . ? Ag1 C3 2.070(3) 2_566 ? Ag1 Pt1 3.1949(2) 1_455 ? Ag1 N4 3.385(3) . ? C3 N3 1.145(4) . ? N3 Ag2 14.846(3) 1_554 ? Ag2 C4 2.067(3) 2 ? Ag2 C4 2.067(3) . ? C4 N4 1.149(4) . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1C N3 0.92 2.51 3.135(3) 125.6 1_565 N1 H1D N3 0.92 2.33 3.221(4) 163.3 2_666 N2 H2C N3 0.92 2.26 3.011(3) 138.3 2_656 N2 H2D N4 0.92 2.09 2.976(4) 161.5 . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 N2 53.7(3) . . . . ? C2 C1 N1 Pt1 -36.7(3) . . . . ? N2 Pt1 N1 C1 -170.21(18) 2_666 . . . ? N2 Pt1 N1 C1 9.79(18) . . . . ? N1 Pt1 N1 C1 -56(100) 2_666 . . . ? Ag1 Pt1 N1 C1 97.18(17) 1_655 . . . ? Ag1 Pt1 N1 C1 -82.82(17) . . . . ? C1 C2 N2 Pt1 -44.9(2) . . . . ? N2 Pt1 N2 C2 117(100) 2_666 . . . ? N1 Pt1 N2 C2 19.51(18) . . . . ? N1 Pt1 N2 C2 -160.49(18) 2_666 . . . ? Ag1 Pt1 N2 C2 -75.55(17) 1_655 . . . ? Ag1 Pt1 N2 C2 104.45(17) . . . . ? N2 Pt1 Ag1 C3 -94.49(10) 2_666 . . . ? N2 Pt1 Ag1 C3 85.51(10) . . . . ? N1 Pt1 Ag1 C3 168.30(10) . . . . ? N1 Pt1 Ag1 C3 -11.70(10) 2_666 . . . ? Ag1 Pt1 Ag1 C3 0.0 1_655 . . . ? N2 Pt1 Ag1 C3 85.51(10) 2_666 . . 2_566 ? N2 Pt1 Ag1 C3 -94.49(10) . . . 2_566 ? N1 Pt1 Ag1 C3 -11.70(10) . . . 2_566 ? N1 Pt1 Ag1 C3 168.30(10) 2_666 . . 2_566 ? Ag1 Pt1 Ag1 C3 0.0 1_655 . . 2_566 ? N2 Pt1 Ag1 Pt1 0.0 2_666 . . 1_455 ? N2 Pt1 Ag1 Pt1 0.0 . . . 1_455 ? N1 Pt1 Ag1 Pt1 0.0 . . . 1_455 ? N1 Pt1 Ag1 Pt1 0.0 2_666 . . 1_455 ? Ag1 Pt1 Ag1 Pt1 0.0 1_655 . . 1_455 ? N2 Pt1 Ag1 N4 -177.92(8) 2_666 . . . ? N2 Pt1 Ag1 N4 2.08(8) . . . . ? N1 Pt1 Ag1 N4 84.87(8) . . . . ? N1 Pt1 Ag1 N4 -95.13(8) 2_666 . . . ? Ag1 Pt1 Ag1 N4 0.0 1_655 . . . ? C3 Ag1 C3 N3 -146(100) 2_566 . . . ? Pt1 Ag1 C3 N3 0(3) . . . . ? Pt1 Ag1 C3 N3 180(100) 1_455 . . . ? N4 Ag1 C3 N3 80(3) . . . . ? Ag1 C3 N3 Ag2 -102(3) . . . 1_554 ? C4 Ag2 C4 N4 32(100) 2 . . . ? Ag2 C4 N4 Ag1 -67(6) . . . . ? C3 Ag1 N4 C4 80.6(3) . . . . ? C3 Ag1 N4 C4 -99.4(3) 2_566 . . . ? Pt1 Ag1 N4 C4 166.4(3) . . . . ? Pt1 Ag1 N4 C4 -13.6(3) 1_455 . . . ?
1100712.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100712.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100712 loop_ _publ_author_name 'Leslie W. Pineda' 'Vojtech Jancik' 'Herbert W. Roesky' 'Regine Herbst-Irmer' _publ_contact_author_address ; Institut f\"ur Anorganische Chemie, Georg-August-Universit\"at G\"ottingen, Tammannstrasse 4, D 37077 G\"ottingen, Germany ; _publ_contact_author_email hroesky@gwdg.de _publ_contact_author_name 'Herbert W. Roesky' _publ_section_title ; OH Functionality of Germanium(II) Compounds for the Formation of Heterobimetallic Oxides ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3537 _journal_page_last 3540 _journal_paper_doi 10.1021/ic048383f _journal_volume 44 _journal_year 2005 _chemical_formula_moiety LGe(m-O)ZrCp2Me _chemical_formula_sum 'C40 H54 Ge N2 O Zr' _chemical_formula_weight 742.66 _chemical_name_systematic ; ? ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 88.64(1) _cell_angle_beta 89.60(1) _cell_angle_gamma 67.44(1) _cell_formula_units_Z 2 _cell_length_a 9.444(1) _cell_length_b 10.522(1) _cell_length_c 19.750(1) _cell_measurement_reflns_used 5044 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 58.96 _cell_measurement_theta_min 2.24 _cell_volume 1811.9(3) _computing_cell_refinement 'Bruker AXS SAINT (v 7.01A, Bruker 2003)' _computing_data_collection 'Proteum (v 1.40, Bruker 2002)' _computing_data_reduction 'Bruker AXS SAINT (v 7.01A, Bruker 2003)' _computing_molecular_graphics 'Bruker AXS SHELXTL (v 6.12)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 5.602 _diffrn_measured_fraction_theta_full 0.966 _diffrn_measured_fraction_theta_max 0.966 _diffrn_measurement_device_type 'Bruker three circle diffractometer' _diffrn_measurement_method 'phi and omega scan' _diffrn_radiation_monochromator 'mirror system' _diffrn_radiation_source 'rotating anode' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0265 _diffrn_reflns_av_sigmaI/netI 0.0284 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 14140 _diffrn_reflns_theta_full 58.96 _diffrn_reflns_theta_max 58.96 _diffrn_reflns_theta_min 2.24 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 3.617 _exptl_absorpt_correction_T_max 0.8992 _exptl_absorpt_correction_T_min 0.7137 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.361 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 776 _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _refine_diff_density_max 1.232 _refine_diff_density_min -0.553 _refine_diff_density_rms 0.062 _refine_ls_extinction_coef 0.00036(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 421 _refine_ls_number_reflns 5044 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.062 _refine_ls_R_factor_all 0.0297 _refine_ls_R_factor_gt 0.0288 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0306P)^2^+2.5234P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0728 _refine_ls_wR_factor_ref 0.0735 _reflns_number_gt 4879 _reflns_number_total 5044 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic048383fsi20041122_032909_2.cif _cod_data_source_block LGem-OZrCp2Me _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'TRICLINIC' changed to 'triclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_cell_volume 1812(1) _cod_database_code 1100712 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr -0.14748(3) 0.92344(2) 0.239776(11) 0.02037(10) Uani 1 1 d . . . Ge1 Ge 0.26023(3) 0.78468(3) 0.251684(14) 0.01964(11) Uani 1 1 d . . . N1 N 0.3612(2) 0.6265(2) 0.18811(10) 0.0194(5) Uani 1 1 d . . . O1 O 0.0661(2) 0.79553(19) 0.24598(9) 0.0242(4) Uani 1 1 d . . . C1 C 0.5647(3) 0.4803(3) 0.39116(13) 0.0236(6) Uani 1 1 d . . . H1A H 0.4913 0.4973 0.4285 0.035 Uiso 0.50 1 calc PR . . H1B H 0.6446 0.5139 0.4030 0.035 Uiso 0.50 1 calc PR . . H1C H 0.6117 0.3813 0.3830 0.035 Uiso 0.50 1 calc PR . . H1D H 0.6737 0.4311 0.3812 0.035 Uiso 0.50 1 calc PR . . H1E H 0.5204 0.4144 0.4067 0.035 Uiso 0.50 1 calc PR . . H1F H 0.5533 0.5470 0.4266 0.035 Uiso 0.50 1 calc PR . . N2 N 0.3370(2) 0.6419(2) 0.33005(10) 0.0183(5) Uani 1 1 d . . . C2 C 0.4822(3) 0.5550(3) 0.32784(13) 0.0187(6) Uani 1 1 d . . . C3 C 0.5663(3) 0.5267(3) 0.26735(13) 0.0194(6) Uani 1 1 d . . . H3A H 0.664(4) 0.476(3) 0.2714(15) 0.023 Uiso 1 1 d . . . C4 C 0.5076(3) 0.5491(3) 0.20125(13) 0.0189(6) Uani 1 1 d . . . C5 C 0.6165(3) 0.4840(3) 0.14429(13) 0.0252(6) Uani 1 1 d . . . H5A H 0.5629 0.4545 0.1095 0.038 Uiso 1 1 calc R . . H5B H 0.7032 0.4041 0.1619 0.038 Uiso 1 1 calc R . . H5C H 0.6543 0.5513 0.1244 0.038 Uiso 1 1 calc R . . C6 C 0.2942(3) 0.6236(3) 0.12282(13) 0.0208(6) Uani 1 1 d . . . C7 C 0.2944(3) 0.7176(3) 0.07119(13) 0.0234(6) Uani 1 1 d . . . C8 C 0.2188(3) 0.7160(3) 0.01059(14) 0.0291(7) Uani 1 1 d . . . H8A H 0.2135 0.7811 -0.0244 0.035 Uiso 1 1 calc R . . C9 C 0.1522(3) 0.6227(3) 0.00064(14) 0.0307(7) Uani 1 1 d . . . H9A H 0.1027 0.6231 -0.0411 0.037 Uiso 1 1 calc R . . C10 C 0.1570(3) 0.5280(3) 0.05131(14) 0.0270(6) Uani 1 1 d . . . H10A H 0.1129 0.4622 0.0434 0.032 Uiso 1 1 calc R . . C11 C 0.2256(3) 0.5274(3) 0.11385(13) 0.0228(6) Uani 1 1 d . . . C12 C 0.2260(3) 0.4253(3) 0.16999(14) 0.0255(6) Uani 1 1 d . . . H12A H 0.2120 0.4739 0.2139 0.031 Uiso 1 1 calc R . . C13 C 0.0969(4) 0.3718(3) 0.16389(16) 0.0351(7) Uani 1 1 d . . . H13A H 0.0001 0.4491 0.1539 0.053 Uiso 1 1 calc R . . H13B H 0.0874 0.3265 0.2066 0.053 Uiso 1 1 calc R . . H13C H 0.1206 0.3057 0.1273 0.053 Uiso 1 1 calc R . . C14 C 0.3777(4) 0.2999(3) 0.17425(16) 0.0347(7) Uani 1 1 d . . . H14A H 0.4616 0.3302 0.1833 0.052 Uiso 1 1 calc R . . H14B H 0.3963 0.2515 0.1313 0.052 Uiso 1 1 calc R . . H14C H 0.3721 0.2376 0.2110 0.052 Uiso 1 1 calc R . . C15 C 0.3790(3) 0.8139(3) 0.07656(13) 0.0261(6) Uani 1 1 d . . . H15A H 0.4360 0.7931 0.1206 0.031 Uiso 1 1 calc R . . C16 C 0.4972(4) 0.7878(3) 0.01904(14) 0.0326(7) Uani 1 1 d . . . H16A H 0.5665 0.6906 0.0201 0.049 Uiso 1 1 calc R . . H16B H 0.5565 0.8454 0.0251 0.049 Uiso 1 1 calc R . . H16C H 0.4437 0.8108 -0.0246 0.049 Uiso 1 1 calc R . . C17 C 0.2706(4) 0.9653(3) 0.07593(15) 0.0352(7) Uani 1 1 d . . . H17A H 0.2036 0.9830 0.1157 0.053 Uiso 1 1 calc R . . H17B H 0.2081 0.9867 0.0346 0.053 Uiso 1 1 calc R . . H17C H 0.3306 1.0234 0.0771 0.053 Uiso 1 1 calc R . . C18 C 0.2531(3) 0.6727(3) 0.39271(12) 0.0188(6) Uani 1 1 d . . . C19 C 0.1388(3) 0.6193(3) 0.40480(13) 0.0205(6) Uani 1 1 d . . . C20 C 0.0532(3) 0.6561(3) 0.46422(13) 0.0238(6) Uani 1 1 d . . . H20A H -0.0239 0.6210 0.4735 0.029 Uiso 1 1 calc R . . C21 C 0.0789(3) 0.7429(3) 0.50986(13) 0.0246(6) Uani 1 1 d . . . H21A H 0.0199 0.7663 0.5502 0.029 Uiso 1 1 calc R . . C22 C 0.1896(3) 0.7954(3) 0.49707(13) 0.0229(6) Uani 1 1 d . . . H22A H 0.2060 0.8547 0.5288 0.027 Uiso 1 1 calc R . . C23 C 0.2782(3) 0.7629(3) 0.43816(13) 0.0204(6) Uani 1 1 d . . . C24 C 0.3941(3) 0.8291(3) 0.42555(13) 0.0235(6) Uani 1 1 d . . . H24A H 0.4521 0.7896 0.3834 0.028 Uiso 1 1 calc R . . C25 C 0.5098(4) 0.7984(3) 0.48390(14) 0.0318(7) Uani 1 1 d . . . H25A H 0.5630 0.6986 0.4901 0.048 Uiso 1 1 calc R . . H25B H 0.4555 0.8375 0.5257 0.048 Uiso 1 1 calc R . . H25C H 0.5846 0.8396 0.4732 0.048 Uiso 1 1 calc R . . C26 C 0.3116(4) 0.9850(3) 0.41394(15) 0.0324(7) Uani 1 1 d . . . H26A H 0.2433 1.0029 0.3746 0.049 Uiso 1 1 calc R . . H26B H 0.3875 1.0261 0.4056 0.049 Uiso 1 1 calc R . . H26C H 0.2513 1.0256 0.4541 0.049 Uiso 1 1 calc R . . C27 C 0.1125(3) 0.5234(3) 0.35456(13) 0.0235(6) Uani 1 1 d . . . H27A H 0.1284 0.5554 0.3081 0.028 Uiso 1 1 calc R . . C28 C -0.0500(3) 0.5243(3) 0.35706(15) 0.0295(7) Uani 1 1 d . . . H28A H -0.1248 0.6190 0.3513 0.044 Uiso 1 1 calc R . . H28B H -0.0664 0.4864 0.4009 0.044 Uiso 1 1 calc R . . H28C H -0.0630 0.4681 0.3206 0.044 Uiso 1 1 calc R . . C29 C 0.2294(3) 0.3752(3) 0.36466(15) 0.0306(7) Uani 1 1 d . . . H29A H 0.3332 0.3728 0.3577 0.046 Uiso 1 1 calc R . . H29B H 0.2090 0.3156 0.3320 0.046 Uiso 1 1 calc R . . H29C H 0.2206 0.3425 0.4108 0.046 Uiso 1 1 calc R . . C30 C -0.1172(4) 1.0793(3) 0.16446(16) 0.0363(7) Uani 1 1 d . . . H30A H -0.0738 1.0333 0.1222 0.055 Uiso 1 1 calc R . . H30B H -0.0478 1.1184 0.1837 0.055 Uiso 1 1 calc R . . H30C H -0.2171 1.1532 0.1551 0.055 Uiso 1 1 calc R . . C31 C -0.1727(4) 0.7859(4) 0.14037(16) 0.0402(8) Uani 1 1 d . . . H31A H -0.0889 0.7532 0.1098 0.048 Uiso 1 1 calc R . . C32 C -0.1926(4) 0.7177(3) 0.19842(17) 0.0396(8) Uani 1 1 d . . . H32A H -0.1251 0.6293 0.2141 0.047 Uiso 1 1 calc R . . C33 C -0.3286(4) 0.8008(3) 0.22983(18) 0.0419(8) Uani 1 1 d . . . H33A H -0.3686 0.7797 0.2710 0.050 Uiso 1 1 calc R . . C34 C -0.3957(4) 0.9210(3) 0.18977(18) 0.0399(8) Uani 1 1 d . . . H34A H -0.4901 0.9950 0.1985 0.048 Uiso 1 1 calc R . . C35 C -0.2990(4) 0.9124(4) 0.13487(17) 0.0431(9) Uani 1 1 d . . . H35A H -0.3154 0.9801 0.0999 0.052 Uiso 1 1 calc R . . C36 C -0.3495(4) 1.0635(3) 0.32486(15) 0.0383(8) Uani 1 1 d . . . H36A H -0.4536 1.0763 0.3178 0.046 Uiso 1 1 calc R . . C37 C -0.2798(4) 1.1505(3) 0.30176(15) 0.0360(8) Uani 1 1 d . . . H37A H -0.3274 1.2324 0.2753 0.043 Uiso 1 1 calc R . . C38 C -0.1256(4) 1.0965(3) 0.32432(15) 0.0344(7) Uani 1 1 d . . . H38A H -0.0513 1.1353 0.3156 0.041 Uiso 1 1 calc R . . C39 C -0.1023(4) 0.9754(3) 0.36177(14) 0.0315(7) Uani 1 1 d . . . H39A H -0.0100 0.9187 0.3840 0.038 Uiso 1 1 calc R . . C40 C -0.2389(4) 0.9524(3) 0.36081(14) 0.0352(7) Uani 1 1 d . . . H40A H -0.2544 0.8758 0.3808 0.042 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr1 0.02375(15) 0.01792(15) 0.01557(14) 0.00181(9) -0.00204(9) -0.00380(10) Ge1 0.02700(19) 0.01648(18) 0.01192(17) 0.00079(12) -0.00216(12) -0.00446(13) N1 0.0254(12) 0.0201(12) 0.0110(11) 0.0006(9) -0.0020(9) -0.0068(10) O1 0.0284(10) 0.0230(10) 0.0164(9) 0.0027(7) -0.0027(8) -0.0049(8) C1 0.0277(15) 0.0236(15) 0.0155(14) 0.0023(11) -0.0047(11) -0.0052(12) N2 0.0246(12) 0.0173(11) 0.0113(10) 0.0007(8) -0.0024(9) -0.0061(9) C2 0.0244(14) 0.0161(14) 0.0156(13) 0.0004(10) -0.0038(11) -0.0077(11) C3 0.0210(14) 0.0159(14) 0.0180(14) 0.0020(11) -0.0028(11) -0.0035(11) C4 0.0263(15) 0.0140(13) 0.0163(13) 0.0005(10) -0.0002(11) -0.0075(11) C5 0.0271(15) 0.0277(16) 0.0164(14) -0.0008(11) -0.0003(11) -0.0057(12) C6 0.0236(14) 0.0219(15) 0.0121(13) -0.0024(11) -0.0010(11) -0.0031(11) C7 0.0265(15) 0.0254(15) 0.0130(13) -0.0017(11) 0.0002(11) -0.0039(12) C8 0.0334(16) 0.0358(17) 0.0138(14) 0.0040(12) -0.0029(12) -0.0087(13) C9 0.0328(16) 0.0425(19) 0.0144(14) -0.0029(13) -0.0053(12) -0.0115(14) C10 0.0294(15) 0.0318(17) 0.0193(14) -0.0061(12) -0.0008(12) -0.0107(13) C11 0.0248(14) 0.0233(15) 0.0168(14) -0.0041(11) -0.0003(11) -0.0050(12) C12 0.0342(16) 0.0247(15) 0.0178(14) -0.0026(11) -0.0023(12) -0.0115(13) C13 0.0420(18) 0.0337(18) 0.0327(17) 0.0009(13) -0.0027(14) -0.0180(15) C14 0.0416(18) 0.0297(17) 0.0311(17) 0.0062(13) -0.0065(14) -0.0119(14) C15 0.0359(16) 0.0284(16) 0.0129(13) 0.0033(11) -0.0005(12) -0.0114(13) C16 0.0407(18) 0.0374(18) 0.0202(15) 0.0041(13) 0.0019(13) -0.0158(14) C17 0.0459(19) 0.0301(17) 0.0273(16) 0.0024(13) 0.0016(14) -0.0121(14) C18 0.0249(14) 0.0164(14) 0.0105(12) 0.0038(10) -0.0028(10) -0.0028(11) C19 0.0257(14) 0.0180(14) 0.0146(13) 0.0066(10) -0.0047(11) -0.0051(11) C20 0.0275(15) 0.0256(15) 0.0166(14) 0.0067(11) -0.0008(11) -0.0087(12) C21 0.0311(15) 0.0257(15) 0.0122(13) 0.0040(11) 0.0017(11) -0.0061(12) C22 0.0308(15) 0.0210(15) 0.0130(13) 0.0000(11) -0.0033(11) -0.0055(12) C23 0.0254(14) 0.0188(14) 0.0136(13) 0.0034(10) -0.0040(11) -0.0048(11) C24 0.0319(15) 0.0260(16) 0.0140(13) -0.0015(11) -0.0012(11) -0.0126(12) C25 0.0363(17) 0.0429(19) 0.0206(15) -0.0029(13) -0.0030(13) -0.0198(14) C26 0.0437(18) 0.0280(17) 0.0283(16) 0.0010(13) -0.0008(13) -0.0170(14) C27 0.0321(15) 0.0241(15) 0.0157(13) 0.0035(11) -0.0027(11) -0.0124(12) C28 0.0351(17) 0.0311(17) 0.0245(15) 0.0054(12) -0.0063(13) -0.0153(13) C29 0.0354(17) 0.0237(16) 0.0326(17) -0.0004(13) -0.0063(13) -0.0113(13) C30 0.0431(19) 0.0309(17) 0.0297(17) 0.0080(13) 0.0035(14) -0.0088(14) C31 0.0390(19) 0.046(2) 0.0309(18) -0.0145(15) -0.0087(14) -0.0099(16) C32 0.046(2) 0.0244(17) 0.045(2) -0.0030(14) -0.0184(16) -0.0094(15) C33 0.044(2) 0.038(2) 0.050(2) -0.0010(16) -0.0065(16) -0.0225(16) C34 0.0279(17) 0.0338(19) 0.054(2) -0.0085(16) -0.0158(15) -0.0072(14) C35 0.055(2) 0.040(2) 0.0333(18) 0.0065(15) -0.0242(17) -0.0169(17) C36 0.0318(17) 0.043(2) 0.0265(16) -0.0060(14) 0.0041(13) 0.0009(15) C37 0.050(2) 0.0210(16) 0.0228(16) -0.0038(12) -0.0021(14) 0.0023(14) C38 0.049(2) 0.0295(17) 0.0234(16) -0.0061(13) -0.0025(14) -0.0130(14) C39 0.0377(18) 0.0281(17) 0.0157(14) -0.0038(12) -0.0033(12) 0.0022(13) C40 0.048(2) 0.0327(18) 0.0202(15) 0.0009(13) 0.0069(14) -0.0098(15) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ge Ge -1.0885 0.8855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -0.1862 2.2449 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zr1 C30 98.52(10) . . ? O1 Zr1 C32 84.07(9) . . ? C30 Zr1 C32 120.47(12) . . ? O1 Zr1 C33 112.17(10) . . ? C30 Zr1 C33 127.16(12) . . ? C32 Zr1 C33 32.22(11) . . ? O1 Zr1 C40 104.36(9) . . ? C30 Zr1 C40 130.16(11) . . ? C32 Zr1 C40 105.62(11) . . ? C33 Zr1 C40 83.31(12) . . ? O1 Zr1 C31 86.98(9) . . ? C30 Zr1 C31 88.58(12) . . ? C32 Zr1 C31 31.92(11) . . ? C33 Zr1 C31 53.21(12) . . ? C40 Zr1 C31 135.66(12) . . ? O1 Zr1 C35 117.45(10) . . ? C30 Zr1 C35 75.08(12) . . ? C32 Zr1 C35 52.86(11) . . ? C33 Zr1 C35 52.94(12) . . ? C40 Zr1 C35 127.41(12) . . ? C31 Zr1 C35 32.12(11) . . ? O1 Zr1 C39 83.31(9) . . ? C30 Zr1 C39 111.72(11) . . ? C32 Zr1 C39 127.52(11) . . ? C33 Zr1 C39 113.64(11) . . ? C40 Zr1 C39 32.00(11) . . ? C31 Zr1 C39 158.56(11) . . ? C35 Zr1 C39 157.69(11) . . ? O1 Zr1 C34 136.26(9) . . ? C30 Zr1 C34 97.23(12) . . ? C32 Zr1 C34 52.96(11) . . ? C33 Zr1 C34 32.10(11) . . ? C40 Zr1 C34 95.80(11) . . ? C31 Zr1 C34 52.92(11) . . ? C35 Zr1 C34 31.65(12) . . ? C39 Zr1 C34 127.06(11) . . ? O1 Zr1 C36 134.94(9) . . ? C30 Zr1 C36 106.18(11) . . ? C32 Zr1 C36 112.98(12) . . ? C33 Zr1 C36 81.67(12) . . ? C40 Zr1 C36 32.28(10) . . ? C31 Zr1 C36 129.88(11) . . ? C35 Zr1 C36 105.18(11) . . ? C39 Zr1 C36 52.77(10) . . ? C34 Zr1 C36 77.49(11) . . ? O1 Zr1 C38 96.32(9) . . ? C30 Zr1 C38 81.24(11) . . ? C32 Zr1 C38 158.08(11) . . ? C33 Zr1 C38 133.02(11) . . ? C40 Zr1 C38 52.95(11) . . ? C31 Zr1 C38 169.64(11) . . ? C35 Zr1 C38 140.89(11) . . ? C39 Zr1 C38 31.73(10) . . ? C34 Zr1 C38 126.35(11) . . ? C36 Zr1 C38 52.59(11) . . ? O1 Zr1 C37 128.35(9) . . ? C30 Zr1 C37 78.25(11) . . ? C32 Zr1 C37 142.07(12) . . ? C33 Zr1 C37 109.85(12) . . ? C40 Zr1 C37 52.82(10) . . ? C31 Zr1 C37 143.47(10) . . ? C35 Zr1 C37 111.41(11) . . ? C39 Zr1 C37 52.64(10) . . ? C34 Zr1 C37 94.75(11) . . ? C36 Zr1 C37 31.33(11) . . ? C38 Zr1 C37 32.03(10) . . ? O1 Ge1 N1 98.95(9) . . ? O1 Ge1 N2 99.31(8) . . ? N1 Ge1 N2 86.95(8) . . ? C4 N1 C6 121.0(2) . . ? C4 N1 Ge1 115.67(17) . . ? C6 N1 Ge1 120.92(16) . . ? Ge1 O1 Zr1 143.80(11) . . ? C2 N2 C18 121.7(2) . . ? C2 N2 Ge1 116.97(17) . . ? C18 N2 Ge1 117.42(16) . . ? N2 C2 C3 122.2(2) . . ? N2 C2 C1 121.0(2) . . ? C3 C2 C1 116.8(2) . . ? C4 C3 C2 127.1(3) . . ? N1 C4 C3 121.9(2) . . ? N1 C4 C5 120.3(2) . . ? C3 C4 C5 117.8(2) . . ? C7 C6 C11 121.8(2) . . ? C7 C6 N1 120.1(2) . . ? C11 C6 N1 118.1(2) . . ? C8 C7 C6 117.5(3) . . ? C8 C7 C15 119.1(2) . . ? C6 C7 C15 123.4(2) . . ? C9 C8 C7 121.6(3) . . ? C8 C9 C10 120.2(3) . . ? C9 C10 C11 121.1(3) . . ? C10 C11 C6 117.8(3) . . ? C10 C11 C12 120.6(3) . . ? C6 C11 C12 121.6(2) . . ? C11 C12 C14 112.6(2) . . ? C11 C12 C13 113.9(2) . . ? C14 C12 C13 107.5(2) . . ? C7 C15 C17 112.5(2) . . ? C7 C15 C16 110.2(2) . . ? C17 C15 C16 110.2(2) . . ? C23 C18 C19 121.3(2) . . ? C23 C18 N2 119.7(2) . . ? C19 C18 N2 118.9(2) . . ? C20 C19 C18 118.0(2) . . ? C20 C19 C27 121.6(2) . . ? C18 C19 C27 120.3(2) . . ? C21 C20 C19 121.1(3) . . ? C22 C21 C20 120.3(2) . . ? C21 C22 C23 121.2(3) . . ? C22 C23 C18 118.1(2) . . ? C22 C23 C24 118.7(2) . . ? C18 C23 C24 123.3(2) . . ? C23 C24 C26 110.4(2) . . ? C23 C24 C25 111.8(2) . . ? C26 C24 C25 110.4(2) . . ? C19 C27 C28 113.4(2) . . ? C19 C27 C29 111.3(2) . . ? C28 C27 C29 109.4(2) . . ? C32 C31 C35 107.7(3) . . ? C32 C31 Zr1 73.44(18) . . ? C35 C31 Zr1 74.88(18) . . ? C31 C32 C33 108.6(3) . . ? C31 C32 Zr1 74.64(19) . . ? C33 C32 Zr1 73.95(18) . . ? C32 C33 C34 107.8(3) . . ? C32 C33 Zr1 73.83(19) . . ? C34 C33 Zr1 75.56(19) . . ? C35 C34 C33 107.8(3) . . ? C35 C34 Zr1 74.05(18) . . ? C33 C34 Zr1 72.34(18) . . ? C34 C35 C31 108.1(3) . . ? C34 C35 Zr1 74.31(18) . . ? C31 C35 Zr1 72.99(17) . . ? C37 C36 C40 108.1(3) . . ? C37 C36 Zr1 74.67(17) . . ? C40 C36 Zr1 72.36(17) . . ? C36 C37 C38 108.3(3) . . ? C36 C37 Zr1 74.00(17) . . ? C38 C37 Zr1 73.89(16) . . ? C39 C38 C37 107.6(3) . . ? C39 C38 Zr1 73.81(17) . . ? C37 C38 Zr1 74.08(17) . . ? C40 C39 C38 108.1(3) . . ? C40 C39 Zr1 72.57(16) . . ? C38 C39 Zr1 74.46(16) . . ? C39 C40 C36 107.9(3) . . ? C39 C40 Zr1 75.43(16) . . ? C36 C40 Zr1 75.37(17) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 O1 1.9510(18) . ? Zr1 C30 2.285(3) . ? Zr1 C32 2.517(3) . ? Zr1 C33 2.518(3) . ? Zr1 C40 2.521(3) . ? Zr1 C31 2.532(3) . ? Zr1 C35 2.556(3) . ? Zr1 C39 2.558(3) . ? Zr1 C34 2.559(3) . ? Zr1 C36 2.560(3) . ? Zr1 C38 2.566(3) . ? Zr1 C37 2.568(3) . ? Ge1 O1 1.7973(19) . ? Ge1 N1 2.030(2) . ? Ge1 N2 2.061(2) . ? N1 C4 1.332(3) . ? N1 C6 1.446(3) . ? C1 C2 1.512(4) . ? N2 C2 1.326(3) . ? N2 C18 1.440(3) . ? C2 C3 1.403(4) . ? C3 C4 1.401(4) . ? C4 C5 1.507(4) . ? C6 C7 1.405(4) . ? C6 C11 1.410(4) . ? C7 C8 1.402(4) . ? C7 C15 1.518(4) . ? C8 C9 1.372(4) . ? C9 C10 1.384(4) . ? C10 C11 1.398(4) . ? C11 C12 1.525(4) . ? C12 C14 1.532(4) . ? C12 C13 1.533(4) . ? C15 C17 1.528(4) . ? C15 C16 1.541(4) . ? C18 C23 1.407(4) . ? C18 C19 1.412(4) . ? C19 C20 1.396(4) . ? C19 C27 1.520(4) . ? C20 C21 1.385(4) . ? C21 C22 1.376(4) . ? C22 C23 1.399(4) . ? C23 C24 1.522(4) . ? C24 C26 1.534(4) . ? C24 C25 1.535(4) . ? C27 C28 1.532(4) . ? C27 C29 1.535(4) . ? C31 C32 1.388(5) . ? C31 C35 1.408(5) . ? C32 C33 1.397(5) . ? C33 C34 1.404(5) . ? C34 C35 1.395(5) . ? C36 C37 1.385(5) . ? C36 C40 1.413(5) . ? C37 C38 1.416(5) . ? C38 C39 1.401(4) . ? C39 C40 1.401(5) . ?
1100713.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100713.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100713 loop_ _publ_author_name 'Leslie W. Pineda' 'Vojtech Jancik' 'Herbert W. Roesky' 'Regine Herbst-Irmer' _publ_contact_author_address ; Institut f\"ur Anorganische Chemie, Georg-August-Universit\"at G\"ottingen, Tammannstrasse 4, D 37077 G\"ottingen, Germany ; _publ_contact_author_email hroesky@gwdg.de _publ_contact_author_name 'Herbert W. Roesky' _publ_section_title ; OH Functionality of Germanium(II) Compounds for the Formation of Heterobimetallic Oxides ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3537 _journal_page_last 3540 _journal_paper_doi 10.1021/ic048383f _journal_volume 44 _journal_year 2005 _chemical_formula_moiety LGe(m-O)HfCp2Me _chemical_formula_sum 'C40 H54 Ge Hf N2 O' _chemical_formula_weight 829.93 _chemical_name_systematic ; ? ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 89.13(1) _cell_angle_beta 89.87(1) _cell_angle_gamma 67.04(1) _cell_formula_units_Z 2 _cell_length_a 9.323(1) _cell_length_b 10.474(1) _cell_length_c 20.200(1) _cell_measurement_reflns_used 5077 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 58.94 _cell_measurement_theta_min 2.191 _cell_volume 1816.0(3) _computing_cell_refinement 'Siemens SAINT (V. 6.31a, Siemens 2002)' _computing_data_collection 'Proteum (Version 1.35)' _computing_data_reduction 'Siemens SAINT (V. 6.31a, Siemens 2002)' _computing_molecular_graphics 'Bruker AXS SHELXTL (V. 5.10)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 5.602 _diffrn_measured_fraction_theta_full 0.968 _diffrn_measured_fraction_theta_max 0.968 _diffrn_measurement_device_type 'Bruker three circle diffractometer' _diffrn_measurement_method 'phi and omega scan' _diffrn_radiation_monochromator 'mirror system' _diffrn_radiation_source 'rotating anode' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0221 _diffrn_reflns_av_sigmaI/netI 0.0237 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 13915 _diffrn_reflns_theta_full 58.94 _diffrn_reflns_theta_max 58.94 _diffrn_reflns_theta_min 2.19 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 6.440 _exptl_absorpt_correction_T_max 0.7827 _exptl_absorpt_correction_T_min 0.5653 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour yellow-orange _exptl_crystal_density_diffrn 1.518 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 840 _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _refine_diff_density_max 1.551 _refine_diff_density_min -0.801 _refine_diff_density_rms 0.098 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.265 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 422 _refine_ls_number_reflns 5077 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.265 _refine_ls_R_factor_all 0.0296 _refine_ls_R_factor_gt 0.0287 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+9.9694P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0782 _refine_ls_wR_factor_ref 0.0785 _reflns_number_gt 4915 _reflns_number_total 5077 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic048383fsi20041122_032909_1.cif _cod_data_source_block LGem-OHfCp2Me _cod_original_cell_volume 1816(1) _cod_database_code 1100713 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hf1 Hf 0.63937(3) 0.05292(3) 0.251570(13) 0.01621(10) Uani 1 1 d . . . Ge1 Ge 0.22776(6) 0.20122(6) 0.24883(3) 0.01490(15) Uani 1 1 d . . . N1 N 0.1410(5) 0.3550(4) 0.1790(2) 0.0156(9) Uani 1 1 d . . . C1 C -0.1181(6) 0.4991(6) 0.3667(3) 0.0225(12) Uani 1 1 d . . . H1A H -0.0563 0.5212 0.4005 0.034 Uiso 1 1 calc R . . H1B H -0.1611 0.4348 0.3855 0.034 Uiso 1 1 calc R . . H1C H -0.2035 0.5845 0.3519 0.034 Uiso 1 1 calc R . . O1 O 0.4261(4) 0.1878(4) 0.24726(17) 0.0189(8) Uani 1 1 d . . . N2 N 0.1345(5) 0.3523(4) 0.3181(2) 0.0152(9) Uani 1 1 d . . . C2 C -0.0162(6) 0.4331(5) 0.3089(3) 0.0170(11) Uani 1 1 d . . . C3 C -0.0849(6) 0.4626(5) 0.2456(3) 0.0175(11) Uani 1 1 d . . . H3A H -0.190(7) 0.523(6) 0.245(3) 0.014(13) Uiso 1 1 d . . . C4 C -0.0079(6) 0.4411(5) 0.1850(3) 0.0162(11) Uani 1 1 d . . . C5 C -0.0954(6) 0.5200(6) 0.1250(3) 0.0214(12) Uani 1 1 d . . . H5A H -0.0400 0.5740 0.1056 0.032 Uiso 1 1 calc R . . H5B H -0.2003 0.5827 0.1380 0.032 Uiso 1 1 calc R . . H5C H -0.1028 0.4546 0.0923 0.032 Uiso 1 1 calc R . . C6 C 0.2230(6) 0.3448(5) 0.1179(2) 0.0163(11) Uani 1 1 d . . . C7 C 0.2122(6) 0.2570(5) 0.0678(3) 0.0183(12) Uani 1 1 d . . . C8 C 0.3002(6) 0.2449(6) 0.0106(3) 0.0227(12) Uani 1 1 d . . . H8A H 0.2943 0.1861 -0.0237 0.027 Uiso 1 1 calc R . . C9 C 0.3957(7) 0.3167(6) 0.0030(3) 0.0255(13) Uani 1 1 d . . . H9A H 0.4537 0.3082 -0.0366 0.031 Uiso 1 1 calc R . . C10 C 0.4067(7) 0.4008(6) 0.0530(3) 0.0255(13) Uani 1 1 d . . . H10A H 0.4745 0.4484 0.0476 0.031 Uiso 1 1 calc R . . C11 C 0.3211(6) 0.4175(6) 0.1110(3) 0.0191(12) Uani 1 1 d . . . C12 C 0.3301(7) 0.5173(6) 0.1634(3) 0.0228(12) Uani 1 1 d . . . H12A H 0.2710 0.5066 0.2030 0.027 Uiso 1 1 calc R . . C13 C 0.4973(7) 0.4859(6) 0.1853(3) 0.0277(13) Uani 1 1 d . . . H13A H 0.5432 0.3919 0.2042 0.042 Uiso 1 1 calc R . . H13B H 0.4974 0.5528 0.2187 0.042 Uiso 1 1 calc R . . H13C H 0.5587 0.4930 0.1470 0.042 Uiso 1 1 calc R . . C14 C 0.2537(7) 0.6681(6) 0.1389(3) 0.0285(14) Uani 1 1 d . . . H14A H 0.1468 0.6879 0.1246 0.043 Uiso 1 1 calc R . . H14B H 0.3133 0.6828 0.1017 0.043 Uiso 1 1 calc R . . H14C H 0.2523 0.7302 0.1750 0.043 Uiso 1 1 calc R . . C15 C 0.1140(6) 0.1716(6) 0.0746(3) 0.0206(12) Uani 1 1 d . . . H15A H 0.0503 0.2008 0.1157 0.025 Uiso 1 1 calc R . . C16 C 0.0012(7) 0.1942(7) 0.0155(3) 0.0289(14) Uani 1 1 d . . . H16A H -0.0588 0.2937 0.0085 0.043 Uiso 1 1 calc R . . H16B H -0.0701 0.1479 0.0249 0.043 Uiso 1 1 calc R . . H16C H 0.0610 0.1551 -0.0245 0.043 Uiso 1 1 calc R . . C17 C 0.2176(7) 0.0175(6) 0.0819(3) 0.0280(13) Uani 1 1 d . . . H17A H 0.2786 0.0017 0.1229 0.042 Uiso 1 1 calc R . . H17B H 0.2882 -0.0113 0.0440 0.042 Uiso 1 1 calc R . . H17C H 0.1524 -0.0366 0.0835 0.042 Uiso 1 1 calc R . . C18 C 0.2051(6) 0.3385(5) 0.3827(2) 0.0153(11) Uani 1 1 d . . . C19 C 0.1997(6) 0.2375(5) 0.4273(3) 0.0176(11) Uani 1 1 d . . . C20 C 0.2769(6) 0.2215(6) 0.4883(3) 0.0231(13) Uani 1 1 d . . . H20A H 0.2768 0.1511 0.5185 0.028 Uiso 1 1 calc R . . C21 C 0.3522(6) 0.3053(6) 0.5051(3) 0.0238(13) Uani 1 1 d . . . H21A H 0.4033 0.2932 0.5467 0.029 Uiso 1 1 calc R . . C22 C 0.3540(6) 0.4080(6) 0.4613(3) 0.0241(13) Uani 1 1 d . . . H22A H 0.4045 0.4670 0.4740 0.029 Uiso 1 1 calc R . . C23 C 0.2835(6) 0.4269(5) 0.3989(3) 0.0186(12) Uani 1 1 d . . . C24 C 0.2952(6) 0.5340(6) 0.3499(3) 0.0221(12) Uani 1 1 d . . . H24A H 0.3271 0.4871 0.3063 0.026 Uiso 1 1 calc R . . C25 C 0.1410(7) 0.6590(6) 0.3387(3) 0.0312(14) Uani 1 1 d . . . H25A H 0.1589 0.7278 0.3102 0.047 Uiso 1 1 calc R . . H25B H 0.0997 0.7006 0.3814 0.047 Uiso 1 1 calc R . . H25C H 0.0657 0.6284 0.3174 0.047 Uiso 1 1 calc R . . C26 C 0.4176(7) 0.5906(6) 0.3691(3) 0.0281(14) Uani 1 1 d . . . H26A H 0.4297 0.6489 0.3328 0.042 Uiso 1 1 calc R . . H26B H 0.5174 0.5132 0.3775 0.042 Uiso 1 1 calc R . . H26C H 0.3841 0.6460 0.4091 0.042 Uiso 1 1 calc R . . C27 C 0.1099(6) 0.1460(6) 0.4143(3) 0.0190(12) Uani 1 1 d . . . H27A H 0.0591 0.1725 0.3698 0.023 Uiso 1 1 calc R . . C28 C -0.0187(6) 0.1713(6) 0.4658(3) 0.0230(12) Uani 1 1 d . . . H28A H -0.0891 0.1278 0.4514 0.035 Uiso 1 1 calc R . . H28B H -0.0776 0.2713 0.4704 0.035 Uiso 1 1 calc R . . H28C H 0.0282 0.1310 0.5085 0.035 Uiso 1 1 calc R . . C29 C 0.2178(7) -0.0074(6) 0.4128(3) 0.0265(13) Uani 1 1 d . . . H29A H 0.2954 -0.0222 0.3778 0.040 Uiso 1 1 calc R . . H29B H 0.1565 -0.0630 0.4041 0.040 Uiso 1 1 calc R . . H29C H 0.2709 -0.0354 0.4556 0.040 Uiso 1 1 calc R . . C30 C 0.5811(7) -0.1296(6) 0.2853(3) 0.0291(14) Uani 1 1 d . . . H30A H 0.5522 -0.1196 0.3322 0.044 Uiso 1 1 calc R . . H30B H 0.6721 -0.2161 0.2793 0.044 Uiso 1 1 calc R . . H30C H 0.4938 -0.1314 0.2590 0.044 Uiso 1 1 calc R . . C31 C 0.6521(7) 0.0952(7) 0.3742(3) 0.0283(14) Uani 1 1 d . . . H31A H 0.5695 0.0946 0.4017 0.034 Uiso 1 1 calc R . . C32 C 0.7904(6) -0.0202(6) 0.3594(3) 0.0233(13) Uani 1 1 d . . . H32A H 0.8169 -0.1123 0.3755 0.028 Uiso 1 1 calc R . . C33 C 0.8812(6) 0.0243(6) 0.3174(3) 0.0248(13) Uani 1 1 d . . . H33A H 0.9808 -0.0318 0.3005 0.030 Uiso 1 1 calc R . . C34 C 0.7987(7) 0.1678(6) 0.3043(3) 0.0280(14) Uani 1 1 d . . . H34A H 0.8310 0.2248 0.2761 0.034 Uiso 1 1 calc R . . C35 C 0.6597(7) 0.2098(6) 0.3409(3) 0.0274(14) Uani 1 1 d . . . H35A H 0.5832 0.3018 0.3427 0.033 Uiso 1 1 calc R . . C36 C 0.8579(7) -0.0063(6) 0.1669(3) 0.0274(13) Uani 1 1 d . . . H36A H 0.9543 -0.0019 0.1791 0.033 Uiso 1 1 calc R . . C37 C 0.8219(7) -0.1236(6) 0.1729(3) 0.0295(14) Uani 1 1 d . . . H37A H 0.8875 -0.2115 0.1906 0.035 Uiso 1 1 calc R . . C38 C 0.6688(7) -0.0864(7) 0.1475(3) 0.0306(14) Uani 1 1 d . . . H38A H 0.6134 -0.1455 0.1451 0.037 Uiso 1 1 calc R . . C39 C 0.6142(7) 0.0516(7) 0.1267(3) 0.0305(15) Uani 1 1 d . . . H39A H 0.5158 0.1024 0.1067 0.037 Uiso 1 1 calc R . . C40 C 0.7298(7) 0.1036(6) 0.1403(3) 0.0286(14) Uani 1 1 d . . . H40A H 0.7219 0.1959 0.1328 0.034 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hf1 0.01510(14) 0.01533(15) 0.01586(15) 0.00033(10) -0.00169(10) -0.00339(10) Ge1 0.0161(3) 0.0134(3) 0.0146(3) 0.0007(2) -0.0027(2) -0.0051(2) N1 0.016(2) 0.013(2) 0.017(2) 0.0014(18) -0.0018(18) -0.0044(19) C1 0.018(3) 0.024(3) 0.021(3) -0.001(2) -0.002(2) -0.003(2) O1 0.0186(19) 0.0185(19) 0.0186(19) 0.0010(15) -0.0021(15) -0.0063(16) N2 0.016(2) 0.014(2) 0.016(2) 0.0002(18) -0.0026(18) -0.0063(19) C2 0.018(3) 0.014(3) 0.022(3) 0.001(2) -0.001(2) -0.009(2) C3 0.013(3) 0.016(3) 0.025(3) -0.003(2) -0.003(2) -0.008(2) C4 0.020(3) 0.013(3) 0.019(3) 0.000(2) -0.005(2) -0.011(2) C5 0.021(3) 0.022(3) 0.021(3) 0.002(2) -0.006(2) -0.007(2) C6 0.018(3) 0.012(3) 0.016(3) 0.007(2) -0.004(2) -0.003(2) C7 0.019(3) 0.017(3) 0.018(3) 0.005(2) -0.004(2) -0.006(2) C8 0.026(3) 0.025(3) 0.016(3) 0.000(2) -0.005(2) -0.008(3) C9 0.027(3) 0.030(3) 0.019(3) 0.004(2) 0.001(2) -0.011(3) C10 0.027(3) 0.034(3) 0.021(3) 0.005(3) -0.003(2) -0.018(3) C11 0.019(3) 0.022(3) 0.017(3) 0.006(2) -0.006(2) -0.009(2) C12 0.027(3) 0.024(3) 0.022(3) 0.000(2) -0.002(2) -0.016(3) C13 0.026(3) 0.023(3) 0.034(3) 0.004(3) -0.008(3) -0.009(3) C14 0.030(3) 0.019(3) 0.036(3) -0.003(3) -0.004(3) -0.009(3) C15 0.027(3) 0.020(3) 0.017(3) -0.001(2) -0.001(2) -0.011(3) C16 0.033(3) 0.036(4) 0.022(3) -0.001(3) -0.003(3) -0.017(3) C17 0.038(4) 0.020(3) 0.029(3) -0.002(2) 0.000(3) -0.015(3) C18 0.014(3) 0.017(3) 0.015(3) -0.004(2) -0.001(2) -0.005(2) C19 0.017(3) 0.019(3) 0.016(3) -0.001(2) 0.000(2) -0.006(2) C20 0.023(3) 0.032(3) 0.016(3) 0.001(2) 0.000(2) -0.012(3) C21 0.023(3) 0.035(3) 0.015(3) -0.002(2) -0.004(2) -0.013(3) C22 0.020(3) 0.032(3) 0.023(3) -0.010(3) 0.001(2) -0.013(3) C23 0.017(3) 0.017(3) 0.020(3) -0.003(2) 0.002(2) -0.004(2) C24 0.024(3) 0.021(3) 0.025(3) -0.005(2) 0.001(2) -0.012(3) C25 0.031(3) 0.020(3) 0.045(4) 0.002(3) -0.007(3) -0.012(3) C26 0.029(3) 0.020(3) 0.037(4) -0.005(3) 0.000(3) -0.012(3) C27 0.022(3) 0.024(3) 0.013(3) 0.003(2) -0.005(2) -0.012(2) C28 0.023(3) 0.028(3) 0.022(3) 0.002(2) -0.004(2) -0.013(3) C29 0.029(3) 0.026(3) 0.027(3) 0.000(2) -0.003(3) -0.013(3) C30 0.031(3) 0.020(3) 0.036(4) -0.001(3) 0.006(3) -0.009(3) C31 0.023(3) 0.042(4) 0.017(3) -0.006(3) -0.002(2) -0.009(3) C32 0.022(3) 0.025(3) 0.019(3) 0.002(2) -0.010(2) -0.006(3) C33 0.016(3) 0.033(3) 0.022(3) -0.004(3) -0.007(2) -0.006(3) C34 0.026(3) 0.029(3) 0.032(3) -0.003(3) -0.010(3) -0.013(3) C35 0.024(3) 0.022(3) 0.031(3) -0.013(3) -0.010(3) -0.002(3) C36 0.027(3) 0.036(4) 0.020(3) -0.001(3) -0.001(2) -0.013(3) C37 0.027(3) 0.026(3) 0.022(3) -0.005(3) 0.001(3) 0.005(3) C38 0.034(4) 0.035(4) 0.018(3) -0.014(3) 0.005(3) -0.008(3) C39 0.028(3) 0.042(4) 0.011(3) -0.001(3) 0.001(2) -0.001(3) C40 0.033(3) 0.030(3) 0.020(3) 0.002(3) 0.005(3) -0.009(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ge Ge -1.0885 0.8855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hf Hf -6.1794 4.9776 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Hf1 C30 96.26(19) . . ? O1 Hf1 C34 107.37(17) . . ? C30 Hf1 C34 131.5(2) . . ? O1 Hf1 C35 82.39(17) . . ? C30 Hf1 C35 116.3(2) . . ? C34 Hf1 C35 32.6(2) . . ? O1 Hf1 C40 98.43(17) . . ? C30 Hf1 C40 129.8(2) . . ? C34 Hf1 C40 88.5(2) . . ? C35 Hf1 C40 113.1(2) . . ? O1 Hf1 C38 103.85(17) . . ? C30 Hf1 C38 76.3(2) . . ? C34 Hf1 C38 133.8(2) . . ? C35 Hf1 C38 165.6(2) . . ? C40 Hf1 C38 53.6(2) . . ? O1 Hf1 C33 135.86(17) . . ? C30 Hf1 C33 104.1(2) . . ? C34 Hf1 C33 32.73(19) . . ? C35 Hf1 C33 53.49(19) . . ? C40 Hf1 C33 97.79(19) . . ? C38 Hf1 C33 118.76(19) . . ? O1 Hf1 C31 90.72(17) . . ? C30 Hf1 C31 84.8(2) . . ? C34 Hf1 C31 54.0(2) . . ? C35 Hf1 C31 32.0(2) . . ? C40 Hf1 C31 142.3(2) . . ? C38 Hf1 C31 157.2(2) . . ? C33 Hf1 C31 53.55(19) . . ? O1 Hf1 C39 84.09(17) . . ? C30 Hf1 C39 103.1(2) . . ? C34 Hf1 C39 120.6(2) . . ? C35 Hf1 C39 139.3(2) . . ? C40 Hf1 C39 32.5(2) . . ? C38 Hf1 C39 31.9(2) . . ? C33 Hf1 C39 127.02(19) . . ? C31 Hf1 C39 170.9(2) . . ? O1 Hf1 C32 122.76(16) . . ? C30 Hf1 C32 77.8(2) . . ? C34 Hf1 C32 53.7(2) . . ? C35 Hf1 C32 53.16(19) . . ? C40 Hf1 C32 129.15(19) . . ? C38 Hf1 C32 128.43(19) . . ? C33 Hf1 C32 31.96(19) . . ? C31 Hf1 C32 32.43(19) . . ? C39 Hf1 C32 153.08(19) . . ? O1 Hf1 C37 135.39(17) . . ? C30 Hf1 C37 83.3(2) . . ? C34 Hf1 C37 105.7(2) . . ? C35 Hf1 C37 137.5(2) . . ? C40 Hf1 C37 53.5(2) . . ? C38 Hf1 C37 32.5(2) . . ? C33 Hf1 C37 86.24(19) . . ? C31 Hf1 C37 133.28(19) . . ? C39 Hf1 C37 53.23(19) . . ? C32 Hf1 C37 100.86(18) . . ? O1 Hf1 C36 130.41(17) . . ? C30 Hf1 C36 114.7(2) . . ? C34 Hf1 C36 80.8(2) . . ? C35 Hf1 C36 113.1(2) . . ? C40 Hf1 C36 32.00(19) . . ? C38 Hf1 C36 53.0(2) . . ? C33 Hf1 C36 74.57(18) . . ? C31 Hf1 C36 127.94(19) . . ? C39 Hf1 C36 52.82(19) . . ? C32 Hf1 C36 101.85(18) . . ? C37 Hf1 C36 31.9(2) . . ? O1 Ge1 N1 97.45(16) . . ? O1 Ge1 N2 100.67(16) . . ? N1 Ge1 N2 86.80(16) . . ? C4 N1 C6 121.2(4) . . ? C4 N1 Ge1 117.1(3) . . ? C6 N1 Ge1 119.4(3) . . ? Ge1 O1 Hf1 141.9(2) . . ? C2 N2 C18 120.6(4) . . ? C2 N2 Ge1 114.8(3) . . ? C18 N2 Ge1 120.6(3) . . ? N2 C2 C3 122.4(5) . . ? N2 C2 C1 120.4(5) . . ? C3 C2 C1 117.2(5) . . ? C4 C3 C2 126.9(5) . . ? N1 C4 C3 122.0(5) . . ? N1 C4 C5 119.4(5) . . ? C3 C4 C5 118.6(5) . . ? C11 C6 C7 121.1(5) . . ? C11 C6 N1 118.5(5) . . ? C7 C6 N1 120.3(5) . . ? C8 C7 C6 118.3(5) . . ? C8 C7 C15 118.9(5) . . ? C6 C7 C15 122.8(5) . . ? C9 C8 C7 121.2(5) . . ? C8 C9 C10 119.8(5) . . ? C9 C10 C11 121.6(5) . . ? C10 C11 C6 118.0(5) . . ? C10 C11 C12 119.9(5) . . ? C6 C11 C12 122.0(5) . . ? C11 C12 C13 112.4(5) . . ? C11 C12 C14 111.3(5) . . ? C13 C12 C14 109.6(5) . . ? C7 C15 C17 110.6(5) . . ? C7 C15 C16 112.3(4) . . ? C17 C15 C16 109.7(5) . . ? C19 C18 C23 121.3(5) . . ? C19 C18 N2 120.0(4) . . ? C23 C18 N2 118.7(5) . . ? C18 C19 C20 118.6(5) . . ? C18 C19 C27 123.4(5) . . ? C20 C19 C27 117.9(5) . . ? C21 C20 C19 121.2(5) . . ? C20 C21 C22 120.1(5) . . ? C21 C22 C23 121.7(5) . . ? C22 C23 C18 117.1(5) . . ? C22 C23 C24 121.0(5) . . ? C18 C23 C24 121.8(5) . . ? C23 C24 C26 113.4(5) . . ? C23 C24 C25 113.7(5) . . ? C26 C24 C25 107.3(5) . . ? C19 C27 C29 111.6(4) . . ? C19 C27 C28 110.6(4) . . ? C29 C27 C28 110.8(4) . . ? C35 C31 C32 107.2(5) . . ? C35 C31 Hf1 73.2(3) . . ? C32 C31 Hf1 73.9(3) . . ? C33 C32 C31 108.5(5) . . ? C33 C32 Hf1 73.8(3) . . ? C31 C32 Hf1 73.7(3) . . ? C32 C33 C34 107.9(5) . . ? C32 C33 Hf1 74.2(3) . . ? C34 C33 Hf1 72.2(3) . . ? C35 C34 C33 107.1(5) . . ? C35 C34 Hf1 74.5(3) . . ? C33 C34 Hf1 75.1(3) . . ? C31 C35 C34 109.2(5) . . ? C31 C35 Hf1 74.7(3) . . ? C34 C35 Hf1 72.9(3) . . ? C40 C36 C37 109.3(5) . . ? C40 C36 Hf1 72.9(3) . . ? C37 C36 Hf1 73.8(3) . . ? C36 C37 C38 107.1(5) . . ? C36 C37 Hf1 74.3(3) . . ? C38 C37 Hf1 73.3(3) . . ? C39 C38 C37 108.0(6) . . ? C39 C38 Hf1 74.2(3) . . ? C37 C38 Hf1 74.2(3) . . ? C38 C39 C40 108.5(5) . . ? C38 C39 Hf1 73.9(3) . . ? C40 C39 Hf1 73.2(3) . . ? C36 C40 C39 107.1(6) . . ? C36 C40 Hf1 75.1(3) . . ? C39 C40 Hf1 74.4(3) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hf1 O1 1.940(3) . ? Hf1 C30 2.276(6) . ? Hf1 C34 2.495(6) . ? Hf1 C35 2.516(5) . ? Hf1 C40 2.520(6) . ? Hf1 C38 2.530(5) . ? Hf1 C33 2.532(5) . ? Hf1 C31 2.534(5) . ? Hf1 C39 2.535(5) . ? Hf1 C32 2.537(5) . ? Hf1 C37 2.542(5) . ? Hf1 C36 2.547(6) . ? Ge1 O1 1.799(3) . ? Ge1 N1 2.038(4) . ? Ge1 N2 2.052(4) . ? N1 C4 1.334(7) . ? N1 C6 1.435(7) . ? C1 C2 1.501(7) . ? N2 C2 1.339(7) . ? N2 C18 1.443(6) . ? C2 C3 1.405(8) . ? C3 C4 1.395(8) . ? C4 C5 1.504(7) . ? C6 C11 1.406(8) . ? C6 C7 1.407(8) . ? C7 C8 1.394(8) . ? C7 C15 1.514(8) . ? C8 C9 1.378(8) . ? C9 C10 1.380(8) . ? C10 C11 1.391(8) . ? C11 C12 1.523(8) . ? C12 C13 1.528(8) . ? C12 C14 1.532(8) . ? C15 C17 1.529(8) . ? C15 C16 1.547(8) . ? C18 C19 1.394(7) . ? C18 C23 1.427(7) . ? C19 C20 1.403(8) . ? C19 C27 1.524(7) . ? C20 C21 1.367(8) . ? C21 C22 1.387(8) . ? C22 C23 1.398(8) . ? C23 C24 1.521(8) . ? C24 C26 1.530(8) . ? C24 C25 1.535(8) . ? C27 C29 1.529(8) . ? C27 C28 1.532(8) . ? C31 C35 1.393(9) . ? C31 C32 1.416(8) . ? C32 C33 1.396(8) . ? C33 C34 1.417(8) . ? C34 C35 1.408(8) . ? C36 C40 1.397(8) . ? C36 C37 1.398(9) . ? C37 C38 1.420(9) . ? C38 C39 1.391(9) . ? C39 C40 1.413(9) . ?
1100714.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100714.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100714 loop_ _publ_author_name 'Jingwen Chen' 'Xiaoyong Wang' 'Yangguang Zhu' 'Jun Lin' 'Xiaoliang Yang' 'Yizhi Li' 'Yi Lu' 'Zijian Guo' _publ_section_title ; An Asymmetric Dizinc Phosphodiesterase Model with Phenolate and Carboxylate Bridges ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3422 _journal_page_last 3430 _journal_paper_doi 10.1021/ic048654m _journal_volume 44 _journal_year 2005 _chemical_formula_moiety '4(C27 H35 N4 O6 Zn2), 4(F6 P), 3(H4 O2), H4 O2, H4 O2' _chemical_formula_sum 'C108 H156 F24 N16 O32 P4 Zn8' _chemical_formula_weight 3293.33 _chemical_name_systematic ; ? ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 106.99(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 23.935(3) _cell_length_b 14.2035(16) _cell_length_c 22.489(3) _cell_measurement_reflns_used 2283 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 20.35 _cell_measurement_theta_min 2.33 _cell_volume 7311.7(18) _computing_cell_refinement SMART _computing_data_collection 'SMART (Bruker, 2000)' _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _computing_structure_refinement SHELXTL _computing_structure_solution 'SHELXTL (Bruker, 2000)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device_type 'Bruker Smart Apex CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0288 _diffrn_reflns_av_sigmaI/netI 0.0325 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_number 19176 _diffrn_reflns_theta_full 26.00 _diffrn_reflns_theta_max 26.00 _diffrn_reflns_theta_min 1.69 _exptl_absorpt_coefficient_mu 1.435 _exptl_absorpt_correction_T_max 0.75 _exptl_absorpt_correction_T_min 0.65 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS(Bruker, 2000)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.496 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 3376 _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.20 _refine_diff_density_max 0.919 _refine_diff_density_min -0.865 _refine_diff_density_rms 0.066 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 453 _refine_ls_number_reflns 7142 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.046 _refine_ls_R_factor_all 0.0631 _refine_ls_R_factor_gt 0.0484 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.09P)^2^+1.55P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1325 _refine_ls_wR_factor_ref 0.1385 _reflns_number_gt 5841 _reflns_number_total 7142 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic048654msi20040925_101616.cif _cod_data_source_block 40615bm _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_sg_symbol_H-M 'C 1 2/c 1 ' _cod_database_code 1100714 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.099395(19) 0.91848(3) 0.408890(19) 0.04350(13) Uani 1 1 d . . . Zn2 Zn 0.097925(17) 0.69338(3) 0.354388(16) 0.03744(13) Uani 1 1 d . . . C1 C 0.18206(18) 0.6917(3) 0.60752(17) 0.0519(9) Uani 1 1 d . . . C2 C 0.13345(16) 0.6466(3) 0.56749(15) 0.0437(8) Uani 1 1 d . . . H2 H 0.1165 0.5962 0.5822 0.052 Uiso 1 1 calc R . . C3 C 0.11043(17) 0.6754(3) 0.50698(16) 0.0463(8) Uani 1 1 d . . . C4 C 0.13742(15) 0.7496(3) 0.48333(15) 0.0408(7) Uani 1 1 d . . . C5 C 0.18627(16) 0.7953(3) 0.52411(18) 0.0519(9) Uani 1 1 d . . . C6 C 0.20707(17) 0.7664(3) 0.58585(16) 0.0479(8) Uani 1 1 d . . . H6 H 0.2383 0.7980 0.6128 0.057 Uiso 1 1 calc R . . C7 C 0.2034(2) 0.6613(3) 0.67495(17) 0.0576(10) Uani 1 1 d . . . H7A H 0.2366 0.6207 0.6809 0.086 Uiso 1 1 calc R . . H7B H 0.1727 0.6282 0.6857 0.086 Uiso 1 1 calc R . . H7C H 0.2143 0.7158 0.7010 0.086 Uiso 1 1 calc R . . C8 C 0.05630(18) 0.6333(3) 0.46411(17) 0.0479(8) Uani 1 1 d . . . H8A H 0.0421 0.5847 0.4864 0.057 Uiso 1 1 calc R . . H8B H 0.0265 0.6817 0.4526 0.057 Uiso 1 1 calc R . . C9 C 0.13842(19) 0.5028(3) 0.37849(19) 0.0574(11) Uani 1 1 d . . . C10 C 0.1720(2) 0.4194(3) 0.3755(2) 0.0602(11) Uani 1 1 d . . . H10 H 0.1695 0.3668 0.3992 0.072 Uiso 1 1 calc R . . C11 C 0.2073(2) 0.4185(3) 0.3376(2) 0.0639(12) Uani 1 1 d . . . H11 H 0.2284 0.3644 0.3352 0.077 Uiso 1 1 calc R . . C12 C 0.21204(19) 0.4933(3) 0.3042(2) 0.0622(11) Uani 1 1 d . . . H12 H 0.2368 0.4928 0.2791 0.075 Uiso 1 1 calc R . . C13 C 0.1788(2) 0.5731(3) 0.3077(2) 0.0658(12) Uani 1 1 d . . . H13 H 0.1813 0.6257 0.2840 0.079 Uiso 1 1 calc R . . C14 C 0.1031(2) 0.5110(3) 0.4226(2) 0.0623(11) Uani 1 1 d . . . H14A H 0.0802 0.4541 0.4210 0.075 Uiso 1 1 calc R . . H14B H 0.1288 0.5177 0.4646 0.075 Uiso 1 1 calc R . . C15 C 0.00653(18) 0.5681(3) 0.36158(18) 0.0502(9) Uani 1 1 d . . . H15A H -0.0175 0.5352 0.3829 0.060 Uiso 1 1 calc R . . H15B H 0.0130 0.5261 0.3302 0.060 Uiso 1 1 calc R . . C16 C -0.02536(19) 0.6550(3) 0.3303(2) 0.0615(11) Uani 1 1 d . . . H16A H -0.0543 0.6386 0.2916 0.074 Uiso 1 1 calc R . . H16B H -0.0448 0.6862 0.3572 0.074 Uiso 1 1 calc R . . C17 C 0.00696(18) 0.8760(3) 0.4811(2) 0.0570(10) Uani 1 1 d . . . H17 H -0.0201 0.8658 0.4425 0.068 Uiso 1 1 calc R . . C18 C -0.00639(19) 0.8467(3) 0.53236(18) 0.0520(9) Uani 1 1 d . . . H18 H -0.0414 0.8157 0.5291 0.062 Uiso 1 1 calc R . . C19 C 0.03293(19) 0.8638(3) 0.5896(2) 0.0579(10) Uani 1 1 d . . . H19 H 0.0246 0.8444 0.6255 0.070 Uiso 1 1 calc R . . C20 C 0.0840(2) 0.9091(3) 0.59368(19) 0.0537(9) Uani 1 1 d . . . H20 H 0.1102 0.9231 0.6321 0.064 Uiso 1 1 calc R . . C21 C 0.09593(18) 0.9339(3) 0.53877(17) 0.0480(8) Uani 1 1 d . . . C22 C 0.15357(19) 0.9827(3) 0.54057(19) 0.0539(9) Uani 1 1 d . . . H22A H 0.1485 1.0503 0.5416 0.065 Uiso 1 1 calc R . . H22B H 0.1834 0.9646 0.5783 0.065 Uiso 1 1 calc R . . C23 C 0.2011(2) 1.0380(4) 0.4633(3) 0.0730(13) Uani 1 1 d . . . H23A H 0.2189 1.0149 0.4325 0.088 Uiso 1 1 calc R . . H23B H 0.2315 1.0657 0.4972 0.088 Uiso 1 1 calc R . . C24 C 0.15508(19) 1.1123(4) 0.4342(2) 0.0644(11) Uani 1 1 d . . . H24A H 0.1437 1.1451 0.4666 0.077 Uiso 1 1 calc R . . H24B H 0.1715 1.1581 0.4119 0.077 Uiso 1 1 calc R . . C25 C 0.21147(15) 0.8785(3) 0.5019(2) 0.0529(9) Uani 1 1 d . . . H25A H 0.2468 0.8969 0.5336 0.064 Uiso 1 1 calc R . . H25B H 0.2223 0.8610 0.4651 0.064 Uiso 1 1 calc R . . C26 C 0.14255(17) 0.8900(3) 0.23101(15) 0.0495(9) Uani 1 1 d . . . H26A H 0.1498 0.9565 0.2328 0.074 Uiso 1 1 calc R . . H26B H 0.1081 0.8764 0.1975 0.074 Uiso 1 1 calc R . . H26C H 0.1754 0.8576 0.2242 0.074 Uiso 1 1 calc R . . C27 C 0.13391(17) 0.8581(3) 0.29043(18) 0.0491(8) Uani 1 1 d . . . N1 N 0.06397(14) 0.5921(2) 0.40727(13) 0.0438(7) Uani 1 1 d . . . N2 N 0.14342(14) 0.5761(2) 0.34424(15) 0.0468(7) Uani 1 1 d . . . N3 N 0.17296(13) 0.9583(3) 0.48720(15) 0.0518(8) Uani 1 1 d . . . N4 N 0.05921(14) 0.9206(2) 0.48305(15) 0.0455(7) Uani 1 1 d . . . O1 O 0.11806(11) 0.77904(16) 0.42378(10) 0.0405(5) Uani 1 1 d . . . O2 O 0.12382(11) 0.77305(17) 0.29412(12) 0.0464(6) Uani 1 1 d . . . O3 O 0.13772(13) 0.91489(19) 0.33327(11) 0.0513(6) Uani 1 1 d . . . O4 O 0.01586(12) 0.71080(18) 0.31982(11) 0.0493(6) Uani 1 1 d . . . O5 O 0.10525(12) 1.06961(18) 0.39255(13) 0.0521(6) Uani 1 1 d . . . H5A H 0.1227 1.0610 0.3651 0.063 Uiso 1 1 d R . . O6 O 0.01797(12) 0.8936(2) 0.34627(13) 0.0553(6) Uani 1 1 d . . . H6A H 0.0217 0.8911 0.3099 0.066 Uiso 1 1 d R . . H6C H 0.0019 0.8353 0.3553 0.083 Uiso 1 1 d R . . O7 O 1.0000 0.0262(3) 0.2500 0.0632(11) Uani 1 2 d S . . H7D H 0.9936 0.0384 0.2116 0.076 Uiso 0.50 1 d PR . . H7E H 1.0321 0.0509 0.2708 0.076 Uiso 0.50 1 d PR . . O8 O 0.0294(3) 0.3154(4) 0.3027(3) 0.0598(14) Uani 0.50 1 d P . . H8F H 0.0243 0.3704 0.3151 0.072 Uiso 0.50 1 d PR . . H8D H -0.0036 0.2889 0.2877 0.072 Uiso 0.50 1 d PR . . O9 O 0.2094(3) 0.0765(4) 0.2917(3) 0.0593(14) Uani 0.50 1 d P . . H9A H 0.2325 0.1233 0.2988 0.071 Uiso 0.50 1 d PR . . H9B H 0.2185 0.0394 0.3227 0.071 Uiso 0.50 1 d PR . . O10 O 0.1173(2) 0.1292(4) 0.2765(3) 0.0574(13) Uani 0.50 1 d P . . H10D H 0.0969 0.1743 0.2838 0.069 Uiso 0.50 1 d PR . . H10A H 0.0953 0.0831 0.2607 0.069 Uiso 0.50 1 d PR . . P1 P 0.33822(5) 0.17925(8) 0.41545(5) 0.0525(3) Uani 1 1 d . . . F1 F 0.27624(11) 0.2218(2) 0.40355(11) 0.0670(7) Uani 1 1 d . . . F2 F 0.36576(10) 0.27680(16) 0.41404(9) 0.0512(5) Uani 1 1 d . . . F3 F 0.34155(10) 0.15390(16) 0.35507(9) 0.0521(5) Uani 1 1 d . . . F4 F 0.31342(10) 0.07823(16) 0.42583(9) 0.0531(5) Uani 1 1 d . . . F5 F 0.34713(11) 0.18465(17) 0.48449(9) 0.0574(6) Uani 1 1 d . . . F6 F 0.39937(11) 0.1213(2) 0.43476(11) 0.0663(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0430(2) 0.0452(2) 0.0422(2) 0.00279(16) 0.01220(18) 0.00238(17) Zn2 0.0384(2) 0.0412(2) 0.0334(2) 0.00135(14) 0.01139(16) -0.00282(15) C1 0.053(2) 0.060(2) 0.0347(18) 0.0033(16) 0.0015(16) -0.0084(18) C2 0.049(2) 0.0492(19) 0.0302(16) 0.0016(13) 0.0072(14) -0.0023(15) C3 0.048(2) 0.052(2) 0.0350(17) -0.0015(14) 0.0056(15) -0.0124(16) C4 0.0418(18) 0.0507(18) 0.0290(16) 0.0031(13) 0.0087(13) -0.0021(15) C5 0.0321(18) 0.076(3) 0.047(2) 0.0027(18) 0.0106(15) -0.0096(17) C6 0.050(2) 0.056(2) 0.0344(17) -0.0024(15) 0.0064(15) -0.0123(17) C7 0.066(3) 0.070(3) 0.0313(17) 0.0076(17) 0.0061(17) -0.012(2) C8 0.063(2) 0.0443(18) 0.0436(19) -0.0051(15) 0.0279(18) 0.0025(17) C9 0.055(2) 0.050(2) 0.051(2) 0.0114(17) -0.0104(19) -0.0043(18) C10 0.060(3) 0.057(2) 0.049(2) 0.0022(17) -0.006(2) -0.0034(19) C11 0.065(3) 0.055(2) 0.057(2) 0.0015(18) -0.004(2) -0.016(2) C12 0.048(2) 0.072(3) 0.066(3) 0.015(2) 0.016(2) -0.004(2) C13 0.068(3) 0.072(3) 0.056(2) 0.022(2) 0.014(2) -0.005(2) C14 0.072(3) 0.055(2) 0.059(2) 0.0131(19) 0.017(2) -0.004(2) C15 0.054(2) 0.0468(19) 0.045(2) 0.0004(15) 0.0075(17) 0.0079(16) C16 0.047(2) 0.090(3) 0.048(2) -0.004(2) 0.0140(18) 0.009(2) C17 0.046(2) 0.056(2) 0.068(3) 0.0017(19) 0.0151(19) -0.0057(18) C18 0.056(2) 0.048(2) 0.049(2) 0.0008(16) 0.0113(18) 0.0050(17) C19 0.051(2) 0.058(2) 0.066(3) 0.0010(19) 0.019(2) -0.0076(18) C20 0.057(2) 0.053(2) 0.048(2) 0.0014(16) 0.0102(18) 0.0044(18) C21 0.054(2) 0.0487(19) 0.0401(19) 0.0080(15) 0.0123(16) -0.0024(16) C22 0.057(2) 0.053(2) 0.049(2) 0.0023(17) 0.0108(18) 0.0056(18) C23 0.057(3) 0.073(3) 0.093(4) -0.006(3) 0.029(3) 0.013(2) C24 0.052(2) 0.084(3) 0.064(3) 0.015(2) 0.029(2) -0.008(2) C25 0.0268(17) 0.064(2) 0.063(2) 0.0149(19) 0.0062(16) 0.0002(16) C26 0.050(2) 0.069(2) 0.0277(16) 0.0008(15) 0.0094(15) -0.0053(18) C27 0.042(2) 0.059(2) 0.048(2) -0.0019(17) 0.0166(16) 0.0026(17) N1 0.0540(18) 0.0389(15) 0.0361(14) -0.0015(11) 0.0095(13) -0.0081(13) N2 0.0410(16) 0.0477(16) 0.0556(18) 0.0095(13) 0.0200(14) -0.0100(13) N3 0.0387(16) 0.070(2) 0.0510(18) 0.0108(15) 0.0202(14) 0.0118(15) N4 0.0454(17) 0.0459(16) 0.0497(17) 0.0069(13) 0.0212(14) -0.0059(13) O1 0.0462(13) 0.0435(12) 0.0300(11) 0.0031(9) 0.0084(10) -0.0001(10) O2 0.0479(14) 0.0477(14) 0.0489(14) 0.0062(11) 0.0222(12) -0.0037(11) O3 0.0645(17) 0.0585(16) 0.0312(12) -0.0040(10) 0.0144(12) -0.0042(13) O4 0.0544(16) 0.0513(14) 0.0397(13) -0.0018(10) 0.0099(12) 0.0021(12) O5 0.0564(16) 0.0465(13) 0.0508(15) 0.0017(11) 0.0116(13) 0.0068(12) O6 0.0548(16) 0.0598(15) 0.0470(14) -0.0054(12) 0.0082(12) -0.0041(13) O7 0.065(3) 0.071(3) 0.045(2) 0.000 0.0029(19) 0.000 O8 0.063(4) 0.052(3) 0.056(3) -0.006(2) 0.005(3) 0.001(3) O9 0.053(3) 0.060(3) 0.060(3) -0.001(3) 0.010(3) 0.002(3) O10 0.048(3) 0.061(3) 0.058(3) -0.004(3) 0.006(3) 0.003(3) P1 0.0579(6) 0.0626(6) 0.0361(5) 0.0021(4) 0.0122(4) -0.0076(5) F1 0.0540(14) 0.0911(18) 0.0552(14) -0.0038(12) 0.0150(11) 0.0162(13) F2 0.0528(13) 0.0633(13) 0.0357(10) 0.0026(9) 0.0102(9) -0.0094(10) F3 0.0583(13) 0.0633(13) 0.0325(10) 0.0046(9) 0.0101(9) -0.0090(11) F4 0.0569(13) 0.0671(14) 0.0328(10) 0.0021(9) 0.0092(9) -0.0080(11) F5 0.0625(14) 0.0725(14) 0.0332(10) 0.0018(10) 0.0076(10) -0.0107(12) F6 0.0501(13) 0.0942(18) 0.0533(13) -0.0043(13) 0.0132(11) 0.0160(13) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 O6 93.63(11) . . ? O1 Zn1 N4 90.71(10) . . ? O6 Zn1 N4 89.11(12) . . ? O1 Zn1 O3 89.04(10) . . ? O6 Zn1 O3 89.56(11) . . ? N4 Zn1 O3 178.64(11) . . ? O1 Zn1 N3 91.88(11) . . ? O6 Zn1 N3 166.90(12) . . ? N4 Zn1 N3 78.94(12) . . ? O3 Zn1 N3 102.41(11) . . ? O1 Zn1 O5 163.64(11) . . ? O6 Zn1 O5 98.44(11) . . ? N4 Zn1 O5 100.44(11) . . ? O3 Zn1 O5 80.09(11) . . ? N3 Zn1 O5 78.72(12) . . ? O4 Zn2 O1 103.45(11) . . ? O4 Zn2 O2 97.87(11) . . ? O1 Zn2 O2 97.94(10) . . ? O4 Zn2 N2 125.51(12) . . ? O1 Zn2 N2 126.26(12) . . ? O2 Zn2 N2 96.04(11) . . ? O4 Zn2 N1 78.65(12) . . ? O1 Zn2 N1 91.13(10) . . ? O2 Zn2 N1 170.83(11) . . ? N2 Zn2 N1 79.48(11) . . ? C6 C1 C2 119.4(3) . . ? C6 C1 C7 121.4(3) . . ? C2 C1 C7 119.1(4) . . ? C3 C2 C1 121.2(3) . . ? C3 C2 H2 119.4 . . ? C1 C2 H2 119.4 . . ? C2 C3 C4 119.9(3) . . ? C2 C3 C8 122.7(3) . . ? C4 C3 C8 117.3(3) . . ? O1 C4 C5 118.7(3) . . ? O1 C4 C3 122.7(3) . . ? C5 C4 C3 118.6(3) . . ? C6 C5 C4 119.9(3) . . ? C6 C5 C25 120.7(4) . . ? C4 C5 C25 119.2(3) . . ? C1 C6 C5 121.0(3) . . ? C1 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? C1 C7 H7A 109.5 . . ? C1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 C3 114.6(3) . . ? N1 C8 H8A 108.6 . . ? C3 C8 H8A 108.6 . . ? N1 C8 H8B 108.6 . . ? C3 C8 H8B 108.6 . . ? H8A C8 H8B 107.6 . . ? N2 C9 C10 118.2(4) . . ? N2 C9 C14 119.7(4) . . ? C10 C9 C14 121.9(4) . . ? C11 C10 C9 119.4(4) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? C12 C11 C10 121.2(5) . . ? C12 C11 H11 119.4 . . ? C10 C11 H11 119.4 . . ? C11 C12 C13 118.2(5) . . ? C11 C12 H12 120.9 . . ? C13 C12 H12 120.9 . . ? N2 C13 C12 122.0(4) . . ? N2 C13 H13 119.0 . . ? C12 C13 H13 119.0 . . ? N1 C14 C9 110.8(3) . . ? N1 C14 H14A 109.5 . . ? C9 C14 H14A 109.5 . . ? N1 C14 H14B 109.5 . . ? C9 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? N1 C15 C16 111.8(3) . . ? N1 C15 H15A 109.3 . . ? C16 C15 H15A 109.3 . . ? N1 C15 H15B 109.3 . . ? C16 C15 H15B 109.3 . . ? H15A C15 H15B 107.9 . . ? O4 C16 C15 105.5(3) . . ? O4 C16 H16A 110.6 . . ? C15 C16 H16A 110.6 . . ? O4 C16 H16B 110.6 . . ? C15 C16 H16B 110.6 . . ? H16A C16 H16B 108.8 . . ? C18 C17 N4 123.3(4) . . ? C18 C17 H17 118.4 . . ? N4 C17 H17 118.4 . . ? C17 C18 C19 118.5(4) . . ? C17 C18 H18 120.8 . . ? C19 C18 H18 120.8 . . ? C20 C19 C18 120.2(4) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C19 C20 C21 118.2(4) . . ? C19 C20 H20 120.9 . . ? C21 C20 H20 120.9 . . ? N4 C21 C20 123.7(4) . . ? N4 C21 C22 115.8(3) . . ? C20 C21 C22 120.5(4) . . ? N3 C22 C21 111.9(3) . . ? N3 C22 H22A 109.2 . . ? C21 C22 H22A 109.2 . . ? N3 C22 H22B 109.2 . . ? C21 C22 H22B 109.2 . . ? H22A C22 H22B 107.9 . . ? N3 C23 C24 109.5(4) . . ? N3 C23 H23A 109.8 . . ? C24 C23 H23A 109.8 . . ? N3 C23 H23B 109.8 . . ? C24 C23 H23B 109.8 . . ? H23A C23 H23B 108.2 . . ? O5 C24 C23 110.4(4) . . ? O5 C24 H24A 109.6 . . ? C23 C24 H24A 109.6 . . ? O5 C24 H24B 109.6 . . ? C23 C24 H24B 109.6 . . ? H24A C24 H24B 108.1 . . ? N3 C25 C5 114.2(3) . . ? N3 C25 H25A 108.7 . . ? C5 C25 H25A 108.7 . . ? N3 C25 H25B 108.7 . . ? C5 C25 H25B 108.7 . . ? H25A C25 H25B 107.6 . . ? C27 C26 H26A 109.5 . . ? C27 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C27 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O3 C27 O2 123.6(4) . . ? O3 C27 C26 120.3(4) . . ? O2 C27 C26 116.0(3) . . ? C14 N1 C8 110.1(3) . . ? C14 N1 C15 112.3(3) . . ? C8 N1 C15 111.5(3) . . ? C14 N1 Zn2 109.6(2) . . ? C8 N1 Zn2 112.1(2) . . ? C15 N1 Zn2 101.0(2) . . ? C9 N2 C13 120.9(4) . . ? C9 N2 Zn2 115.8(3) . . ? C13 N2 Zn2 123.2(3) . . ? C25 N3 C22 109.7(3) . . ? C25 N3 C23 110.7(3) . . ? C22 N3 C23 113.8(4) . . ? C25 N3 Zn1 107.2(3) . . ? C22 N3 Zn1 110.7(2) . . ? C23 N3 Zn1 104.5(3) . . ? C21 N4 C17 116.1(3) . . ? C21 N4 Zn1 114.4(3) . . ? C17 N4 Zn1 124.7(3) . . ? C4 O1 Zn2 122.7(2) . . ? C4 O1 Zn1 117.4(2) . . ? Zn2 O1 Zn1 119.36(11) . . ? C27 O2 Zn2 134.6(2) . . ? C27 O3 Zn1 132.6(3) . . ? C16 O4 Zn2 125.2(3) . . ? C24 O5 Zn1 113.0(3) . . ? C24 O5 H5A 92.5 . . ? Zn1 O5 H5A 92.9 . . ? Zn1 O6 H6A 108.5 . . ? Zn1 O6 H6C 111.1 . . ? H6A O6 H6C 109.2 . . ? H7D O7 H7E 109.8 . . ? H8F O8 H8D 109.5 . . ? H9A O9 H9B 109.5 . . ? H10D O10 H10A 109.8 . . ? F3 P1 F5 164.10(16) . . ? F3 P1 F2 93.67(13) . . ? F5 P1 F2 92.46(13) . . ? F3 P1 F1 104.49(15) . . ? F5 P1 F1 89.90(14) . . ? F2 P1 F1 92.28(16) . . ? F3 P1 F4 92.23(13) . . ? F5 P1 F4 80.89(13) . . ? F2 P1 F4 173.02(13) . . ? F1 P1 F4 89.85(15) . . ? F3 P1 F6 80.23(14) . . ? F5 P1 F6 84.55(14) . . ? F2 P1 F6 95.95(15) . . ? F1 P1 F6 170.26(16) . . ? F4 P1 F6 81.38(14) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 2.036(2) . ? Zn1 O6 2.074(3) . ? Zn1 N4 2.155(3) . ? Zn1 O3 2.156(3) . ? Zn1 N3 2.170(3) . ? Zn1 O5 2.189(3) . ? Zn2 O4 1.906(3) . ? Zn2 O1 1.926(2) . ? Zn2 O2 1.998(2) . ? Zn2 N2 2.040(3) . ? Zn2 N1 2.170(3) . ? C1 C6 1.375(5) . ? C1 C2 1.401(5) . ? C1 C7 1.515(5) . ? C2 C3 1.373(5) . ? C2 H2 0.9300 . ? C3 C4 1.418(5) . ? C3 C8 1.495(5) . ? C4 O1 1.349(4) . ? C4 C5 1.415(5) . ? C5 C6 1.393(5) . ? C5 C25 1.479(5) . ? C6 H6 0.9300 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 N1 1.465(4) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 N2 1.320(5) . ? C9 C10 1.444(6) . ? C9 C14 1.485(7) . ? C10 C11 1.364(7) . ? C10 H10 0.9300 . ? C11 C12 1.325(6) . ? C11 H11 0.9300 . ? C12 C13 1.401(7) . ? C12 H12 0.9300 . ? C13 N2 1.341(6) . ? C13 H13 0.9300 . ? C14 N1 1.461(5) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 N1 1.496(5) . ? C15 C16 1.513(6) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 O4 1.339(5) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.349(6) . ? C17 N4 1.391(5) . ? C17 H17 0.9300 . ? C18 C19 1.376(6) . ? C18 H18 0.9300 . ? C19 C20 1.361(6) . ? C19 H19 0.9300 . ? C20 C21 1.391(6) . ? C20 H20 0.9300 . ? C21 N4 1.317(5) . ? C21 C22 1.534(6) . ? C22 N3 1.450(5) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 N3 1.495(6) . ? C23 C24 1.529(7) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 O5 1.419(5) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 N3 1.437(5) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.481(5) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 O3 1.239(5) . ? C27 O2 1.239(5) . ? O5 H5A 0.8500 . ? O6 H6A 0.8501 . ? O6 H6C 0.9599 . ? O7 H7D 0.8501 . ? O7 H7E 0.8500 . ? O8 H8F 0.8499 . ? O8 H8D 0.8500 . ? O9 H9A 0.8500 . ? O9 H9B 0.8499 . ? O10 H10D 0.8500 . ? O10 H10A 0.8499 . ? P1 F3 1.429(2) . ? P1 F5 1.506(2) . ? P1 F2 1.539(2) . ? P1 F1 1.551(3) . ? P1 F4 1.596(2) . ? P1 F6 1.624(3) . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H5A O3 0.85 2.26 2.796(4) 121.3 . O6 H6C O4 0.96 2.01 2.661(4) 123.5 . O10 H10A O7 0.85 2.37 3.067(6) 140.2 1_455 O5 H5A O10 0.85 2.18 2.838(7) 133.5 1_565 O6 H6A O7 0.85 2.31 2.807(4) 117.2 1_465 O7 H7E O10 0.85 2.29 3.067(6) 151.4 1_655
1100715.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100715.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100715 loop_ _publ_author_name 'Kay H. Horn' 'Natascha B\"ores' 'Nicolai Lehnert' 'Klaus Mersmann' 'Christian N\"ather' 'Gerhard Peters' 'Felix Tuczek' _publ_contact_author_name 'Felix Tuczek' _publ_section_title ; Reduction Pathway of End-On Terminally Coordinated Dinitrogen. IV. Geometric, Electronic, and Vibrational Structure of a W(IV) Dialkylhydrazido Complex and Its Two-Electron-Reduced Derivative Undergoing N-N Cleavage upon Protonation ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3016 _journal_page_last 3030 _journal_paper_doi 10.1021/ic048675g _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C57 H58 N2 P4 W' _chemical_formula_weight 1078.79 _chemical_name_systematic ; ? ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 84.980(11) _cell_angle_beta 76.410(10) _cell_angle_gamma 67.177(10) _cell_formula_units_Z 2 _cell_length_a 12.6448(11) _cell_length_b 12.9364(12) _cell_length_c 16.7806(16) _cell_measurement_reflns_used 7998 _cell_measurement_temperature 180(2) _cell_measurement_theta_max 20.5 _cell_measurement_theta_min 11.5 _cell_volume 2459.2(4) _computing_data_collection 'IPDS program package' _computing_data_reduction 'IPDS program package' _computing_molecular_graphics 'XP in SHELXTL-PC' _computing_publication_material 'CIFTAB in SHELXL-97' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 180(2) _diffrn_measured_fraction_theta_full 0.934 _diffrn_measured_fraction_theta_max 0.934 _diffrn_measurement_device_type 'STOE IPDS' _diffrn_measurement_method Phi-Scans _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0652 _diffrn_reflns_av_sigmaI/netI 0.0830 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 16042 _diffrn_reflns_theta_full 24.94 _diffrn_reflns_theta_max 24.94 _diffrn_reflns_theta_min 2.10 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.519 _exptl_absorpt_correction_type none _exptl_crystal_density_diffrn 1.457 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1096 _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _refine_diff_density_max 0.944 _refine_diff_density_min -1.313 _refine_diff_density_rms 0.132 _refine_ls_extinction_coef 0.0027(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 621 _refine_ls_number_reflns 8020 _refine_ls_number_restraints 118 _refine_ls_restrained_S_all 0.999 _refine_ls_R_factor_all 0.0599 _refine_ls_R_factor_gt 0.0423 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0533P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0922 _refine_ls_wR_factor_ref 0.0989 _reflns_number_gt 6467 _reflns_number_total 8020 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic048675gsi20040929_105115.cif _cod_data_source_block ja029735p _cod_database_code 1100715 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.61866(2) 0.26517(2) 0.244537(14) 0.02035(10) Uani 1 1 d . . . P1 P 0.70341(14) 0.35100(14) 0.32248(9) 0.0220(3) Uani 1 1 d . . . P2 P 0.45459(14) 0.43240(14) 0.29642(8) 0.0210(3) Uani 1 1 d . . . C1 C 0.5893(6) 0.4337(6) 0.4077(3) 0.0256(14) Uani 1 1 d . . . H1A H 0.5641 0.3839 0.4492 0.031 Uiso 1 1 calc R . . H1B H 0.6195 0.4787 0.4343 0.031 Uiso 1 1 calc R . . C2 C 0.4859(6) 0.5110(6) 0.3701(3) 0.0247(13) Uani 1 1 d . . . H2A H 0.5051 0.5737 0.3413 0.030 Uiso 1 1 calc R . . H2B H 0.4150 0.5430 0.4144 0.030 Uiso 1 1 calc R . . C11 C 0.8283(6) 0.2713(6) 0.3707(4) 0.0307(15) Uani 1 1 d . . . C12 C 0.9226(7) 0.1856(7) 0.3258(5) 0.0419(18) Uani 1 1 d . . . H12 H 0.9227 0.1702 0.2714 0.050 Uiso 1 1 calc R . . C13 C 1.0172(9) 0.1224(9) 0.3607(7) 0.066(3) Uani 1 1 d . . . H13 H 1.0815 0.0636 0.3296 0.079 Uiso 1 1 calc R . . C14 C 1.0202(9) 0.1423(8) 0.4385(6) 0.057(2) Uani 1 1 d . . . H14 H 1.0858 0.0984 0.4613 0.068 Uiso 1 1 calc R . . C15 C 0.9275(8) 0.2264(9) 0.4826(5) 0.052(2) Uani 1 1 d . . . H15 H 0.9285 0.2400 0.5371 0.063 Uiso 1 1 calc R . . C16 C 0.8305(7) 0.2934(7) 0.4501(4) 0.0404(18) Uani 1 1 d . . . H16 H 0.7674 0.3528 0.4814 0.048 Uiso 1 1 calc R . . C21 C 0.7516(6) 0.4638(6) 0.2722(4) 0.0253(14) Uani 1 1 d . . . C22 C 0.7090(7) 0.5168(7) 0.2046(4) 0.0404(19) Uani 1 1 d . . . H22 H 0.6662 0.4878 0.1797 0.048 Uiso 1 1 calc R . . C23 C 0.7286(8) 0.6123(7) 0.1730(4) 0.045(2) Uani 1 1 d . . . H23 H 0.6971 0.6496 0.1275 0.055 Uiso 1 1 calc R . . C24 C 0.7927(9) 0.6526(8) 0.2068(5) 0.054(2) Uani 1 1 d . . . H24 H 0.8061 0.7177 0.1848 0.065 Uiso 1 1 calc R . . C25 C 0.8384(9) 0.5993(9) 0.2732(5) 0.056(3) Uani 1 1 d . . . H25 H 0.8841 0.6271 0.2962 0.068 Uiso 1 1 calc R . . C26 C 0.8177(7) 0.5062(7) 0.3060(5) 0.0393(18) Uani 1 1 d . . . H26 H 0.8485 0.4702 0.3520 0.047 Uiso 1 1 calc R . . C31 C 0.3076(6) 0.4373(6) 0.3508(4) 0.0283(14) Uani 1 1 d . . . C32 C 0.2905(7) 0.4103(6) 0.4338(4) 0.0365(17) Uani 1 1 d . . . H32 H 0.3507 0.3992 0.4623 0.044 Uiso 1 1 calc R . . C33 C 0.1860(9) 0.3992(9) 0.4755(5) 0.059(3) Uani 1 1 d . . . H33 H 0.1739 0.3839 0.5327 0.070 Uiso 1 1 calc R . . C34 C 0.1016(9) 0.4102(10) 0.4341(6) 0.070(3) Uani 1 1 d . . . H34 H 0.0321 0.3990 0.4617 0.084 Uiso 1 1 calc R . . C35 C 0.1172(8) 0.4379(9) 0.3517(6) 0.061(3) Uani 1 1 d . . . H35 H 0.0577 0.4464 0.3233 0.073 Uiso 1 1 calc R . . C36 C 0.2185(7) 0.4534(7) 0.3102(4) 0.0404(18) Uani 1 1 d . . . H36 H 0.2270 0.4750 0.2542 0.049 Uiso 1 1 calc R . . C41 C 0.4072(6) 0.5491(6) 0.2237(4) 0.0268(14) Uani 1 1 d . . . C42 C 0.3274(7) 0.6553(6) 0.2501(5) 0.0381(17) Uani 1 1 d . . . H42 H 0.2902 0.6674 0.3065 0.046 Uiso 1 1 calc R . . C43 C 0.3009(9) 0.7434(7) 0.1961(5) 0.052(2) Uani 1 1 d . . . H43 H 0.2470 0.8160 0.2154 0.062 Uiso 1 1 calc R . . C44 C 0.3537(10) 0.7253(8) 0.1135(6) 0.061(3) Uani 1 1 d . . . H44 H 0.3358 0.7858 0.0760 0.074 Uiso 1 1 calc R . . C45 C 0.4318(9) 0.6203(8) 0.0854(5) 0.052(2) Uani 1 1 d . . . H45 H 0.4664 0.6078 0.0286 0.062 Uiso 1 1 calc R . . C46 C 0.4594(7) 0.5337(7) 0.1404(4) 0.0345(16) Uani 1 1 d . . . H46 H 0.5151 0.4618 0.1211 0.041 Uiso 1 1 calc R . . P3 P 0.63055(16) 0.12390(14) 0.35025(9) 0.0257(4) Uani 1 1 d . . . P4 P 0.48201(15) 0.18338(15) 0.22039(9) 0.0242(4) Uani 1 1 d . . . C3 C 0.5268(7) 0.0512(6) 0.3531(4) 0.0347(17) Uani 1 1 d . . . H3A H 0.5691 -0.0202 0.3220 0.042 Uiso 1 1 calc R . . H3B H 0.4973 0.0335 0.4105 0.042 Uiso 1 1 calc R . . C4 C 0.4231(6) 0.1255(6) 0.3158(4) 0.0308(15) Uani 1 1 d . . . H4A H 0.3681 0.1868 0.3542 0.037 Uiso 1 1 calc R . . H4B H 0.3800 0.0807 0.3046 0.037 Uiso 1 1 calc R . . C51 C 0.6092(7) 0.1453(6) 0.4616(4) 0.0332(16) Uani 1 1 d . . . C52 C 0.7019(8) 0.1236(6) 0.5010(4) 0.0388(18) Uani 1 1 d . . . H52 H 0.7810 0.0938 0.4708 0.047 Uiso 1 1 calc R . . C53 C 0.6777(9) 0.1458(7) 0.5845(4) 0.044(2) Uani 1 1 d . . . H53 H 0.7413 0.1286 0.6109 0.053 Uiso 1 1 calc R . . C54 C 0.5652(9) 0.1915(7) 0.6295(4) 0.046(2) Uani 1 1 d . . . H54 H 0.5507 0.2075 0.6861 0.055 Uiso 1 1 calc R . . C55 C 0.4715(8) 0.2147(7) 0.5912(4) 0.0432(19) Uani 1 1 d . . . H55 H 0.3928 0.2457 0.6217 0.052 Uiso 1 1 calc R . . C56 C 0.4943(7) 0.1921(6) 0.5087(4) 0.0357(16) Uani 1 1 d . . . H56 H 0.4302 0.2089 0.4830 0.043 Uiso 1 1 calc R . . C61 C 0.7668(7) -0.0019(6) 0.3346(4) 0.0298(15) Uani 1 1 d . . . C62 C 0.8533(8) -0.0156(7) 0.2626(4) 0.0402(18) Uani 1 1 d . . . H62 H 0.8414 0.0426 0.2231 0.048 Uiso 1 1 calc R . . C63 C 0.9543(8) -0.1093(7) 0.2469(5) 0.046(2) Uani 1 1 d . . . H63 H 1.0115 -0.1148 0.1975 0.055 Uiso 1 1 calc R . . C64 C 0.9734(8) -0.1961(7) 0.3027(5) 0.0422(19) Uani 1 1 d . . . H64 H 1.0435 -0.2614 0.2920 0.051 Uiso 1 1 calc R . . C65 C 0.8898(8) -0.1870(6) 0.3739(5) 0.0406(19) Uani 1 1 d . . . H65 H 0.9025 -0.2466 0.4124 0.049 Uiso 1 1 calc R . . C66 C 0.7881(7) -0.0926(6) 0.3902(4) 0.0328(16) Uani 1 1 d . . . H66 H 0.7312 -0.0884 0.4395 0.039 Uiso 1 1 calc R . . C71 C 0.3528(6) 0.2568(6) 0.1753(4) 0.0294(15) Uani 1 1 d . . . C72 C 0.2439(7) 0.2437(8) 0.2052(5) 0.0433(19) Uani 1 1 d . . . H72 H 0.2338 0.1966 0.2506 0.052 Uiso 1 1 calc R . . C73 C 0.1518(8) 0.3027(8) 0.1657(6) 0.052(2) Uani 1 1 d . . . H73 H 0.0776 0.2970 0.1864 0.062 Uiso 1 1 calc R . . C74 C 0.1642(8) 0.3670(7) 0.0997(6) 0.051(2) Uani 1 1 d . . . H74 H 0.1008 0.4032 0.0730 0.061 Uiso 1 1 calc R . . C75 C 0.2708(8) 0.3803(7) 0.0705(5) 0.047(2) Uani 1 1 d . . . H75 H 0.2799 0.4278 0.0251 0.056 Uiso 1 1 calc R . . C76 C 0.3639(7) 0.3231(6) 0.1088(4) 0.0330(16) Uani 1 1 d . . . H76 H 0.4372 0.3306 0.0878 0.040 Uiso 1 1 calc R . . C81 C 0.5501(6) 0.0635(6) 0.1486(4) 0.0305(15) Uani 1 1 d . . . C82 C 0.5094(8) -0.0229(7) 0.1544(5) 0.045(2) Uani 1 1 d . . . H82 H 0.4494 -0.0256 0.1999 0.054 Uiso 1 1 calc R . . C83 C 0.5552(10) -0.1044(8) 0.0950(6) 0.060(3) Uani 1 1 d . . . H83 H 0.5279 -0.1641 0.1007 0.072 Uiso 1 1 calc R . . C84 C 0.6398(9) -0.1014(7) 0.0273(6) 0.054(2) Uani 1 1 d . . . H84 H 0.6693 -0.1572 -0.0141 0.065 Uiso 1 1 calc R . . C85 C 0.6819(8) -0.0152(8) 0.0203(5) 0.051(2) Uani 1 1 d . . . H85 H 0.7401 -0.0118 -0.0262 0.061 Uiso 1 1 calc R . . C86 C 0.6383(7) 0.0651(7) 0.0814(4) 0.0406(19) Uani 1 1 d . . . H86 H 0.6691 0.1222 0.0775 0.049 Uiso 1 1 calc R . . N1 N 0.8015(5) 0.2355(5) 0.0745(3) 0.0305(13) Uani 1 1 d D . . C91 C 0.9087(10) 0.1360(12) 0.0719(7) 0.036(3) Uani 0.574(17) 1 d PDU A 1 H91A H 0.8878 0.0699 0.0891 0.043 Uiso 0.574(17) 1 calc PR A 1 H91B H 0.9520 0.1454 0.1110 0.043 Uiso 0.574(17) 1 calc PR A 1 C92 C 0.9865(14) 0.1158(16) -0.0123(8) 0.053(4) Uani 0.574(17) 1 d PDU A 1 H92A H 1.0601 0.0502 -0.0109 0.064 Uiso 0.574(17) 1 calc PR A 1 H92B H 0.9465 0.0981 -0.0502 0.064 Uiso 0.574(17) 1 calc PR A 1 C93 C 1.0160(14) 0.2149(16) -0.0437(11) 0.050(4) Uani 0.574(17) 1 d PDU A 1 H93A H 1.0672 0.1993 -0.0994 0.060 Uiso 0.574(17) 1 calc PR A 1 H93B H 1.0578 0.2328 -0.0072 0.060 Uiso 0.574(17) 1 calc PR A 1 C94 C 0.899(2) 0.3139(19) -0.0459(9) 0.048(5) Uani 0.574(17) 1 d PDU A 1 H94A H 0.9146 0.3821 -0.0656 0.057 Uiso 0.574(17) 1 calc PR A 1 H94B H 0.8594 0.2966 -0.0844 0.057 Uiso 0.574(17) 1 calc PR A 1 C95 C 0.8213(14) 0.3342(13) 0.0377(8) 0.039(4) Uani 0.574(17) 1 d PDU A 1 H95A H 0.8570 0.3614 0.0737 0.047 Uiso 0.574(17) 1 calc PR A 1 H95B H 0.7445 0.3942 0.0346 0.047 Uiso 0.574(17) 1 calc PR A 1 C91' C 0.9216(13) 0.202(2) 0.0911(11) 0.054(6) Uani 0.426(17) 1 d PDU A 2 H91C H 0.9389 0.1340 0.1260 0.065 Uiso 0.426(17) 1 calc PR A 2 H91D H 0.9255 0.2628 0.1205 0.065 Uiso 0.426(17) 1 calc PR A 2 C92' C 1.010(2) 0.178(3) 0.0110(14) 0.078(8) Uani 0.426(17) 1 d PDU A 2 H92C H 1.0104 0.1122 -0.0155 0.093 Uiso 0.426(17) 1 calc PR A 2 H92D H 1.0892 0.1592 0.0212 0.093 Uiso 0.426(17) 1 calc PR A 2 C93' C 0.981(2) 0.280(2) -0.0474(13) 0.056(6) Uani 0.426(17) 1 d PDU A 2 H93C H 0.9959 0.3413 -0.0265 0.067 Uiso 0.426(17) 1 calc PR A 2 H93D H 1.0326 0.2583 -0.1026 0.067 Uiso 0.426(17) 1 calc PR A 2 C94' C 0.857(2) 0.319(3) -0.0529(11) 0.055(8) Uani 0.426(17) 1 d PDU A 2 H94C H 0.8461 0.2627 -0.0825 0.066 Uiso 0.426(17) 1 calc PR A 2 H94D H 0.8371 0.3897 -0.0850 0.066 Uiso 0.426(17) 1 calc PR A 2 C95' C 0.7750(5) 0.3402(4) 0.0293(3) 0.046(7) Uani 0.426(17) 1 d PDU A 2 H95C H 0.7847 0.3972 0.0596 0.055 Uiso 0.426(17) 1 calc PR A 2 H95D H 0.6927 0.3687 0.0229 0.055 Uiso 0.426(17) 1 calc PR A 2 N2 N 0.7195(5) 0.2498(4) 0.1482(3) 0.0253(12) Uani 1 1 d R A . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.02260(16) 0.02412(15) 0.01964(13) 0.00174(8) -0.00730(8) -0.01335(11) P1 0.0221(9) 0.0264(9) 0.0237(7) 0.0017(6) -0.0096(6) -0.0135(8) P2 0.0225(9) 0.0260(9) 0.0183(7) 0.0005(6) -0.0058(6) -0.0125(8) C1 0.032(4) 0.032(4) 0.021(3) -0.002(2) -0.007(2) -0.019(3) C2 0.025(4) 0.029(4) 0.022(3) 0.000(2) -0.006(2) -0.013(3) C11 0.033(4) 0.033(4) 0.034(3) 0.006(3) -0.016(3) -0.016(4) C12 0.035(5) 0.036(4) 0.053(4) -0.007(3) -0.022(4) -0.003(4) C13 0.049(7) 0.052(6) 0.092(7) -0.005(5) -0.039(5) 0.000(5) C14 0.047(6) 0.056(6) 0.071(6) 0.007(5) -0.042(5) -0.009(6) C15 0.051(6) 0.067(6) 0.056(5) 0.014(4) -0.036(4) -0.029(6) C16 0.042(5) 0.047(5) 0.040(4) 0.000(3) -0.017(3) -0.021(4) C21 0.025(4) 0.030(4) 0.026(3) 0.000(3) -0.005(2) -0.017(3) C22 0.043(5) 0.055(5) 0.035(4) 0.005(3) -0.013(3) -0.030(5) C23 0.067(6) 0.049(5) 0.041(4) 0.011(3) -0.016(4) -0.043(5) C24 0.069(7) 0.054(6) 0.051(5) 0.000(4) 0.001(4) -0.044(6) C25 0.065(6) 0.071(7) 0.064(5) 0.003(5) -0.016(4) -0.056(6) C26 0.042(5) 0.044(5) 0.048(4) 0.002(3) -0.018(3) -0.029(4) C31 0.029(4) 0.031(4) 0.028(3) -0.003(3) -0.002(3) -0.015(3) C32 0.048(5) 0.038(4) 0.029(3) -0.002(3) 0.002(3) -0.027(4) C33 0.068(7) 0.073(7) 0.051(5) -0.010(4) 0.011(4) -0.056(6) C34 0.052(6) 0.093(9) 0.074(6) -0.036(6) 0.027(5) -0.052(7) C35 0.028(5) 0.091(8) 0.071(6) -0.038(5) 0.002(4) -0.032(6) C36 0.030(4) 0.053(5) 0.042(4) -0.017(3) -0.005(3) -0.017(4) C41 0.029(4) 0.028(4) 0.030(3) 0.003(3) -0.013(3) -0.015(3) C42 0.045(5) 0.027(4) 0.042(4) 0.003(3) -0.020(3) -0.007(4) C43 0.068(7) 0.029(4) 0.059(5) 0.003(4) -0.034(5) -0.009(5) C44 0.086(8) 0.046(6) 0.056(5) 0.032(4) -0.035(5) -0.024(6) C45 0.067(7) 0.047(5) 0.038(4) 0.018(4) -0.015(4) -0.021(5) C46 0.039(5) 0.039(4) 0.027(3) 0.001(3) -0.010(3) -0.016(4) P3 0.0370(11) 0.0255(9) 0.0220(7) 0.0073(6) -0.0113(7) -0.0186(9) P4 0.0278(10) 0.0281(9) 0.0246(7) 0.0019(6) -0.0091(6) -0.0176(8) C3 0.049(5) 0.037(4) 0.032(3) 0.010(3) -0.016(3) -0.029(4) C4 0.037(4) 0.036(4) 0.029(3) 0.002(3) -0.007(3) -0.024(4) C51 0.045(5) 0.027(4) 0.038(4) 0.003(3) -0.015(3) -0.022(4) C52 0.058(5) 0.031(4) 0.040(4) 0.004(3) -0.022(3) -0.024(4) C53 0.080(7) 0.038(4) 0.025(3) 0.010(3) -0.026(4) -0.027(5) C54 0.089(7) 0.035(4) 0.019(3) 0.003(3) -0.011(4) -0.031(5) C55 0.068(6) 0.033(4) 0.027(3) 0.002(3) 0.001(3) -0.024(4) C56 0.044(5) 0.033(4) 0.030(3) 0.005(3) -0.006(3) -0.017(4) C61 0.040(4) 0.028(4) 0.031(3) -0.001(3) -0.014(3) -0.019(4) C62 0.055(6) 0.034(4) 0.027(3) 0.000(3) -0.007(3) -0.014(4) C63 0.044(6) 0.042(5) 0.038(4) -0.002(3) -0.009(3) 0.000(5) C64 0.053(6) 0.026(4) 0.050(4) -0.006(3) -0.025(4) -0.009(4) C65 0.050(5) 0.024(4) 0.059(5) 0.006(3) -0.031(4) -0.017(4) C66 0.044(5) 0.026(4) 0.038(4) 0.006(3) -0.017(3) -0.019(4) C71 0.037(4) 0.022(3) 0.034(3) -0.005(3) -0.010(3) -0.013(3) C72 0.035(5) 0.055(5) 0.052(4) 0.000(4) -0.017(3) -0.025(5) C73 0.031(5) 0.055(6) 0.075(6) -0.014(5) -0.015(4) -0.018(5) C74 0.047(6) 0.041(5) 0.070(5) 0.000(4) -0.036(4) -0.011(5) C75 0.056(6) 0.038(5) 0.054(5) 0.009(4) -0.034(4) -0.017(5) C76 0.036(4) 0.031(4) 0.041(4) 0.004(3) -0.018(3) -0.016(4) C81 0.031(4) 0.030(4) 0.036(3) 0.007(3) -0.020(3) -0.012(4) C82 0.060(6) 0.045(5) 0.047(4) 0.004(4) -0.019(4) -0.035(5) C83 0.079(8) 0.052(6) 0.070(6) 0.000(5) -0.027(5) -0.040(6) C84 0.064(7) 0.035(5) 0.069(6) -0.013(4) -0.033(5) -0.011(5) C85 0.057(6) 0.052(5) 0.050(4) -0.015(4) -0.010(4) -0.024(5) C86 0.045(5) 0.044(5) 0.043(4) -0.016(3) -0.008(3) -0.024(4) N1 0.029(4) 0.032(3) 0.024(3) -0.004(2) 0.006(2) -0.012(3) C91 0.027(7) 0.041(8) 0.031(6) 0.002(5) 0.001(5) -0.010(7) C92 0.040(9) 0.070(11) 0.035(7) -0.008(7) 0.013(6) -0.015(8) C93 0.041(9) 0.066(11) 0.042(8) 0.000(9) 0.009(7) -0.028(9) C94 0.042(12) 0.059(10) 0.037(8) 0.001(7) 0.015(8) -0.028(11) C95 0.046(11) 0.045(8) 0.027(6) -0.002(6) 0.014(6) -0.031(8) C91' 0.025(10) 0.064(15) 0.058(11) 0.027(11) -0.007(8) -0.007(11) C92' 0.043(12) 0.084(15) 0.060(12) 0.007(12) 0.028(10) 0.002(12) C93' 0.048(14) 0.071(15) 0.036(9) 0.016(11) 0.022(10) -0.031(13) C94' 0.052(16) 0.072(13) 0.030(10) -0.003(9) 0.010(10) -0.021(13) C95' 0.029(13) 0.052(12) 0.044(11) 0.010(9) 0.008(9) -0.013(11) N2 0.027(3) 0.027(3) 0.027(3) -0.003(2) -0.008(2) -0.013(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 W1 P2 126.31(18) . . ? N2 W1 P3 125.90(18) . . ? P2 W1 P3 107.69(6) . . ? N2 W1 P1 99.29(15) . . ? P2 W1 P1 77.76(5) . . ? P3 W1 P1 87.93(5) . . ? N2 W1 P4 103.61(15) . . ? P2 W1 P4 89.70(6) . . ? P3 W1 P4 77.58(5) . . ? P1 W1 P4 157.06(5) . . ? C1 P1 C11 103.5(3) . . ? C1 P1 C21 98.3(3) . . ? C11 P1 C21 100.0(3) . . ? C1 P1 W1 109.80(19) . . ? C11 P1 W1 123.9(2) . . ? C21 P1 W1 117.65(19) . . ? C31 P2 C41 98.2(3) . . ? C31 P2 C2 100.6(3) . . ? C41 P2 C2 97.5(3) . . ? C31 P2 W1 124.9(2) . . ? C41 P2 W1 118.0(2) . . ? C2 P2 W1 113.1(2) . . ? C2 C1 P1 106.3(4) . . ? C1 C2 P2 111.0(4) . . ? C12 C11 C16 119.4(7) . . ? C12 C11 P1 117.9(5) . . ? C16 C11 P1 122.7(6) . . ? C11 C12 C13 119.5(8) . . ? C14 C13 C12 121.9(10) . . ? C15 C14 C13 118.6(8) . . ? C14 C15 C16 121.9(8) . . ? C11 C16 C15 118.8(8) . . ? C22 C21 C26 118.5(6) . . ? C22 C21 P1 118.8(4) . . ? C26 C21 P1 122.2(5) . . ? C21 C22 C23 120.4(6) . . ? C24 C23 C22 120.2(7) . . ? C23 C24 C25 120.4(7) . . ? C26 C25 C24 119.9(7) . . ? C25 C26 C21 120.6(7) . . ? C36 C31 C32 118.8(6) . . ? C36 C31 P2 122.4(5) . . ? C32 C31 P2 118.4(5) . . ? C31 C32 C33 120.8(7) . . ? C34 C33 C32 119.8(8) . . ? C33 C34 C35 119.8(7) . . ? C34 C35 C36 120.9(8) . . ? C35 C36 C31 119.7(7) . . ? C42 C41 C46 117.9(6) . . ? C42 C41 P2 122.1(5) . . ? C46 C41 P2 119.8(6) . . ? C43 C42 C41 121.4(7) . . ? C42 C43 C44 119.4(9) . . ? C45 C44 C43 120.5(7) . . ? C44 C45 C46 119.5(8) . . ? C45 C46 C41 121.4(8) . . ? C61 P3 C51 99.3(3) . . ? C61 P3 C3 97.1(3) . . ? C51 P3 C3 99.8(3) . . ? C61 P3 W1 116.0(2) . . ? C51 P3 W1 126.6(2) . . ? C3 P3 W1 113.1(2) . . ? C4 P4 C71 103.8(3) . . ? C4 P4 C81 104.0(3) . . ? C71 P4 C81 96.0(3) . . ? C4 P4 W1 109.9(2) . . ? C71 P4 W1 125.8(2) . . ? C81 P4 W1 114.7(2) . . ? C4 C3 P3 110.6(4) . . ? C3 C4 P4 107.7(5) . . ? C56 C51 C52 117.6(6) . . ? C56 C51 P3 118.7(5) . . ? C52 C51 P3 123.6(6) . . ? C53 C52 C51 119.9(8) . . ? C54 C53 C52 121.8(7) . . ? C53 C54 C55 119.2(6) . . ? C56 C55 C54 119.5(8) . . ? C55 C56 C51 122.0(7) . . ? C62 C61 C66 116.0(7) . . ? C62 C61 P3 120.4(5) . . ? C66 C61 P3 123.4(6) . . ? C63 C62 C61 122.7(7) . . ? C62 C63 C64 120.0(8) . . ? C65 C64 C63 119.3(8) . . ? C66 C65 C64 120.9(7) . . ? C65 C66 C61 121.1(7) . . ? C76 C71 C72 118.9(7) . . ? C76 C71 P4 118.4(5) . . ? C72 C71 P4 122.7(5) . . ? C73 C72 C71 117.9(7) . . ? C74 C73 C72 122.6(8) . . ? C73 C74 C75 119.5(7) . . ? C74 C75 C76 119.2(7) . . ? C71 C76 C75 121.9(7) . . ? C82 C81 C86 118.5(7) . . ? C82 C81 P4 122.6(6) . . ? C86 C81 P4 118.6(5) . . ? C83 C82 C81 120.4(8) . . ? C82 C83 C84 121.2(8) . . ? C83 C84 C85 119.2(8) . . ? C86 C85 C84 119.6(8) . . ? C85 C86 C81 120.9(7) . . ? N2 N1 C95' 109.9(5) . . ? N2 N1 C95 117.5(7) . . ? C95' N1 C95 24.2(7) . . ? N2 N1 C91 113.8(6) . . ? C95' N1 C91 132.9(6) . . ? C95 N1 C91 114.1(9) . . ? N2 N1 C91' 109.6(8) . . ? C95' N1 C91' 108.4(9) . . ? C95 N1 C91' 84.4(12) . . ? C91 N1 C91' 40.2(10) . . ? N1 C91 C92 111.6(10) . . ? C93 C92 C91 112.0(13) . . ? C92 C93 C94 107.1(12) . . ? C95 C94 C93 109.8(14) . . ? N1 C95 C94 113.7(13) . . ? N1 C91' C92' 108.8(16) . . ? C91' C92' C93' 111.4(17) . . ? C94' C93' C92' 109.8(17) . . ? C93' C94' C95' 112.5(17) . . ? N1 C95' C94' 108.6(14) . . ? N1 N2 W1 177.9(5) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 N2 1.781(5) . ? W1 P2 2.3961(18) . ? W1 P3 2.4195(15) . ? W1 P1 2.4346(14) . ? W1 P4 2.4682(14) . ? P1 C1 1.836(7) . ? P1 C11 1.845(7) . ? P1 C21 1.856(6) . ? P2 C31 1.847(7) . ? P2 C41 1.857(6) . ? P2 C2 1.866(6) . ? C1 C2 1.539(9) . ? C11 C12 1.385(11) . ? C11 C16 1.395(9) . ? C12 C13 1.389(12) . ? C13 C14 1.364(13) . ? C14 C15 1.360(14) . ? C15 C16 1.400(11) . ? C21 C22 1.382(9) . ? C21 C26 1.398(8) . ? C22 C23 1.389(10) . ? C23 C24 1.358(11) . ? C24 C25 1.382(13) . ? C25 C26 1.372(11) . ? C31 C36 1.390(10) . ? C31 C32 1.392(9) . ? C32 C33 1.398(11) . ? C33 C34 1.362(14) . ? C34 C35 1.386(14) . ? C35 C36 1.387(11) . ? C41 C42 1.386(11) . ? C41 C46 1.394(9) . ? C42 C43 1.378(11) . ? C43 C44 1.387(13) . ? C44 C45 1.377(14) . ? C45 C46 1.377(11) . ? P3 C61 1.837(8) . ? P3 C51 1.854(7) . ? P3 C3 1.878(6) . ? P4 C4 1.828(6) . ? P4 C71 1.842(7) . ? P4 C81 1.844(8) . ? C3 C4 1.528(10) . ? C51 C56 1.401(11) . ? C51 C52 1.402(10) . ? C52 C53 1.394(10) . ? C53 C54 1.365(13) . ? C54 C55 1.398(12) . ? C55 C56 1.379(10) . ? C61 C62 1.397(10) . ? C61 C66 1.414(9) . ? C62 C63 1.366(12) . ? C63 C64 1.381(11) . ? C64 C65 1.376(12) . ? C65 C66 1.376(11) . ? C71 C76 1.362(9) . ? C71 C72 1.421(10) . ? C72 C73 1.401(12) . ? C73 C74 1.342(12) . ? C74 C75 1.393(13) . ? C75 C76 1.394(10) . ? C81 C82 1.389(9) . ? C81 C86 1.393(10) . ? C82 C83 1.372(13) . ? C83 C84 1.374(14) . ? C84 C85 1.395(12) . ? C85 C86 1.383(11) . ? N1 N2 1.388(7) . ? N1 C95' 1.452(7) . ? N1 C95 1.453(14) . ? N1 C91 1.458(12) . ? N1 C91' 1.496(16) . ? C91 C92 1.497(13) . ? C92 C93 1.49(2) . ? C93 C94 1.54(2) . ? C94 C95 1.490(14) . ? C91' C92' 1.500(16) . ? C92' C93' 1.55(3) . ? C93' C94' 1.47(2) . ? C94' C95' 1.492(15) . ?
1100716.cif	#------------------------------------------------------------------------------ #$Date: 2018-09-01 03:50:19 +0300 (Sat, 01 Sep 2018) $ #$Revision: 210285 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/10/07/1100716.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100716 loop_ _publ_author_name 'Akashi, Haruo' 'Isobe, Kiyoshi' 'Shibahara, Takashi' _publ_section_title ; Synthesis and characterization of a twin Cubane-type molybdenum-rhodium-sulfur cluster, [{Mo3RhCp*S4(H2O)7(O)}2]8+. X-ray structure of [{Mo3RhCpS4(H2O7O}2](CH3C6H4SO3)(8).14H2O. ; _journal_coden_ASTM INOCAJ _journal_issue 10 _journal_name_full 'Inorganic Chemistry' _journal_page_first 3494 _journal_page_last 3498 _journal_paper_doi 10.1021/ic048733y _journal_volume 44 _journal_year 2005 _chemical_formula_moiety 'C76 H142 Mo6 O54 Rh2 S16' _chemical_formula_sum 'C76 H142 Mo6 O54 Rh2 S16' _chemical_formula_weight 3214.34 _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _audit_creation_date 2004-09-16 _audit_creation_method 'by CrystalStructure 3.6.0' _cell_angle_alpha 63.704(3) _cell_angle_beta 78.688(2) _cell_angle_gamma 81.038(2) _cell_formula_units_Z 1 _cell_length_a 12.2631(8) _cell_length_b 15.911(1) _cell_length_c 17.389(3) _cell_measurement_reflns_used 7019 _cell_measurement_temperature 93.1 _cell_measurement_theta_max 27.5 _cell_measurement_theta_min 3.1 _cell_volume 2973.5(6) _computing_cell_refinement CRYSTALCLEAR _computing_data_collection CRYSTALCLEAR _computing_data_reduction CrystalStructure _computing_publication_material 'CrystalStructure 3.6.0' _computing_structure_refinement CRYSTALS _computing_structure_solution SIR92 _diffrn_detector_area_resol_mean 7.32 _diffrn_measured_fraction_theta_full 0.9960 _diffrn_measured_fraction_theta_max 0.9861 _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents 0.073 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 33644 _diffrn_reflns_theta_full 25.75 _diffrn_reflns_theta_max 27.48 _exptl_absorpt_coefficient_mu 1.249 _exptl_absorpt_correction_T_max 0.939 _exptl_absorpt_correction_T_min 0.695 _exptl_absorpt_correction_type empirical _exptl_crystal_colour black _exptl_crystal_density_diffrn 1.795 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 1628.00 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _refine_diff_density_max 2.61 _refine_diff_density_min -3.49 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_hydrogen_treatment refall _refine_ls_number_parameters 737 _refine_ls_number_reflns 11328 _refine_ls_R_factor_gt 0.0610 _refine_ls_shift/su_max 0.0000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[0.0010Fo^2^ + 1.0000\s(Fo^2^) + 0.5000]/(4Fo^2^)' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.1630 _reflns_number_gt 7661 _reflns_number_total 13440 _reflns_threshold_expression F^2^>2.0\s(F^2^) _cod_duplicate_entry 4340411 _cod_data_source_file ic048733ysi20040923_125311.cif _cod_data_source_block 010214B _cod_original_cell_volume 2973.5(5) _cod_original_formula_sum 'C38 H71 Mo3 O27 Rh1 S8' _cod_database_code 1100716 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh(1) Rh 0.01465(5) 0.18656(4) 0.63249(4) 0.0137(2) Uani 1.00 1 d . . . Mo(1) Mo 0.01154(5) 0.37297(5) 0.46407(4) 0.0129(2) Uani 1.00 1 d . . . Mo(2) Mo 0.21417(5) 0.26746(5) 0.51156(4) 0.0129(2) Uani 1.00 1 d . . . Mo(3) Mo 0.09712(5) 0.37460(5) 0.59911(4) 0.0128(2) Uani 1.00 1 d . . . S(1) S 0.1802(1) 0.4324(1) 0.4544(1) 0.0145(5) Uani 1.00 1 d . . . S(2) S 0.0679(1) 0.2145(1) 0.4839(1) 0.0152(5) Uani 1.00 1 d . . . S(3) S 0.1808(1) 0.2175(1) 0.6613(1) 0.0146(5) Uani 1.00 1 d . . . S(4) S -0.0809(1) 0.3395(1) 0.6034(1) 0.0140(5) Uani 1.00 1 d . . . S(5) S 0.2638(2) 0.7438(1) -0.3246(1) 0.0183(5) Uani 1.00 1 d . . . S(6) S 0.4775(2) 1.0366(1) -0.3047(1) 0.0173(5) Uani 1.00 1 d . . . S(7) S 0.2726(2) 0.5643(1) 0.2151(1) 0.0201(5) Uani 1.00 1 d . . . S(8) S 0.7893(2) 0.7544(1) 0.0996(1) 0.0207(5) Uani 1.00 1 d . . . O(1) O -0.1446(4) 0.3397(4) 0.4441(4) 0.019(1) Uani 1.00 1 d . . . O(2) O 0.0514(4) 0.4009(4) 0.3260(3) 0.017(1) Uani 1.00 1 d . . . O(3) O 0.2997(4) 0.1306(4) 0.5357(4) 0.021(1) Uani 1.00 1 d . . . O(4) O 0.3796(4) 0.2901(4) 0.5260(4) 0.017(1) Uani 1.00 1 d . . . O(5) O 0.2991(4) 0.2966(4) 0.3842(3) 0.016(1) Uani 1.00 1 d . . . O(6) O 0.0346(4) 0.3459(4) 0.7360(3) 0.018(1) Uani 1.00 1 d . . . O(7) O 0.0538(4) 0.5014(4) 0.5785(3) 0.018(1) Uani 1.00 1 d . . . O(8) O 0.2472(4) 0.4049(4) 0.6307(3) 0.014(1) Uani 1.00 1 d . . . O(9) O 0.3114(5) 0.6475(4) -0.3049(4) 0.022(2) Uani 1.00 1 d . . . O(10) O 0.1630(5) 0.7642(4) -0.3646(4) 0.022(2) Uani 1.00 1 d . . . O(11) O 0.3454(5) 0.8121(4) -0.3755(4) 0.024(2) Uani 1.00 1 d . . . O(12) O 0.4824(4) 1.1384(4) -0.3413(4) 0.020(1) Uani 1.00 1 d . . . O(13) O 0.3790(5) 1.0129(4) -0.3231(4) 0.024(2) Uani 1.00 1 d . . . O(14) O 0.5801(5) 0.9889(4) -0.3299(4) 0.023(2) Uani 1.00 1 d . . . O(15) O 0.2910(5) 0.6422(4) 0.2315(4) 0.024(2) Uani 1.00 1 d . . . O(16) O 0.1525(5) 0.5552(4) 0.2222(4) 0.026(2) Uani 1.00 1 d . . . O(17) O 0.3288(5) 0.4764(4) 0.2689(4) 0.023(2) Uani 1.00 1 d . . . O(18) O 0.8458(5) 0.6637(4) 0.1500(4) 0.026(2) Uani 1.00 1 d . . . O(19) O 0.8394(5) 0.8318(5) 0.0957(4) 0.028(2) Uani 1.00 1 d . . . O(20) O 0.6681(5) 0.7561(5) 0.1266(4) 0.031(2) Uani 1.00 1 d . . . O(21) O 0.8788(5) 0.4644(4) 0.2362(4) 0.027(2) Uani 1.00 1 d . . . O(22) O 0.5859(4) 0.7142(4) 0.2919(4) 0.020(1) Uani 1.00 1 d . . . O(23) O 0.4229(5) 0.5895(4) 0.3567(4) 0.025(2) Uani 1.00 1 d . . . O(24) O 0.5550(5) 0.8188(5) -0.3442(4) 0.029(2) Uani 1.00 1 d . . . O(25) O 0.3088(5) 0.9945(5) -0.5088(4) 0.030(2) Uani 1.00 1 d . . . O(26) O -0.3330(4) 0.4331(4) 0.4803(4) 0.022(2) Uani 1.00 1 d . . . O(27) O 0.4871(4) 0.5930(4) -0.4008(4) 0.021(1) Uani 1.00 1 d . . . C(1) C 0.0185(7) 0.0565(6) 0.7514(5) 0.019(2) Uani 1.00 1 d . . . C(2) C 0.0155(6) 0.0343(5) 0.6817(5) 0.018(2) Uani 1.00 1 d . . . C(3) C -0.0895(6) 0.0788(5) 0.6473(5) 0.017(2) Uani 1.00 1 d . . . C(4) C -0.1475(7) 0.1273(6) 0.6969(5) 0.021(2) Uani 1.00 1 d . . . C(5) C -0.0794(6) 0.1159(6) 0.7608(5) 0.018(2) Uani 1.00 1 d . . . C(6) C 0.1037(7) 0.0168(6) 0.8122(6) 0.025(2) Uani 1.00 1 d . . . C(7) C 0.0961(7) -0.0290(6) 0.6519(6) 0.023(2) Uani 1.00 1 d . . . C(8) C -0.1360(7) 0.0679(7) 0.5794(6) 0.027(2) Uani 1.00 1 d . . . C(9) C -0.2611(6) 0.1767(6) 0.6876(6) 0.022(2) Uani 1.00 1 d . . . C(10) C -0.1072(7) 0.1517(7) 0.8292(6) 0.027(2) Uani 1.00 1 d . . . C(11) C 0.2223(6) 0.7534(6) -0.2254(5) 0.016(2) Uani 1.00 1 d . . . C(12) C 0.1269(7) 0.7107(6) -0.1708(6) 0.022(2) Uani 1.00 1 d . . . C(13) C 0.0969(7) 0.7157(6) -0.0922(6) 0.025(2) Uani 1.00 1 d . . . C(14) C 0.1572(7) 0.7636(7) -0.0663(6) 0.026(2) Uani 1.00 1 d . . . C(15) C 0.2515(7) 0.8037(6) -0.1205(5) 0.018(2) Uani 1.00 1 d . . . C(16) C 0.2839(6) 0.8010(6) -0.2009(5) 0.018(2) Uani 1.00 1 d . . . C(17) C 0.1206(9) 0.7699(8) 0.0191(6) 0.035(3) Uani 1.00 1 d . . . C(18) C 0.4632(6) 0.9937(6) -0.1913(5) 0.016(2) Uani 1.00 1 d . . . C(19) C 0.3765(6) 1.0308(6) -0.1487(5) 0.018(2) Uani 1.00 1 d . . . C(20) C 0.3582(7) 0.9938(5) -0.0590(5) 0.017(2) Uani 1.00 1 d . . . C(21) C 0.4305(6) 0.9180(6) -0.0100(5) 0.019(2) Uani 1.00 1 d . . . C(22) C 0.5175(6) 0.8830(6) -0.0542(6) 0.020(2) Uani 1.00 1 d . . . C(23) C 0.5350(6) 0.9192(6) -0.1439(6) 0.020(2) Uani 1.00 1 d . . . C(24) C 0.4092(7) 0.8770(7) 0.0874(6) 0.025(2) Uani 1.00 1 d . . . C(25) C 0.8070(6) 0.7628(6) -0.0076(5) 0.021(2) Uani 1.00 1 d . . . C(26) C 0.8315(7) 0.8485(6) -0.0788(6) 0.022(2) Uani 1.00 1 d . . . C(27) C 0.8388(7) 0.8538(6) -0.1608(6) 0.024(2) Uani 1.00 1 d . . . C(28) C 0.8221(7) 0.7783(6) -0.1758(6) 0.023(2) Uani 1.00 1 d . . . C(29) C 0.7963(8) 0.6953(7) -0.1040(6) 0.029(3) Uani 1.00 1 d . . . C(30) C 0.7886(7) 0.6865(7) -0.0207(6) 0.029(2) Uani 1.00 1 d . . . C(31) C 0.8323(8) 0.7861(8) -0.2657(7) 0.035(3) Uani 1.00 1 d . . . C(32) C 0.3305(7) 0.5883(6) 0.1083(6) 0.023(2) Uani 1.00 1 d . . . C(33) C 0.4292(8) 0.6312(7) 0.0735(6) 0.029(2) Uani 1.00 1 d . . . C(34) C 0.4798(9) 0.6428(7) -0.0104(7) 0.033(3) Uani 1.00 1 d . . . C(35) C 0.4344(9) 0.6112(7) -0.0582(6) 0.035(3) Uani 1.00 1 d . . . C(36) C 0.3336(8) 0.5684(7) -0.0216(6) 0.029(2) Uani 1.00 1 d . . . C(37) C 0.2816(7) 0.5572(6) 0.0597(6) 0.025(2) Uani 1.00 1 d . . . C(38) C 0.4899(9) 0.6230(9) -0.1460(7) 0.045(3) Uani 1.00 1 d . . . H(1) H 0.1589 -0.0223 0.7942 0.030 Uiso 1.00 1 c R . . H(2) H 0.0684 -0.0191 0.8692 0.030 Uiso 1.00 1 c R . . H(3) H 0.1376 0.0669 0.8117 0.030 Uiso 1.00 1 c R . . H(4) H 0.0701 -0.0347 0.6065 0.030 Uiso 1.00 1 c R . . H(5) H 0.1030 -0.0893 0.6989 0.030 Uiso 1.00 1 c R . . H(6) H 0.1668 -0.0036 0.6312 0.030 Uiso 1.00 1 c R . . H(7) H -0.2073 0.1014 0.5724 0.034 Uiso 1.00 1 c R . . H(8) H -0.1428 0.0032 0.5964 0.034 Uiso 1.00 1 c R . . H(9) H -0.0874 0.0921 0.5260 0.034 Uiso 1.00 1 c R . . H(10) H -0.2823 0.2013 0.7296 0.024 Uiso 1.00 1 c R . . H(11) H -0.3128 0.1336 0.6961 0.024 Uiso 1.00 1 c R . . H(12) H -0.2607 0.2266 0.6312 0.024 Uiso 1.00 1 c R . . H(13) H -0.0497 0.1303 0.8646 0.031 Uiso 1.00 1 c R . . H(14) H -0.1757 0.1291 0.8640 0.031 Uiso 1.00 1 c R . . H(15) H -0.1142 0.2185 0.8027 0.031 Uiso 1.00 1 c R . . H(16) H 0.0836 0.6789 -0.1878 0.028 Uiso 1.00 1 c R . . H(17) H 0.0334 0.6857 -0.0546 0.031 Uiso 1.00 1 c R . . H(18) H 0.2955 0.8341 -0.1026 0.025 Uiso 1.00 1 c R . . H(19) H 0.3474 0.8313 -0.2383 0.022 Uiso 1.00 1 c R . . H(20) H 0.0709 0.8244 0.0107 0.045 Uiso 1.00 1 c R . . H(21) H 0.1840 0.7738 0.0408 0.045 Uiso 1.00 1 c R . . H(22) H 0.0838 0.7156 0.0594 0.045 Uiso 1.00 1 c R . . H(23) H 0.3290 1.0823 -0.1813 0.023 Uiso 1.00 1 c R . . H(24) H 0.2975 1.0190 -0.0304 0.022 Uiso 1.00 1 c R . . H(25) H 0.5667 0.8326 -0.0222 0.024 Uiso 1.00 1 c R . . H(26) H 0.5951 0.8938 -0.1728 0.025 Uiso 1.00 1 c R . . H(27) H 0.4479 0.9094 0.1070 0.031 Uiso 1.00 1 c R . . H(28) H 0.4348 0.8123 0.1106 0.031 Uiso 1.00 1 c R . . H(29) H 0.3315 0.8831 0.1064 0.031 Uiso 1.00 1 c R . . H(30) H 0.8427 0.9015 -0.0705 0.027 Uiso 1.00 1 c R . . H(31) H 0.8560 0.9115 -0.2091 0.030 Uiso 1.00 1 c R . . H(32) H 0.7835 0.6428 -0.1124 0.038 Uiso 1.00 1 c R . . H(33) H 0.7709 0.6287 0.0274 0.032 Uiso 1.00 1 c R . . H(34) H 0.7616 0.8066 -0.2853 0.043 Uiso 1.00 1 c R . . H(35) H 0.8567 0.7264 -0.2657 0.043 Uiso 1.00 1 c R . . H(36) H 0.8847 0.8304 -0.3029 0.043 Uiso 1.00 1 c R . . H(37) H 0.4627 0.6528 0.1056 0.035 Uiso 1.00 1 c R . . H(38) H 0.5472 0.6733 -0.0346 0.038 Uiso 1.00 1 c R . . H(39) H 0.3004 0.5465 -0.0537 0.035 Uiso 1.00 1 c R . . H(40) H 0.2129 0.5286 0.0830 0.032 Uiso 1.00 1 c R . . H(41) H 0.4635 0.6812 -0.1884 0.046 Uiso 1.00 1 c R . . H(42) H 0.4738 0.5730 -0.1569 0.046 Uiso 1.00 1 c R . . H(43) H 0.5683 0.6218 -0.1492 0.046 Uiso 1.00 1 c R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Rh(1) 0.0149(3) 0.0148(3) 0.0128(3) -0.0002(2) -0.0030(2) -0.0070(3) Mo(1) 0.0147(3) 0.0138(3) 0.0126(3) 0.0007(2) -0.0040(2) -0.0074(3) Mo(2) 0.0139(3) 0.0137(3) 0.0118(3) 0.0009(2) -0.0029(2) -0.0062(3) Mo(3) 0.0142(3) 0.0143(3) 0.0115(3) 0.0004(2) -0.0029(2) -0.0070(3) S(1) 0.0151(8) 0.017(1) 0.0130(9) 0.0016(7) -0.0039(7) -0.0076(8) S(2) 0.0193(9) 0.016(1) 0.0120(9) -0.0005(7) -0.0033(7) -0.0078(8) S(3) 0.0162(8) 0.016(1) 0.014(1) 0.0003(7) -0.0047(7) -0.0077(8) S(4) 0.0138(8) 0.016(1) 0.0136(9) 0.0018(7) -0.0033(7) -0.0084(8) S(5) 0.0204(9) 0.019(1) 0.019(1) 0.0007(8) -0.0059(8) -0.0107(9) S(6) 0.0197(9) 0.018(1) 0.015(1) 0.0004(8) -0.0049(7) -0.0080(8) S(7) 0.0208(9) 0.021(1) 0.017(1) 0.0005(8) -0.0019(8) -0.0081(9) S(8) 0.0211(9) 0.025(1) 0.016(1) 0.0031(8) -0.0066(8) -0.0090(9) O(1) 0.018(3) 0.026(3) 0.020(3) 0.000(2) -0.008(2) -0.014(3) O(2) 0.023(3) 0.018(3) 0.011(3) 0.003(2) -0.007(2) -0.008(2) O(3) 0.016(3) 0.021(3) 0.023(3) 0.005(2) -0.002(2) -0.010(3) O(4) 0.014(2) 0.019(3) 0.017(3) -0.000(2) -0.005(2) -0.007(2) O(5) 0.017(3) 0.016(3) 0.013(3) -0.001(2) 0.005(2) -0.008(2) O(6) 0.022(3) 0.025(3) 0.009(3) -0.001(2) 0.002(2) -0.010(2) O(7) 0.014(2) 0.030(3) 0.012(3) -0.003(2) -0.001(2) -0.011(2) O(8) 0.010(2) 0.014(3) 0.017(3) -0.001(2) -0.003(2) -0.006(2) O(9) 0.029(3) 0.018(3) 0.022(3) 0.000(2) -0.003(2) -0.012(3) O(10) 0.026(3) 0.023(3) 0.024(3) 0.005(2) -0.012(2) -0.015(3) O(11) 0.033(3) 0.024(3) 0.018(3) -0.004(2) -0.004(2) -0.012(3) O(12) 0.021(3) 0.020(3) 0.014(3) -0.000(2) -0.002(2) -0.005(2) O(13) 0.025(3) 0.027(3) 0.020(3) -0.005(2) -0.009(2) -0.006(3) O(14) 0.026(3) 0.027(3) 0.017(3) 0.004(2) -0.003(2) -0.012(3) O(15) 0.027(3) 0.027(3) 0.021(3) 0.001(2) -0.002(2) -0.014(3) O(16) 0.020(3) 0.029(3) 0.028(3) -0.005(2) 0.000(2) -0.011(3) O(17) 0.024(3) 0.021(3) 0.019(3) 0.005(2) -0.003(2) -0.005(3) O(18) 0.030(3) 0.029(3) 0.016(3) -0.001(3) -0.009(2) -0.006(3) O(19) 0.038(3) 0.027(3) 0.024(3) 0.002(3) -0.012(3) -0.012(3) O(20) 0.027(3) 0.045(4) 0.019(3) 0.001(3) -0.003(2) -0.014(3) O(21) 0.030(3) 0.024(3) 0.026(3) -0.001(3) -0.011(3) -0.007(3) O(22) 0.023(3) 0.018(3) 0.019(3) -0.003(2) -0.007(2) -0.006(2) O(23) 0.023(3) 0.025(3) 0.026(3) -0.001(2) -0.005(2) -0.010(3) O(24) 0.030(3) 0.027(3) 0.035(4) 0.002(3) -0.002(3) -0.019(3) O(25) 0.040(4) 0.026(3) 0.023(3) -0.005(3) -0.003(3) -0.011(3) O(26) 0.018(3) 0.026(3) 0.025(3) -0.001(2) -0.003(2) -0.013(3) O(27) 0.018(3) 0.024(3) 0.019(3) -0.003(2) 0.001(2) -0.008(3) C(1) 0.026(4) 0.013(4) 0.013(4) -0.005(3) 0.002(3) -0.001(3) C(2) 0.023(4) 0.006(4) 0.018(4) -0.003(3) -0.003(3) 0.002(3) C(3) 0.025(4) 0.005(4) 0.016(4) -0.004(3) -0.003(3) 0.000(3) C(4) 0.026(4) 0.017(4) 0.017(4) -0.008(3) -0.004(3) -0.001(3) C(5) 0.019(4) 0.013(4) 0.011(4) -0.003(3) 0.004(3) 0.003(3) C(6) 0.022(4) 0.026(5) 0.026(5) -0.005(3) -0.008(3) -0.007(4) C(7) 0.025(4) 0.021(4) 0.030(5) -0.007(3) 0.008(4) -0.019(4) C(8) 0.030(4) 0.026(5) 0.029(5) -0.013(4) -0.010(4) -0.010(4) C(9) 0.007(3) 0.022(4) 0.031(5) -0.004(3) -0.007(3) -0.002(4) C(10) 0.031(5) 0.025(5) 0.021(5) 0.005(4) 0.002(4) -0.011(4) C(11) 0.019(4) 0.014(4) 0.016(4) 0.005(3) -0.010(3) -0.006(3) C(12) 0.019(4) 0.023(5) 0.028(5) 0.001(3) -0.005(3) -0.015(4) C(13) 0.023(4) 0.023(5) 0.031(5) 0.004(3) -0.004(4) -0.015(4) C(14) 0.026(4) 0.027(5) 0.028(5) 0.010(4) -0.007(4) -0.016(4) C(15) 0.027(4) 0.017(4) 0.019(4) 0.002(3) -0.009(3) -0.015(4) C(16) 0.017(4) 0.018(4) 0.019(4) 0.000(3) -0.003(3) -0.008(3) C(17) 0.046(6) 0.039(6) 0.027(5) 0.015(5) -0.013(4) -0.026(5) C(18) 0.013(3) 0.018(4) 0.015(4) -0.004(3) -0.002(3) -0.004(3) C(19) 0.020(4) 0.018(4) 0.019(4) -0.004(3) -0.001(3) -0.011(3) C(20) 0.028(4) 0.010(4) 0.016(4) -0.004(3) -0.000(3) -0.008(3) C(21) 0.021(4) 0.027(5) 0.018(4) -0.011(3) 0.001(3) -0.016(4) C(22) 0.018(4) 0.020(4) 0.023(5) 0.004(3) -0.013(3) -0.008(4) C(23) 0.016(4) 0.025(5) 0.021(4) 0.003(3) -0.004(3) -0.013(4) C(24) 0.025(4) 0.032(5) 0.022(5) -0.009(4) -0.004(3) -0.012(4) C(25) 0.017(4) 0.029(5) 0.015(4) 0.004(3) -0.002(3) -0.009(4) C(26) 0.027(4) 0.019(4) 0.021(4) -0.002(3) -0.004(3) -0.010(4) C(27) 0.030(4) 0.020(4) 0.024(5) 0.005(4) -0.006(4) -0.012(4) C(28) 0.023(4) 0.023(5) 0.028(5) 0.003(3) -0.012(4) -0.012(4) C(29) 0.042(5) 0.031(5) 0.023(5) -0.008(4) -0.005(4) -0.017(4) C(30) 0.034(5) 0.021(5) 0.026(5) -0.006(4) -0.006(4) -0.003(4) C(31) 0.036(5) 0.039(6) 0.031(5) 0.007(4) -0.016(4) -0.014(5) C(32) 0.022(4) 0.019(4) 0.024(5) -0.001(3) 0.003(3) -0.008(4) C(33) 0.034(5) 0.028(5) 0.026(5) 0.001(4) 0.002(4) -0.015(4) C(34) 0.044(5) 0.019(5) 0.030(5) 0.002(4) 0.001(4) -0.010(4) C(35) 0.048(6) 0.035(6) 0.012(4) 0.017(4) -0.006(4) -0.008(4) C(36) 0.034(5) 0.036(5) 0.018(5) 0.010(4) -0.002(4) -0.018(4) C(37) 0.028(4) 0.021(4) 0.030(5) 0.011(4) -0.010(4) -0.018(4) C(38) 0.043(6) 0.049(7) 0.025(5) 0.016(5) -0.000(4) -0.006(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Mo Mo -1.683 0.686 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Rh Rh -1.118 0.919 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Rh(1) Mo(2) Mo(1) 65.41(2) ? . . . Rh(1) Mo(2) Mo(3) 64.61(2) ? . . . Rh(1) Mo(2) S(2) 52.55(5) ? . . . S(2) Rh(1) Mo(2) 50.07(6) ? . . . Rh(1) Mo(2) S(3) 51.73(5) ? . . . S(3) Rh(1) Mo(2) 50.76(5) ? . . . S(4) Rh(1) Mo(2) 92.38(4) ? . . . C(1) Rh(1) Mo(2) 124.1(2) ? . . . C(2) Rh(1) Mo(2) 114.5(2) ? . . . C(3) Rh(1) Mo(2) 133.0(2) ? . . . C(4) Rh(1) Mo(2) 167.0(3) ? . . . C(5) Rh(1) Mo(2) 154.1(2) ? . . . Rh(1) Mo(2) S(1) 107.21(5) ? . . . Rh(1) Mo(2) O(3) 92.7(1) ? . . . Rh(1) Mo(2) O(4) 134.7(1) ? . . . Rh(1) Mo(2) O(5) 143.0(2) ? . . . Rh(1) S(2) Mo(1) 81.17(8) ? . . . Rh(1) S(2) Mo(2) 77.38(8) ? . . . S(3) Rh(1) S(2) 100.09(7) ? . . . S(4) Rh(1) S(2) 95.62(7) ? . . . C(1) Rh(1) S(2) 130.9(3) ? . . . C(2) Rh(1) S(2) 95.3(3) ? . . . C(3) Rh(1) S(2) 88.2(2) ? . . . C(4) Rh(1) S(2) 117.0(3) ? . . . C(5) Rh(1) S(2) 152.5(3) ? . . . Rh(1) S(3) Mo(2) 77.52(7) ? . . . Rh(1) S(3) Mo(3) 80.80(6) ? . . . S(4) Rh(1) S(3) 96.54(8) ? . . . C(1) Rh(1) S(3) 86.9(3) ? . . . C(2) Rh(1) S(3) 107.2(2) ? . . . C(3) Rh(1) S(3) 146.3(2) ? . . . C(4) Rh(1) S(3) 142.2(3) ? . . . C(5) Rh(1) S(3) 103.7(3) ? . . . Rh(1) S(4) Mo(1) 82.19(7) ? . . . Rh(1) S(4) Mo(3) 81.32(6) ? . . . C(1) Rh(1) S(4) 132.1(2) ? . . . C(2) Rh(1) S(4) 151.7(2) ? . . . C(3) Rh(1) S(4) 115.2(2) ? . . . C(4) Rh(1) S(4) 87.4(2) ? . . . C(5) Rh(1) S(4) 95.3(2) ? . . . Rh(1) C(1) C(2) 71.0(4) ? . . . C(2) Rh(1) C(1) 37.8(4) ? . . . C(3) Rh(1) C(1) 64.0(3) ? . . . C(4) Rh(1) C(1) 63.9(3) ? . . . Rh(1) C(1) C(5) 70.5(4) ? . . . C(5) Rh(1) C(1) 38.5(3) ? . . . Rh(1) C(1) C(6) 129.6(6) ? . . . Rh(1) C(2) C(1) 71.3(5) ? . . . Rh(1) C(2) C(3) 70.7(4) ? . . . C(3) Rh(1) C(2) 39.3(3) ? . . . C(4) Rh(1) C(2) 64.4(3) ? . . . C(5) Rh(1) C(2) 64.5(3) ? . . . Rh(1) C(2) C(7) 127.4(5) ? . . . Rh(1) C(3) C(2) 70.0(5) ? . . . Rh(1) C(3) C(4) 71.8(5) ? . . . C(4) Rh(1) C(3) 37.7(4) ? . . . C(5) Rh(1) C(3) 64.3(4) ? . . . Rh(1) C(3) C(8) 128.8(5) ? . . . Rh(1) C(4) C(3) 70.5(5) ? . . . Rh(1) C(4) C(5) 69.6(4) ? . . . C(5) Rh(1) C(4) 38.6(4) ? . . . Rh(1) C(4) C(9) 128.0(5) ? . . . Rh(1) C(5) C(1) 71.1(4) ? . . . Rh(1) C(5) C(4) 71.8(4) ? . . . Rh(1) C(5) C(10) 126.1(6) ? . . . Mo(1) Mo(2) Mo(3) 58.69(3) ? . . . Mo(3) Mo(1) Mo(2) 60.69(3) ? . . . Mo(1) Mo(2) S(2) 54.57(5) ? . . . S(2) Mo(1) Mo(2) 51.77(6) ? . . . Mo(1) Mo(2) S(3) 100.90(5) ? . . . S(4) Mo(1) Mo(2) 97.30(5) ? . . . Mo(1) Mo(2) S(1) 53.13(5) ? . . . S(1) Mo(1) Mo(2) 53.30(5) ? . . . O(1) Mo(1) Mo(2) 133.8(2) ? . . . O(2) Mo(1) Mo(2) 95.6(1) ? . . . Mo(1) Mo(2) O(3) 141.3(2) ? . . . Mo(1) Mo(2) O(4) 138.7(2) ? . . . Mo(1) Mo(2) O(5) 97.6(1) ? . . . Mo(1) Mo(3) Mo(2) 60.62(3) ? . . . S(2) Mo(1) Mo(3) 100.19(6) ? . . . Mo(1) Mo(3) S(3) 100.96(7) ? . . . Mo(1) Mo(3) S(4) 53.57(6) ? . . . S(4) Mo(1) Mo(3) 53.29(6) ? . . . Mo(1) Mo(3) S(1) 54.13(6) ? . . . S(1) Mo(1) Mo(3) 53.55(5) ? . . . O(1) Mo(1) Mo(3) 137.1(2) ? . . . O(2) Mo(1) Mo(3) 143.0(2) ? . . . Mo(1) Mo(3) O(7) 98.3(2) ? . . . Mo(1) Mo(3) O(6) 135.8(2) ? . . . Mo(1) Mo(3) O(8) 142.0(1) ? . . . Mo(1) S(1) Mo(2) 73.57(7) ? . . . Mo(1) S(1) Mo(3) 72.31(6) ? . . . S(2) Mo(1) S(1) 103.07(7) ? . . . S(4) Mo(1) S(1) 106.15(8) ? . . . O(1) Mo(1) S(1) 167.7(1) ? . . . O(2) Mo(1) S(1) 89.8(2) ? . . . Mo(1) S(2) Mo(2) 73.66(8) ? . . . S(4) Mo(1) S(2) 97.78(7) ? . . . O(1) Mo(1) S(2) 82.1(2) ? . . . O(2) Mo(1) S(2) 82.3(2) ? . . . Mo(1) S(4) Mo(3) 73.13(5) ? . . . O(1) Mo(1) S(4) 83.9(2) ? . . . O(2) Mo(1) S(4) 163.5(2) ? . . . O(2) Mo(1) O(1) 79.8(2) ? . . . S(2) Mo(2) Mo(3) 100.73(6) ? . . . Mo(2) Mo(3) S(3) 52.32(6) ? . . . S(3) Mo(2) Mo(3) 54.25(5) ? . . . Mo(2) Mo(3) S(4) 97.44(7) ? . . . Mo(2) Mo(3) S(1) 53.39(6) ? . . . S(1) Mo(2) Mo(3) 52.66(5) ? . . . Mo(2) Mo(3) O(7) 140.1(2) ? . . . O(3) Mo(2) Mo(3) 141.5(2) ? . . . O(4) Mo(2) Mo(3) 94.5(2) ? . . . O(5) Mo(2) Mo(3) 136.0(2) ? . . . Mo(2) Mo(3) O(6) 135.3(2) ? . . . Mo(2) Mo(3) O(8) 95.0(2) ? . . . Mo(2) S(1) Mo(3) 73.95(5) ? . . . S(2) Mo(2) S(1) 105.59(7) ? . . . S(3) Mo(2) S(1) 104.48(8) ? . . . O(3) Mo(2) S(1) 160.1(1) ? . . . O(4) Mo(2) S(1) 85.9(2) ? . . . O(5) Mo(2) S(1) 83.4(2) ? . . . S(3) Mo(2) S(2) 103.50(7) ? . . . O(3) Mo(2) S(2) 86.7(2) ? . . . O(4) Mo(2) S(2) 164.5(2) ? . . . O(5) Mo(2) S(2) 90.6(2) ? . . . Mo(2) S(3) Mo(3) 73.43(5) ? . . . O(3) Mo(2) S(3) 87.2(2) ? . . . O(4) Mo(2) S(3) 83.2(2) ? . . . O(5) Mo(2) S(3) 161.0(1) ? . . . O(4) Mo(2) O(3) 79.5(2) ? . . . O(5) Mo(2) O(3) 80.9(2) ? . . . O(5) Mo(2) O(4) 80.2(2) ? . . . S(3) Mo(3) S(1) 103.33(7) ? . . . S(4) Mo(3) S(1) 107.00(8) ? . . . O(7) Mo(3) S(1) 86.7(2) ? . . . O(6) Mo(3) S(1) 167.4(2) ? . . . O(8) Mo(3) S(1) 88.2(1) ? . . . S(4) Mo(3) S(3) 98.34(7) ? . . . O(7) Mo(3) S(3) 160.6(2) ? . . . O(6) Mo(3) S(3) 83.3(2) ? . . . O(8) Mo(3) S(3) 81.7(1) ? . . . O(7) Mo(3) S(4) 94.4(2) ? . . . O(6) Mo(3) S(4) 82.2(2) ? . . . O(8) Mo(3) S(4) 164.3(2) ? . . . O(7) Mo(3) O(6) 84.0(2) ? . . . O(8) Mo(3) O(6) 82.1(2) ? . . . O(8) Mo(3) O(7) 82.2(2) ? . . . O(10) S(5) O(9) 111.3(4) ? . . . O(11) S(5) O(9) 112.0(3) ? . . . C(11) S(5) O(9) 107.7(4) ? . . . O(11) S(5) O(10) 112.5(3) ? . . . C(11) S(5) O(10) 106.3(4) ? . . . C(11) S(5) O(11) 106.6(4) ? . . . S(5) C(11) C(12) 119.2(8) ? . . . S(5) C(11) C(16) 120.6(6) ? . . . O(13) S(6) O(12) 111.1(3) ? . . . O(14) S(6) O(12) 112.9(3) ? . . . C(18) S(6) O(12) 107.5(4) ? . . . O(14) S(6) O(13) 112.7(4) ? . . . C(18) S(6) O(13) 106.1(4) ? . . . C(18) S(6) O(14) 106.0(3) ? . . . S(6) C(18) C(19) 119.5(6) ? . . . S(6) C(18) C(23) 120.5(7) ? . . . O(17) S(7) O(15) 112.7(4) ? . . . O(16) S(7) O(15) 111.7(4) ? . . . C(32) S(7) O(15) 107.5(4) ? . . . O(17) S(7) O(16) 111.4(3) ? . . . C(32) S(7) O(16) 106.8(4) ? . . . C(32) S(7) O(17) 106.3(4) ? . . . S(7) C(32) C(33) 120.1(9) ? . . . S(7) C(32) C(37) 120.0(6) ? . . . O(19) S(8) O(18) 112.3(4) ? . . . O(20) S(8) O(18) 111.9(3) ? . . . C(25) S(8) O(18) 105.3(4) ? . . . O(20) S(8) O(19) 114.2(4) ? . . . C(25) S(8) O(19) 107.6(4) ? . . . C(25) S(8) O(20) 104.6(4) ? . . . S(8) C(25) C(26) 119.9(9) ? . . . S(8) C(25) C(30) 119.8(6) ? . . . C(1) C(2) C(3) 107.2(7) ? . . . C(5) C(1) C(2) 109.4(8) ? . . . C(6) C(1) C(2) 125.7(8) ? . . . C(1) C(2) C(7) 127.9(8) ? . . . C(1) C(5) C(4) 107.2(9) ? . . . C(6) C(1) C(5) 124.6(9) ? . . . C(1) C(5) C(10) 125.0(8) ? . . . C(2) C(3) C(4) 108.0(9) ? . . . C(7) C(2) C(3) 124.7(9) ? . . . C(2) C(3) C(8) 127.4(8) ? . . . C(3) C(4) C(5) 108.1(7) ? . . . C(8) C(3) C(4) 124.3(7) ? . . . C(3) C(4) C(9) 125.7(9) ? . . . C(9) C(4) C(5) 126.1(9) ? . . . C(4) C(5) C(10) 127.6(7) ? . . . C(16) C(11) C(12) 120.2(9) ? . . . C(11) C(12) C(13) 118(1) ? . . . C(11) C(16) C(15) 119.1(7) ? . . . C(12) C(13) C(14) 121.9(8) ? . . . C(13) C(14) C(15) 118(1) ? . . . C(13) C(14) C(17) 120.6(8) ? . . . C(14) C(15) C(16) 121(1) ? . . . C(17) C(14) C(15) 121(1) ? . . . C(23) C(18) C(19) 119.9(8) ? . . . C(18) C(19) C(20) 120.8(7) ? . . . C(18) C(23) C(22) 119.3(8) ? . . . C(19) C(20) C(21) 119.8(8) ? . . . C(20) C(21) C(22) 118.3(8) ? . . . C(20) C(21) C(24) 119.6(8) ? . . . C(21) C(22) C(23) 121.9(7) ? . . . C(24) C(21) C(22) 122.1(7) ? . . . C(30) C(25) C(26) 120.1(9) ? . . . C(25) C(26) C(27) 118(1) ? . . . C(25) C(30) C(29) 119.5(8) ? . . . C(26) C(27) C(28) 122.8(8) ? . . . C(27) C(28) C(29) 117(1) ? . . . C(27) C(28) C(31) 121.4(8) ? . . . C(28) C(29) C(30) 122(1) ? . . . C(31) C(28) C(29) 121(1) ? . . . C(37) C(32) C(33) 119.8(9) ? . . . C(32) C(33) C(34) 119(1) ? . . . C(32) C(37) C(36) 119.7(8) ? . . . C(33) C(34) C(35) 121.9(9) ? . . . C(34) C(35) C(38) 121(1) ? . . . C(34) C(35) C(36) 117.7(9) ? . . . C(35) C(36) C(37) 121(1) ? . . . C(38) C(35) C(36) 121(1) ? . . . C(1) C(6) H(3) 109.3308 ? . . . C(1) C(6) H(1) 109.4681 ? . . . C(1) C(6) H(2) 109.4691 ? . . . C(2) C(7) H(6) 109.4484 ? . . . C(2) C(7) H(4) 109.5468 ? . . . C(2) C(7) H(5) 109.4630 ? . . . C(3) C(8) H(9) 109.6008 ? . . . C(3) C(8) H(7) 109.5284 ? . . . C(3) C(8) H(8) 109.4718 ? . . . C(4) C(9) H(12) 109.5946 ? . . . C(4) C(9) H(10) 109.4789 ? . . . C(4) C(9) H(11) 109.4704 ? . . . C(5) C(10) H(15) 109.5474 ? . . . C(5) C(10) H(13) 109.6461 ? . . . C(5) C(10) H(14) 109.4681 ? . . . H(3) C(6) H(1) 109.4748 ? . . . H(2) C(6) H(1) 109.4735 ? . . . H(3) C(6) H(2) 109.6109 ? . . . H(6) C(7) H(4) 109.4713 ? . . . H(5) C(7) H(4) 109.4396 ? . . . H(6) C(7) H(5) 109.4581 ? . . . H(9) C(8) H(7) 109.4742 ? . . . H(8) C(8) H(7) 109.4425 ? . . . H(9) C(8) H(8) 109.3093 ? . . . H(12) C(9) H(10) 109.4732 ? . . . H(11) C(9) H(10) 109.4659 ? . . . H(12) C(9) H(11) 109.3441 ? . . . H(15) C(10) H(13) 109.4703 ? . . . H(14) C(10) H(13) 109.3851 ? . . . H(15) C(10) H(14) 109.3097 ? . . . C(11) C(12) H(16) 120.5205 ? . . . C(11) C(16) H(19) 120.4508 ? . . . H(16) C(12) C(13) 120.5191 ? . . . C(12) C(13) H(17) 119.0730 ? . . . H(17) C(13) C(14) 119.0723 ? . . . C(14) C(15) H(18) 119.1172 ? . . . C(14) C(17) H(21) 109.4744 ? . . . C(14) C(17) H(22) 109.5352 ? . . . C(14) C(17) H(20) 109.2602 ? . . . C(15) C(16) H(19) 120.4563 ? . . . H(18) C(15) C(16) 119.1146 ? . . . H(21) C(17) H(20) 109.5748 ? . . . H(22) C(17) H(20) 109.4723 ? . . . H(22) C(17) H(21) 109.5101 ? . . . C(18) C(19) H(23) 119.6079 ? . . . C(18) C(23) H(26) 120.3594 ? . . . H(23) C(19) C(20) 119.6098 ? . . . C(19) C(20) H(24) 120.0867 ? . . . H(24) C(20) C(21) 120.0870 ? . . . C(21) C(22) H(25) 119.0566 ? . . . C(21) C(24) H(28) 109.4717 ? . . . C(21) C(24) H(29) 109.7778 ? . . . C(21) C(24) H(27) 109.5595 ? . . . C(22) C(23) H(26) 120.3648 ? . . . H(25) C(22) C(23) 119.0579 ? . . . H(28) C(24) H(27) 109.4276 ? . . . H(29) C(24) H(27) 109.4691 ? . . . H(29) C(24) H(28) 109.1204 ? . . . C(25) C(26) H(30) 120.8306 ? . . . C(25) C(30) H(33) 120.2704 ? . . . H(30) C(26) C(27) 120.8376 ? . . . C(26) C(27) H(31) 118.5967 ? . . . H(31) C(27) C(28) 118.5935 ? . . . C(28) C(29) H(32) 118.9516 ? . . . C(28) C(31) H(34) 109.2295 ? . . . C(28) C(31) H(35) 109.4685 ? . . . C(28) C(31) H(36) 109.2748 ? . . . C(29) C(30) H(33) 120.2696 ? . . . H(32) C(29) C(30) 118.9498 ? . . . H(35) C(31) H(34) 109.5916 ? . . . H(36) C(31) H(34) 109.4766 ? . . . H(36) C(31) H(35) 109.7845 ? . . . C(32) C(33) H(37) 120.4022 ? . . . C(32) C(37) H(40) 120.1498 ? . . . H(37) C(33) C(34) 120.3973 ? . . . C(33) C(34) H(38) 119.0358 ? . . . H(38) C(34) C(35) 119.0479 ? . . . C(35) C(36) H(39) 119.1743 ? . . . C(35) C(38) H(41) 109.7109 ? . . . C(35) C(38) H(42) 109.4658 ? . . . C(35) C(38) H(43) 109.5984 ? . . . C(36) C(37) H(40) 120.1361 ? . . . H(39) C(36) C(37) 119.1788 ? . . . H(42) C(38) H(41) 109.3538 ? . . . H(43) C(38) H(41) 109.4660 ? . . . H(43) C(38) H(42) 109.2310 ? . . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Rh(1) Mo(2) 2.9377(8) ? . . Rh(1) S(2) 2.390(2) ? . . Rh(1) S(3) 2.362(2) ? . . Rh(1) S(4) 2.409(2) ? . . Rh(1) C(1) 2.186(7) ? . . Rh(1) C(2) 2.181(8) ? . . Rh(1) C(3) 2.191(9) ? . . Rh(1) C(4) 2.208(8) ? . . Rh(1) C(5) 2.178(7) ? . . Mo(1) Mo(2) 2.8199(8) ? . . Mo(1) Mo(3) 2.765(1) ? . . Mo(1) S(1) 2.352(2) ? . . Mo(1) S(2) 2.394(2) ? . . Mo(1) S(4) 2.325(2) ? . . Mo(1) O(1) 2.192(6) ? . . Mo(1) O(2) 2.205(6) ? . . Mo(2) Mo(3) 2.822(1) ? . . Mo(2) S(1) 2.357(2) ? . . Mo(2) S(2) 2.309(2) ? . . Mo(2) S(3) 2.330(2) ? . . Mo(2) O(3) 2.162(6) ? . . Mo(2) O(4) 2.194(6) ? . . Mo(2) O(5) 2.130(5) ? . . Mo(3) S(1) 2.335(2) ? . . Mo(3) S(3) 2.389(2) ? . . Mo(3) S(4) 2.316(2) ? . . Mo(3) O(6) 2.213(6) ? . . Mo(3) O(7) 1.892(6) ? . . Mo(3) O(8) 2.198(6) ? . . S(5) O(9) 1.463(6) ? . . S(5) O(10) 1.460(7) ? . . S(5) O(11) 1.450(6) ? . . S(5) C(11) 1.77(1) ? . . S(6) O(12) 1.461(6) ? . . S(6) O(13) 1.451(7) ? . . S(6) O(14) 1.461(6) ? . . S(6) C(18) 1.758(9) ? . . S(7) O(15) 1.448(8) ? . . S(7) O(16) 1.477(6) ? . . S(7) O(17) 1.449(5) ? . . S(7) C(32) 1.743(9) ? . . S(8) O(18) 1.462(6) ? . . S(8) O(19) 1.432(8) ? . . S(8) O(20) 1.468(6) ? . . S(8) C(25) 1.78(1) ? . . C(1) C(2) 1.41(2) ? . . C(1) C(5) 1.44(1) ? . . C(1) C(6) 1.50(1) ? . . C(2) Rh(1) 2.181(8) ? . . C(2) C(1) 1.41(2) ? . . C(2) C(3) 1.47(1) ? . . C(2) C(7) 1.49(1) ? . . C(3) C(2) 1.47(1) ? . . C(3) C(4) 1.42(1) ? . . C(3) C(8) 1.49(2) ? . . C(4) C(5) 1.45(1) ? . . C(4) C(9) 1.49(1) ? . . C(5) C(10) 1.50(2) ? . . C(7) C(2) 1.49(1) ? . . C(11) C(12) 1.40(1) ? . . C(11) C(16) 1.38(1) ? . . C(12) C(13) 1.38(2) ? . . C(13) C(14) 1.39(2) ? . . C(14) C(15) 1.38(1) ? . . C(14) C(17) 1.51(2) ? . . C(15) C(16) 1.40(1) ? . . C(18) C(19) 1.38(1) ? . . C(18) C(23) 1.40(1) ? . . C(19) C(20) 1.39(1) ? . . C(20) C(21) 1.42(1) ? . . C(21) C(22) 1.38(1) ? . . C(21) C(24) 1.50(1) ? . . C(22) C(23) 1.39(1) ? . . C(25) C(26) 1.40(1) ? . . C(25) C(30) 1.39(2) ? . . C(26) C(27) 1.38(2) ? . . C(27) C(28) 1.39(2) ? . . C(28) C(29) 1.38(1) ? . . C(28) C(31) 1.49(2) ? . . C(29) C(30) 1.38(2) ? . . C(32) C(33) 1.38(1) ? . . C(32) C(37) 1.41(2) ? . . C(33) C(34) 1.41(1) ? . . C(34) C(35) 1.38(2) ? . . C(35) C(36) 1.40(1) ? . . C(35) C(38) 1.49(2) ? . . C(36) C(37) 1.38(1) ? . . C(6) H(1) 0.9500 ? . . C(6) H(2) 0.9499 ? . . C(6) H(3) 0.9500 ? . . C(7) H(4) 0.9500 ? . . C(7) H(5) 0.9500 ? . . C(7) H(6) 0.9500 ? . . C(8) H(7) 0.9501 ? . . C(8) H(8) 0.9501 ? . . C(8) H(9) 0.9501 ? . . C(9) H(10) 0.9501 ? . . C(9) H(11) 0.9501 ? . . C(9) H(12) 0.9499 ? . . C(10) H(13) 0.9500 ? . . C(10) H(14) 0.9500 ? . . C(10) H(15) 0.9500 ? . . C(12) H(16) 0.9501 ? . . C(13) H(17) 0.9500 ? . . C(15) H(18) 0.9500 ? . . C(16) H(19) 0.9500 ? . . C(17) H(20) 0.9500 ? . . C(17) H(21) 0.9500 ? . . C(17) H(22) 0.9500 ? . . C(19) H(23) 0.9500 ? . . C(20) H(24) 0.9499 ? . . C(22) H(25) 0.9500 ? . . C(23) H(26) 0.9501 ? . . C(24) H(27) 0.9499 ? . . C(24) H(28) 0.9500 ? . . C(24) H(29) 0.9500 ? . . C(26) H(30) 0.9500 ? . . C(27) H(31) 0.9500 ? . . C(29) H(32) 0.9500 ? . . C(30) H(33) 0.9499 ? . . C(31) H(34) 0.9500 ? . . C(31) H(35) 0.9500 ? . . C(31) H(36) 0.9501 ? . . C(33) H(37) 0.9500 ? . . C(34) H(38) 0.9500 ? . . C(36) H(39) 0.9501 ? . . C(37) H(40) 0.9500 ? . . C(38) H(41) 0.9501 ? . . C(38) H(42) 0.9500 ? . . C(38) H(43) 0.9500 ? . . H(1) C(6) 0.9500 ? . . H(3) C(6) 0.9500 ? . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Rh(1) Mo(1) 3.1125(7) ? . . Rh(1) Mo(3) 3.080(1) ? . . Rh(1) C(6) 3.346(8) ? . . Rh(1) C(7) 3.30(1) ? . . Rh(1) C(8) 3.34(1) ? . . Rh(1) C(9) 3.337(7) ? . . Rh(1) C(10) 3.288(9) ? . . Mo(1) O(7) 3.569(8) ? . . S(1) O(2) 3.217(7) ? . . S(1) O(4) 3.102(5) ? . . S(1) O(5) 2.989(7) ? . . S(1) O(7) 2.919(7) ? . . S(1) O(8) 3.155(7) ? . . S(1) O(17) 3.211(6) ? . . S(2) S(4) 3.556(3) ? . . S(2) O(1) 3.017(5) ? . . S(2) O(2) 3.031(5) ? . . S(2) O(3) 3.072(6) ? . . S(2) O(5) 3.158(5) ? . . S(2) C(2) 3.381(7) ? . . S(2) C(3) 3.190(7) ? . . S(2) C(8) 3.347(9) ? . . S(3) S(4) 3.561(2) ? . . S(3) O(3) 3.101(7) ? . . S(3) O(4) 3.005(5) ? . . S(3) O(6) 3.061(7) ? . . S(3) O(8) 3.003(7) ? . . S(3) C(1) 3.129(9) ? . . S(3) C(5) 3.571(8) ? . . S(3) C(6) 3.244(8) ? . . S(4) O(1) 3.020(8) ? . . S(4) O(6) 2.979(7) ? . . S(4) O(7) 3.100(7) ? . . S(4) C(4) 3.192(9) ? . . S(4) C(5) 3.394(7) ? . . S(4) C(9) 3.300(9) ? . . S(5) O(1) 3.530(8) ? . 56502 S(5) O(21) 3.555(7) ? . 66502 S(5) C(12) 2.742(9) ? . . S(5) C(16) 2.74(1) ? . . S(6) O(3) 3.519(6) ? . 56401 S(6) C(19) 2.719(9) ? . . S(6) C(23) 2.745(8) ? . . S(7) O(23) 3.537(8) ? . . S(7) C(33) 2.710(9) ? . . S(7) C(37) 2.73(1) ? . . S(8) C(26) 2.761(8) ? . . S(8) C(30) 2.75(1) ? . . O(1) S(5) 3.530(8) ? . 56502 O(1) O(2) 2.822(7) ? . . O(1) O(9) 3.39(1) ? . 56502 O(1) O(10) 2.64(1) ? . 56502 O(1) O(21) 3.240(8) ? . 45501 O(1) O(26) 2.670(8) ? . . O(2) O(5) 3.339(7) ? . . O(2) O(16) 2.640(8) ? . . O(2) O(17) 3.591(8) ? . . O(2) O(21) 2.678(9) ? . 45501 O(2) C(31) 3.58(1) ? . 66502 O(3) O(4) 2.79(1) ? . . O(3) O(5) 2.784(7) ? . . O(3) O(24) 3.263(9) ? . 66502 O(3) C(7) 3.49(1) ? . . O(4) O(5) 2.785(9) ? . . O(4) O(8) 3.187(9) ? . . O(4) O(27) 2.615(7) ? . 66502 O(5) O(17) 2.701(7) ? . . O(5) O(24) 2.584(9) ? . 66502 O(5) O(27) 3.495(9) ? . 66502 O(5) C(31) 3.60(2) ? . 66502 O(6) O(7) 2.757(6) ? . . O(6) O(8) 2.898(7) ? . . O(6) C(10) 3.37(1) ? . . O(7) O(8) 2.698(7) ? . . O(9) O(1) 3.39(1) ? . 56502 O(9) O(10) 2.412(7) ? . . O(9) O(11) 2.415(8) ? . . O(9) O(21) 2.890(9) ? . 66502 O(9) O(27) 2.733(8) ? . . O(9) C(11) 2.62(1) ? . . O(9) C(12) 3.30(1) ? . . O(9) C(16) 3.57(1) ? . . O(10) O(1) 2.64(1) ? . 56502 O(10) O(11) 2.420(9) ? . . O(10) O(21) 3.379(8) ? . 66502 O(10) C(7) 3.39(1) ? . 56401 O(10) C(8) 3.54(1) ? . 56502 O(10) C(11) 2.59(1) ? . . O(10) C(12) 3.04(1) ? . . O(11) O(24) 2.76(1) ? . . O(11) O(25) 2.835(7) ? . . O(11) C(11) 2.587(9) ? . . O(11) C(16) 2.91(1) ? . . O(12) O(3) 3.44(1) ? . 56401 O(12) O(4) 2.828(7) ? . 56401 O(12) O(13) 2.40(1) ? . . O(12) O(14) 2.434(9) ? . . O(12) C(9) 3.47(1) ? . 66401 O(12) C(18) 2.601(8) ? . . O(12) C(19) 3.120(9) ? . . O(13) O(3) 2.604(8) ? . 56401 O(13) O(14) 2.423(8) ? . . O(13) O(24) 3.60(1) ? . . O(13) C(16) 3.34(1) ? . . O(13) C(18) 2.57(1) ? . . O(13) C(19) 3.16(1) ? . . O(13) C(23) 3.59(1) ? . . O(14) O(24) 2.89(1) ? . . O(14) C(18) 2.58(1) ? . . O(14) C(23) 2.88(1) ? . . O(15) O(16) 2.42(1) ? . . O(15) O(17) 2.412(9) ? . . O(15) O(23) 2.72(1) ? . . O(15) C(32) 2.58(1) ? . . O(15) C(33) 2.99(1) ? . . O(16) O(17) 2.418(8) ? . . O(16) C(32) 2.590(9) ? . . O(16) C(37) 2.94(1) ? . . O(17) O(23) 3.27(1) ? . . O(17) O(27) 3.253(9) ? . 66502 O(17) C(32) 2.56(1) ? . . O(17) C(33) 3.319(9) ? . . O(17) C(37) 3.42(1) ? . . O(17) C(38) 3.47(1) ? . 66502 O(18) O(19) 2.404(9) ? . . O(18) O(20) 2.428(8) ? . . O(18) O(21) 2.846(8) ? . . O(18) C(25) 2.58(1) ? . . O(18) C(30) 3.04(1) ? . . O(19) O(20) 2.44(1) ? . . O(19) C(17) 3.60(1) ? . 65501 O(19) C(25) 2.60(1) ? . . O(19) C(26) 2.95(1) ? . . O(20) O(22) 2.663(9) ? . . O(20) C(22) 3.59(1) ? . . O(20) C(24) 3.47(1) ? . . O(20) C(25) 2.58(1) ? . . O(20) C(26) 3.52(1) ? . . O(20) C(30) 3.24(1) ? . . O(21) S(5) 3.555(7) ? . 66502 O(21) O(1) 3.240(8) ? . 65501 O(21) O(2) 2.678(9) ? . 65501 O(21) O(9) 2.890(9) ? . 66502 O(21) O(10) 3.379(8) ? . 66502 O(21) C(12) 3.46(1) ? . 66502 O(22) O(23) 2.753(9) ? . . O(23) O(27) 2.756(9) ? . 66502 O(24) O(3) 3.263(9) ? . 66502 O(24) O(5) 2.584(9) ? . 66502 O(24) C(38) 3.52(1) ? . . O(25) O(3) 2.58(1) ? . 56401 O(25) C(7) 3.36(1) ? . 56401 O(25) C(8) 3.12(1) ? . 56502 O(26) O(27) 2.73(1) ? . 56502 O(27) O(4) 2.615(7) ? . 66502 O(27) O(5) 3.495(9) ? . 66502 O(27) O(17) 3.253(9) ? . 66502 O(27) O(23) 2.756(9) ? . 66502 O(27) O(26) 2.73(1) ? . 56502 C(1) C(3) 2.32(1) ? . . C(1) C(4) 2.33(1) ? . . C(1) C(7) 2.61(2) ? . . C(1) C(10) 2.60(1) ? . . C(2) S(2) 3.381(7) ? . . C(2) C(4) 2.34(1) ? . . C(2) C(5) 2.33(1) ? . . C(2) C(6) 2.59(1) ? . . C(2) C(8) 2.65(1) ? . . C(3) C(5) 2.33(1) ? . . C(3) C(7) 2.62(1) ? . . C(3) C(9) 2.59(1) ? . . C(4) C(2) 2.34(1) ? . . C(4) C(8) 2.58(2) ? . . C(4) C(10) 2.64(2) ? . . C(5) C(2) 2.33(1) ? . . C(5) C(6) 2.60(1) ? . . C(5) C(9) 2.62(1) ? . . C(6) C(2) 2.59(1) ? . . C(6) C(7) 3.20(2) ? . . C(6) C(10) 3.15(1) ? . . C(7) C(8) 3.22(1) ? . . C(8) O(10) 3.54(1) ? . 56502 C(8) O(25) 3.12(1) ? . 56502 C(8) C(2) 2.65(1) ? . . C(8) C(9) 3.13(2) ? . . C(9) C(10) 3.24(2) ? . . C(11) C(7) 3.47(1) ? . 56401 C(11) C(13) 2.40(1) ? . . C(11) C(14) 2.79(1) ? . . C(11) C(15) 2.39(2) ? . . C(12) O(21) 3.46(1) ? . 66502 C(12) C(14) 2.42(2) ? . . C(12) C(15) 2.77(2) ? . . C(12) C(16) 2.42(1) ? . . C(13) C(15) 2.38(1) ? . . C(13) C(16) 2.77(1) ? . . C(13) C(17) 2.52(2) ? . . C(13) C(36) 3.49(1) ? . . C(14) C(16) 2.42(1) ? . . C(14) C(36) 3.37(1) ? . . C(14) C(37) 3.36(1) ? . . C(15) C(6) 3.40(1) ? . 56401 C(15) C(17) 2.52(1) ? . . C(15) C(35) 3.38(1) ? . . C(15) C(36) 3.43(1) ? . . C(16) C(35) 3.48(1) ? . . C(16) C(38) 3.41(1) ? . . C(17) O(19) 3.60(1) ? . 45501 C(17) C(32) 3.56(1) ? . . C(17) C(37) 3.49(1) ? . . C(18) C(20) 2.41(1) ? . . C(18) C(21) 2.80(1) ? . . C(18) C(22) 2.40(1) ? . . C(19) C(21) 2.43(1) ? . . C(19) C(22) 2.76(1) ? . . C(19) C(23) 2.41(1) ? . . C(20) C(22) 2.41(1) ? . . C(20) C(23) 2.79(1) ? . . C(20) C(24) 2.53(1) ? . . C(21) C(23) 2.42(1) ? . . C(22) C(24) 2.53(1) ? . . C(25) C(27) 2.39(1) ? . . C(25) C(28) 2.80(1) ? . . C(25) C(29) 2.39(2) ? . . C(26) C(28) 2.43(2) ? . . C(26) C(29) 2.77(2) ? . . C(26) C(30) 2.42(1) ? . . C(27) C(29) 2.37(1) ? . . C(27) C(30) 2.75(1) ? . . C(27) C(31) 2.51(2) ? . . C(28) C(30) 2.42(1) ? . . C(29) C(31) 2.51(1) ? . . C(31) O(2) 3.58(1) ? . 66502 C(31) O(5) 3.60(2) ? . 66502 C(32) C(34) 2.41(1) ? . . C(32) C(35) 2.81(1) ? . . C(32) C(36) 2.41(2) ? . . C(32) C(38) 3.59(1) ? . 66502 C(33) C(35) 2.44(2) ? . . C(33) C(36) 2.77(2) ? . . C(33) C(37) 2.41(2) ? . . C(34) C(36) 2.38(2) ? . . C(34) C(37) 2.77(1) ? . . C(34) C(38) 2.49(2) ? . . C(35) C(35) 3.52(1) ? . 66502 C(35) C(37) 2.43(1) ? . . C(36) C(38) 2.52(1) ? . . C(38) O(17) 3.47(1) ? . 66502 C(38) C(32) 3.59(1) ? . 66502 Rh(1) H(3) 3.3615 ? . . Rh(1) H(6) 3.3042 ? . . Rh(1) H(9) 3.3486 ? . . Rh(1) H(12) 3.3400 ? . . Rh(1) H(15) 3.2803 ? . . S(2) H(4) 3.5734 ? . . S(2) H(6) 3.4795 ? . . S(2) H(9) 2.7013 ? . . S(2) H(35) 3.4455 ? . 66502 S(2) H(36) 3.4501 ? . 66502 S(3) H(1) 3.4980 ? . . S(3) H(3) 2.6763 ? . . S(4) H(10) 3.3228 ? . . S(4) H(12) 2.8926 ? . . S(4) H(15) 3.1083 ? . . S(5) H(5) 3.1816 ? . 56401 S(5) H(16) 2.8430 ? . . S(5) H(19) 2.8527 ? . . S(5) H(41) 3.4674 ? . . S(6) H(11) 3.2031 ? . 66401 S(6) H(19) 3.4809 ? . . S(6) H(23) 2.8082 ? . . S(6) H(26) 2.8566 ? . . S(7) H(21) 3.5617 ? . . S(7) H(37) 2.8195 ? . . S(7) H(40) 2.8418 ? . . S(8) H(22) 3.5516 ? . 65501 S(8) H(25) 3.5144 ? . . S(8) H(30) 2.8706 ? . . S(8) H(33) 2.8459 ? . . O(1) H(7) 3.5626 ? . . O(1) H(9) 3.5496 ? . . O(1) H(12) 3.1060 ? . . O(2) H(35) 2.6792 ? . 66502 O(3) H(6) 2.6173 ? . . O(5) H(34) 3.0985 ? . 66502 O(5) H(35) 3.2353 ? . 66502 O(6) H(13) 3.3530 ? . . O(6) H(15) 2.6507 ? . . O(9) H(16) 3.2291 ? . . O(9) H(41) 3.2600 ? . . O(9) H(42) 3.2503 ? . . O(10) H(4) 3.0741 ? . 56401 O(10) H(5) 2.9356 ? . 56401 O(10) H(7) 3.2655 ? . 56502 O(10) H(9) 2.9380 ? . 56502 O(10) H(16) 2.7898 ? . . O(10) H(36) 3.5153 ? . 45501 O(11) H(5) 3.4351 ? . 56401 O(11) H(6) 3.4074 ? . 56401 O(11) H(19) 2.5399 ? . . O(11) H(41) 3.4532 ? . . O(12) H(11) 2.6971 ? . 66401 O(12) H(12) 3.5088 ? . 66401 O(12) H(23) 2.8886 ? . . O(13) H(1) 3.0095 ? . 56401 O(13) H(6) 2.9469 ? . 56401 O(13) H(19) 2.6503 ? . . O(13) H(23) 3.0463 ? . . O(14) H(7) 3.1481 ? . 66401 O(14) H(8) 3.3931 ? . 66401 O(14) H(11) 3.0553 ? . 66401 O(14) H(26) 2.4969 ? . . O(14) H(34) 3.2621 ? . . O(15) H(21) 3.4343 ? . . O(15) H(28) 3.1374 ? . . O(15) H(29) 3.5288 ? . . O(15) H(37) 2.6888 ? . . O(16) H(21) 3.5236 ? . . O(16) H(22) 3.0176 ? . . O(16) H(40) 2.5877 ? . . O(17) H(37) 3.3435 ? . . O(17) H(40) 3.4954 ? . . O(17) H(42) 3.0307 ? . 66502 O(17) H(43) 3.0987 ? . 66502 O(18) H(22) 3.0787 ? . 65501 O(18) H(33) 2.7725 ? . . O(19) H(20) 2.9430 ? . 65501 O(19) H(22) 3.3719 ? . 65501 O(19) H(30) 2.5920 ? . . O(20) H(25) 2.7787 ? . . O(20) H(27) 3.3058 ? . . O(20) H(28) 2.8913 ? . . O(20) H(33) 3.1820 ? . . O(20) H(37) 3.3704 ? . . O(21) H(16) 2.7092 ? . 66502 O(22) H(28) 3.5838 ? . . O(24) H(19) 2.8706 ? . . O(24) H(34) 2.8631 ? . . O(24) H(41) 2.7765 ? . . O(24) H(43) 3.4630 ? . . O(25) H(4) 3.1788 ? . 56401 O(25) H(6) 2.7110 ? . 56401 O(25) H(7) 2.7787 ? . 56502 O(25) H(8) 2.7577 ? . 56502 O(25) H(9) 3.3484 ? . 56502 O(26) H(12) 3.2915 ? . . C(1) H(1) 2.0232 ? . . C(1) H(2) 2.0231 ? . . C(1) H(3) 2.0215 ? . . C(1) H(4) 3.3438 ? . . C(1) H(5) 2.8369 ? . . C(1) H(6) 2.8856 ? . . C(1) H(13) 2.6549 ? . . C(1) H(14) 3.1872 ? . . C(1) H(15) 3.2010 ? . . C(2) H(1) 2.6511 ? . . C(2) H(2) 3.1576 ? . . C(2) H(3) 3.1976 ? . . C(2) H(4) 2.0157 ? . . C(2) H(5) 2.0148 ? . . C(2) H(6) 2.0146 ? . . C(2) H(7) 3.3987 ? . . C(2) H(8) 2.8807 ? . . C(2) H(9) 2.9227 ? . . C(3) H(4) 2.6613 ? . . C(3) H(5) 3.2043 ? . . C(3) H(6) 3.2200 ? . . C(3) H(7) 2.0199 ? . . C(3) H(8) 2.0192 ? . . C(3) H(9) 2.0207 ? . . C(3) H(10) 3.3390 ? . . C(3) H(11) 2.8247 ? . . C(3) H(12) 2.8508 ? . . C(4) H(7) 2.6273 ? . . C(4) H(8) 3.1522 ? . . C(4) H(9) 3.1893 ? . . C(4) H(10) 2.0158 ? . . C(4) H(11) 2.0157 ? . . C(4) H(12) 2.0170 ? . . C(4) H(13) 3.3862 ? . . C(4) H(14) 2.8713 ? . . C(4) H(15) 2.9160 ? . . C(5) H(1) 3.3531 ? . . C(5) H(2) 2.8267 ? . . C(5) H(3) 2.8526 ? . . C(5) H(10) 2.6755 ? . . C(5) H(11) 3.2047 ? . . C(5) H(12) 3.2179 ? . . C(5) H(13) 2.0235 ? . . C(5) H(14) 2.0214 ? . . C(5) H(15) 2.0224 ? . . C(6) H(5) 3.1136 ? . . C(6) H(6) 3.2377 ? . . C(6) H(13) 2.7114 ? . . C(7) H(1) 2.7821 ? . . C(7) H(8) 3.1599 ? . . C(7) H(9) 3.2274 ? . . C(8) H(4) 2.7884 ? . . C(8) H(11) 3.0597 ? . . C(8) H(12) 3.1300 ? . . C(9) H(7) 2.6923 ? . . C(9) H(14) 3.1676 ? . . C(9) H(15) 3.2641 ? . . C(10) H(2) 3.0979 ? . . C(10) H(3) 3.1100 ? . . C(10) H(10) 2.8205 ? . . C(11) H(5) 2.6137 ? . 56401 C(11) H(6) 3.5965 ? . 56401 C(11) H(16) 2.0573 ? . . C(11) H(17) 3.2548 ? . . C(11) H(18) 3.2484 ? . . C(11) H(19) 2.0363 ? . . C(11) H(39) 3.4788 ? . . C(11) H(41) 3.0841 ? . . C(12) H(5) 2.9875 ? . 56401 C(12) H(17) 2.0187 ? . . C(12) H(19) 3.2781 ? . . C(12) H(39) 3.2798 ? . . C(13) H(5) 3.5785 ? . 56401 C(13) H(16) 2.0330 ? . . C(13) H(18) 3.2351 ? . . C(13) H(20) 2.9389 ? . . C(13) H(21) 3.2429 ? . . C(13) H(22) 2.6076 ? . . C(13) H(39) 3.2997 ? . . C(13) H(40) 3.5366 ? . . C(14) H(1) 3.1888 ? . 56401 C(14) H(2) 3.2034 ? . 56401 C(14) H(16) 3.2778 ? . . C(14) H(17) 2.0317 ? . . C(14) H(18) 2.0197 ? . . C(14) H(19) 3.2768 ? . . C(14) H(20) 2.0299 ? . . C(14) H(21) 2.0324 ? . . C(14) H(22) 2.0331 ? . . C(14) H(39) 3.5570 ? . . C(14) H(40) 3.5334 ? . . C(15) H(1) 2.6823 ? . 56401 C(15) H(2) 3.2794 ? . 56401 C(15) H(5) 3.5517 ? . 56401 C(15) H(17) 3.2330 ? . . C(15) H(19) 2.0475 ? . . C(15) H(20) 2.9452 ? . . C(15) H(21) 2.6099 ? . . C(15) H(22) 3.2355 ? . . C(15) H(41) 3.3479 ? . . C(16) H(1) 2.9605 ? . 56401 C(16) H(5) 2.9357 ? . 56401 C(16) H(6) 3.5309 ? . 56401 C(16) H(16) 3.2755 ? . . C(16) H(18) 2.0343 ? . . C(16) H(41) 2.6531 ? . . C(17) H(2) 3.2723 ? . 56401 C(17) H(17) 2.6627 ? . . C(17) H(18) 2.6667 ? . . C(17) H(40) 3.5509 ? . . C(18) H(11) 3.5029 ? . 66401 C(18) H(18) 3.1566 ? . . C(18) H(19) 3.5820 ? . . C(18) H(23) 2.0274 ? . . C(18) H(24) 3.2613 ? . . C(18) H(25) 3.2564 ? . . C(18) H(26) 2.0486 ? . . C(19) H(1) 3.3620 ? . 56401 C(19) H(3) 3.0504 ? . 56401 C(19) H(18) 3.1397 ? . . C(19) H(24) 2.0348 ? . . C(19) H(26) 3.2652 ? . . C(20) H(3) 3.5797 ? . 56401 C(20) H(18) 3.1880 ? . . C(20) H(23) 2.0302 ? . . C(20) H(25) 3.2665 ? . . C(20) H(27) 2.9500 ? . . C(20) H(28) 3.2576 ? . . C(20) H(29) 2.6091 ? . . C(21) H(18) 3.2789 ? . . C(21) H(23) 3.2862 ? . . C(21) H(24) 2.0678 ? . . C(21) H(25) 2.0222 ? . . C(21) H(26) 3.2736 ? . . C(21) H(27) 2.0303 ? . . C(21) H(28) 2.0293 ? . . C(21) H(29) 2.0329 ? . . C(22) H(18) 3.2953 ? . . C(22) H(24) 3.2669 ? . . C(22) H(26) 2.0385 ? . . C(22) H(27) 2.9600 ? . . C(22) H(28) 2.6199 ? . . C(22) H(29) 3.2418 ? . . C(22) H(37) 3.5502 ? . . C(22) H(38) 3.1693 ? . . C(23) H(18) 3.2438 ? . . C(23) H(23) 3.2626 ? . . C(23) H(25) 2.0255 ? . . C(23) H(38) 3.5060 ? . . C(24) H(24) 2.6851 ? . . C(24) H(25) 2.6805 ? . . C(24) H(37) 3.4079 ? . . C(25) H(17) 2.9692 ? . 65501 C(25) H(25) 3.0010 ? . . C(25) H(30) 2.0576 ? . . C(25) H(31) 3.2417 ? . . C(25) H(32) 3.2414 ? . . C(25) H(33) 2.0391 ? . . C(26) H(2) 3.5893 ? . 66401 C(26) H(17) 3.2347 ? . 65501 C(26) H(20) 3.4788 ? . 65501 C(26) H(25) 3.2179 ? . . C(26) H(26) 3.4293 ? . . C(26) H(31) 2.0119 ? . . C(26) H(33) 3.2773 ? . . C(27) H(17) 3.4089 ? . 65501 C(27) H(26) 2.9856 ? . . C(27) H(30) 2.0338 ? . . C(27) H(32) 3.2285 ? . . C(27) H(34) 2.9349 ? . . C(27) H(35) 3.2351 ? . . C(27) H(36) 2.6009 ? . . C(28) H(16) 3.3589 ? . 65501 C(28) H(17) 3.3957 ? . 65501 C(28) H(26) 3.0922 ? . . C(28) H(30) 3.2834 ? . . C(28) H(31) 2.0245 ? . . C(28) H(32) 2.0234 ? . . C(28) H(33) 3.2696 ? . . C(28) H(34) 2.0156 ? . . C(28) H(35) 2.0184 ? . . C(28) H(36) 2.0162 ? . . C(29) H(16) 3.5559 ? . 65501 C(29) H(17) 3.1520 ? . 65501 C(29) H(26) 3.5885 ? . . C(29) H(31) 3.2257 ? . . C(29) H(33) 2.0288 ? . . C(29) H(34) 2.9329 ? . . C(29) H(35) 2.6007 ? . . C(29) H(36) 3.2287 ? . . C(29) H(38) 3.0702 ? . . C(29) H(40) 3.4347 ? . 66502 C(29) H(43) 3.5348 ? . . C(30) H(17) 2.9424 ? . 65501 C(30) H(25) 3.2882 ? . . C(30) H(30) 3.2787 ? . . C(30) H(32) 2.0159 ? . . C(30) H(38) 3.0644 ? . . C(31) H(8) 3.2379 ? . 66401 C(31) H(16) 3.4923 ? . 65501 C(31) H(31) 2.6590 ? . . C(31) H(32) 2.6599 ? . . C(32) H(21) 3.0691 ? . . C(32) H(22) 3.3988 ? . . C(32) H(37) 2.0316 ? . . C(32) H(38) 3.2571 ? . . C(32) H(39) 3.2631 ? . . C(32) H(40) 2.0550 ? . . C(32) H(42) 3.1657 ? . 66502 C(32) H(43) 3.1892 ? . 66502 C(33) H(21) 3.4511 ? . . C(33) H(25) 3.4254 ? . . C(33) H(28) 3.2320 ? . . C(33) H(38) 2.0478 ? . . C(33) H(40) 3.2660 ? . . C(33) H(42) 3.0628 ? . 66502 C(34) H(18) 3.4488 ? . . C(34) H(25) 3.2660 ? . . C(34) H(37) 2.0612 ? . . C(34) H(39) 3.2351 ? . . C(34) H(41) 2.9187 ? . . C(34) H(42) 3.2136 ? . . C(34) H(42) 3.4311 ? . 66502 C(34) H(43) 2.5853 ? . . C(35) H(18) 3.5039 ? . . C(35) H(37) 3.2869 ? . . C(35) H(38) 2.0157 ? . . C(35) H(39) 2.0413 ? . . C(35) H(40) 3.2816 ? . . C(35) H(41) 2.0161 ? . . C(35) H(42) 2.0132 ? . . C(35) H(43) 2.0147 ? . . C(36) H(32) 3.4692 ? . 66502 C(36) H(38) 3.2382 ? . . C(36) H(40) 2.0283 ? . . C(36) H(41) 2.9391 ? . . C(36) H(42) 2.6066 ? . . C(36) H(43) 3.2428 ? . . C(36) H(43) 3.4245 ? . 66502 C(37) H(21) 3.3582 ? . . C(37) H(22) 3.2118 ? . . C(37) H(32) 3.0863 ? . 66502 C(37) H(37) 3.2716 ? . . C(37) H(39) 2.0190 ? . . C(37) H(43) 3.0800 ? . 66502 C(38) H(19) 3.3465 ? . . C(38) H(38) 2.6399 ? . . C(38) H(39) 2.6733 ? . . H(1) S(3) 3.4980 ? . . H(1) C(1) 2.0232 ? . . H(1) C(2) 2.6511 ? . . H(1) C(5) 3.3531 ? . . H(1) C(7) 2.7821 ? . . H(2) C(2) 3.1576 ? . . H(3) Rh(1) 3.3615 ? . . H(3) S(3) 2.6763 ? . . H(3) C(1) 2.0215 ? . . H(3) C(2) 3.1976 ? . . H(3) C(5) 2.8526 ? . . H(3) C(10) 3.1100 ? . . H(4) C(2) 2.0157 ? . . H(5) C(2) 2.0148 ? . . H(6) C(2) 2.0146 ? . . H(7) O(10) 3.2655 ? . 56502 H(7) O(25) 2.7787 ? . 56502 H(7) C(2) 3.3987 ? . . H(8) O(25) 2.7577 ? . 56502 H(8) C(2) 2.8807 ? . . H(9) O(10) 2.9380 ? . 56502 H(9) O(25) 3.3484 ? . 56502 H(9) C(2) 2.9227 ? . . H(16) O(21) 2.7092 ? . 66502 H(16) C(28) 3.3589 ? . 45501 H(16) C(29) 3.5559 ? . 45501 H(16) C(31) 3.4923 ? . 45501 H(17) C(25) 2.9692 ? . 45501 H(17) C(26) 3.2347 ? . 45501 H(17) C(27) 3.4089 ? . 45501 H(17) C(28) 3.3957 ? . 45501 H(17) C(29) 3.1520 ? . 45501 H(17) C(30) 2.9424 ? . 45501 H(18) C(6) 3.4066 ? . 56401 H(20) O(19) 2.9430 ? . 45501 H(20) C(6) 3.4540 ? . 56401 H(20) C(26) 3.4788 ? . 45501 H(22) S(8) 3.5516 ? . 45501 H(22) O(18) 3.0787 ? . 45501 H(22) O(19) 3.3719 ? . 45501 H(23) S(3) 3.3068 ? . 56401 H(23) C(6) 3.1394 ? . 56401 H(30) C(1) 3.5485 ? . 66401 H(30) C(5) 3.4939 ? . 66401 H(31) C(1) 3.0424 ? . 66401 H(31) C(2) 2.7739 ? . 66401 H(31) C(3) 2.7877 ? . 66401 H(31) C(4) 3.0764 ? . 66401 H(31) C(5) 3.2573 ? . 66401 H(31) C(7) 3.3849 ? . 66401 H(31) C(8) 3.3994 ? . 66401 H(32) C(36) 3.4692 ? . 66502 H(32) C(37) 3.0863 ? . 66502 H(34) O(5) 3.0985 ? . 66502 H(35) S(2) 3.4455 ? . 66502 H(35) O(2) 2.6792 ? . 66502 H(35) O(5) 3.2353 ? . 66502 H(36) S(2) 3.4501 ? . 66502 H(36) O(10) 3.5153 ? . 65501 H(36) C(7) 3.4344 ? . 66401 H(36) C(8) 3.4045 ? . 66401 H(40) C(29) 3.4347 ? . 66502 H(42) O(17) 3.0307 ? . 66502 H(42) C(32) 3.1657 ? . 66502 H(42) C(33) 3.0628 ? . 66502 H(42) C(34) 3.4311 ? . 66502 H(43) O(17) 3.0987 ? . 66502 H(43) C(32) 3.1892 ? . 66502 H(43) C(36) 3.4245 ? . 66502 H(43) C(37) 3.0800 ? . 66502 Rh(1) Mo(1) 3.1125(7) ? . . Rh(1) Mo(3) 3.080(1) ? . . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 S(2) Rh(1) Mo(2) Mo(1) 63.08(3) ? . . . . S(2) Rh(1) Mo(2) Mo(3) 128.54(3) ? . . . . S(2) Rh(1) Mo(2) S(1) 96.73(7) ? . . . . S(2) Rh(1) Mo(2) S(3) -168.15(7) ? . . . . S(2) Rh(1) Mo(2) O(3) -83.8(2) ? . . . . S(2) Rh(1) Mo(2) O(4) -161.8(2) ? . . . . S(2) Rh(1) Mo(2) O(5) -5.4(2) ? . . . . S(3) Rh(1) Mo(2) Mo(1) -128.77(4) ? . . . . S(3) Rh(1) Mo(2) Mo(3) -63.31(3) ? . . . . S(3) Rh(1) Mo(2) S(1) -95.12(7) ? . . . . S(3) Rh(1) Mo(2) S(2) 168.15(7) ? . . . . S(3) Rh(1) Mo(2) O(3) 84.3(2) ? . . . . S(3) Rh(1) Mo(2) O(4) 6.4(2) ? . . . . S(3) Rh(1) Mo(2) O(5) 162.8(2) ? . . . . S(4) Rh(1) Mo(2) Mo(1) -32.24(3) ? . . . . S(4) Rh(1) Mo(2) Mo(3) 33.22(3) ? . . . . S(4) Rh(1) Mo(2) S(1) 1.42(7) ? . . . . S(4) Rh(1) Mo(2) S(2) -95.32(6) ? . . . . S(4) Rh(1) Mo(2) S(3) 96.53(7) ? . . . . S(4) Rh(1) Mo(2) O(3) -179.2(2) ? . . . . S(4) Rh(1) Mo(2) O(4) 102.9(2) ? . . . . S(4) Rh(1) Mo(2) O(5) -100.7(2) ? . . . . C(1) Rh(1) Mo(2) Mo(1) -179.18(5) ? . . . . C(1) Rh(1) Mo(2) Mo(3) -113.72(5) ? . . . . C(1) Rh(1) Mo(2) S(1) -145.52(7) ? . . . . C(1) Rh(1) Mo(2) S(2) 117.75(8) ? . . . . C(1) Rh(1) Mo(2) S(3) -50.40(8) ? . . . . C(1) Rh(1) Mo(2) O(3) 33.9(2) ? . . . . C(1) Rh(1) Mo(2) O(4) -44.0(2) ? . . . . C(1) Rh(1) Mo(2) O(5) 112.3(2) ? . . . . C(2) Rh(1) Mo(2) Mo(1) 138.49(5) ? . . . . C(2) Rh(1) Mo(2) Mo(3) -156.05(4) ? . . . . C(2) Rh(1) Mo(2) S(1) 172.15(7) ? . . . . C(2) Rh(1) Mo(2) S(2) 75.42(7) ? . . . . C(2) Rh(1) Mo(2) S(3) -92.73(7) ? . . . . C(2) Rh(1) Mo(2) O(3) -8.4(2) ? . . . . C(2) Rh(1) Mo(2) O(4) -86.3(2) ? . . . . C(2) Rh(1) Mo(2) O(5) 70.0(2) ? . . . . C(3) Rh(1) Mo(2) Mo(1) 96.36(4) ? . . . . C(3) Rh(1) Mo(2) Mo(3) 161.82(4) ? . . . . C(3) Rh(1) Mo(2) S(1) 130.01(7) ? . . . . C(3) Rh(1) Mo(2) S(2) 33.28(7) ? . . . . C(3) Rh(1) Mo(2) S(3) -134.87(8) ? . . . . C(3) Rh(1) Mo(2) O(3) -50.6(2) ? . . . . C(3) Rh(1) Mo(2) O(4) -128.5(2) ? . . . . C(3) Rh(1) Mo(2) O(5) 27.9(2) ? . . . . C(4) Rh(1) Mo(2) Mo(1) 56.6(2) ? . . . . C(4) Rh(1) Mo(2) Mo(3) 122.1(2) ? . . . . C(4) Rh(1) Mo(2) S(1) 90.3(2) ? . . . . C(4) Rh(1) Mo(2) S(2) -6.5(2) ? . . . . C(4) Rh(1) Mo(2) S(3) -174.6(2) ? . . . . C(4) Rh(1) Mo(2) O(3) -90.3(2) ? . . . . C(4) Rh(1) Mo(2) O(4) -168.2(3) ? . . . . C(4) Rh(1) Mo(2) O(5) -11.9(3) ? . . . . C(5) Rh(1) Mo(2) Mo(1) -139.66(9) ? . . . . C(5) Rh(1) Mo(2) Mo(3) -74.20(9) ? . . . . C(5) Rh(1) Mo(2) S(1) -106.0(1) ? . . . . C(5) Rh(1) Mo(2) S(2) 157.3(1) ? . . . . C(5) Rh(1) Mo(2) S(3) -10.9(1) ? . . . . C(5) Rh(1) Mo(2) O(3) 73.4(2) ? . . . . C(5) Rh(1) Mo(2) O(4) -4.5(3) ? . . . . C(5) Rh(1) Mo(2) O(5) 151.9(2) ? . . . . Mo(2) Rh(1) S(2) Mo(1) -75.13(6) ? . . . . S(3) Rh(1) S(2) Mo(1) -84.42(5) ? . . . . S(3) Rh(1) S(2) Mo(2) -9.29(5) ? . . . . S(4) Rh(1) S(2) Mo(1) 13.30(5) ? . . . . S(4) Rh(1) S(2) Mo(2) 88.42(5) ? . . . . C(1) Rh(1) S(2) Mo(1) -179.09(5) ? . . . . C(1) Rh(1) S(2) Mo(2) -103.96(7) ? . . . . C(2) Rh(1) S(2) Mo(1) 166.94(5) ? . . . . C(2) Rh(1) S(2) Mo(2) -117.93(5) ? . . . . C(3) Rh(1) S(2) Mo(1) 128.59(5) ? . . . . C(3) Rh(1) S(2) Mo(2) -156.28(5) ? . . . . C(4) Rh(1) S(2) Mo(1) 103.24(6) ? . . . . C(4) Rh(1) S(2) Mo(2) 178.37(4) ? . . . . C(5) Rh(1) S(2) Mo(1) 126.3(1) ? . . . . C(5) Rh(1) S(2) Mo(2) -158.53(8) ? . . . . Mo(2) Rh(1) S(3) Mo(3) 74.94(5) ? . . . . S(2) Rh(1) S(3) Mo(2) 9.20(6) ? . . . . S(2) Rh(1) S(3) Mo(3) 84.14(5) ? . . . . S(4) Rh(1) S(3) Mo(2) -87.72(5) ? . . . . S(4) Rh(1) S(3) Mo(3) -12.78(5) ? . . . . C(1) Rh(1) S(3) Mo(2) 140.28(5) ? . . . . C(1) Rh(1) S(3) Mo(3) -144.79(5) ? . . . . C(2) Rh(1) S(3) Mo(2) 108.01(5) ? . . . . C(2) Rh(1) S(3) Mo(3) -177.05(4) ? . . . . C(3) Rh(1) S(3) Mo(2) 111.06(9) ? . . . . C(3) Rh(1) S(3) Mo(3) -174.00(8) ? . . . . C(4) Rh(1) S(3) Mo(2) 178.03(7) ? . . . . C(4) Rh(1) S(3) Mo(3) -107.04(8) ? . . . . C(5) Rh(1) S(3) Mo(2) 175.12(5) ? . . . . C(5) Rh(1) S(3) Mo(3) -109.94(5) ? . . . . Mo(2) Rh(1) S(4) Mo(1) 36.43(6) ? . . . . Mo(2) Rh(1) S(4) Mo(3) -37.58(5) ? . . . . S(2) Rh(1) S(4) Mo(1) -13.66(6) ? . . . . S(2) Rh(1) S(4) Mo(3) -87.67(5) ? . . . . S(3) Rh(1) S(4) Mo(1) 87.18(6) ? . . . . S(3) Rh(1) S(4) Mo(3) 13.17(6) ? . . . . C(1) Rh(1) S(4) Mo(1) 178.94(5) ? . . . . C(1) Rh(1) S(4) Mo(3) 104.93(7) ? . . . . C(2) Rh(1) S(4) Mo(1) -125.7(1) ? . . . . C(2) Rh(1) S(4) Mo(3) 160.3(1) ? . . . . C(3) Rh(1) S(4) Mo(1) -104.25(6) ? . . . . C(3) Rh(1) S(4) Mo(3) -178.26(4) ? . . . . C(4) Rh(1) S(4) Mo(1) -130.55(6) ? . . . . C(4) Rh(1) S(4) Mo(3) 155.44(6) ? . . . . C(5) Rh(1) S(4) Mo(1) -168.37(6) ? . . . . C(5) Rh(1) S(4) Mo(3) 117.62(5) ? . . . . Mo(2) Rh(1) C(1) C(2) -87.1(5) ? . . . . Mo(2) Rh(1) C(1) C(5) 153.4(5) ? . . . . Mo(2) Rh(1) C(1) C(6) 33(1) ? . . . . S(2) Rh(1) C(1) C(2) -23.1(6) ? . . . . S(2) Rh(1) C(1) C(5) -142.7(5) ? . . . . S(2) Rh(1) C(1) C(6) 97.9(9) ? . . . . S(3) Rh(1) C(1) C(2) -123.7(4) ? . . . . S(3) Rh(1) C(1) C(5) 116.7(6) ? . . . . S(3) Rh(1) C(1) C(6) -2.7(9) ? . . . . S(4) Rh(1) C(1) C(2) 140.2(4) ? . . . . S(4) Rh(1) C(1) C(5) 20.6(7) ? . . . . S(4) Rh(1) C(1) C(6) -98.8(8) ? . . . . C(2) Rh(1) C(1) C(5) -119.6(7) ? . . . . C(2) Rh(1) C(1) C(6) 121(1) ? . . . . C(3) Rh(1) C(1) C(2) 38.7(4) ? . . . . C(3) Rh(1) C(1) C(5) -80.9(5) ? . . . . C(3) Rh(1) C(1) C(6) 159.7(9) ? . . . . C(4) Rh(1) C(1) C(2) 81.0(4) ? . . . . C(4) Rh(1) C(1) C(5) -38.6(5) ? . . . . C(4) Rh(1) C(1) C(6) -157(1) ? . . . . C(5) Rh(1) C(1) C(2) 119.6(6) ? . . . . C(5) Rh(1) C(1) C(6) -119(1) ? . . . . Mo(2) Rh(1) C(2) C(1) 114.5(4) ? . . . . Mo(2) Rh(1) C(2) C(3) -128.6(4) ? . . . . Mo(2) Rh(1) C(2) C(7) -9.3(9) ? . . . . S(2) Rh(1) C(2) C(1) 162.7(4) ? . . . . S(2) Rh(1) C(2) C(3) -80.4(5) ? . . . . S(2) Rh(1) C(2) C(7) 38.9(8) ? . . . . S(3) Rh(1) C(2) C(1) 60.4(4) ? . . . . S(3) Rh(1) C(2) C(3) 177.3(4) ? . . . . S(3) Rh(1) C(2) C(7) -63.4(9) ? . . . . S(4) Rh(1) C(2) C(1) -85.2(7) ? . . . . S(4) Rh(1) C(2) C(3) 31.7(8) ? . . . . S(4) Rh(1) C(2) C(7) 151.0(6) ? . . . . C(1) Rh(1) C(2) C(3) 116.9(6) ? . . . . C(1) Rh(1) C(2) C(7) -123(1) ? . . . . C(3) Rh(1) C(2) C(1) -116.9(5) ? . . . . C(3) Rh(1) C(2) C(7) 119(1) ? . . . . C(4) Rh(1) C(2) C(1) -79.8(4) ? . . . . C(4) Rh(1) C(2) C(3) 37.1(4) ? . . . . C(4) Rh(1) C(2) C(7) 156.4(9) ? . . . . C(5) Rh(1) C(2) C(1) -36.8(4) ? . . . . C(5) Rh(1) C(2) C(3) 80.1(4) ? . . . . C(5) Rh(1) C(2) C(7) -160.6(9) ? . . . . Mo(2) Rh(1) C(3) C(2) 75.9(5) ? . . . . Mo(2) Rh(1) C(3) C(4) -166.4(3) ? . . . . Mo(2) Rh(1) C(3) C(8) -46.7(8) ? . . . . S(2) Rh(1) C(3) C(2) 100.8(5) ? . . . . S(2) Rh(1) C(3) C(4) -141.5(4) ? . . . . S(2) Rh(1) C(3) C(8) -21.8(7) ? . . . . S(3) Rh(1) C(3) C(2) -4.6(7) ? . . . . S(3) Rh(1) C(3) C(4) 113.1(5) ? . . . . S(3) Rh(1) C(3) C(8) -127.2(6) ? . . . . S(4) Rh(1) C(3) C(2) -163.9(4) ? . . . . S(4) Rh(1) C(3) C(4) -46.2(5) ? . . . . S(4) Rh(1) C(3) C(8) 73.5(7) ? . . . . C(1) Rh(1) C(3) C(2) -37.5(4) ? . . . . C(1) Rh(1) C(3) C(4) 80.2(4) ? . . . . C(1) Rh(1) C(3) C(8) -160.1(8) ? . . . . C(2) Rh(1) C(3) C(4) 117.7(6) ? . . . . C(2) Rh(1) C(3) C(8) -122.6(9) ? . . . . C(4) Rh(1) C(3) C(2) -117.7(6) ? . . . . C(4) Rh(1) C(3) C(8) 119.7(8) ? . . . . C(5) Rh(1) C(3) C(2) -80.4(5) ? . . . . C(5) Rh(1) C(3) C(4) 37.3(4) ? . . . . C(5) Rh(1) C(3) C(8) 157.0(7) ? . . . . Mo(2) Rh(1) C(4) C(3) 49(1) ? . . . . Mo(2) Rh(1) C(4) C(5) 168.7(8) ? . . . . Mo(2) Rh(1) C(4) C(9) -70(1) ? . . . . S(2) Rh(1) C(4) C(3) 44.3(4) ? . . . . S(2) Rh(1) C(4) C(5) 163.1(4) ? . . . . S(2) Rh(1) C(4) C(9) -76(1) ? . . . . S(3) Rh(1) C(4) C(3) -123.4(5) ? . . . . S(3) Rh(1) C(4) C(5) -4.5(7) ? . . . . S(3) Rh(1) C(4) C(9) 116.0(8) ? . . . . S(4) Rh(1) C(4) C(3) 139.2(4) ? . . . . S(4) Rh(1) C(4) C(5) -101.9(5) ? . . . . S(4) Rh(1) C(4) C(9) 18.7(9) ? . . . . C(1) Rh(1) C(4) C(3) -80.4(4) ? . . . . C(1) Rh(1) C(4) C(5) 38.4(4) ? . . . . C(1) Rh(1) C(4) C(9) 158(1) ? . . . . C(2) Rh(1) C(4) C(3) -38.2(4) ? . . . . C(2) Rh(1) C(4) C(5) 80.7(5) ? . . . . C(2) Rh(1) C(4) C(9) -158(1) ? . . . . C(3) Rh(1) C(4) C(5) 118.9(6) ? . . . . C(3) Rh(1) C(4) C(9) -120(1) ? . . . . C(5) Rh(1) C(4) C(3) -118.9(5) ? . . . . C(5) Rh(1) C(4) C(9) 120(1) ? . . . . Mo(2) Rh(1) C(5) C(1) -58.0(9) ? . . . . Mo(2) Rh(1) C(5) C(4) -174.2(4) ? . . . . Mo(2) Rh(1) C(5) C(10) 62.5(9) ? . . . . S(2) Rh(1) C(5) C(1) 82.1(7) ? . . . . S(2) Rh(1) C(5) C(4) -34.1(7) ? . . . . S(2) Rh(1) C(5) C(10) -157.4(5) ? . . . . S(3) Rh(1) C(5) C(1) -66.7(6) ? . . . . S(3) Rh(1) C(5) C(4) 177.1(5) ? . . . . S(3) Rh(1) C(5) C(10) 53.8(6) ? . . . . S(4) Rh(1) C(5) C(1) -164.8(6) ? . . . . S(4) Rh(1) C(5) C(4) 79.0(5) ? . . . . S(4) Rh(1) C(5) C(10) -44.3(6) ? . . . . C(1) Rh(1) C(5) C(4) -116.2(7) ? . . . . C(1) Rh(1) C(5) C(10) 120.5(8) ? . . . . C(2) Rh(1) C(5) C(1) 36.2(5) ? . . . . C(2) Rh(1) C(5) C(4) -80.0(5) ? . . . . C(2) Rh(1) C(5) C(10) 156.7(7) ? . . . . C(3) Rh(1) C(5) C(1) 79.6(6) ? . . . . C(3) Rh(1) C(5) C(4) -36.6(5) ? . . . . C(3) Rh(1) C(5) C(10) -159.9(7) ? . . . . C(4) Rh(1) C(5) C(1) 116.2(7) ? . . . . C(4) Rh(1) C(5) C(10) -123.3(7) ? . . . . Mo(3) Mo(1) Mo(2) Rh(1) 74.14(3) ? . . . . Mo(3) Mo(1) Mo(2) S(1) -64.43(7) ? . . . . Mo(3) Mo(1) Mo(2) S(2) 134.48(6) ? . . . . Mo(3) Mo(1) Mo(2) S(3) 35.59(6) ? . . . . Mo(3) Mo(1) Mo(2) O(3) 134.9(2) ? . . . . Mo(3) Mo(1) Mo(2) O(4) -56.5(2) ? . . . . Mo(3) Mo(1) Mo(2) O(5) -140.2(2) ? . . . . S(1) Mo(1) Mo(2) Rh(1) 138.57(4) ? . . . . S(1) Mo(1) Mo(2) Mo(3) 64.43(3) ? . . . . S(1) Mo(1) Mo(2) S(2) -161.09(7) ? . . . . S(1) Mo(1) Mo(2) S(3) 100.02(7) ? . . . . S(1) Mo(1) Mo(2) O(3) -160.7(2) ? . . . . S(1) Mo(1) Mo(2) O(4) 7.9(2) ? . . . . S(1) Mo(1) Mo(2) O(5) -75.8(2) ? . . . . S(2) Mo(1) Mo(2) Rh(1) -60.34(3) ? . . . . S(2) Mo(1) Mo(2) Mo(3) -134.48(3) ? . . . . S(2) Mo(1) Mo(2) S(1) 161.09(7) ? . . . . S(2) Mo(1) Mo(2) S(3) -98.89(7) ? . . . . S(2) Mo(1) Mo(2) O(3) 0.4(2) ? . . . . S(2) Mo(1) Mo(2) O(4) 169.0(2) ? . . . . S(2) Mo(1) Mo(2) O(5) 85.3(2) ? . . . . S(4) Mo(1) Mo(2) Rh(1) 33.84(3) ? . . . . S(4) Mo(1) Mo(2) Mo(3) -40.29(3) ? . . . . S(4) Mo(1) Mo(2) S(1) -104.72(8) ? . . . . S(4) Mo(1) Mo(2) S(2) 94.19(6) ? . . . . S(4) Mo(1) Mo(2) S(3) -4.70(7) ? . . . . S(4) Mo(1) Mo(2) O(3) 94.6(2) ? . . . . S(4) Mo(1) Mo(2) O(4) -96.8(2) ? . . . . S(4) Mo(1) Mo(2) O(5) 179.5(2) ? . . . . O(1) Mo(1) Mo(2) Rh(1) -54.60(5) ? . . . . O(1) Mo(1) Mo(2) Mo(3) -128.74(5) ? . . . . O(1) Mo(1) Mo(2) S(1) 166.83(8) ? . . . . O(1) Mo(1) Mo(2) S(2) 5.74(7) ? . . . . O(1) Mo(1) Mo(2) S(3) -93.15(8) ? . . . . O(1) Mo(1) Mo(2) O(3) 6.2(3) ? . . . . O(1) Mo(1) Mo(2) O(4) 174.7(2) ? . . . . O(1) Mo(1) Mo(2) O(5) 91.1(2) ? . . . . O(2) Mo(1) Mo(2) Rh(1) -135.95(4) ? . . . . O(2) Mo(1) Mo(2) Mo(3) 149.91(4) ? . . . . O(2) Mo(1) Mo(2) S(1) 85.48(7) ? . . . . O(2) Mo(1) Mo(2) S(2) -75.61(7) ? . . . . O(2) Mo(1) Mo(2) S(3) -174.50(7) ? . . . . O(2) Mo(1) Mo(2) O(3) -75.2(2) ? . . . . O(2) Mo(1) Mo(2) O(4) 93.4(2) ? . . . . O(2) Mo(1) Mo(2) O(5) 9.7(2) ? . . . . Mo(2) Mo(1) Mo(3) S(1) 64.11(6) ? . . . . Mo(2) Mo(1) Mo(3) S(3) -34.56(5) ? . . . . Mo(2) Mo(1) Mo(3) S(4) -126.89(7) ? . . . . Mo(2) Mo(1) Mo(3) O(6) -126.1(2) ? . . . . Mo(2) Mo(1) Mo(3) O(7) 143.8(1) ? . . . . Mo(2) Mo(1) Mo(3) O(8) 55.9(2) ? . . . . S(1) Mo(1) Mo(3) Mo(2) -64.11(3) ? . . . . S(1) Mo(1) Mo(3) S(3) -98.67(5) ? . . . . S(1) Mo(1) Mo(3) S(4) 169.00(7) ? . . . . S(1) Mo(1) Mo(3) O(6) 169.8(2) ? . . . . S(1) Mo(1) Mo(3) O(7) 79.7(1) ? . . . . S(1) Mo(1) Mo(3) O(8) -8.2(2) ? . . . . S(2) Mo(1) Mo(3) Mo(2) 34.71(2) ? . . . . S(2) Mo(1) Mo(3) S(1) 98.82(6) ? . . . . S(2) Mo(1) Mo(3) S(3) 0.15(5) ? . . . . S(2) Mo(1) Mo(3) S(4) -92.18(7) ? . . . . S(2) Mo(1) Mo(3) O(6) -91.4(2) ? . . . . S(2) Mo(1) Mo(3) O(7) 178.5(1) ? . . . . S(2) Mo(1) Mo(3) O(8) 90.6(2) ? . . . . S(4) Mo(1) Mo(3) Mo(2) 126.89(3) ? . . . . S(4) Mo(1) Mo(3) S(1) -169.00(7) ? . . . . S(4) Mo(1) Mo(3) S(3) 92.33(5) ? . . . . S(4) Mo(1) Mo(3) O(6) 0.8(2) ? . . . . S(4) Mo(1) Mo(3) O(7) -89.3(1) ? . . . . S(4) Mo(1) Mo(3) O(8) -177.2(2) ? . . . . O(1) Mo(1) Mo(3) Mo(2) 124.13(5) ? . . . . O(1) Mo(1) Mo(3) S(1) -171.76(8) ? . . . . O(1) Mo(1) Mo(3) S(3) 89.57(7) ? . . . . O(1) Mo(1) Mo(3) S(4) -2.76(8) ? . . . . O(1) Mo(1) Mo(3) O(6) -2.0(2) ? . . . . O(1) Mo(1) Mo(3) O(7) -92.1(2) ? . . . . O(1) Mo(1) Mo(3) O(8) 180.0(2) ? . . . . O(2) Mo(1) Mo(3) Mo(2) -56.10(6) ? . . . . O(2) Mo(1) Mo(3) S(1) 8.01(8) ? . . . . O(2) Mo(1) Mo(3) S(3) -90.66(7) ? . . . . O(2) Mo(1) Mo(3) S(4) 177.01(9) ? . . . . O(2) Mo(1) Mo(3) O(6) 177.8(2) ? . . . . O(2) Mo(1) Mo(3) O(7) 87.7(2) ? . . . . O(2) Mo(1) Mo(3) O(8) -0.2(2) ? . . . . Mo(2) Mo(1) S(1) Mo(3) -77.95(5) ? . . . . Mo(3) Mo(1) S(1) Mo(2) 77.95(5) ? . . . . S(2) Mo(1) S(1) Mo(2) -15.15(6) ? . . . . S(2) Mo(1) S(1) Mo(3) -93.10(5) ? . . . . S(4) Mo(1) S(1) Mo(2) 87.12(6) ? . . . . S(4) Mo(1) S(1) Mo(3) 9.17(6) ? . . . . O(1) Mo(1) S(1) Mo(2) -129.3(3) ? . . . . O(1) Mo(1) S(1) Mo(3) 152.7(3) ? . . . . O(2) Mo(1) S(1) Mo(2) -97.25(5) ? . . . . O(2) Mo(1) S(1) Mo(3) -175.20(5) ? . . . . Mo(2) Mo(1) S(2) Rh(1) 79.35(6) ? . . . . Mo(3) Mo(1) S(2) Rh(1) 40.13(5) ? . . . . Mo(3) Mo(1) S(2) Mo(2) -39.21(5) ? . . . . S(1) Mo(1) S(2) Rh(1) 94.83(5) ? . . . . S(1) Mo(1) S(2) Mo(2) 15.48(5) ? . . . . S(4) Mo(1) S(2) Rh(1) -13.85(6) ? . . . . S(4) Mo(1) S(2) Mo(2) -93.20(5) ? . . . . O(1) Mo(1) S(2) Rh(1) -96.47(5) ? . . . . O(1) Mo(1) S(2) Mo(2) -175.82(5) ? . . . . O(2) Mo(1) S(2) Rh(1) -177.19(6) ? . . . . O(2) Mo(1) S(2) Mo(2) 103.46(5) ? . . . . Mo(2) Mo(1) S(4) Rh(1) -38.55(6) ? . . . . Mo(2) Mo(1) S(4) Mo(3) 44.68(5) ? . . . . Mo(3) Mo(1) S(4) Rh(1) -83.23(5) ? . . . . S(1) Mo(1) S(4) Rh(1) -92.43(6) ? . . . . S(1) Mo(1) S(4) Mo(3) -9.20(6) ? . . . . S(2) Mo(1) S(4) Rh(1) 13.70(6) ? . . . . S(2) Mo(1) S(4) Mo(3) 96.94(5) ? . . . . O(1) Mo(1) S(4) Rh(1) 94.88(6) ? . . . . O(1) Mo(1) S(4) Mo(3) 178.11(5) ? . . . . O(2) Mo(1) S(4) Rh(1) 103.1(2) ? . . . . O(2) Mo(1) S(4) Mo(3) -173.7(2) ? . . . . Rh(1) Mo(2) Mo(3) Mo(1) -75.48(2) ? . . . . Rh(1) Mo(2) Mo(3) S(1) -140.70(7) ? . . . . Rh(1) Mo(2) Mo(3) S(3) 59.76(7) ? . . . . Rh(1) Mo(2) Mo(3) S(4) -35.02(4) ? . . . . Rh(1) Mo(2) Mo(3) O(6) 51.4(2) ? . . . . Rh(1) Mo(2) Mo(3) O(7) -141.0(3) ? . . . . Rh(1) Mo(2) Mo(3) O(8) 135.3(1) ? . . . . Mo(1) Mo(2) Mo(3) S(1) -65.22(7) ? . . . . Mo(1) Mo(2) Mo(3) S(3) 135.24(7) ? . . . . Mo(1) Mo(2) Mo(3) S(4) 40.46(5) ? . . . . Mo(1) Mo(2) Mo(3) O(6) 126.9(2) ? . . . . Mo(1) Mo(2) Mo(3) O(7) -65.5(3) ? . . . . Mo(1) Mo(2) Mo(3) O(8) -149.2(1) ? . . . . S(1) Mo(2) Mo(3) Mo(1) 65.22(3) ? . . . . S(1) Mo(2) Mo(3) S(3) -159.54(7) ? . . . . S(1) Mo(2) Mo(3) S(4) 105.68(5) ? . . . . S(1) Mo(2) Mo(3) O(6) -167.9(2) ? . . . . S(1) Mo(2) Mo(3) O(7) -0.3(3) ? . . . . S(1) Mo(2) Mo(3) O(8) -84.0(1) ? . . . . S(2) Mo(2) Mo(3) Mo(1) -36.27(2) ? . . . . S(2) Mo(2) Mo(3) S(1) -101.49(7) ? . . . . S(2) Mo(2) Mo(3) S(3) 98.97(7) ? . . . . S(2) Mo(2) Mo(3) S(4) 4.18(5) ? . . . . S(2) Mo(2) Mo(3) O(6) 90.6(2) ? . . . . S(2) Mo(2) Mo(3) O(7) -101.8(3) ? . . . . S(2) Mo(2) Mo(3) O(8) 174.5(1) ? . . . . S(3) Mo(2) Mo(3) Mo(1) -135.24(3) ? . . . . S(3) Mo(2) Mo(3) S(1) 159.54(7) ? . . . . S(3) Mo(2) Mo(3) S(4) -94.79(5) ? . . . . S(3) Mo(2) Mo(3) O(6) -8.4(2) ? . . . . S(3) Mo(2) Mo(3) O(7) 159.2(3) ? . . . . S(3) Mo(2) Mo(3) O(8) 75.5(1) ? . . . . O(3) Mo(2) Mo(3) Mo(1) -134.68(6) ? . . . . O(3) Mo(2) Mo(3) S(1) 160.10(9) ? . . . . O(3) Mo(2) Mo(3) S(3) 0.57(8) ? . . . . O(3) Mo(2) Mo(3) S(4) -94.22(7) ? . . . . O(3) Mo(2) Mo(3) O(6) -7.8(2) ? . . . . O(3) Mo(2) Mo(3) O(7) 159.8(3) ? . . . . O(3) Mo(2) Mo(3) O(8) 76.1(1) ? . . . . O(4) Mo(2) Mo(3) Mo(1) 146.46(3) ? . . . . O(4) Mo(2) Mo(3) S(1) 81.24(7) ? . . . . O(4) Mo(2) Mo(3) S(3) -78.30(7) ? . . . . O(4) Mo(2) Mo(3) S(4) -173.08(5) ? . . . . O(4) Mo(2) Mo(3) O(6) -86.7(2) ? . . . . O(4) Mo(2) Mo(3) O(7) 80.9(3) ? . . . . O(4) Mo(2) Mo(3) O(8) -2.8(1) ? . . . . O(5) Mo(2) Mo(3) Mo(1) 65.98(5) ? . . . . O(5) Mo(2) Mo(3) S(1) 0.76(8) ? . . . . O(5) Mo(2) Mo(3) S(3) -158.78(9) ? . . . . O(5) Mo(2) Mo(3) S(4) 106.44(7) ? . . . . O(5) Mo(2) Mo(3) O(6) -167.2(2) ? . . . . O(5) Mo(2) Mo(3) O(7) 0.5(3) ? . . . . O(5) Mo(2) Mo(3) O(8) -83.3(1) ? . . . . Rh(1) Mo(2) S(1) Mo(1) -39.04(6) ? . . . . Rh(1) Mo(2) S(1) Mo(3) 36.80(6) ? . . . . Mo(1) Mo(2) S(1) Mo(3) 75.84(5) ? . . . . Mo(3) Mo(2) S(1) Mo(1) -75.84(5) ? . . . . S(2) Mo(2) S(1) Mo(1) 15.91(6) ? . . . . S(2) Mo(2) S(1) Mo(3) 91.75(6) ? . . . . S(3) Mo(2) S(1) Mo(1) -92.88(5) ? . . . . S(3) Mo(2) S(1) Mo(3) -17.04(6) ? . . . . O(3) Mo(2) S(1) Mo(1) 142.6(2) ? . . . . O(3) Mo(2) S(1) Mo(3) -141.5(2) ? . . . . O(4) Mo(2) S(1) Mo(1) -174.78(6) ? . . . . O(4) Mo(2) S(1) Mo(3) -98.94(5) ? . . . . O(5) Mo(2) S(1) Mo(1) 104.70(5) ? . . . . O(5) Mo(2) S(1) Mo(3) -179.47(6) ? . . . . Rh(1) Mo(2) S(2) Mo(1) 84.35(6) ? . . . . Mo(1) Mo(2) S(2) Rh(1) -84.35(6) ? . . . . Mo(3) Mo(2) S(2) Rh(1) -46.00(5) ? . . . . Mo(3) Mo(2) S(2) Mo(1) 38.35(4) ? . . . . S(1) Mo(2) S(2) Rh(1) -99.96(5) ? . . . . S(1) Mo(2) S(2) Mo(1) -15.62(5) ? . . . . S(3) Mo(2) S(2) Rh(1) 9.54(5) ? . . . . S(3) Mo(2) S(2) Mo(1) 93.89(4) ? . . . . O(3) Mo(2) S(2) Rh(1) 95.91(4) ? . . . . O(3) Mo(2) S(2) Mo(1) -179.74(5) ? . . . . O(4) Mo(2) S(2) Rh(1) 123.8(2) ? . . . . O(4) Mo(2) S(2) Mo(1) -151.9(2) ? . . . . O(5) Mo(2) S(2) Rh(1) 176.76(5) ? . . . . O(5) Mo(2) S(2) Mo(1) -98.90(4) ? . . . . Rh(1) Mo(2) S(3) Mo(3) -83.99(5) ? . . . . Mo(1) Mo(2) S(3) Rh(1) 46.21(6) ? . . . . Mo(1) Mo(2) S(3) Mo(3) -37.78(5) ? . . . . Mo(3) Mo(2) S(3) Rh(1) 83.99(5) ? . . . . S(1) Mo(2) S(3) Rh(1) 100.67(5) ? . . . . S(1) Mo(2) S(3) Mo(3) 16.68(6) ? . . . . S(2) Mo(2) S(3) Rh(1) -9.65(6) ? . . . . S(2) Mo(2) S(3) Mo(3) -93.64(5) ? . . . . O(3) Mo(2) S(3) Rh(1) -95.66(5) ? . . . . O(3) Mo(2) S(3) Mo(3) -179.65(5) ? . . . . O(4) Mo(2) S(3) Rh(1) -175.43(6) ? . . . . O(4) Mo(2) S(3) Mo(3) 100.58(5) ? . . . . O(5) Mo(2) S(3) Rh(1) -146.7(2) ? . . . . O(5) Mo(2) S(3) Mo(3) 129.3(2) ? . . . . Mo(1) Mo(3) S(1) Mo(2) -77.42(6) ? . . . . Mo(2) Mo(3) S(1) Mo(1) 77.42(6) ? . . . . S(3) Mo(3) S(1) Mo(1) 93.93(5) ? . . . . S(3) Mo(3) S(1) Mo(2) 16.51(6) ? . . . . S(4) Mo(3) S(1) Mo(1) -9.24(6) ? . . . . S(4) Mo(3) S(1) Mo(2) -86.66(5) ? . . . . O(6) Mo(3) S(1) Mo(1) -145.2(2) ? . . . . O(6) Mo(3) S(1) Mo(2) 137.4(2) ? . . . . O(7) Mo(3) S(1) Mo(1) -102.78(5) ? . . . . O(7) Mo(3) S(1) Mo(2) 179.81(6) ? . . . . O(8) Mo(3) S(1) Mo(1) 174.94(5) ? . . . . O(8) Mo(3) S(1) Mo(2) 97.52(5) ? . . . . Mo(1) Mo(3) S(3) Rh(1) -40.98(5) ? . . . . Mo(1) Mo(3) S(3) Mo(2) 38.66(5) ? . . . . Mo(2) Mo(3) S(3) Rh(1) -79.64(7) ? . . . . S(1) Mo(3) S(3) Rh(1) -96.42(5) ? . . . . S(1) Mo(3) S(3) Mo(2) -16.77(6) ? . . . . S(4) Mo(3) S(3) Rh(1) 13.35(6) ? . . . . S(4) Mo(3) S(3) Mo(2) 92.99(5) ? . . . . O(6) Mo(3) S(3) Rh(1) 94.42(5) ? . . . . O(6) Mo(3) S(3) Mo(2) 174.06(6) ? . . . . O(7) Mo(3) S(3) Rh(1) 143.9(1) ? . . . . O(7) Mo(3) S(3) Mo(2) -136.5(1) ? . . . . O(8) Mo(3) S(3) Rh(1) 177.49(6) ? . . . . O(8) Mo(3) S(3) Mo(2) -102.87(5) ? . . . . Mo(1) Mo(3) S(4) Rh(1) 84.41(7) ? . . . . Mo(2) Mo(3) S(4) Rh(1) 39.76(5) ? . . . . Mo(2) Mo(3) S(4) Mo(1) -44.65(5) ? . . . . S(1) Mo(3) S(4) Rh(1) 93.71(5) ? . . . . S(1) Mo(3) S(4) Mo(1) 9.31(6) ? . . . . S(3) Mo(3) S(4) Rh(1) -13.06(6) ? . . . . S(3) Mo(3) S(4) Mo(1) -97.47(5) ? . . . . O(6) Mo(3) S(4) Rh(1) -95.07(5) ? . . . . O(6) Mo(3) S(4) Mo(1) -179.47(5) ? . . . . O(7) Mo(3) S(4) Rh(1) -178.48(5) ? . . . . O(7) Mo(3) S(4) Mo(1) 97.12(5) ? . . . . O(8) Mo(3) S(4) Rh(1) -101.9(2) ? . . . . O(8) Mo(3) S(4) Mo(1) 173.7(2) ? . . . . O(9) S(5) C(11) C(12) -73.3(6) ? . . . . O(9) S(5) C(11) C(16) 105.7(6) ? . . . . O(10) S(5) C(11) C(12) 46.0(6) ? . . . . O(10) S(5) C(11) C(16) -135.0(6) ? . . . . O(11) S(5) C(11) C(12) 166.2(5) ? . . . . O(11) S(5) C(11) C(16) -14.8(6) ? . . . . O(12) S(6) C(18) C(19) 54.9(8) ? . . . . O(12) S(6) C(18) C(23) -128.5(7) ? . . . . O(13) S(6) C(18) C(19) -64.1(8) ? . . . . O(13) S(6) C(18) C(23) 112.5(7) ? . . . . O(14) S(6) C(18) C(19) 176.0(7) ? . . . . O(14) S(6) C(18) C(23) -7.4(9) ? . . . . O(15) S(7) C(32) C(33) 37.6(7) ? . . . . O(15) S(7) C(32) C(37) -146.8(6) ? . . . . O(16) S(7) C(32) C(33) 157.7(6) ? . . . . O(16) S(7) C(32) C(37) -26.7(7) ? . . . . O(17) S(7) C(32) C(33) -83.2(7) ? . . . . O(17) S(7) C(32) C(37) 92.4(7) ? . . . . O(18) S(8) C(25) C(26) -138.8(6) ? . . . . O(18) S(8) C(25) C(30) 46.0(7) ? . . . . O(19) S(8) C(25) C(26) -18.8(7) ? . . . . O(19) S(8) C(25) C(30) 166.0(6) ? . . . . O(20) S(8) C(25) C(26) 103.0(6) ? . . . . O(20) S(8) C(25) C(30) -72.2(7) ? . . . . Rh(1) C(1) C(2) C(3) -61.9(5) ? . . . . Rh(1) C(1) C(2) C(7) 123.3(8) ? . . . . C(5) C(1) C(2) Rh(1) 60.4(5) ? . . . . C(5) C(1) C(2) C(3) -1.5(8) ? . . . . C(5) C(1) C(2) C(7) -176.3(7) ? . . . . C(6) C(1) C(2) Rh(1) -125.5(7) ? . . . . C(6) C(1) C(2) C(3) 172.6(7) ? . . . . C(6) C(1) C(2) C(7) -2(1) ? . . . . Rh(1) C(1) C(5) C(4) 63.1(6) ? . . . . Rh(1) C(1) C(5) C(10) -121.4(8) ? . . . . C(2) C(1) C(5) Rh(1) -60.7(5) ? . . . . C(2) C(1) C(5) C(4) 2.5(8) ? . . . . C(2) C(1) C(5) C(10) 177.9(7) ? . . . . C(6) C(1) C(5) Rh(1) 125.1(8) ? . . . . C(6) C(1) C(5) C(4) -171.7(7) ? . . . . C(6) C(1) C(5) C(10) 3(1) ? . . . . Rh(1) C(2) C(3) C(4) -62.3(6) ? . . . . Rh(1) C(2) C(3) C(8) 124.7(7) ? . . . . C(1) C(2) C(3) Rh(1) 62.2(5) ? . . . . C(1) C(2) C(3) C(4) -0.1(6) ? . . . . C(1) C(2) C(3) C(8) -173.1(7) ? . . . . C(7) C(2) C(3) Rh(1) -122.8(7) ? . . . . C(7) C(2) C(3) C(4) 175.0(6) ? . . . . C(7) C(2) C(3) C(8) 1(1) ? . . . . Rh(1) C(3) C(4) C(5) -59.7(6) ? . . . . Rh(1) C(3) C(4) C(9) 123.1(7) ? . . . . C(2) C(3) C(4) Rh(1) 61.3(5) ? . . . . C(2) C(3) C(4) C(5) 1.6(8) ? . . . . C(2) C(3) C(4) C(9) -175.7(7) ? . . . . C(8) C(3) C(4) Rh(1) -125.4(6) ? . . . . C(8) C(3) C(4) C(5) 174.9(6) ? . . . . C(8) C(3) C(4) C(9) -2(1) ? . . . . Rh(1) C(4) C(5) C(1) -62.7(5) ? . . . . Rh(1) C(4) C(5) C(10) 122.0(8) ? . . . . C(3) C(4) C(5) Rh(1) 60.1(5) ? . . . . C(3) C(4) C(5) C(1) -2.5(8) ? . . . . C(3) C(4) C(5) C(10) -177.9(7) ? . . . . C(9) C(4) C(5) Rh(1) -122.6(8) ? . . . . C(9) C(4) C(5) C(1) 174.7(7) ? . . . . C(9) C(4) C(5) C(10) 0(1) ? . . . . S(5) C(11) C(12) C(13) 177.8(6) ? . . . . C(16) C(11) C(12) C(13) -1(1) ? . . . . S(5) C(11) C(16) C(15) -177.3(6) ? . . . . C(12) C(11) C(16) C(15) 1(1) ? . . . . C(11) C(12) C(13) C(14) 1(1) ? . . . . C(12) C(13) C(14) C(15) -2(1) ? . . . . C(12) C(13) C(14) C(17) 177.8(8) ? . . . . C(13) C(14) C(15) C(16) 3(1) ? . . . . C(17) C(14) C(15) C(16) -177.3(7) ? . . . . C(14) C(15) C(16) C(11) -2(1) ? . . . . S(6) C(18) C(19) C(20) 175.3(8) ? . . . . C(23) C(18) C(19) C(20) -1(1) ? . . . . S(6) C(18) C(23) C(22) -176.3(8) ? . . . . C(19) C(18) C(23) C(22) 0(1) ? . . . . C(18) C(19) C(20) C(21) 1(1) ? . . . . C(19) C(20) C(21) C(22) 0(1) ? . . . . C(19) C(20) C(21) C(24) -178.7(9) ? . . . . C(20) C(21) C(22) C(23) 0(1) ? . . . . C(24) C(21) C(22) C(23) 177.7(9) ? . . . . C(21) C(22) C(23) C(18) 0(1) ? . . . . S(8) C(25) C(26) C(27) -176.5(7) ? . . . . C(30) C(25) C(26) C(27) -1(1) ? . . . . S(8) C(25) C(30) C(29) 176.3(7) ? . . . . C(26) C(25) C(30) C(29) 1(1) ? . . . . C(25) C(26) C(27) C(28) 0(1) ? . . . . C(26) C(27) C(28) C(29) 0(1) ? . . . . C(26) C(27) C(28) C(31) -179.1(8) ? . . . . C(27) C(28) C(29) C(30) -1(1) ? . . . . C(31) C(28) C(29) C(30) 178.8(8) ? . . . . C(28) C(29) C(30) C(25) 0(1) ? . . . . S(7) C(32) C(33) C(34) 174.8(7) ? . . . . C(37) C(32) C(33) C(34) 0(1) ? . . . . S(7) C(32) C(37) C(36) -173.6(7) ? . . . . C(33) C(32) C(37) C(36) 2(1) ? . . . . C(32) C(33) C(34) C(35) 0(1) ? . . . . C(33) C(34) C(35) C(36) 1(1) ? . . . . C(33) C(34) C(35) C(38) -178.6(9) ? . . . . C(34) C(35) C(36) C(37) 0(1) ? . . . . C(38) C(35) C(36) C(37) 179.9(6) ? . . . . C(35) C(36) C(37) C(32) -1(1) ? . . . .
1100717.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100717.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100717 loop_ _publ_author_name 'Chong Zheng' 'Hansj\"urgen Mattausch' 'Arndt Simon' _publ_section_title ; La9Sb16Br3 and Ce9Sb16Cl3: Stars and Stripes in Rare Earth Halide and Intermetallic Compounds ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3684 _journal_page_last 3689 _journal_paper_doi 10.1021/ic049220u _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'Br3 La9 Sb16' _chemical_formula_weight 3437.92 _chemical_name_systematic ; ? ; _space_group_IT_number 176 _symmetry_cell_setting hexagonal _symmetry_space_group_name_Hall '-P 6c' _symmetry_space_group_name_H-M 'P 63/m' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_formula_units_Z 2 _cell_length_a 21.232(5) _cell_length_b 21.232(5) _cell_length_c 4.323(2) _cell_measurement_reflns_used 565 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 14 _cell_measurement_theta_min -14 _cell_volume 1687.7(10) _computing_cell_refinement 'SMART and SAINT (Bruker, 1999)' _computing_data_collection 'SMART (Bruker, 1999)' _computing_data_reduction 'SAINT (Bruker, 1999)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _computing_structure_refinement 'SHELXTL (Sheldrick, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 0 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Siemens SMART CCD PLATFORM' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0233 _diffrn_reflns_av_sigmaI/netI 0.0130 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_number 8423 _diffrn_reflns_theta_full 24.98 _diffrn_reflns_theta_max 24.98 _diffrn_reflns_theta_min 1.92 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 27.202 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.474137 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Sheldrick, 2000)' _exptl_crystal_colour metallic _exptl_crystal_density_diffrn 6.766 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 2868 _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _refine_diff_density_max 4.202 _refine_diff_density_min -2.276 _refine_diff_density_rms 0.333 _refine_ls_extinction_coef 0.000206(19) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.608 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 58 _refine_ls_number_reflns 1130 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.608 _refine_ls_R_factor_all 0.0411 _refine_ls_R_factor_gt 0.0411 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+85.2061P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0866 _refine_ls_wR_factor_ref 0.0866 _reflns_number_gt 1130 _reflns_number_total 1130 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic049220usi20040615_061213.cif _cod_data_source_block La9Sb16Br3 _cod_original_cell_volume 1687.5(10) _cod_database_code 1100717 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, x-y, z' '-x+y, -x, z' 'x-y, x, z+1/2' 'y, -x+y, z+1/2' '-x, -y, -z' 'x, y, -z-1/2' 'y, -x+y, -z' 'x-y, x, -z' '-x+y, -x, -z-1/2' '-y, x-y, -z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group La1 La 0.54177(6) 0.30907(6) 0.2500 0.0116(3) Uani 1 2 d S . . La2 La 0.15177(7) 0.24644(7) 0.2500 0.0142(3) Uani 1 2 d S . . La3 La 0.39401(7) 0.40126(7) 0.2500 0.0133(3) Uani 1 2 d S . . Sb1 Sb 0.3333 0.6667 0.2500 0.0126(5) Uani 1 6 d S . . Sb2 Sb 0.48461(8) 0.58790(8) 0.2500 0.0139(3) Uani 1 2 d S . . Sb3 Sb 0.50849(8) 0.13684(8) 0.2500 0.0163(4) Uani 1 2 d S . . Sb4 Sb 0.25005(7) 0.42872(8) 0.2500 0.0129(3) Uani 1 2 d S . . Sb5 Sb 0.35740(8) 0.22580(8) 0.2500 0.0164(4) Uani 1 2 d S . . Sb6 Sb 0.00952(8) 0.28500(8) 0.2500 0.0151(3) Uani 1 2 d S . . Br Br 0.14803(12) 0.09809(12) 0.2500 0.0180(5) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La1 0.0121(6) 0.0111(6) 0.0119(6) 0.000 0.000 0.0061(5) La2 0.0144(6) 0.0143(6) 0.0149(7) 0.000 0.000 0.0080(5) La3 0.0131(6) 0.0129(6) 0.0143(7) 0.000 0.000 0.0068(5) Sb1 0.0131(7) 0.0131(7) 0.0115(13) 0.000 0.000 0.0066(4) Sb2 0.0140(7) 0.0146(7) 0.0141(8) 0.000 0.000 0.0079(6) Sb3 0.0144(7) 0.0126(7) 0.0199(9) 0.000 0.000 0.0051(6) Sb4 0.0122(7) 0.0128(7) 0.0135(8) 0.000 0.000 0.0061(6) Sb5 0.0125(7) 0.0125(7) 0.0211(8) 0.000 0.000 0.0038(6) Sb6 0.0163(7) 0.0131(7) 0.0153(8) 0.000 0.000 0.0070(6) Br 0.0203(11) 0.0180(11) 0.0183(12) 0.000 0.000 0.0114(9) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Sb1 La1 Sb1 83.17(4) 7_666 7_665 ? Sb1 La1 Sb2 81.71(3) 7_666 7_666 ? Sb1 La1 Sb2 136.15(5) 7_665 7_666 ? Sb1 La1 Sb2 136.15(5) 7_666 7_665 ? Sb1 La1 Sb2 81.71(3) 7_665 7_665 ? Sb2 La1 Sb2 81.35(5) 7_666 7_665 ? Sb1 La1 Sb3 83.37(3) 7_666 4_665 ? Sb1 La1 Sb3 83.37(3) 7_665 4_665 ? Sb2 La1 Sb3 54.15(3) 7_666 4_665 ? Sb2 La1 Sb3 54.15(3) 7_665 4_665 ? Sb1 La1 Sb3 83.32(3) 7_666 . ? Sb1 La1 Sb3 83.32(3) 7_665 . ? Sb2 La1 Sb3 134.83(3) 7_666 . ? Sb2 La1 Sb3 134.83(3) 7_665 . ? Sb3 La1 Sb3 162.18(5) 4_665 . ? Sb1 La1 Sb4 137.88(4) 7_666 9 ? Sb1 La1 Sb4 83.91(3) 7_665 9 ? Sb2 La1 Sb4 132.17(5) 7_666 9 ? Sb2 La1 Sb4 80.72(4) 7_665 9 ? Sb3 La1 Sb4 134.38(3) 4_665 9 ? Sb3 La1 Sb4 55.41(3) . 9 ? Sb1 La1 Sb4 83.91(3) 7_666 9_556 ? Sb1 La1 Sb4 137.88(5) 7_665 9_556 ? Sb2 La1 Sb4 80.72(4) 7_666 9_556 ? Sb2 La1 Sb4 132.17(5) 7_665 9_556 ? Sb3 La1 Sb4 134.38(3) 4_665 9_556 ? Sb3 La1 Sb4 55.41(3) . 9_556 ? Sb4 La1 Sb4 79.38(5) 9 9_556 ? Sb1 La1 Sb5 135.90(2) 7_666 . ? Sb1 La1 Sb5 135.90(2) 7_665 . ? Sb2 La1 Sb5 79.19(4) 7_666 . ? Sb2 La1 Sb5 79.19(4) 7_665 . ? Sb3 La1 Sb5 115.12(5) 4_665 . ? Sb3 La1 Sb5 82.70(4) . . ? Sb4 La1 Sb5 54.02(3) 9 . ? Sb4 La1 Sb5 54.02(3) 9_556 . ? Sb1 La1 La1 49.629(16) 7_666 4_665 ? Sb1 La1 La1 49.629(15) 7_665 4_665 ? Sb2 La1 La1 90.43(4) 7_666 4_665 ? Sb2 La1 La1 90.43(4) 7_665 4_665 ? Sb3 La1 La1 51.13(4) 4_665 4_665 ? Sb3 La1 La1 111.05(4) . 4_665 ? Sb4 La1 La1 133.53(3) 9 4_665 ? Sb4 La1 La1 133.53(3) 9_556 4_665 ? Sb5 La1 La1 166.25(5) . 4_665 ? Sb1 La1 La1 49.628(15) 7_666 3_655 ? Sb1 La1 La1 49.628(15) 7_665 3_655 ? Sb2 La1 La1 131.34(3) 7_666 3_655 ? Sb2 La1 La1 131.34(3) 7_665 3_655 ? Sb3 La1 La1 111.12(4) 4_665 3_655 ? Sb3 La1 La1 51.05(4) . 3_655 ? Sb4 La1 La1 92.71(4) 9 3_655 ? Sb4 La1 La1 92.71(4) 9_556 3_655 ? Sb5 La1 La1 133.75(5) . 3_655 ? La1 La1 La1 60.0 4_665 3_655 ? Br La2 Br 90.93(8) 10 10_556 ? Br La2 Br 69.75(7) 10 . ? Br La2 Br 69.75(7) 10_556 . ? Br La2 Sb4 127.79(5) 10 . ? Br La2 Sb4 127.79(5) 10_556 . ? Br La2 Sb4 148.68(6) . . ? Br La2 Sb6 146.00(6) 10 9_556 ? Br La2 Sb6 85.00(5) 10_556 9_556 ? Br La2 Sb6 77.23(5) . 9_556 ? Sb4 La2 Sb6 78.90(4) . 9_556 ? Br La2 Sb6 85.00(5) 10 9 ? Br La2 Sb6 146.00(6) 10_556 9 ? Br La2 Sb6 77.23(5) . 9 ? Sb4 La2 Sb6 78.90(4) . 9 ? Sb6 La2 Sb6 79.98(5) 9_556 9 ? Br La2 Sb5 129.88(6) 10 10_556 ? Br La2 Sb5 74.29(5) 10_556 10_556 ? Br La2 Sb5 139.30(3) . 10_556 ? Sb4 La2 Sb5 54.42(3) . 10_556 ? Sb6 La2 Sb5 81.33(4) 9_556 10_556 ? Sb6 La2 Sb5 132.19(5) 9 10_556 ? Br La2 Sb5 74.29(5) 10 10 ? Br La2 Sb5 129.88(6) 10_556 10 ? Br La2 Sb5 139.30(3) . 10 ? Sb4 La2 Sb5 54.42(3) . 10 ? Sb6 La2 Sb5 132.19(5) 9_556 10 ? Sb6 La2 Sb5 81.33(4) 9 10 ? Sb5 La2 Sb5 79.54(5) 10_556 10 ? Br La2 Sb6 76.11(5) 10 . ? Br La2 Sb6 76.11(5) 10_556 . ? Br La2 Sb6 130.41(6) . . ? Sb4 La2 Sb6 80.91(4) . . ? Sb6 La2 Sb6 134.58(3) 9_556 . ? Sb6 La2 Sb6 134.58(3) 9 . ? Sb5 La2 Sb6 53.99(3) 10_556 . ? Sb5 La2 Sb6 53.99(3) 10 . ? Sb2 La3 Sb2 82.37(5) 7_666 7_665 ? Sb2 La3 Sb6 133.91(5) 7_666 9 ? Sb2 La3 Sb6 80.48(4) 7_665 9 ? Sb2 La3 Sb6 80.48(4) 7_666 9_556 ? Sb2 La3 Sb6 133.91(5) 7_665 9_556 ? Sb6 La3 Sb6 81.42(5) 9 9_556 ? Sb2 La3 Sb3 84.28(4) 7_666 10_556 ? Sb2 La3 Sb3 138.80(5) 7_665 10_556 ? Sb6 La3 Sb3 133.73(5) 9 10_556 ? Sb6 La3 Sb3 81.22(4) 9_556 10_556 ? Sb2 La3 Sb3 138.80(5) 7_666 10 ? Sb2 La3 Sb3 84.28(4) 7_665 10 ? Sb6 La3 Sb3 81.22(4) 9 10 ? Sb6 La3 Sb3 133.73(5) 9_556 10 ? Sb3 La3 Sb3 80.62(5) 10_556 10 ? Sb2 La3 Sb4 137.11(3) 7_666 . ? Sb2 La3 Sb4 137.11(3) 7_665 . ? Sb6 La3 Sb4 79.16(4) 9 . ? Sb6 La3 Sb4 79.16(4) 9_556 . ? Sb3 La3 Sb4 55.57(3) 10_556 . ? Sb3 La3 Sb4 55.57(3) 10 . ? Sb2 La3 Sb5 79.53(4) 7_666 . ? Sb2 La3 Sb5 79.53(4) 7_665 . ? Sb6 La3 Sb5 55.43(3) 9 . ? Sb6 La3 Sb5 55.43(3) 9_556 . ? Sb3 La3 Sb5 135.51(3) 10_556 . ? Sb3 La3 Sb5 135.51(3) 10 . ? Sb4 La3 Sb5 117.17(5) . . ? Sb2 La3 Sb2 87.24(4) 7_666 . ? Sb2 La3 Sb2 87.24(4) 7_665 . ? Sb6 La3 Sb2 133.87(3) 9 . ? Sb6 La3 Sb2 133.87(3) 9_556 . ? Sb3 La3 Sb2 53.26(3) 10_556 . ? Sb3 La3 Sb2 53.26(3) 10 . ? Sb4 La3 Sb2 80.46(4) . . ? Sb5 La3 Sb2 162.37(5) . . ? La1 Sb1 La1 83.17(4) 10 10_556 ? La1 Sb1 La1 136.078(15) 10 9_566 ? La1 Sb1 La1 80.74(3) 10_556 9_566 ? La1 Sb1 La1 80.74(3) 10 9_565 ? La1 Sb1 La1 136.078(14) 10_556 9_565 ? La1 Sb1 La1 83.17(4) 9_566 9_565 ? La1 Sb1 La1 136.077(15) 10 7_666 ? La1 Sb1 La1 80.74(3) 10_556 7_666 ? La1 Sb1 La1 80.75(3) 9_566 7_666 ? La1 Sb1 La1 136.079(14) 9_565 7_666 ? La1 Sb1 La1 80.74(3) 10 7_665 ? La1 Sb1 La1 136.077(14) 10_556 7_665 ? La1 Sb1 La1 136.079(14) 9_566 7_665 ? La1 Sb1 La1 80.75(3) 9_565 7_665 ? La1 Sb1 La1 83.17(4) 7_666 7_665 ? Sb3 Sb2 Sb3 90.74(6) 10 10_556 ? Sb3 Sb2 La3 151.89(6) 10 7_666 ? Sb3 Sb2 La3 86.84(4) 10_556 7_666 ? Sb3 Sb2 La3 86.84(4) 10 7_665 ? Sb3 Sb2 La3 151.89(6) 10_556 7_665 ? La3 Sb2 La3 82.37(5) 7_666 7_665 ? Sb3 Sb2 La1 118.89(6) 10 7_666 ? Sb3 Sb2 La1 63.60(4) 10_556 7_666 ? La3 Sb2 La1 84.85(4) 7_666 7_666 ? La3 Sb2 La1 140.23(6) 7_665 7_666 ? Sb3 Sb2 La1 63.60(4) 10 7_665 ? Sb3 Sb2 La1 118.89(6) 10_556 7_665 ? La3 Sb2 La1 140.23(6) 7_666 7_665 ? La3 Sb2 La1 84.85(4) 7_665 7_665 ? La1 Sb2 La1 81.35(5) 7_666 7_665 ? Sb3 Sb2 La3 61.82(4) 10 . ? Sb3 Sb2 La3 61.82(4) 10_556 . ? La3 Sb2 La3 92.76(4) 7_666 . ? La3 Sb2 La3 92.76(4) 7_665 . ? La1 Sb2 La3 125.42(4) 7_666 . ? La1 Sb2 La3 125.42(4) 7_665 . ? Sb2 Sb3 Sb2 90.74(6) 9_556 9 ? Sb2 Sb3 Sb4 177.21(6) 9_556 9 ? Sb2 Sb3 Sb4 91.02(4) 9 9 ? Sb2 Sb3 Sb4 91.02(4) 9_556 9_556 ? Sb2 Sb3 Sb4 177.21(6) 9 9_556 ? Sb4 Sb3 Sb4 87.14(6) 9 9_556 ? Sb2 Sb3 La3 119.80(6) 9_556 9 ? Sb2 Sb3 La3 64.92(4) 9 9 ? Sb4 Sb3 La3 62.95(4) 9 9 ? Sb4 Sb3 La3 115.91(6) 9_556 9 ? Sb2 Sb3 La3 64.92(4) 9_556 9_556 ? Sb2 Sb3 La3 119.80(6) 9 9_556 ? Sb4 Sb3 La3 115.91(6) 9 9_556 ? Sb4 Sb3 La3 62.95(4) 9_556 9_556 ? La3 Sb3 La3 80.62(5) 9 9_556 ? Sb2 Sb3 La1 62.25(4) 9_556 3_655 ? Sb2 Sb3 La1 62.25(4) 9 3_655 ? Sb4 Sb3 La1 116.83(4) 9 3_655 ? Sb4 Sb3 La1 116.83(4) 9_556 3_655 ? La3 Sb3 La1 127.17(4) 9 3_655 ? La3 Sb3 La1 127.17(4) 9_556 3_655 ? Sb2 Sb3 La1 114.58(4) 9_556 . ? Sb2 Sb3 La1 114.58(4) 9 . ? Sb4 Sb3 La1 62.69(4) 9 . ? Sb4 Sb3 La1 62.69(4) 9_556 . ? La3 Sb3 La1 125.61(4) 9 . ? La3 Sb3 La1 125.61(4) 9_556 . ? La1 Sb3 La1 77.82(5) 3_655 . ? Sb5 Sb4 Sb5 89.16(6) 10 10_556 ? Sb5 Sb4 Sb3 177.30(6) 10 10_556 ? Sb5 Sb4 Sb3 91.79(4) 10_556 10_556 ? Sb5 Sb4 Sb3 91.79(4) 10 10 ? Sb5 Sb4 Sb3 177.30(6) 10_556 10 ? Sb3 Sb4 Sb3 87.14(6) 10_556 10 ? Sb5 Sb4 La2 63.18(4) 10 . ? Sb5 Sb4 La2 63.18(4) 10_556 . ? Sb3 Sb4 La2 119.49(4) 10_556 . ? Sb3 Sb4 La2 119.49(4) 10 . ? Sb5 Sb4 La1 116.44(5) 10 10_556 ? Sb5 Sb4 La1 63.18(4) 10_556 10_556 ? Sb3 Sb4 La1 61.89(4) 10_556 10_556 ? Sb3 Sb4 La1 114.16(5) 10 10_556 ? La2 Sb4 La1 126.35(4) . 10_556 ? Sb5 Sb4 La1 63.18(4) 10 10 ? Sb5 Sb4 La1 116.44(5) 10_556 10 ? Sb3 Sb4 La1 114.16(5) 10_556 10 ? Sb3 Sb4 La1 61.89(4) 10 10 ? La2 Sb4 La1 126.35(4) . 10 ? La1 Sb4 La1 79.38(5) 10_556 10 ? Sb5 Sb4 La3 120.07(4) 10 . ? Sb5 Sb4 La3 120.07(4) 10_556 . ? Sb3 Sb4 La3 61.49(4) 10_556 . ? Sb3 Sb4 La3 61.49(4) 10 . ? La2 Sb4 La3 84.01(4) . . ? La1 Sb4 La3 123.36(4) 10_556 . ? La1 Sb4 La3 123.36(4) 10 . ? Sb4 Sb5 Sb4 89.16(6) 9_556 9 ? Sb4 Sb5 Sb6 179.07(5) 9_556 9 ? Sb4 Sb5 Sb6 91.67(4) 9 9 ? Sb4 Sb5 Sb6 91.67(4) 9_556 9_556 ? Sb4 Sb5 Sb6 179.07(5) 9 9_556 ? Sb6 Sb5 Sb6 87.50(6) 9 9_556 ? Sb4 Sb5 La2 115.77(6) 9_556 9 ? Sb4 Sb5 La2 62.40(4) 9 9 ? Sb6 Sb5 La2 65.02(4) 9 9 ? Sb6 Sb5 La2 117.55(6) 9_556 9 ? Sb4 Sb5 La2 62.40(4) 9_556 9_556 ? Sb4 Sb5 La2 115.77(6) 9 9_556 ? Sb6 Sb5 La2 117.55(6) 9 9_556 ? Sb6 Sb5 La2 65.02(4) 9_556 9_556 ? La2 Sb5 La2 79.54(5) 9 9_556 ? Sb4 Sb5 La1 62.80(4) 9_556 . ? Sb4 Sb5 La1 62.80(4) 9 . ? Sb6 Sb5 La1 117.25(4) 9 . ? Sb6 Sb5 La1 117.25(4) 9_556 . ? La2 Sb5 La1 125.20(4) 9 . ? La2 Sb5 La1 125.20(4) 9_556 . ? Sb4 Sb5 La3 118.39(4) 9_556 . ? Sb4 Sb5 La3 118.39(4) 9 . ? Sb6 Sb5 La3 60.82(4) 9 . ? Sb6 Sb5 La3 60.82(4) 9_556 . ? La2 Sb5 La3 125.83(4) 9 . ? La2 Sb5 La3 125.83(4) 9_556 . ? La1 Sb5 La3 81.79(4) . . ? Sb5 Sb6 Sb5 87.50(6) 10_556 10 ? Sb5 Sb6 La3 63.75(4) 10_556 10_556 ? Sb5 Sb6 La3 117.37(6) 10 10_556 ? Sb5 Sb6 La3 117.37(6) 10_556 10 ? Sb5 Sb6 La3 63.75(4) 10 10 ? La3 Sb6 La3 81.42(5) 10_556 10 ? Sb5 Sb6 La2 153.27(6) 10_556 10 ? Sb5 Sb6 La2 90.25(4) 10 10 ? La3 Sb6 La2 138.72(6) 10_556 10 ? La3 Sb6 La2 85.02(4) 10 10 ? Sb5 Sb6 La2 90.25(4) 10_556 10_556 ? Sb5 Sb6 La2 153.27(6) 10 10_556 ? La3 Sb6 La2 85.02(4) 10_556 10_556 ? La3 Sb6 La2 138.72(6) 10 10_556 ? La2 Sb6 La2 79.98(5) 10 10_556 ? Sb5 Sb6 La2 60.98(4) 10_556 . ? Sb5 Sb6 La2 60.98(4) 10 . ? La3 Sb6 La2 124.73(4) 10_556 . ? La3 Sb6 La2 124.73(4) 10 . ? La2 Sb6 La2 94.87(5) 10 . ? La2 Sb6 La2 94.87(5) 10_556 . ? La2 Br La2 90.92(8) 9_556 9 ? La2 Br La2 110.81(6) 9_556 . ? La2 Br La2 110.81(6) 9 . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag La1 Sb1 3.2561(12) 7_666 ? La1 Sb1 3.2561(12) 7_665 ? La1 Sb2 3.3159(16) 7_666 ? La1 Sb2 3.3159(16) 7_665 ? La1 Sb3 3.356(2) 4_665 ? La1 Sb3 3.360(2) . ? La1 Sb4 3.3842(16) 9 ? La1 Sb4 3.3842(16) 9_556 ? La1 Sb5 3.395(2) . ? La1 La1 4.218(2) 4_665 ? La1 La1 4.218(2) 3_655 ? La2 Br 3.032(2) 10 ? La2 Br 3.032(2) 10_556 ? La2 Br 3.111(3) . ? La2 Sb4 3.355(2) . ? La2 Sb6 3.3629(16) 9_556 ? La2 Sb6 3.3629(16) 9 ? La2 Sb5 3.3785(16) 10_556 ? La2 Sb5 3.3785(16) 10 ? La2 Sb6 3.502(2) . ? La3 Sb2 3.2822(16) 7_666 ? La3 Sb2 3.2822(16) 7_665 ? La3 Sb6 3.3136(16) 9 ? La3 Sb6 3.3136(16) 9_556 ? La3 Sb3 3.3407(16) 10_556 ? La3 Sb3 3.3407(16) 10 ? La3 Sb4 3.386(2) . ? La3 Sb5 3.404(2) . ? La3 Sb2 3.432(2) . ? Sb1 La1 3.2561(12) 10 ? Sb1 La1 3.2561(12) 10_556 ? Sb1 La1 3.2561(12) 9_566 ? Sb1 La1 3.2561(12) 9_565 ? Sb1 La1 3.2561(12) 7_666 ? Sb1 La1 3.2561(12) 7_665 ? Sb2 Sb3 3.0369(16) 10 ? Sb2 Sb3 3.0369(16) 10_556 ? Sb2 La3 3.2823(16) 7_666 ? Sb2 La3 3.2823(16) 7_665 ? Sb2 La1 3.3158(16) 7_666 ? Sb2 La1 3.3158(16) 7_665 ? Sb3 Sb2 3.0369(16) 9_556 ? Sb3 Sb2 3.0369(16) 9 ? Sb3 Sb4 3.1356(16) 9 ? Sb3 Sb4 3.1356(16) 9_556 ? Sb3 La3 3.3407(16) 9 ? Sb3 La3 3.3407(16) 9_556 ? Sb3 La1 3.356(2) 3_655 ? Sb4 Sb5 3.0791(16) 10 ? Sb4 Sb5 3.0791(16) 10_556 ? Sb4 Sb3 3.1356(17) 10_556 ? Sb4 Sb3 3.1356(16) 10 ? Sb4 La1 3.3842(16) 10_556 ? Sb4 La1 3.3842(16) 10 ? Sb5 Sb4 3.0791(16) 9_556 ? Sb5 Sb4 3.0791(16) 9 ? Sb5 Sb6 3.1253(17) 9 ? Sb5 Sb6 3.1253(17) 9_556 ? Sb5 La2 3.3785(16) 9 ? Sb5 La2 3.3785(16) 9_556 ? Sb6 Sb5 3.1254(17) 10_556 ? Sb6 Sb5 3.1254(17) 10 ? Sb6 La3 3.3135(16) 10_556 ? Sb6 La3 3.3135(16) 10 ? Sb6 La2 3.3628(16) 10 ? Sb6 La2 3.3628(16) 10_556 ? Br La2 3.032(2) 9_556 ? Br La2 3.032(2) 9 ?
1100718.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100718.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100718 loop_ _publ_author_name 'Chong Zheng' 'Hansj\"urgen Mattausch' 'Arndt Simon' _publ_section_title ; La9Sb16Br3 and Ce9Sb16Cl3: Stars and Stripes in Rare Earth Halide and Intermetallic Compounds ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3684 _journal_page_last 3689 _journal_paper_doi 10.1021/ic049220u _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'Ce9 Cl3 Sb16' _chemical_formula_weight 3315.43 _chemical_name_systematic ; ? ; _space_group_IT_number 176 _symmetry_cell_setting hexagonal _symmetry_space_group_name_Hall '-P 6c' _symmetry_space_group_name_H-M 'P 63/m' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_formula_units_Z 2 _cell_length_a 20.8622(16) _cell_length_b 20.8622(16) _cell_length_c 4.2728(7) _cell_measurement_reflns_used 327 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 14 _cell_measurement_theta_min -14 _cell_volume 1610.5(3) _computing_cell_refinement 'SMART and SAINT (Bruker, 1999)' _computing_data_collection 'SMART (Bruker, 1999)' _computing_data_reduction 'SAINT (Bruker, 1999)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _computing_structure_refinement 'SHELXTL (Sheldrick, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 0 _diffrn_measured_fraction_theta_full 0.906 _diffrn_measured_fraction_theta_max 0.906 _diffrn_measurement_device_type 'Siemens SMART CCD PLATFORM' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0432 _diffrn_reflns_av_sigmaI/netI 0.0199 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_number 9996 _diffrn_reflns_theta_full 24.98 _diffrn_reflns_theta_max 24.98 _diffrn_reflns_theta_min 1.95 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 25.812 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.788 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Sheldrick, 2000)' _exptl_crystal_colour metallic _exptl_crystal_density_diffrn 6.837 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 2778 _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _refine_diff_density_max 3.160 _refine_diff_density_min -3.015 _refine_diff_density_rms 0.512 _refine_ls_extinction_coef 0.000061(19) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.486 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 58 _refine_ls_number_reflns 979 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.486 _refine_ls_R_factor_all 0.0521 _refine_ls_R_factor_gt 0.0519 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+164.7807P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1043 _refine_ls_wR_factor_ref 0.1044 _reflns_number_gt 976 _reflns_number_total 979 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic049220usi20040615_061240.cif _cod_data_source_block Ce9Sb16Cl3 _cod_database_code 1100718 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, x-y, z' '-x+y, -x, z' 'x-y, x, z+1/2' 'y, -x+y, z+1/2' '-x, -y, -z' 'x, y, -z-1/2' 'y, -x+y, -z' 'x-y, x, -z' '-x+y, -x, -z-1/2' '-y, x-y, -z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ce1 Ce 0.54055(8) 0.30873(9) 0.2500 0.0091(4) Uani 1 2 d S . . Ce2 Ce 0.14413(9) 0.23798(9) 0.2500 0.0103(4) Uani 1 2 d S . . Ce3 Ce 0.39230(9) 0.40020(9) 0.2500 0.0106(4) Uani 1 2 d S . . Sb1 Sb 0.3333 0.6667 0.2500 0.0099(7) Uani 1 6 d S . . Sb2 Sb 0.48666(10) 0.58939(10) 0.2500 0.0105(4) Uani 1 2 d S . . Sb3 Sb 0.50829(10) 0.13678(10) 0.2500 0.0127(5) Uani 1 2 d S . . Sb4 Sb 0.24782(10) 0.42551(10) 0.2500 0.0108(4) Uani 1 2 d S . . Sb5 Sb 0.35343(10) 0.22453(10) 0.2500 0.0117(5) Uani 1 2 d S . . Sb6 Sb 0.00488(11) 0.28013(11) 0.2500 0.0127(5) Uani 1 2 d S . . Cl Cl 0.1475(4) 0.0985(4) 0.2500 0.0169(15) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ce1 0.0073(8) 0.0081(8) 0.0110(9) 0.000 0.000 0.0032(6) Ce2 0.0084(8) 0.0112(8) 0.0108(8) 0.000 0.000 0.0045(6) Ce3 0.0106(8) 0.0111(8) 0.0117(9) 0.000 0.000 0.0067(7) Sb1 0.0101(10) 0.0101(10) 0.0094(17) 0.000 0.000 0.0051(5) Sb2 0.0089(9) 0.0112(10) 0.0130(10) 0.000 0.000 0.0061(8) Sb3 0.0113(10) 0.0108(10) 0.0146(11) 0.000 0.000 0.0045(8) Sb4 0.0086(9) 0.0104(9) 0.0133(10) 0.000 0.000 0.0047(7) Sb5 0.0074(9) 0.0090(9) 0.0161(11) 0.000 0.000 0.0022(8) Sb6 0.0126(10) 0.0125(10) 0.0144(11) 0.000 0.000 0.0072(8) Cl 0.010(3) 0.014(3) 0.023(4) 0.000 0.000 0.004(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Sb1 Ce1 Sb1 82.97(4) 7_666 7_665 ? Sb1 Ce1 Sb2 81.73(3) 7_666 7_666 ? Sb1 Ce1 Sb2 136.48(6) 7_665 7_666 ? Sb1 Ce1 Sb2 136.48(6) 7_666 7_665 ? Sb1 Ce1 Sb2 81.73(3) 7_665 7_665 ? Sb2 Ce1 Sb2 81.97(6) 7_666 7_665 ? Sb1 Ce1 Sb3 83.10(4) 7_666 . ? Sb1 Ce1 Sb3 83.10(4) 7_665 . ? Sb2 Ce1 Sb3 134.54(4) 7_666 . ? Sb2 Ce1 Sb3 134.54(4) 7_665 . ? Sb1 Ce1 Sb3 83.03(4) 7_666 4_665 ? Sb1 Ce1 Sb3 83.03(4) 7_665 4_665 ? Sb2 Ce1 Sb3 54.82(4) 7_666 4_665 ? Sb2 Ce1 Sb3 54.82(4) 7_665 4_665 ? Sb3 Ce1 Sb3 161.44(7) . 4_665 ? Sb1 Ce1 Sb4 138.28(6) 7_666 9 ? Sb1 Ce1 Sb4 84.38(3) 7_665 9 ? Sb2 Ce1 Sb4 131.52(7) 7_666 9 ? Sb2 Ce1 Sb4 80.03(4) 7_665 9 ? Sb3 Ce1 Sb4 55.96(4) . 9 ? Sb3 Ce1 Sb4 134.37(4) 4_665 9 ? Sb1 Ce1 Sb4 84.38(3) 7_666 9_556 ? Sb1 Ce1 Sb4 138.28(6) 7_665 9_556 ? Sb2 Ce1 Sb4 80.03(4) 7_666 9_556 ? Sb2 Ce1 Sb4 131.52(7) 7_665 9_556 ? Sb3 Ce1 Sb4 55.96(4) . 9_556 ? Sb3 Ce1 Sb4 134.37(4) 4_665 9_556 ? Sb4 Ce1 Sb4 79.18(5) 9 9_556 ? Sb1 Ce1 Sb5 136.03(3) 7_666 . ? Sb1 Ce1 Sb5 136.03(3) 7_665 . ? Sb2 Ce1 Sb5 78.86(5) 7_666 . ? Sb2 Ce1 Sb5 78.86(5) 7_665 . ? Sb3 Ce1 Sb5 83.14(6) . . ? Sb3 Ce1 Sb5 115.42(6) 4_665 . ? Sb4 Ce1 Sb5 53.66(4) 9 . ? Sb4 Ce1 Sb5 53.66(4) 9_556 . ? Cl Ce2 Cl 95.6(2) 10 10_556 ? Cl Ce2 Cl 72.6(2) 10 . ? Cl Ce2 Cl 72.6(2) 10_556 . ? Cl Ce2 Sb6 149.08(16) 10 9_556 ? Cl Ce2 Sb6 84.50(13) 10_556 9_556 ? Cl Ce2 Sb6 77.97(11) . 9_556 ? Cl Ce2 Sb6 84.50(13) 10 9 ? Cl Ce2 Sb6 149.08(16) 10_556 9 ? Cl Ce2 Sb6 77.97(11) . 9 ? Sb6 Ce2 Sb6 80.14(6) 9_556 9 ? Cl Ce2 Sb5 131.40(15) 10 10_556 ? Cl Ce2 Sb5 73.55(13) 10_556 10_556 ? Cl Ce2 Sb5 140.14(3) . 10_556 ? Sb6 Ce2 Sb5 78.37(4) 9_556 10_556 ? Sb6 Ce2 Sb5 128.25(7) 9 10_556 ? Cl Ce2 Sb5 73.55(13) 10 10 ? Cl Ce2 Sb5 131.40(15) 10_556 10 ? Cl Ce2 Sb5 140.14(3) . 10 ? Sb6 Ce2 Sb5 128.25(7) 9_556 10 ? Sb6 Ce2 Sb5 78.37(4) 9 10 ? Sb5 Ce2 Sb5 79.21(5) 10_556 10 ? Cl Ce2 Sb4 126.00(12) 10 . ? Cl Ce2 Sb4 126.00(12) 10_556 . ? Cl Ce2 Sb4 145.32(15) . . ? Sb6 Ce2 Sb4 75.66(5) 9_556 . ? Sb6 Ce2 Sb4 75.66(5) 9 . ? Sb5 Ce2 Sb4 53.59(4) 10_556 . ? Sb5 Ce2 Sb4 53.59(4) 10 . ? Cl Ce2 Sb6 76.96(15) 10 . ? Cl Ce2 Sb6 76.96(15) 10_556 . ? Cl Ce2 Sb6 134.01(15) . . ? Sb6 Ce2 Sb6 132.41(4) 9_556 . ? Sb6 Ce2 Sb6 132.41(4) 9 . ? Sb5 Ce2 Sb6 54.48(4) 10_556 . ? Sb5 Ce2 Sb6 54.48(4) 10 . ? Sb4 Ce2 Sb6 80.67(6) . . ? Sb2 Ce3 Sb2 82.79(6) 7_666 7_665 ? Sb2 Ce3 Sb6 135.07(7) 7_666 9 ? Sb2 Ce3 Sb6 81.12(4) 7_665 9 ? Sb2 Ce3 Sb6 81.12(4) 7_666 9_556 ? Sb2 Ce3 Sb6 135.07(7) 7_665 9_556 ? Sb6 Ce3 Sb6 81.39(6) 9 9_556 ? Sb2 Ce3 Sb3 83.74(4) 7_666 10_556 ? Sb2 Ce3 Sb3 138.59(7) 7_665 10_556 ? Sb6 Ce3 Sb3 133.03(7) 9 10_556 ? Sb6 Ce3 Sb3 80.52(4) 9_556 10_556 ? Sb2 Ce3 Sb3 138.59(7) 7_666 10 ? Sb2 Ce3 Sb3 83.74(4) 7_665 10 ? Sb6 Ce3 Sb3 80.52(4) 9 10 ? Sb6 Ce3 Sb3 133.03(7) 9_556 10 ? Sb3 Ce3 Sb3 81.02(6) 10_556 10 ? Sb2 Ce3 Sb4 137.11(3) 7_666 . ? Sb2 Ce3 Sb4 137.11(3) 7_665 . ? Sb6 Ce3 Sb4 77.39(5) 9 . ? Sb6 Ce3 Sb4 77.39(5) 9_556 . ? Sb3 Ce3 Sb4 56.48(4) 10_556 . ? Sb3 Ce3 Sb4 56.48(4) 10 . ? Sb2 Ce3 Sb5 80.00(5) 7_666 . ? Sb2 Ce3 Sb5 80.00(5) 7_665 . ? Sb6 Ce3 Sb5 56.02(4) 9 . ? Sb6 Ce3 Sb5 56.02(4) 9_556 . ? Sb3 Ce3 Sb5 135.29(4) 10_556 . ? Sb3 Ce3 Sb5 135.29(4) 10 . ? Sb4 Ce3 Sb5 115.78(7) . . ? Sb2 Ce3 Sb2 86.73(5) 7_666 . ? Sb2 Ce3 Sb2 86.73(5) 7_665 . ? Sb6 Ce3 Sb2 133.51(4) 9 . ? Sb6 Ce3 Sb2 133.51(4) 9_556 . ? Sb3 Ce3 Sb2 53.52(4) 10_556 . ? Sb3 Ce3 Sb2 53.52(4) 10 . ? Sb4 Ce3 Sb2 81.97(6) . . ? Sb5 Ce3 Sb2 162.25(7) . . ? Ce1 Sb1 Ce1 82.98(4) 10 10_556 ? Ce1 Sb1 Ce1 136.007(13) 10 9_566 ? Ce1 Sb1 Ce1 80.89(3) 10_556 9_566 ? Ce1 Sb1 Ce1 80.89(3) 10 9_565 ? Ce1 Sb1 Ce1 136.007(14) 10_556 9_565 ? Ce1 Sb1 Ce1 82.98(4) 9_566 9_565 ? Ce1 Sb1 Ce1 136.006(13) 10 7_666 ? Ce1 Sb1 Ce1 80.89(3) 10_556 7_666 ? Ce1 Sb1 Ce1 80.89(3) 9_566 7_666 ? Ce1 Sb1 Ce1 136.009(14) 9_565 7_666 ? Ce1 Sb1 Ce1 80.89(3) 10 7_665 ? Ce1 Sb1 Ce1 136.006(13) 10_556 7_665 ? Ce1 Sb1 Ce1 136.009(14) 9_566 7_665 ? Ce1 Sb1 Ce1 80.89(3) 9_565 7_665 ? Ce1 Sb1 Ce1 82.97(4) 7_666 7_665 ? Sb3 Sb2 Sb3 89.97(7) 10 10_556 ? Sb3 Sb2 Ce3 151.74(8) 10 7_666 ? Sb3 Sb2 Ce3 86.90(4) 10_556 7_666 ? Sb3 Sb2 Ce3 86.90(4) 10 7_665 ? Sb3 Sb2 Ce3 151.74(8) 10_556 7_665 ? Ce3 Sb2 Ce3 82.79(6) 7_666 7_665 ? Sb3 Sb2 Ce1 118.68(7) 10 7_666 ? Sb3 Sb2 Ce1 63.42(5) 10_556 7_666 ? Ce3 Sb2 Ce1 84.70(4) 7_666 7_666 ? Ce3 Sb2 Ce1 140.81(7) 7_665 7_666 ? Sb3 Sb2 Ce1 63.42(5) 10 7_665 ? Sb3 Sb2 Ce1 118.68(7) 10_556 7_665 ? Ce3 Sb2 Ce1 140.81(7) 7_666 7_665 ? Ce3 Sb2 Ce1 84.70(4) 7_665 7_665 ? Ce1 Sb2 Ce1 81.98(6) 7_666 7_665 ? Sb3 Sb2 Ce3 61.05(5) 10 . ? Sb3 Sb2 Ce3 61.05(5) 10_556 . ? Ce3 Sb2 Ce3 93.28(5) 7_666 . ? Ce3 Sb2 Ce3 93.28(5) 7_665 . ? Ce1 Sb2 Ce3 124.46(5) 7_666 . ? Ce1 Sb2 Ce3 124.46(5) 7_665 . ? Sb2 Sb3 Sb2 89.97(7) 9_556 9 ? Sb2 Sb3 Sb4 177.59(7) 9_556 9 ? Sb2 Sb3 Sb4 91.82(4) 9 9 ? Sb2 Sb3 Sb4 91.82(4) 9_556 9_556 ? Sb2 Sb3 Sb4 177.59(7) 9 9_556 ? Sb4 Sb3 Sb4 86.35(7) 9 9_556 ? Sb2 Sb3 Ce3 120.17(7) 9_556 9 ? Sb2 Sb3 Ce3 65.43(5) 9 9 ? Sb4 Sb3 Ce3 62.10(5) 9 9 ? Sb4 Sb3 Ce3 114.91(7) 9_556 9 ? Sb2 Sb3 Ce3 65.43(5) 9_556 9_556 ? Sb2 Sb3 Ce3 120.17(7) 9 9_556 ? Sb4 Sb3 Ce3 114.91(7) 9 9_556 ? Sb4 Sb3 Ce3 62.10(5) 9_556 9_556 ? Ce3 Sb3 Ce3 81.02(6) 9 9_556 ? Sb2 Sb3 Ce1 114.92(6) 9_556 . ? Sb2 Sb3 Ce1 114.92(6) 9 . ? Sb4 Sb3 Ce1 62.83(5) 9 . ? Sb4 Sb3 Ce1 62.83(5) 9_556 . ? Ce3 Sb3 Ce1 124.90(5) 9 . ? Ce3 Sb3 Ce1 124.90(5) 9_556 . ? Sb2 Sb3 Ce1 61.76(5) 9_556 3_655 ? Sb2 Sb3 Ce1 61.76(5) 9 3_655 ? Sb4 Sb3 Ce1 117.82(6) 9 3_655 ? Sb4 Sb3 Ce1 117.82(6) 9_556 3_655 ? Ce3 Sb3 Ce1 127.17(5) 9 3_655 ? Ce3 Sb3 Ce1 127.17(5) 9_556 3_655 ? Ce1 Sb3 Ce1 78.55(7) . 3_655 ? Sb5 Sb4 Sb5 89.25(7) 10 10_556 ? Sb5 Sb4 Sb3 176.73(8) 10 10_556 ? Sb5 Sb4 Sb3 92.12(4) 10_556 10_556 ? Sb5 Sb4 Sb3 92.12(4) 10 10 ? Sb5 Sb4 Sb3 176.73(8) 10_556 10 ? Sb3 Sb4 Sb3 86.35(7) 10_556 10 ? Sb5 Sb4 Ce3 120.26(5) 10 . ? Sb5 Sb4 Ce3 120.26(5) 10_556 . ? Sb3 Sb4 Ce3 61.42(5) 10_556 . ? Sb3 Sb4 Ce3 61.42(5) 10 . ? Sb5 Sb4 Ce1 116.94(7) 10 10_556 ? Sb5 Sb4 Ce1 63.75(4) 10_556 10_556 ? Sb3 Sb4 Ce1 61.22(5) 10_556 10_556 ? Sb3 Sb4 Ce1 113.00(7) 10 10_556 ? Ce3 Sb4 Ce1 122.61(5) . 10_556 ? Sb5 Sb4 Ce1 63.75(4) 10 10 ? Sb5 Sb4 Ce1 116.94(7) 10_556 10 ? Sb3 Sb4 Ce1 113.00(7) 10_556 10 ? Sb3 Sb4 Ce1 61.22(5) 10 10 ? Ce3 Sb4 Ce1 122.61(5) . 10 ? Ce1 Sb4 Ce1 79.19(5) 10_556 10 ? Sb5 Sb4 Ce2 62.48(5) 10 . ? Sb5 Sb4 Ce2 62.48(5) 10_556 . ? Sb3 Sb4 Ce2 120.78(6) 10_556 . ? Sb3 Sb4 Ce2 120.78(5) 10 . ? Ce3 Sb4 Ce2 85.56(6) . . ? Ce1 Sb4 Ce2 126.22(5) 10_556 . ? Ce1 Sb4 Ce2 126.22(5) 10 . ? Sb4 Sb5 Sb4 89.25(7) 9_556 9 ? Sb4 Sb5 Sb6 178.65(7) 9_556 9 ? Sb4 Sb5 Sb6 91.89(4) 9 9 ? Sb4 Sb5 Sb6 91.89(4) 9_556 9_556 ? Sb4 Sb5 Sb6 178.65(7) 9 9_556 ? Sb6 Sb5 Sb6 86.95(7) 9 9_556 ? Sb4 Sb5 Ce3 117.75(6) 9_556 . ? Sb4 Sb5 Ce3 117.75(6) 9 . ? Sb6 Sb5 Ce3 61.05(5) 9 . ? Sb6 Sb5 Ce3 61.05(5) 9_556 . ? Sb4 Sb5 Ce2 117.14(7) 9_556 9 ? Sb4 Sb5 Ce2 63.93(5) 9 9 ? Sb6 Sb5 Ce2 64.06(5) 9 9 ? Sb6 Sb5 Ce2 116.09(7) 9_556 9 ? Ce3 Sb5 Ce2 125.10(5) . 9 ? Sb4 Sb5 Ce2 63.93(5) 9_556 9_556 ? Sb4 Sb5 Ce2 117.14(7) 9 9_556 ? Sb6 Sb5 Ce2 116.09(7) 9 9_556 ? Sb6 Sb5 Ce2 64.06(5) 9_556 9_556 ? Ce3 Sb5 Ce2 125.10(5) . 9_556 ? Ce2 Sb5 Ce2 79.21(5) 9 9_556 ? Sb4 Sb5 Ce1 62.60(5) 9_556 . ? Sb4 Sb5 Ce1 62.60(5) 9 . ? Sb6 Sb5 Ce1 117.36(6) 9 . ? Sb6 Sb5 Ce1 117.36(6) 9_556 . ? Ce3 Sb5 Ce1 81.14(6) . . ? Ce2 Sb5 Ce1 126.53(5) 9 . ? Ce2 Sb5 Ce1 126.53(5) 9_556 . ? Sb5 Sb6 Sb5 86.95(7) 10_556 10 ? Sb5 Sb6 Ce3 62.93(5) 10_556 10_556 ? Sb5 Sb6 Ce3 116.25(7) 10 10_556 ? Sb5 Sb6 Ce3 116.25(7) 10_556 10 ? Sb5 Sb6 Ce3 62.93(5) 10 10 ? Ce3 Sb6 Ce3 81.39(6) 10_556 10 ? Sb5 Sb6 Ce2 150.71(8) 10_556 10 ? Sb5 Sb6 Ce2 89.21(4) 10 10 ? Ce3 Sb6 Ce2 142.47(8) 10_556 10 ? Ce3 Sb6 Ce2 87.34(4) 10 10 ? Sb5 Sb6 Ce2 89.21(4) 10_556 10_556 ? Sb5 Sb6 Ce2 150.71(8) 10 10_556 ? Ce3 Sb6 Ce2 87.34(4) 10_556 10_556 ? Ce3 Sb6 Ce2 142.47(8) 10 10_556 ? Ce2 Sb6 Ce2 80.14(6) 10 10_556 ? Sb5 Sb6 Ce2 61.46(5) 10_556 . ? Sb5 Sb6 Ce2 61.46(5) 10 . ? Ce3 Sb6 Ce2 124.39(5) 10_556 . ? Ce3 Sb6 Ce2 124.39(5) 10 . ? Ce2 Sb6 Ce2 91.37(6) 10 . ? Ce2 Sb6 Ce2 91.37(6) 10_556 . ? Ce2 Cl Ce2 95.6(2) 9_556 9 ? Ce2 Cl Ce2 111.85(17) 9_556 . ? Ce2 Cl Ce2 111.85(17) 9 . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ce1 Sb1 3.2250(12) 7_666 ? Ce1 Sb1 3.2250(12) 7_665 ? Ce1 Sb2 3.2573(19) 7_666 ? Ce1 Sb2 3.2573(19) 7_665 ? Ce1 Sb3 3.303(2) . ? Ce1 Sb3 3.307(2) 4_665 ? Ce1 Sb4 3.3522(19) 9 ? Ce1 Sb4 3.3522(19) 9_556 ? Ce1 Sb5 3.386(2) . ? Ce2 Cl 2.884(5) 10 ? Ce2 Cl 2.884(5) 10_556 ? Ce2 Cl 2.947(8) . ? Ce2 Sb6 3.3186(19) 9_556 ? Ce2 Sb6 3.3186(19) 9 ? Ce2 Sb5 3.3512(18) 10_556 ? Ce2 Sb5 3.3512(18) 10 ? Ce2 Sb4 3.394(2) . ? Ce2 Sb6 3.430(3) . ? Ce3 Sb2 3.2310(18) 7_666 ? Ce3 Sb2 3.2310(18) 7_665 ? Ce3 Sb6 3.2764(19) 9 ? Ce3 Sb6 3.2764(19) 9_556 ? Ce3 Sb3 3.2888(19) 10_556 ? Ce3 Sb3 3.2888(19) 10 ? Ce3 Sb4 3.310(2) . ? Ce3 Sb5 3.334(2) . ? Ce3 Sb2 3.418(2) . ? Sb1 Ce1 3.2249(12) 10 ? Sb1 Ce1 3.2249(12) 10_556 ? Sb1 Ce1 3.2249(12) 9_566 ? Sb1 Ce1 3.2249(12) 9_565 ? Sb1 Ce1 3.2250(12) 7_666 ? Sb1 Ce1 3.2250(12) 7_665 ? Sb2 Sb3 3.0222(19) 10 ? Sb2 Sb3 3.0222(19) 10_556 ? Sb2 Ce3 3.2309(18) 7_666 ? Sb2 Ce3 3.2309(18) 7_665 ? Sb2 Ce1 3.2572(19) 7_666 ? Sb2 Ce1 3.2572(19) 7_665 ? Sb3 Sb2 3.0221(19) 9_556 ? Sb3 Sb2 3.0221(19) 9 ? Sb3 Sb4 3.122(2) 9 ? Sb3 Sb4 3.122(2) 9_556 ? Sb3 Ce3 3.2888(19) 9 ? Sb3 Ce3 3.2888(19) 9_556 ? Sb3 Ce1 3.307(2) 3_655 ? Sb4 Sb5 3.0413(19) 10 ? Sb4 Sb5 3.0413(19) 10_556 ? Sb4 Sb3 3.122(2) 10_556 ? Sb4 Sb3 3.122(2) 10 ? Sb4 Ce1 3.3521(19) 10_556 ? Sb4 Ce1 3.3521(19) 10 ? Sb5 Sb4 3.0413(19) 9_556 ? Sb5 Sb4 3.0413(19) 9 ? Sb5 Sb6 3.105(2) 9 ? Sb5 Sb6 3.105(2) 9_556 ? Sb5 Ce2 3.3512(18) 9 ? Sb5 Ce2 3.3512(18) 9_556 ? Sb6 Sb5 3.105(2) 10_556 ? Sb6 Sb5 3.105(2) 10 ? Sb6 Ce3 3.2764(19) 10_556 ? Sb6 Ce3 3.2764(19) 10 ? Sb6 Ce2 3.3187(19) 10 ? Sb6 Ce2 3.3187(19) 10_556 ? Cl Ce2 2.884(5) 9_556 ? Cl Ce2 2.884(5) 9 ?
1100719.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100719.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100719 loop_ _publ_author_name 'Aaron M. Appel' 'Rachel Newell' 'Daniel L. DuBois' 'M. Rakowski DuBois' _publ_contact_author_address '215 UCB, Boulder, CO, 80309-0215, USA' _publ_contact_author_name 'Mary Rakowski-DuBois' _publ_section_title ; Concentration of Carbon Dioxide by Electrochemically Modulated Complexation with a Binuclear Copper Complex ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3046 _journal_page_last 3056 _journal_paper_doi 10.1021/ic050023k _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C67 H84 B2 Cu2 N8 O7' _chemical_formula_weight 1262.12 _chemical_name_common AMA232 _chemical_name_systematic ; ? ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 73.2260(10) _cell_angle_beta 86.0700(10) _cell_angle_gamma 64.3680(10) _cell_formula_units_Z 2 _cell_length_a 13.3916(5) _cell_length_b 13.4574(5) _cell_length_c 20.1343(7) _cell_measurement_reflns_used 4614 _cell_measurement_temperature 141(2) _cell_measurement_theta_max 25.046 _cell_measurement_theta_min 2.308 _cell_volume 3125.6(2) _computing_cell_refinement 'Bruker XSCANS' _computing_data_collection 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 141(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0813 _diffrn_reflns_av_sigmaI/netI 0.1460 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 20450 _diffrn_reflns_theta_full 25.03 _diffrn_reflns_theta_max 25.03 _diffrn_reflns_theta_min 2.05 _exptl_absorpt_coefficient_mu 0.741 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_correction_T_min 0.339227 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; absorption correction applied using SADABS (Blessing, R. H. Acta Crystallogr., Sect. A 1995, 51, 33-38) ; _exptl_crystal_colour Blue _exptl_crystal_density_diffrn 1.341 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Pie _exptl_crystal_F_000 1332 _exptl_crystal_size_max .5 _exptl_crystal_size_mid .4 _exptl_crystal_size_min .3 _refine_diff_density_max 0.675 _refine_diff_density_min -0.682 _refine_diff_density_rms 0.087 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.985 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 775 _refine_ls_number_reflns 10981 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.985 _refine_ls_R_factor_all 0.1163 _refine_ls_R_factor_gt 0.0663 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0587P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1515 _refine_ls_wR_factor_ref 0.1763 _reflns_number_gt 6774 _reflns_number_total 10981 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic050023ksi20050107_041449.cif _cod_data_source_block ama232fm _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_database_code 1100719 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.66391(4) 0.63808(5) 0.21518(3) 0.02867(18) Uani 1 1 d . . . Cu2 Cu 0.98588(5) 0.32718(5) 0.21692(3) 0.03011(18) Uani 1 1 d . . . O1 O 0.8154(2) 0.5307(3) 0.18644(16) 0.0316(8) Uani 1 1 d . . . O2 O 0.9324(2) 0.4286(3) 0.12185(16) 0.0308(8) Uani 1 1 d . . . O3 O 0.8153(3) 0.6128(3) 0.07205(17) 0.0357(8) Uani 1 1 d . . . O4 O 0.9453(4) 0.6490(4) 0.2457(2) 0.0719(13) Uani 1 1 d . . . O5 O 0.9426(3) 0.6712(3) -0.02623(18) 0.0417(9) Uani 1 1 d . . . O6 O 0.8333(3) 0.7831(4) 0.1169(2) 0.0560(11) Uani 1 1 d . . . O7 O 0.9443(4) 0.8551(4) 0.0039(2) 0.0674(13) Uani 1 1 d . . . N1 N 0.5690(3) 0.5493(4) 0.2137(2) 0.0328(10) Uani 1 1 d . . . N2 N 0.6620(3) 0.5816(4) 0.3231(2) 0.0385(11) Uani 1 1 d . . . N3 N 1.0128(3) 0.2480(4) 0.3217(2) 0.0402(11) Uani 1 1 d . . . N4 N 0.9184(3) 0.2169(4) 0.2141(2) 0.0346(10) Uani 1 1 d . . . N5 N 0.5992(3) 0.7280(4) 0.11747(19) 0.0335(10) Uani 1 1 d . . . H1N5 H 0.5609 0.8048 0.1146 0.047 Uiso 1 1 calc R . . H2N5 H 0.6555 0.7199 0.0876 0.047 Uiso 1 1 calc R . . N6 N 0.6886(4) 0.7658(4) 0.2348(2) 0.0482(12) Uani 1 1 d . . . H1N6 H 0.7632 0.7467 0.2382 0.068 Uiso 1 1 calc R . . H2N6 H 0.6547 0.8334 0.1998 0.068 Uiso 1 1 calc R . . N7 N 1.0690(3) 0.4121(4) 0.2335(2) 0.0403(11) Uani 1 1 d . . . H1N7 H 1.1264 0.4038 0.2044 0.056 Uiso 1 1 calc R . . H2N7 H 1.0223 0.4892 0.2242 0.056 Uiso 1 1 calc R . . N8 N 1.1375(3) 0.1928(4) 0.1770(2) 0.0440(12) Uani 1 1 d . . . H1N8 H 1.1537 0.2268 0.1337 0.062 Uiso 1 1 calc R . . H2N8 H 1.1992 0.1612 0.2071 0.062 Uiso 1 1 calc R . . C1 C 0.5275(4) 0.5253(5) 0.2847(3) 0.0451(14) Uani 1 1 d . . . H1A H 0.5666 0.4420 0.3090 0.063 Uiso 1 1 calc R . . H1B H 0.4472 0.5459 0.2805 0.063 Uiso 1 1 calc R . . C2 C 0.5459(4) 0.5931(5) 0.3268(3) 0.0434(14) Uani 1 1 d . . . H2A H 0.4933 0.6753 0.3090 0.061 Uiso 1 1 calc R . . H2B H 0.5313 0.5649 0.3759 0.061 Uiso 1 1 calc R . . C3 C 0.7393(4) 0.4617(5) 0.3654(3) 0.0489(15) Uani 1 1 d . . . H3A H 0.7158 0.4061 0.3565 0.068 Uiso 1 1 calc R . . H3B H 0.7325 0.4569 0.4153 0.068 Uiso 1 1 calc R . . C4 C 0.8602(4) 0.4274(5) 0.3493(3) 0.0418(14) Uani 1 1 d . . . H4A H 0.8934 0.4595 0.3750 0.059 Uiso 1 1 calc R . . H4B H 0.8650 0.4595 0.2990 0.059 Uiso 1 1 calc R . . C5 C 0.9248(4) 0.2969(5) 0.3699(3) 0.0485(15) Uani 1 1 d . . . H5A H 0.9611 0.2711 0.4169 0.068 Uiso 1 1 calc R . . H5B H 0.8712 0.2634 0.3731 0.068 Uiso 1 1 calc R . . C6 C 1.0280(5) 0.1292(5) 0.3281(3) 0.0528(16) Uani 1 1 d . . . H6A H 1.0246 0.0896 0.3774 0.074 Uiso 1 1 calc R . . H6B H 1.1019 0.0853 0.3129 0.074 Uiso 1 1 calc R . . C7 C 0.9389(5) 0.1323(5) 0.2843(3) 0.0497(15) Uani 1 1 d . . . H7A H 0.9614 0.0547 0.2790 0.070 Uiso 1 1 calc R . . H7B H 0.8691 0.1526 0.3085 0.070 Uiso 1 1 calc R . . C8 C 0.7984(4) 0.2765(5) 0.1887(3) 0.0408(13) Uani 1 1 d . . . H8A H 0.7730 0.2177 0.1881 0.057 Uiso 1 1 calc R . . H8B H 0.7914 0.3252 0.1402 0.057 Uiso 1 1 calc R . . C9 C 0.7232(4) 0.3507(5) 0.2318(3) 0.0368(13) Uani 1 1 d . . . H9A H 0.7015 0.3026 0.2717 0.051 Uiso 1 1 calc R . . H9B H 0.7635 0.3847 0.2503 0.051 Uiso 1 1 calc R . . C10 C 0.6213(4) 0.4448(5) 0.1892(3) 0.0398(13) Uani 1 1 d . . . H10A H 0.6408 0.4674 0.1406 0.056 Uiso 1 1 calc R . . H10B H 0.5660 0.4143 0.1891 0.056 Uiso 1 1 calc R . . C11 C 0.4773(4) 0.6365(5) 0.1620(3) 0.0376(13) Uani 1 1 d . . . H11A H 0.4278 0.6986 0.1821 0.053 Uiso 1 1 calc R . . H11B H 0.4330 0.6004 0.1501 0.053 Uiso 1 1 calc R . . C12 C 0.5235(4) 0.6872(5) 0.0964(3) 0.0382(13) Uani 1 1 d . . . H12A H 0.5642 0.6279 0.0723 0.053 Uiso 1 1 calc R . . H12B H 0.4623 0.7520 0.0643 0.053 Uiso 1 1 calc R . . C13 C 0.6747(5) 0.6660(6) 0.3521(3) 0.0534(16) Uani 1 1 d . . . H13A H 0.6316 0.6720 0.3938 0.075 Uiso 1 1 calc R . . H13B H 0.7538 0.6373 0.3666 0.075 Uiso 1 1 calc R . . C14 C 0.6378(6) 0.7784(6) 0.3029(3) 0.0657(19) Uani 1 1 d . . . H14A H 0.6608 0.8273 0.3206 0.092 Uiso 1 1 calc R . . H14B H 0.5558 0.8155 0.2961 0.092 Uiso 1 1 calc R . . C15 C 1.1197(4) 0.2460(6) 0.3385(3) 0.0505(16) Uani 1 1 d . . . H15A H 1.1809 0.1903 0.3191 0.071 Uiso 1 1 calc R . . H15B H 1.1344 0.2215 0.3896 0.071 Uiso 1 1 calc R . . C16 C 1.1144(4) 0.3641(6) 0.3082(3) 0.0506(16) Uani 1 1 d . . . H16A H 1.1896 0.3602 0.3108 0.071 Uiso 1 1 calc R . . H16B H 1.0661 0.4155 0.3354 0.071 Uiso 1 1 calc R . . C17 C 0.9786(4) 0.1583(5) 0.1609(3) 0.0415(13) Uani 1 1 d . . . H17A H 0.9577 0.2152 0.1143 0.058 Uiso 1 1 calc R . . H17B H 0.9551 0.0979 0.1609 0.058 Uiso 1 1 calc R . . C18 C 1.1028(4) 0.1044(5) 0.1739(3) 0.0457(14) Uani 1 1 d . . . H18A H 1.1254 0.0420 0.2184 0.064 Uiso 1 1 calc R . . H18B H 1.1391 0.0707 0.1361 0.064 Uiso 1 1 calc R . . C19 C 0.8520(4) 0.5265(5) 0.1259(2) 0.0311(12) Uani 1 1 d . . . B1 B 0.8361(4) 0.2728(5) 0.6214(3) 0.0270(12) Uani 1 1 d . A 1 B2 B 1.5229(4) -0.1913(5) 0.8463(3) 0.0270(12) Uani 1 1 d . B 1 C20 C 0.9471(4) 0.2664(4) 0.5787(2) 0.0284(11) Uani 1 1 d . A 1 C21 C 1.0212(4) 0.1676(5) 0.5618(2) 0.0324(12) Uani 1 1 d . A 1 H21 H 1.0017 0.1053 0.5699 0.039 Uiso 1 1 calc R A 1 C22 C 1.1223(4) 0.1552(5) 0.5339(3) 0.0366(13) Uani 1 1 d . A 1 H22 H 1.1696 0.0858 0.5234 0.044 Uiso 1 1 calc R A 1 C23 C 1.1541(4) 0.2439(5) 0.5213(3) 0.0416(14) Uani 1 1 d . A 1 H23 H 1.2232 0.2361 0.5025 0.050 Uiso 1 1 calc R A 1 C24 C 1.0826(4) 0.3441(5) 0.5367(3) 0.0429(14) Uani 1 1 d . A 1 H24 H 1.1025 0.4063 0.5282 0.051 Uiso 1 1 calc R A 1 C25 C 0.9808(4) 0.3544(5) 0.5648(3) 0.0378(13) Uani 1 1 d . A 1 H25 H 0.9331 0.4242 0.5748 0.045 Uiso 1 1 calc R A 1 C26 C 0.7409(3) 0.4079(4) 0.6041(2) 0.0255(11) Uani 1 1 d . A 1 C27 C 0.7391(4) 0.4833(4) 0.6402(2) 0.0302(11) Uani 1 1 d . A 1 H27 H 0.7947 0.4555 0.6764 0.036 Uiso 1 1 calc R A 1 C28 C 0.6601(4) 0.5964(4) 0.6256(3) 0.0349(12) Uani 1 1 d . A 1 H28 H 0.6624 0.6437 0.6520 0.042 Uiso 1 1 calc R A 1 C29 C 0.5778(4) 0.6415(4) 0.5731(3) 0.0332(12) Uani 1 1 d . A 1 H29 H 0.5240 0.7194 0.5626 0.040 Uiso 1 1 calc R A 1 C30 C 0.5760(4) 0.5704(4) 0.5363(2) 0.0328(12) Uani 1 1 d . A 1 H30 H 0.5199 0.5989 0.5003 0.039 Uiso 1 1 calc R A 1 C31 C 0.6564(4) 0.4565(4) 0.5517(2) 0.0292(11) Uani 1 1 d . A 1 H31 H 0.6534 0.4098 0.5252 0.035 Uiso 1 1 calc R A 1 C32 C 0.8761(4) 0.2219(4) 0.7049(2) 0.0285(11) Uani 1 1 d . A 1 C33 C 0.7997(4) 0.2377(4) 0.7572(2) 0.0301(11) Uani 1 1 d . A 1 H33 H 0.7228 0.2781 0.7432 0.036 Uiso 1 1 calc R A 1 C34 C 0.8299(4) 0.1981(4) 0.8273(2) 0.0325(12) Uani 1 1 d . A 1 H34 H 0.7747 0.2128 0.8600 0.039 Uiso 1 1 calc R A 1 C35 C 0.9418(4) 0.1362(5) 0.8502(3) 0.0359(12) Uani 1 1 d . A 1 H35 H 0.9636 0.1071 0.8984 0.043 Uiso 1 1 calc R A 1 C36 C 1.0198(4) 0.1181(4) 0.8016(3) 0.0351(12) Uani 1 1 d . A 1 H36 H 1.0964 0.0770 0.8163 0.042 Uiso 1 1 calc R A 1 C37 C 0.9876(4) 0.1593(4) 0.7314(3) 0.0325(12) Uani 1 1 d . A 1 H37 H 1.0438 0.1446 0.6993 0.039 Uiso 1 1 calc R A 1 C38 C 0.7812(3) 0.1978(4) 0.5992(2) 0.0256(10) Uani 1 1 d . A 1 C39 C 0.7252(4) 0.1423(4) 0.6439(2) 0.0267(11) Uani 1 1 d . A 1 H39 H 0.7253 0.1400 0.6915 0.032 Uiso 1 1 calc R A 1 C40 C 0.6687(4) 0.0898(4) 0.6218(2) 0.0307(11) Uani 1 1 d . A 1 H40 H 0.6321 0.0523 0.6543 0.037 Uiso 1 1 calc R A 1 C41 C 0.6662(4) 0.0927(5) 0.5529(3) 0.0363(12) Uani 1 1 d . A 1 H41 H 0.6270 0.0582 0.5376 0.044 Uiso 1 1 calc R A 1 C42 C 0.7210(4) 0.1460(5) 0.5064(3) 0.0359(12) Uani 1 1 d . A 1 H42 H 0.7199 0.1486 0.4588 0.043 Uiso 1 1 calc R A 1 C43 C 0.7780(4) 0.1960(4) 0.5300(2) 0.0333(12) Uani 1 1 d . A 1 H43 H 0.8168 0.2308 0.4976 0.040 Uiso 1 1 calc R A 1 C44 C 1.6306(4) -0.3171(4) 0.8572(2) 0.0268(11) Uani 1 1 d . B 1 C45 C 1.6421(4) -0.3901(5) 0.8161(2) 0.0321(12) Uani 1 1 d . B 1 H45 H 1.5893 -0.3621 0.7782 0.039 Uiso 1 1 calc R B 1 C46 C 1.7264(4) -0.5004(5) 0.8284(3) 0.0360(12) Uani 1 1 d . B 1 H46 H 1.7307 -0.5460 0.7990 0.043 Uiso 1 1 calc R B 1 C47 C 1.8054(4) -0.5449(5) 0.8841(3) 0.0396(13) Uani 1 1 d . B 1 H47 H 1.8634 -0.6207 0.8933 0.048 Uiso 1 1 calc R B 1 C48 C 1.7967(4) -0.4757(5) 0.9254(3) 0.0392(13) Uani 1 1 d . B 1 H48 H 1.8494 -0.5042 0.9635 0.047 Uiso 1 1 calc R B 1 C49 C 1.7126(4) -0.3660(5) 0.9119(3) 0.0341(12) Uani 1 1 d . B 1 H49 H 1.7099 -0.3208 0.9412 0.041 Uiso 1 1 calc R B 1 C50 C 1.4278(4) -0.2093(4) 0.8983(2) 0.0287(11) Uani 1 1 d . B 1 C51 C 1.4299(4) -0.3170(4) 0.9323(2) 0.0319(12) Uani 1 1 d . B 1 H51 H 1.4904 -0.3840 0.9264 0.038 Uiso 1 1 calc R B 1 C52 C 1.3468(4) -0.3300(5) 0.9747(3) 0.0387(13) Uani 1 1 d . B 1 H52 H 1.3512 -0.4046 0.9964 0.046 Uiso 1 1 calc R B 1 C53 C 1.2582(4) -0.2343(5) 0.9849(3) 0.0406(14) Uani 1 1 d . B 1 H53 H 1.2012 -0.2431 1.0133 0.049 Uiso 1 1 calc R B 1 C54 C 1.2525(4) -0.1261(5) 0.9540(3) 0.0392(13) Uani 1 1 d . B 1 H54 H 1.1920 -0.0599 0.9610 0.047 Uiso 1 1 calc R B 1 C55 C 1.3377(4) -0.1154(5) 0.9119(2) 0.0342(12) Uani 1 1 d . B 1 H55 H 1.3340 -0.0407 0.8917 0.041 Uiso 1 1 calc R B 1 C56 C 1.4736(4) -0.1392(4) 0.7645(2) 0.0283(11) Uani 1 1 d . B 1 C57 C 1.5449(4) -0.1407(4) 0.7101(2) 0.0308(11) Uani 1 1 d . B 1 H57 H 1.6225 -0.1756 0.7216 0.037 Uiso 1 1 calc R B 1 C58 C 1.5084(4) -0.0941(4) 0.6404(2) 0.0354(12) Uani 1 1 d . B 1 H58 H 1.5604 -0.0986 0.6055 0.042 Uiso 1 1 calc R B 1 C59 C 1.3953(4) -0.0406(5) 0.6217(3) 0.0409(13) Uani 1 1 d . B 1 H59 H 1.3689 -0.0079 0.5742 0.049 Uiso 1 1 calc R B 1 C60 C 1.3218(4) -0.0360(5) 0.6739(3) 0.0425(14) Uani 1 1 d . B 1 H60 H 1.2442 0.0008 0.6621 0.051 Uiso 1 1 calc R B 1 C61 C 1.3603(4) -0.0844(5) 0.7428(3) 0.0372(13) Uani 1 1 d . B 1 H61 H 1.3077 -0.0806 0.7773 0.045 Uiso 1 1 calc R B 1 C62 C 1.5614(3) -0.1019(4) 0.8662(2) 0.0264(11) Uani 1 1 d . B 1 C63 C 1.5805(4) -0.1099(5) 0.9353(3) 0.0348(12) Uani 1 1 d . B 1 H63 H 1.5633 -0.1630 0.9710 0.042 Uiso 1 1 calc R B 1 C64 C 1.6235(4) -0.0442(5) 0.9544(3) 0.0348(12) Uani 1 1 d . B 1 H64 H 1.6360 -0.0540 1.0022 0.042 Uiso 1 1 calc R B 1 C65 C 1.6479(4) 0.0345(5) 0.9048(3) 0.0351(12) Uani 1 1 d . B 1 H65 H 1.6803 0.0773 0.9175 0.042 Uiso 1 1 calc R B 1 C66 C 1.6243(4) 0.0503(5) 0.8353(3) 0.0378(13) Uani 1 1 d . B 1 H66 H 1.6371 0.1072 0.8002 0.045 Uiso 1 1 calc R B 1 C67 C 1.5822(4) -0.0162(4) 0.8171(3) 0.0318(11) Uani 1 1 d . B 1 H67 H 1.5667 -0.0034 0.7692 0.038 Uiso 1 1 calc R B 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0250(3) 0.0320(4) 0.0280(3) -0.0099(3) 0.0033(2) -0.0108(3) Cu2 0.0256(3) 0.0307(4) 0.0328(4) -0.0060(3) -0.0003(2) -0.0126(3) O1 0.0231(17) 0.036(2) 0.0266(19) -0.0057(15) 0.0014(13) -0.0061(17) O2 0.0276(18) 0.027(2) 0.0297(19) -0.0098(15) 0.0012(14) -0.0035(17) O3 0.0298(19) 0.031(2) 0.032(2) -0.0042(16) 0.0022(15) -0.0034(18) O4 0.078(3) 0.060(3) 0.090(4) -0.021(3) -0.011(3) -0.039(3) O5 0.039(2) 0.038(2) 0.045(2) -0.0147(18) 0.0026(16) -0.0119(19) O6 0.068(3) 0.056(3) 0.056(3) -0.021(2) 0.008(2) -0.035(2) O7 0.090(3) 0.077(3) 0.056(3) -0.031(2) 0.012(2) -0.048(3) N1 0.022(2) 0.033(3) 0.040(3) -0.012(2) 0.0029(17) -0.008(2) N2 0.036(3) 0.041(3) 0.035(3) -0.012(2) 0.0047(19) -0.013(2) N3 0.030(2) 0.046(3) 0.034(3) -0.002(2) 0.0006(18) -0.012(2) N4 0.028(2) 0.030(3) 0.047(3) -0.010(2) 0.0088(19) -0.015(2) N5 0.027(2) 0.039(3) 0.030(2) -0.010(2) 0.0033(17) -0.011(2) N6 0.049(3) 0.049(3) 0.051(3) -0.017(2) 0.004(2) -0.025(3) N7 0.031(2) 0.050(3) 0.046(3) -0.014(2) 0.0035(19) -0.024(2) N8 0.032(2) 0.044(3) 0.048(3) -0.010(2) 0.005(2) -0.012(2) C1 0.024(3) 0.052(4) 0.055(4) -0.013(3) 0.009(2) -0.016(3) C2 0.035(3) 0.049(4) 0.041(3) -0.015(3) 0.016(2) -0.015(3) C3 0.036(3) 0.063(4) 0.031(3) -0.009(3) 0.004(2) -0.008(3) C4 0.044(3) 0.053(4) 0.025(3) -0.011(3) 0.001(2) -0.019(3) C5 0.033(3) 0.058(4) 0.036(3) -0.001(3) 0.000(2) -0.010(3) C6 0.038(3) 0.036(4) 0.058(4) 0.007(3) -0.003(3) -0.004(3) C7 0.044(3) 0.037(4) 0.057(4) -0.002(3) 0.006(3) -0.015(3) C8 0.026(3) 0.032(3) 0.068(4) -0.024(3) 0.003(2) -0.011(3) C9 0.029(3) 0.032(3) 0.053(3) -0.013(3) 0.007(2) -0.016(3) C10 0.027(3) 0.035(3) 0.060(4) -0.021(3) -0.001(2) -0.010(3) C11 0.018(3) 0.041(3) 0.051(3) -0.020(3) -0.002(2) -0.005(3) C12 0.028(3) 0.043(4) 0.038(3) -0.015(3) -0.002(2) -0.007(3) C13 0.065(4) 0.061(5) 0.049(4) -0.030(3) 0.007(3) -0.032(4) C14 0.092(5) 0.056(5) 0.054(4) -0.028(4) 0.004(4) -0.029(4) C15 0.040(3) 0.066(5) 0.040(3) -0.010(3) -0.008(2) -0.020(3) C16 0.029(3) 0.075(5) 0.054(4) -0.025(3) -0.008(2) -0.022(3) C17 0.037(3) 0.032(3) 0.059(4) -0.020(3) 0.009(3) -0.014(3) C18 0.043(3) 0.033(3) 0.060(4) -0.019(3) 0.006(3) -0.012(3) C19 0.031(3) 0.034(3) 0.027(3) -0.005(2) -0.001(2) -0.015(3) B1 0.024(3) 0.029(3) 0.025(3) -0.008(2) 0.002(2) -0.008(3) B2 0.029(3) 0.033(3) 0.023(3) -0.007(2) -0.001(2) -0.017(3) C20 0.022(2) 0.026(3) 0.028(3) -0.006(2) -0.0041(19) -0.002(2) C21 0.030(3) 0.031(3) 0.030(3) -0.005(2) -0.002(2) -0.009(3) C22 0.028(3) 0.035(3) 0.033(3) -0.006(2) 0.001(2) -0.004(3) C23 0.026(3) 0.053(4) 0.035(3) -0.005(3) 0.001(2) -0.013(3) C24 0.034(3) 0.045(4) 0.049(4) -0.003(3) 0.000(2) -0.022(3) C25 0.033(3) 0.040(3) 0.039(3) -0.014(3) 0.006(2) -0.013(3) C26 0.021(2) 0.029(3) 0.025(3) -0.007(2) 0.0032(18) -0.010(2) C27 0.020(2) 0.032(3) 0.034(3) -0.010(2) -0.0069(19) -0.007(2) C28 0.034(3) 0.030(3) 0.040(3) -0.009(2) -0.006(2) -0.012(3) C29 0.024(3) 0.025(3) 0.043(3) -0.007(2) -0.003(2) -0.006(2) C30 0.030(3) 0.035(3) 0.029(3) -0.004(2) -0.004(2) -0.013(3) C31 0.030(3) 0.030(3) 0.025(3) -0.009(2) 0.000(2) -0.009(3) C32 0.029(3) 0.022(3) 0.036(3) -0.010(2) 0.000(2) -0.011(2) C33 0.024(3) 0.030(3) 0.034(3) -0.011(2) 0.003(2) -0.007(2) C34 0.041(3) 0.032(3) 0.030(3) -0.016(2) 0.008(2) -0.017(3) C35 0.044(3) 0.039(3) 0.026(3) -0.006(2) -0.006(2) -0.020(3) C36 0.035(3) 0.026(3) 0.040(3) -0.009(2) -0.009(2) -0.009(3) C37 0.029(3) 0.031(3) 0.039(3) -0.016(2) 0.003(2) -0.012(3) C38 0.018(2) 0.022(3) 0.028(3) -0.008(2) 0.0004(18) -0.001(2) C39 0.028(3) 0.022(3) 0.025(3) -0.010(2) 0.0019(19) -0.005(2) C40 0.029(3) 0.023(3) 0.037(3) -0.010(2) 0.006(2) -0.009(2) C41 0.039(3) 0.034(3) 0.040(3) -0.016(2) 0.000(2) -0.016(3) C42 0.044(3) 0.037(3) 0.029(3) -0.013(2) 0.001(2) -0.017(3) C43 0.036(3) 0.031(3) 0.030(3) -0.008(2) 0.003(2) -0.014(3) C44 0.024(2) 0.026(3) 0.029(3) -0.003(2) -0.0002(19) -0.012(2) C45 0.033(3) 0.038(3) 0.029(3) -0.013(2) 0.003(2) -0.017(3) C46 0.035(3) 0.035(3) 0.043(3) -0.014(3) 0.007(2) -0.018(3) C47 0.032(3) 0.029(3) 0.053(4) -0.004(3) 0.008(2) -0.013(3) C48 0.034(3) 0.039(4) 0.040(3) -0.004(3) -0.006(2) -0.014(3) C49 0.033(3) 0.035(3) 0.034(3) -0.008(2) 0.000(2) -0.014(3) C50 0.027(3) 0.031(3) 0.027(3) -0.006(2) -0.0074(19) -0.012(3) C51 0.031(3) 0.033(3) 0.033(3) -0.006(2) -0.004(2) -0.016(3) C52 0.043(3) 0.043(4) 0.035(3) -0.005(3) 0.001(2) -0.027(3) C53 0.037(3) 0.054(4) 0.034(3) -0.012(3) 0.000(2) -0.023(3) C54 0.033(3) 0.044(4) 0.039(3) -0.016(3) 0.004(2) -0.012(3) C55 0.038(3) 0.036(3) 0.032(3) -0.008(2) -0.002(2) -0.020(3) C56 0.031(3) 0.026(3) 0.028(3) -0.008(2) -0.002(2) -0.011(2) C57 0.028(3) 0.034(3) 0.031(3) -0.010(2) 0.000(2) -0.013(3) C58 0.047(3) 0.035(3) 0.028(3) -0.014(2) 0.009(2) -0.019(3) C59 0.056(4) 0.046(4) 0.024(3) -0.009(2) -0.008(2) -0.025(3) C60 0.039(3) 0.048(4) 0.036(3) -0.008(3) -0.011(2) -0.016(3) C61 0.037(3) 0.044(4) 0.032(3) -0.008(2) 0.001(2) -0.021(3) C62 0.018(2) 0.028(3) 0.024(3) -0.004(2) -0.0016(18) -0.004(2) C63 0.039(3) 0.034(3) 0.030(3) -0.008(2) 0.004(2) -0.016(3) C64 0.039(3) 0.039(3) 0.030(3) -0.013(2) 0.000(2) -0.019(3) C65 0.028(3) 0.034(3) 0.047(3) -0.021(3) 0.003(2) -0.011(3) C66 0.037(3) 0.026(3) 0.047(3) -0.010(2) 0.008(2) -0.011(3) C67 0.030(3) 0.026(3) 0.030(3) -0.007(2) -0.001(2) -0.005(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Cu1 N6 95.08(18) . . ? N5 Cu1 O1 95.29(14) . . ? N6 Cu1 O1 105.82(16) . . ? N5 Cu1 N2 156.16(16) . . ? N6 Cu1 N2 83.82(18) . . ? O1 Cu1 N2 107.96(15) . . ? N5 Cu1 N1 85.41(16) . . ? N6 Cu1 N1 153.00(17) . . ? O1 Cu1 N1 100.99(14) . . ? N2 Cu1 N1 85.06(16) . . ? O2 Cu2 N7 93.42(16) . . ? O2 Cu2 N3 167.85(15) . . ? N7 Cu2 N3 85.60(18) . . ? O2 Cu2 N4 96.04(15) . . ? N7 Cu2 N4 169.96(17) . . ? N3 Cu2 N4 85.85(17) . . ? O2 Cu2 N8 92.13(15) . . ? N7 Cu2 N8 94.83(16) . . ? N3 Cu2 N8 100.02(17) . . ? N4 Cu2 N8 81.49(15) . . ? C19 O1 Cu1 130.9(3) . . ? C19 O2 Cu2 108.3(3) . . ? C11 N1 C10 107.1(4) . . ? C11 N1 C1 111.0(4) . . ? C10 N1 C1 112.4(4) . . ? C11 N1 Cu1 101.5(3) . . ? C10 N1 Cu1 117.5(3) . . ? C1 N1 Cu1 106.8(3) . . ? C13 N2 C2 111.3(4) . . ? C13 N2 C3 108.4(4) . . ? C2 N2 C3 108.7(4) . . ? C13 N2 Cu1 107.6(3) . . ? C2 N2 Cu1 98.2(3) . . ? C3 N2 Cu1 122.2(3) . . ? C15 N3 C6 110.0(4) . . ? C15 N3 C5 111.7(4) . . ? C6 N3 C5 108.4(4) . . ? C15 N3 Cu2 103.2(3) . . ? C6 N3 Cu2 103.8(3) . . ? C5 N3 Cu2 119.3(3) . . ? C7 N4 C17 111.0(4) . . ? C7 N4 C8 112.7(4) . . ? C17 N4 C8 105.3(4) . . ? C7 N4 Cu2 108.1(3) . . ? C17 N4 Cu2 105.6(3) . . ? C8 N4 Cu2 113.9(3) . . ? C12 N5 Cu1 110.7(3) . . ? C14 N6 Cu1 105.9(4) . . ? C16 N7 Cu2 109.1(3) . . ? C18 N8 Cu2 105.2(3) . . ? N1 C1 C2 111.2(4) . . ? N2 C2 C1 111.0(4) . . ? N2 C3 C4 113.6(5) . . ? C3 C4 C5 110.5(5) . . ? N3 C5 C4 116.2(5) . . ? N3 C6 C7 110.6(4) . . ? N4 C7 C6 112.3(5) . . ? N4 C8 C9 114.1(4) . . ? C10 C9 C8 110.9(5) . . ? N1 C10 C9 114.6(4) . . ? N1 C11 C12 110.2(4) . . ? N5 C12 C11 107.8(4) . . ? C14 C13 N2 112.6(5) . . ? C13 C14 N6 108.7(5) . . ? N3 C15 C16 109.3(5) . . ? C15 C16 N7 110.1(4) . . ? N4 C17 C18 112.6(4) . . ? N8 C18 C17 109.2(4) . . ? O3 C19 O1 122.7(5) . . ? O3 C19 O2 120.3(4) . . ? O1 C19 O2 117.0(4) . . ? C20 B1 C38 111.3(4) . . ? C20 B1 C32 106.7(4) . . ? C38 B1 C32 111.0(4) . . ? C20 B1 C26 110.1(4) . . ? C38 B1 C26 107.9(4) . . ? C32 B1 C26 109.8(4) . . ? C50 B2 C44 108.4(4) . . ? C50 B2 C56 110.4(4) . . ? C44 B2 C56 109.4(4) . . ? C50 B2 C62 109.5(4) . . ? C44 B2 C62 109.4(4) . . ? C56 B2 C62 109.6(4) . . ? C25 C20 C21 115.0(4) . . ? C25 C20 B1 121.9(4) . . ? C21 C20 B1 122.6(4) . . ? C22 C21 C20 123.6(5) . . ? C23 C22 C21 120.1(5) . . ? C24 C23 C22 118.4(5) . . ? C23 C24 C25 120.3(5) . . ? C20 C25 C24 122.7(5) . . ? C31 C26 C27 114.3(4) . . ? C31 C26 B1 122.8(4) . . ? C27 C26 B1 122.9(4) . . ? C28 C27 C26 123.1(4) . . ? C29 C28 C27 120.8(5) . . ? C30 C29 C28 118.1(5) . . ? C29 C30 C31 120.3(4) . . ? C26 C31 C30 123.4(4) . . ? C37 C32 C33 113.3(4) . . ? C37 C32 B1 124.4(4) . . ? C33 C32 B1 122.3(4) . . ? C34 C33 C32 123.9(4) . . ? C33 C34 C35 119.9(4) . . ? C36 C35 C34 118.7(5) . . ? C35 C36 C37 120.5(5) . . ? C36 C37 C32 123.7(5) . . ? C39 C38 C43 114.8(4) . . ? C39 C38 B1 124.0(4) . . ? C43 C38 B1 120.9(4) . . ? C38 C39 C40 122.9(4) . . ? C41 C40 C39 119.9(5) . . ? C40 C41 C42 119.6(5) . . ? C41 C42 C43 119.3(5) . . ? C42 C43 C38 123.5(5) . . ? C49 C44 C45 114.2(4) . . ? C49 C44 B2 123.3(4) . . ? C45 C44 B2 122.2(4) . . ? C46 C45 C44 123.3(4) . . ? C45 C46 C47 120.0(5) . . ? C48 C47 C46 118.3(5) . . ? C49 C48 C47 120.7(5) . . ? C48 C49 C44 123.6(5) . . ? C55 C50 C51 114.9(5) . . ? C55 C50 B2 121.3(4) . . ? C51 C50 B2 123.8(4) . . ? C52 C51 C50 122.8(5) . . ? C53 C52 C51 119.9(5) . . ? C52 C53 C54 120.0(5) . . ? C53 C54 C55 118.9(5) . . ? C50 C55 C54 123.3(5) . . ? C61 C56 C57 114.4(4) . . ? C61 C56 B2 124.7(4) . . ? C57 C56 B2 120.9(4) . . ? C58 C57 C56 123.6(4) . . ? C57 C58 C59 119.7(5) . . ? C60 C59 C58 118.6(5) . . ? C61 C60 C59 120.6(5) . . ? C60 C61 C56 123.1(5) . . ? C63 C62 C67 114.5(4) . . ? C63 C62 B2 121.3(4) . . ? C67 C62 B2 124.2(4) . . ? C64 C63 C62 123.2(5) . . ? C65 C64 C63 120.4(5) . . ? C64 C65 C66 118.4(5) . . ? C67 C66 C65 120.5(5) . . ? C66 C67 C62 122.8(5) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N5 2.009(4) . ? Cu1 N6 2.029(4) . ? Cu1 O1 2.079(3) . ? Cu1 N2 2.087(4) . ? Cu1 N1 2.094(4) . ? Cu2 O2 1.968(3) . ? Cu2 N7 2.007(4) . ? Cu2 N3 2.047(4) . ? Cu2 N4 2.059(4) . ? Cu2 N8 2.340(4) . ? O1 C19 1.290(5) . ? O2 C19 1.312(6) . ? O3 C19 1.272(6) . ? N1 C11 1.481(6) . ? N1 C10 1.487(6) . ? N1 C1 1.494(6) . ? N2 C13 1.490(7) . ? N2 C2 1.493(6) . ? N2 C3 1.511(7) . ? N3 C15 1.481(6) . ? N3 C6 1.489(7) . ? N3 C5 1.518(7) . ? N4 C7 1.491(7) . ? N4 C17 1.497(6) . ? N4 C8 1.500(6) . ? N5 C12 1.477(6) . ? N6 C14 1.509(7) . ? N7 C16 1.508(6) . ? N8 C18 1.470(7) . ? C1 C2 1.512(7) . ? C3 C4 1.519(7) . ? C4 C5 1.522(8) . ? C6 C7 1.511(7) . ? C8 C9 1.508(7) . ? C9 C10 1.497(7) . ? C11 C12 1.525(7) . ? C13 C14 1.438(9) . ? C15 C16 1.500(8) . ? C17 C18 1.505(7) . ? B1 C20 1.646(7) . ? B1 C38 1.645(7) . ? B1 C32 1.650(7) . ? B1 C26 1.656(7) . ? B2 C50 1.648(7) . ? B2 C44 1.647(7) . ? B2 C56 1.649(7) . ? B2 C62 1.648(7) . ? C20 C25 1.393(7) . ? C20 C21 1.393(7) . ? C21 C22 1.389(7) . ? C22 C23 1.386(7) . ? C23 C24 1.384(8) . ? C24 C25 1.405(7) . ? C26 C31 1.394(6) . ? C26 C27 1.401(6) . ? C27 C28 1.383(7) . ? C28 C29 1.383(6) . ? C29 C30 1.376(7) . ? C30 C31 1.395(7) . ? C32 C37 1.408(6) . ? C32 C33 1.414(6) . ? C33 C34 1.376(6) . ? C34 C35 1.394(7) . ? C35 C36 1.372(7) . ? C36 C37 1.385(7) . ? C38 C39 1.391(6) . ? C38 C43 1.404(6) . ? C39 C40 1.399(6) . ? C40 C41 1.379(6) . ? C41 C42 1.380(7) . ? C42 C43 1.393(7) . ? C44 C49 1.405(6) . ? C44 C45 1.413(6) . ? C45 C46 1.384(7) . ? C46 C47 1.402(7) . ? C47 C48 1.383(7) . ? C48 C49 1.376(7) . ? C50 C55 1.401(7) . ? C50 C51 1.402(7) . ? C51 C52 1.395(7) . ? C52 C53 1.380(7) . ? C53 C54 1.378(8) . ? C54 C55 1.408(7) . ? C56 C61 1.405(6) . ? C56 C57 1.402(6) . ? C57 C58 1.387(7) . ? C58 C59 1.390(7) . ? C59 C60 1.385(7) . ? C60 C61 1.379(7) . ? C62 C63 1.396(6) . ? C62 C67 1.403(7) . ? C63 C64 1.389(7) . ? C64 C65 1.367(7) . ? C65 C66 1.391(7) . ? C66 C67 1.381(7) . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5 Cu1 O1 C19 0.3(4) . . . . ? N6 Cu1 O1 C19 -96.6(4) . . . . ? N2 Cu1 O1 C19 174.9(4) . . . . ? N1 Cu1 O1 C19 86.6(4) . . . . ? N7 Cu2 O2 C19 -75.6(3) . . . . ? N3 Cu2 O2 C19 9.4(9) . . . . ? N4 Cu2 O2 C19 107.8(3) . . . . ? N8 Cu2 O2 C19 -170.6(3) . . . . ? N5 Cu1 N1 C11 -26.5(3) . . . . ? N6 Cu1 N1 C11 65.7(5) . . . . ? O1 Cu1 N1 C11 -121.0(3) . . . . ? N2 Cu1 N1 C11 131.6(3) . . . . ? N5 Cu1 N1 C10 89.8(4) . . . . ? N6 Cu1 N1 C10 -178.0(4) . . . . ? O1 Cu1 N1 C10 -4.7(4) . . . . ? N2 Cu1 N1 C10 -112.0(4) . . . . ? N5 Cu1 N1 C1 -142.9(3) . . . . ? N6 Cu1 N1 C1 -50.7(5) . . . . ? O1 Cu1 N1 C1 122.6(3) . . . . ? N2 Cu1 N1 C1 15.2(3) . . . . ? N5 Cu1 N2 C13 -86.4(5) . . . . ? N6 Cu1 N2 C13 2.1(3) . . . . ? O1 Cu1 N2 C13 106.8(3) . . . . ? N1 Cu1 N2 C13 -153.2(3) . . . . ? N5 Cu1 N2 C2 29.0(6) . . . . ? N6 Cu1 N2 C2 117.6(3) . . . . ? O1 Cu1 N2 C2 -137.7(3) . . . . ? N1 Cu1 N2 C2 -37.7(3) . . . . ? N5 Cu1 N2 C3 147.3(4) . . . . ? N6 Cu1 N2 C3 -124.1(4) . . . . ? O1 Cu1 N2 C3 -19.4(4) . . . . ? N1 Cu1 N2 C3 80.5(4) . . . . ? O2 Cu2 N3 C15 -116.3(7) . . . . ? N7 Cu2 N3 C15 -30.5(4) . . . . ? N4 Cu2 N3 C15 144.3(4) . . . . ? N8 Cu2 N3 C15 63.7(4) . . . . ? O2 Cu2 N3 C6 128.9(7) . . . . ? N7 Cu2 N3 C6 -145.3(3) . . . . ? N4 Cu2 N3 C6 29.4(3) . . . . ? N8 Cu2 N3 C6 -51.1(3) . . . . ? O2 Cu2 N3 C5 8.2(10) . . . . ? N7 Cu2 N3 C5 94.0(4) . . . . ? N4 Cu2 N3 C5 -91.3(4) . . . . ? N8 Cu2 N3 C5 -171.8(4) . . . . ? O2 Cu2 N4 C7 -175.5(3) . . . . ? N7 Cu2 N4 C7 24.2(11) . . . . ? N3 Cu2 N4 C7 -7.5(3) . . . . ? N8 Cu2 N4 C7 93.2(3) . . . . ? O2 Cu2 N4 C17 65.7(3) . . . . ? N7 Cu2 N4 C17 -94.6(10) . . . . ? N3 Cu2 N4 C17 -126.3(3) . . . . ? N8 Cu2 N4 C17 -25.6(3) . . . . ? O2 Cu2 N4 C8 -49.4(3) . . . . ? N7 Cu2 N4 C8 150.3(9) . . . . ? N3 Cu2 N4 C8 118.6(3) . . . . ? N8 Cu2 N4 C8 -140.6(3) . . . . ? N6 Cu1 N5 C12 -153.2(3) . . . . ? O1 Cu1 N5 C12 100.4(3) . . . . ? N2 Cu1 N5 C12 -67.0(6) . . . . ? N1 Cu1 N5 C12 -0.3(3) . . . . ? N5 Cu1 N6 C14 129.7(4) . . . . ? O1 Cu1 N6 C14 -133.3(4) . . . . ? N2 Cu1 N6 C14 -26.4(4) . . . . ? N1 Cu1 N6 C14 39.8(6) . . . . ? O2 Cu2 N7 C16 173.9(3) . . . . ? N3 Cu2 N7 C16 6.0(3) . . . . ? N4 Cu2 N7 C16 -25.7(11) . . . . ? N8 Cu2 N7 C16 -93.7(3) . . . . ? O2 Cu2 N8 C18 -97.3(3) . . . . ? N7 Cu2 N8 C18 169.1(3) . . . . ? N3 Cu2 N8 C18 82.7(3) . . . . ? N4 Cu2 N8 C18 -1.5(3) . . . . ? C11 N1 C1 C2 -97.7(5) . . . . ? C10 N1 C1 C2 142.4(4) . . . . ? Cu1 N1 C1 C2 12.1(5) . . . . ? C13 N2 C2 C1 168.5(5) . . . . ? C3 N2 C2 C1 -72.3(5) . . . . ? Cu1 N2 C2 C1 55.9(5) . . . . ? N1 C1 C2 N2 -48.3(6) . . . . ? C13 N2 C3 C4 -75.7(5) . . . . ? C2 N2 C3 C4 163.2(4) . . . . ? Cu1 N2 C3 C4 50.2(6) . . . . ? N2 C3 C4 C5 -157.5(4) . . . . ? C15 N3 C5 C4 85.3(6) . . . . ? C6 N3 C5 C4 -153.3(5) . . . . ? Cu2 N3 C5 C4 -35.0(6) . . . . ? C3 C4 C5 N3 142.2(4) . . . . ? C15 N3 C6 C7 -156.3(5) . . . . ? C5 N3 C6 C7 81.4(5) . . . . ? Cu2 N3 C6 C7 -46.5(5) . . . . ? C17 N4 C7 C6 98.6(5) . . . . ? C8 N4 C7 C6 -143.6(5) . . . . ? Cu2 N4 C7 C6 -16.7(6) . . . . ? N3 C6 C7 N4 43.5(7) . . . . ? C7 N4 C8 C9 64.2(6) . . . . ? C17 N4 C8 C9 -174.7(4) . . . . ? Cu2 N4 C8 C9 -59.5(5) . . . . ? N4 C8 C9 C10 154.3(4) . . . . ? C11 N1 C10 C9 174.5(4) . . . . ? C1 N1 C10 C9 -63.4(5) . . . . ? Cu1 N1 C10 C9 61.1(5) . . . . ? C8 C9 C10 N1 -153.7(4) . . . . ? C10 N1 C11 C12 -74.6(5) . . . . ? C1 N1 C11 C12 162.4(4) . . . . ? Cu1 N1 C11 C12 49.2(4) . . . . ? Cu1 N5 C12 C11 27.0(5) . . . . ? N1 C11 C12 N5 -52.8(5) . . . . ? C2 N2 C13 C14 -81.7(6) . . . . ? C3 N2 C13 C14 158.9(5) . . . . ? Cu1 N2 C13 C14 24.9(6) . . . . ? N2 C13 C14 N6 -48.7(7) . . . . ? Cu1 N6 C14 C13 47.5(6) . . . . ? C6 N3 C15 C16 159.9(5) . . . . ? C5 N3 C15 C16 -79.7(6) . . . . ? Cu2 N3 C15 C16 49.7(5) . . . . ? N3 C15 C16 N7 -47.8(6) . . . . ? Cu2 N7 C16 C15 20.2(5) . . . . ? C7 N4 C17 C18 -64.2(6) . . . . ? C8 N4 C17 C18 173.6(4) . . . . ? Cu2 N4 C17 C18 52.7(5) . . . . ? Cu2 N8 C18 C17 28.6(5) . . . . ? N4 C17 C18 N8 -56.3(6) . . . . ? Cu1 O1 C19 O3 24.5(7) . . . . ? Cu1 O1 C19 O2 -157.1(3) . . . . ? Cu2 O2 C19 O3 169.0(4) . . . . ? Cu2 O2 C19 O1 -9.4(5) . . . . ? C38 B1 C20 C25 152.5(4) . . . . ? C32 B1 C20 C25 -86.2(5) . . . . ? C26 B1 C20 C25 32.9(6) . . . . ? C38 B1 C20 C21 -35.9(6) . . . . ? C32 B1 C20 C21 85.4(5) . . . . ? C26 B1 C20 C21 -155.5(4) . . . . ? C25 C20 C21 C22 0.6(7) . . . . ? B1 C20 C21 C22 -171.5(4) . . . . ? C20 C21 C22 C23 0.0(8) . . . . ? C21 C22 C23 C24 -0.5(7) . . . . ? C22 C23 C24 C25 0.4(8) . . . . ? C21 C20 C25 C24 -0.7(7) . . . . ? B1 C20 C25 C24 171.5(5) . . . . ? C23 C24 C25 C20 0.2(8) . . . . ? C20 B1 C26 C31 93.7(5) . . . . ? C38 B1 C26 C31 -28.0(6) . . . . ? C32 B1 C26 C31 -149.1(4) . . . . ? C20 B1 C26 C27 -85.5(5) . . . . ? C38 B1 C26 C27 152.8(4) . . . . ? C32 B1 C26 C27 31.7(6) . . . . ? C31 C26 C27 C28 0.3(7) . . . . ? B1 C26 C27 C28 179.6(4) . . . . ? C26 C27 C28 C29 -0.5(8) . . . . ? C27 C28 C29 C30 0.7(7) . . . . ? C28 C29 C30 C31 -0.7(7) . . . . ? C27 C26 C31 C30 -0.3(7) . . . . ? B1 C26 C31 C30 -179.6(4) . . . . ? C29 C30 C31 C26 0.6(7) . . . . ? C20 B1 C32 C37 -14.5(6) . . . . ? C38 B1 C32 C37 106.9(5) . . . . ? C26 B1 C32 C37 -133.9(5) . . . . ? C20 B1 C32 C33 165.6(4) . . . . ? C38 B1 C32 C33 -73.0(6) . . . . ? C26 B1 C32 C33 46.2(6) . . . . ? C37 C32 C33 C34 1.1(7) . . . . ? B1 C32 C33 C34 -179.0(4) . . . . ? C32 C33 C34 C35 -1.4(7) . . . . ? C33 C34 C35 C36 1.2(7) . . . . ? C34 C35 C36 C37 -0.8(8) . . . . ? C35 C36 C37 C32 0.6(8) . . . . ? C33 C32 C37 C36 -0.6(7) . . . . ? B1 C32 C37 C36 179.4(5) . . . . ? C20 B1 C38 C39 148.7(4) . . . . ? C32 B1 C38 C39 30.0(6) . . . . ? C26 B1 C38 C39 -90.3(5) . . . . ? C20 B1 C38 C43 -38.2(6) . . . . ? C32 B1 C38 C43 -156.9(4) . . . . ? C26 B1 C38 C43 82.8(5) . . . . ? C43 C38 C39 C40 -0.7(7) . . . . ? B1 C38 C39 C40 172.7(4) . . . . ? C38 C39 C40 C41 -0.6(7) . . . . ? C39 C40 C41 C42 1.0(7) . . . . ? C40 C41 C42 C43 0.0(8) . . . . ? C41 C42 C43 C38 -1.5(8) . . . . ? C39 C38 C43 C42 1.8(7) . . . . ? B1 C38 C43 C42 -171.9(5) . . . . ? C50 B2 C44 C49 -81.5(5) . . . . ? C56 B2 C44 C49 158.0(4) . . . . ? C62 B2 C44 C49 37.9(6) . . . . ? C50 B2 C44 C45 91.9(5) . . . . ? C56 B2 C44 C45 -28.6(6) . . . . ? C62 B2 C44 C45 -148.7(4) . . . . ? C49 C44 C45 C46 0.1(7) . . . . ? B2 C44 C45 C46 -173.8(4) . . . . ? C44 C45 C46 C47 0.4(7) . . . . ? C45 C46 C47 C48 -0.4(7) . . . . ? C46 C47 C48 C49 0.0(7) . . . . ? C47 C48 C49 C44 0.6(8) . . . . ? C45 C44 C49 C48 -0.6(7) . . . . ? B2 C44 C49 C48 173.3(5) . . . . ? C44 B2 C50 C55 165.8(4) . . . . ? C56 B2 C50 C55 -74.3(5) . . . . ? C62 B2 C50 C55 46.4(5) . . . . ? C44 B2 C50 C51 -13.7(6) . . . . ? C56 B2 C50 C51 106.1(5) . . . . ? C62 B2 C50 C51 -133.1(4) . . . . ? C55 C50 C51 C52 2.2(6) . . . . ? B2 C50 C51 C52 -178.2(4) . . . . ? C50 C51 C52 C53 -0.6(7) . . . . ? C51 C52 C53 C54 -0.7(7) . . . . ? C52 C53 C54 C55 0.3(7) . . . . ? C51 C50 C55 C54 -2.6(7) . . . . ? B2 C50 C55 C54 177.8(4) . . . . ? C53 C54 C55 C50 1.5(7) . . . . ? C50 B2 C56 C61 18.5(7) . . . . ? C44 B2 C56 C61 137.8(5) . . . . ? C62 B2 C56 C61 -102.2(5) . . . . ? C50 B2 C56 C57 -165.5(4) . . . . ? C44 B2 C56 C57 -46.2(6) . . . . ? C62 B2 C56 C57 73.8(6) . . . . ? C61 C56 C57 C58 -0.9(7) . . . . ? B2 C56 C57 C58 -177.3(4) . . . . ? C56 C57 C58 C59 1.1(8) . . . . ? C57 C58 C59 C60 -0.3(8) . . . . ? C58 C59 C60 C61 -0.5(8) . . . . ? C59 C60 C61 C56 0.8(8) . . . . ? C57 C56 C61 C60 0.0(7) . . . . ? B2 C56 C61 C60 176.2(5) . . . . ? C50 B2 C62 C63 43.0(6) . . . . ? C44 B2 C62 C63 -75.7(5) . . . . ? C56 B2 C62 C63 164.2(4) . . . . ? C50 B2 C62 C67 -139.8(4) . . . . ? C44 B2 C62 C67 101.4(5) . . . . ? C56 B2 C62 C67 -18.6(6) . . . . ? C67 C62 C63 C64 -4.0(7) . . . . ? B2 C62 C63 C64 173.4(5) . . . . ? C62 C63 C64 C65 1.0(8) . . . . ? C63 C64 C65 C66 2.7(7) . . . . ? C64 C65 C66 C67 -3.1(7) . . . . ? C65 C66 C67 C62 -0.1(7) . . . . ? C63 C62 C67 C66 3.6(7) . . . . ? B2 C62 C67 C66 -173.8(4) . . . . ?
1100720.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100720.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100720 loop_ _publ_author_name 'Aaron M. Appel' 'Rachel Newell' 'Daniel L. DuBois' 'M. Rakowski DuBois' _publ_contact_author_address '215 UCB, Boulder, CO, 80309-0215, USA' _publ_contact_author_name 'Mary Rakowski-DuBois' _publ_section_title ; Concentration of Carbon Dioxide by Electrochemically Modulated Complexation with a Binuclear Copper Complex ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3046 _journal_page_last 3056 _journal_paper_doi 10.1021/ic050023k _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C340.43 H348.62 B8 Cu8 N36.22 O20' _chemical_formula_weight 5862.30 _chemical_name_common Cu2(CO3)(tpmc)(BPh4)2 _chemical_name_systematic ; ? ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 101.7900(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 1 _cell_length_a 9.4708(4) _cell_length_b 25.9130(11) _cell_length_c 31.6182(13) _cell_measurement_reflns_used 7501 _cell_measurement_temperature 141(2) _cell_measurement_theta_max 28.0015 _cell_measurement_theta_min 2.3185 _cell_volume 7595.9(6) _computing_cell_refinement 'SAINT, Bruker' _computing_data_collection 'SMART, Bruker' _computing_data_reduction 'SAINT, Bruker' _computing_molecular_graphics 'SHELXTL, Bruker' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 141(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1144 _diffrn_reflns_av_sigmaI/netI 0.1066 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_number 58343 _diffrn_reflns_theta_full 27.48 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_min 1.53 _exptl_absorpt_coefficient_mu 0.619 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.2395 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; absorption correction applied using SADABS (Blessing, R. H. Acta Crystallogr., Sect. A 1995, 51, 33-38) ; _exptl_crystal_colour blue-green _exptl_crystal_density_diffrn 1.282 _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'cut prism' _exptl_crystal_F_000 3076 _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.25 _refine_diff_density_max 1.372 _refine_diff_density_min -0.709 _refine_diff_density_rms 0.104 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.159 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 1032 _refine_ls_number_reflns 17414 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.159 _refine_ls_R_factor_all 0.1448 _refine_ls_R_factor_gt 0.1092 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0611P)^2^+31.3481P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2472 _refine_ls_wR_factor_ref 0.2644 _reflns_number_gt 12425 _reflns_number_total 17414 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic050023ksi20050107_041509.cif _cod_data_source_block final _cod_original_sg_symbol_H-M 'P 1 21/n 1' _cod_database_code 1100720 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.82686(7) 0.10762(2) 0.17915(2) 0.02832(17) Uani 1 1 d . . . Cu2 Cu 0.93908(9) 0.14320(3) 0.31880(2) 0.0410(2) Uani 1 1 d . . . B1 B 0.2480(8) 0.3107(3) 0.1121(2) 0.0367(15) Uani 1 1 d . . . B2 B 0.7782(7) 0.4089(2) 0.37678(19) 0.0261(12) Uani 1 1 d . . . N1 N 0.7858(6) 0.18321(19) 0.15834(16) 0.0393(12) Uani 1 1 d . B . N2 N 0.6054(5) 0.10084(18) 0.17131(14) 0.0325(10) Uani 1 1 d . B . N3 N 0.7118(5) 0.13459(18) 0.32639(15) 0.0327(10) Uani 1 1 d . B . N4 N 0.8919(5) 0.22129(18) 0.31270(15) 0.0333(10) Uani 1 1 d . B . N5 N 0.8391(5) 0.09779(19) 0.11033(15) 0.0359(11) Uani 1 1 d . B . N6 N 0.8231(5) 0.03291(18) 0.19432(16) 0.0353(11) Uani 1 1 d . B . N7 N 0.9395(5) 0.06977(15) 0.32743(15) 0.0286(10) Uani 1 1 d . B . N8 N 1.0289(6) 0.1645(2) 0.38239(16) 0.0397(12) Uani 1 1 d . B . N9 N 1.424(2) 0.1074(9) 0.4046(5) 0.142(10) Uani 0.568(15) 1 d P A 1 N10 N 0.128(3) 0.5660(8) 0.0268(7) 0.132(11) Uani 0.486(14) 1 d P . . O1A O 0.9604(6) 0.1319(2) 0.26184(18) 0.0348(14) Uiso 0.739(7) 1 d P B 1 O1B O 0.942(2) 0.1264(8) 0.2315(7) 0.061(6) Uiso 0.261(7) 1 d P B 2 O2A O 1.0336(5) 0.11362(18) 0.20200(16) 0.0293(13) Uiso 0.739(7) 1 d P B 1 O2B O 1.0960(18) 0.1386(6) 0.2895(5) 0.042(4) Uiso 0.261(7) 1 d P B 2 O3A O 1.1962(7) 0.1152(2) 0.2642(2) 0.0457(16) Uiso 0.739(7) 1 d P B 1 O3B O 1.177(2) 0.1053(7) 0.2341(7) 0.056(5) Uiso 0.261(7) 1 d P B 2 O4B O 1.354(3) 0.1388(11) 0.3543(9) 0.094(9) Uiso 0.261(7) 1 d P B 2 O4A O 1.2103(9) 0.1116(3) 0.1444(2) 0.0514(18) Uiso 0.739(7) 1 d P B 1 O5B O 1.151(4) 0.1206(11) 0.1444(9) 0.083(9) Uiso 0.261(7) 1 d P B 2 O5A O 1.2835(10) 0.1752(3) 0.3348(3) 0.079(3) Uiso 0.739(7) 1 d P B 1 C1 C 0.6238(7) 0.1882(2) 0.14356(19) 0.0405(14) Uani 1 1 d . . . H1A H 0.5835 0.2074 0.1654 0.06(2) Uiso 1 1 d R B . H1B H 0.6048 0.2087 0.1166 0.06(2) Uiso 1 1 d R . . C2 C 0.5483(7) 0.1371(2) 0.13503(19) 0.0391(14) Uani 1 1 d . B . H2A H 0.4435 0.1423 0.1328 0.035(16) Uiso 1 1 d R . . H2B H 0.5634 0.1224 0.1074 0.047(19) Uiso 1 1 d R . . C3 C 0.5387(6) 0.1138(2) 0.20870(18) 0.0320(12) Uani 1 1 d . . . H3A H 0.4408 0.0986 0.2039 0.07(2) Uiso 1 1 d R B . H3B H 0.5279 0.1518 0.2097 0.027(15) Uiso 1 1 d R . . C4 C 0.6234(6) 0.0954(2) 0.25223(18) 0.0345(12) Uani 1 1 d . B . H4A H 0.5971 0.0593 0.2572 0.029(15) Uiso 1 1 d R . . H4B H 0.7281 0.0965 0.2525 0.020(13) Uiso 1 1 d R . . C5 C 0.5901(7) 0.1296(3) 0.28820(19) 0.0406(14) Uani 1 1 d . . . H5A H 0.5640 0.1643 0.2763 0.08(3) Uiso 1 1 d R B . H5B H 0.5056 0.1154 0.2980 0.036(16) Uiso 1 1 d R . . C6 C 0.6965(7) 0.1840(2) 0.34831(17) 0.0356(13) Uani 1 1 d . . . H6A H 0.7561 0.1821 0.3778 0.046(18) Uiso 1 1 d R B . H6B H 0.5950 0.1892 0.3507 0.07(2) Uiso 1 1 d R . . C7 C 0.7469(7) 0.2291(2) 0.3248(2) 0.0398(14) Uani 1 1 d . B . H7A H 0.7521 0.2603 0.3432 0.042(17) Uiso 1 1 d R . . H7B H 0.6734 0.2356 0.2983 0.07(3) Uiso 1 1 d R . . C8 C 0.8975(7) 0.2444(2) 0.26968(19) 0.0378(13) Uani 1 1 d . . . H8A H 0.9950 0.2386 0.2639 0.037(17) Uiso 1 1 d R B . H8B H 0.8826 0.2820 0.2710 0.08(3) Uiso 1 1 d R . . C9 C 0.7877(7) 0.2227(2) 0.23237(18) 0.0366(13) Uani 1 1 d . B . H9A H 0.6981 0.2434 0.2282 0.05(2) Uiso 1 1 d R . . H9B H 0.7641 0.1868 0.2391 0.023(14) Uiso 1 1 d R . . C10 C 0.8476(8) 0.2233(2) 0.19109(19) 0.0420(15) Uani 1 1 d . . . H10A H 0.8284 0.2576 0.1774 0.08(3) Uiso 1 1 d R B . H10B H 0.9532 0.2187 0.1989 0.005(11) Uiso 1 1 d R . . C11 C 0.8605(9) 0.1892(3) 0.1209(2) 0.0485(17) Uani 1 1 d . . . H11A H 0.9654 0.1936 0.1318 0.07(2) Uiso 1 1 d R B . H11B H 0.8238 0.2208 0.1047 0.06(2) Uiso 1 1 d R . . C12 C 0.8359(7) 0.1444(2) 0.09091(19) 0.0387(13) Uani 1 1 d . B . C13 C 0.8165(8) 0.1497(3) 0.0464(2) 0.0437(15) Uani 1 1 d . . . H13 H 0.8124 0.1829 0.0334 0.10(3) Uiso 1 1 d R B . C14 C 0.8026(8) 0.1051(3) 0.0213(2) 0.0483(16) Uani 1 1 d . B . H14 H 0.7891 0.1071 -0.0092 0.10(3) Uiso 1 1 d R . . C15 C 0.8090(7) 0.0578(3) 0.0411(2) 0.0436(15) Uani 1 1 d . . . H15 H 0.8002 0.0270 0.0247 0.05(2) Uiso 1 1 d R B . C16 C 0.8266(6) 0.0557(2) 0.0851(2) 0.0385(13) Uani 1 1 d . B . H16 H 0.8313 0.0228 0.0982 0.028(15) Uiso 1 1 d R . . C17 C 0.5760(7) 0.0452(2) 0.1587(2) 0.0390(14) Uani 1 1 d . . . H17A H 0.4792 0.0350 0.1630 0.021(13) Uiso 1 1 d R B . H17B H 0.5777 0.0409 0.1277 0.036(16) Uiso 1 1 d R . . C18 C 0.6880(6) 0.0118(2) 0.18495(18) 0.0332(12) Uani 1 1 d . B . C19 C 0.6650(7) -0.0375(2) 0.1993(2) 0.0417(14) Uani 1 1 d . . . H19 H 0.5703 -0.0515 0.1941 0.06(2) Uiso 1 1 d R B . C20 C 0.7779(9) -0.0662(3) 0.2208(3) 0.0571(19) Uani 1 1 d . B . H20 H 0.7639 -0.1000 0.2307 0.07(2) Uiso 1 1 d R . . C21 C 0.9177(8) -0.0447(3) 0.2278(2) 0.0522(17) Uani 1 1 d . . . H21 H 0.9987 -0.0644 0.2412 0.06(2) Uiso 1 1 d R B . C22 C 0.9324(7) 0.0043(2) 0.2146(2) 0.0442(15) Uani 1 1 d . B . H22 H 1.0263 0.0188 0.2201 0.015(12) Uiso 1 1 d R . . C23 C 0.7189(8) 0.0891(2) 0.3540(2) 0.0422(14) Uani 1 1 d . . . H23A H 0.6222 0.0730 0.3489 0.06(2) Uiso 1 1 d R B . H23B H 0.7439 0.0995 0.3847 0.11(4) Uiso 1 1 d R . . C24 C 0.8229(8) 0.0491(2) 0.34431(19) 0.0405(14) Uani 1 1 d . B . C25 C 0.8035(9) -0.0029(3) 0.3501(3) 0.057(2) Uani 1 1 d . . . H25 H 0.7162 -0.0151 0.3568 0.10(3) Uiso 1 1 d R B . C26 C 0.9160(11) -0.0366(3) 0.3453(3) 0.066(2) Uani 1 1 d . B . H26 H 0.9078 -0.0724 0.3503 0.043(18) Uiso 1 1 d R . . C27 C 1.0358(10) -0.0177(3) 0.3335(3) 0.064(2) Uani 1 1 d . . . H27 H 1.1123 -0.0396 0.3294 0.07(2) Uiso 1 1 d R B . C28 C 1.0454(9) 0.0345(3) 0.3264(2) 0.0515(18) Uani 1 1 d . B . H28 H 1.1341 0.0479 0.3224 0.11(4) Uiso 1 1 d R . . C29 C 1.0052(8) 0.2465(2) 0.3447(2) 0.0468(16) Uani 1 1 d . . . H29A H 0.9774 0.2820 0.3501 0.07(2) Uiso 1 1 d R B . H29B H 1.0905 0.2481 0.3316 0.027(15) Uiso 1 1 d R . . C30 C 1.0489(7) 0.2164(2) 0.38600(19) 0.0409(14) Uani 1 1 d . B . C31 C 1.1136(8) 0.2398(3) 0.4250(2) 0.0475(16) Uani 1 1 d . . . H31 H 1.1258 0.2761 0.4270 0.08(3) Uiso 1 1 d R B . C32 C 1.1587(9) 0.2092(3) 0.4597(2) 0.063(2) Uani 1 1 d . B . H32 H 1.2045 0.2239 0.4865 0.07(2) Uiso 1 1 d R . . C33 C 1.1366(9) 0.1558(3) 0.4571(2) 0.063(2) Uani 1 1 d . . . H33 H 1.1680 0.1340 0.4812 0.07(3) Uiso 1 1 d R B . C34 C 1.0695(8) 0.1359(3) 0.4171(2) 0.0498(17) Uani 1 1 d . B . H34 H 1.0532 0.1000 0.4151 0.021(13) Uiso 1 1 d R . . C35A C 1.0676(11) 0.1197(3) 0.2430(4) 0.040(3) Uiso 0.739(7) 1 d P B 1 C35B C 1.0768(5) 0.12290(17) 0.25075(15) 0.017(7) Uiso 0.261(7) 1 d P B 2 C36 C 0.3160(5) 0.36729(17) 0.10279(15) 0.0404(14) Uani 1 1 d R . . C37 C 0.4572(5) 0.38258(17) 0.12220(15) 0.0491(17) Uani 1 1 d R . . H37 H 0.5130 0.3607 0.1431 0.08(3) Uiso 1 1 d R . . C38 C 0.5187(9) 0.4286(3) 0.1106(2) 0.0550(19) Uani 1 1 d . . . H38 H 0.6139 0.4372 0.1249 0.06(2) Uiso 1 1 d R . . C39 C 0.4415(10) 0.4599(3) 0.0791(3) 0.061(2) Uani 1 1 d . . . H39 H 0.5089 0.4869 0.0750 0.07(2) Uiso 1 1 d R . . C40 C 0.3075(10) 0.4465(3) 0.0600(3) 0.062(2) Uani 1 1 d . . . H40 H 0.2529 0.4676 0.0380 0.10(3) Uiso 1 1 d R . . C41 C 0.2435(8) 0.4016(2) 0.0716(2) 0.0466(16) Uani 1 1 d . . . H41 H 0.1475 0.3934 0.0578 0.030(15) Uiso 1 1 d R . . C42 C 0.2982(7) 0.2682(2) 0.07973(18) 0.0373(13) Uani 1 1 d . . . C43 C 0.4202(7) 0.2743(2) 0.0624(2) 0.0423(14) Uani 1 1 d . . . H43 H 0.4771 0.3042 0.0697 0.046(19) Uiso 1 1 d R . . C44 C 0.4671(8) 0.2383(3) 0.0349(2) 0.0513(17) Uani 1 1 d . . . H44 H 0.5525 0.2437 0.0247 0.05(2) Uiso 1 1 d R . . C45 C 0.3871(10) 0.1940(3) 0.0236(2) 0.057(2) Uani 1 1 d . . . H45 H 0.4140 0.1697 0.0043 0.07(3) Uiso 1 1 d R . . C46 C 0.2672(11) 0.1866(3) 0.0402(2) 0.066(2) Uani 1 1 d . . . H46 H 0.2113 0.1562 0.0331 0.06(2) Uiso 1 1 d R . . C47 C 0.2233(9) 0.2227(2) 0.0672(2) 0.0518(18) Uani 1 1 d . . . H47 H 0.1394 0.2159 0.0783 0.07(2) Uiso 1 1 d R . . C48 C 0.0701(7) 0.3170(2) 0.1011(2) 0.0408(14) Uani 1 1 d . . . C49 C -0.0106(8) 0.3119(3) 0.0589(3) 0.0555(18) Uani 1 1 d . . . H49 H 0.0350 0.2991 0.0374 0.07(2) Uiso 1 1 d R . . C50 C -0.1591(9) 0.3230(4) 0.0491(3) 0.075(3) Uani 1 1 d . . . H50 H -0.2072 0.3104 0.0231 0.11(4) Uiso 1 1 d R . . C51 C -0.2275(9) 0.3391(3) 0.0812(3) 0.071(2) Uani 1 1 d . . . H51 H -0.3269 0.3459 0.0754 0.10(3) Uiso 1 1 d R . . C52 C -0.1527(9) 0.3439(3) 0.1226(3) 0.062(2) Uani 1 1 d . . . H52 H -0.1998 0.3556 0.1445 0.08(3) Uiso 1 1 d R . . C53 C -0.0064(8) 0.3322(2) 0.1329(3) 0.0475(16) Uani 1 1 d . . . H53 H 0.0432 0.3346 0.1621 0.020(14) Uiso 1 1 d R . . C54 C 0.2967(7) 0.2926(2) 0.1629(2) 0.0389(13) Uani 1 1 d . . . C55 C 0.3409(8) 0.3259(3) 0.1982(2) 0.0444(15) Uani 1 1 d . . . H55 H 0.3712 0.3612 0.1901 0.042(17) Uiso 1 1 d R . . C56 C 0.3689(8) 0.3093(3) 0.2410(2) 0.0522(17) Uani 1 1 d . . . H56 H 0.4031 0.3332 0.2629 0.06(2) Uiso 1 1 d R . . C57 C 0.3528(8) 0.2583(3) 0.2508(2) 0.0484(16) Uani 1 1 d . . . H57 H 0.3708 0.2475 0.2801 0.06(2) Uiso 1 1 d R . . C58 C 0.3070(7) 0.2241(2) 0.2173(2) 0.0433(15) Uani 1 1 d . . . H58 H 0.2930 0.1888 0.2236 0.042(18) Uiso 1 1 d R . . C59 C 0.2839(7) 0.2409(2) 0.1749(2) 0.0411(14) Uani 1 1 d . . . H59 H 0.2559 0.2163 0.1525 0.038(17) Uiso 1 1 d R . . C60 C 0.7212(6) 0.4548(2) 0.40583(16) 0.0265(11) Uani 1 1 d . . . C61 C 0.5920(6) 0.4513(2) 0.42018(18) 0.0323(12) Uani 1 1 d . . . H61 H 0.5351 0.4212 0.4133 0.035(16) Uiso 1 1 d R . . C62 C 0.5405(7) 0.4902(2) 0.44373(18) 0.0368(13) Uani 1 1 d . . . H62 H 0.4532 0.4856 0.4536 0.042(18) Uiso 1 1 d R . . C63 C 0.6177(7) 0.5352(2) 0.45288(19) 0.0390(14) Uani 1 1 d . . . H63 H 0.5825 0.5626 0.4679 0.07(3) Uiso 1 1 d R . . C64 C 0.7457(8) 0.5405(2) 0.4400(2) 0.0452(16) Uani 1 1 d . . . H64 H 0.8021 0.5707 0.4473 0.025(14) Uiso 1 1 d R . . C65 C 0.7959(7) 0.5004(2) 0.4166(2) 0.0396(14) Uani 1 1 d . . . H65 H 0.8844 0.5054 0.4075 0.042(18) Uiso 1 1 d R . . C66 C 0.7099(6) 0.3538(2) 0.38904(18) 0.0299(11) Uani 1 1 d . . . C67 C 0.7831(7) 0.3212(2) 0.42124(18) 0.0338(12) Uani 1 1 d . . . H67 H 0.8791 0.3296 0.4345 0.020(13) Uiso 1 1 d R . . C68 C 0.7187(8) 0.2777(2) 0.4350(2) 0.0459(16) Uani 1 1 d . . . H68 H 0.7716 0.2572 0.4576 0.05(2) Uiso 1 1 d R . . C69 C 0.5808(8) 0.2641(2) 0.4164(2) 0.0472(17) Uani 1 1 d . . . H69 H 0.5365 0.2348 0.4260 0.07(2) Uiso 1 1 d R . . C70 C 0.5048(7) 0.2940(2) 0.3834(2) 0.0406(15) Uani 1 1 d . . . H70 H 0.4098 0.2848 0.3692 0.038(17) Uiso 1 1 d R . . C71 C 0.5689(6) 0.3380(2) 0.3702(2) 0.0353(13) Uani 1 1 d . . . H71 H 0.5154 0.3586 0.3478 0.039(17) Uiso 1 1 d R . . C72 C 0.7325(6) 0.4232(2) 0.32543(17) 0.0272(11) Uani 1 1 d . . . C73 C 0.7295(6) 0.4745(2) 0.31001(18) 0.0323(12) Uani 1 1 d . . . H73 H 0.7544 0.5013 0.3307 0.029(15) Uiso 1 1 d R . . C74 C 0.6945(7) 0.4879(3) 0.2668(2) 0.0419(14) Uani 1 1 d . . . H74 H 0.6941 0.5230 0.2584 0.036(16) Uiso 1 1 d R . . C75 C 0.6597(8) 0.4494(3) 0.2357(2) 0.0547(19) Uani 1 1 d . . . H75 H 0.6329 0.4575 0.2062 0.042(17) Uiso 1 1 d R . . C76 C 0.6652(8) 0.3988(3) 0.2487(2) 0.0532(18) Uani 1 1 d . . . H76 H 0.6453 0.3721 0.2282 0.07(2) Uiso 1 1 d R . . C77 C 0.6991(7) 0.3860(2) 0.29230(19) 0.0387(13) Uani 1 1 d . . . H77 H 0.6997 0.3508 0.3003 0.034(16) Uiso 1 1 d R . . C78 C 0.9550(6) 0.40446(19) 0.38996(17) 0.0256(11) Uani 1 1 d . . . C79 C 1.0341(6) 0.4132(2) 0.43229(19) 0.0375(13) Uani 1 1 d . . . H79 H 0.9855 0.4274 0.4529 0.032(15) Uiso 1 1 d R . . C80 C 1.1784(7) 0.4023(2) 0.4445(2) 0.0403(14) Uani 1 1 d . . . H80 H 1.2270 0.4091 0.4732 0.040(17) Uiso 1 1 d R . . C81 C 1.2540(6) 0.3808(2) 0.4152(2) 0.0368(13) Uani 1 1 d . . . H81 H 1.3526 0.3717 0.4240 0.029(15) Uiso 1 1 d R . . C82 C 1.1828(6) 0.3730(2) 0.3736(2) 0.0379(13) Uani 1 1 d . . . H82 H 1.2330 0.3595 0.3530 0.08(3) Uiso 1 1 d R . . C83 C 1.0363(6) 0.3848(2) 0.36114(17) 0.0298(11) Uani 1 1 d . . . H83 H 0.9898 0.3799 0.3318 0.041(18) Uiso 1 1 d R . . C84 C 1.459(2) 0.1099(7) 0.4408(5) 0.083(6) Uani 0.568(15) 1 d P A 1 C85 C 1.510(2) 0.1164(10) 0.4840(5) 0.118(9) Uani 0.568(15) 1 d P A 1 H85A H 1.6008 0.1344 0.4885 0.165 Uiso 0.568(15) 1 calc PR A 1 H85B H 1.5239 0.0833 0.4979 0.165 Uiso 0.568(15) 1 calc PR A 1 H85C H 1.4425 0.1362 0.4961 0.165 Uiso 0.568(15) 1 calc PR A 1 C86 C 0.126(2) 0.5529(7) -0.0074(7) 0.078(6) Uani 0.486(14) 1 d P . . C87 C 0.123(3) 0.5354(10) -0.0506(7) 0.102(8) Uani 0.486(14) 1 d P . . H87A H 0.1084 0.4987 -0.0521 0.143 Uiso 0.486(14) 1 calc PR . . H87B H 0.2134 0.5435 -0.0584 0.143 Uiso 0.486(14) 1 calc PR . . H87C H 0.0461 0.5522 -0.0702 0.143 Uiso 0.486(14) 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0296(4) 0.0275(3) 0.0279(3) -0.0034(3) 0.0059(2) -0.0027(3) Cu2 0.0589(5) 0.0325(4) 0.0362(4) 0.0046(3) 0.0203(4) 0.0099(3) B1 0.041(4) 0.033(3) 0.038(4) -0.003(3) 0.012(3) -0.003(3) B2 0.027(3) 0.026(3) 0.027(3) -0.004(2) 0.009(2) -0.002(2) N1 0.053(3) 0.034(3) 0.036(3) -0.003(2) 0.020(2) -0.008(2) N2 0.032(3) 0.040(3) 0.025(2) -0.0015(19) 0.0059(18) -0.004(2) N3 0.035(3) 0.033(2) 0.031(2) 0.0010(19) 0.008(2) 0.003(2) N4 0.040(3) 0.030(2) 0.028(2) 0.0019(18) 0.003(2) 0.000(2) N5 0.033(3) 0.047(3) 0.028(2) -0.003(2) 0.006(2) -0.008(2) N6 0.034(3) 0.036(3) 0.036(3) -0.011(2) 0.008(2) -0.003(2) N7 0.031(2) 0.0118(18) 0.052(3) -0.0115(18) 0.031(2) -0.0009(16) N8 0.045(3) 0.044(3) 0.030(3) -0.001(2) 0.007(2) -0.001(2) N9 0.118(15) 0.25(3) 0.056(10) 0.006(12) 0.013(9) 0.114(16) N10 0.23(3) 0.097(15) 0.073(13) 0.009(11) 0.035(15) 0.086(16) C1 0.052(4) 0.037(3) 0.031(3) 0.004(2) 0.005(3) 0.011(3) C2 0.035(3) 0.049(4) 0.032(3) -0.002(3) 0.002(2) 0.005(3) C3 0.027(3) 0.037(3) 0.034(3) -0.004(2) 0.010(2) 0.002(2) C4 0.032(3) 0.038(3) 0.034(3) -0.005(2) 0.009(2) 0.001(2) C5 0.042(4) 0.046(4) 0.034(3) -0.013(3) 0.010(3) 0.005(3) C6 0.048(4) 0.037(3) 0.023(3) -0.002(2) 0.010(2) 0.006(3) C7 0.054(4) 0.032(3) 0.037(3) -0.005(2) 0.019(3) 0.010(3) C8 0.052(4) 0.028(3) 0.035(3) 0.001(2) 0.014(3) 0.002(3) C9 0.047(4) 0.032(3) 0.031(3) 0.001(2) 0.009(3) 0.005(3) C10 0.060(4) 0.036(3) 0.034(3) -0.006(2) 0.019(3) -0.008(3) C11 0.069(5) 0.051(4) 0.029(3) 0.000(3) 0.019(3) -0.013(3) C12 0.036(3) 0.050(4) 0.032(3) -0.008(3) 0.011(2) -0.007(3) C13 0.055(4) 0.045(4) 0.035(3) 0.003(3) 0.020(3) -0.002(3) C14 0.052(4) 0.071(5) 0.024(3) -0.005(3) 0.014(3) -0.007(3) C15 0.038(4) 0.054(4) 0.041(3) -0.013(3) 0.013(3) -0.009(3) C16 0.031(3) 0.042(3) 0.042(3) -0.004(3) 0.007(3) -0.005(3) C17 0.031(3) 0.043(3) 0.040(3) -0.006(3) 0.001(2) -0.006(3) C18 0.034(3) 0.033(3) 0.033(3) -0.012(2) 0.009(2) -0.008(2) C19 0.040(4) 0.033(3) 0.054(4) -0.007(3) 0.014(3) -0.003(3) C20 0.071(5) 0.032(3) 0.070(5) -0.006(3) 0.019(4) -0.003(3) C21 0.057(5) 0.039(4) 0.058(4) -0.007(3) 0.002(3) 0.008(3) C22 0.037(4) 0.039(3) 0.053(4) -0.014(3) 0.002(3) 0.000(3) C23 0.048(4) 0.039(3) 0.043(4) 0.003(3) 0.016(3) 0.004(3) C24 0.060(4) 0.032(3) 0.032(3) 0.004(2) 0.013(3) 0.006(3) C25 0.073(6) 0.036(3) 0.070(5) 0.007(3) 0.031(4) 0.004(3) C26 0.105(7) 0.030(3) 0.068(5) 0.009(3) 0.032(5) 0.019(4) C27 0.083(6) 0.041(4) 0.075(5) 0.010(4) 0.034(5) 0.026(4) C28 0.072(5) 0.042(4) 0.046(4) 0.017(3) 0.024(4) 0.014(3) C29 0.058(4) 0.039(3) 0.041(4) -0.004(3) 0.005(3) -0.012(3) C30 0.044(4) 0.046(4) 0.032(3) -0.004(3) 0.005(3) -0.006(3) C31 0.050(4) 0.056(4) 0.035(3) -0.010(3) 0.005(3) -0.010(3) C32 0.077(6) 0.080(6) 0.029(4) -0.012(3) 0.002(3) -0.028(4) C33 0.070(5) 0.080(6) 0.036(4) 0.004(4) 0.001(3) -0.016(4) C34 0.056(4) 0.055(4) 0.037(4) 0.002(3) 0.005(3) -0.009(3) C36 0.051(4) 0.031(3) 0.043(3) -0.009(3) 0.017(3) -0.007(3) C37 0.056(4) 0.046(4) 0.050(4) -0.009(3) 0.020(3) -0.005(3) C38 0.059(5) 0.058(4) 0.055(4) -0.019(4) 0.027(4) -0.022(4) C39 0.086(6) 0.041(4) 0.067(5) -0.004(4) 0.042(5) -0.022(4) C40 0.091(7) 0.046(4) 0.057(5) 0.007(4) 0.031(4) -0.002(4) C41 0.059(5) 0.037(3) 0.045(4) -0.002(3) 0.013(3) -0.003(3) C42 0.050(4) 0.032(3) 0.028(3) 0.003(2) 0.003(3) 0.001(3) C43 0.043(4) 0.040(3) 0.041(3) -0.007(3) 0.001(3) 0.001(3) C44 0.048(4) 0.058(4) 0.044(4) -0.009(3) 0.003(3) 0.010(3) C45 0.088(6) 0.041(4) 0.043(4) -0.006(3) 0.013(4) 0.018(4) C46 0.117(8) 0.028(3) 0.053(4) -0.004(3) 0.018(5) -0.006(4) C47 0.078(5) 0.036(3) 0.045(4) -0.005(3) 0.022(4) -0.006(3) C48 0.044(4) 0.027(3) 0.052(4) 0.002(3) 0.011(3) -0.006(3) C49 0.045(4) 0.058(4) 0.061(5) -0.014(4) 0.003(3) 0.001(3) C50 0.051(5) 0.073(6) 0.097(7) -0.016(5) 0.004(5) -0.007(4) C51 0.042(5) 0.061(5) 0.111(8) -0.005(5) 0.019(5) -0.007(4) C52 0.057(5) 0.038(4) 0.098(7) 0.000(4) 0.034(5) -0.001(3) C53 0.055(4) 0.027(3) 0.065(5) 0.004(3) 0.023(4) -0.002(3) C54 0.042(4) 0.036(3) 0.039(3) -0.004(2) 0.010(3) 0.003(3) C55 0.057(4) 0.039(3) 0.038(3) -0.003(3) 0.011(3) -0.002(3) C56 0.061(5) 0.052(4) 0.044(4) -0.007(3) 0.012(3) -0.002(3) C57 0.049(4) 0.058(4) 0.039(4) 0.006(3) 0.011(3) 0.007(3) C58 0.043(4) 0.039(3) 0.051(4) 0.004(3) 0.017(3) 0.000(3) C59 0.043(4) 0.042(3) 0.040(3) -0.005(3) 0.012(3) -0.007(3) C60 0.025(3) 0.029(3) 0.024(3) 0.002(2) 0.001(2) 0.002(2) C61 0.034(3) 0.029(3) 0.035(3) -0.001(2) 0.011(2) -0.001(2) C62 0.040(3) 0.039(3) 0.033(3) -0.001(2) 0.013(3) 0.007(3) C63 0.046(4) 0.035(3) 0.035(3) -0.008(2) 0.005(3) 0.014(3) C64 0.057(4) 0.033(3) 0.046(4) -0.019(3) 0.010(3) -0.009(3) C65 0.038(3) 0.035(3) 0.049(4) -0.009(3) 0.015(3) -0.003(3) C66 0.030(3) 0.028(3) 0.033(3) -0.009(2) 0.012(2) 0.004(2) C67 0.043(3) 0.032(3) 0.028(3) -0.006(2) 0.011(2) -0.004(2) C68 0.075(5) 0.033(3) 0.034(3) 0.002(3) 0.020(3) 0.004(3) C69 0.068(5) 0.030(3) 0.056(4) -0.006(3) 0.041(4) -0.010(3) C70 0.037(3) 0.034(3) 0.056(4) -0.016(3) 0.022(3) -0.006(3) C71 0.033(3) 0.030(3) 0.045(3) -0.005(2) 0.013(3) 0.003(2) C72 0.019(2) 0.032(3) 0.029(3) 0.000(2) 0.003(2) 0.002(2) C73 0.026(3) 0.036(3) 0.036(3) -0.002(2) 0.007(2) -0.002(2) C74 0.036(3) 0.047(4) 0.044(4) 0.014(3) 0.012(3) 0.005(3) C75 0.043(4) 0.084(5) 0.034(4) 0.017(3) -0.001(3) -0.011(4) C76 0.056(4) 0.067(5) 0.034(3) -0.013(3) 0.003(3) -0.016(4) C77 0.046(4) 0.034(3) 0.034(3) -0.002(2) 0.003(3) -0.005(3) C78 0.024(3) 0.025(3) 0.029(3) 0.002(2) 0.009(2) -0.0003(19) C79 0.034(3) 0.045(3) 0.034(3) -0.005(3) 0.009(2) 0.000(3) C80 0.038(3) 0.044(3) 0.036(3) -0.003(3) 0.000(3) -0.004(3) C81 0.024(3) 0.040(3) 0.046(3) 0.006(3) 0.004(2) 0.000(2) C82 0.030(3) 0.043(3) 0.046(3) 0.006(3) 0.019(3) 0.003(2) C83 0.031(3) 0.035(3) 0.025(3) 0.003(2) 0.010(2) 0.001(2) C84 0.108(15) 0.097(13) 0.052(9) -0.005(8) 0.038(9) 0.029(10) C85 0.097(15) 0.21(3) 0.039(9) -0.012(12) 0.007(9) -0.022(16) C86 0.102(17) 0.062(11) 0.073(13) 0.010(10) 0.024(11) 0.017(10) C87 0.103(19) 0.14(2) 0.069(14) 0.001(13) 0.023(12) 0.001(15) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1B Cu1 O2A 44.4(7) . . ? O1B Cu1 N6 94.3(6) . . ? O2A Cu1 N6 93.1(2) . . ? O1B Cu1 N2 121.7(7) . . ? O2A Cu1 N2 165.47(19) . . ? N6 Cu1 N2 83.05(19) . . ? O1B Cu1 N1 94.2(6) . . ? O2A Cu1 N1 98.7(2) . . ? N6 Cu1 N1 168.2(2) . . ? N2 Cu1 N1 85.6(2) . . ? O1B Cu1 N5 140.3(7) . . ? O2A Cu1 N5 97.05(19) . . ? N6 Cu1 N5 97.56(19) . . ? N2 Cu1 N5 97.35(18) . . ? N1 Cu1 N5 80.88(19) . . ? O1A Cu2 O2B 43.7(5) . . ? O1A Cu2 N7 89.1(2) . . ? O2B Cu2 N7 91.6(5) . . ? O1A Cu2 N4 97.2(2) . . ? O2B Cu2 N4 100.9(5) . . ? N7 Cu2 N4 166.87(19) . . ? O1A Cu2 N8 149.5(2) . . ? O2B Cu2 N8 106.2(5) . . ? N7 Cu2 N8 97.8(2) . . ? N4 Cu2 N8 82.51(19) . . ? O1A Cu2 N3 112.6(2) . . ? O2B Cu2 N3 155.8(5) . . ? N7 Cu2 N3 81.92(17) . . ? N4 Cu2 N3 85.02(18) . . ? N8 Cu2 N3 97.77(19) . . ? C42 B1 C54 111.1(5) . . ? C42 B1 C36 108.1(5) . . ? C54 B1 C36 112.6(5) . . ? C42 B1 C48 110.3(5) . . ? C54 B1 C48 107.7(5) . . ? C36 B1 C48 106.9(5) . . ? C72 B2 C78 108.5(4) . . ? C72 B2 C66 113.1(4) . . ? C78 B2 C66 108.0(4) . . ? C72 B2 C60 109.8(4) . . ? C78 B2 C60 109.9(4) . . ? C66 B2 C60 107.6(4) . . ? C10 N1 C11 106.9(5) . . ? C10 N1 C1 112.5(5) . . ? C11 N1 C1 111.0(5) . . ? C10 N1 Cu1 114.4(4) . . ? C11 N1 Cu1 105.0(4) . . ? C1 N1 Cu1 106.8(3) . . ? C3 N2 C2 108.7(4) . . ? C3 N2 C17 109.9(4) . . ? C2 N2 C17 112.2(4) . . ? C3 N2 Cu1 118.1(3) . . ? C2 N2 Cu1 103.8(3) . . ? C17 N2 Cu1 104.0(3) . . ? C23 N3 C6 114.6(5) . . ? C23 N3 C5 110.3(5) . . ? C6 N3 C5 108.7(4) . . ? C23 N3 Cu2 102.6(4) . . ? C6 N3 Cu2 98.8(3) . . ? C5 N3 Cu2 121.6(4) . . ? C29 N4 C8 106.9(5) . . ? C29 N4 C7 109.8(5) . . ? C8 N4 C7 112.3(5) . . ? C29 N4 Cu2 104.9(4) . . ? C8 N4 Cu2 115.3(3) . . ? C7 N4 Cu2 107.3(3) . . ? C16 N5 C12 117.6(5) . . ? C16 N5 Cu1 131.4(4) . . ? C12 N5 Cu1 110.0(4) . . ? C22 N6 C18 118.9(5) . . ? C22 N6 Cu1 127.4(4) . . ? C18 N6 Cu1 113.5(4) . . ? C28 N7 C24 112.8(5) . . ? C28 N7 Cu2 129.9(4) . . ? C24 N7 Cu2 116.5(3) . . ? C34 N8 C30 118.3(6) . . ? C34 N8 Cu2 130.3(5) . . ? C30 N8 Cu2 111.4(4) . . ? C35A O1A Cu2 135.8(7) . . ? C35B O1B Cu1 137.8(15) . . ? C35A O2A Cu1 114.2(5) . . ? C35B O2B Cu2 121.1(11) . . ? C2 C1 N1 113.3(5) . . ? N2 C2 C1 109.3(5) . . ? N2 C3 C4 114.6(5) . . ? C3 C4 C5 110.0(5) . . ? N3 C5 C4 114.2(5) . . ? N3 C6 C7 111.6(4) . . ? N4 C7 C6 114.5(5) . . ? N4 C8 C9 114.5(5) . . ? C8 C9 C10 110.3(5) . . ? N1 C10 C9 115.0(5) . . ? C12 C11 N1 112.5(5) . . ? N5 C12 C13 122.4(6) . . ? N5 C12 C11 114.9(5) . . ? C13 C12 C11 122.7(6) . . ? C12 C13 C14 118.2(6) . . ? C15 C14 C13 119.4(6) . . ? C16 C15 C14 118.9(6) . . ? N5 C16 C15 123.5(6) . . ? C18 C17 N2 109.7(5) . . ? N6 C18 C19 120.0(6) . . ? N6 C18 C17 114.7(5) . . ? C19 C18 C17 125.3(5) . . ? C20 C19 C18 120.3(6) . . ? C19 C20 C21 118.5(7) . . ? C22 C21 C20 118.3(7) . . ? N6 C22 C21 123.7(7) . . ? N3 C23 C24 112.8(5) . . ? C25 C24 N7 123.5(6) . . ? C25 C24 C23 122.5(6) . . ? N7 C24 C23 114.0(5) . . ? C24 C25 C26 117.9(7) . . ? C27 C26 C25 119.9(7) . . ? C26 C27 C28 119.1(7) . . ? N7 C28 C27 125.6(7) . . ? N4 C29 C30 113.5(5) . . ? N8 C30 C31 122.1(6) . . ? N8 C30 C29 115.6(5) . . ? C31 C30 C29 122.2(6) . . ? C32 C31 C30 118.1(7) . . ? C31 C32 C33 120.9(7) . . ? C34 C33 C32 117.1(7) . . ? N8 C34 C33 123.5(7) . . ? O3A C35A O2A 122.7(9) . . ? O3A C35A O1A 121.7(11) . . ? O2A C35A O1A 115.6(9) . . ? O3B C35B O2B 123.1(13) . . ? O3B C35B O1B 125.7(14) . . ? O2B C35B O1B 111.2(13) . . ? C41 C36 C37 114.5(4) . . ? C41 C36 B1 122.4(5) . . ? C37 C36 B1 122.8(3) . . ? C38 C37 C36 122.0(4) . . ? C39 C38 C37 120.1(7) . . ? C40 C39 C38 119.4(7) . . ? C39 C40 C41 121.4(8) . . ? C40 C41 C36 122.5(7) . . ? C43 C42 C47 113.8(6) . . ? C43 C42 B1 122.8(5) . . ? C47 C42 B1 123.4(6) . . ? C42 C43 C44 124.2(6) . . ? C45 C44 C43 119.0(7) . . ? C46 C45 C44 118.4(7) . . ? C45 C46 C47 121.4(7) . . ? C46 C47 C42 123.2(7) . . ? C49 C48 C53 116.4(7) . . ? C49 C48 B1 121.6(6) . . ? C53 C48 B1 121.7(6) . . ? C48 C49 C50 121.1(8) . . ? C51 C50 C49 119.9(9) . . ? C52 C51 C50 120.5(9) . . ? C51 C52 C53 120.1(8) . . ? C52 C53 C48 121.8(8) . . ? C59 C54 C55 113.6(6) . . ? C59 C54 B1 120.8(5) . . ? C55 C54 B1 125.3(5) . . ? C56 C55 C54 123.2(6) . . ? C57 C56 C55 120.7(7) . . ? C56 C57 C58 118.4(6) . . ? C57 C58 C59 120.2(6) . . ? C58 C59 C54 123.8(6) . . ? C65 C60 C61 114.4(5) . . ? C65 C60 B2 122.7(5) . . ? C61 C60 B2 122.8(5) . . ? C60 C61 C62 123.6(5) . . ? C63 C62 C61 119.6(6) . . ? C64 C63 C62 119.3(5) . . ? C63 C64 C65 119.8(6) . . ? C60 C65 C64 123.2(6) . . ? C67 C66 C71 114.9(5) . . ? C67 C66 B2 122.4(5) . . ? C71 C66 B2 122.5(5) . . ? C68 C67 C66 122.3(6) . . ? C69 C68 C67 121.1(6) . . ? C68 C69 C70 119.2(6) . . ? C69 C70 C71 119.5(6) . . ? C70 C71 C66 123.0(6) . . ? C77 C72 C73 113.6(5) . . ? C77 C72 B2 123.9(5) . . ? C73 C72 B2 122.5(5) . . ? C74 C73 C72 124.0(5) . . ? C73 C74 C75 119.5(6) . . ? C76 C75 C74 118.9(6) . . ? C75 C76 C77 120.9(6) . . ? C76 C77 C72 123.1(6) . . ? C83 C78 C79 114.7(5) . . ? C83 C78 B2 121.7(5) . . ? C79 C78 B2 123.0(5) . . ? C80 C79 C78 122.6(5) . . ? C79 C80 C81 120.8(6) . . ? C82 C81 C80 118.6(6) . . ? C81 C82 C83 120.5(5) . . ? C82 C83 C78 122.8(5) . . ? N9 C84 C85 174(3) . . ? N10 C86 C87 179(2) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1B 1.85(2) . ? Cu1 O2A 1.950(5) . ? Cu1 N6 1.997(5) . ? Cu1 N2 2.068(5) . ? Cu1 N1 2.078(5) . ? Cu1 N5 2.217(5) . ? Cu2 O1A 1.876(6) . ? Cu2 O2B 1.909(17) . ? Cu2 N7 1.922(4) . ? Cu2 N4 2.073(5) . ? Cu2 N8 2.091(5) . ? Cu2 N3 2.225(5) . ? B1 C42 1.640(9) . ? B1 C54 1.646(9) . ? B1 C36 1.654(8) . ? B1 C48 1.657(10) . ? B2 C72 1.635(8) . ? B2 C78 1.645(8) . ? B2 C66 1.647(8) . ? B2 C60 1.658(8) . ? N1 C10 1.499(8) . ? N1 C11 1.505(7) . ? N1 C1 1.516(8) . ? N2 C3 1.489(7) . ? N2 C2 1.495(7) . ? N2 C17 1.507(7) . ? N3 C23 1.459(8) . ? N3 C6 1.477(7) . ? N3 C5 1.495(8) . ? N4 C29 1.470(8) . ? N4 C8 1.497(7) . ? N4 C7 1.513(8) . ? N5 C16 1.342(8) . ? N5 C12 1.352(8) . ? N6 C22 1.328(8) . ? N6 C18 1.367(7) . ? N7 C28 1.362(8) . ? N7 C24 1.426(7) . ? N8 C34 1.315(8) . ? N8 C30 1.359(8) . ? N9 C84 1.13(2) . ? N10 C86 1.13(2) . ? O1A C35A 1.317(11) . ? O1B C35B 1.30(2) . ? O2A C35A 1.279(14) . ? O2B C35B 1.268(17) . ? O3A C35A 1.271(12) . ? O3B C35B 1.26(2) . ? C1 C2 1.503(9) . ? C3 C4 1.522(8) . ? C4 C5 1.524(7) . ? C6 C7 1.514(8) . ? C8 C9 1.513(9) . ? C9 C10 1.526(8) . ? C11 C12 1.489(9) . ? C12 C13 1.389(8) . ? C13 C14 1.392(9) . ? C14 C15 1.374(10) . ? C15 C16 1.365(9) . ? C17 C18 1.486(9) . ? C18 C19 1.388(8) . ? C19 C20 1.365(10) . ? C20 C21 1.411(11) . ? C21 C22 1.352(10) . ? C23 C24 1.505(9) . ? C24 C25 1.376(9) . ? C25 C26 1.410(11) . ? C26 C27 1.356(12) . ? C27 C28 1.378(10) . ? C29 C30 1.505(9) . ? C30 C31 1.398(8) . ? C31 C32 1.350(10) . ? C32 C33 1.399(11) . ? C33 C34 1.391(10) . ? C36 C41 1.398(8) . ? C36 C37 1.4091 . ? C37 C38 1.407(8) . ? C38 C39 1.373(12) . ? C39 C40 1.336(12) . ? C40 C41 1.396(10) . ? C42 C43 1.385(9) . ? C42 C47 1.390(9) . ? C43 C44 1.407(9) . ? C44 C45 1.382(11) . ? C45 C46 1.357(12) . ? C46 C47 1.389(10) . ? C48 C49 1.402(10) . ? C48 C53 1.410(9) . ? C49 C50 1.406(11) . ? C50 C51 1.377(13) . ? C51 C52 1.360(13) . ? C52 C53 1.392(11) . ? C54 C59 1.404(9) . ? C54 C55 1.405(9) . ? C55 C56 1.393(9) . ? C56 C57 1.372(10) . ? C57 C58 1.383(9) . ? C58 C59 1.384(9) . ? C60 C65 1.384(8) . ? C60 C61 1.392(8) . ? C61 C62 1.398(8) . ? C62 C63 1.377(9) . ? C63 C64 1.363(9) . ? C64 C65 1.413(8) . ? C66 C67 1.394(8) . ? C66 C71 1.406(8) . ? C67 C68 1.393(8) . ? C68 C69 1.364(10) . ? C69 C70 1.379(10) . ? C70 C71 1.396(8) . ? C72 C77 1.410(8) . ? C72 C73 1.416(8) . ? C73 C74 1.383(8) . ? C74 C75 1.393(10) . ? C75 C76 1.372(10) . ? C76 C77 1.389(9) . ? C78 C83 1.403(7) . ? C78 C79 1.412(8) . ? C79 C80 1.371(9) . ? C80 C81 1.397(9) . ? C81 C82 1.364(9) . ? C82 C83 1.397(8) . ? C84 C85 1.36(2) . ? C86 C87 1.43(3) . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1B Cu1 N1 C10 -4.2(8) . . . . ? O2A Cu1 N1 C10 -48.7(4) . . . . ? N6 Cu1 N1 C10 132.3(9) . . . . ? N2 Cu1 N1 C10 117.3(4) . . . . ? N5 Cu1 N1 C10 -144.5(4) . . . . ? O1B Cu1 N1 C11 112.7(8) . . . . ? O2A Cu1 N1 C11 68.3(4) . . . . ? N6 Cu1 N1 C11 -110.8(9) . . . . ? N2 Cu1 N1 C11 -125.7(4) . . . . ? N5 Cu1 N1 C11 -27.5(4) . . . . ? O1B Cu1 N1 C1 -129.4(7) . . . . ? O2A Cu1 N1 C1 -173.8(4) . . . . ? N6 Cu1 N1 C1 7.1(11) . . . . ? N2 Cu1 N1 C1 -7.8(3) . . . . ? N5 Cu1 N1 C1 90.4(4) . . . . ? O1B Cu1 N2 C3 2.7(9) . . . . ? O2A Cu1 N2 C3 18.2(10) . . . . ? N6 Cu1 N2 C3 93.5(4) . . . . ? N1 Cu1 N2 C3 -89.5(4) . . . . ? N5 Cu1 N2 C3 -169.7(4) . . . . ? O1B Cu1 N2 C2 123.1(8) . . . . ? O2A Cu1 N2 C2 138.5(7) . . . . ? N6 Cu1 N2 C2 -146.1(4) . . . . ? N1 Cu1 N2 C2 30.9(3) . . . . ? N5 Cu1 N2 C2 -49.3(4) . . . . ? O1B Cu1 N2 C17 -119.4(8) . . . . ? O2A Cu1 N2 C17 -103.9(8) . . . . ? N6 Cu1 N2 C17 -28.5(3) . . . . ? N1 Cu1 N2 C17 148.4(4) . . . . ? N5 Cu1 N2 C17 68.2(4) . . . . ? O1A Cu2 N3 C23 113.8(4) . . . . ? O2B Cu2 N3 C23 103.9(13) . . . . ? N7 Cu2 N3 C23 28.2(4) . . . . ? N4 Cu2 N3 C23 -150.4(4) . . . . ? N8 Cu2 N3 C23 -68.7(4) . . . . ? O1A Cu2 N3 C6 -128.4(3) . . . . ? O2B Cu2 N3 C6 -138.3(12) . . . . ? N7 Cu2 N3 C6 146.0(3) . . . . ? N4 Cu2 N3 C6 -32.6(3) . . . . ? N8 Cu2 N3 C6 49.1(3) . . . . ? O1A Cu2 N3 C5 -9.9(5) . . . . ? O2B Cu2 N3 C5 -19.7(13) . . . . ? N7 Cu2 N3 C5 -95.5(4) . . . . ? N4 Cu2 N3 C5 85.9(4) . . . . ? N8 Cu2 N3 C5 167.6(4) . . . . ? O1A Cu2 N4 C29 -120.8(4) . . . . ? O2B Cu2 N4 C29 -76.7(6) . . . . ? N7 Cu2 N4 C29 120.7(9) . . . . ? N8 Cu2 N4 C29 28.4(4) . . . . ? N3 Cu2 N4 C29 127.0(4) . . . . ? O1A Cu2 N4 C8 -3.5(4) . . . . ? O2B Cu2 N4 C8 40.6(7) . . . . ? N7 Cu2 N4 C8 -121.9(9) . . . . ? N8 Cu2 N4 C8 145.8(4) . . . . ? N3 Cu2 N4 C8 -115.7(4) . . . . ? O1A Cu2 N4 C7 122.5(4) . . . . ? O2B Cu2 N4 C7 166.6(6) . . . . ? N7 Cu2 N4 C7 4.0(11) . . . . ? N8 Cu2 N4 C7 -88.3(4) . . . . ? N3 Cu2 N4 C7 10.3(4) . . . . ? O1B Cu1 N5 C16 114.8(11) . . . . ? O2A Cu1 N5 C16 102.8(5) . . . . ? N6 Cu1 N5 C16 8.7(6) . . . . ? N2 Cu1 N5 C16 -75.3(6) . . . . ? N1 Cu1 N5 C16 -159.5(6) . . . . ? O1B Cu1 N5 C12 -76.9(11) . . . . ? O2A Cu1 N5 C12 -89.0(4) . . . . ? N6 Cu1 N5 C12 176.9(4) . . . . ? N2 Cu1 N5 C12 93.0(4) . . . . ? N1 Cu1 N5 C12 8.7(4) . . . . ? O1B Cu1 N6 C22 -41.9(8) . . . . ? O2A Cu1 N6 C22 2.6(5) . . . . ? N2 Cu1 N6 C22 -163.3(5) . . . . ? N1 Cu1 N6 C22 -178(31) . . . . ? N5 Cu1 N6 C22 100.1(5) . . . . ? O1B Cu1 N6 C18 132.9(8) . . . . ? O2A Cu1 N6 C18 177.3(4) . . . . ? N2 Cu1 N6 C18 11.4(4) . . . . ? N1 Cu1 N6 C18 -3.6(11) . . . . ? N5 Cu1 N6 C18 -85.2(4) . . . . ? O1A Cu2 N7 C28 63.5(6) . . . . ? O2B Cu2 N7 C28 19.9(8) . . . . ? N4 Cu2 N7 C28 -177.2(7) . . . . ? N8 Cu2 N7 C28 -86.7(6) . . . . ? N3 Cu2 N7 C28 176.5(6) . . . . ? O1A Cu2 N7 C24 -128.0(4) . . . . ? O2B Cu2 N7 C24 -171.6(7) . . . . ? N4 Cu2 N7 C24 -8.8(11) . . . . ? N8 Cu2 N7 C24 81.7(4) . . . . ? N3 Cu2 N7 C24 -15.1(4) . . . . ? O1A Cu2 N8 C34 -102.9(7) . . . . ? O2B Cu2 N8 C34 -95.2(8) . . . . ? N7 Cu2 N8 C34 -1.2(6) . . . . ? N4 Cu2 N8 C34 165.6(6) . . . . ? N3 Cu2 N8 C34 81.7(6) . . . . ? O1A Cu2 N8 C30 75.3(6) . . . . ? O2B Cu2 N8 C30 83.0(7) . . . . ? N7 Cu2 N8 C30 177.0(4) . . . . ? N4 Cu2 N8 C30 -16.3(4) . . . . ? N3 Cu2 N8 C30 -100.2(4) . . . . ? O2B Cu2 O1A C35A 15.0(10) . . . . ? N7 Cu2 O1A C35A -78.2(8) . . . . ? N4 Cu2 O1A C35A 113.3(8) . . . . ? N8 Cu2 O1A C35A 25.8(10) . . . . ? N3 Cu2 O1A C35A -159.1(7) . . . . ? O2A Cu1 O1B C35B -14.8(15) . . . . ? N6 Cu1 O1B C35B 75(2) . . . . ? N2 Cu1 O1B C35B 159.7(17) . . . . ? N1 Cu1 O1B C35B -113(2) . . . . ? N5 Cu1 O1B C35B -32(3) . . . . ? O1B Cu1 O2A C35A 11.4(10) . . . . ? N6 Cu1 O2A C35A -81.7(5) . . . . ? N2 Cu1 O2A C35A -7.5(11) . . . . ? N1 Cu1 O2A C35A 98.5(5) . . . . ? N5 Cu1 O2A C35A -179.7(5) . . . . ? O1A Cu2 O2B C35B -10.6(7) . . . . ? N7 Cu2 O2B C35B 76.5(12) . . . . ? N4 Cu2 O2B C35B -99.6(12) . . . . ? N8 Cu2 O2B C35B 175.1(11) . . . . ? N3 Cu2 O2B C35B 3(2) . . . . ? C10 N1 C1 C2 -144.1(5) . . . . ? C11 N1 C1 C2 96.1(6) . . . . ? Cu1 N1 C1 C2 -17.8(6) . . . . ? C3 N2 C2 C1 78.1(6) . . . . ? C17 N2 C2 C1 -160.0(5) . . . . ? Cu1 N2 C2 C1 -48.4(5) . . . . ? N1 C1 C2 N2 45.7(7) . . . . ? C2 N2 C3 C4 -158.0(5) . . . . ? C17 N2 C3 C4 78.7(6) . . . . ? Cu1 N2 C3 C4 -40.3(6) . . . . ? N2 C3 C4 C5 154.0(5) . . . . ? C23 N3 C5 C4 -79.5(6) . . . . ? C6 N3 C5 C4 154.1(5) . . . . ? Cu2 N3 C5 C4 40.6(7) . . . . ? C3 C4 C5 N3 -149.8(5) . . . . ? C23 N3 C6 C7 157.8(5) . . . . ? C5 N3 C6 C7 -78.3(6) . . . . ? Cu2 N3 C6 C7 49.5(5) . . . . ? C29 N4 C7 C6 -98.4(6) . . . . ? C8 N4 C7 C6 142.8(5) . . . . ? Cu2 N4 C7 C6 15.0(6) . . . . ? N3 C6 C7 N4 -47.7(7) . . . . ? C29 N4 C8 C9 179.8(5) . . . . ? C7 N4 C8 C9 -59.7(6) . . . . ? Cu2 N4 C8 C9 63.6(6) . . . . ? N4 C8 C9 C10 -148.3(5) . . . . ? C11 N1 C10 C9 -178.6(6) . . . . ? C1 N1 C10 C9 59.3(7) . . . . ? Cu1 N1 C10 C9 -62.8(7) . . . . ? C8 C9 C10 N1 153.2(5) . . . . ? C10 N1 C11 C12 166.3(6) . . . . ? C1 N1 C11 C12 -70.8(7) . . . . ? Cu1 N1 C11 C12 44.3(7) . . . . ? C16 N5 C12 C13 1.7(9) . . . . ? Cu1 N5 C12 C13 -168.4(5) . . . . ? C16 N5 C12 C11 -176.0(6) . . . . ? Cu1 N5 C12 C11 13.9(7) . . . . ? N1 C11 C12 N5 -40.2(8) . . . . ? N1 C11 C12 C13 142.2(6) . . . . ? N5 C12 C13 C14 -1.2(10) . . . . ? C11 C12 C13 C14 176.3(7) . . . . ? C12 C13 C14 C15 -0.3(10) . . . . ? C13 C14 C15 C16 1.0(10) . . . . ? C12 N5 C16 C15 -0.9(9) . . . . ? Cu1 N5 C16 C15 166.7(5) . . . . ? C14 C15 C16 N5 -0.5(10) . . . . ? C3 N2 C17 C18 -86.4(6) . . . . ? C2 N2 C17 C18 152.5(5) . . . . ? Cu1 N2 C17 C18 41.0(5) . . . . ? C22 N6 C18 C19 4.6(8) . . . . ? Cu1 N6 C18 C19 -170.7(4) . . . . ? C22 N6 C18 C17 -174.6(5) . . . . ? Cu1 N6 C18 C17 10.2(6) . . . . ? N2 C17 C18 N6 -35.5(7) . . . . ? N2 C17 C18 C19 145.4(6) . . . . ? N6 C18 C19 C20 -3.4(9) . . . . ? C17 C18 C19 C20 175.6(6) . . . . ? C18 C19 C20 C21 -0.4(10) . . . . ? C19 C20 C21 C22 3.0(11) . . . . ? C18 N6 C22 C21 -1.9(9) . . . . ? Cu1 N6 C22 C21 172.6(5) . . . . ? C20 C21 C22 N6 -1.9(11) . . . . ? C6 N3 C23 C24 -142.3(6) . . . . ? C5 N3 C23 C24 94.7(6) . . . . ? Cu2 N3 C23 C24 -36.3(6) . . . . ? C28 N7 C24 C25 -13.2(9) . . . . ? Cu2 N7 C24 C25 176.3(6) . . . . ? C28 N7 C24 C23 168.7(6) . . . . ? Cu2 N7 C24 C23 -1.7(7) . . . . ? N3 C23 C24 C25 -149.5(7) . . . . ? N3 C23 C24 N7 28.5(8) . . . . ? N7 C24 C25 C26 9.9(11) . . . . ? C23 C24 C25 C26 -172.2(7) . . . . ? C24 C25 C26 C27 -2.7(12) . . . . ? C25 C26 C27 C28 0.0(13) . . . . ? C24 N7 C28 C27 10.5(10) . . . . ? Cu2 N7 C28 C27 179.3(6) . . . . ? C26 C27 C28 N7 -4.5(13) . . . . ? C8 N4 C29 C30 -160.1(5) . . . . ? C7 N4 C29 C30 77.8(7) . . . . ? Cu2 N4 C29 C30 -37.2(6) . . . . ? C34 N8 C30 C31 1.3(10) . . . . ? Cu2 N8 C30 C31 -177.1(5) . . . . ? C34 N8 C30 C29 177.8(6) . . . . ? Cu2 N8 C30 C29 -0.6(7) . . . . ? N4 C29 C30 N8 26.5(9) . . . . ? N4 C29 C30 C31 -157.0(6) . . . . ? N8 C30 C31 C32 1.0(11) . . . . ? C29 C30 C31 C32 -175.3(7) . . . . ? C30 C31 C32 C33 -2.3(12) . . . . ? C31 C32 C33 C34 1.4(13) . . . . ? C30 N8 C34 C33 -2.4(11) . . . . ? Cu2 N8 C34 C33 175.7(6) . . . . ? C32 C33 C34 N8 1.0(12) . . . . ? Cu1 O2A C35A O3A 167.2(7) . . . . ? Cu1 O2A C35A O1A -13.9(9) . . . . ? Cu2 O1A C35A O3A -3.8(13) . . . . ? Cu2 O1A C35A O2A 177.2(5) . . . . ? Cu2 O2B C35B O3B -159.1(12) . . . . ? Cu2 O2B C35B O1B 19.5(17) . . . . ? Cu1 O1B C35B O3B 5(3) . . . . ? Cu1 O1B C35B O2B -174.0(18) . . . . ? C42 B1 C36 C41 88.8(6) . . . . ? C54 B1 C36 C41 -148.1(5) . . . . ? C48 B1 C36 C41 -30.0(7) . . . . ? C42 B1 C36 C37 -84.4(5) . . . . ? C54 B1 C36 C37 38.7(6) . . . . ? C48 B1 C36 C37 156.8(3) . . . . ? C41 C36 C37 C38 -0.3(4) . . . . ? B1 C36 C37 C38 173.3(6) . . . . ? C36 C37 C38 C39 -0.7(8) . . . . ? C37 C38 C39 C40 0.4(11) . . . . ? C38 C39 C40 C41 0.9(12) . . . . ? C39 C40 C41 C36 -2.0(11) . . . . ? C37 C36 C41 C40 1.7(7) . . . . ? B1 C36 C41 C40 -172.0(6) . . . . ? C54 B1 C42 C43 -99.8(7) . . . . ? C36 B1 C42 C43 24.2(8) . . . . ? C48 B1 C42 C43 140.9(6) . . . . ? C54 B1 C42 C47 80.0(8) . . . . ? C36 B1 C42 C47 -156.0(6) . . . . ? C48 B1 C42 C47 -39.4(8) . . . . ? C47 C42 C43 C44 -0.6(9) . . . . ? B1 C42 C43 C44 179.2(6) . . . . ? C42 C43 C44 C45 0.9(11) . . . . ? C43 C44 C45 C46 -1.1(11) . . . . ? C44 C45 C46 C47 1.1(12) . . . . ? C45 C46 C47 C42 -0.9(13) . . . . ? C43 C42 C47 C46 0.6(10) . . . . ? B1 C42 C47 C46 -179.2(7) . . . . ? C42 B1 C48 C49 -33.1(8) . . . . ? C54 B1 C48 C49 -154.5(6) . . . . ? C36 B1 C48 C49 84.2(7) . . . . ? C42 B1 C48 C53 152.5(5) . . . . ? C54 B1 C48 C53 31.1(7) . . . . ? C36 B1 C48 C53 -90.2(6) . . . . ? C53 C48 C49 C50 2.0(10) . . . . ? B1 C48 C49 C50 -172.7(7) . . . . ? C48 C49 C50 C51 -0.2(13) . . . . ? C49 C50 C51 C52 -0.5(13) . . . . ? C50 C51 C52 C53 -0.6(12) . . . . ? C51 C52 C53 C48 2.5(10) . . . . ? C49 C48 C53 C52 -3.1(9) . . . . ? B1 C48 C53 C52 171.6(6) . . . . ? C42 B1 C54 C59 -41.1(8) . . . . ? C36 B1 C54 C59 -162.5(5) . . . . ? C48 B1 C54 C59 79.8(7) . . . . ? C42 B1 C54 C55 145.0(6) . . . . ? C36 B1 C54 C55 23.6(9) . . . . ? C48 B1 C54 C55 -94.1(7) . . . . ? C59 C54 C55 C56 -0.2(10) . . . . ? B1 C54 C55 C56 174.1(6) . . . . ? C54 C55 C56 C57 -0.6(11) . . . . ? C55 C56 C57 C58 -0.6(11) . . . . ? C56 C57 C58 C59 2.6(10) . . . . ? C57 C58 C59 C54 -3.7(10) . . . . ? C55 C54 C59 C58 2.3(10) . . . . ? B1 C54 C59 C58 -172.3(6) . . . . ? C72 B2 C60 C65 -81.8(6) . . . . ? C78 B2 C60 C65 37.4(7) . . . . ? C66 B2 C60 C65 154.7(5) . . . . ? C72 B2 C60 C61 96.0(6) . . . . ? C78 B2 C60 C61 -144.8(5) . . . . ? C66 B2 C60 C61 -27.5(7) . . . . ? C65 C60 C61 C62 -0.3(8) . . . . ? B2 C60 C61 C62 -178.3(5) . . . . ? C60 C61 C62 C63 1.6(9) . . . . ? C61 C62 C63 C64 -2.1(9) . . . . ? C62 C63 C64 C65 1.4(10) . . . . ? C61 C60 C65 C64 -0.3(9) . . . . ? B2 C60 C65 C64 177.6(6) . . . . ? C63 C64 C65 C60 -0.2(10) . . . . ? C72 B2 C66 C67 145.9(5) . . . . ? C78 B2 C66 C67 25.9(6) . . . . ? C60 B2 C66 C67 -92.6(6) . . . . ? C72 B2 C66 C71 -39.2(7) . . . . ? C78 B2 C66 C71 -159.2(5) . . . . ? C60 B2 C66 C71 82.3(6) . . . . ? C71 C66 C67 C68 -2.9(8) . . . . ? B2 C66 C67 C68 172.4(5) . . . . ? C66 C67 C68 C69 1.9(9) . . . . ? C67 C68 C69 C70 0.4(9) . . . . ? C68 C69 C70 C71 -1.4(9) . . . . ? C69 C70 C71 C66 0.3(9) . . . . ? C67 C66 C71 C70 1.8(8) . . . . ? B2 C66 C71 C70 -173.5(5) . . . . ? C78 B2 C72 C77 91.9(6) . . . . ? C66 B2 C72 C77 -27.8(7) . . . . ? C60 B2 C72 C77 -148.0(5) . . . . ? C78 B2 C72 C73 -85.1(6) . . . . ? C66 B2 C72 C73 155.2(5) . . . . ? C60 B2 C72 C73 35.0(7) . . . . ? C77 C72 C73 C74 1.2(8) . . . . ? B2 C72 C73 C74 178.5(5) . . . . ? C72 C73 C74 C75 0.0(9) . . . . ? C73 C74 C75 C76 -1.9(10) . . . . ? C74 C75 C76 C77 2.6(11) . . . . ? C75 C76 C77 C72 -1.3(11) . . . . ? C73 C72 C77 C76 -0.5(9) . . . . ? B2 C72 C77 C76 -177.8(6) . . . . ? C72 B2 C78 C83 -35.0(6) . . . . ? C66 B2 C78 C83 87.9(6) . . . . ? C60 B2 C78 C83 -155.0(5) . . . . ? C72 B2 C78 C79 153.8(5) . . . . ? C66 B2 C78 C79 -83.3(6) . . . . ? C60 B2 C78 C79 33.9(7) . . . . ? C83 C78 C79 C80 -1.4(8) . . . . ? B2 C78 C79 C80 170.4(5) . . . . ? C78 C79 C80 C81 -1.2(10) . . . . ? C79 C80 C81 C82 3.0(9) . . . . ? C80 C81 C82 C83 -2.1(9) . . . . ? C81 C82 C83 C78 -0.6(9) . . . . ? C79 C78 C83 C82 2.3(8) . . . . ? B2 C78 C83 C82 -169.6(5) . . . . ?
1100721.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100721.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100721 loop_ _publ_author_name 'Xiaohui Liu' 'Manuel Krott' 'Paul M\"uller' 'Chunhua Hu' 'Heiko Lueken' 'Richard Dronskowski' _publ_section_title ; Synthesis, Crystal Structure, and Properties of MnNCN, the First Carbodiimide of a Magnetic Transition Metal ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3001 _journal_page_last 3003 _journal_paper_doi 10.1021/ic050050a _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C Mn N2' _chemical_formula_weight 94.97 _chemical_name_common 'Manganese carbodiimide' _chemical_name_systematic ; ? ; _space_group_IT_number 166 _symmetry_cell_setting trigonal _symmetry_space_group_name_Hall '-R 3 2"' _symmetry_space_group_name_H-M 'R -3 m :H' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_formula_units_Z 3 _cell_length_a 3.3583(4) _cell_length_b 3.3583(4) _cell_length_c 14.3468(19) _cell_measurement_temperature 293(2) _cell_volume 140.13(3) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.313 _diffrn_measured_fraction_theta_max 0.313 _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0506 _diffrn_reflns_av_sigmaI/netI 0.0196 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 610 _diffrn_reflns_theta_full 30.36 _diffrn_reflns_theta_max 30.36 _diffrn_reflns_theta_min 4.26 _exptl_absorpt_coefficient_mu 6.574 _exptl_crystal_colour green _exptl_crystal_density_diffrn 3.376 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 135 _refine_diff_density_max 1.707 _refine_diff_density_min -0.401 _refine_diff_density_rms 0.181 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.166 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 8 _refine_ls_number_reflns 68 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.166 _refine_ls_R_factor_all 0.0251 _refine_ls_R_factor_gt 0.0251 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0475P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0593 _refine_ls_wR_factor_ref 0.0594 _reflns_number_gt 68 _reflns_number_total 68 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic050050asi20050113_112336.cif _cod_data_source_block mnncn _cod_depositor_comments ; The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w=1/[\s^2^(Fo^2^)+(0.0475P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w=1/[\s^2^(Fo^2^)+(0.0475P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_sg_symbol_H-M 'R 3 2' _cod_database_code 1100721 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z' 'x-y, -y, -z' '-x, -x+y, -z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+1/3' 'x-y+2/3, -y+1/3, -z+1/3' '-x+2/3, -x+y+1/3, -z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+2/3' 'x-y+1/3, -y+2/3, -z+2/3' '-x+1/3, -x+y+2/3, -z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z' '-x+y, y, z' 'x, x-y, z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z+1/3' '-x+y+2/3, y+1/3, z+1/3' 'x+2/3, x-y+1/3, z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+2/3' '-x+y+1/3, y+2/3, z+2/3' 'x+1/3, x-y+2/3, z+2/3' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn Mn 0.3333 0.6667 0.6667 0.0092(4) Uani 1 d S . . C C 0.0000 0.0000 0.5000 0.0085(11) Uani 1 d S . . N N 0.0000 0.0000 0.5855(3) 0.0115(8) Uani 1 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn 0.0096(4) 0.0096(4) 0.0084(5) 0.000 0.000 0.0048(2) C 0.0063(16) 0.0063(16) 0.013(3) 0.000 0.000 0.0031(8) N 0.0122(12) 0.0122(12) 0.0101(15) 0.000 0.000 0.0061(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N Mn N 95.88(12) . 1_565 ? N Mn N 95.88(11) . 1_665 ? N Mn N 95.88(11) 1_565 1_665 ? N Mn N 84.12(12) . 25_556 ? N Mn N 180.0 1_565 25_556 ? N Mn N 84.12(11) 1_665 25_556 ? N Mn N 179.999(1) . 25_566 ? N Mn N 84.12(12) 1_565 25_566 ? N Mn N 84.12(11) 1_665 25_566 ? N Mn N 95.88(12) 25_556 25_566 ? N Mn N 84.12(12) . 25_456 ? N Mn N 84.12(12) 1_565 25_456 ? N Mn N 180.0 1_665 25_456 ? N Mn N 95.88(11) 25_556 25_456 ? N Mn N 95.88(11) 25_566 25_456 ? N C N 180.0 19_556 . ? C N Mn 120.98(9) . 1_445 ? C N Mn 120.98(9) . 1_545 ? Mn N Mn 95.88(12) 1_445 1_545 ? C N Mn 120.98(9) . . ? Mn N Mn 95.88(12) 1_445 . ? Mn N Mn 95.88(12) 1_545 . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn N 2.262(2) . ? Mn N 2.262(2) 1_565 ? Mn N 2.262(2) 1_665 ? Mn N 2.262(2) 25_556 ? Mn N 2.262(2) 25_566 ? Mn N 2.262(2) 25_456 ? C N 1.227(4) 19_556 ? C N 1.227(4) . ? N Mn 2.262(2) 1_445 ? N Mn 2.262(2) 1_545 ?
1100722.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $ #$Revision: 176432 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100722.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100722 loop_ _publ_author_name 'Andrea C. Sudik' 'Adrien P. C\^ot\'e' 'Omar M. Yaghi' _publ_contact_author_address ; department of chemistry university of michigan 930 n. university ave. ann arbor, mi 48109-1055 united states of america ; _publ_contact_author_email oyaghi@umich.edu _publ_contact_author_name 'professor omar m. yaghi' _publ_section_title ; Metal-Organic Frameworks Based on Trigonal Prismatic Building Blocks and the New "acs" Topology ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 2998 _journal_page_last 3000 _journal_paper_doi 10.1021/ic050064g _journal_volume 44 _journal_year 2005 _chemical_formula_moiety '(C33 H15 Fe3 N3 O16), (Cl4 Fe), O' _chemical_formula_sum 'C33 H15 Cl4 Fe4 N3 O17' _chemical_formula_weight 1090.61 _chemical_name_systematic ; ? ; _space_group_IT_number 190 _symmetry_cell_setting hexagonal _symmetry_space_group_name_Hall 'P -6c -2c' _symmetry_space_group_name_H-M 'P -6 2 c' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_formula_units_Z 2 _cell_length_a 12.531(3) _cell_length_b 12.531(3) _cell_length_c 18.476(11) _cell_measurement_reflns_used 715 _cell_measurement_temperature 153(2) _cell_measurement_theta_max 25.14 _cell_measurement_theta_min 1.88 _cell_volume 2512.5(17) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 153(2) _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1441 _diffrn_reflns_av_sigmaI/netI 0.1009 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 11323 _diffrn_reflns_theta_full 25.15 _diffrn_reflns_theta_max 25.15 _diffrn_reflns_theta_min 1.88 _exptl_absorpt_coefficient_mu 1.407 _exptl_absorpt_correction_T_max 0.9498 _exptl_absorpt_correction_T_min 0.9433 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-58' _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.442 _exptl_crystal_density_method 'not measured' _exptl_crystal_description octahedral _exptl_crystal_F_000 1084 _exptl_crystal_size_max 0.042 _exptl_crystal_size_mid 0.041 _exptl_crystal_size_min 0.037 _refine_diff_density_max 0.718 _refine_diff_density_min -0.711 _refine_diff_density_rms 0.159 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(10) _refine_ls_extinction_coef 0.015(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.260 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 116 _refine_ls_number_reflns 1543 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.260 _refine_ls_R_factor_all 0.1241 _refine_ls_R_factor_gt 0.1044 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1172P)^2^+5.2365P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2454 _refine_ls_wR_factor_ref 0.2550 _reflns_number_gt 1292 _reflns_number_total 1543 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic050064gsi20050115_040515_2.cif _cod_data_source_block MOF-235 _cod_original_cell_volume 2512.6(17) _cod_original_sg_symbol_Hall P-6c-2c _cod_database_code 1100722 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x, y, -z+1/2' '-y, x-y, -z+1/2' '-x+y, -x, -z+1/2' 'y, x, -z' 'x-y, -y, -z' '-x, -x+y, -z' 'y, x, z+1/2' 'x-y, -y, z+1/2' '-x, -x+y, z+1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.7270(2) 1.2195(2) 0.7500 0.0233(6) Uani 1 2 d S . . O1 O 0.6667 1.3333 0.7500 0.018(4) Uani 1 6 d S . . O2 O 0.8499(8) 1.3019(7) 0.6692(4) 0.034(2) Uani 1 1 d . . . O3 O 0.7800(11) 1.0882(12) 0.7500 0.047(3) Uani 1 2 d S . . O4 O 0.6106(8) 1.1159(8) 0.6719(5) 0.042(2) Uani 1 1 d . . . C1 C 0.716(3) 0.982(3) 0.7500 0.21(3) Uani 1 2 d S . . H1 H 0.6321 0.9569 0.7500 0.255 Uiso 1 2 calc SR . . N1 N 0.738(2) 0.893(2) 0.7500 0.119(10) Uani 1 2 d SD . . C3 C 0.5160(11) 1.1110(13) 0.6423(8) 0.046(3) Uani 1 1 d . . . C4 C 0.5680(13) 1.0240(18) 0.5353(7) 0.064(5) Uani 1 1 d . . . H4 H 0.6384 1.0371 0.5598 0.03(3) Uiso 1 1 calc R . . C5 C 0.4835(12) 1.0521(13) 0.5685(7) 0.047(4) Uani 1 1 d . . . C6 C 0.3754(11) 1.0259(11) 0.5325(6) 0.041(3) Uani 1 1 d . . . H6 H 0.3204 1.0452 0.5545 0.050 Uiso 1 1 calc R . . C7 C 0.805(6) 0.896(5) 0.692(3) 0.16(3) Uani 0.50 1 d P . . C8 C 0.643(5) 0.767(3) 0.7500 0.30(4) Uani 1 2 d SD . . O1W O 0.3333 0.6667 0.594(6) 0.22(4) Uani 0.50 3 d SP . . Fe2 Fe 0.0000 1.0000 0.5000 0.099(3) Uani 1 6 d S . . Cl1 Cl -0.1618(12) 1.0000 0.5000 0.051(4) Uani 0.333 2 d SP . . Cl2 Cl -0.1453(17) 0.9805(19) 0.574(2) 0.31(2) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0169(11) 0.0207(12) 0.0349(10) 0.000 0.000 0.0114(10) O1 0.001(5) 0.001(5) 0.053(11) 0.000 0.000 0.000(2) O2 0.040(5) 0.030(5) 0.041(5) 0.012(4) 0.018(4) 0.024(4) O3 0.041(8) 0.033(8) 0.069(9) 0.000 0.000 0.019(6) O4 0.041(6) 0.037(5) 0.054(5) -0.017(4) -0.010(4) 0.024(4) C1 0.042(16) 0.032(17) 0.56(10) 0.000 0.000 0.018(14) N1 0.11(2) 0.053(14) 0.23(3) 0.000 0.000 0.069(15) C3 0.037(8) 0.032(8) 0.072(9) -0.017(7) -0.018(6) 0.018(7) C4 0.051(9) 0.116(14) 0.038(7) -0.038(9) -0.021(7) 0.052(10) C5 0.037(9) 0.042(8) 0.052(7) -0.011(6) 0.000(6) 0.014(7) C6 0.022(6) 0.054(8) 0.047(6) 0.000(6) -0.003(6) 0.019(6) C7 0.31(8) 0.17(5) 0.15(4) 0.06(4) 0.13(5) 0.21(7) C8 0.21(6) 0.06(3) 0.63(14) 0.000 0.000 0.07(4) O1W 0.13(4) 0.13(4) 0.39(12) 0.000 0.000 0.065(18) Fe2 0.097(4) 0.097(4) 0.105(5) 0.000 0.000 0.0483(19) Cl1 0.020(5) 0.050(9) 0.095(12) -0.004(9) -0.002(5) 0.025(4) Cl2 0.105(12) 0.118(16) 0.65(5) -0.14(3) 0.12(2) 0.004(11) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Fe1 O4 93.0(2) . 4_556 ? O1 Fe1 O4 93.0(2) . . ? O4 Fe1 O4 92.3(6) 4_556 . ? O1 Fe1 O2 95.9(2) . 4_556 ? O4 Fe1 O2 85.5(4) 4_556 4_556 ? O4 Fe1 O2 170.9(3) . 4_556 ? O1 Fe1 O2 95.9(2) . . ? O4 Fe1 O2 170.9(3) 4_556 . ? O4 Fe1 O2 85.4(4) . . ? O2 Fe1 O2 95.4(5) 4_556 . ? O1 Fe1 O3 176.3(4) . . ? O4 Fe1 O3 84.5(3) 4_556 . ? O4 Fe1 O3 84.5(3) . . ? O2 Fe1 O3 86.6(3) 4_556 . ? O2 Fe1 O3 86.6(3) . . ? Fe1 O1 Fe1 120.000(2) 3_575 . ? Fe1 O1 Fe1 120.0 3_575 2_775 ? Fe1 O1 Fe1 120.001(1) . 2_775 ? C3 O2 Fe1 129.4(8) 2_775 . ? C1 O3 Fe1 126.8(17) . . ? C3 O4 Fe1 134.2(8) . . ? O3 C1 N1 132(3) . . ? O3 C1 H1 114.0 . . ? N1 C1 H1 114.0 . . ? C1 N1 C7 113(2) . . ? C1 N1 C7 113(2) . 4_556 ? C7 N1 C7 105(6) . 4_556 ? C1 N1 C8 123(3) . . ? C7 N1 C8 101(3) . . ? C7 N1 C8 101(3) 4_556 . ? O2 C3 O4 125.4(12) 3_575 . ? O2 C3 C5 119.3(12) 3_575 . ? O4 C3 C5 115.3(12) . . ? C4 C4 C5 118.9(8) 8_676 . ? C4 C4 H4 120.6 8_676 . ? C5 C4 H4 120.6 . . ? C6 C5 C4 119.8(12) . . ? C6 C5 C3 122.7(12) . . ? C4 C5 C3 117.5(12) . . ? C6 C6 C5 121.2(8) 8_676 . ? C6 C6 H6 119.4 8_676 . ? C5 C6 H6 119.4 . . ? Cl1 Fe2 Cl1 119.998(1) 3_575 1_455 ? Cl1 Fe2 Cl1 120.001(6) 3_575 2_665 ? Cl1 Fe2 Cl1 120.001(10) 1_455 2_665 ? Cl2 Cl1 Cl2 153(2) 8_676 . ? Cl2 Cl1 Fe2 76.6(11) 8_676 1_655 ? Cl2 Cl1 Fe2 76.6(11) . 1_655 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O1 1.920(2) . ? Fe1 O4 2.001(9) 4_556 ? Fe1 O4 2.001(9) . ? Fe1 O2 2.019(8) 4_556 ? Fe1 O2 2.019(8) . ? Fe1 O3 2.059(13) . ? O1 Fe1 1.920(2) 3_575 ? O1 Fe1 1.920(2) 2_775 ? O2 C3 1.235(16) 2_775 ? O3 C1 1.16(3) . ? O4 C3 1.278(15) . ? C1 N1 1.27(3) . ? C1 H1 0.9300 . ? N1 C7 1.36(4) . ? N1 C7 1.36(4) 4_556 ? N1 C8 1.43(2) . ? C3 O2 1.235(16) 3_575 ? C3 C5 1.507(18) . ? C4 C4 1.41(3) 8_676 ? C4 C5 1.412(19) . ? C4 H4 0.9300 . ? C5 C6 1.393(17) . ? C6 C6 1.33(2) 8_676 ? C6 H6 0.9300 . ? Fe2 Cl1 2.028(16) . ? Fe2 Cl1 2.028(16) . ? Fe2 Cl1 2.028(16) . ? Fe2 Cl2 2.19(2) . ? Fe2 Cl2 2.19(2) . ? Fe2 Cl2 2.19(2) . ? Fe2 Cl2 2.19(2) . ? Fe2 Cl2 2.19(2) . ? Fe2 Cl2 2.19(2) . ? Cl1 Fe2 2.028(16) . ? Cl2 Fe2 2.19(2) . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Fe1 O1 Fe1 -46.3(3) 4_556 . . 3_575 ? O4 Fe1 O1 Fe1 46.3(3) . . . 3_575 ? O2 Fe1 O1 Fe1 -132.0(3) 4_556 . . 3_575 ? O2 Fe1 O1 Fe1 132.0(3) . . . 3_575 ? O4 Fe1 O1 Fe1 133.7(3) 4_556 . . 2_775 ? O4 Fe1 O1 Fe1 -133.7(3) . . . 2_775 ? O2 Fe1 O1 Fe1 48.0(3) 4_556 . . 2_775 ? O2 Fe1 O1 Fe1 -48.0(3) . . . 2_775 ? O1 Fe1 O2 C3 13.9(12) . . . 2_775 ? O4 Fe1 O2 C3 106.4(12) . . . 2_775 ? O2 Fe1 O2 C3 -82.7(12) 4_556 . . 2_775 ? O3 Fe1 O2 C3 -168.9(12) . . . 2_775 ? O4 Fe1 O3 C1 46.5(3) 4_556 . . . ? O4 Fe1 O3 C1 -46.5(3) . . . . ? O2 Fe1 O3 C1 132.2(3) 4_556 . . . ? O2 Fe1 O3 C1 -132.2(3) . . . . ? O1 Fe1 O4 C3 -11.8(13) . . . . ? O4 Fe1 O4 C3 81.2(13) 4_556 . . . ? O2 Fe1 O4 C3 -107.5(13) . . . . ? O3 Fe1 O4 C3 165.5(13) . . . . ? Fe1 O3 C1 N1 180.0 . . . . ? O3 C1 N1 C7 -59(4) . . . . ? O3 C1 N1 C7 59(4) . . . 4_556 ? O3 C1 N1 C8 180.0 . . . . ? Fe1 O4 C3 O2 -21(2) . . . 3_575 ? Fe1 O4 C3 C5 158.7(9) . . . . ? C4 C4 C5 C6 3(3) 8_676 . . . ? C4 C4 C5 C3 -176(2) 8_676 . . . ? O2 C3 C5 C6 -8(2) 3_575 . . . ? O4 C3 C5 C6 172.1(13) . . . . ? O2 C3 C5 C4 171.5(15) 3_575 . . . ? O4 C3 C5 C4 -8(2) . . . . ? C4 C5 C6 C6 0(3) . . . 8_676 ? C3 C5 C6 C6 179.9(15) . . . 8_676 ? Cl2 Cl1 Cl2 Fe2 0.00(2) 8_676 . . 1_655 ?
1100723.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $ #$Revision: 176435 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100723.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100723 loop_ _publ_author_name 'Andrea C. Sudik' 'Adrien P. C\^ot\'e' 'Omar M. Yaghi' _publ_contact_author_address ; department of chemistry university of michigan 930 n. university ave. ann arbor, mi 48109-1055 united states of america ; _publ_contact_author_email oyaghi@umich.edu _publ_contact_author_name 'professor omar m. yaghi' _publ_section_title ; Metal-Organic Frameworks Based on Trigonal Prismatic Building Blocks and the New "acs" Topology ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 2998 _journal_page_last 3000 _journal_paper_doi 10.1021/ic050064g _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C40.5 H18 Fe3 N3 O16' _chemical_formula_weight 970.13 _chemical_name_common 'C40.50 H18 Fe3 N3 O16' _chemical_name_systematic ; ? ; _space_group_IT_number 190 _symmetry_cell_setting hexagonal _symmetry_space_group_name_Hall 'P -6c -2c' _symmetry_space_group_name_H-M 'P -6 2 c' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_formula_units_Z 2 _cell_length_a 13.010(4) _cell_length_b 13.010(4) _cell_length_c 14.874(9) _cell_measurement_reflns_used 828 _cell_measurement_temperature 153(2) _cell_measurement_theta_max 23.28 _cell_measurement_theta_min 2.23 _cell_volume 2180.3(16) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 153(2) _diffrn_measured_fraction_theta_full 0.984 _diffrn_measured_fraction_theta_max 0.984 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.2551 _diffrn_reflns_av_sigmaI/netI 0.1806 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 6065 _diffrn_reflns_theta_full 22.21 _diffrn_reflns_theta_max 22.21 _diffrn_reflns_theta_min 2.27 _exptl_absorpt_coefficient_mu 1.057 _exptl_absorpt_correction_T_max 0.9780 _exptl_absorpt_correction_T_min 0.9641 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-58' _exptl_crystal_colour green _exptl_crystal_density_diffrn 1.478 _exptl_crystal_density_method 'not measured' _exptl_crystal_description octahedral _exptl_crystal_F_000 976 _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _refine_diff_density_max 0.367 _refine_diff_density_min -0.581 _refine_diff_density_rms 0.077 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.17(8) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 92 _refine_ls_number_reflns 946 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 1.005 _refine_ls_R_factor_all 0.1382 _refine_ls_R_factor_gt 0.0651 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0275P)^2^+0.9999P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1039 _refine_ls_wR_factor_ref 0.1193 _reflns_number_gt 543 _reflns_number_total 946 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic050064gsi20050115_040515_1.cif _cod_data_source_block MOF-236 _cod_original_formula_sum 'C40.50 H18 Fe3 N3 O16' _cod_database_code 1100723 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x-y, -y, -z' '-x, -x+y, -z' 'y, x, -z' 'y, x, z+1/2' '-x, -x+y, z+1/2' 'x-y, -y, z+1/2' 'x, y, -z+1/2' '-x+y, -x, -z+1/2' '-y, x-y, -z+1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7051(15) 0.5566(11) 0.8734(6) 0.038(3) Uani 1 1 d U . . C2 C 0.7201(9) 0.6484(10) 0.9398(7) 0.047(3) Uiso 1 1 d . . . C3 C 0.844(2) 0.736(3) 0.9652(18) 0.050(7) Uiso 0.50 1 d P . . C4 C 0.6304(11) 0.6304(11) 1.0000 0.029(4) Uiso 1 2 d S . . H8 H 0.5574 0.5574 1.0000 0.034 Uiso 1 2 calc SR . . C5 C 0.853(5) 0.853(5) 1.0000 0.14(2) Uiso 0.50 2 d SP . . C6 C 1.0700(13) 0.6569(12) 0.8264(8) 0.060(4) Uani 1 1 d D . . H1 H 1.0278 0.6270 0.8811 0.073 Uiso 1 1 calc R . . C7 C 1.1884(15) 0.7472(15) 0.8315(9) 0.086(6) Uani 1 1 d D . . H2 H 1.2302 0.7742 0.8867 0.103 Uiso 1 1 calc R . . C8 C 1.239(2) 0.793(2) 0.7500 0.113(10) Uani 1 2 d S . . H3 H 1.3149 0.8625 0.7500 0.136 Uiso 1 2 calc SR . . C3A C 0.813(2) 0.765(3) 0.9184(17) 0.064(8) Uiso 0.50 1 d P . . C5A C 0.814(3) 0.861(4) 0.951(2) 0.111(12) Uiso 0.50 1 d P . . Fe1 Fe 0.8252(2) 0.4636(2) 0.7500 0.0341(7) Uani 1 2 d S . . N1 N 1.0124(11) 0.6101(13) 0.7500 0.043(4) Uani 1 2 d S . . O1 O 0.6667 0.3333 0.7500 0.009(4) Uani 1 6 d S . . O2 O 0.8000(8) 0.5607(7) 0.8452(4) 0.055(3) Uani 1 1 d U . . O3 O 0.6005(8) 0.4863(7) 0.8485(4) 0.044(2) Uani 1 1 d . . . O1W O 0.919(5) 0.913(6) 0.7500 0.38(2) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.073(10) 0.039(9) 0.007(6) 0.006(6) 0.008(7) 0.031(10) C6 0.075(11) 0.061(11) 0.045(8) -0.006(8) -0.007(8) 0.034(10) C7 0.070(13) 0.078(13) 0.070(11) -0.013(9) 0.000(10) 0.008(12) C8 0.068(18) 0.080(19) 0.13(2) 0.000 0.000 -0.009(16) Fe1 0.0479(18) 0.0508(17) 0.0063(8) 0.000 0.000 0.0267(16) N1 0.039(9) 0.056(11) 0.015(8) 0.000 0.000 0.008(9) O1 0.003(6) 0.003(6) 0.022(9) 0.000 0.000 0.001(3) O2 0.054(6) 0.067(7) 0.039(5) 0.000(4) 0.020(4) 0.027(6) O3 0.052(6) 0.061(6) 0.020(4) -0.016(4) -0.019(4) 0.029(6) O1W 0.31(5) 0.39(7) 0.133(13) 0.000 0.000 -0.07(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 C1 O2 127.2(10) . . ? O3 C1 C2 116.2(12) . . ? O2 C1 C2 116.6(12) . . ? C4 C2 C3A 120.9(15) . . ? C4 C2 C1 122.0(11) . . ? C3A C2 C1 114.1(14) . . ? C4 C2 C3 117.5(13) . . ? C3A C2 C3 39.0(12) . . ? C1 C2 C3 116.2(15) . . ? C3A C3 C2 67(3) . . ? C3A C3 C5A 106(3) . 6_557 ? C2 C3 C5A 117(2) . 6_557 ? C3A C3 C5 72(3) . . ? C2 C3 C5 111(3) . . ? C5A C3 C5 34.5(14) 6_557 . ? C3A C3 C5A 43(2) . . ? C2 C3 C5A 91(2) . . ? C5A C3 C5A 63(2) 6_557 . ? C5 C3 C5A 29.6(15) . . ? C2 C4 C2 119.7(14) . 6_557 ? C2 C4 H8 120.1 . . ? C2 C4 H8 120.1 6_557 . ? C5A C5 C5A 155(10) 6_557 . ? C5A C5 C3A 58(3) 6_557 6_557 ? C5A C5 C3A 108(5) . 6_557 ? C5A C5 C3A 108(5) 6_557 . ? C5A C5 C3A 58(3) . . ? C3A C5 C3A 116(5) 6_557 . ? C5A C5 C3 73(4) 6_557 . ? C5A C5 C3 94(4) . . ? C3A C5 C3 105(3) 6_557 . ? C3A C5 C3 36.4(14) . . ? C5A C5 C3 94(4) 6_557 6_557 ? C5A C5 C3 73(4) . 6_557 ? C3A C5 C3 36.4(14) 6_557 6_557 ? C3A C5 C3 105(3) . 6_557 ? C3 C5 C3 117(5) . 6_557 ? N1 C6 C7 124.4(14) . . ? N1 C6 H1 117.8 . . ? C7 C6 H1 117.8 . . ? C8 C7 C6 113.9(17) . . ? C8 C7 H2 123.1 . . ? C6 C7 H2 123.1 . . ? C7 C8 C7 125(2) . 10_556 ? C7 C8 H3 117.4 . . ? C7 C8 H3 117.4 10_556 . ? C3 C3A C5A 107(3) . . ? C3 C3A C2 74(3) . . ? C5A C3A C2 122(3) . . ? C3 C3A C5 71(2) . . ? C5A C3A C5 36.0(17) . . ? C2 C3A C5 113(3) . . ? C3 C3A C5A 47.1(19) . 6_557 ? C5A C3A C5A 60(3) . 6_557 ? C2 C3A C5A 94.8(17) . 6_557 ? C5 C3A C5A 25.4(17) . 6_557 ? C5 C5A C3A 86(4) . . ? C5 C5A C3 73(4) . 6_557 ? C3A C5A C3 117(3) . 6_557 ? C5 C5A C5A 12(6) . 6_557 ? C3A C5A C5A 80(2) . 6_557 ? C3 C5A C5A 67(2) 6_557 6_557 ? C5 C5A C3 56(3) . . ? C3A C5A C3 30.0(15) . . ? C3 C5A C3 101(2) 6_557 . ? C5A C5A C3 50.2(15) 6_557 . ? C5 C5A C3A 47(4) . 6_557 ? C3A C5A C3A 102(3) . 6_557 ? C3 C5A C3A 27.3(14) 6_557 6_557 ? C5A C5A C3A 39.8(14) 6_557 6_557 ? C3 C5A C3A 78.1(17) . 6_557 ? O1 Fe1 O3 96.0(3) . 11_666 ? O1 Fe1 O3 96.0(3) . 3_665 ? O3 Fe1 O3 92.4(4) 11_666 3_665 ? O1 Fe1 O2 96.5(2) . 10_556 ? O3 Fe1 O2 88.2(3) 11_666 10_556 ? O3 Fe1 O2 167.3(3) 3_665 10_556 ? O1 Fe1 O2 96.5(2) . . ? O3 Fe1 O2 167.3(3) 11_666 . ? O3 Fe1 O2 88.2(3) 3_665 . ? O2 Fe1 O2 88.4(4) 10_556 . ? O1 Fe1 N1 177.7(4) . . ? O3 Fe1 N1 82.4(4) 11_666 . ? O3 Fe1 N1 82.4(4) 3_665 . ? O2 Fe1 N1 85.1(3) 10_556 . ? O2 Fe1 N1 85.1(3) . . ? C6 N1 C6 117.4(16) 10_556 . ? C6 N1 Fe1 121.3(8) 10_556 . ? C6 N1 Fe1 121.3(8) . . ? Fe1 O1 Fe1 120.001(1) 2_655 . ? Fe1 O1 Fe1 120.000(1) 2_655 3_665 ? Fe1 O1 Fe1 120.0 . 3_665 ? C1 O2 Fe1 130.9(8) . . ? C1 O3 Fe1 131.1(7) . 2_655 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O3 1.257(14) . ? C1 O2 1.280(13) . ? C1 C2 1.485(13) . ? C2 C4 1.395(11) . ? C2 C3A 1.43(3) . ? C2 C3 1.49(3) . ? C3 C3A 0.98(3) . ? C3 C5A 1.56(3) 6_557 ? C3 C5 1.56(4) . ? C3 C5A 1.87(5) . ? C4 C2 1.395(11) 6_557 ? C4 H8 0.9500 . ? C5 C5A 0.92(4) 6_557 ? C5 C5A 0.92(4) . ? C5 C3A 1.57(4) 6_557 ? C5 C3A 1.57(4) . ? C5 C3 1.56(4) 6_557 ? C6 N1 1.330(13) . ? C6 C7 1.396(17) . ? C6 H1 0.9500 . ? C7 C8 1.365(14) . ? C7 H2 0.9500 . ? C8 C7 1.365(14) 10_556 ? C8 H3 0.9500 . ? C3A C5A 1.33(4) . ? C3A C5A 2.05(4) 6_557 ? C5A C3 1.56(3) 6_557 ? C5A C5A 1.80(7) 6_557 ? C5A C3A 2.05(4) 6_557 ? Fe1 O1 1.905(2) . ? Fe1 O3 2.030(7) 11_666 ? Fe1 O3 2.030(7) 3_665 ? Fe1 O2 2.031(7) 10_556 ? Fe1 O2 2.031(7) . ? Fe1 N1 2.218(13) . ? N1 C6 1.330(13) 10_556 ? O1 Fe1 1.905(2) 2_655 ? O1 Fe1 1.905(2) 3_665 ? O3 Fe1 2.030(7) 2_655 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 C1 C2 C4 27.4(14) . . . . ? O2 C1 C2 C4 -155.3(8) . . . . ? O3 C1 C2 C3A -133.3(16) . . . . ? O2 C1 C2 C3A 44.1(19) . . . . ? O3 C1 C2 C3 -176.6(14) . . . . ? O2 C1 C2 C3 0.8(19) . . . . ? C4 C2 C3 C3A -106(2) . . . . ? C1 C2 C3 C3A 97(2) . . . . ? C4 C2 C3 C5A -10(3) . . . 6_557 ? C3A C2 C3 C5A 96(3) . . . 6_557 ? C1 C2 C3 C5A -167(2) . . . 6_557 ? C4 C2 C3 C5 -47(2) . . . . ? C3A C2 C3 C5 59(2) . . . . ? C1 C2 C3 C5 156.0(15) . . . . ? C4 C2 C3 C5A -70(2) . . . . ? C3A C2 C3 C5A 37(2) . . . . ? C1 C2 C3 C5A 133.3(16) . . . . ? C3A C2 C4 C2 -19.7(14) . . . 6_557 ? C1 C2 C4 C2 -179.1(11) . . . 6_557 ? C3 C2 C4 C2 25.1(14) . . . 6_557 ? C3A C3 C5 C5A 164(6) . . . 6_557 ? C2 C3 C5 C5A 107(5) . . . 6_557 ? C5A C3 C5 C5A 159(10) . . . 6_557 ? C3A C3 C5 C5A 5(5) . . . . ? C2 C3 C5 C5A -51(6) . . . . ? C5A C3 C5 C5A -159(10) 6_557 . . . ? C3A C3 C5 C3A 114(4) . . . 6_557 ? C2 C3 C5 C3A 58(2) . . . 6_557 ? C5A C3 C5 C3A -49(3) 6_557 . . 6_557 ? C5A C3 C5 C3A 110(7) . . . 6_557 ? C2 C3 C5 C3A -56(2) . . . . ? C5A C3 C5 C3A -164(6) 6_557 . . . ? C5A C3 C5 C3A -5(6) . . . . ? C3A C3 C5 C3 78(2) . . . 6_557 ? C2 C3 C5 C3 21.5(11) . . . 6_557 ? C5A C3 C5 C3 -86(5) 6_557 . . 6_557 ? C5A C3 C5 C3 73(5) . . . 6_557 ? N1 C6 C7 C8 6(3) . . . . ? C6 C7 C8 C7 -9(4) . . . 10_556 ? C2 C3 C3A C5A 119(3) . . . . ? C5A C3 C3A C5A 6(4) 6_557 . . . ? C5 C3 C3A C5A -4(4) . . . . ? C5A C3 C3A C2 -113(2) 6_557 . . . ? C5 C3 C3A C2 -122(2) . . . . ? C5A C3 C3A C2 -119(3) . . . . ? C2 C3 C3A C5 122(3) . . . . ? C5A C3 C3A C5 10(3) 6_557 . . . ? C5A C3 C3A C5 4(4) . . . . ? C2 C3 C3A C5A 113(2) . . . 6_557 ? C5 C3 C3A C5A -10(3) . . . 6_557 ? C5A C3 C3A C5A -6(4) . . . 6_557 ? C4 C2 C3A C3 97(2) . . . . ? C1 C2 C3A C3 -102(2) . . . . ? C4 C2 C3A C5A -4(4) . . . . ? C1 C2 C3A C5A 157(3) . . . . ? C3 C2 C3A C5A -100(4) . . . . ? C4 C2 C3A C5 36(2) . . . . ? C1 C2 C3A C5 -163.1(14) . . . . ? C3 C2 C3A C5 -61(2) . . . . ? C4 C2 C3A C5A 54(2) . . . 6_557 ? C1 C2 C3A C5A -145.1(15) . . . 6_557 ? C3 C2 C3A C5A -42.7(18) . . . 6_557 ? C5A C5 C3A C3 -17(5) 6_557 . . . ? C5A C5 C3A C3 -174(7) . . . . ? C3A C5 C3A C3 -79(2) 6_557 . . . ? C3 C5 C3A C3 -116(4) 6_557 . . . ? C5A C5 C3A C5A 158(10) 6_557 . . . ? C3A C5 C3A C5A 95(5) 6_557 . . . ? C3 C5 C3A C5A 174(7) . . . . ? C3 C5 C3A C5A 58(4) 6_557 . . . ? C5A C5 C3A C2 46(5) 6_557 . . . ? C5A C5 C3A C2 -112(6) . . . . ? C3A C5 C3A C2 -16.6(12) 6_557 . . . ? C3 C5 C3A C2 62(3) . . . . ? C3 C5 C3A C2 -54(3) 6_557 . . . ? C5A C5 C3A C5A -158(10) . . . 6_557 ? C3A C5 C3A C5A -62(5) 6_557 . . 6_557 ? C3 C5 C3A C5A 17(5) . . . 6_557 ? C3 C5 C3A C5A -99(7) 6_557 . . 6_557 ? C5A C5 C5A C3A -59.8(18) 6_557 . . . ? C3A C5 C5A C3A -110(4) 6_557 . . . ? C3 C5 C5A C3A -3(4) . . . . ? C3 C5 C5A C3A -120(2) 6_557 . . . ? C5A C5 C5A C3 60.4(13) 6_557 . . 6_557 ? C3A C5 C5A C3 10(3) 6_557 . . 6_557 ? C3A C5 C5A C3 120(2) . . . 6_557 ? C3 C5 C5A C3 117(4) . . . 6_557 ? C3A C5 C5A C5A -50(3) 6_557 . . 6_557 ? C3A C5 C5A C5A 59.8(19) . . . 6_557 ? C3 C5 C5A C5A 56(3) . . . 6_557 ? C3 C5 C5A C5A -60.4(13) 6_557 . . 6_557 ? C5A C5 C5A C3 -56(3) 6_557 . . . ? C3A C5 C5A C3 -107(6) 6_557 . . . ? C3A C5 C5A C3 3(4) . . . . ? C3 C5 C5A C3 -117(4) 6_557 . . . ? C5A C5 C5A C3A 50(3) 6_557 . . 6_557 ? C3A C5 C5A C3A 110(4) . . . 6_557 ? C3 C5 C5A C3A 107(6) . . . 6_557 ? C3 C5 C5A C3A -10(3) 6_557 . . 6_557 ? C3 C3A C5A C5 6(7) . . . . ? C2 C3A C5A C5 87(6) . . . . ? C5A C3A C5A C5 11(5) 6_557 . . . ? C3 C3A C5A C3 -63(4) . . . 6_557 ? C2 C3A C5A C3 19(4) . . . 6_557 ? C5 C3A C5A C3 -68(5) . . . 6_557 ? C5A C3A C5A C3 -57(3) 6_557 . . 6_557 ? C3 C3A C5A C5A -5(3) . . . 6_557 ? C2 C3A C5A C5A 76(2) . . . 6_557 ? C5 C3A C5A C5A -11(5) . . . 6_557 ? C2 C3A C5A C3 81(4) . . . . ? C5 C3A C5A C3 -6(7) . . . . ? C5A C3A C5A C3 5(3) 6_557 . . . ? C3 C3A C5A C3A -39(4) . . . 6_557 ? C2 C3A C5A C3A 43(3) . . . 6_557 ? C5 C3A C5A C3A -44(4) . . . 6_557 ? C5A C3A C5A C3A -33.5(19) 6_557 . . 6_557 ? C3A C3 C5A C5 -173(8) . . . . ? C2 C3 C5A C5 133(6) . . . . ? C5A C3 C5A C5 13(6) 6_557 . . . ? C2 C3 C5A C3A -54(4) . . . . ? C5A C3 C5A C3A -173(4) 6_557 . . . ? C5 C3 C5A C3A 173(8) . . . . ? C3A C3 C5A C3 127(4) . . . 6_557 ? C2 C3 C5A C3 73(2) . . . 6_557 ? C5A C3 C5A C3 -47(3) 6_557 . . 6_557 ? C5 C3 C5A C3 -60(5) . . . 6_557 ? C3A C3 C5A C5A 173(4) . . . 6_557 ? C2 C3 C5A C5A 119.7(19) . . . 6_557 ? C5 C3 C5A C5A -13(6) . . . 6_557 ? C3A C3 C5A C3A 141(5) . . . 6_557 ? C2 C3 C5A C3A 87.5(16) . . . 6_557 ? C5A C3 C5A C3A -32(2) 6_557 . . 6_557 ? C5 C3 C5A C3A -45(5) . . . 6_557 ? C7 C6 N1 C6 -4(3) . . . 10_556 ? C7 C6 N1 Fe1 178.4(12) . . . . ? O1 Fe1 N1 C6 91.0(11) . . . 10_556 ? O3 Fe1 N1 C6 44.3(11) 11_666 . . 10_556 ? O3 Fe1 N1 C6 137.8(12) 3_665 . . 10_556 ? O2 Fe1 N1 C6 -44.5(11) 10_556 . . 10_556 ? O2 Fe1 N1 C6 -133.4(12) . . . 10_556 ? O1 Fe1 N1 C6 -91.0(11) . . . . ? O3 Fe1 N1 C6 -137.8(12) 11_666 . . . ? O3 Fe1 N1 C6 -44.3(11) 3_665 . . . ? O2 Fe1 N1 C6 133.4(12) 10_556 . . . ? O2 Fe1 N1 C6 44.5(11) . . . . ? O3 Fe1 O1 Fe1 -133.5(2) 11_666 . . 2_655 ? O3 Fe1 O1 Fe1 133.5(2) 3_665 . . 2_655 ? O2 Fe1 O1 Fe1 -44.6(2) 10_556 . . 2_655 ? O2 Fe1 O1 Fe1 44.6(2) . . . 2_655 ? N1 Fe1 O1 Fe1 180.0 . . . 2_655 ? O3 Fe1 O1 Fe1 46.5(2) 11_666 . . 3_665 ? O3 Fe1 O1 Fe1 -46.5(2) 3_665 . . 3_665 ? O2 Fe1 O1 Fe1 135.4(2) 10_556 . . 3_665 ? O2 Fe1 O1 Fe1 -135.4(2) . . . 3_665 ? N1 Fe1 O1 Fe1 0.0 . . . 3_665 ? O3 C1 O2 Fe1 1.8(17) . . . . ? C2 C1 O2 Fe1 -175.3(7) . . . . ? O1 Fe1 O2 C1 -20.3(9) . . . . ? O3 Fe1 O2 C1 151.0(14) 11_666 . . . ? O3 Fe1 O2 C1 -116.1(9) 3_665 . . . ? O2 Fe1 O2 C1 76.1(10) 10_556 . . . ? N1 Fe1 O2 C1 161.3(9) . . . . ? O2 C1 O3 Fe1 -5.6(16) . . . 2_655 ? C2 C1 O3 Fe1 171.5(7) . . . 2_655 ?
1100724.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100724.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100724 loop_ _publ_author_name 'Tara J. Burchell' 'Richard J. Puddephatt' _publ_section_title ; Self-Assembly of Chiral Coordination Polymers and Macrocycles: A Metal Template Effect on the Polymer-Macrocycle Equilibrium ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3718 _journal_page_last 3730 _journal_paper_doi 10.1021/ic050097w _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C36 H30 N4 O3' _chemical_formula_weight 566.64 _chemical_name_systematic ; ? ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 105.54(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 9.5809(19) _cell_length_b 18.196(4) _cell_length_c 17.263(4) _cell_measurement_temperature 150(2) _cell_volume 2899.5(12) _computing_cell_refinement 'Nonius DENZO' _computing_data_collection 'Nonius COLLECT' _computing_data_reduction 'Nonius DENZO' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'phi\omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.044 _diffrn_reflns_av_sigmaI/netI 0.0602 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 28792 _diffrn_reflns_theta_full 27.51 _diffrn_reflns_theta_max 27.51 _diffrn_reflns_theta_min 2.55 _exptl_absorpt_coefficient_mu 0.084 _exptl_absorpt_correction_T_max 0.9592 _exptl_absorpt_correction_T_min 0.9572 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.298 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1192 _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.52 _exptl_crystal_size_min 0.50 _refine_diff_density_max 0.347 _refine_diff_density_min -0.387 _refine_diff_density_rms 0.045 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 403 _refine_ls_number_reflns 6657 _refine_ls_number_restraints 22 _refine_ls_restrained_S_all 1.163 _refine_ls_R_factor_all 0.1053 _refine_ls_R_factor_gt 0.0574 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0863P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1497 _refine_ls_wR_factor_ref 0.1667 _reflns_number_gt 4039 _reflns_number_total 6657 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic050097wsi20050217_082525_01.cif _cod_data_source_block rac-1 _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_cell_volume 2899.3(10) _cod_database_code 1100724 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C5 C 0.8327(2) -0.18279(11) 0.41685(12) 0.0394(5) Uani 1 1 d . . . H5A H 0.8556 -0.2129 0.4635 0.047 Uiso 1 1 calc R . . C1 C 0.8832(2) -0.11163(11) 0.42426(12) 0.0360(5) Uani 1 1 d . . . H1B H 0.9418 -0.0940 0.4742 0.043 Uiso 1 1 calc R . . C2 C 0.84682(19) -0.06616(10) 0.35748(11) 0.0295(4) Uani 1 1 d . . . C3 C 0.7652(2) -0.09529(11) 0.28598(12) 0.0366(5) Uani 1 1 d . . . H3A H 0.7377 -0.0657 0.2390 0.044 Uiso 1 1 calc R . . C4 C 0.7238(2) -0.16849(11) 0.28382(13) 0.0404(5) Uani 1 1 d . . . H4A H 0.6713 -0.1885 0.2336 0.048 Uiso 1 1 calc R . . N1 N 0.75316(18) -0.21223(9) 0.34770(10) 0.0374(4) Uani 1 1 d . . . C6 C 0.8996(2) 0.01161(10) 0.36525(12) 0.0307(4) Uani 1 1 d . . . O1 O 1.02112(14) 0.02707(7) 0.40641(9) 0.0427(4) Uani 1 1 d . . . N2 N 0.80295(16) 0.06160(8) 0.32527(10) 0.0360(4) Uani 1 1 d . . . H2A H 0.7177 0.0453 0.2977 0.043 Uiso 1 1 calc R . . C7 C 0.8278(2) 0.13851(10) 0.32414(13) 0.0347(5) Uani 1 1 d . . . C8 C 0.9581(2) 0.16496(12) 0.31094(15) 0.0477(6) Uani 1 1 d . . . H8A H 1.0303 0.1313 0.3050 0.057 Uiso 1 1 calc R . . C9 C 0.9804(2) 0.23787(12) 0.30680(15) 0.0515(6) Uani 1 1 d . . . H9A H 1.0689 0.2549 0.2983 0.062 Uiso 1 1 calc R . . C10 C 0.8748(2) 0.28960(11) 0.31477(13) 0.0406(5) Uani 1 1 d . . . C11 C 0.8948(3) 0.36622(12) 0.30937(16) 0.0529(6) Uani 1 1 d . . . H11A H 0.9822 0.3842 0.3004 0.064 Uiso 1 1 calc R . . C12 C 0.7909(3) 0.41477(12) 0.31672(15) 0.0554(7) Uani 1 1 d . . . H12A H 0.8050 0.4660 0.3114 0.066 Uiso 1 1 calc R . . C13 C 0.6632(2) 0.38904(12) 0.33209(14) 0.0479(6) Uani 1 1 d . . . H13A H 0.5916 0.4231 0.3381 0.057 Uiso 1 1 calc R . . C14 C 0.6404(2) 0.31537(11) 0.33860(12) 0.0381(5) Uani 1 1 d . . . H14A H 0.5537 0.2990 0.3498 0.046 Uiso 1 1 calc R . . C15 C 0.7440(2) 0.26316(10) 0.32896(12) 0.0333(5) Uani 1 1 d . . . C16 C 0.72195(19) 0.18606(10) 0.33402(11) 0.0285(4) Uani 1 1 d . . . C17 C 0.58945(19) 0.15650(9) 0.35431(11) 0.0280(4) Uani 1 1 d . . . C18 C 0.5975(2) 0.13819(10) 0.43604(12) 0.0310(5) Uani 1 1 d . . . C19 C 0.7243(2) 0.14951(11) 0.49929(13) 0.0409(5) Uani 1 1 d . . . H19A H 0.8080 0.1696 0.4877 0.049 Uiso 1 1 calc R . . C20 C 0.7286(3) 0.13211(13) 0.57628(14) 0.0526(6) Uani 1 1 d . . . H20A H 0.8150 0.1402 0.6177 0.063 Uiso 1 1 calc R . . C21 C 0.6074(3) 0.10238(13) 0.59545(14) 0.0525(6) Uani 1 1 d . . . H21A H 0.6117 0.0907 0.6497 0.063 Uiso 1 1 calc R . . C22 C 0.4831(2) 0.09016(12) 0.53632(14) 0.0453(6) Uani 1 1 d . . . H22A H 0.4014 0.0697 0.5497 0.054 Uiso 1 1 calc R . . C23 C 0.4742(2) 0.10759(10) 0.45542(12) 0.0333(5) Uani 1 1 d . . . C24 C 0.3458(2) 0.09663(10) 0.39297(13) 0.0374(5) Uani 1 1 d . . . H24A H 0.2630 0.0761 0.4051 0.045 Uiso 1 1 calc R . . C25 C 0.3396(2) 0.11506(10) 0.31633(13) 0.0343(5) Uani 1 1 d . . . H25A H 0.2522 0.1078 0.2753 0.041 Uiso 1 1 calc R . . C26 C 0.46184(19) 0.14503(10) 0.29656(11) 0.0281(4) Uani 1 1 d . . . N3 N 0.44668(16) 0.16062(8) 0.21330(9) 0.0303(4) Uani 1 1 d . . . H3B H 0.4138 0.2037 0.1933 0.036 Uiso 1 1 calc R . . C27 C 0.48259(19) 0.10949(10) 0.16553(12) 0.0307(5) Uani 1 1 d . . . O2 O 0.54664(14) 0.05229(7) 0.19118(8) 0.0404(4) Uani 1 1 d . . . C28 C 0.4351(2) 0.12537(10) 0.07762(12) 0.0336(5) Uani 1 1 d . . . C29 C 0.4277(2) 0.19453(11) 0.04417(12) 0.0370(5) Uani 1 1 d . . . H29A H 0.4581 0.2364 0.0773 0.044 Uiso 1 1 calc R . . C30 C 0.3457(4) 0.08096(14) -0.05574(16) 0.0842(10) Uani 1 1 d . . . H30A H 0.3196 0.0400 -0.0908 0.101 Uiso 1 1 calc R . . N4 N 0.3345(3) 0.14723(10) -0.08841(12) 0.0616(6) Uani 1 1 d . . . C32 C 0.3927(3) 0.06723(12) 0.02573(14) 0.0625(8) Uani 1 1 d . . . H32A H 0.3956 0.0184 0.0457 0.075 Uiso 1 1 calc R . . C31 C 0.3757(2) 0.20221(12) -0.03793(13) 0.0458(6) Uani 1 1 d . . . H31A H 0.3691 0.2505 -0.0596 0.055 Uiso 1 1 calc R . . O50 O 1.0569(4) 0.08096(19) 0.1367(3) 0.0620(10) Uiso 0.55 1 d PD A 1 C51 C 0.9148(7) 0.0542(4) 0.1273(5) 0.063(2) Uiso 0.55 1 d PD A 1 H51A H 0.8946 0.0124 0.0893 0.075 Uiso 0.55 1 calc PR A 1 H51B H 0.9017 0.0377 0.1796 0.075 Uiso 0.55 1 calc PR A 1 C52 C 0.8230(6) 0.1135(3) 0.0971(5) 0.0610(14) Uiso 0.55 1 d PD A 1 H52A H 0.7824 0.1336 0.1397 0.073 Uiso 0.55 1 calc PR A 1 H52B H 0.7417 0.0969 0.0520 0.073 Uiso 0.55 1 calc PR A 1 C53 C 0.9064(7) 0.1708(4) 0.0689(5) 0.073(2) Uiso 0.55 1 d PD A 1 H53A H 0.9201 0.2150 0.1036 0.088 Uiso 0.55 1 calc PR A 1 H53B H 0.8602 0.1850 0.0125 0.088 Uiso 0.55 1 calc PR A 1 C54 C 1.0514(6) 0.1289(3) 0.0772(4) 0.0676(18) Uiso 0.55 1 d PD A 1 H54A H 1.0511 0.1032 0.0267 0.081 Uiso 0.55 1 calc PR A 1 H54B H 1.1349 0.1631 0.0913 0.081 Uiso 0.55 1 calc PR A 1 O60 O 0.9939(15) 0.0806(6) 0.1533(6) 0.069(3) Uiso 0.20 1 d PD B 2 C61 C 1.0656(12) 0.0810(8) 0.0941(9) 0.049(3) Uiso 0.20 1 d PD B 2 H61A H 1.0830 0.0304 0.0778 0.059 Uiso 0.20 1 calc PR B 2 H61B H 1.1594 0.1071 0.1120 0.059 Uiso 0.20 1 calc PR B 2 C62 C 0.9538(15) 0.1247(8) 0.0211(8) 0.063(4) Uiso 0.20 1 d PD B 2 H62A H 0.9960 0.1724 0.0114 0.075 Uiso 0.20 1 calc PR B 2 H62B H 0.9337 0.0954 -0.0290 0.075 Uiso 0.20 1 calc PR B 2 C63 C 0.8172(14) 0.1369(10) 0.0457(8) 0.067(4) Uiso 0.20 1 d PD B 2 H63A H 0.7408 0.1016 0.0189 0.081 Uiso 0.20 1 calc PR B 2 H63B H 0.7806 0.1876 0.0335 0.081 Uiso 0.20 1 calc PR B 2 C64 C 0.867(2) 0.1235(13) 0.1352(11) 0.120(9) Uiso 0.20 1 d PD B 2 H64A H 0.8860 0.1710 0.1640 0.144 Uiso 0.20 1 calc PR B 2 H64B H 0.7899 0.0976 0.1530 0.144 Uiso 0.20 1 calc PR B 2 C74 C 0.8123(11) 0.0939(7) 0.0615(9) 0.069(4) Uiso 0.25 1 d PD C 3 H74A H 0.7441 0.1081 0.0930 0.082 Uiso 0.25 1 calc PR C 3 H74B H 0.7588 0.0696 0.0110 0.082 Uiso 0.25 1 calc PR C 3 C73 C 0.9073(11) 0.1634(5) 0.0451(7) 0.034(3) Uiso 0.25 1 d PD C 3 H73A H 0.8593 0.1877 -0.0065 0.041 Uiso 0.25 1 calc PR C 3 H73B H 0.9219 0.1999 0.0890 0.041 Uiso 0.25 1 calc PR C 3 C72 C 1.0330(12) 0.1334(5) 0.0424(9) 0.050(3) Uiso 0.25 1 d PD C 3 H72A H 1.1130 0.1496 0.0884 0.060 Uiso 0.25 1 calc PR C 3 H72B H 1.0570 0.1460 -0.0084 0.060 Uiso 0.25 1 calc PR C 3 O70 O 0.9364(11) 0.0467(5) 0.1102(6) 0.069(3) Uiso 0.25 1 d PD C 3 C71 C 1.0047(15) 0.0548(7) 0.0469(9) 0.100(4) Uiso 0.25 1 d PD C 3 H71A H 0.9404 0.0371 -0.0046 0.120 Uiso 0.25 1 calc PR C 3 H71B H 1.0963 0.0266 0.0588 0.120 Uiso 0.25 1 calc PR C 3 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C5 0.0426(12) 0.0370(12) 0.0348(12) 0.0063(10) 0.0038(9) -0.0010(9) C1 0.0334(11) 0.0382(12) 0.0310(11) -0.0016(9) -0.0008(9) 0.0005(9) C2 0.0228(9) 0.0306(10) 0.0355(11) -0.0033(9) 0.0087(8) 0.0006(8) C3 0.0408(12) 0.0352(11) 0.0307(11) 0.0030(9) 0.0040(9) -0.0027(9) C4 0.0474(13) 0.0378(12) 0.0318(12) -0.0009(10) 0.0031(9) -0.0069(10) N1 0.0389(10) 0.0341(9) 0.0368(10) 0.0005(8) 0.0059(8) -0.0047(7) C6 0.0263(10) 0.0329(11) 0.0349(11) -0.0023(9) 0.0114(9) -0.0018(8) O1 0.0302(8) 0.0432(8) 0.0501(9) -0.0015(7) 0.0027(7) -0.0082(6) N2 0.0230(8) 0.0283(9) 0.0554(11) -0.0017(8) 0.0085(8) -0.0016(7) C7 0.0279(10) 0.0294(10) 0.0463(13) -0.0023(9) 0.0091(9) -0.0044(8) C8 0.0292(11) 0.0394(13) 0.0780(17) 0.0024(11) 0.0203(11) -0.0006(9) C9 0.0312(12) 0.0470(14) 0.0791(18) 0.0081(12) 0.0201(11) -0.0089(10) C10 0.0355(12) 0.0352(12) 0.0490(14) 0.0016(10) 0.0075(10) -0.0080(9) C11 0.0489(14) 0.0382(13) 0.0688(17) 0.0053(12) 0.0106(12) -0.0129(11) C12 0.0615(16) 0.0292(12) 0.0677(17) 0.0008(11) 0.0038(13) -0.0111(11) C13 0.0526(14) 0.0311(12) 0.0547(15) -0.0051(10) 0.0056(11) 0.0008(10) C14 0.0391(12) 0.0329(11) 0.0396(12) -0.0046(9) 0.0057(9) 0.0007(9) C15 0.0315(11) 0.0317(11) 0.0339(11) -0.0022(9) 0.0039(9) -0.0037(8) C16 0.0240(10) 0.0286(10) 0.0319(11) -0.0026(8) 0.0059(8) -0.0030(8) C17 0.0268(10) 0.0228(9) 0.0345(11) -0.0012(8) 0.0085(8) 0.0022(7) C18 0.0295(10) 0.0271(10) 0.0364(12) -0.0003(8) 0.0088(9) 0.0034(8) C19 0.0350(12) 0.0463(13) 0.0388(13) 0.0030(10) 0.0051(10) 0.0028(9) C20 0.0485(15) 0.0650(16) 0.0385(14) 0.0039(12) 0.0015(11) 0.0085(12) C21 0.0621(16) 0.0611(16) 0.0348(13) 0.0122(11) 0.0142(12) 0.0161(12) C22 0.0483(13) 0.0438(13) 0.0491(14) 0.0123(10) 0.0222(11) 0.0092(10) C23 0.0341(11) 0.0281(10) 0.0399(12) 0.0032(9) 0.0141(9) 0.0058(8) C24 0.0307(11) 0.0341(11) 0.0515(14) 0.0021(10) 0.0182(10) -0.0016(9) C25 0.0229(10) 0.0359(11) 0.0424(13) -0.0037(9) 0.0059(9) 0.0000(8) C26 0.0282(10) 0.0239(10) 0.0328(11) -0.0027(8) 0.0093(8) 0.0019(7) N3 0.0314(9) 0.0245(8) 0.0337(9) -0.0015(7) 0.0067(7) 0.0020(7) C27 0.0264(10) 0.0279(10) 0.0379(12) -0.0025(9) 0.0087(8) 0.0003(8) O2 0.0446(8) 0.0315(8) 0.0441(9) -0.0011(6) 0.0100(7) 0.0088(6) C28 0.0351(11) 0.0319(11) 0.0369(12) -0.0040(9) 0.0153(9) 0.0005(8) C29 0.0442(12) 0.0299(11) 0.0406(13) -0.0027(9) 0.0176(10) -0.0033(9) C30 0.170(3) 0.0405(15) 0.0377(15) -0.0079(12) 0.0204(17) -0.0225(17) N4 0.1051(17) 0.0459(12) 0.0358(11) -0.0006(10) 0.0222(11) -0.0097(12) C32 0.118(2) 0.0300(12) 0.0393(14) -0.0028(11) 0.0201(14) -0.0065(13) C31 0.0619(15) 0.0377(13) 0.0426(14) 0.0052(11) 0.0226(11) -0.0011(11) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C5 C1 124.02(19) . . ? C5 C1 C2 118.74(18) . . ? C3 C2 C1 118.12(17) . . ? C3 C2 C6 122.76(17) . . ? C1 C2 C6 119.11(16) . . ? C2 C3 C4 118.88(18) . . ? N1 C4 C3 123.90(19) . . ? C4 N1 C5 116.25(17) . . ? O1 C6 N2 123.94(17) . . ? O1 C6 C2 121.04(17) . . ? N2 C6 C2 115.01(16) . . ? C6 N2 C7 125.24(16) . . ? C16 C7 C8 121.18(18) . . ? C16 C7 N2 119.03(17) . . ? C8 C7 N2 119.77(18) . . ? C9 C8 C7 120.2(2) . . ? C8 C9 C10 121.43(19) . . ? C11 C10 C9 122.5(2) . . ? C11 C10 C15 119.0(2) . . ? C9 C10 C15 118.50(18) . . ? C12 C11 C10 121.2(2) . . ? C11 C12 C13 119.9(2) . . ? C14 C13 C12 120.7(2) . . ? C13 C14 C15 121.0(2) . . ? C14 C15 C10 118.09(18) . . ? C14 C15 C16 122.23(18) . . ? C10 C15 C16 119.68(18) . . ? C7 C16 C15 118.97(17) . . ? C7 C16 C17 119.96(16) . . ? C15 C16 C17 120.98(16) . . ? C26 C17 C18 118.93(17) . . ? C26 C17 C16 121.94(17) . . ? C18 C17 C16 119.11(16) . . ? C19 C18 C23 118.07(18) . . ? C19 C18 C17 122.39(18) . . ? C23 C18 C17 119.54(17) . . ? C20 C19 C18 121.1(2) . . ? C19 C20 C21 120.9(2) . . ? C22 C21 C20 120.0(2) . . ? C21 C22 C23 120.8(2) . . ? C22 C23 C24 122.06(19) . . ? C22 C23 C18 119.07(18) . . ? C24 C23 C18 118.85(18) . . ? C25 C24 C23 120.78(19) . . ? C24 C25 C26 120.69(18) . . ? C17 C26 C25 121.21(18) . . ? C17 C26 N3 122.01(17) . . ? C25 C26 N3 116.75(16) . . ? C27 N3 C26 120.20(15) . . ? O2 C27 N3 123.29(18) . . ? O2 C27 C28 121.17(17) . . ? N3 C27 C28 115.51(16) . . ? C32 C28 C29 117.1(2) . . ? C32 C28 C27 118.04(18) . . ? C29 C28 C27 124.80(18) . . ? C31 C29 C28 119.17(19) . . ? N4 C30 C32 124.5(2) . . ? C31 N4 C30 115.8(2) . . ? C28 C32 C30 118.9(2) . . ? N4 C31 C29 124.5(2) . . ? C54 O50 C51 107.3(4) . . ? C52 C51 O50 105.4(5) . . ? C51 C52 C53 109.0(5) . . ? C52 C53 C54 100.0(5) . . ? O50 C54 C53 103.9(5) . . ? C61 O60 C64 113.9(11) . . ? O60 C61 C62 102.8(9) . . ? C63 C62 C61 107.3(10) . . ? C62 C63 C64 101.9(10) . . ? O60 C64 C63 109.5(13) . . ? O70 C74 C73 98.3(7) . . ? C72 C73 C74 104.0(8) . . ? C73 C72 C71 102.5(9) . . ? C71 O70 C74 88.3(9) . . ? O70 C71 C72 105.8(11) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C5 N1 1.344(3) . ? C5 C1 1.376(3) . ? C1 C2 1.386(3) . ? C2 C3 1.378(3) . ? C2 C6 1.496(3) . ? C3 C4 1.387(3) . ? C4 N1 1.328(3) . ? C6 O1 1.223(2) . ? C6 N2 1.348(2) . ? N2 C7 1.421(2) . ? C7 C16 1.378(3) . ? C7 C8 1.413(3) . ? C8 C9 1.349(3) . ? C9 C10 1.415(3) . ? C10 C11 1.414(3) . ? C10 C15 1.424(3) . ? C11 C12 1.362(3) . ? C12 C13 1.400(3) . ? C13 C14 1.368(3) . ? C14 C15 1.416(3) . ? C15 C16 1.425(3) . ? C16 C17 1.504(3) . ? C17 C26 1.371(3) . ? C17 C18 1.431(3) . ? C18 C19 1.414(3) . ? C18 C23 1.425(3) . ? C19 C20 1.356(3) . ? C20 C21 1.399(3) . ? C21 C22 1.363(3) . ? C22 C23 1.412(3) . ? C23 C24 1.416(3) . ? C24 C25 1.351(3) . ? C25 C26 1.414(3) . ? C26 N3 1.434(3) . ? N3 C27 1.348(2) . ? C27 O2 1.229(2) . ? C27 C28 1.491(3) . ? C28 C32 1.375(3) . ? C28 C29 1.378(3) . ? C29 C31 1.378(3) . ? C30 N4 1.323(3) . ? C30 C32 1.380(3) . ? N4 C31 1.316(3) . ? O50 C54 1.338(7) . ? O50 C51 1.414(7) . ? C51 C52 1.403(8) . ? C52 C53 1.472(8) . ? C53 C54 1.557(8) . ? O60 C61 1.376(14) . ? O60 C64 1.409(16) . ? C61 C62 1.626(14) . ? C62 C63 1.497(15) . ? C63 C64 1.509(17) . ? C74 O70 1.524(13) . ? C74 C73 1.626(13) . ? C73 C72 1.334(13) . ? C72 C71 1.461(14) . ? O70 C71 1.423(13) . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2A O2 0.88 2.11 2.893(2) 147.3 . N3 H3B N1 0.88 2.19 3.008(2) 154.5 2_655
1100725.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100725.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100725 loop_ _publ_author_name 'Tara J. Burchell' 'Richard J. Puddephatt' _publ_section_title ; Self-Assembly of Chiral Coordination Polymers and Macrocycles: A Metal Template Effect on the Polymer-Macrocycle Equilibrium ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3718 _journal_page_last 3730 _journal_paper_doi 10.1021/ic050097w _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C33 H24 Cl4 Hg N4 O2' _chemical_formula_weight 850.95 _chemical_name_systematic ; ? ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 93.11(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 10.188(2) _cell_length_b 22.928(5) _cell_length_c 13.624(3) _cell_measurement_temperature 150(2) _cell_measurement_theta_max 30 _cell_measurement_theta_min 2.55 _cell_volume 3177.7(12) _computing_cell_refinement 'Nonius DENZO' _computing_data_collection 'Nonius COLLECT' _computing_data_reduction 'Nonius DENZO' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'phi\omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.055 _diffrn_reflns_av_sigmaI/netI 0.0495 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 40273 _diffrn_reflns_theta_full 28.28 _diffrn_reflns_theta_max 28.28 _diffrn_reflns_theta_min 2.56 _exptl_absorpt_coefficient_mu 5.217 _exptl_absorpt_correction_T_max 0.2625 _exptl_absorpt_correction_T_min 0.1546 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.779 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1656 _exptl_crystal_size_max 0.57 _exptl_crystal_size_mid 0.41 _exptl_crystal_size_min 0.35 _refine_diff_density_max 3.260 _refine_diff_density_min -2.900 _refine_diff_density_rms 0.161 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 390 _refine_ls_number_reflns 7892 _refine_ls_number_restraints 10 _refine_ls_restrained_S_all 1.102 _refine_ls_R_factor_all 0.0607 _refine_ls_R_factor_gt 0.0413 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0622P)^2^+3.7004P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1103 _refine_ls_wR_factor_ref 0.1170 _reflns_number_gt 6056 _reflns_number_total 7892 _reflns_threshold_expression I>2sigma(I) _cod_data_source_file ic050097wsi20050217_082525_02.cif _cod_data_source_block 3a* _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_cell_volume 3177.8(11) _cod_database_code 1100725 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hg1 Hg 1.56291(2) -0.486990(9) 0.240458(13) 0.02451(8) Uani 1 1 d . . . Cl1 Cl 1.72641(14) -0.41871(6) 0.28017(11) 0.0338(3) Uani 1 1 d . . . Cl2 Cl 1.35895(15) -0.52622(6) 0.19138(11) 0.0333(3) Uani 1 1 d . . . N1 N 1.6879(5) -0.5558(2) 0.1362(3) 0.0272(10) Uani 1 1 d . . . C1 C 1.7463(6) -0.6033(2) 0.1730(4) 0.0283(12) Uani 1 1 d . . . H1A H 1.7565 -0.6072 0.2424 0.034 Uiso 1 1 calc R . . C2 C 1.7929(5) -0.6472(2) 0.1154(4) 0.0251(12) Uani 1 1 d . . . H2A H 1.8331 -0.6807 0.1450 0.030 Uiso 1 1 calc R . . C3 C 1.7808(5) -0.6423(2) 0.0137(4) 0.0208(10) Uani 1 1 d . . . C4 C 1.7226(5) -0.5919(2) -0.0251(4) 0.0226(11) Uani 1 1 d . . . H4A H 1.7134 -0.5862 -0.0942 0.027 Uiso 1 1 calc R . . C5 C 1.6782(6) -0.5504(2) 0.0384(4) 0.0269(12) Uani 1 1 d . . . H5A H 1.6387 -0.5161 0.0112 0.032 Uiso 1 1 calc R . . C6 C 1.8292(5) -0.6913(2) -0.0474(4) 0.0226(11) Uani 1 1 d . . . O1 O 1.9080(4) -0.72758(17) -0.0131(3) 0.0293(9) Uani 1 1 d . . . N2 N 1.7801(4) -0.69307(19) -0.1411(3) 0.0236(10) Uani 1 1 d . . . H2B H 1.7191 -0.6674 -0.1589 0.028 Uiso 1 1 calc R . . C7 C 1.8192(5) -0.7331(2) -0.2136(3) 0.0214(11) Uani 1 1 d . . . C8 C 1.9505(5) -0.7331(3) -0.2418(4) 0.0305(13) Uani 1 1 d . . . H8A H 2.0145 -0.7098 -0.2069 0.037 Uiso 1 1 calc R . . C9 C 1.9856(6) -0.7663(3) -0.3186(4) 0.0341(14) Uani 1 1 d . . . H9A H 2.0741 -0.7663 -0.3371 0.041 Uiso 1 1 calc R . . C10 C 1.8901(6) -0.8010(3) -0.3713(4) 0.0289(12) Uani 1 1 d . . . C11 C 1.9231(7) -0.8328(3) -0.4562(4) 0.0389(15) Uani 1 1 d . . . H11A H 2.0106 -0.8314 -0.4768 0.047 Uiso 1 1 calc R . . C12 C 1.8320(7) -0.8652(3) -0.5082(4) 0.0393(16) Uani 1 1 d . . . H12A H 1.8554 -0.8857 -0.5652 0.047 Uiso 1 1 calc R . . C13 C 1.7024(7) -0.8680(3) -0.4772(5) 0.0409(16) Uani 1 1 d . . . H13A H 1.6387 -0.8908 -0.5133 0.049 Uiso 1 1 calc R . . C14 C 1.6675(6) -0.8382(3) -0.3951(4) 0.0320(13) Uani 1 1 d . . . H14A H 1.5804 -0.8414 -0.3741 0.038 Uiso 1 1 calc R . . C15 C 1.7593(5) -0.8027(2) -0.3416(4) 0.0241(11) Uani 1 1 d . . . C16 C 1.7241(5) -0.7678(2) -0.2600(3) 0.0206(11) Uani 1 1 d . . . C17 C 1.5893(5) -0.7685(2) -0.2235(3) 0.0208(11) Uani 1 1 d . . . C18 C 1.5628(6) -0.8033(2) -0.1396(4) 0.0285(12) Uani 1 1 d . . . C19 C 1.6614(7) -0.8385(3) -0.0922(4) 0.0413(16) Uani 1 1 d . . . H19A H 1.7471 -0.8399 -0.1165 0.050 Uiso 1 1 calc R . . C20 C 1.6325(8) -0.8709(3) -0.0106(5) 0.056(2) Uani 1 1 d . . . H20A H 1.6980 -0.8953 0.0199 0.067 Uiso 1 1 calc R . . C21 C 1.5089(9) -0.8681(4) 0.0273(6) 0.064(2) Uani 1 1 d . . . H21A H 1.4922 -0.8893 0.0852 0.076 Uiso 1 1 calc R . . C22 C 1.4119(8) -0.8356(3) -0.0171(5) 0.0499(18) Uani 1 1 d . . . H22A H 1.3270 -0.8354 0.0086 0.060 Uiso 1 1 calc R . . C23 C 1.4357(6) -0.8018(3) -0.1016(4) 0.0311(13) Uani 1 1 d . . . C24 C 1.3377(6) -0.7657(3) -0.1472(4) 0.0303(12) Uani 1 1 d . . . H24A H 1.2528 -0.7642 -0.1217 0.036 Uiso 1 1 calc R . . C25 C 1.3640(6) -0.7330(3) -0.2275(4) 0.0271(12) Uani 1 1 d . . . H25A H 1.2976 -0.7089 -0.2577 0.033 Uiso 1 1 calc R . . C26 C 1.4892(5) -0.7351(2) -0.2654(4) 0.0218(11) Uani 1 1 d . . . N3 N 1.5113(4) -0.70130(18) -0.3513(3) 0.0195(9) Uani 1 1 d . . . H3A H 1.4874 -0.7157 -0.4094 0.023 Uiso 1 1 calc R . . C27 C 1.5672(5) -0.6482(2) -0.3461(3) 0.0208(11) Uani 1 1 d . . . O2 O 1.6105(4) -0.62582(16) -0.2686(2) 0.0248(8) Uani 1 1 d . . . C28 C 1.5761(5) -0.6156(2) -0.4420(3) 0.0208(10) Uani 1 1 d . . . C29 C 1.5163(6) -0.6353(2) -0.5310(4) 0.0291(12) Uani 1 1 d . . . H29A H 1.4687 -0.6710 -0.5339 0.035 Uiso 1 1 calc R . . C30 C 1.5281(6) -0.6017(3) -0.6143(4) 0.0331(14) Uani 1 1 d . . . H30A H 1.4875 -0.6151 -0.6746 0.040 Uiso 1 1 calc R . . C31 C 1.6536(5) -0.5341(2) -0.5281(4) 0.0267(11) Uani 1 1 d . . . H31A H 1.7036 -0.4991 -0.5275 0.032 Uiso 1 1 calc R . . C32 C 1.6458(5) -0.5642(2) -0.4414(4) 0.0249(11) Uani 1 1 d . . . H32A H 1.6877 -0.5499 -0.3823 0.030 Uiso 1 1 calc R . . N4 N 1.5940(5) -0.5514(2) -0.6138(3) 0.0287(11) Uani 1 1 d . . . C50 C 1.5139(13) -1.0057(4) -0.2904(6) 0.093(3) Uiso 0.30 1 d PD A 1 H50A H 1.5634 -0.9867 -0.3421 0.112 Uiso 0.30 1 calc PR A 1 H50B H 1.4204 -1.0065 -0.3143 0.112 Uiso 0.30 1 calc PR A 1 Cl4 Cl 1.5656(3) -1.07487(15) -0.2813(2) 0.0974(9) Uiso 0.30 1 d PD A 1 Cl3 Cl 1.5245(8) -0.9644(4) -0.1956(6) 0.054(2) Uiso 0.30 1 d PD A 1 C50A C 1.5139(13) -1.0057(4) -0.2904(6) 0.093(3) Uiso 0.35 1 d P B 2 H50C H 1.4274 -1.0007 -0.2618 0.112 Uiso 0.35 1 calc PR B 2 H50D H 1.5780 -0.9785 -0.2578 0.112 Uiso 0.35 1 calc PR B 2 Cl4A Cl 1.5656(3) -1.07487(15) -0.2813(2) 0.0974(9) Uiso 0.35 1 d PD B 2 Cl5 Cl 1.5038(6) -0.9962(3) -0.4088(4) 0.0552(13) Uiso 0.35 1 d PD B 2 C50B C 1.5139(13) -1.0057(4) -0.2904(6) 0.093(3) Uiso 0.35 1 d PD C 3 H50E H 1.4235 -1.0043 -0.3209 0.112 Uiso 0.35 1 calc PR C 3 H50F H 1.5722 -0.9830 -0.3320 0.112 Uiso 0.35 1 calc PR C 3 Cl4B Cl 1.5656(3) -1.07487(15) -0.2813(2) 0.0974(9) Uiso 0.35 1 d P C 3 Cl3B Cl 1.5168(6) -0.9759(3) -0.1715(5) 0.0444(15) Uiso 0.35 1 d PD C 3 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hg1 0.03521(13) 0.02145(12) 0.01704(11) -0.00013(8) 0.00295(8) -0.00019(9) Cl1 0.0333(8) 0.0295(7) 0.0385(8) -0.0025(6) 0.0004(6) -0.0014(6) Cl2 0.0349(8) 0.0308(7) 0.0335(7) -0.0005(6) -0.0032(6) -0.0002(6) N1 0.031(3) 0.026(2) 0.025(2) -0.0044(18) 0.0038(19) 0.002(2) C1 0.037(3) 0.031(3) 0.016(2) 0.000(2) 0.001(2) 0.006(3) C2 0.032(3) 0.024(3) 0.018(2) 0.001(2) -0.001(2) 0.005(2) C3 0.020(3) 0.023(3) 0.020(2) -0.001(2) 0.002(2) -0.001(2) C4 0.028(3) 0.024(3) 0.016(2) 0.001(2) 0.005(2) 0.001(2) C5 0.033(3) 0.025(3) 0.024(3) 0.001(2) 0.005(2) 0.004(2) C6 0.026(3) 0.021(3) 0.020(2) 0.001(2) 0.001(2) 0.000(2) O1 0.038(2) 0.027(2) 0.0226(18) -0.0013(15) -0.0074(16) 0.0116(17) N2 0.023(2) 0.027(2) 0.021(2) -0.0038(18) -0.0026(18) 0.0103(19) C7 0.024(3) 0.023(3) 0.017(2) -0.002(2) -0.002(2) 0.004(2) C8 0.024(3) 0.034(3) 0.033(3) -0.008(2) -0.002(2) 0.003(2) C9 0.026(3) 0.038(4) 0.038(3) -0.006(3) 0.005(3) 0.005(3) C10 0.036(3) 0.030(3) 0.021(3) -0.001(2) 0.003(2) 0.012(2) C11 0.043(4) 0.042(4) 0.033(3) -0.004(3) 0.010(3) 0.013(3) C12 0.060(4) 0.032(3) 0.025(3) -0.008(2) 0.003(3) 0.014(3) C13 0.056(4) 0.031(3) 0.035(3) -0.013(3) -0.010(3) 0.004(3) C14 0.041(3) 0.027(3) 0.028(3) -0.002(2) -0.002(3) 0.004(3) C15 0.028(3) 0.022(3) 0.022(2) -0.002(2) -0.003(2) 0.004(2) C16 0.024(3) 0.022(3) 0.016(2) 0.0040(19) 0.000(2) 0.004(2) C17 0.028(3) 0.020(3) 0.014(2) -0.0005(19) -0.002(2) -0.001(2) C18 0.040(3) 0.024(3) 0.022(3) 0.006(2) 0.003(2) 0.002(2) C19 0.047(4) 0.043(4) 0.034(3) 0.015(3) 0.002(3) 0.005(3) C20 0.066(5) 0.053(5) 0.047(4) 0.034(4) 0.004(4) 0.011(4) C21 0.093(7) 0.059(5) 0.039(4) 0.032(4) 0.009(4) -0.001(5) C22 0.056(5) 0.054(5) 0.041(4) 0.010(3) 0.018(3) -0.009(4) C23 0.044(4) 0.026(3) 0.024(3) 0.002(2) 0.006(2) -0.008(3) C24 0.029(3) 0.031(3) 0.032(3) -0.002(2) 0.010(2) -0.005(2) C25 0.028(3) 0.029(3) 0.024(3) -0.002(2) 0.000(2) 0.001(2) C26 0.028(3) 0.016(2) 0.021(2) -0.0008(19) -0.001(2) -0.002(2) N3 0.026(2) 0.019(2) 0.0133(18) 0.0016(16) -0.0030(17) -0.0013(17) C27 0.021(3) 0.021(3) 0.020(2) 0.0010(19) 0.001(2) 0.007(2) O2 0.034(2) 0.0219(19) 0.0175(17) 0.0006(14) -0.0061(15) -0.0025(16) C28 0.024(3) 0.022(3) 0.016(2) 0.0028(19) 0.001(2) 0.001(2) C29 0.038(3) 0.028(3) 0.021(2) 0.001(2) -0.007(2) -0.009(3) C30 0.047(4) 0.033(3) 0.019(3) 0.002(2) -0.005(2) -0.013(3) C31 0.032(3) 0.024(3) 0.024(3) 0.003(2) 0.001(2) -0.003(2) C32 0.029(3) 0.026(3) 0.019(2) -0.002(2) -0.002(2) -0.001(2) N4 0.042(3) 0.027(3) 0.017(2) 0.0018(18) 0.002(2) -0.004(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Hg1 Cl2 160.47(5) . . ? Cl1 Hg1 N4 98.95(11) . 1_556 ? Cl2 Hg1 N4 94.19(12) . 1_556 ? Cl1 Hg1 N1 100.10(11) . . ? Cl2 Hg1 N1 93.82(11) . . ? N4 Hg1 N1 91.83(15) 1_556 . ? C1 N1 C5 117.4(5) . . ? C1 N1 Hg1 122.1(3) . . ? C5 N1 Hg1 119.5(4) . . ? N1 C1 C2 123.1(5) . . ? C1 C2 C3 119.6(5) . . ? C2 C3 C4 117.4(5) . . ? C2 C3 C6 118.6(5) . . ? C4 C3 C6 124.0(4) . . ? C5 C4 C3 118.9(5) . . ? N1 C5 C4 123.5(5) . . ? O1 C6 N2 122.8(5) . . ? O1 C6 C3 121.6(4) . . ? N2 C6 C3 115.6(4) . . ? C6 N2 C7 125.0(4) . . ? C16 C7 C8 121.8(5) . . ? C16 C7 N2 118.3(5) . . ? C8 C7 N2 119.7(5) . . ? C9 C8 C7 120.2(5) . . ? C8 C9 C10 120.1(6) . . ? C15 C10 C9 120.0(5) . . ? C15 C10 C11 119.1(5) . . ? C9 C10 C11 120.8(6) . . ? C12 C11 C10 121.3(6) . . ? C11 C12 C13 119.6(6) . . ? C14 C13 C12 120.6(6) . . ? C13 C14 C15 120.9(6) . . ? C14 C15 C10 118.5(5) . . ? C14 C15 C16 122.4(5) . . ? C10 C15 C16 119.1(5) . . ? C7 C16 C15 118.6(5) . . ? C7 C16 C17 119.4(5) . . ? C15 C16 C17 122.0(5) . . ? C26 C17 C18 118.4(5) . . ? C26 C17 C16 122.2(4) . . ? C18 C17 C16 119.4(5) . . ? C19 C18 C23 119.1(5) . . ? C19 C18 C17 121.4(6) . . ? C23 C18 C17 119.5(5) . . ? C20 C19 C18 119.7(7) . . ? C19 C20 C21 120.9(7) . . ? C22 C21 C20 120.9(6) . . ? C21 C22 C23 120.7(7) . . ? C24 C23 C18 119.3(5) . . ? C24 C23 C22 121.9(6) . . ? C18 C23 C22 118.8(6) . . ? C25 C24 C23 120.6(5) . . ? C24 C25 C26 119.9(5) . . ? C17 C26 C25 122.3(5) . . ? C17 C26 N3 119.7(5) . . ? C25 C26 N3 118.0(5) . . ? C27 N3 C26 122.1(4) . . ? O2 C27 N3 123.6(5) . . ? O2 C27 C28 119.8(5) . . ? N3 C27 C28 116.6(4) . . ? C32 C28 C29 118.8(5) . . ? C32 C28 C27 118.3(4) . . ? C29 C28 C27 122.9(5) . . ? C30 C29 C28 118.5(5) . . ? N4 C30 C29 122.9(5) . . ? N4 C31 C32 123.5(5) . . ? C28 C32 C31 118.7(5) . . ? C30 N4 C31 117.6(5) . . ? C30 N4 Hg1 117.9(3) . 1_554 ? C31 N4 Hg1 123.3(4) . 1_554 ? Cl3 C50 Cl4 119.6(7) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg1 Cl1 2.3282(15) . ? Hg1 Cl2 2.3289(15) . ? Hg1 N4 2.482(4) 1_556 ? Hg1 N1 2.515(5) . ? N1 C1 1.327(7) . ? N1 C5 1.336(7) . ? C1 C2 1.377(7) . ? C2 C3 1.389(7) . ? C3 C4 1.389(7) . ? C3 C6 1.498(7) . ? C4 C5 1.379(7) . ? C6 O1 1.230(6) . ? C6 N2 1.346(6) . ? N2 C7 1.422(6) . ? C7 C16 1.381(7) . ? C7 C8 1.411(7) . ? C8 C9 1.356(8) . ? C9 C10 1.422(8) . ? C10 C15 1.414(8) . ? C10 C11 1.422(8) . ? C11 C12 1.357(9) . ? C12 C13 1.409(10) . ? C13 C14 1.374(8) . ? C14 C15 1.411(8) . ? C15 C16 1.431(7) . ? C16 C17 1.486(7) . ? C17 C26 1.375(7) . ? C17 C18 1.432(7) . ? C18 C19 1.417(8) . ? C18 C23 1.421(8) . ? C19 C20 1.382(9) . ? C20 C21 1.388(11) . ? C21 C22 1.354(11) . ? C22 C23 1.420(8) . ? C23 C24 1.415(8) . ? C24 C25 1.365(8) . ? C25 C26 1.403(8) . ? C26 N3 1.431(6) . ? N3 C27 1.344(7) . ? C27 O2 1.235(6) . ? C27 C28 1.512(7) . ? C28 C32 1.374(7) . ? C28 C29 1.403(7) . ? C29 C30 1.383(7) . ? C30 N4 1.334(7) . ? C31 N4 1.347(7) . ? C31 C32 1.374(7) . ? N4 Hg1 2.482(4) 1_554 ? C50 Cl3 1.599(10) . ? C50 Cl4 1.674(8) . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2B O2 0.88 2.05 2.837(5) 149.1 . N3 H3A O1 0.88 2.05 2.894(5) 159.5 4_545
1100726.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100726.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100726 loop_ _publ_author_name 'Tara J. Burchell' 'Richard J. Puddephatt' _publ_section_title ; Self-Assembly of Chiral Coordination Polymers and Macrocycles: A Metal Template Effect on the Polymer-Macrocycle Equilibrium ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3718 _journal_page_last 3730 _journal_paper_doi 10.1021/ic050097w _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C33 H24 Cl4 Hg N4 O2' _chemical_formula_weight 850.95 _chemical_name_systematic ; ? ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 103.84(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 17.124(3) _cell_length_b 11.727(2) _cell_length_c 16.249(3) _cell_measurement_reflns_used 7532 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 27.4 _cell_measurement_theta_min 1.70 _cell_volume 3168.3(11) _computing_cell_refinement 'Nonius DENZO' _computing_data_collection 'Nonius COLLECT' _computing_data_reduction 'Nonius DENZO' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'phi\omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.113 _diffrn_reflns_av_sigmaI/netI 0.1045 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 36528 _diffrn_reflns_theta_full 25.03 _diffrn_reflns_theta_max 25.03 _diffrn_reflns_theta_min 2.58 _exptl_absorpt_coefficient_mu 5.233 _exptl_absorpt_correction_T_max 0.7799 _exptl_absorpt_correction_T_min 0.3545 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.784 _exptl_crystal_density_method 'not measured' _exptl_crystal_description rod _exptl_crystal_F_000 1656 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _refine_diff_density_max 1.373 _refine_diff_density_min -1.173 _refine_diff_density_rms 0.158 _refine_ls_extinction_coef 0.00066(10) _refine_ls_extinction_expression Fc^^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 0.910 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 398 _refine_ls_number_reflns 5589 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.910 _refine_ls_R_factor_all 0.0920 _refine_ls_R_factor_gt 0.0432 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0468P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0840 _refine_ls_wR_factor_ref 0.0983 _reflns_number_gt 3502 _reflns_number_total 5589 _reflns_threshold_expression I>2sigma(I) _cod_data_source_file ic050097wsi20050217_082525_03.cif _cod_data_source_block 3a* _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_cell_volume 3168.2(11) _cod_database_code 1100726 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hg1 Hg 0.340571(17) 0.70129(3) 0.025233(18) 0.03244(13) Uani 1 1 d . . . Cl1 Cl 0.26623(11) 0.60244(19) -0.09621(11) 0.0399(5) Uani 1 1 d . . . Cl2 Cl 0.36134(14) 0.7404(2) 0.16986(12) 0.0517(6) Uani 1 1 d . . . N1 N 0.3128(3) 0.8827(5) -0.0431(3) 0.0270(15) Uani 1 1 d . . . N2 N 0.2428(3) 1.2150(5) -0.2402(3) 0.0249(15) Uani 1 1 d . . . H2A H 0.2666 1.1590 -0.2608 0.030 Uiso 1 1 calc R . . N3 N 0.2439(3) 1.1232(5) -0.4569(3) 0.0250(15) Uani 1 1 d . . . H3A H 0.2400 1.1545 -0.5069 0.030 Uiso 1 1 calc R . . N4 N 0.5327(3) 1.1690(5) -0.4896(4) 0.0326(17) Uani 1 1 d . . . O1 O 0.2101(3) 1.2822(4) -0.1215(3) 0.0310(13) Uani 1 1 d . . . O2 O 0.3257(3) 1.0731(5) -0.3307(3) 0.0350(14) Uani 1 1 d . . . C1 C 0.3179(4) 0.9799(8) 0.0013(4) 0.032(2) Uani 1 1 d . . . H1A H 0.3406 0.9765 0.0606 0.038 Uiso 1 1 calc R . . C2 C 0.2925(4) 1.0844(6) -0.0337(4) 0.0232(17) Uani 1 1 d . . . H2B H 0.2958 1.1504 0.0009 0.028 Uiso 1 1 calc R . . C3 C 0.2620(4) 1.0911(7) -0.1200(4) 0.0239(18) Uani 1 1 d . . . C4 C 0.2557(4) 0.9926(7) -0.1663(4) 0.0281(19) Uani 1 1 d . . . H4A H 0.2334 0.9944 -0.2257 0.034 Uiso 1 1 calc R . . C5 C 0.2816(4) 0.8907(7) -0.1267(4) 0.034(2) Uani 1 1 d . . . H5A H 0.2772 0.8235 -0.1601 0.040 Uiso 1 1 calc R . . C6 C 0.2354(4) 1.2047(7) -0.1591(4) 0.0251(17) Uani 1 1 d . . . C7 C 0.2151(4) 1.3088(7) -0.2942(4) 0.0253(17) Uani 1 1 d . . . C8 C 0.2433(4) 1.4198(7) -0.2694(4) 0.0255(18) Uani 1 1 d . . . H8A H 0.2793 1.4324 -0.2158 0.031 Uiso 1 1 calc R . . C9 C 0.2182(4) 1.5082(7) -0.3234(5) 0.037(2) Uani 1 1 d . . . H9A H 0.2358 1.5832 -0.3063 0.044 Uiso 1 1 calc R . . C10 C 0.1659(4) 1.4908(7) -0.4051(5) 0.031(2) Uani 1 1 d . . . C11 C 0.1417(5) 1.5819(8) -0.4640(5) 0.045(2) Uani 1 1 d . . . H11A H 0.1584 1.6576 -0.4479 0.053 Uiso 1 1 calc R . . C12 C 0.0949(5) 1.5614(9) -0.5424(5) 0.048(3) Uani 1 1 d . . . H12A H 0.0797 1.6226 -0.5813 0.057 Uiso 1 1 calc R . . C13 C 0.0694(5) 1.4524(9) -0.5661(5) 0.044(2) Uani 1 1 d . . . H13A H 0.0365 1.4397 -0.6213 0.053 Uiso 1 1 calc R . . C14 C 0.0901(4) 1.3624(8) -0.5125(4) 0.037(2) Uani 1 1 d . . . H14A H 0.0713 1.2882 -0.5306 0.045 Uiso 1 1 calc R . . C15 C 0.1398(4) 1.3786(8) -0.4292(4) 0.0300(19) Uani 1 1 d . . . C16 C 0.1648(4) 1.2855(7) -0.3713(4) 0.0242(18) Uani 1 1 d . . . C17 C 0.1343(4) 1.1681(7) -0.3906(4) 0.0276(19) Uani 1 1 d . . . C18 C 0.0661(4) 1.1305(7) -0.3607(4) 0.029(2) Uani 1 1 d . . . C19 C 0.0241(4) 1.2035(8) -0.3178(5) 0.039(2) Uani 1 1 d . . . H19A H 0.0404 1.2808 -0.3085 0.047 Uiso 1 1 calc R . . C20 C -0.0396(5) 1.1642(9) -0.2894(5) 0.051(3) Uani 1 1 d . . . H20A H -0.0671 1.2145 -0.2602 0.062 Uiso 1 1 calc R . . C21 C -0.0655(5) 1.0505(9) -0.3026(5) 0.051(3) Uani 1 1 d . . . H21A H -0.1105 1.0248 -0.2830 0.061 Uiso 1 1 calc R . . C22 C -0.0263(4) 0.9773(9) -0.3435(5) 0.050(3) Uani 1 1 d . . . H22A H -0.0439 0.9004 -0.3516 0.059 Uiso 1 1 calc R . . C23 C 0.0409(4) 1.0138(8) -0.3744(4) 0.035(2) Uani 1 1 d . . . C24 C 0.0804(4) 0.9389(8) -0.4186(4) 0.041(2) Uani 1 1 d . . . H24A H 0.0622 0.8627 -0.4296 0.049 Uiso 1 1 calc R . . C25 C 0.1448(4) 0.9774(7) -0.4454(4) 0.035(2) Uani 1 1 d . . . H25A H 0.1722 0.9262 -0.4741 0.042 Uiso 1 1 calc R . . C26 C 0.1725(4) 1.0901(7) -0.4321(4) 0.0273(19) Uani 1 1 d . . . C27 C 0.3170(4) 1.1072(7) -0.4047(4) 0.0268(18) Uani 1 1 d . . . C28 C 0.3905(4) 1.1306(7) -0.4382(4) 0.0283(19) Uani 1 1 d . . . C29 C 0.4624(4) 1.1454(7) -0.3788(4) 0.034(2) Uani 1 1 d . . . H29A H 0.4641 1.1434 -0.3199 0.041 Uiso 1 1 calc R . . C30 C 0.5320(4) 1.1634(7) -0.4065(5) 0.041(2) Uani 1 1 d . . . H30A H 0.5814 1.1722 -0.3653 0.050 Uiso 1 1 calc R . . C31 C 0.4622(4) 1.1528(7) -0.5453(5) 0.033(2) Uani 1 1 d . . . H31A H 0.4612 1.1555 -0.6040 0.040 Uiso 1 1 calc R . . C32 C 0.3916(4) 1.1325(7) -0.5229(4) 0.0297(19) Uani 1 1 d . . . H32A H 0.3435 1.1197 -0.5653 0.036 Uiso 1 1 calc R . . C40 C 0.4682(5) 1.5466(8) -0.6866(5) 0.052(3) Uani 1 1 d . . . H40A H 0.4521 1.6141 -0.6581 0.062 Uiso 1 1 calc R . . H40B H 0.4263 1.5333 -0.7394 0.062 Uiso 1 1 calc R . . Cl3 Cl 0.55969(12) 1.5756(2) -0.71279(13) 0.0550(7) Uani 1 1 d . . . Cl4 Cl 0.47290(14) 1.4286(3) -0.62088(17) 0.0865(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hg1 0.03329(19) 0.0314(2) 0.03407(19) 0.00340(17) 0.01083(13) 0.00414(17) Cl1 0.0438(12) 0.0320(14) 0.0418(11) -0.0021(10) 0.0060(9) -0.0055(11) Cl2 0.0702(15) 0.0526(17) 0.0308(11) 0.0033(11) 0.0090(10) 0.0163(13) N1 0.033(3) 0.021(4) 0.026(3) 0.007(3) 0.005(3) 0.003(3) N2 0.034(3) 0.020(4) 0.025(3) 0.000(3) 0.014(3) 0.014(3) N3 0.022(3) 0.026(4) 0.029(3) 0.003(3) 0.011(3) 0.001(3) N4 0.022(3) 0.042(5) 0.035(4) -0.004(3) 0.009(3) 0.000(3) O1 0.045(3) 0.025(4) 0.024(3) -0.003(3) 0.010(2) 0.007(3) O2 0.035(3) 0.048(4) 0.024(3) 0.003(3) 0.011(2) 0.000(3) C1 0.030(4) 0.047(6) 0.023(4) -0.007(4) 0.012(3) -0.015(4) C2 0.033(4) 0.010(5) 0.029(4) -0.001(4) 0.011(3) -0.001(4) C3 0.016(4) 0.025(5) 0.032(4) -0.006(4) 0.008(3) -0.001(4) C4 0.029(4) 0.033(6) 0.022(4) 0.003(4) 0.006(3) -0.004(4) C5 0.043(5) 0.032(6) 0.026(4) 0.001(4) 0.007(4) 0.001(4) C6 0.024(4) 0.026(5) 0.024(4) -0.001(4) 0.003(3) -0.001(4) C7 0.032(4) 0.017(5) 0.029(4) 0.008(4) 0.011(3) 0.008(4) C8 0.031(4) 0.024(5) 0.025(4) 0.000(4) 0.014(3) 0.005(4) C9 0.045(5) 0.029(6) 0.044(5) -0.003(4) 0.025(4) -0.003(4) C10 0.029(4) 0.031(6) 0.040(5) 0.011(4) 0.023(4) 0.010(4) C11 0.043(5) 0.033(6) 0.066(6) 0.021(5) 0.030(5) 0.017(5) C12 0.042(5) 0.058(8) 0.044(5) 0.031(5) 0.013(4) 0.018(5) C13 0.033(5) 0.062(8) 0.035(5) 0.013(5) 0.003(4) 0.007(5) C14 0.029(4) 0.049(6) 0.034(5) 0.010(4) 0.010(4) 0.009(4) C15 0.031(4) 0.035(6) 0.030(4) 0.008(4) 0.018(3) 0.007(4) C16 0.021(4) 0.027(5) 0.026(4) 0.005(4) 0.011(3) 0.000(4) C17 0.022(4) 0.036(6) 0.026(4) 0.000(4) 0.007(3) -0.004(4) C18 0.022(4) 0.040(6) 0.023(4) 0.014(4) 0.003(3) 0.004(4) C19 0.029(4) 0.048(6) 0.041(5) 0.013(5) 0.011(4) 0.004(5) C20 0.041(5) 0.069(8) 0.052(6) 0.012(5) 0.025(4) 0.013(5) C21 0.028(5) 0.074(9) 0.053(6) 0.023(6) 0.018(4) -0.008(5) C22 0.028(5) 0.078(8) 0.041(5) 0.016(5) 0.005(4) -0.009(5) C23 0.023(4) 0.053(7) 0.027(4) 0.011(4) 0.004(3) -0.014(4) C24 0.036(5) 0.050(7) 0.040(5) 0.001(4) 0.016(4) -0.012(4) C25 0.039(5) 0.034(6) 0.031(4) -0.003(4) 0.006(4) -0.003(4) C26 0.021(4) 0.038(6) 0.023(4) -0.002(4) 0.007(3) 0.000(4) C27 0.025(4) 0.030(5) 0.027(4) -0.007(4) 0.012(3) 0.001(4) C28 0.033(4) 0.031(5) 0.026(4) -0.002(4) 0.017(3) -0.003(4) C29 0.041(5) 0.041(6) 0.024(4) -0.004(4) 0.016(4) -0.009(4) C30 0.028(4) 0.065(7) 0.032(5) -0.006(4) 0.009(3) 0.000(4) C31 0.035(5) 0.037(6) 0.033(4) 0.003(4) 0.020(4) 0.002(4) C32 0.030(4) 0.032(6) 0.027(4) -0.004(4) 0.007(3) 0.000(4) C40 0.044(5) 0.053(7) 0.061(6) 0.006(5) 0.016(4) -0.013(5) Cl3 0.0439(12) 0.069(2) 0.0516(13) 0.0126(13) 0.0111(10) -0.0015(13) Cl4 0.0490(15) 0.121(3) 0.0928(19) 0.0526(19) 0.0232(14) 0.0088(16) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl2 Hg1 Cl1 148.51(8) . . ? Cl2 Hg1 N1 104.93(15) . . ? Cl1 Hg1 N1 92.32(15) . . ? Cl2 Hg1 N4 110.10(15) . 2_644 ? Cl1 Hg1 N4 93.35(15) . 2_644 ? N1 Hg1 N4 96.8(2) . 2_644 ? C5 N1 C1 116.4(7) . . ? C5 N1 Hg1 121.3(5) . . ? C1 N1 Hg1 121.7(5) . . ? C6 N2 C7 125.1(6) . . ? C27 N3 C26 120.9(6) . . ? C31 N4 C30 116.4(6) . . ? C31 N4 Hg1 125.5(5) . 2_654 ? C30 N4 Hg1 118.1(5) . 2_654 ? N1 C1 C2 124.1(6) . . ? C3 C2 C1 118.5(7) . . ? C4 C3 C2 118.2(7) . . ? C4 C3 C6 122.8(6) . . ? C2 C3 C6 119.0(7) . . ? C3 C4 C5 120.0(7) . . ? N1 C5 C4 122.7(8) . . ? O1 C6 N2 122.8(7) . . ? O1 C6 C3 123.6(6) . . ? N2 C6 C3 113.6(7) . . ? C16 C7 C8 122.9(7) . . ? C16 C7 N2 117.2(7) . . ? C8 C7 N2 119.9(6) . . ? C9 C8 C7 119.0(7) . . ? C8 C9 C10 121.5(8) . . ? C15 C10 C11 119.3(7) . . ? C15 C10 C9 118.4(7) . . ? C11 C10 C9 122.3(8) . . ? C12 C11 C10 120.6(9) . . ? C11 C12 C13 120.3(8) . . ? C14 C13 C12 121.7(8) . . ? C13 C14 C15 120.6(8) . . ? C10 C15 C14 117.6(7) . . ? C10 C15 C16 120.0(7) . . ? C14 C15 C16 122.4(8) . . ? C7 C16 C15 118.1(7) . . ? C7 C16 C17 119.6(7) . . ? C15 C16 C17 122.2(6) . . ? C26 C17 C18 118.5(7) . . ? C26 C17 C16 122.2(6) . . ? C18 C17 C16 119.2(7) . . ? C19 C18 C23 119.2(7) . . ? C19 C18 C17 122.3(8) . . ? C23 C18 C17 118.5(7) . . ? C20 C19 C18 120.5(9) . . ? C19 C20 C21 121.2(9) . . ? C22 C21 C20 120.0(8) . . ? C21 C22 C23 121.2(9) . . ? C24 C23 C22 121.2(8) . . ? C24 C23 C18 120.8(7) . . ? C22 C23 C18 117.9(8) . . ? C25 C24 C23 118.9(8) . . ? C24 C25 C26 122.3(8) . . ? C17 C26 C25 120.9(7) . . ? C17 C26 N3 119.4(7) . . ? C25 C26 N3 119.5(7) . . ? O2 C27 N3 122.2(6) . . ? O2 C27 C28 119.3(6) . . ? N3 C27 C28 118.5(6) . . ? C29 C28 C32 118.2(6) . . ? C29 C28 C27 116.8(6) . . ? C32 C28 C27 124.9(6) . . ? C28 C29 C30 118.9(6) . . ? N4 C30 C29 123.0(7) . . ? N4 C31 C32 124.0(7) . . ? C31 C32 C28 119.5(7) . . ? Cl4 C40 Cl3 113.0(5) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg1 Cl2 2.337(2) . ? Hg1 Cl1 2.378(2) . ? Hg1 N1 2.394(6) . ? Hg1 N4 2.406(6) 2_644 ? N1 C5 1.338(8) . ? N1 C1 1.341(9) . ? N2 C6 1.359(8) . ? N2 C7 1.415(8) . ? N3 C27 1.346(8) . ? N3 C26 1.430(8) . ? N4 C31 1.338(8) . ? N4 C30 1.356(9) . ? N4 Hg1 2.406(6) 2_654 ? O1 C6 1.231(8) . ? O2 C27 1.242(7) . ? C1 C2 1.377(10) . ? C2 C3 1.376(9) . ? C3 C4 1.368(10) . ? C3 C6 1.500(10) . ? C4 C5 1.379(10) . ? C7 C16 1.367(9) . ? C7 C8 1.413(10) . ? C8 C9 1.359(10) . ? C9 C10 1.428(10) . ? C10 C15 1.415(11) . ? C10 C11 1.427(10) . ? C11 C12 1.355(11) . ? C12 C13 1.376(11) . ? C13 C14 1.360(11) . ? C14 C15 1.429(10) . ? C15 C16 1.439(10) . ? C16 C17 1.479(10) . ? C17 C26 1.389(10) . ? C17 C18 1.438(10) . ? C18 C19 1.405(10) . ? C18 C23 1.435(11) . ? C19 C20 1.363(11) . ? C20 C21 1.405(12) . ? C21 C22 1.356(12) . ? C22 C23 1.428(10) . ? C23 C24 1.406(11) . ? C24 C25 1.356(10) . ? C25 C26 1.403(11) . ? C27 C28 1.512(9) . ? C28 C29 1.382(9) . ? C28 C32 1.381(9) . ? C29 C30 1.387(10) . ? C31 C32 1.364(9) . ? C40 Cl4 1.737(8) . ? C40 Cl3 1.752(8) . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2A O2 0.88 1.97 2.819(7) 161.7 . N3 H3A O1 0.88 1.95 2.824(7) 169.3 4_585
1100727.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100727.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100727 loop_ _publ_author_name 'Tara J. Burchell' 'Richard J. Puddephatt' _publ_section_title ; Self-Assembly of Chiral Coordination Polymers and Macrocycles: A Metal Template Effect on the Polymer-Macrocycle Equilibrium ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3718 _journal_page_last 3730 _journal_paper_doi 10.1021/ic050097w _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C33 H24 Br2 Cl2 Hg N4 O2' _chemical_formula_weight 939.87 _chemical_name_systematic ; ? ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 103.34(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 17.239(3) _cell_length_b 11.940(2) _cell_length_c 16.268(3) _cell_measurement_reflns_used 7735 _cell_measurement_temperature 123(2) _cell_measurement_theta_max 27.48 _cell_measurement_theta_min 1.70 _cell_volume 3258.2(11) _computing_cell_refinement 'Nonius DENZO' _computing_data_collection 'Nonius COLLECT' _computing_data_reduction 'Nonius DENZO' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 123(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'phi\omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.072 _diffrn_reflns_av_sigmaI/netI 0.0520 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 36306 _diffrn_reflns_theta_full 25.03 _diffrn_reflns_theta_max 25.03 _diffrn_reflns_theta_min 2.57 _exptl_absorpt_coefficient_mu 7.378 _exptl_absorpt_correction_T_max 0.5258 _exptl_absorpt_correction_T_min 0.0723 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.916 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 1800 _exptl_crystal_size_max 0.75 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.10 _refine_diff_density_max 1.371 _refine_diff_density_min -1.336 _refine_diff_density_rms 0.133 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 401 _refine_ls_number_reflns 5744 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.018 _refine_ls_R_factor_all 0.0631 _refine_ls_R_factor_gt 0.0426 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0530P)^2^+11.3000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1016 _refine_ls_wR_factor_ref 0.1092 _reflns_number_gt 4461 _reflns_number_total 5744 _reflns_threshold_expression I>2sigma(I) _cod_data_source_file ic050097wsi20050217_082525_04.cif _cod_data_source_block 3b _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_database_code 1100727 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hg1 Hg 0.656578(18) -1.28664(2) -0.022004(17) 0.03552(12) Uani 1 1 d . . . Br1 Br 0.63993(7) -1.25596(9) -0.17440(5) 0.0661(3) Uani 1 1 d . . . Br2 Br 0.73298(6) -1.39146(7) 0.10382(5) 0.0503(2) Uani 1 1 d . . . N1 N 0.6856(4) -1.1071(5) 0.0444(4) 0.0359(15) Uani 1 1 d . . . C1 C 0.7166(5) -1.1006(6) 0.1288(4) 0.0343(18) Uani 1 1 d . . . H1A H 0.7207 -1.1671 0.1616 0.041 Uiso 1 1 calc R . . C2 C 0.7420(5) -1.0021(6) 0.1683(4) 0.0357(18) Uani 1 1 d . . . H2A H 0.7629 -1.0011 0.2277 0.043 Uiso 1 1 calc R . . C3 C 0.7374(4) -0.9031(6) 0.1223(4) 0.0296(16) Uani 1 1 d . . . C4 C 0.7084(4) -0.9102(6) 0.0354(4) 0.0299(16) Uani 1 1 d . . . H4A H 0.7064 -0.8454 0.0011 0.036 Uiso 1 1 calc R . . C5 C 0.6824(4) -1.0124(6) -0.0005(4) 0.0325(17) Uani 1 1 d . . . H5A H 0.6612 -1.0157 -0.0598 0.039 Uiso 1 1 calc R . . C6 C 0.7644(4) -0.7930(6) 0.1630(4) 0.0291(16) Uani 1 1 d . . . O1 O 0.7875(3) -0.7163(4) 0.1238(3) 0.0361(12) Uani 1 1 d . . . N2 N 0.7615(3) -0.7857(5) 0.2435(3) 0.0290(13) Uani 1 1 d . . . H2B H 0.7406 -0.8432 0.2645 0.035 Uiso 1 1 calc R . . C7 C 0.7887(4) -0.6948(6) 0.3000(4) 0.0306(17) Uani 1 1 d . . . C8 C 0.7635(5) -0.5844(6) 0.2767(5) 0.0345(18) Uani 1 1 d . . . H8A H 0.7289 -0.5700 0.2232 0.041 Uiso 1 1 calc R . . C9 C 0.7892(5) -0.4987(6) 0.3315(5) 0.0374(19) Uani 1 1 d . . . H9A H 0.7731 -0.4243 0.3152 0.045 Uiso 1 1 calc R . . C10 C 0.8390(5) -0.5177(7) 0.4114(5) 0.041(2) Uani 1 1 d . . . C11 C 0.8632(5) -0.4315(8) 0.4709(6) 0.052(2) Uani 1 1 d . . . H11A H 0.8473 -0.3566 0.4560 0.062 Uiso 1 1 calc R . . C12 C 0.9082(6) -0.4527(9) 0.5483(6) 0.060(3) Uani 1 1 d . . . H12A H 0.9232 -0.3930 0.5874 0.072 Uiso 1 1 calc R . . C13 C 0.9328(6) -0.5605(10) 0.5716(6) 0.063(3) Uani 1 1 d . . . H13A H 0.9650 -0.5736 0.6266 0.075 Uiso 1 1 calc R . . C14 C 0.9119(5) -0.6496(8) 0.5172(5) 0.044(2) Uani 1 1 d . . . H14A H 0.9297 -0.7230 0.5346 0.053 Uiso 1 1 calc R . . C15 C 0.8643(4) -0.6313(7) 0.4360(4) 0.0350(18) Uani 1 1 d . . . C16 C 0.8391(4) -0.7201(6) 0.3768(4) 0.0290(16) Uani 1 1 d . . . C17 C 0.8668(4) -0.8379(6) 0.3936(4) 0.0305(17) Uani 1 1 d . . . C18 C 0.9349(4) -0.8756(7) 0.3640(4) 0.0389(19) Uani 1 1 d . . . C19 C 0.9783(5) -0.8027(8) 0.3225(5) 0.047(2) Uani 1 1 d . . . H19A H 0.9631 -0.7263 0.3140 0.057 Uiso 1 1 calc R . . C20 C 1.0418(5) -0.8426(10) 0.2948(5) 0.059(3) Uani 1 1 d . . . H20A H 1.0719 -0.7928 0.2687 0.071 Uiso 1 1 calc R . . C21 C 1.0637(5) -0.9560(10) 0.3043(6) 0.060(3) Uani 1 1 d . . . H21A H 1.1068 -0.9825 0.2822 0.072 Uiso 1 1 calc R . . C22 C 1.0244(5) -1.0275(9) 0.3442(5) 0.056(3) Uani 1 1 d . . . H22A H 1.0406 -1.1036 0.3511 0.068 Uiso 1 1 calc R . . C23 C 0.9581(5) -0.9897(7) 0.3763(5) 0.041(2) Uani 1 1 d . . . C24 C 0.9146(5) -1.0633(8) 0.4166(5) 0.050(2) Uani 1 1 d . . . H24A H 0.9291 -1.1401 0.4229 0.060 Uiso 1 1 calc R . . C25 C 0.8521(5) -1.0253(7) 0.4465(5) 0.045(2) Uani 1 1 d . . . H25A H 0.8249 -1.0747 0.4760 0.053 Uiso 1 1 calc R . . C26 C 0.8276(4) -0.9125(6) 0.4337(4) 0.0311(17) Uani 1 1 d . . . N3 N 0.7567(3) -0.8789(5) 0.4599(3) 0.0291(13) Uani 1 1 d . . . H3A H 0.7603 -0.8504 0.5105 0.035 Uiso 1 1 calc R . . C27 C 0.6854(4) -0.8913(6) 0.4068(4) 0.0312(17) Uani 1 1 d . . . O2 O 0.6765(3) -0.9234(5) 0.3331(3) 0.0385(13) Uani 1 1 d . . . C28 C 0.6119(4) -0.8659(6) 0.4397(4) 0.0297(16) Uani 1 1 d . . . C29 C 0.5420(6) -0.8445(9) 0.3808(5) 0.064(3) Uani 1 1 d . . . H29A H 0.5411 -0.8451 0.3222 0.077 Uiso 1 1 calc R . . C30 C 0.4736(5) -0.8222(10) 0.4079(5) 0.066(3) Uani 1 1 d . . . H30A H 0.4257 -0.8095 0.3666 0.079 Uiso 1 1 calc R . . C31 C 0.5380(4) -0.8420(6) 0.5449(4) 0.0337(17) Uani 1 1 d . . . H31A H 0.5371 -0.8422 0.6030 0.040 Uiso 1 1 calc R . . C32 C 0.6088(5) -0.8671(6) 0.5229(5) 0.0352(18) Uani 1 1 d . . . H32A H 0.6550 -0.8851 0.5653 0.042 Uiso 1 1 calc R . . N4 N 0.4713(4) -0.8175(6) 0.4887(4) 0.0399(16) Uani 1 1 d . . . C40 C 0.5292(7) -0.4655(11) 0.6958(7) 0.095(4) Uani 0.70 1 d PD A 1 H40A H 0.5525 -0.3976 0.6762 0.114 Uiso 0.70 1 calc PR A 1 H40B H 0.5656 -0.4899 0.7491 0.114 Uiso 0.70 1 calc PR A 1 Cl1 Cl 0.43772(18) -0.4294(3) 0.71741(19) 0.0885(9) Uani 0.70 1 d PD A 1 Cl2 Cl 0.5256(2) -0.5703(5) 0.6209(3) 0.0819(13) Uani 0.70 1 d PD A 1 C40A C 0.5292(7) -0.4655(11) 0.6958(7) 0.095(4) Uani 0.30 1 d PD B 2 H40C H 0.5672 -0.4027 0.7113 0.114 Uiso 0.30 1 calc PR B 2 H40D H 0.5515 -0.5317 0.7298 0.114 Uiso 0.30 1 calc PR B 2 Cl1A Cl 0.43772(18) -0.4294(3) 0.71741(19) 0.0885(9) Uani 0.30 1 d PD B 2 Cl2A Cl 0.5166(10) -0.4948(14) 0.5925(8) 0.123(5) Uiso 0.30 1 d PD B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hg1 0.03614(19) 0.04118(19) 0.03023(17) -0.00207(13) 0.00970(13) -0.00580(15) Br1 0.0983(9) 0.0711(6) 0.0290(4) -0.0042(4) 0.0150(5) -0.0199(6) Br2 0.0637(6) 0.0426(5) 0.0414(5) 0.0014(4) 0.0053(4) 0.0066(4) N1 0.041(4) 0.043(4) 0.025(3) -0.002(3) 0.011(3) -0.005(3) C1 0.051(5) 0.029(4) 0.027(4) -0.001(3) 0.017(4) 0.004(4) C2 0.043(5) 0.041(4) 0.022(4) -0.001(3) 0.006(3) 0.000(4) C3 0.027(4) 0.040(4) 0.021(3) 0.000(3) 0.004(3) -0.004(3) C4 0.028(4) 0.037(4) 0.025(4) 0.004(3) 0.008(3) 0.003(3) C5 0.029(4) 0.042(5) 0.026(4) -0.004(3) 0.006(3) 0.003(4) C6 0.026(4) 0.039(4) 0.021(3) 0.005(3) 0.003(3) 0.000(3) O1 0.041(3) 0.039(3) 0.029(3) 0.001(2) 0.007(2) -0.007(3) N2 0.035(4) 0.030(3) 0.023(3) 0.000(2) 0.010(3) -0.009(3) C7 0.031(4) 0.039(4) 0.023(4) -0.004(3) 0.009(3) -0.005(3) C8 0.037(5) 0.036(4) 0.035(4) 0.003(3) 0.017(4) -0.009(4) C9 0.045(5) 0.030(4) 0.043(4) -0.002(4) 0.022(4) -0.003(4) C10 0.040(5) 0.040(5) 0.051(5) -0.014(4) 0.026(4) -0.014(4) C11 0.051(6) 0.050(5) 0.061(6) -0.021(5) 0.029(5) -0.018(5) C12 0.046(6) 0.078(8) 0.061(6) -0.040(6) 0.020(5) -0.023(5) C13 0.045(6) 0.095(9) 0.045(5) -0.032(6) 0.007(4) -0.020(6) C14 0.031(5) 0.067(6) 0.035(4) -0.009(4) 0.010(4) -0.007(4) C15 0.024(4) 0.051(5) 0.032(4) -0.013(4) 0.011(3) -0.013(4) C16 0.017(4) 0.041(4) 0.030(4) -0.005(3) 0.010(3) -0.009(3) C17 0.026(4) 0.042(4) 0.020(3) -0.006(3) 0.001(3) 0.002(3) C18 0.023(4) 0.067(6) 0.025(4) -0.012(4) 0.002(3) 0.002(4) C19 0.028(4) 0.070(6) 0.044(5) -0.012(4) 0.009(4) -0.004(4) C20 0.030(5) 0.102(8) 0.050(5) -0.017(5) 0.019(4) -0.012(5) C21 0.026(5) 0.098(8) 0.056(6) -0.022(6) 0.011(4) 0.006(5) C22 0.038(5) 0.088(7) 0.040(5) -0.020(5) 0.001(4) 0.021(5) C23 0.032(5) 0.055(5) 0.034(4) -0.010(4) 0.001(4) 0.013(4) C24 0.060(6) 0.050(5) 0.041(5) 0.001(4) 0.015(4) 0.017(5) C25 0.055(6) 0.043(5) 0.037(4) 0.005(4) 0.015(4) 0.013(4) C26 0.032(4) 0.042(4) 0.018(3) -0.002(3) 0.003(3) 0.006(4) N3 0.027(3) 0.034(3) 0.027(3) -0.005(3) 0.007(3) 0.001(3) C27 0.033(5) 0.031(4) 0.034(4) 0.005(3) 0.016(4) 0.003(3) O2 0.035(3) 0.057(3) 0.026(3) -0.006(2) 0.011(2) -0.001(3) C28 0.026(4) 0.038(4) 0.025(4) 0.007(3) 0.008(3) 0.003(3) C29 0.055(6) 0.106(8) 0.034(5) 0.016(5) 0.015(5) 0.023(6) C30 0.030(5) 0.132(9) 0.040(5) 0.012(5) 0.018(4) 0.025(6) C31 0.030(4) 0.042(4) 0.031(4) 0.000(3) 0.009(3) 0.006(4) C32 0.032(4) 0.040(4) 0.034(4) 0.003(3) 0.008(3) 0.002(4) N4 0.030(4) 0.061(4) 0.032(3) 0.012(3) 0.015(3) 0.014(3) C40 0.074(9) 0.112(10) 0.095(9) -0.021(8) 0.009(7) 0.009(8) Cl1 0.072(2) 0.116(3) 0.0774(18) -0.0277(17) 0.0159(16) -0.0144(18) Cl2 0.053(2) 0.113(4) 0.083(3) -0.042(3) 0.022(2) -0.013(2) C40A 0.074(9) 0.112(10) 0.095(9) -0.021(8) 0.009(7) 0.009(8) Cl1A 0.072(2) 0.116(3) 0.0774(18) -0.0277(17) 0.0159(16) -0.0144(18) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Hg1 N4 98.1(2) . 2_645 ? N1 Hg1 Br1 106.54(14) . . ? N4 Hg1 Br1 110.43(15) 2_645 . ? N1 Hg1 Br2 93.60(15) . . ? N4 Hg1 Br2 94.33(16) 2_645 . ? Br1 Hg1 Br2 144.88(4) . . ? C5 N1 C1 117.4(6) . . ? C5 N1 Hg1 122.0(5) . . ? C1 N1 Hg1 120.0(5) . . ? N1 C1 C2 122.4(7) . . ? C1 C2 C3 120.5(6) . . ? C4 C3 C2 117.3(7) . . ? C4 C3 C6 120.3(6) . . ? C2 C3 C6 122.4(6) . . ? C5 C4 C3 119.3(7) . . ? N1 C5 C4 123.1(7) . . ? O1 C6 N2 123.6(7) . . ? O1 C6 C3 121.9(6) . . ? N2 C6 C3 114.5(6) . . ? C6 N2 C7 127.1(6) . . ? C16 C7 C8 122.5(7) . . ? C16 C7 N2 117.4(6) . . ? C8 C7 N2 120.1(6) . . ? C9 C8 C7 119.5(7) . . ? C8 C9 C10 121.5(7) . . ? C9 C10 C11 122.7(8) . . ? C9 C10 C15 119.2(7) . . ? C11 C10 C15 118.1(8) . . ? C12 C11 C10 121.5(9) . . ? C11 C12 C13 120.6(9) . . ? C14 C13 C12 121.7(9) . . ? C13 C14 C15 119.6(9) . . ? C14 C15 C16 122.6(8) . . ? C14 C15 C10 118.6(7) . . ? C16 C15 C10 118.8(7) . . ? C7 C16 C15 118.5(7) . . ? C7 C16 C17 118.7(6) . . ? C15 C16 C17 122.8(6) . . ? C26 C17 C18 119.1(7) . . ? C26 C17 C16 121.9(6) . . ? C18 C17 C16 118.9(6) . . ? C19 C18 C23 119.6(7) . . ? C19 C18 C17 121.9(8) . . ? C23 C18 C17 118.5(7) . . ? C20 C19 C18 119.7(9) . . ? C19 C20 C21 121.1(9) . . ? C22 C21 C20 120.8(8) . . ? C21 C22 C23 120.5(9) . . ? C24 C23 C18 120.0(7) . . ? C24 C23 C22 121.8(8) . . ? C18 C23 C22 118.2(8) . . ? C25 C24 C23 120.6(8) . . ? C24 C25 C26 120.1(8) . . ? C17 C26 C25 121.7(7) . . ? C17 C26 N3 120.3(6) . . ? C25 C26 N3 117.9(7) . . ? C27 N3 C26 119.6(6) . . ? O2 C27 N3 123.5(6) . . ? O2 C27 C28 118.6(7) . . ? N3 C27 C28 117.9(6) . . ? C32 C28 C29 117.6(7) . . ? C32 C28 C27 125.0(7) . . ? C29 C28 C27 117.3(6) . . ? C30 C29 C28 119.2(8) . . ? N4 C30 C29 123.4(8) . . ? N4 C31 C32 123.2(7) . . ? C28 C32 C31 119.5(7) . . ? C30 N4 C31 117.0(6) . . ? C30 N4 Hg1 117.9(5) . 2_655 ? C31 N4 Hg1 124.8(5) . 2_655 ? Cl2 C40 Cl1 115.5(7) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg1 N1 2.400(6) . ? Hg1 N4 2.416(6) 2_645 ? Hg1 Br1 2.4564(10) . ? Hg1 Br2 2.4995(11) . ? N1 C5 1.341(9) . ? N1 C1 1.356(9) . ? C1 C2 1.362(10) . ? C2 C3 1.391(10) . ? C3 C4 1.389(9) . ? C3 C6 1.498(10) . ? C4 C5 1.383(10) . ? C6 O1 1.232(8) . ? C6 N2 1.325(8) . ? N2 C7 1.430(9) . ? C7 C16 1.381(10) . ? C7 C8 1.412(10) . ? C8 C9 1.363(10) . ? C9 C10 1.400(11) . ? C10 C11 1.410(11) . ? C10 C15 1.452(12) . ? C11 C12 1.341(13) . ? C12 C13 1.381(14) . ? C13 C14 1.377(12) . ? C14 C15 1.403(11) . ? C15 C16 1.430(10) . ? C16 C17 1.490(11) . ? C17 C26 1.371(10) . ? C17 C18 1.441(10) . ? C18 C19 1.415(11) . ? C18 C23 1.421(12) . ? C19 C20 1.363(11) . ? C20 C21 1.404(15) . ? C21 C22 1.348(13) . ? C22 C23 1.434(11) . ? C23 C24 1.412(12) . ? C24 C25 1.357(11) . ? C25 C26 1.414(11) . ? C26 N3 1.440(9) . ? N3 C27 1.338(9) . ? C27 O2 1.234(8) . ? C27 C28 1.516(9) . ? C28 C32 1.367(9) . ? C28 C29 1.379(11) . ? C29 C30 1.377(11) . ? C30 N4 1.325(10) . ? C31 N4 1.327(9) . ? C31 C32 1.381(10) . ? N4 Hg1 2.416(6) 2_655 ? C40 Cl2 1.737(10) . ? C40 Cl1 1.747(9) . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2B O2 0.88 1.99 2.822(7) 157.6 . N3 H3A O1 0.88 1.96 2.834(7) 170.3 4_546
1100728.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $ #$Revision: 176435 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100728.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100728 loop_ _publ_author_name 'Tara J. Burchell' 'Richard J. Puddephatt' _publ_section_title ; Self-Assembly of Chiral Coordination Polymers and Macrocycles: A Metal Template Effect on the Polymer-Macrocycle Equilibrium ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3718 _journal_page_last 3730 _journal_paper_doi 10.1021/ic050097w _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C34.25 H27 Cl4.5 Hg I2 N4 O2' _chemical_formula_weight 1140.51 _chemical_name_systematic ; ? ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 96.91(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 20.856(4) _cell_length_b 15.847(3) _cell_length_c 23.865(5) _cell_measurement_temperature 150(2) _cell_measurement_theta_max 25 _cell_measurement_theta_min 2.55 _cell_volume 7830(3) _computing_cell_refinement 'Nonius DENZO' _computing_data_collection 'Nonius COLLECT' _computing_data_reduction 'Nonius DENZO' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'phi\omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.057 _diffrn_reflns_av_sigmaI/netI 0.0719 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 32703 _diffrn_reflns_theta_full 25.02 _diffrn_reflns_theta_max 25.02 _diffrn_reflns_theta_min 2.57 _exptl_absorpt_coefficient_mu 5.851 _exptl_absorpt_correction_T_max 0.6680 _exptl_absorpt_correction_T_min 0.4067 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.935 _exptl_crystal_density_method 'not measured' _exptl_crystal_description rod _exptl_crystal_F_000 4312 _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _refine_diff_density_max 3.039 _refine_diff_density_min -2.320 _refine_diff_density_rms 0.166 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.975 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 430 _refine_ls_number_reflns 6894 _refine_ls_number_restraints 22 _refine_ls_restrained_S_all 0.975 _refine_ls_R_factor_all 0.1469 _refine_ls_R_factor_gt 0.0740 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1030P)^2^+150.7700P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1917 _refine_ls_wR_factor_ref 0.2271 _reflns_number_gt 3577 _reflns_number_total 6894 _reflns_threshold_expression I>2sigma(I) _cod_data_source_file ic050097wsi20050217_082525_05.cif _cod_data_source_block 3c _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_formula_sum 'C34.25 H27 Cl4.50 Hg I2 N4 O2' _cod_database_code 1100728 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hg1 Hg 0.52001(3) 1.21116(5) -0.48837(2) 0.0828(3) Uani 1 1 d . . . I1 I 0.50941(6) 1.37636(8) -0.47671(5) 0.0896(4) Uani 1 1 d . . . I2 I 0.59041(7) 1.07246(12) -0.49635(5) 0.1268(7) Uani 1 1 d . . . N1 N 0.4585(6) 1.1705(8) -0.4105(5) 0.069(3) Uani 1 1 d . . . C1 C 0.4808(8) 1.1152(11) -0.3723(7) 0.085(5) Uani 1 1 d . . . H1A H 0.5191 1.0851 -0.3776 0.102 Uiso 1 1 calc R . . C2 C 0.4520(8) 1.0989(10) -0.3258(6) 0.075(4) Uani 1 1 d . . . H2A H 0.4703 1.0585 -0.2991 0.090 Uiso 1 1 calc R . . C3 C 0.3958(6) 1.1408(9) -0.3166(6) 0.058(3) Uani 1 1 d . . . C4 C 0.3732(8) 1.1972(11) -0.3551(7) 0.081(5) Uani 1 1 d . . . H4A H 0.3348 1.2277 -0.3510 0.097 Uiso 1 1 calc R . . C5 C 0.4057(8) 1.2111(10) -0.4012(6) 0.078(5) Uani 1 1 d . . . H5A H 0.3891 1.2525 -0.4279 0.093 Uiso 1 1 calc R . . C6 C 0.3643(6) 1.1185(10) -0.2641(6) 0.061(4) Uani 1 1 d . . . O1 O 0.3851(5) 1.0600(6) -0.2334(4) 0.067(3) Uani 1 1 d . . . N2 N 0.3154(5) 1.1682(8) -0.2531(5) 0.063(3) Uani 1 1 d . . . H2B H 0.2993 1.2058 -0.2781 0.076 Uiso 1 1 calc R . . C7 C 0.2890(7) 1.1596(10) -0.1997(7) 0.069(4) Uani 1 1 d . . . C8 C 0.3203(9) 1.2075(10) -0.1520(8) 0.079(5) Uani 1 1 d . . . H8A H 0.3562 1.2427 -0.1565 0.095 Uiso 1 1 calc R . . C9 C 0.2979(11) 1.2016(12) -0.1013(8) 0.101(6) Uani 1 1 d . . . H9A H 0.3181 1.2332 -0.0703 0.121 Uiso 1 1 calc R . . C10 C 0.2458(9) 1.1499(13) -0.0941(6) 0.095(6) Uani 1 1 d D . . C11 C 0.2239(9) 1.1418(13) -0.0406(8) 0.127(8) Uani 1 1 d D . . H11A H 0.2453 1.1720 -0.0094 0.152 Uiso 1 1 calc R . . C12 C 0.1720(9) 1.0907(15) -0.0329(10) 0.158(12) Uani 1 1 d D . . H12A H 0.1580 1.0857 0.0033 0.190 Uiso 1 1 calc R . . C13 C 0.1404(9) 1.0466(18) -0.0786(8) 0.163(13) Uani 1 1 d D . . H13A H 0.1050 1.0111 -0.0732 0.196 Uiso 1 1 calc R . . C14 C 0.1602(7) 1.0539(15) -0.1323(8) 0.123(8) Uani 1 1 d D . . H14A H 0.1374 1.0253 -0.1636 0.148 Uiso 1 1 calc R . . C15 C 0.2142(7) 1.1042(11) -0.1397(7) 0.089(5) Uani 1 1 d D . . C16 C 0.2381(7) 1.1109(11) -0.1942(7) 0.077(5) Uani 1 1 d . . . C17 C 0.2048(7) 1.0591(12) -0.2437(7) 0.075(4) Uani 1 1 d . . . C18 C 0.1489(8) 1.0925(13) -0.2779(8) 0.089(5) Uani 1 1 d . . . C19 C 0.1228(7) 1.1718(14) -0.2660(7) 0.089(5) Uani 1 1 d . . . H19A H 0.1440 1.2067 -0.2371 0.107 Uiso 1 1 calc R . . C20 C 0.0646(10) 1.1986(17) -0.2976(10) 0.117(8) Uani 1 1 d . . . H20A H 0.0454 1.2508 -0.2893 0.141 Uiso 1 1 calc R . . C21 C 0.0358(10) 1.148(2) -0.3409(11) 0.120(9) Uani 1 1 d . . . H21A H -0.0027 1.1667 -0.3626 0.144 Uiso 1 1 calc R . . C22 C 0.0612(10) 1.0729(18) -0.3529(10) 0.123(8) Uani 1 1 d . . . H22A H 0.0396 1.0407 -0.3831 0.148 Uiso 1 1 calc R . . C23 C 0.1191(9) 1.0387(15) -0.3226(8) 0.096(6) Uani 1 1 d . . . C24 C 0.1452(9) 0.9581(13) -0.3323(8) 0.095(6) Uani 1 1 d . . . H24A H 0.1257 0.9239 -0.3623 0.114 Uiso 1 1 calc R . . C25 C 0.1978(9) 0.9300(12) -0.2988(8) 0.094(6) Uani 1 1 d . . . H25A H 0.2153 0.8760 -0.3054 0.113 Uiso 1 1 calc R . . C26 C 0.2268(8) 0.9804(12) -0.2539(7) 0.076(4) Uani 1 1 d . . . N3 N 0.2797(6) 0.9442(8) -0.2173(5) 0.072(3) Uani 1 1 d . . . H3A H 0.3163 0.9724 -0.2129 0.087 Uiso 1 1 calc R . . C27 C 0.2776(7) 0.8720(10) -0.1898(6) 0.060(4) Uani 1 1 d . . . O2 O 0.2318(5) 0.8225(7) -0.1988(4) 0.072(3) Uani 1 1 d . . . C28 C 0.3340(6) 0.8555(9) -0.1462(5) 0.058(4) Uani 1 1 d . . . C29 C 0.3848(9) 0.9063(11) -0.1347(7) 0.098(6) Uani 1 1 d . . . H29A H 0.3874 0.9576 -0.1548 0.117 Uiso 1 1 calc R . . C30 C 0.4342(11) 0.8829(13) -0.0924(8) 0.119(8) Uani 1 1 d . . . H30A H 0.4709 0.9186 -0.0859 0.143 Uiso 1 1 calc R . . C31 C 0.3837(7) 0.7642(10) -0.0750(6) 0.068(4) Uani 1 1 d . . . H31A H 0.3829 0.7127 -0.0548 0.082 Uiso 1 1 calc R . . C32 C 0.3325(7) 0.7807(10) -0.1171(6) 0.069(4) Uani 1 1 d . . . H32A H 0.2980 0.7418 -0.1252 0.083 Uiso 1 1 calc R . . N4 N 0.4331(6) 0.8155(9) -0.0616(5) 0.079(4) Uani 1 1 d . . . C50 C 0.2257(11) 1.4153(15) -0.5137(8) 0.169(12) Uani 1 1 d D A 1 H50C H 0.2212 1.4674 -0.4916 0.203 Uiso 1 1 calc R A 1 H50D H 0.1826 1.3885 -0.5210 0.203 Uiso 1 1 calc R A 1 Cl2 Cl 0.2537(5) 1.4407(5) -0.5776(3) 0.178(3) Uani 1 1 d D A 1 Cl1 Cl 0.2780(6) 1.3484(7) -0.4762(6) 0.283(7) Uani 1 1 d D A 1 C60 C 0.6290(9) 0.9005(13) -0.1721(12) 0.163(11) Uani 1 1 d D . . H60A H 0.6514 0.9050 -0.2062 0.196 Uiso 1 1 calc R . . H60B H 0.6336 0.9547 -0.1514 0.196 Uiso 1 1 calc R . . Cl3 Cl 0.5487(5) 0.8762(6) -0.1901(7) 0.282(7) Uani 1 1 d D . . Cl4 Cl 0.6606(6) 0.8195(8) -0.1300(5) 0.261(6) Uani 1 1 d D . . C70 C 0.0000 0.903(4) -0.2500 0.18(3) Uiso 0.50 2 d SPD . . H70A H -0.0364 0.9411 -0.2449 0.215 Uiso 0.50 1 calc PR . . H70B H 0.0364 0.9411 -0.2551 0.215 Uiso 0.50 1 calc PR . . Cl5 Cl -0.0210(7) 0.8696(9) -0.3162(6) 0.146(4) Uiso 0.50 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hg1 0.0747(5) 0.1209(7) 0.0530(4) -0.0056(4) 0.0087(3) 0.0189(4) I1 0.0893(8) 0.1090(10) 0.0739(7) 0.0067(6) 0.0234(6) -0.0130(7) I2 0.1015(9) 0.1954(17) 0.0805(8) -0.0283(9) -0.0015(7) 0.0744(10) N1 0.078(8) 0.074(9) 0.058(7) -0.002(7) 0.017(6) 0.019(7) C1 0.103(13) 0.081(12) 0.078(11) 0.011(10) 0.034(9) 0.044(10) C2 0.085(11) 0.070(11) 0.071(10) 0.021(8) 0.012(8) 0.033(9) C3 0.052(8) 0.057(10) 0.064(8) -0.003(7) 0.007(6) -0.002(7) C4 0.063(9) 0.105(14) 0.078(11) 0.034(10) 0.022(8) 0.032(9) C5 0.074(10) 0.093(13) 0.065(9) 0.020(9) 0.002(8) 0.041(9) C6 0.044(8) 0.068(11) 0.071(9) 0.001(8) 0.005(7) -0.008(8) O1 0.069(6) 0.058(7) 0.077(6) 0.008(6) 0.023(5) 0.009(5) N2 0.058(7) 0.056(8) 0.077(8) 0.009(6) 0.016(6) 0.010(6) C7 0.061(9) 0.069(11) 0.083(11) 0.004(9) 0.024(8) 0.005(8) C8 0.083(11) 0.065(11) 0.089(12) -0.001(9) 0.012(9) -0.005(9) C9 0.116(16) 0.103(16) 0.089(13) -0.018(11) 0.028(12) 0.011(12) C10 0.082(12) 0.131(18) 0.078(12) -0.013(12) 0.031(10) 0.020(12) C11 0.091(14) 0.19(2) 0.109(15) -0.030(15) 0.044(12) 0.009(15) C12 0.078(15) 0.30(4) 0.098(16) 0.04(2) 0.033(13) 0.016(19) C13 0.056(12) 0.32(4) 0.118(17) 0.07(2) 0.039(12) 0.016(17) C14 0.052(10) 0.21(3) 0.110(15) 0.024(16) 0.016(10) -0.014(13) C15 0.054(9) 0.129(16) 0.087(12) 0.021(11) 0.027(9) 0.022(10) C16 0.049(9) 0.093(13) 0.090(11) 0.009(10) 0.011(8) 0.005(9) C17 0.050(9) 0.092(14) 0.082(11) 0.016(10) 0.008(8) -0.010(9) C18 0.056(10) 0.102(15) 0.112(14) 0.039(12) 0.024(10) 0.002(10) C19 0.056(10) 0.123(16) 0.093(12) 0.027(11) 0.022(9) 0.022(10) C20 0.077(14) 0.17(2) 0.109(16) 0.046(16) 0.040(12) 0.032(14) C21 0.065(13) 0.19(3) 0.113(18) 0.064(19) 0.022(12) 0.014(16) C22 0.073(14) 0.16(2) 0.131(18) 0.047(18) -0.003(13) -0.012(15) C23 0.073(12) 0.122(18) 0.088(12) 0.047(12) -0.015(10) -0.023(12) C24 0.095(14) 0.080(14) 0.108(14) 0.021(11) -0.002(11) -0.017(11) C25 0.101(13) 0.077(13) 0.098(13) 0.029(11) -0.012(11) 0.012(11) C26 0.068(10) 0.079(13) 0.078(11) 0.010(10) -0.005(8) -0.011(10) N3 0.054(7) 0.068(9) 0.092(9) 0.010(8) -0.001(6) -0.006(6) C27 0.064(9) 0.066(11) 0.054(8) 0.010(8) 0.020(7) 0.001(8) O2 0.063(6) 0.074(7) 0.078(7) 0.002(6) 0.002(5) -0.027(6) C28 0.064(9) 0.061(10) 0.051(8) -0.003(7) 0.013(7) -0.018(7) C29 0.123(15) 0.073(12) 0.084(11) 0.020(9) -0.042(11) -0.048(11) C30 0.151(19) 0.098(16) 0.094(13) 0.019(12) -0.042(13) -0.065(14) C31 0.070(10) 0.067(11) 0.072(10) 0.025(8) 0.022(8) -0.001(8) C32 0.050(8) 0.087(13) 0.069(9) -0.003(9) 0.004(7) -0.016(8) N4 0.076(9) 0.091(11) 0.069(8) 0.010(8) 0.008(6) -0.036(8) C50 0.075(13) 0.17(2) 0.27(4) -0.07(2) 0.030(17) 0.040(15) Cl2 0.199(8) 0.181(7) 0.148(6) -0.007(5) -0.002(5) -0.023(6) Cl1 0.325(13) 0.216(10) 0.357(15) 0.112(10) 0.234(12) 0.124(10) C60 0.18(3) 0.070(15) 0.24(3) 0.071(18) 0.03(2) -0.020(16) Cl3 0.202(10) 0.151(8) 0.48(2) -0.088(10) -0.022(11) -0.036(7) Cl4 0.278(13) 0.234(11) 0.270(13) -0.051(10) 0.029(10) 0.104(10) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Hg1 N1 95.0(4) 6_575 . ? N4 Hg1 I1 100.7(3) 6_575 . ? N1 Hg1 I1 97.0(3) . . ? N4 Hg1 I2 100.2(3) 6_575 . ? N1 Hg1 I2 100.3(3) . . ? I1 Hg1 I2 151.45(5) . . ? C1 N1 C5 116.4(13) . . ? C1 N1 Hg1 121.7(10) . . ? C5 N1 Hg1 121.4(10) . . ? N1 C1 C2 123.0(14) . . ? C1 C2 C3 120.5(14) . . ? C4 C3 C2 116.8(13) . . ? C4 C3 C6 124.9(13) . . ? C2 C3 C6 118.3(13) . . ? C3 C4 C5 119.4(14) . . ? N1 C5 C4 124.0(13) . . ? O1 C6 N2 123.4(13) . . ? O1 C6 C3 120.6(13) . . ? N2 C6 C3 116.0(13) . . ? C6 N2 C7 119.6(12) . . ? C16 C7 N2 122.1(15) . . ? C16 C7 C8 120.8(15) . . ? N2 C7 C8 117.1(13) . . ? C9 C8 C7 119.6(17) . . ? C8 C9 C10 120.9(18) . . ? C9 C10 C15 120.6(14) . . ? C9 C10 C11 120.6(17) . . ? C15 C10 C11 118.8(18) . . ? C12 C11 C10 121.1(19) . . ? C11 C12 C13 120(2) . . ? C12 C13 C14 121(2) . . ? C13 C14 C15 119.3(18) . . ? C10 C15 C14 120.2(16) . . ? C10 C15 C16 118.5(13) . . ? C14 C15 C16 121.3(15) . . ? C7 C16 C15 119.7(15) . . ? C7 C16 C17 121.6(14) . . ? C15 C16 C17 118.6(14) . . ? C26 C17 C18 120.1(17) . . ? C26 C17 C16 119.8(14) . . ? C18 C17 C16 120.0(17) . . ? C19 C18 C17 121.2(19) . . ? C19 C18 C23 122.1(17) . . ? C17 C18 C23 116.6(18) . . ? C18 C19 C20 119(2) . . ? C21 C20 C19 119(2) . . ? C22 C21 C20 122(2) . . ? C21 C22 C23 124(3) . . ? C24 C23 C22 125(2) . . ? C24 C23 C18 120.8(16) . . ? C22 C23 C18 114(2) . . ? C25 C24 C23 120.0(19) . . ? C24 C25 C26 120.3(19) . . ? C17 C26 C25 122.1(16) . . ? C17 C26 N3 120.4(15) . . ? C25 C26 N3 117.5(16) . . ? C27 N3 C26 125.2(13) . . ? O2 C27 N3 122.4(13) . . ? O2 C27 C28 122.4(13) . . ? N3 C27 C28 115.2(13) . . ? C29 C28 C32 118.8(14) . . ? C29 C28 C27 125.2(14) . . ? C32 C28 C27 116.0(12) . . ? C28 C29 C30 119.1(16) . . ? N4 C30 C29 124.2(17) . . ? N4 C31 C32 124.4(14) . . ? C28 C32 C31 117.5(13) . . ? C30 N4 C31 115.8(14) . . ? C30 N4 Hg1 119.5(11) . 6_576 ? C31 N4 Hg1 124.6(11) . 6_576 ? Cl1 C50 Cl2 110.1(12) . . ? Cl4 C60 Cl3 105.8(11) . . ? Cl5 C70 Cl5 143(4) . 2_554 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg1 N4 2.400(13) 6_575 ? Hg1 N1 2.467(12) . ? Hg1 I1 2.6447(17) . ? Hg1 I2 2.6628(16) . ? N1 C1 1.309(18) . ? N1 C5 1.317(18) . ? C1 C2 1.35(2) . ? C2 C3 1.386(19) . ? C3 C4 1.328(19) . ? C3 C6 1.526(19) . ? C4 C5 1.38(2) . ? C6 O1 1.227(16) . ? C6 N2 1.339(17) . ? N2 C7 1.454(18) . ? C7 C16 1.33(2) . ? C7 C8 1.46(2) . ? C8 C9 1.35(2) . ? C9 C10 1.39(3) . ? C10 C15 1.404(14) . ? C10 C11 1.411(14) . ? C11 C12 1.382(15) . ? C12 C13 1.392(15) . ? C13 C14 1.399(14) . ? C14 C15 1.407(14) . ? C15 C16 1.45(2) . ? C16 C17 1.53(2) . ? C17 C26 1.36(2) . ? C17 C18 1.44(2) . ? C18 C19 1.41(3) . ? C18 C23 1.45(3) . ? C19 C20 1.42(3) . ? C20 C21 1.39(3) . ? C21 C22 1.35(3) . ? C22 C23 1.44(3) . ? C23 C24 1.42(3) . ? C24 C25 1.35(2) . ? C25 C26 1.41(2) . ? C26 N3 1.441(19) . ? N3 C27 1.322(17) . ? C27 O2 1.234(16) . ? C27 C28 1.496(19) . ? C28 C29 1.332(19) . ? C28 C32 1.38(2) . ? C29 C30 1.40(2) . ? C30 N4 1.30(2) . ? C31 N4 1.320(19) . ? C31 C32 1.40(2) . ? N4 Hg1 2.400(13) 6_576 ? C50 Cl1 1.697(16) . ? C50 Cl2 1.744(17) . ? C60 Cl4 1.711(15) . ? C60 Cl3 1.722(16) . ? C70 Cl5 1.674(16) . ? C70 Cl5 1.674(16) 2_554 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2B O2 0.88 2.02 2.828(16) 153.0 4_554 N3 H3A O1 0.88 2.10 2.925(16) 156.5 .
1100729.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100729.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100729 loop_ _publ_author_name 'Tara J. Burchell' 'Richard J. Puddephatt' _publ_section_title ; Self-Assembly of Chiral Coordination Polymers and Macrocycles: A Metal Template Effect on the Polymer-Macrocycle Equilibrium ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3718 _journal_page_last 3730 _journal_paper_doi 10.1021/ic050097w _journal_volume 44 _journal_year 2005 _chemical_absolute_configuration rm _chemical_formula_sum 'C37 H34 Cl2 Hg I2 N4 O3' _chemical_formula_weight 1107.97 _chemical_name_systematic ? _space_group_IT_number 19 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P 21 21 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 15.023(3) _cell_length_b 15.582(3) _cell_length_c 16.554(3) _cell_measurement_reflns_used 4942 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 27.48 _cell_measurement_theta_min 1.70 _cell_volume 3875.1(13) _computing_cell_refinement 'Nonius DENZO' _computing_data_collection 'Nonius COLLECT' _computing_data_reduction 'Nonius DENZO' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'nonius Kappa CCD' _diffrn_measurement_method 'phi\omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.102 _diffrn_reflns_av_sigmaI/netI 0.0627 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 38716 _diffrn_reflns_theta_full 27.53 _diffrn_reflns_theta_max 27.53 _diffrn_reflns_theta_min 1.79 _exptl_absorpt_coefficient_mu 5.744 _exptl_absorpt_correction_T_max 0.6726 _exptl_absorpt_correction_T_min 0.4795 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.899 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 2112 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _refine_diff_density_max 1.535 _refine_diff_density_min -2.429 _refine_diff_density_rms 0.192 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.035(6) _refine_ls_extinction_coef 0.00287(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 443 _refine_ls_number_reflns 8892 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.045 _refine_ls_R_factor_all 0.0689 _refine_ls_R_factor_gt 0.0465 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0650P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1014 _refine_ls_wR_factor_ref 0.1096 _reflns_number_gt 7109 _reflns_number_total 8892 _reflns_threshold_expression I>2sigma(I) _cod_data_source_file ic050097wsi20050217_082525_06.cif _cod_data_source_block 4c _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_cell_volume 3874.8(13) _cod_database_code 1100729 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hg1 Hg 1.27857(2) 0.03911(2) 0.468830(18) 0.02735(10) Uani 1 1 d . . . I2 I 1.30880(4) 0.00387(4) 0.62186(3) 0.03696(16) Uani 1 1 d . . . I3 I 1.30948(5) 0.13248(4) 0.34053(4) 0.04108(17) Uani 1 1 d . . . N1 N 1.1165(5) 0.0266(4) 0.4640(4) 0.0264(15) Uani 1 1 d . . . C1 C 1.0713(5) -0.0284(5) 0.5089(5) 0.0251(18) Uani 1 1 d . . . H1A H 1.1029 -0.0590 0.5494 0.030 Uiso 1 1 calc R . . C2 C 0.9811(6) -0.0442(6) 0.5008(5) 0.0289(19) Uani 1 1 d . . . H2A H 0.9522 -0.0855 0.5339 0.035 Uiso 1 1 calc R . . C3 C 0.9338(6) 0.0014(5) 0.4434(4) 0.0241(17) Uani 1 1 d . . . C4 C 0.9798(6) 0.0592(5) 0.3967(5) 0.035(2) Uani 1 1 d . . . H4A H 0.9498 0.0919 0.3566 0.042 Uiso 1 1 calc R . . C5 C 1.0711(7) 0.0694(5) 0.4089(5) 0.035(2) Uani 1 1 d . . . H5A H 1.1022 0.1091 0.3758 0.042 Uiso 1 1 calc R . . C6 C 0.8368(6) -0.0143(4) 0.4344(4) 0.0249(19) Uani 1 1 d . . . O1 O 0.7943(4) -0.0571(3) 0.4839(3) 0.0299(14) Uani 1 1 d . . . N2 N 0.7977(5) 0.0168(4) 0.3672(4) 0.0266(16) Uani 1 1 d . . . H2B H 0.8284 0.0540 0.3383 0.032 Uiso 1 1 calc R . . C7 C 0.7126(5) -0.0048(5) 0.3392(4) 0.0226(16) Uani 1 1 d . . . C8 C 0.6366(5) 0.0121(5) 0.3870(5) 0.0251(18) Uani 1 1 d . . . H8A H 0.6427 0.0368 0.4392 0.030 Uiso 1 1 calc R . . C9 C 0.5543(6) -0.0076(5) 0.3572(5) 0.031(2) Uani 1 1 d . . . H9A H 0.5031 0.0045 0.3888 0.037 Uiso 1 1 calc R . . C10 C 0.5436(5) -0.0456(5) 0.2803(5) 0.0262(17) Uani 1 1 d . . . C11 C 0.4591(7) -0.0652(6) 0.2484(6) 0.039(2) Uani 1 1 d . . . H11A H 0.4075 -0.0503 0.2785 0.046 Uiso 1 1 calc R . . C12 C 0.4493(7) -0.1043(6) 0.1772(6) 0.044(3) Uani 1 1 d . . . H12A H 0.3914 -0.1182 0.1582 0.052 Uiso 1 1 calc R . . C13 C 0.5249(6) -0.1251(6) 0.1298(6) 0.037(2) Uani 1 1 d . . . H13A H 0.5174 -0.1535 0.0795 0.045 Uiso 1 1 calc R . . C14 C 0.6088(6) -0.1048(5) 0.1561(5) 0.0259(18) Uani 1 1 d . . . H14A H 0.6593 -0.1183 0.1240 0.031 Uiso 1 1 calc R . . C15 C 0.6195(6) -0.0626(5) 0.2330(5) 0.0225(18) Uani 1 1 d . . . C16 C 0.7057(5) -0.0409(5) 0.2636(4) 0.0227(17) Uani 1 1 d . . . C17 C 0.7895(5) -0.0614(4) 0.2187(4) 0.0199(16) Uani 1 1 d . . . C18 C 0.8354(6) -0.1382(5) 0.2371(5) 0.0222(17) Uani 1 1 d . . . C19 C 0.8066(7) -0.1958(5) 0.2964(5) 0.030(2) Uani 1 1 d . . . H19A H 0.7524 -0.1846 0.3240 0.036 Uiso 1 1 calc R . . C20 C 0.8532(7) -0.2667(5) 0.3157(6) 0.040(2) Uani 1 1 d . . . H20A H 0.8322 -0.3036 0.3572 0.048 Uiso 1 1 calc R . . C21 C 0.9315(7) -0.2864(6) 0.2757(6) 0.040(2) Uani 1 1 d . . . H21A H 0.9631 -0.3372 0.2893 0.048 Uiso 1 1 calc R . . C22 C 0.9638(7) -0.2332(5) 0.2165(5) 0.035(2) Uani 1 1 d . . . H22A H 1.0181 -0.2468 0.1899 0.042 Uiso 1 1 calc R . . C23 C 0.9170(6) -0.1587(5) 0.1953(5) 0.0283(19) Uani 1 1 d . . . C24 C 0.9462(6) -0.1018(6) 0.1334(6) 0.037(2) Uani 1 1 d . . . H24A H 0.9972 -0.1161 0.1023 0.045 Uiso 1 1 calc R . . C25 C 0.9028(6) -0.0279(5) 0.1183(5) 0.032(2) Uani 1 1 d . . . H25A H 0.9259 0.0110 0.0794 0.038 Uiso 1 1 calc R . . C26 C 0.8233(5) -0.0077(5) 0.1598(4) 0.0219(16) Uani 1 1 d . . . N3 N 0.7817(5) 0.0733(4) 0.1413(4) 0.0245(14) Uani 1 1 d . . . H3A H 0.7430 0.0766 0.1015 0.029 Uiso 1 1 calc R . . C27 C 0.8015(6) 0.1435(5) 0.1844(4) 0.0232(18) Uani 1 1 d . . . O2 O 0.8423(5) 0.1416(4) 0.2480(3) 0.0340(15) Uani 1 1 d . . . C28 C 0.7712(6) 0.2298(4) 0.1511(4) 0.0187(15) Uani 1 1 d . . . C29 C 0.7959(6) 0.3022(5) 0.1924(5) 0.031(2) Uani 1 1 d . . . H29A H 0.8278 0.2977 0.2418 0.037 Uiso 1 1 calc R . . C30 C 0.7743(7) 0.3808(5) 0.1619(5) 0.034(2) Uani 1 1 d . . . H30A H 0.7905 0.4302 0.1921 0.041 Uiso 1 1 calc R . . C31 C 0.7077(6) 0.3223(5) 0.0523(5) 0.030(2) Uani 1 1 d . . . H31A H 0.6762 0.3285 0.0029 0.036 Uiso 1 1 calc R . . C32 C 0.7266(6) 0.2392(5) 0.0797(4) 0.0274(18) Uani 1 1 d . . . H32A H 0.7088 0.1904 0.0492 0.033 Uiso 1 1 calc R . . N4 N 0.7313(5) 0.3921(4) 0.0914(4) 0.0263(15) Uani 1 1 d . . . C33 C 0.7575(9) -0.2386(8) -0.0868(7) 0.071(4) Uani 1 1 d . . . H33A H 0.7647 -0.1928 -0.1277 0.085 Uiso 1 1 calc R . . H33B H 0.7608 -0.2942 -0.1156 0.085 Uiso 1 1 calc R . . Cl1 Cl 0.8474(3) -0.2329(2) -0.0205(2) 0.0983(14) Uani 1 1 d . . . Cl2 Cl 0.6565(3) -0.2297(2) -0.04757(19) 0.0743(10) Uani 1 1 d . . . C34 C 0.9702(8) 0.2027(8) 0.0212(7) 0.066(4) Uani 1 1 d . . . H34A H 0.9220 0.1793 0.0544 0.098 Uiso 1 1 calc R . . H34B H 0.9971 0.2519 0.0489 0.098 Uiso 1 1 calc R . . H34C H 1.0156 0.1584 0.0125 0.098 Uiso 1 1 calc R . . C35 C 0.9324(7) 0.2322(6) -0.0616(6) 0.045(3) Uani 1 1 d . . . H35A H 0.9050 0.1831 -0.0903 0.054 Uiso 1 1 calc R . . H35B H 0.8865 0.2770 -0.0537 0.054 Uiso 1 1 calc R . . O3 O 1.0033(5) 0.2645(4) -0.1055(4) 0.0437(17) Uani 1 1 d . . . C36 C 0.9739(7) 0.2912(6) -0.1837(5) 0.041(2) Uani 1 1 d . . . H36A H 0.9316 0.3395 -0.1785 0.049 Uiso 1 1 calc R . . H36B H 0.9432 0.2432 -0.2113 0.049 Uiso 1 1 calc R . . C37 C 1.0527(8) 0.3182(6) -0.2311(6) 0.048(3) Uani 1 1 d . . . H37A H 1.0337 0.3362 -0.2852 0.072 Uiso 1 1 calc R . . H37B H 1.0943 0.2701 -0.2358 0.072 Uiso 1 1 calc R . . H37C H 1.0821 0.3663 -0.2039 0.072 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hg1 0.02981(18) 0.02412(15) 0.02812(15) 0.00114(13) -0.00158(14) -0.00126(15) I2 0.0483(4) 0.0322(3) 0.0303(3) 0.0013(2) -0.0090(3) 0.0002(3) I3 0.0479(4) 0.0365(3) 0.0389(3) 0.0082(3) 0.0095(3) -0.0005(3) N1 0.026(4) 0.023(4) 0.030(3) 0.009(3) -0.005(3) -0.002(3) C1 0.024(5) 0.021(4) 0.030(4) 0.000(3) -0.005(3) 0.004(3) C2 0.038(5) 0.025(4) 0.024(4) 0.008(4) 0.001(3) 0.005(4) C3 0.030(5) 0.020(4) 0.022(4) -0.004(3) 0.000(3) 0.003(4) C4 0.031(5) 0.034(5) 0.041(5) 0.014(4) -0.007(4) -0.013(4) C5 0.038(6) 0.028(4) 0.038(5) 0.009(4) 0.004(4) 0.000(4) C6 0.040(6) 0.011(3) 0.023(4) -0.001(3) -0.001(4) 0.001(3) O1 0.030(4) 0.033(3) 0.026(3) 0.009(2) 0.008(2) -0.007(3) N2 0.030(4) 0.027(4) 0.022(3) 0.005(3) -0.002(3) -0.009(3) C7 0.028(5) 0.016(3) 0.025(4) 0.003(3) 0.000(4) 0.003(4) C8 0.023(5) 0.019(4) 0.033(4) 0.005(3) 0.003(3) -0.004(3) C9 0.027(5) 0.031(4) 0.034(5) 0.005(4) 0.011(4) 0.006(4) C10 0.019(4) 0.019(4) 0.040(5) 0.009(4) -0.001(3) -0.004(4) C11 0.026(6) 0.035(5) 0.056(6) 0.012(5) 0.002(4) 0.005(4) C12 0.036(6) 0.030(5) 0.065(7) -0.003(5) -0.010(5) -0.009(4) C13 0.036(6) 0.033(5) 0.043(5) 0.000(4) 0.002(4) -0.007(4) C14 0.023(5) 0.017(4) 0.037(5) 0.007(3) -0.007(4) -0.006(3) C15 0.017(5) 0.020(4) 0.031(4) 0.006(3) -0.001(3) -0.005(3) C16 0.027(5) 0.017(3) 0.024(4) 0.002(3) 0.003(3) 0.001(4) C17 0.013(4) 0.022(4) 0.025(4) -0.006(3) -0.005(3) 0.000(3) C18 0.022(5) 0.016(4) 0.029(4) 0.004(3) -0.004(3) 0.003(3) C19 0.038(6) 0.026(4) 0.026(4) 0.008(3) 0.001(4) 0.001(4) C20 0.059(7) 0.025(4) 0.036(5) 0.001(4) -0.004(5) 0.004(5) C21 0.050(7) 0.030(5) 0.040(5) 0.000(4) -0.005(5) 0.013(5) C22 0.035(6) 0.029(4) 0.042(5) -0.003(4) -0.004(4) 0.007(4) C23 0.022(5) 0.027(4) 0.036(5) -0.009(4) 0.004(4) -0.001(4) C24 0.026(5) 0.032(5) 0.054(6) -0.012(4) 0.008(4) 0.000(4) C25 0.027(5) 0.025(5) 0.043(5) 0.007(4) 0.007(4) -0.003(4) C26 0.024(4) 0.021(4) 0.021(4) -0.003(3) -0.001(3) -0.002(3) N3 0.024(4) 0.022(3) 0.028(3) 0.005(3) 0.000(3) -0.003(3) C27 0.031(5) 0.020(4) 0.018(4) 0.006(3) 0.002(3) -0.002(4) O2 0.043(4) 0.031(3) 0.028(3) 0.005(3) -0.010(3) -0.005(3) C28 0.019(4) 0.016(3) 0.021(3) 0.004(3) -0.001(3) -0.001(3) C29 0.039(6) 0.026(4) 0.028(4) 0.001(3) -0.010(4) 0.002(4) C30 0.051(6) 0.025(4) 0.026(4) -0.007(3) -0.013(4) 0.007(4) C31 0.027(6) 0.037(5) 0.027(4) 0.007(3) -0.007(3) -0.005(4) C32 0.032(5) 0.024(4) 0.026(4) 0.000(3) -0.006(4) -0.005(4) N4 0.038(5) 0.014(3) 0.027(3) -0.001(2) 0.002(3) 0.004(3) C33 0.090(12) 0.044(6) 0.078(8) 0.007(6) -0.026(7) 0.009(7) Cl1 0.119(4) 0.078(2) 0.098(3) 0.026(2) -0.042(3) -0.014(2) Cl2 0.095(3) 0.0588(18) 0.069(2) 0.0152(15) 0.0045(18) 0.0211(18) C34 0.048(8) 0.073(8) 0.075(8) 0.031(7) 0.027(6) 0.013(6) C35 0.036(7) 0.040(5) 0.058(6) -0.007(5) 0.011(5) -0.004(5) O3 0.046(5) 0.043(4) 0.042(4) 0.007(3) -0.008(3) -0.011(3) C36 0.050(7) 0.033(5) 0.039(5) 0.003(4) -0.008(5) -0.008(5) C37 0.059(8) 0.036(5) 0.050(6) 0.010(5) -0.015(5) -0.003(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Hg1 N4 81.7(2) . 3_745 ? N1 Hg1 I3 101.21(14) . . ? N4 Hg1 I3 101.29(14) 3_745 . ? N1 Hg1 I2 100.78(15) . . ? N4 Hg1 I2 101.72(14) 3_745 . ? I3 Hg1 I2 150.11(3) . . ? C5 N1 C1 116.9(8) . . ? C5 N1 Hg1 119.8(6) . . ? C1 N1 Hg1 123.0(5) . . ? N1 C1 C2 124.3(7) . . ? C3 C2 C1 118.5(8) . . ? C4 C3 C2 117.8(8) . . ? C4 C3 C6 123.0(7) . . ? C2 C3 C6 119.2(7) . . ? C3 C4 C5 119.2(8) . . ? N1 C5 C4 123.4(8) . . ? O1 C6 N2 121.1(8) . . ? O1 C6 C3 122.0(7) . . ? N2 C6 C3 116.8(7) . . ? C6 N2 C7 125.7(7) . . ? C16 C7 N2 117.8(7) . . ? C16 C7 C8 121.6(8) . . ? N2 C7 C8 120.5(7) . . ? C9 C8 C7 119.1(8) . . ? C8 C9 C10 121.5(8) . . ? C11 C10 C15 118.7(8) . . ? C11 C10 C9 122.0(8) . . ? C15 C10 C9 119.2(7) . . ? C12 C11 C10 121.9(10) . . ? C11 C12 C13 120.3(9) . . ? C14 C13 C12 120.5(9) . . ? C13 C14 C15 119.2(8) . . ? C10 C15 C16 119.4(7) . . ? C10 C15 C14 119.1(8) . . ? C16 C15 C14 121.4(7) . . ? C7 C16 C15 119.1(7) . . ? C7 C16 C17 118.4(7) . . ? C15 C16 C17 122.4(6) . . ? C26 C17 C18 119.1(7) . . ? C26 C17 C16 122.1(7) . . ? C18 C17 C16 118.9(7) . . ? C19 C18 C17 123.0(8) . . ? C19 C18 C23 117.2(7) . . ? C17 C18 C23 119.8(7) . . ? C20 C19 C18 122.1(9) . . ? C19 C20 C21 120.7(9) . . ? C22 C21 C20 120.5(9) . . ? C21 C22 C23 120.1(9) . . ? C22 C23 C24 122.8(8) . . ? C22 C23 C18 119.3(8) . . ? C24 C23 C18 117.9(8) . . ? C25 C24 C23 121.2(9) . . ? C24 C25 C26 120.6(8) . . ? C17 C26 C25 121.2(7) . . ? C17 C26 N3 121.4(7) . . ? C25 C26 N3 117.3(7) . . ? C27 N3 C26 120.3(7) . . ? O2 C27 N3 123.5(7) . . ? O2 C27 C28 119.0(7) . . ? N3 C27 C28 117.5(6) . . ? C32 C28 C29 118.4(7) . . ? C32 C28 C27 123.6(7) . . ? C29 C28 C27 117.8(7) . . ? C30 C29 C28 119.4(7) . . ? N4 C30 C29 123.6(7) . . ? N4 C31 C32 123.4(7) . . ? C28 C32 C31 118.6(7) . . ? C31 N4 C30 116.6(6) . . ? C31 N4 Hg1 123.0(5) . 3_755 ? C30 N4 Hg1 119.6(5) . 3_755 ? Cl2 C33 Cl1 117.3(7) . . ? O3 C35 C34 106.8(9) . . ? C35 O3 C36 110.1(8) . . ? O3 C36 C37 108.5(8) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg1 N1 2.445(7) . ? Hg1 N4 2.502(6) 3_745 ? Hg1 I3 2.6160(7) . ? Hg1 I2 2.6316(8) . ? N1 C5 1.318(10) . ? N1 C1 1.322(10) . ? C1 C2 1.385(12) . ? C2 C3 1.383(11) . ? C3 C4 1.373(11) . ? C3 C6 1.486(12) . ? C4 C5 1.396(13) . ? C6 O1 1.234(9) . ? C6 N2 1.349(10) . ? N2 C7 1.401(10) . ? C7 C16 1.377(10) . ? C7 C8 1.413(11) . ? C8 C9 1.367(12) . ? C9 C10 1.413(12) . ? C10 C11 1.408(13) . ? C10 C15 1.408(12) . ? C11 C12 1.335(14) . ? C12 C13 1.418(14) . ? C13 C14 1.370(12) . ? C14 C15 1.441(11) . ? C15 C16 1.432(11) . ? C16 C17 1.497(11) . ? C17 C26 1.381(10) . ? C17 C18 1.414(10) . ? C18 C19 1.400(11) . ? C18 C23 1.444(12) . ? C19 C20 1.346(12) . ? C20 C21 1.384(14) . ? C21 C22 1.373(13) . ? C22 C23 1.402(12) . ? C23 C24 1.424(13) . ? C24 C25 1.346(12) . ? C25 C26 1.414(11) . ? C26 N3 1.441(10) . ? N3 C27 1.340(10) . ? C27 O2 1.218(9) . ? C27 C28 1.523(10) . ? C28 C32 1.368(10) . ? C28 C29 1.370(11) . ? C29 C30 1.363(11) . ? C30 N4 1.346(10) . ? C31 N4 1.315(10) . ? C31 C32 1.401(11) . ? N4 Hg1 2.502(6) 3_755 ? C33 Cl2 1.656(15) . ? C33 Cl1 1.743(13) . ? C34 C35 1.553(14) . ? C35 O3 1.385(12) . ? O3 C36 1.428(11) . ? C36 C37 1.481(15) . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2B O2 0.88 2.04 2.849(8) 153.3 . N3 H3A O1 0.88 2.05 2.856(8) 152.1 2_654
1100730.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $ #$Revision: 176435 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100730.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100730 loop_ _publ_author_name 'Tara J. Burchell' 'Richard J. Puddephatt' _publ_section_title ; Self-Assembly of Chiral Coordination Polymers and Macrocycles: A Metal Template Effect on the Polymer-Macrocycle Equilibrium ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3718 _journal_page_last 3730 _journal_paper_doi 10.1021/ic050097w _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C33 H25.2 Cl2.8 Hg0.95 N4 O2.6' _chemical_formula_weight 809.19 _chemical_name_systematic ; ? ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 91.91(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 18.204(4) _cell_length_b 10.865(2) _cell_length_c 16.030(3) _cell_measurement_reflns_used 7278 _cell_measurement_temperature 396(2) _cell_measurement_theta_max 27.48 _cell_measurement_theta_min 1.70 _cell_volume 3168.8(11) _computing_cell_refinement 'Nonius DENZO' _computing_data_collection 'Nonius COLLECT' _computing_data_reduction 'Nonius DENZO' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 396(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'phi\omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.052 _diffrn_reflns_av_sigmaI/netI 0.0447 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 32365 _diffrn_reflns_theta_full 26.37 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_min 2.74 _exptl_absorpt_coefficient_mu 4.891 _exptl_absorpt_correction_T_max 0.7920 _exptl_absorpt_correction_T_min 0.1158 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.696 _exptl_crystal_density_method 'not measured' _exptl_crystal_description rod _exptl_crystal_F_000 1582 _exptl_crystal_size_max 0.78 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _refine_diff_density_max 7.664 _refine_diff_density_min -3.521 _refine_diff_density_rms 0.230 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 405 _refine_ls_number_reflns 6474 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.049 _refine_ls_R_factor_all 0.0876 _refine_ls_R_factor_gt 0.0709 _refine_ls_shift/su_max 0.020 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+51.6000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1892 _refine_ls_wR_factor_ref 0.2008 _reflns_number_gt 5176 _reflns_number_total 6474 _reflns_threshold_expression I>2sigma(I) _cod_data_source_file ic050097wsi20050217_082525_07.cif _cod_data_source_block 5a _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_cell_volume 3168.7(11) _cod_original_formula_sum 'C33 H25.20 Cl2.80 Hg0.95 N4 O2.60' _cod_database_code 1100730 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hg1 Hg 0.45441(2) 1.07802(4) -0.23063(2) 0.03502(18) Uani 0.95 1 d P . . Cl1 Cl 0.40269(16) 0.9632(3) -0.12286(19) 0.0489(7) Uani 1 1 d . . . Cl2 Cl 0.44539(17) 1.2605(3) -0.31303(18) 0.0468(7) Uani 1 1 d . . . N1 N 0.5777(5) 1.0976(8) -0.1793(5) 0.0307(18) Uani 1 1 d . . . N2 N 0.7597(4) 1.2607(7) -0.3033(5) 0.0255(16) Uani 1 1 d . . . H2A H 0.7431 1.1924 -0.3234 0.031 Uiso 1 1 calc R . . N3 N 0.7516(4) 1.0921(7) -0.5045(5) 0.0277(17) Uani 1 1 d . . . H3A H 0.7532 1.1094 -0.5568 0.033 Uiso 1 1 calc R . . N4 N 0.5482(4) 1.0473(8) -0.6453(5) 0.0287(17) Uani 1 1 d . . . O1 O 0.7766(4) 1.3673(7) -0.1803(4) 0.0345(16) Uani 1 1 d . . . O2 O 0.6808(4) 1.0815(6) -0.3913(4) 0.0335(16) Uani 1 1 d . . . C1 C 0.5992(6) 1.0394(9) -0.1088(6) 0.030(2) Uani 1 1 d . . . H1A H 0.5659 0.9881 -0.0830 0.036 Uiso 1 1 calc R . . C2 C 0.6699(5) 1.0531(10) -0.0728(6) 0.033(2) Uani 1 1 d . . . H2B H 0.6837 1.0106 -0.0244 0.040 Uiso 1 1 calc R . . C3 C 0.7183(5) 1.1300(10) -0.1102(6) 0.030(2) Uani 1 1 d . . . H3B H 0.7655 1.1407 -0.0872 0.036 Uiso 1 1 calc R . . C4 C 0.6964(5) 1.1927(9) -0.1836(5) 0.0244(19) Uani 1 1 d . . . C5 C 0.6259(5) 1.1735(9) -0.2158(6) 0.028(2) Uani 1 1 d . . . H5A H 0.6111 1.2144 -0.2645 0.034 Uiso 1 1 calc R . . C6 C 0.7471(5) 1.2841(9) -0.2222(6) 0.0268(19) Uani 1 1 d . . . C7 C 0.7978(5) 1.3387(8) -0.3580(6) 0.0240(18) Uani 1 1 d . . . C8 C 0.7880(5) 1.4675(9) -0.3549(6) 0.027(2) Uani 1 1 d . . . H8A H 0.7589 1.5022 -0.3145 0.033 Uiso 1 1 calc R . . C9 C 0.8217(6) 1.5412(9) -0.4117(6) 0.032(2) Uani 1 1 d . . . H9A H 0.8162 1.6261 -0.4084 0.038 Uiso 1 1 calc R . . C10 C 0.8646(5) 1.4901(9) -0.4753(6) 0.028(2) Uani 1 1 d . . . C11 C 0.8958(6) 1.5650(10) -0.5379(7) 0.037(2) Uani 1 1 d . . . H11A H 0.8899 1.6500 -0.5365 0.044 Uiso 1 1 calc R . . C12 C 0.9346(7) 1.5119(11) -0.6004(7) 0.042(3) Uani 1 1 d . . . H12A H 0.9536 1.5607 -0.6421 0.050 Uiso 1 1 calc R . . C13 C 0.9456(7) 1.3863(11) -0.6015(7) 0.043(3) Uani 1 1 d . . . H13A H 0.9729 1.3520 -0.6436 0.052 Uiso 1 1 calc R . . C14 C 0.9175(6) 1.3112(9) -0.5427(6) 0.031(2) Uani 1 1 d . . . H14A H 0.9266 1.2271 -0.5446 0.038 Uiso 1 1 calc R . . C15 C 0.8739(5) 1.3603(9) -0.4779(6) 0.027(2) Uani 1 1 d . . . C16 C 0.8408(5) 1.2850(8) -0.4174(5) 0.0224(18) Uani 1 1 d . . . C17 C 0.8591(5) 1.1496(9) -0.4167(5) 0.0249(19) Uani 1 1 d . . . C18 C 0.9264(5) 1.1144(9) -0.3748(6) 0.0257(19) Uani 1 1 d . . . C19 C 0.9718(5) 1.2029(10) -0.3317(6) 0.029(2) Uani 1 1 d . . . H19A H 0.9566 1.2845 -0.3285 0.035 Uiso 1 1 calc R . . C20 C 1.0376(6) 1.1675(10) -0.2953(7) 0.034(2) Uani 1 1 d . . . H20A H 1.0672 1.2258 -0.2681 0.041 Uiso 1 1 calc R . . C21 C 1.0615(6) 1.0420(11) -0.2985(7) 0.038(2) Uani 1 1 d . . . H21A H 1.1065 1.0195 -0.2738 0.046 Uiso 1 1 calc R . . C22 C 1.0190(6) 0.9563(9) -0.3373(6) 0.032(2) Uani 1 1 d . . . H22A H 1.0347 0.8749 -0.3383 0.038 Uiso 1 1 calc R . . C23 C 0.9494(6) 0.9891(9) -0.3771(6) 0.030(2) Uani 1 1 d . . . C24 C 0.9056(6) 0.9036(10) -0.4199(7) 0.037(2) Uani 1 1 d . . . H24A H 0.9205 0.8217 -0.4214 0.044 Uiso 1 1 calc R . . C25 C 0.8408(6) 0.9372(9) -0.4601(7) 0.037(2) Uani 1 1 d . . . H25A H 0.8118 0.8786 -0.4878 0.044 Uiso 1 1 calc R . . C26 C 0.8183(5) 1.0633(9) -0.4589(6) 0.027(2) Uani 1 1 d . . . C27 C 0.6858(6) 1.0928(8) -0.4672(6) 0.029(2) Uani 1 1 d . . . C28 C 0.6188(5) 1.1039(9) -0.5212(6) 0.027(2) Uani 1 1 d . . . C29 C 0.5569(6) 1.1659(10) -0.4917(7) 0.035(2) Uani 1 1 d . . . H29A H 0.5593 1.2046 -0.4399 0.042 Uiso 1 1 calc R . . C30 C 0.4946(6) 1.1691(11) -0.5382(8) 0.043(3) Uani 1 1 d . . . H30A H 0.4538 1.2113 -0.5197 0.052 Uiso 1 1 calc R . . C31 C 0.4915(6) 1.1083(10) -0.6153(7) 0.038(2) Uani 1 1 d . . . H31A H 0.4477 1.1107 -0.6469 0.046 Uiso 1 1 calc R . . C32 C 0.6121(6) 1.0460(9) -0.5993(6) 0.029(2) Uani 1 1 d . . . H32A H 0.6526 1.0056 -0.6201 0.035 Uiso 1 1 calc R . . Cl3 Cl 1.3075(3) 1.2704(5) -0.1419(4) 0.0254(11) Uani 0.40 1 d PD A -1 Cl4 Cl 1.2311(4) 1.2549(11) -0.3030(6) 0.079(3) Uani 0.40 1 d PD A -1 C50 C 1.2754(12) 1.359(2) -0.2300(9) 0.024(5) Uiso 0.40 1 d PD A -1 H50A H 1.3164 1.4003 -0.2557 0.029 Uiso 0.40 1 calc PR A -1 H50B H 1.2409 1.4217 -0.2126 0.029 Uiso 0.40 1 calc PR A -1 O3 O 1.3137(7) 1.2136(12) -0.2119(9) 0.046(3) Uani 0.60 1 d P B -2 H63 H 1.2974 1.2027 -0.2596 0.069 Uiso 0.60 1 calc PR B -2 C51 C 1.2736(8) 1.3334(13) -0.1712(9) 0.022(3) Uiso 0.60 1 d P B -2 H51A H 1.2478 1.3084 -0.1229 0.032 Uiso 0.60 1 calc PR B -2 H51B H 1.2395 1.3684 -0.2116 0.032 Uiso 0.60 1 calc PR B -2 H51C H 1.3101 1.3937 -0.1554 0.032 Uiso 0.60 1 calc PR B -2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hg1 0.0298(3) 0.0475(3) 0.0272(2) 0.00447(17) -0.00617(16) -0.01402(18) Cl1 0.0349(15) 0.0655(19) 0.0469(16) 0.0174(14) 0.0120(12) -0.0009(13) Cl2 0.0514(17) 0.0426(15) 0.0463(15) 0.0046(12) 0.0000(13) 0.0038(13) N1 0.023(4) 0.043(5) 0.025(4) 0.001(3) -0.005(3) -0.007(4) N2 0.027(4) 0.027(4) 0.023(4) -0.002(3) 0.004(3) -0.007(3) N3 0.024(4) 0.036(4) 0.023(4) 0.002(3) -0.003(3) -0.002(3) N4 0.022(4) 0.035(4) 0.029(4) 0.006(3) -0.004(3) -0.007(3) O1 0.032(4) 0.044(4) 0.027(3) -0.010(3) -0.001(3) -0.011(3) O2 0.037(4) 0.039(4) 0.024(3) -0.006(3) -0.001(3) -0.011(3) C1 0.030(5) 0.032(5) 0.028(5) 0.000(4) 0.000(4) 0.003(4) C2 0.022(5) 0.047(6) 0.030(5) 0.002(4) -0.008(4) 0.006(4) C3 0.023(5) 0.039(5) 0.029(5) -0.002(4) -0.004(4) 0.003(4) C4 0.019(4) 0.033(5) 0.021(4) -0.002(4) 0.002(3) -0.006(4) C5 0.024(5) 0.039(5) 0.022(4) 0.002(4) 0.002(4) -0.003(4) C6 0.020(4) 0.037(5) 0.024(4) -0.005(4) -0.002(3) -0.005(4) C7 0.020(4) 0.028(5) 0.024(4) -0.004(4) -0.001(3) -0.003(4) C8 0.023(5) 0.028(5) 0.031(5) -0.006(4) -0.001(4) 0.003(4) C9 0.031(5) 0.028(5) 0.035(5) 0.001(4) -0.001(4) -0.001(4) C10 0.026(5) 0.026(5) 0.033(5) 0.001(4) -0.002(4) -0.001(4) C11 0.045(6) 0.032(5) 0.035(5) 0.007(4) 0.000(5) -0.005(5) C12 0.049(7) 0.038(6) 0.039(6) 0.012(5) 0.008(5) -0.007(5) C13 0.045(7) 0.047(6) 0.038(6) 0.003(5) 0.013(5) 0.000(5) C14 0.032(5) 0.033(5) 0.030(5) 0.004(4) 0.005(4) 0.003(4) C15 0.022(5) 0.036(5) 0.024(4) 0.001(4) -0.002(4) -0.002(4) C16 0.021(4) 0.026(4) 0.020(4) 0.002(3) 0.000(3) -0.003(4) C17 0.027(5) 0.028(5) 0.019(4) -0.002(3) 0.004(3) 0.000(4) C18 0.025(5) 0.029(5) 0.024(4) 0.006(4) 0.002(4) 0.002(4) C19 0.022(5) 0.036(5) 0.029(5) -0.001(4) 0.001(4) 0.003(4) C20 0.024(5) 0.042(6) 0.036(5) 0.000(4) -0.009(4) -0.001(4) C21 0.026(5) 0.049(6) 0.038(6) 0.003(5) -0.004(4) 0.013(5) C22 0.030(5) 0.032(5) 0.034(5) 0.003(4) -0.003(4) 0.013(4) C23 0.030(5) 0.035(5) 0.024(5) 0.002(4) 0.000(4) 0.003(4) C24 0.040(6) 0.029(5) 0.041(6) -0.005(4) -0.003(5) 0.005(4) C25 0.043(6) 0.028(5) 0.038(6) -0.009(4) -0.012(5) 0.000(4) C26 0.026(5) 0.033(5) 0.022(4) -0.001(4) -0.002(4) 0.000(4) C27 0.033(5) 0.025(5) 0.027(5) -0.002(4) 0.000(4) -0.008(4) C28 0.029(5) 0.027(5) 0.025(4) -0.001(4) 0.001(4) -0.006(4) C29 0.039(6) 0.034(5) 0.033(5) -0.003(4) 0.003(4) -0.005(4) C30 0.030(6) 0.047(6) 0.052(7) 0.002(5) -0.004(5) 0.008(5) C31 0.031(6) 0.041(6) 0.042(6) 0.005(5) -0.008(5) -0.002(5) C32 0.035(5) 0.029(5) 0.023(4) -0.002(4) -0.001(4) -0.010(4) Cl3 0.015(2) 0.017(2) 0.045(3) 0.006(2) 0.013(2) -0.0038(19) Cl4 0.029(4) 0.125(9) 0.080(6) 0.034(6) -0.028(4) -0.030(5) O3 0.034(7) 0.040(7) 0.063(9) 0.011(7) -0.001(6) -0.013(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Hg1 N1 100.9(2) . . ? Cl1 Hg1 Cl2 145.64(11) . . ? N1 Hg1 Cl2 99.5(2) . . ? Cl1 Hg1 N4 108.0(2) . 3_674 ? N1 Hg1 N4 109.2(3) . 3_674 ? Cl2 Hg1 N4 90.8(2) . 3_674 ? C1 N1 C5 118.6(8) . . ? C1 N1 Hg1 119.7(7) . . ? C5 N1 Hg1 121.6(6) . . ? C6 N2 C7 125.8(8) . . ? C27 N3 C26 121.5(8) . . ? C31 N4 C32 118.0(9) . . ? C31 N4 Hg1 125.8(7) . 3_674 ? C32 N4 Hg1 115.9(7) . 3_674 ? N1 C1 C2 122.3(10) . . ? C3 C2 C1 118.8(9) . . ? C2 C3 C4 119.6(9) . . ? C5 C4 C3 118.3(9) . . ? C5 C4 C6 121.3(8) . . ? C3 C4 C6 120.3(8) . . ? N1 C5 C4 122.5(9) . . ? O1 C6 N2 125.1(9) . . ? O1 C6 C4 121.3(8) . . ? N2 C6 C4 113.5(8) . . ? C16 C7 C8 121.2(9) . . ? C16 C7 N2 118.3(8) . . ? C8 C7 N2 120.4(8) . . ? C9 C8 C7 119.7(9) . . ? C8 C9 C10 121.2(9) . . ? C9 C10 C15 118.5(9) . . ? C9 C10 C11 121.7(9) . . ? C15 C10 C11 119.7(9) . . ? C12 C11 C10 120.1(10) . . ? C11 C12 C13 120.3(10) . . ? C14 C13 C12 121.8(11) . . ? C13 C14 C15 120.7(10) . . ? C16 C15 C10 120.0(9) . . ? C16 C15 C14 122.6(9) . . ? C10 C15 C14 117.4(9) . . ? C7 C16 C15 119.4(9) . . ? C7 C16 C17 122.5(8) . . ? C15 C16 C17 118.0(8) . . ? C26 C17 C18 119.6(9) . . ? C26 C17 C16 123.5(9) . . ? C18 C17 C16 116.7(8) . . ? C23 C18 C17 119.5(9) . . ? C23 C18 C19 119.3(9) . . ? C17 C18 C19 121.2(9) . . ? C20 C19 C18 120.0(9) . . ? C19 C20 C21 121.0(10) . . ? C22 C21 C20 120.2(9) . . ? C21 C22 C23 121.0(9) . . ? C24 C23 C18 119.1(9) . . ? C24 C23 C22 122.2(9) . . ? C18 C23 C22 118.6(9) . . ? C25 C24 C23 121.5(10) . . ? C24 C25 C26 119.3(9) . . ? C17 C26 C25 121.0(9) . . ? C17 C26 N3 122.9(9) . . ? C25 C26 N3 116.1(8) . . ? O2 C27 N3 122.1(9) . . ? O2 C27 C28 120.1(9) . . ? N3 C27 C28 117.8(8) . . ? C32 C28 C29 117.9(9) . . ? C32 C28 C27 122.1(9) . . ? C29 C28 C27 119.8(9) . . ? C30 C29 C28 119.9(10) . . ? C29 C30 C31 119.3(11) . . ? N4 C31 C30 123.0(10) . . ? N4 C32 C28 121.9(10) . . ? Cl3 C50 Cl4 107.3(12) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg1 Cl1 2.353(3) . ? Hg1 N1 2.375(8) . ? Hg1 Cl2 2.385(3) . ? Hg1 N4 2.409(8) 3_674 ? N1 C1 1.341(13) . ? N1 C5 1.352(12) . ? N2 C6 1.351(12) . ? N2 C7 1.418(12) . ? N3 C27 1.356(13) . ? N3 C26 1.432(12) . ? N4 C31 1.332(14) . ? N4 C32 1.355(13) . ? N4 Hg1 2.409(8) 3_674 ? O1 C6 1.238(11) . ? O2 C27 1.230(12) . ? C1 C2 1.402(14) . ? C2 C3 1.367(15) . ? C3 C4 1.406(13) . ? C4 C5 1.384(13) . ? C4 C6 1.503(13) . ? C7 C16 1.383(13) . ? C7 C8 1.411(14) . ? C8 C9 1.372(14) . ? C9 C10 1.419(14) . ? C10 C15 1.421(14) . ? C10 C11 1.425(14) . ? C11 C12 1.372(16) . ? C12 C13 1.379(17) . ? C13 C14 1.359(15) . ? C14 C15 1.431(14) . ? C15 C16 1.418(13) . ? C16 C17 1.507(13) . ? C17 C26 1.362(13) . ? C17 C18 1.429(13) . ? C18 C23 1.425(14) . ? C18 C19 1.431(14) . ? C19 C20 1.371(14) . ? C20 C21 1.433(15) . ? C21 C22 1.349(16) . ? C22 C23 1.444(13) . ? C23 C24 1.391(15) . ? C24 C25 1.375(15) . ? C25 C26 1.430(14) . ? C27 C28 1.477(14) . ? C28 C32 1.403(13) . ? C28 C29 1.408(15) . ? C29 C30 1.337(15) . ? C30 C31 1.400(16) . ? Cl3 C50 1.795(17) . ? Cl4 C50 1.802(17) . ? O3 C51 1.64(2) . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2A O2 0.86 1.96 2.776(10) 158.2 . N3 H3A O1 0.86 2.05 2.902(10) 168.7 4_585
1100731.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100731.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100731 loop_ _publ_author_name 'Tara J. Burchell' 'Richard J. Puddephatt' _publ_section_title ; Self-Assembly of Chiral Coordination Polymers and Macrocycles: A Metal Template Effect on the Polymer-Macrocycle Equilibrium ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3718 _journal_page_last 3730 _journal_paper_doi 10.1021/ic050097w _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C33 H22 Br2 Cl2 Hg N4 O2' _chemical_formula_weight 937.86 _chemical_name_systematic ; ? ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 92.50(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 18.187(4) _cell_length_b 11.165(2) _cell_length_c 16.286(3) _cell_measurement_temperature 150(2) _cell_volume 3303.9(11) _computing_cell_refinement 'Nonius DENZO' _computing_data_collection 'Nonius COLLECT' _computing_data_reduction 'Nonius DENZO' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'phi\omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.061 _diffrn_reflns_av_sigmaI/netI 0.0385 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 38979 _diffrn_reflns_theta_full 25.03 _diffrn_reflns_theta_max 25.03 _diffrn_reflns_theta_min 2.70 _exptl_absorpt_coefficient_mu 7.276 _exptl_absorpt_correction_T_max 0.6114 _exptl_absorpt_correction_T_min 0.1147 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Denzo-SMN (Otwinowski & Minor, 1997)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.886 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 1792 _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _refine_diff_density_max 1.968 _refine_diff_density_min -2.581 _refine_diff_density_rms 0.138 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 392 _refine_ls_number_reflns 5841 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 0.988 _refine_ls_R_factor_all 0.0741 _refine_ls_R_factor_gt 0.0514 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0799P)^2^+19.5444P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1331 _refine_ls_wR_factor_ref 0.1486 _reflns_number_gt 4343 _reflns_number_total 5841 _reflns_threshold_expression I>2sigma(I) _cod_data_source_file ic050097wsi20050217_082525_08.cif _cod_data_source_block 5b _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_cell_volume 3303.6(11) _cod_database_code 1100731 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hg1 Hg -0.044168(19) 0.41744(4) 0.26885(2) 0.05495(16) Uani 1 1 d . . . Br1 Br -0.07021(18) 0.2448(3) 0.17696(19) 0.0784(11) Uiso 0.55 1 d P A 1 Br2 Br -0.09631(14) 0.5032(3) 0.39137(15) 0.0661(8) Uiso 0.55 1 d P A 1 Br1A Br -0.04987(19) 0.2364(3) 0.17715(18) 0.0581(9) Uiso 0.45 1 d P A 2 Br2A Br -0.09616(14) 0.5414(3) 0.38116(15) 0.0505(7) Uiso 0.45 1 d P A 2 N1 N 0.0828(4) 0.3976(6) 0.3151(4) 0.0436(17) Uani 1 1 d . A . C1 C 0.1048(5) 0.4536(8) 0.3844(5) 0.047(2) Uani 1 1 d . . . H1A H 0.0712 0.5040 0.4112 0.057 Uiso 1 1 calc R A . C2 C 0.1754(5) 0.4394(8) 0.4176(5) 0.054(2) Uani 1 1 d . A . H2A H 0.1906 0.4807 0.4664 0.065 Uiso 1 1 calc R . . C3 C 0.2241(5) 0.3641(8) 0.3791(5) 0.047(2) Uani 1 1 d . . . H3A H 0.2726 0.3528 0.4016 0.056 Uiso 1 1 calc R A . C4 C 0.2013(4) 0.3065(7) 0.3083(4) 0.0376(17) Uani 1 1 d . A . C5 C 0.1299(4) 0.3249(8) 0.2767(4) 0.0423(19) Uani 1 1 d . . . H5A H 0.1139 0.2857 0.2274 0.051 Uiso 1 1 calc R A . C6 C 0.2516(4) 0.2178(7) 0.2701(5) 0.0395(18) Uani 1 1 d . . . O1 O 0.2786(3) 0.1360(6) 0.3109(3) 0.0561(16) Uani 1 1 d . A . N2 N 0.2624(3) 0.2384(6) 0.1904(4) 0.0396(15) Uani 1 1 d . A . H2B H 0.2441 0.3055 0.1698 0.048 Uiso 1 1 calc R . . C7 C 0.3006(4) 0.1628(7) 0.1352(4) 0.0365(17) Uani 1 1 d . . . C8 C 0.2923(4) 0.0364(8) 0.1411(5) 0.0443(19) Uani 1 1 d . A . H8A H 0.2646 0.0022 0.1834 0.053 Uiso 1 1 calc R . . C9 C 0.3245(5) -0.0344(8) 0.0856(5) 0.049(2) Uani 1 1 d . . . H9A H 0.3193 -0.1188 0.0897 0.059 Uiso 1 1 calc R A . C10 C 0.3656(5) 0.0131(8) 0.0217(5) 0.045(2) Uani 1 1 d . A . C11 C 0.3973(6) -0.0579(9) -0.0391(6) 0.062(3) Uani 1 1 d . . . H11A H 0.3918 -0.1424 -0.0372 0.074 Uiso 1 1 calc R A . C12 C 0.4351(6) -0.0087(11) -0.0995(7) 0.071(3) Uani 1 1 d . A . H12A H 0.4549 -0.0586 -0.1404 0.085 Uiso 1 1 calc R . . C13 C 0.4456(6) 0.1139(10) -0.1029(6) 0.067(3) Uani 1 1 d . . . H13A H 0.4727 0.1476 -0.1458 0.080 Uiso 1 1 calc R A . C14 C 0.4171(5) 0.1868(9) -0.0449(5) 0.052(2) Uani 1 1 d . A . H14A H 0.4256 0.2707 -0.0471 0.063 Uiso 1 1 calc R . . C15 C 0.3749(4) 0.1391(7) 0.0185(4) 0.0372(17) Uani 1 1 d . . . C16 C 0.3415(4) 0.2137(7) 0.0770(4) 0.0333(16) Uani 1 1 d . A . C17 C 0.3599(4) 0.3460(7) 0.0769(4) 0.0369(17) Uani 1 1 d . . . C18 C 0.4257(4) 0.3825(7) 0.1196(4) 0.0388(18) Uani 1 1 d . A . C19 C 0.4713(5) 0.3007(9) 0.1654(5) 0.048(2) Uani 1 1 d . . . H19A H 0.4565 0.2194 0.1698 0.058 Uiso 1 1 calc R A . C20 C 0.5363(5) 0.3375(10) 0.2032(6) 0.063(3) Uani 1 1 d . A . H20A H 0.5669 0.2812 0.2321 0.075 Uiso 1 1 calc R . . C21 C 0.5576(6) 0.4567(12) 0.1994(6) 0.073(3) Uani 1 1 d . . . H21A H 0.6028 0.4812 0.2257 0.087 Uiso 1 1 calc R A . C22 C 0.5153(6) 0.5376(11) 0.1590(6) 0.067(3) Uani 1 1 d . A . H22A H 0.5303 0.6191 0.1587 0.081 Uiso 1 1 calc R . . C23 C 0.4481(5) 0.5039(9) 0.1164(5) 0.054(2) Uani 1 1 d . . . C24 C 0.4052(6) 0.5859(9) 0.0694(7) 0.065(3) Uani 1 1 d . A . H24A H 0.4205 0.6671 0.0659 0.078 Uiso 1 1 calc R . . C25 C 0.3421(6) 0.5495(9) 0.0291(6) 0.059(2) Uani 1 1 d . . . H25A H 0.3129 0.6059 -0.0014 0.071 Uiso 1 1 calc R A . C26 C 0.3195(5) 0.4283(7) 0.0321(5) 0.0411(19) Uani 1 1 d . A . N3 N 0.2522(4) 0.3986(6) -0.0130(4) 0.0407(16) Uani 1 1 d . . . H3B H 0.2538 0.3806 -0.0655 0.049 Uiso 1 1 calc R A . C27 C 0.1874(5) 0.3976(7) 0.0222(5) 0.0415(19) Uani 1 1 d . A . O2 O 0.1813(4) 0.4052(6) 0.0977(3) 0.0558(16) Uani 1 1 d . . . C28 C 0.1185(4) 0.3897(7) -0.0304(5) 0.0402(18) Uani 1 1 d . . . C29 C 0.0576(5) 0.3328(9) -0.0013(5) 0.057(2) Uani 1 1 d . A . H29A H 0.0603 0.2940 0.0506 0.069 Uiso 1 1 calc R . . C30 C -0.0067(6) 0.3330(10) -0.0481(6) 0.067(3) Uani 1 1 d . . . H30A H -0.0487 0.2919 -0.0296 0.080 Uiso 1 1 calc R A . C31 C -0.0102(6) 0.3929(9) -0.1220(6) 0.060(3) Uani 1 1 d . A . H31A H -0.0557 0.3952 -0.1530 0.072 Uiso 1 1 calc R . . C32 C 0.1115(5) 0.4458(7) -0.1060(5) 0.0419(19) Uani 1 1 d . A . H32A H 0.1535 0.4844 -0.1265 0.050 Uiso 1 1 calc R . . N4 N 0.0488(4) 0.4485(7) -0.1517(4) 0.0533(19) Uani 1 1 d . . . C51 C 0.270(5) -0.258(3) 0.231(2) 0.23(4) Uiso 0.40 1 d PD B 1 Cl3 Cl 0.2665(8) -0.1801(14) 0.3212(9) 0.156(5) Uiso 0.40 1 d PD B 1 Cl1 Cl 0.3019(11) -0.4014(17) 0.2414(12) 0.188(7) Uiso 0.40 1 d PD B 1 Cl2 Cl 0.2011(4) -0.2766(7) 0.1406(5) 0.127(2) Uiso 0.60 1 d PD C 2 C50 C 0.2292(10) -0.3767(18) 0.2147(10) 0.074(5) Uiso 0.60 1 d PD C 2 Cl4 Cl 0.2762(12) -0.303(2) 0.2902(12) 0.307(9) Uiso 0.60 1 d PD C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hg1 0.0483(2) 0.0754(3) 0.0404(2) -0.00160(16) -0.00598(14) 0.01616(18) N1 0.034(4) 0.062(5) 0.034(3) 0.004(3) -0.005(3) 0.009(3) C1 0.041(5) 0.057(5) 0.043(5) -0.004(4) 0.001(4) 0.005(4) C2 0.060(6) 0.058(6) 0.044(5) -0.012(4) -0.006(4) 0.004(5) C3 0.039(5) 0.060(5) 0.041(4) -0.001(4) -0.006(3) 0.006(4) C4 0.034(4) 0.045(5) 0.034(4) 0.008(3) 0.002(3) 0.001(4) C5 0.039(4) 0.059(5) 0.029(4) 0.000(4) -0.004(3) 0.004(4) C6 0.031(4) 0.048(5) 0.039(4) 0.006(4) 0.002(3) 0.004(4) O1 0.062(4) 0.065(4) 0.042(3) 0.014(3) 0.006(3) 0.024(3) N2 0.041(4) 0.046(4) 0.032(3) 0.009(3) 0.006(3) 0.007(3) C7 0.034(4) 0.042(4) 0.033(4) -0.002(3) 0.000(3) 0.007(3) C8 0.038(5) 0.046(5) 0.048(5) 0.008(4) 0.001(4) -0.002(4) C9 0.056(5) 0.040(5) 0.051(5) 0.003(4) -0.004(4) -0.004(4) C10 0.040(5) 0.050(5) 0.046(4) -0.007(4) -0.010(4) 0.005(4) C11 0.073(7) 0.055(6) 0.056(6) -0.018(5) -0.005(5) 0.016(5) C12 0.075(7) 0.076(8) 0.064(6) -0.025(6) 0.017(5) 0.012(6) C13 0.073(7) 0.075(7) 0.055(6) -0.007(5) 0.025(5) 0.011(6) C14 0.052(5) 0.062(6) 0.044(5) -0.005(4) 0.013(4) 0.005(5) C15 0.030(4) 0.047(5) 0.033(4) -0.004(3) -0.005(3) 0.003(3) C16 0.026(4) 0.043(4) 0.030(4) 0.000(3) -0.005(3) 0.003(3) C17 0.034(4) 0.046(5) 0.031(4) -0.004(3) 0.004(3) -0.004(4) C18 0.043(5) 0.043(5) 0.031(4) -0.002(3) 0.006(3) -0.006(4) C19 0.041(5) 0.062(6) 0.042(4) -0.001(4) -0.004(4) 0.004(4) C20 0.054(6) 0.078(8) 0.056(5) -0.005(5) -0.008(4) 0.003(5) C21 0.058(6) 0.108(10) 0.051(6) -0.007(6) -0.005(5) -0.025(7) C22 0.074(7) 0.074(7) 0.054(6) -0.006(5) 0.001(5) -0.029(6) C23 0.053(6) 0.066(6) 0.044(5) -0.003(4) 0.002(4) -0.012(5) C24 0.069(7) 0.050(6) 0.076(7) 0.004(5) -0.010(5) -0.019(5) C25 0.061(6) 0.055(6) 0.060(6) 0.011(5) -0.012(5) 0.003(5) C26 0.046(5) 0.044(5) 0.033(4) 0.000(3) -0.004(3) -0.003(4) N3 0.039(4) 0.048(4) 0.034(3) -0.001(3) -0.006(3) 0.006(3) C27 0.048(5) 0.042(5) 0.035(4) 0.005(3) -0.002(3) 0.009(4) O2 0.056(4) 0.082(5) 0.029(3) 0.009(3) -0.001(3) 0.010(3) C28 0.043(5) 0.041(5) 0.037(4) 0.001(3) 0.000(3) 0.010(4) C29 0.061(6) 0.070(6) 0.041(5) 0.010(4) -0.001(4) -0.010(5) C30 0.056(6) 0.078(7) 0.066(6) 0.005(5) -0.006(5) -0.019(5) C31 0.051(6) 0.079(7) 0.050(5) -0.008(5) -0.014(4) -0.001(5) C32 0.038(4) 0.050(5) 0.037(4) 0.006(3) -0.006(3) 0.007(4) N4 0.054(5) 0.064(5) 0.041(4) 0.001(3) -0.004(3) 0.006(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Hg1 N4 107.6(2) . 3_565 ? N1 Hg1 Br2 100.49(17) . . ? N4 Hg1 Br2 113.54(19) 3_565 . ? N1 Hg1 Br1 105.84(19) . . ? N4 Hg1 Br1 90.3(2) 3_565 . ? Br2 Hg1 Br1 136.82(10) . . ? N1 Hg1 Br2A 102.10(17) . . ? N4 Hg1 Br2A 103.39(19) 3_565 . ? Br2 Hg1 Br2A 10.48(8) . . ? Br1 Hg1 Br2A 143.32(10) . . ? N1 Hg1 Br1A 97.22(19) . . ? N4 Hg1 Br1A 91.71(19) 3_565 . ? Br2 Hg1 Br1A 142.54(10) . . ? Br1 Hg1 Br1A 8.73(11) . . ? Br2A Hg1 Br1A 150.37(10) . . ? C1 N1 C5 119.9(7) . . ? C1 N1 Hg1 117.9(5) . . ? C5 N1 Hg1 122.0(5) . . ? N1 C1 C2 121.1(8) . . ? C1 C2 C3 119.5(8) . . ? C4 C3 C2 119.3(8) . . ? C3 C4 C5 119.1(7) . . ? C3 C4 C6 119.4(7) . . ? C5 C4 C6 121.4(7) . . ? N1 C5 C4 121.2(7) . . ? O1 C6 N2 125.7(7) . . ? O1 C6 C4 120.3(7) . . ? N2 C6 C4 113.9(7) . . ? C6 N2 C7 126.9(7) . . ? C16 C7 C8 121.7(7) . . ? C16 C7 N2 119.2(7) . . ? C8 C7 N2 119.1(7) . . ? C9 C8 C7 118.9(8) . . ? C8 C9 C10 122.2(8) . . ? C9 C10 C11 123.5(9) . . ? C9 C10 C15 118.0(8) . . ? C11 C10 C15 118.5(8) . . ? C12 C11 C10 121.6(10) . . ? C11 C12 C13 120.6(9) . . ? C14 C13 C12 120.4(10) . . ? C13 C14 C15 120.9(9) . . ? C14 C15 C10 118.1(7) . . ? C14 C15 C16 121.9(8) . . ? C10 C15 C16 120.0(7) . . ? C7 C16 C15 119.2(7) . . ? C7 C16 C17 122.5(7) . . ? C15 C16 C17 118.0(7) . . ? C26 C17 C18 119.5(7) . . ? C26 C17 C16 122.8(7) . . ? C18 C17 C16 117.5(7) . . ? C17 C18 C23 119.6(8) . . ? C17 C18 C19 122.3(8) . . ? C23 C18 C19 118.1(8) . . ? C20 C19 C18 121.0(9) . . ? C19 C20 C21 120.3(10) . . ? C22 C21 C20 120.8(10) . . ? C21 C22 C23 121.4(10) . . ? C24 C23 C18 119.3(8) . . ? C24 C23 C22 122.3(9) . . ? C18 C23 C22 118.4(9) . . ? C25 C24 C23 120.2(9) . . ? C24 C25 C26 120.6(9) . . ? C17 C26 C25 120.7(8) . . ? C17 C26 N3 122.9(7) . . ? C25 C26 N3 116.4(7) . . ? C27 N3 C26 122.0(7) . . ? O2 C27 N3 122.9(8) . . ? O2 C27 C28 117.7(8) . . ? N3 C27 C28 119.4(7) . . ? C29 C28 C32 118.1(8) . . ? C29 C28 C27 119.9(7) . . ? C32 C28 C27 121.8(8) . . ? C30 C29 C28 119.3(8) . . ? C29 C30 C31 119.5(9) . . ? N4 C31 C30 122.1(9) . . ? N4 C32 C28 123.3(8) . . ? C32 N4 C31 117.6(8) . . ? C32 N4 Hg1 116.9(6) . 3_565 ? C31 N4 Hg1 124.5(6) . 3_565 ? Cl1 C51 Cl3 115(3) . . ? Cl4 C50 Cl2 108.7(15) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg1 N1 2.407(6) . ? Hg1 N4 2.423(7) 3_565 ? Hg1 Br2 2.442(2) . ? Hg1 Br1 2.474(3) . ? Hg1 Br2A 2.511(3) . ? Hg1 Br1A 2.513(3) . ? N1 C1 1.336(11) . ? N1 C5 1.352(10) . ? C1 C2 1.382(12) . ? C2 C3 1.390(12) . ? C3 C4 1.369(11) . ? C4 C5 1.391(11) . ? C4 C6 1.503(11) . ? C6 O1 1.220(9) . ? C6 N2 1.340(9) . ? N2 C7 1.434(9) . ? C7 C16 1.356(10) . ? C7 C8 1.424(12) . ? C8 C9 1.354(12) . ? C9 C10 1.409(12) . ? C10 C11 1.411(12) . ? C10 C15 1.418(12) . ? C11 C12 1.343(15) . ? C12 C13 1.384(16) . ? C13 C14 1.366(12) . ? C14 C15 1.416(11) . ? C15 C16 1.422(10) . ? C16 C17 1.515(11) . ? C17 C26 1.367(11) . ? C17 C18 1.417(11) . ? C18 C23 1.417(13) . ? C18 C19 1.422(12) . ? C19 C20 1.372(13) . ? C20 C21 1.388(16) . ? C21 C22 1.340(16) . ? C22 C23 1.430(14) . ? C23 C24 1.407(14) . ? C24 C25 1.360(14) . ? C25 C26 1.415(13) . ? C26 N3 1.439(10) . ? N3 C27 1.333(11) . ? C27 O2 1.243(9) . ? C27 C28 1.489(11) . ? C28 C29 1.378(12) . ? C28 C32 1.382(11) . ? C29 C30 1.367(13) . ? C30 C31 1.376(14) . ? C31 N4 1.349(13) . ? C32 N4 1.334(11) . ? N4 Hg1 2.423(7) 3_565 ? C51 Cl1 1.71(2) . ? C51 Cl3 1.71(2) . ? Cl2 C50 1.707(17) . ? C50 Cl4 1.685(18) . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2B O2 0.88 1.95 2.780(9) 156.5 . N3 H3B O1 0.88 2.09 2.953(9) 166.8 4_565
1100732.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $ #$Revision: 176435 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100732.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100732 loop_ _publ_author_name 'Tara J. Burchell' 'Richard J. Puddephatt' _publ_section_title ; Self-Assembly of Chiral Coordination Polymers and Macrocycles: A Metal Template Effect on the Polymer-Macrocycle Equilibrium ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3718 _journal_page_last 3730 _journal_paper_doi 10.1021/ic050097w _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C32.5 H24 Br3 Hg1.5 N4 O2.5' _chemical_formula_weight 1051.17 _chemical_name_systematic ; ? ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 102.03(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 16.652(3) _cell_length_b 12.318(3) _cell_length_c 16.223(3) _cell_measurement_reflns_used 7560 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 27.48 _cell_measurement_theta_min 1.7 _cell_volume 3254.6(12) _computing_cell_refinement 'Nonius DENZO' _computing_data_collection 'Nonius COLLECT' _computing_data_reduction 'Nonius DENZO' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'phi\omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.070 _diffrn_reflns_av_sigmaI/netI 0.0504 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 34242 _diffrn_reflns_theta_full 25.02 _diffrn_reflns_theta_max 25.02 _diffrn_reflns_theta_min 2.57 _exptl_absorpt_coefficient_mu 10.797 _exptl_absorpt_correction_T_max 0.5186 _exptl_absorpt_correction_T_min 0.3574 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.145 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1968 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _refine_diff_density_max 3.155 _refine_diff_density_min -5.641 _refine_diff_density_rms 0.324 _refine_ls_extinction_coef 0.00071(17) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 403 _refine_ls_number_reflns 5754 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.027 _refine_ls_R_factor_all 0.0810 _refine_ls_R_factor_gt 0.0625 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1110P)^2^+79.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1820 _refine_ls_wR_factor_ref 0.1954 _reflns_number_gt 4495 _reflns_number_total 5754 _reflns_threshold_expression I>2sigma(I) _cod_data_source_file ic050097wsi20050217_082525_09.cif _cod_data_source_block 6b _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_cell_volume 3254.4(11) _cod_original_formula_sum 'C32.50 H24 Br3 Hg1.50 N4 O2.50' _cod_database_code 1100732 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hg1 Hg 0.14697(3) 0.21819(4) 1.34689(3) 0.0255(2) Uani 1 1 d . . . Br1 Br 0.1383(6) 0.2444(11) 1.4966(9) 0.048(2) Uani 0.70 1 d P A 1 Br1A Br 0.1617(15) 0.233(3) 1.499(2) 0.055(6) Uani 0.30 1 d P A 2 Br2 Br 0.21240(9) 0.10610(11) 1.24991(9) 0.0319(4) Uani 1 1 d . A . Hg2 Hg 0.0000 0.5000 1.0000 0.0501(3) Uani 1 2 d S . . Br3 Br 0.03187(12) 0.54867(15) 1.14561(11) 0.0519(5) Uani 1 1 d . . . O1 O -0.1672(6) 0.4086(8) 0.9993(5) 0.026(2) Uani 1 1 d . . . O2 O -0.2924(6) 0.2243(7) 0.7286(5) 0.025(2) Uani 1 1 d . . . N1 N 0.0226(6) 0.2623(9) 1.2507(6) 0.021(2) Uani 1 1 d . A . N2 N -0.2565(7) 0.3745(8) 1.0836(6) 0.021(2) Uani 1 1 d . . . H2A H -0.2632 0.3501 1.1326 0.025 Uiso 1 1 calc R . . N3 N -0.2625(7) 0.2920(8) 0.8618(6) 0.024(2) Uani 1 1 d . . . H3A H -0.2382 0.3458 0.8930 0.029 Uiso 1 1 calc R . . N4 N -0.1958(7) 0.6071(8) 0.6948(6) 0.022(2) Uani 1 1 d . . . C1 C 0.0157(9) 0.2413(11) 1.1704(8) 0.028(3) Uani 1 1 d . . . H1A H 0.0585 0.2012 1.1539 0.033 Uiso 1 1 calc R A . C2 C -0.0498(8) 0.2736(11) 1.1080(8) 0.028(3) Uani 1 1 d . A . H2B H -0.0520 0.2581 1.0503 0.033 Uiso 1 1 calc R . . C3 C -0.1141(7) 0.3316(10) 1.1348(8) 0.020(3) Uani 1 1 d . . . C4 C -0.1072(8) 0.3517(10) 1.2180(8) 0.023(3) Uani 1 1 d . A . H4A H -0.1493 0.3901 1.2372 0.027 Uiso 1 1 calc R . . C5 C -0.0383(8) 0.3161(11) 1.2751(8) 0.027(3) Uani 1 1 d . . . H5A H -0.0342 0.3303 1.3333 0.032 Uiso 1 1 calc R A . C6 C -0.1812(7) 0.3757(10) 1.0657(7) 0.018(2) Uani 1 1 d . A . C7 C -0.3263(8) 0.4132(11) 1.0225(7) 0.023(3) Uani 1 1 d . . . C8 C -0.3448(9) 0.5267(10) 1.0225(8) 0.028(3) Uani 1 1 d . . . H8A H -0.3137 0.5735 1.0637 0.033 Uiso 1 1 calc R . . C9 C -0.4071(9) 0.5663(12) 0.9630(9) 0.030(3) Uani 1 1 d . . . H9A H -0.4193 0.6417 0.9629 0.037 Uiso 1 1 calc R . . C10 C -0.4545(9) 0.4991(12) 0.9015(8) 0.030(3) Uani 1 1 d . . . C11 C -0.5226(9) 0.5399(14) 0.8400(9) 0.038(4) Uani 1 1 d . . . H11A H -0.5346 0.6153 0.8383 0.046 Uiso 1 1 calc R . . C12 C -0.5699(10) 0.4723(16) 0.7845(10) 0.047(4) Uani 1 1 d . . . H12A H -0.6145 0.5008 0.7441 0.056 Uiso 1 1 calc R . . C13 C -0.5536(10) 0.3594(15) 0.7861(10) 0.044(4) Uani 1 1 d . . . H13A H -0.5878 0.3122 0.7478 0.053 Uiso 1 1 calc R . . C14 C -0.4877(9) 0.3185(14) 0.8436(9) 0.035(3) Uani 1 1 d . . . H14A H -0.4763 0.2429 0.8432 0.043 Uiso 1 1 calc R . . C15 C -0.4365(8) 0.3859(11) 0.9032(8) 0.025(3) Uani 1 1 d . . . C16 C -0.3697(8) 0.3435(11) 0.9639(8) 0.024(3) Uani 1 1 d . . . C17 C -0.3436(8) 0.2284(10) 0.9585(8) 0.024(3) Uani 1 1 d . . . C18 C -0.3717(8) 0.1430(11) 1.0054(8) 0.026(3) Uani 1 1 d . . . C19 C -0.4213(8) 0.1635(14) 1.0645(9) 0.034(3) Uani 1 1 d . . . H19A H -0.4397 0.2352 1.0715 0.041 Uiso 1 1 calc R . . C20 C -0.4425(10) 0.0814(15) 1.1110(10) 0.047(4) Uani 1 1 d . . . H20A H -0.4727 0.0965 1.1534 0.057 Uiso 1 1 calc R . . C21 C -0.4201(10) -0.0266(14) 1.0971(10) 0.046(4) Uani 1 1 d . . . H21A H -0.4382 -0.0838 1.1281 0.055 Uiso 1 1 calc R . . C22 C -0.3732(11) -0.0503(13) 1.0404(10) 0.042(4) Uani 1 1 d . . . H22A H -0.3582 -0.1234 1.0325 0.050 Uiso 1 1 calc R . . C23 C -0.3466(10) 0.0344(12) 0.9929(9) 0.036(4) Uani 1 1 d . . . C24 C -0.2950(10) 0.0143(12) 0.9364(9) 0.037(4) Uani 1 1 d . . . H24A H -0.2792 -0.0582 0.9274 0.045 Uiso 1 1 calc R . . C25 C -0.2670(10) 0.0971(11) 0.8940(8) 0.032(3) Uani 1 1 d . . . H25A H -0.2302 0.0830 0.8577 0.038 Uiso 1 1 calc R . . C26 C -0.2935(8) 0.2031(10) 0.9046(7) 0.022(3) Uani 1 1 d . . . C27 C -0.2679(8) 0.2986(10) 0.7785(8) 0.021(3) Uani 1 1 d . . . C28 C -0.2440(8) 0.4080(10) 0.7505(8) 0.021(3) Uani 1 1 d . . . C29 C -0.2124(8) 0.4136(10) 0.6779(7) 0.021(3) Uani 1 1 d . . . H29A H -0.2087 0.3507 0.6450 0.025 Uiso 1 1 calc R . . C30 C -0.1861(8) 0.5157(10) 0.6547(7) 0.022(3) Uani 1 1 d . . . H30A H -0.1601 0.5193 0.6079 0.026 Uiso 1 1 calc R . . C31 C -0.2283(9) 0.6002(11) 0.7648(8) 0.029(3) Uani 1 1 d . . . H31A H -0.2343 0.6647 0.7952 0.035 Uiso 1 1 calc R . . C32 C -0.2529(9) 0.5029(11) 0.7931(9) 0.031(3) Uani 1 1 d . . . H32A H -0.2760 0.5009 0.8419 0.037 Uiso 1 1 calc R . . O3 O -0.030(3) 0.487(4) 1.478(3) 0.134(17) Uiso 0.50 1 d P B -1 H3Z H -0.0683 0.4902 1.4348 0.202 Uiso 0.50 1 calc PR B -1 C33 C 0.018(5) 0.402(6) 1.472(5) 0.13(2) Uiso 0.50 1 d P B -1 H33A H 0.0669 0.4272 1.4519 0.197 Uiso 0.50 1 calc PR B -1 H33B H -0.0117 0.3493 1.4321 0.197 Uiso 0.50 1 calc PR B -1 H33C H 0.0358 0.3684 1.5275 0.197 Uiso 0.50 1 calc PR B -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hg1 0.0287(3) 0.0257(3) 0.0219(3) 0.0030(2) 0.0045(2) 0.0038(2) Br1 0.053(4) 0.067(5) 0.027(2) -0.007(3) 0.016(3) -0.007(3) Br1A 0.080(16) 0.066(6) 0.022(4) 0.001(3) 0.017(10) 0.017(10) Br2 0.0364(8) 0.0235(7) 0.0388(8) -0.0003(6) 0.0143(6) 0.0056(6) Hg2 0.0585(7) 0.0489(6) 0.0417(5) 0.0007(4) 0.0079(4) -0.0067(5) Br3 0.0540(11) 0.0549(11) 0.0466(10) -0.0052(8) 0.0101(8) -0.0047(9) O1 0.026(5) 0.038(5) 0.014(4) 0.006(4) 0.004(4) -0.005(4) O2 0.033(5) 0.018(5) 0.023(5) -0.006(4) 0.004(4) -0.004(4) N1 0.015(5) 0.025(6) 0.022(5) 0.003(4) -0.003(4) 0.004(4) N2 0.028(6) 0.022(5) 0.012(5) 0.004(4) 0.004(4) 0.002(5) N3 0.040(7) 0.015(5) 0.017(5) -0.003(4) 0.006(5) -0.007(5) N4 0.030(6) 0.015(5) 0.021(5) 0.000(4) 0.003(5) -0.008(4) C1 0.028(8) 0.033(7) 0.023(7) -0.002(6) 0.005(6) 0.010(6) C2 0.025(7) 0.041(8) 0.018(6) -0.005(6) 0.006(5) 0.001(6) C3 0.013(6) 0.019(6) 0.026(6) -0.001(5) -0.002(5) -0.003(5) C4 0.027(7) 0.023(6) 0.020(6) 0.003(5) 0.009(5) 0.001(5) C5 0.030(8) 0.033(7) 0.018(6) 0.001(5) 0.006(5) 0.010(6) C6 0.017(6) 0.018(6) 0.015(6) 0.001(5) -0.001(5) 0.002(5) C7 0.021(7) 0.030(7) 0.016(6) 0.005(5) 0.000(5) -0.002(5) C8 0.049(9) 0.015(6) 0.020(6) -0.003(5) 0.009(6) 0.000(6) C9 0.029(8) 0.027(7) 0.036(8) 0.011(6) 0.008(6) 0.013(6) C10 0.026(7) 0.040(8) 0.026(7) 0.008(6) 0.011(6) 0.005(6) C11 0.034(9) 0.050(9) 0.032(8) 0.012(7) 0.010(7) 0.012(7) C12 0.023(8) 0.077(13) 0.038(9) 0.016(9) 0.001(7) 0.001(8) C13 0.033(9) 0.060(11) 0.032(8) 0.011(8) -0.011(7) -0.006(8) C14 0.027(8) 0.051(9) 0.027(7) 0.001(7) 0.002(6) -0.007(7) C15 0.021(7) 0.035(7) 0.019(6) 0.005(5) 0.004(5) 0.000(6) C16 0.019(7) 0.028(7) 0.025(7) 0.008(6) 0.005(5) -0.004(5) C17 0.024(7) 0.027(7) 0.016(6) 0.005(5) -0.008(5) -0.001(6) C18 0.027(7) 0.025(7) 0.022(6) 0.005(5) -0.003(5) -0.010(6) C19 0.020(7) 0.052(9) 0.030(7) 0.003(7) 0.003(6) -0.015(7) C20 0.036(9) 0.067(12) 0.032(8) 0.018(8) -0.006(7) -0.018(8) C21 0.044(10) 0.046(10) 0.041(9) 0.018(8) -0.007(8) -0.027(8) C22 0.050(10) 0.030(8) 0.036(8) 0.011(7) -0.013(7) -0.018(7) C23 0.041(9) 0.030(8) 0.029(7) 0.004(6) -0.011(6) -0.018(7) C24 0.056(10) 0.027(7) 0.024(7) -0.005(6) -0.006(7) 0.006(7) C25 0.047(9) 0.026(7) 0.021(6) -0.004(6) 0.001(6) -0.011(6) C26 0.034(8) 0.018(6) 0.011(6) -0.006(5) 0.000(5) -0.005(5) C27 0.024(7) 0.022(6) 0.017(6) 0.000(5) 0.006(5) 0.008(5) C28 0.020(7) 0.023(6) 0.019(6) -0.002(5) -0.001(5) -0.010(5) C29 0.022(7) 0.025(7) 0.014(6) 0.001(5) 0.002(5) 0.004(5) C30 0.028(7) 0.022(6) 0.017(6) 0.009(5) 0.008(5) -0.003(5) C31 0.039(8) 0.019(7) 0.028(7) 0.003(6) 0.006(6) -0.001(6) C32 0.040(9) 0.028(7) 0.027(7) -0.005(6) 0.013(6) 0.003(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Hg1 Br1A 122.5(6) . . ? N1 Hg1 N4 84.9(4) . 3_567 ? Br1A Hg1 N4 104.1(9) . 3_567 ? N1 Hg1 Br1 113.0(3) . . ? Br1A Hg1 Br1 9.4(7) . . ? N4 Hg1 Br1 104.3(4) 3_567 . ? N1 Hg1 Br2 98.5(3) . . ? Br1A Hg1 Br2 135.4(6) . . ? N4 Hg1 Br2 95.6(3) 3_567 . ? Br1 Hg1 Br2 143.8(3) . . ? Br3 Hg2 Br3 180.0 . 3_567 ? C1 N1 C5 118.5(11) . . ? C1 N1 Hg1 119.4(9) . . ? C5 N1 Hg1 121.9(8) . . ? C6 N2 C7 120.2(10) . . ? C27 N3 C26 125.1(10) . . ? C30 N4 C31 117.9(10) . . ? C30 N4 Hg1 122.0(8) . 3_567 ? C31 N4 Hg1 119.9(8) . 3_567 ? N1 C1 C2 124.2(13) . . ? C1 C2 C3 116.7(12) . . ? C4 C3 C2 118.8(12) . . ? C4 C3 C6 124.8(12) . . ? C2 C3 C6 116.1(11) . . ? C3 C4 C5 119.6(12) . . ? N1 C5 C4 122.2(12) . . ? O1 C6 N2 123.6(11) . . ? O1 C6 C3 121.9(11) . . ? N2 C6 C3 114.5(10) . . ? C16 C7 C8 122.0(12) . . ? C16 C7 N2 120.2(12) . . ? C8 C7 N2 117.7(11) . . ? C9 C8 C7 119.0(13) . . ? C8 C9 C10 121.9(13) . . ? C9 C10 C15 118.5(12) . . ? C9 C10 C11 122.2(14) . . ? C15 C10 C11 119.2(14) . . ? C12 C11 C10 120.9(16) . . ? C11 C12 C13 120.6(15) . . ? C14 C13 C12 119.6(15) . . ? C13 C14 C15 121.9(16) . . ? C14 C15 C16 122.0(13) . . ? C14 C15 C10 117.8(13) . . ? C16 C15 C10 120.2(13) . . ? C7 C16 C15 118.3(12) . . ? C7 C16 C17 121.2(11) . . ? C15 C16 C17 120.3(12) . . ? C26 C17 C18 118.9(12) . . ? C26 C17 C16 118.6(11) . . ? C18 C17 C16 122.4(12) . . ? C19 C18 C23 119.6(13) . . ? C19 C18 C17 122.1(13) . . ? C23 C18 C17 118.3(13) . . ? C20 C19 C18 120.3(17) . . ? C19 C20 C21 120.3(17) . . ? C22 C21 C20 121.4(14) . . ? C21 C22 C23 119.9(16) . . ? C24 C23 C22 121.8(15) . . ? C24 C23 C18 119.7(13) . . ? C22 C23 C18 118.5(15) . . ? C25 C24 C23 121.1(14) . . ? C24 C25 C26 119.1(14) . . ? C17 C26 C25 122.8(12) . . ? C17 C26 N3 117.5(11) . . ? C25 C26 N3 119.6(12) . . ? O2 C27 N3 124.1(12) . . ? O2 C27 C28 122.6(11) . . ? N3 C27 C28 113.2(10) . . ? C32 C28 C29 118.8(12) . . ? C32 C28 C27 123.0(11) . . ? C29 C28 C27 118.2(11) . . ? C28 C29 C30 117.7(11) . . ? N4 C30 C29 123.4(11) . . ? N4 C31 C32 122.0(12) . . ? C31 C32 C28 120.0(13) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg1 N1 2.381(10) . ? Hg1 Br1A 2.44(3) . ? Hg1 N4 2.445(10) 3_567 ? Hg1 Br1 2.484(14) . ? Hg1 Br2 2.5067(15) . ? Hg2 Br3 2.3871(18) . ? Hg2 Br3 2.3871(18) 3_567 ? O1 C6 1.218(14) . ? O2 C27 1.233(15) . ? N1 C1 1.310(17) . ? N1 C5 1.338(17) . ? N2 C6 1.344(16) . ? N2 C7 1.442(16) . ? N3 C27 1.338(16) . ? N3 C26 1.447(16) . ? N4 C30 1.327(16) . ? N4 C31 1.359(17) . ? N4 Hg1 2.445(10) 3_567 ? C1 C2 1.383(19) . ? C2 C3 1.427(18) . ? C3 C4 1.354(18) . ? C3 C6 1.509(16) . ? C4 C5 1.387(18) . ? C7 C16 1.370(18) . ? C7 C8 1.431(18) . ? C8 C9 1.353(19) . ? C9 C10 1.41(2) . ? C10 C15 1.43(2) . ? C10 C11 1.44(2) . ? C11 C12 1.35(2) . ? C12 C13 1.42(3) . ? C13 C14 1.38(2) . ? C14 C15 1.42(2) . ? C15 C16 1.422(18) . ? C16 C17 1.491(19) . ? C17 C26 1.37(2) . ? C17 C18 1.433(18) . ? C18 C19 1.41(2) . ? C18 C23 1.43(2) . ? C19 C20 1.35(2) . ? C20 C21 1.41(3) . ? C21 C22 1.36(3) . ? C22 C23 1.42(2) . ? C23 C24 1.40(2) . ? C24 C25 1.36(2) . ? C25 C26 1.401(19) . ? C27 C28 1.503(17) . ? C28 C32 1.381(18) . ? C28 C29 1.387(17) . ? C29 C30 1.408(17) . ? C31 C32 1.377(19) . ? O3 C33 1.34(8) . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3A O1 0.88 2.03 2.843(14) 153.1 . N2 H2A O2 0.88 1.95 2.822(13) 169.0 4_566
1100733.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $ #$Revision: 176435 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100733.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100733 loop_ _publ_author_name 'Tara J. Burchell' 'Richard J. Puddephatt' _publ_section_title ; Self-Assembly of Chiral Coordination Polymers and Macrocycles: A Metal Template Effect on the Polymer-Macrocycle Equilibrium ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3718 _journal_page_last 3730 _journal_paper_doi 10.1021/ic050097w _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C34 H30 Hg1.5 I3 N4 O4' _chemical_formula_weight 1240.20 _chemical_name_systematic ; ? ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 103.28(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 34.840(7) _cell_length_b 13.241(3) _cell_length_c 16.423(3) _cell_measurement_temperature 150(2) _cell_measurement_theta_max 27.48 _cell_measurement_theta_min 1.70 _cell_volume 7374(3) _computing_cell_refinement 'Nonius DENZO' _computing_data_collection 'Nonius COLLECT' _computing_data_reduction 'Nonius DENZO' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'phi\omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0107 _diffrn_reflns_av_sigmaI/netI 0.0693 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 36959 _diffrn_reflns_theta_full 25.03 _diffrn_reflns_theta_max 25.03 _diffrn_reflns_theta_min 2.55 _exptl_absorpt_coefficient_mu 8.799 _exptl_absorpt_correction_T_max 0.4182 _exptl_absorpt_correction_T_min 0.1777 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.234 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 4584 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.12 _refine_diff_density_max 6.482 _refine_diff_density_min -8.406 _refine_diff_density_rms 0.510 _refine_ls_extinction_coef 0.00042(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 406 _refine_ls_number_reflns 6522 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.015 _refine_ls_R_factor_all 0.1247 _refine_ls_R_factor_gt 0.0957 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1987P)^2^+508.2304P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2766 _refine_ls_wR_factor_ref 0.3016 _reflns_number_gt 4660 _reflns_number_total 6522 _reflns_threshold_expression I>2sigma(I) _cod_data_source_file ic050097wsi20050217_082525_10.cif _cod_data_source_block 6c _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_formula_sum 'C34 H30 Hg1.50 I3 N4 O4' _cod_database_code 1100733 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hg1 Hg 0.67090(2) 1.01529(6) 0.76464(5) 0.0268(3) Uani 1 1 d . . . I2 I 0.66983(5) 0.98704(12) 0.92250(9) 0.0456(5) Uani 1 1 d . . . I1 I 0.64274(5) 1.13855(11) 0.63700(9) 0.0405(5) Uani 1 1 d . . . Hg2 Hg 0.2500 0.2500 0.5000 0.0836(7) Uani 1 2 d S . . I3 I 0.26101(7) 0.31661(19) 0.36126(16) 0.0715(7) Uani 0.90 1 d P A 1 I3A I 0.2854(9) 0.389(2) 0.4206(19) 0.098(8) Uiso 0.10 1 d P A 2 N1 N 0.6511(5) 0.8500(12) 0.7029(10) 0.030(4) Uani 1 1 d . . . N2 N 0.6190(4) 0.5505(12) 0.5090(9) 0.023(3) Uani 1 1 d . . . H2A H 0.6267 0.6035 0.4845 0.027 Uiso 1 1 calc R . . N3 N 0.6290(5) 0.6151(11) 0.2948(9) 0.023(3) Uani 1 1 d . . . H3A H 0.6270 0.5864 0.2457 0.028 Uiso 1 1 calc R . . N4 N 0.7670(5) 0.5286(14) 0.2686(11) 0.032(4) Uani 1 1 d . . . O1 O 0.6159(4) 0.4855(10) 0.6366(9) 0.032(3) Uani 1 1 d . . . O2 O 0.6691(4) 0.6548(11) 0.4199(8) 0.032(3) Uani 1 1 d . . . C1 C 0.6555(6) 0.7654(15) 0.7484(12) 0.029(4) Uani 1 1 d . . . H1A H 0.6658 0.7705 0.8071 0.035 Uiso 1 1 calc R . . C2 C 0.6457(6) 0.6697(17) 0.7136(12) 0.032(5) Uani 1 1 d . . . H2B H 0.6489 0.6117 0.7486 0.039 Uiso 1 1 calc R . . C3 C 0.6313(5) 0.6594(14) 0.6282(11) 0.020(4) Uani 1 1 d . . . C4 C 0.6268(6) 0.7479(16) 0.5803(12) 0.032(5) Uani 1 1 d . . . H4B H 0.6170 0.7443 0.5214 0.038 Uiso 1 1 calc R . . C5 C 0.6362(8) 0.8379(16) 0.6171(13) 0.041(6) Uani 1 1 d . . . H5A H 0.6326 0.8965 0.5828 0.049 Uiso 1 1 calc R . . C6 C 0.6215(5) 0.5577(14) 0.5920(12) 0.024(4) Uani 1 1 d . . . C7 C 0.6055(5) 0.4678(14) 0.4580(11) 0.020(4) Uani 1 1 d . . . C8 C 0.6159(5) 0.3647(15) 0.4844(11) 0.024(4) Uani 1 1 d . . . H8A H 0.6313 0.3509 0.5390 0.029 Uiso 1 1 calc R . . C9 C 0.6032(6) 0.2872(15) 0.4286(13) 0.031(5) Uani 1 1 d . . . H9A H 0.6103 0.2200 0.4459 0.037 Uiso 1 1 calc R . . C10 C 0.5806(6) 0.3024(15) 0.3493(14) 0.033(5) Uani 1 1 d . . . C11 C 0.5683(7) 0.2210(16) 0.2935(15) 0.039(6) Uani 1 1 d . . . H11A H 0.5753 0.1540 0.3116 0.047 Uiso 1 1 calc R . . C12 C 0.5473(7) 0.2364(19) 0.2170(16) 0.049(7) Uani 1 1 d . . . H12A H 0.5383 0.1805 0.1816 0.059 Uiso 1 1 calc R . . C13 C 0.5380(6) 0.339(2) 0.1863(16) 0.045(6) Uani 1 1 d . . . H13A H 0.5245 0.3498 0.1298 0.055 Uiso 1 1 calc R . . C14 C 0.5486(5) 0.4184(17) 0.2396(12) 0.031(5) Uani 1 1 d . . . H14A H 0.5408 0.4850 0.2214 0.037 Uiso 1 1 calc R . . C15 C 0.5711(6) 0.4022(15) 0.3210(12) 0.028(4) Uiso 1 1 d . . . C16 C 0.5830(6) 0.4864(14) 0.3780(12) 0.023(4) Uani 1 1 d . . . C17 C 0.5713(5) 0.5934(15) 0.3560(11) 0.023(4) Uani 1 1 d . . . C18 C 0.5373(5) 0.6337(15) 0.3767(10) 0.023(4) Uani 1 1 d . . . C19 C 0.5119(6) 0.5764(16) 0.4099(13) 0.030(4) Uani 1 1 d . . . H19A H 0.5177 0.5069 0.4205 0.036 Uiso 1 1 calc R . . C20 C 0.4775(7) 0.616(2) 0.4287(15) 0.047(6) Uani 1 1 d . . . H20A H 0.4601 0.5741 0.4505 0.056 Uiso 1 1 calc R . . C21 C 0.4701(9) 0.716(3) 0.415(2) 0.078(10) Uani 1 1 d . . . H21A H 0.4473 0.7444 0.4280 0.093 Uiso 1 1 calc R . . C22 C 0.4945(10) 0.776(2) 0.382(2) 0.077(10) Uani 1 1 d . . . H22A H 0.4881 0.8454 0.3723 0.092 Uiso 1 1 calc R . . C23 C 0.5287(9) 0.738(2) 0.3622(16) 0.053(7) Uani 1 1 d . . . C24 C 0.5544(9) 0.801(2) 0.328(2) 0.074(11) Uani 1 1 d . . . H24A H 0.5491 0.8711 0.3198 0.089 Uiso 1 1 calc R . . C25 C 0.5867(8) 0.759(2) 0.3086(18) 0.055(7) Uani 1 1 d . . . H25A H 0.6044 0.8004 0.2876 0.066 Uiso 1 1 calc R . . C26 C 0.5948(6) 0.6528(15) 0.3187(13) 0.030(4) Uani 1 1 d . . . C27 C 0.6641(5) 0.6241(14) 0.3482(12) 0.024(4) Uani 1 1 d . . . C28 C 0.6989(6) 0.5847(15) 0.3162(11) 0.025(4) Uani 1 1 d . . . C29 C 0.7299(7) 0.5409(19) 0.3739(14) 0.039(5) Uani 1 1 d . . . H29A H 0.7287 0.5293 0.4303 0.047 Uiso 1 1 calc R . . C30 C 0.7622(7) 0.5155(17) 0.3441(14) 0.039(5) Uani 1 1 d . . . H30A H 0.7835 0.4849 0.3829 0.047 Uiso 1 1 calc R . . C31 C 0.7368(6) 0.5713(16) 0.2114(12) 0.029(4) Uani 1 1 d . . . H31A H 0.7391 0.5806 0.1554 0.035 Uiso 1 1 calc R . . C32 C 0.7033(6) 0.6008(16) 0.2347(12) 0.031(4) Uani 1 1 d . . . H32A H 0.6828 0.6326 0.1950 0.037 Uiso 1 1 calc R . . O4 O 0.7144(4) 0.3154(10) 0.4810(8) 0.027(3) Uiso 1 1 d D B -1 H40 H 0.7173 0.3119 0.5331 0.032 Uiso 1 1 calc R B -1 C71 C 0.7452(13) 0.268(4) 0.459(3) 0.16(2) Uiso 1 1 d D B -1 H71A H 0.7497 0.2981 0.4072 0.187 Uiso 1 1 calc R B -1 H71B H 0.7389 0.1958 0.4488 0.187 Uiso 1 1 calc R B -1 H71C H 0.7690 0.2746 0.5035 0.187 Uiso 1 1 calc R B -1 O3 O 0.5269(11) 0.0466(18) 0.4404(19) 0.127(12) Uani 1 1 d . . . H60 H 0.5035 0.0672 0.4281 0.152 Uiso 1 1 calc R . . C60 C 0.534(3) -0.019(6) 0.527(5) 0.22(4) Uiso 1 1 d . . . H60A H 0.5569 0.0088 0.5673 0.260 Uiso 1 1 calc R . . H60B H 0.5397 -0.0895 0.5148 0.260 Uiso 1 1 calc R . . H60C H 0.5108 -0.0158 0.5497 0.260 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hg1 0.0343(5) 0.0273(5) 0.0209(5) 0.0005(3) 0.0109(3) 0.0034(3) I2 0.0645(11) 0.0545(10) 0.0203(8) -0.0003(6) 0.0147(7) -0.0078(7) I1 0.0630(10) 0.0342(8) 0.0269(8) 0.0055(6) 0.0157(7) 0.0196(7) Hg2 0.0946(15) 0.0780(13) 0.0842(14) -0.0013(10) 0.0331(12) -0.0009(11) I3 0.0687(15) 0.0713(15) 0.0763(16) 0.0028(12) 0.0205(12) -0.0035(11) N1 0.049(11) 0.019(8) 0.025(9) -0.001(7) 0.015(8) 0.001(7) N2 0.029(8) 0.019(8) 0.018(8) 0.004(6) 0.001(6) -0.004(6) N3 0.035(9) 0.024(8) 0.014(8) 0.005(6) 0.014(7) 0.007(7) N4 0.015(8) 0.055(12) 0.028(10) -0.005(8) 0.005(7) 0.003(7) O1 0.046(9) 0.030(8) 0.019(7) 0.008(6) 0.008(6) -0.002(6) O2 0.036(8) 0.042(9) 0.016(7) -0.006(6) 0.007(6) -0.001(6) C1 0.029(10) 0.035(11) 0.019(10) 0.003(8) -0.003(8) 0.001(9) C2 0.047(12) 0.043(12) 0.011(9) 0.001(8) 0.015(9) -0.008(10) C3 0.008(8) 0.033(10) 0.019(9) 0.003(7) -0.001(7) -0.001(7) C4 0.049(13) 0.034(11) 0.010(9) 0.008(8) 0.004(9) 0.007(9) C5 0.076(17) 0.023(11) 0.022(11) 0.004(9) 0.005(11) 0.003(10) C6 0.023(9) 0.019(9) 0.031(11) 0.006(8) 0.008(8) 0.003(7) C7 0.019(9) 0.032(10) 0.012(9) -0.005(7) 0.010(7) -0.002(7) C8 0.021(9) 0.038(11) 0.012(9) 0.005(8) 0.003(7) 0.000(8) C9 0.041(12) 0.022(10) 0.031(12) -0.001(8) 0.013(9) 0.000(9) C10 0.030(11) 0.027(11) 0.046(13) 0.002(9) 0.018(10) -0.010(8) C11 0.057(14) 0.019(11) 0.054(15) -0.026(10) 0.038(12) -0.021(10) C12 0.054(15) 0.048(15) 0.048(16) -0.033(12) 0.018(12) -0.015(12) C13 0.018(10) 0.063(17) 0.050(15) -0.018(12) -0.003(10) -0.002(10) C14 0.023(10) 0.050(13) 0.019(10) -0.001(9) 0.004(8) 0.006(9) C16 0.026(10) 0.029(10) 0.017(10) -0.003(7) 0.008(8) -0.002(8) C17 0.020(9) 0.032(10) 0.017(9) 0.002(8) 0.003(7) 0.004(8) C18 0.013(8) 0.051(12) 0.006(8) -0.001(8) 0.002(6) 0.008(8) C19 0.022(10) 0.036(12) 0.034(12) -0.002(9) 0.007(8) -0.012(8) C20 0.043(14) 0.059(17) 0.040(14) 0.003(12) 0.012(11) 0.010(12) C21 0.040(16) 0.11(3) 0.09(2) -0.01(2) 0.021(15) 0.021(17) C22 0.09(2) 0.060(19) 0.11(3) 0.026(18) 0.08(2) 0.027(17) C23 0.072(18) 0.050(15) 0.043(15) 0.009(12) 0.023(13) 0.021(13) C24 0.08(2) 0.038(14) 0.14(3) 0.037(17) 0.09(2) 0.023(13) C25 0.064(17) 0.048(15) 0.070(18) 0.024(13) 0.053(15) 0.003(12) C26 0.034(11) 0.028(11) 0.029(11) 0.002(8) 0.008(9) 0.012(9) C27 0.020(9) 0.017(9) 0.033(12) 0.004(8) 0.003(8) 0.012(7) C28 0.033(11) 0.031(10) 0.014(9) -0.001(8) 0.015(8) -0.003(8) C29 0.045(13) 0.055(14) 0.025(11) -0.004(10) 0.019(10) 0.000(11) C30 0.046(13) 0.048(14) 0.025(12) 0.005(10) 0.015(10) 0.003(10) C31 0.026(10) 0.045(13) 0.019(10) -0.009(9) 0.011(8) -0.005(9) C32 0.037(11) 0.037(12) 0.015(10) 0.001(8) 0.000(8) -0.004(9) O3 0.20(3) 0.034(12) 0.12(2) -0.009(14) -0.01(2) -0.002(16) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Hg1 N1 82.7(6) 7_666 . ? N4 Hg1 I2 113.8(4) 7_666 . ? N1 Hg1 I2 102.4(4) . . ? N4 Hg1 I1 99.0(4) 7_666 . ? N1 Hg1 I1 101.8(4) . . ? I2 Hg1 I1 141.13(6) . . ? I3 Hg2 I3 180.000(1) 7_556 . ? I3 Hg2 I3A 32.6(6) 7_556 7_556 ? I3 Hg2 I3A 147.4(6) . 7_556 ? I3 Hg2 I3A 147.4(6) 7_556 . ? I3 Hg2 I3A 32.6(6) . . ? I3A Hg2 I3A 180.0(10) 7_556 . ? C1 N1 C5 116.0(17) . . ? C1 N1 Hg1 122.2(13) . . ? C5 N1 Hg1 121.7(13) . . ? C6 N2 C7 126.7(16) . . ? C27 N3 C26 118.9(16) . . ? C30 N4 C31 117.7(18) . . ? C30 N4 Hg1 120.0(14) . 7_666 ? C31 N4 Hg1 122.2(13) . 7_666 ? N1 C1 C2 122.9(18) . . ? C3 C2 C1 120.1(19) . . ? C2 C3 C4 117.0(18) . . ? C2 C3 C6 119.6(17) . . ? C4 C3 C6 123.4(16) . . ? C5 C4 C3 120.4(18) . . ? C4 C5 N1 123.5(19) . . ? O1 C6 N2 123.9(18) . . ? O1 C6 C3 121.0(18) . . ? N2 C6 C3 115.1(16) . . ? C16 C7 N2 117.9(17) . . ? C16 C7 C8 119.8(16) . . ? N2 C7 C8 122.2(16) . . ? C9 C8 C7 118.7(17) . . ? C10 C9 C8 123.3(19) . . ? C9 C10 C15 119.2(19) . . ? C9 C10 C11 122(2) . . ? C15 C10 C11 119(2) . . ? C12 C11 C10 121(2) . . ? C11 C12 C13 120(2) . . ? C14 C13 C12 119(2) . . ? C13 C14 C15 120(2) . . ? C14 C15 C10 119.6(19) . . ? C14 C15 C16 120.7(18) . . ? C10 C15 C16 119.7(18) . . ? C7 C16 C15 119.3(17) . . ? C7 C16 C17 117.4(16) . . ? C15 C16 C17 123.3(17) . . ? C26 C17 C18 120.6(18) . . ? C26 C17 C16 119.5(16) . . ? C18 C17 C16 119.9(17) . . ? C19 C18 C17 122.8(19) . . ? C19 C18 C23 118.2(19) . . ? C17 C18 C23 119.0(19) . . ? C18 C19 C20 123(2) . . ? C21 C20 C19 118(3) . . ? C20 C21 C22 122(3) . . ? C21 C22 C23 122(3) . . ? C22 C23 C18 118(2) . . ? C22 C23 C24 122(2) . . ? C18 C23 C24 120(2) . . ? C25 C24 C23 119(2) . . ? C24 C25 C26 122(2) . . ? C17 C26 N3 122.8(17) . . ? C17 C26 C25 119.3(18) . . ? N3 C26 C25 117.7(18) . . ? O2 C27 N3 124.8(17) . . ? O2 C27 C28 119.8(16) . . ? N3 C27 C28 115.2(16) . . ? C29 C28 C32 118.5(18) . . ? C29 C28 C27 117.7(16) . . ? C32 C28 C27 123.4(18) . . ? C30 C29 C28 115.7(19) . . ? N4 C30 C29 127(2) . . ? N4 C31 C32 120.0(18) . . ? C31 C32 C28 120.9(19) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg1 N4 2.421(16) 7_666 ? Hg1 N1 2.445(16) . ? Hg1 I2 2.6281(17) . ? Hg1 I1 2.6602(16) . ? Hg2 I3 2.553(3) 7_556 ? Hg2 I3 2.553(3) . ? Hg2 I3A 2.71(3) 7_556 ? Hg2 I3A 2.71(3) . ? N1 C1 1.34(3) . ? N1 C5 1.39(3) . ? N2 C6 1.35(2) . ? N2 C7 1.39(2) . ? N3 C27 1.34(2) . ? N3 C26 1.43(2) . ? N4 C30 1.30(3) . ? N4 C31 1.36(3) . ? N4 Hg1 2.421(16) 7_666 ? O1 C6 1.25(2) . ? O2 C27 1.22(2) . ? C1 C2 1.40(3) . ? C2 C3 1.38(3) . ? C3 C4 1.40(3) . ? C3 C6 1.48(3) . ? C4 C5 1.34(3) . ? C7 C16 1.39(3) . ? C7 C8 1.45(3) . ? C8 C9 1.38(3) . ? C9 C10 1.37(3) . ? C10 C15 1.41(3) . ? C10 C11 1.42(3) . ? C11 C12 1.32(4) . ? C12 C13 1.45(4) . ? C13 C14 1.37(3) . ? C14 C15 1.40(3) . ? C15 C16 1.45(3) . ? C16 C17 1.50(3) . ? C17 C26 1.38(3) . ? C17 C18 1.41(2) . ? C18 C19 1.37(3) . ? C18 C23 1.42(3) . ? C19 C20 1.40(3) . ? C20 C21 1.36(5) . ? C21 C22 1.36(4) . ? C22 C23 1.40(4) . ? C23 C24 1.43(4) . ? C24 C25 1.36(3) . ? C25 C26 1.43(3) . ? C27 C28 1.52(2) . ? C28 C29 1.39(3) . ? C28 C32 1.40(3) . ? C29 C30 1.37(3) . ? C31 C32 1.37(3) . ? O4 C71 1.37(2) . ? O3 C60 1.63(8) . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3A O1 0.88 1.99 2.86(2) 172.7 6_565 N2 H2A O2 0.88 2.12 2.88(2) 143.5 .
1100734.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100734.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100734 loop_ _publ_author_name 'Tara J. Burchell' 'Richard J. Puddephatt' _publ_section_title ; Self-Assembly of Chiral Coordination Polymers and Macrocycles: A Metal Template Effect on the Polymer-Macrocycle Equilibrium ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3718 _journal_page_last 3730 _journal_paper_doi 10.1021/ic050097w _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C65 H46.33 Cl2 Hg2.17 I4.33 N8 O4.17' _chemical_formula_weight 2061.51 _chemical_name_systematic ; ? ; _space_group_IT_number 148 _symmetry_cell_setting rhombohedral _symmetry_space_group_name_Hall '-R 3' _symmetry_space_group_name_H-M 'R -3 :H' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_formula_units_Z 18 _cell_length_a 26.836(4) _cell_length_b 26.836(4) _cell_length_c 53.305(11) _cell_measurement_temperature 150(2) _cell_measurement_theta_max 25.03 _cell_measurement_theta_min 1.70 _cell_volume 33246(10) _computing_cell_refinement 'Nonius DENZO' _computing_data_collection 'Nonius COLLECT' _computing_data_reduction 'Nonius DENZO' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'phi\omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.072 _diffrn_reflns_av_sigmaI/netI 0.0653 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_l_max 58 _diffrn_reflns_limit_l_min -63 _diffrn_reflns_number 13042 _diffrn_reflns_theta_full 25.02 _diffrn_reflns_theta_max 25.02 _diffrn_reflns_theta_min 2.59 _exptl_absorpt_coefficient_mu 6.426 _exptl_absorpt_correction_T_max 0.6274 _exptl_absorpt_correction_T_min 0.5127 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.853 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 17328 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _refine_diff_density_max 3.612 _refine_diff_density_min -3.180 _refine_diff_density_rms 0.251 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 402 _refine_ls_number_reflns 13025 _refine_ls_number_restraints 279 _refine_ls_restrained_S_all 1.005 _refine_ls_R_factor_all 0.1482 _refine_ls_R_factor_gt 0.0954 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1333P)^2^+1880.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2451 _refine_ls_wR_factor_ref 0.2819 _reflns_number_gt 8097 _reflns_number_total 13025 _reflns_threshold_expression I>2sigma(I) _cod_data_source_file ic050097wsi20050217_082525_11.cif _cod_data_source_block 7c _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Rhombohedral' changed to 'rhombohedral' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_cell_volume 33245(9) _cod_original_sg_symbol_H-M 'R -3' _cod_database_code 1100734 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hg1 Hg -0.94460(5) -0.14236(5) -0.37590(3) 0.0868(4) Uani 1 1 d . . . I1 I -0.94789(8) -0.04875(8) -0.36525(3) 0.0729(5) Uani 1 1 d . A . I2 I -0.98753(15) -0.25254(12) -0.36602(7) 0.0867(9) Uani 0.70 1 d P A 1 I2A I -0.9888(4) -0.2538(4) -0.3822(2) 0.107(3) Uiso 0.30 1 d P A 2 Hg2 Hg -0.62317(5) -0.13545(5) -0.21885(3) 0.0805(4) Uani 1 1 d . . . I3 I -0.62342(7) -0.22797(7) -0.20126(3) 0.0715(5) Uani 1 1 d . . . I4 I -0.66692(11) -0.06655(10) -0.21814(5) 0.1076(8) Uani 1 1 d . . . Hg3 Hg -0.6667 -0.3333 -0.3333 0.169(2) Uani 1 6 d S . . I5 I -0.6667 -0.3333 -0.38164(13) 0.146(2) Uani 1 3 d S . . N1 N -0.8410(6) -0.1043(7) -0.3803(3) 0.086(7) Uani 1 1 d G A . C1 C -0.8198(8) -0.1396(6) -0.3726(4) 0.088(9) Uiso 1 1 d G . . H1A H -0.8456 -0.1788 -0.3685 0.106 Uiso 1 1 calc R A . C2 C -0.7608(9) -0.1176(8) -0.3707(4) 0.167(19) Uiso 1 1 d G A . H2A H -0.7462 -0.1417 -0.3654 0.200 Uiso 1 1 calc R . . C3 C -0.7230(6) -0.0603(9) -0.3766(4) 0.081(8) Uiso 1 1 d G . . C4 C -0.7442(7) -0.0250(6) -0.3843(3) 0.077(7) Uiso 1 1 d G A . H4A H -0.7183 0.0142 -0.3884 0.093 Uiso 1 1 calc R . . C5 C -0.8032(7) -0.0470(6) -0.3862(3) 0.073(7) Uiso 1 1 d G . . H5A H -0.8177 -0.0229 -0.3915 0.087 Uiso 1 1 calc R A . C6 C -0.6599(11) -0.0424(11) -0.3713(5) 0.065(6) Uiso 1 1 d . A . O1 O -0.6456(9) -0.0566(9) -0.3520(4) 0.094(6) Uani 1 1 d . . . N2 N -0.6196(9) -0.0035(10) -0.3857(5) 0.085(7) Uani 1 1 d . . . H2B H -0.6292 0.0069 -0.3997 0.102 Uiso 1 1 calc R A . C7 C -0.5618(11) 0.0213(9) -0.3791(4) 0.070(7) Uiso 1 1 d D A . C8 C -0.5349(11) 0.0757(10) -0.3678(4) 0.089(9) Uiso 1 1 d D . . H8A H -0.5560 0.0953 -0.3661 0.106 Uiso 1 1 calc R A . C9 C -0.4788(11) 0.1020(14) -0.3589(5) 0.115(12) Uiso 1 1 d D A . H9A H -0.4623 0.1383 -0.3507 0.138 Uiso 1 1 calc R . . C10 C -0.4468(11) 0.0739(10) -0.3624(5) 0.077(7) Uiso 1 1 d D . . C11 C -0.3921(13) 0.1023(17) -0.3515(6) 0.131(14) Uiso 1 1 d D A . H11A H -0.3759 0.1385 -0.3433 0.157 Uiso 1 1 calc R . . C12 C -0.3643(17) 0.0703(15) -0.3544(7) 0.123(13) Uiso 1 1 d D . . H12A H -0.3264 0.0863 -0.3478 0.147 Uiso 1 1 calc R A . C13 C -0.3877(15) 0.0167(15) -0.3660(7) 0.131(14) Uiso 1 1 d D A . H13A H -0.3656 -0.0017 -0.3681 0.157 Uiso 1 1 calc R . . C14 C -0.4444(14) -0.0090(16) -0.3743(6) 0.111(11) Uiso 1 1 d D . . H14A H -0.4623 -0.0474 -0.3804 0.133 Uiso 1 1 calc R A . C15 C -0.4760(10) 0.0196(10) -0.3741(5) 0.086(8) Uiso 1 1 d D A . C16 C -0.5337(10) -0.0105(10) -0.3827(5) 0.088(9) Uiso 1 1 d D . . C17 C -0.5561(8) -0.0623(8) -0.3966(3) 0.063(6) Uiso 1 1 d D A . C18 C -0.5556(6) -0.0620(8) -0.4230(3) 0.076(7) Uiso 1 1 d D . . C19 C -0.5363(10) -0.0126(11) -0.4379(4) 0.084(8) Uiso 1 1 d D A . H19A H -0.5210 0.0229 -0.4291 0.101 Uiso 1 1 calc R . . C20 C -0.5368(13) -0.0090(12) -0.4640(4) 0.097(10) Uiso 1 1 d D . . H20A H -0.5255 0.0257 -0.4729 0.117 Uiso 1 1 calc R A . C21 C -0.5557(12) -0.0623(10) -0.4755(5) 0.090(9) Uiso 1 1 d D A . H21A H -0.5540 -0.0628 -0.4932 0.107 Uiso 1 1 calc R . . C22 C -0.5770(12) -0.1147(11) -0.4631(4) 0.082(8) Uiso 1 1 d D . . H22A H -0.5925 -0.1501 -0.4719 0.098 Uiso 1 1 calc R A . C23 C -0.5742(9) -0.1124(8) -0.4368(3) 0.060(6) Uiso 1 1 d D A . C24 C -0.5942(11) -0.1636(10) -0.4237(4) 0.080(8) Uiso 1 1 d D . . H24A H -0.6067 -0.1982 -0.4330 0.097 Uiso 1 1 calc R A . C25 C -0.5966(11) -0.1664(10) -0.3978(4) 0.076(7) Uiso 1 1 d D A . H25A H -0.6108 -0.2021 -0.3892 0.092 Uiso 1 1 calc R . . C26 C -0.5774(9) -0.1151(7) -0.3846(4) 0.054(5) Uiso 1 1 d D . . N3 N -0.5803(11) -0.1148(10) -0.3580(4) 0.080(7) Uani 1 1 d . A . H3A H -0.5824 -0.0855 -0.3518 0.096 Uiso 1 1 calc R . . C27 C -0.5803(14) -0.1484(14) -0.3418(5) 0.086(8) Uiso 1 1 d . . . O2 O -0.5768(11) -0.1943(11) -0.3478(4) 0.112(8) Uani 1 1 d . A . C31 C -0.5798(8) -0.1782(7) -0.2982(3) 0.092(9) Uiso 1 1 d G . . H4B H -0.5664 -0.2027 -0.3042 0.110 Uiso 1 1 calc R A . C28 C -0.5905(7) -0.1449(7) -0.31489(19) 0.064(6) Uiso 1 1 d G A . C29 C -0.6101(7) -0.1090(6) -0.3061(2) 0.057(6) Uiso 1 1 d G A . H29A H -0.6175 -0.0863 -0.3175 0.069 Uiso 1 1 calc R . . C30 C -0.6190(7) -0.1064(6) -0.2806(2) 0.064(6) Uiso 1 1 d G A . H30A H -0.6325 -0.0819 -0.2745 0.077 Uiso 1 1 calc R . . N4 N -0.6083(6) -0.1396(6) -0.26382(18) 0.067(6) Uani 1 1 d G A . C32 C -0.5887(7) -0.1755(6) -0.2726(2) 0.061(6) Uiso 1 1 d G A . H32A H -0.5814 -0.1983 -0.2612 0.073 Uiso 1 1 calc R . . N5 N -0.5163(5) -0.0688(6) -0.2190(3) 0.068(6) Uani 1 1 d G . . C33 C -0.4830(7) -0.0936(5) -0.2250(3) 0.104(10) Uiso 1 1 d G . . H33A H -0.5011 -0.1333 -0.2291 0.125 Uiso 1 1 calc R . . C34 C -0.4234(7) -0.0602(8) -0.2250(4) 0.085(8) Uiso 1 1 d G . . H34A H -0.4007 -0.0772 -0.2290 0.102 Uiso 1 1 calc R . . C35 C -0.3969(5) -0.0021(7) -0.2190(3) 0.079(8) Uiso 1 1 d G . . C36 C -0.4302(6) 0.0227(5) -0.2130(3) 0.062(6) Uiso 1 1 d G . . H36A H -0.4121 0.0624 -0.2089 0.074 Uiso 1 1 calc R . . C37 C -0.4898(6) -0.0107(6) -0.2130(3) 0.080(8) Uiso 1 1 d G . . H37A H -0.5126 0.0063 -0.2089 0.096 Uiso 1 1 calc R . . C38 C -0.3311(13) 0.0282(13) -0.2190(5) 0.077(7) Uiso 1 1 d . . . O3 O -0.3056(8) 0.0067(8) -0.2330(4) 0.086(6) Uani 1 1 d . . . N6 N -0.3080(10) 0.0694(8) -0.2039(4) 0.078(7) Uani 1 1 d . . . H6A H -0.3285 0.0825 -0.1966 0.094 Uiso 1 1 calc R . . C39 C -0.2469(12) 0.0951(10) -0.1987(4) 0.081(8) Uiso 1 1 d D . . C40 C -0.2272(11) 0.0616(12) -0.1860(4) 0.086(8) Uiso 1 1 d D . . H40A H -0.2534 0.0220 -0.1831 0.103 Uiso 1 1 calc R . . C41 C -0.1696(10) 0.0857(11) -0.1775(4) 0.088(8) Uiso 1 1 d D . . H41A H -0.1576 0.0631 -0.1685 0.105 Uiso 1 1 calc R . . C42 C -0.1301(11) 0.1448(11) -0.1830(5) 0.112(11) Uiso 1 1 d D . . C43 C -0.0719(10) 0.1694(11) -0.1744(5) 0.080(8) Uiso 1 1 d D . . H43A H -0.0588 0.1458 -0.1669 0.096 Uiso 1 1 calc R . . C44 C -0.0338(14) 0.2295(11) -0.1773(6) 0.104(10) Uiso 1 1 d D . . H44A H 0.0047 0.2469 -0.1714 0.125 Uiso 1 1 calc R . . C45 C -0.0544(13) 0.2631(17) -0.1893(7) 0.135(14) Uiso 1 1 d D . . H45A H -0.0295 0.3033 -0.1915 0.162 Uiso 1 1 calc R . . C46 C -0.1125(11) 0.2368(10) -0.1981(5) 0.081(8) Uiso 1 1 d D . . H46A H -0.1262 0.2605 -0.2049 0.097 Uiso 1 1 calc R . . C47 C -0.1509(10) 0.1758(9) -0.1969(5) 0.082(8) Uiso 1 1 d D . . C48 C -0.2090(10) 0.1536(11) -0.2056(5) 0.107(11) Uiso 1 1 d D . . C49 C -0.2265(10) 0.1851(10) -0.2204(4) 0.088(9) Uiso 1 1 d D . . C50 C -0.2240(7) 0.1854(8) -0.2464(4) 0.077(7) Uiso 1 1 d D . . C51 C -0.2059(11) 0.1533(12) -0.2596(5) 0.102(10) Uiso 1 1 d D . . H51A H -0.1927 0.1315 -0.2506 0.123 Uiso 1 1 calc R . . C52 C -0.2060(12) 0.1517(12) -0.2853(5) 0.089(9) Uiso 1 1 d D . . H52A H -0.1985 0.1243 -0.2931 0.107 Uiso 1 1 calc R . . C53 C -0.2165(13) 0.1872(12) -0.3007(6) 0.105(11) Uiso 1 1 d D . . H53A H -0.2092 0.1912 -0.3183 0.126 Uiso 1 1 calc R . . C54 C -0.2384(12) 0.2157(12) -0.2876(4) 0.084(8) Uiso 1 1 d D . . H54A H -0.2538 0.2352 -0.2968 0.100 Uiso 1 1 calc R . . C55 C -0.2396(12) 0.2177(11) -0.2616(4) 0.082(8) Uiso 1 1 d D . . C56 C -0.2560(11) 0.2524(11) -0.2494(4) 0.070(6) Uiso 1 1 d D . . H56A H -0.2638 0.2775 -0.2592 0.084 Uiso 1 1 calc R . . C57 C -0.2618(13) 0.2525(13) -0.2238(4) 0.091(8) Uiso 1 1 d D . . H57A H -0.2769 0.2740 -0.2160 0.109 Uiso 1 1 calc R . . C58 C -0.2448(12) 0.2201(11) -0.2097(5) 0.085(8) Uiso 1 1 d D . . N7 N -0.2452(9) 0.2278(11) -0.1821(5) 0.102(9) Uani 1 1 d . . . H7A H -0.2171 0.2587 -0.1751 0.122 Uiso 1 1 calc R . . C59 C -0.2886(13) 0.1876(13) -0.1676(5) 0.080(8) Uiso 1 1 d . . . O4 O -0.3326(8) 0.1448(9) -0.1768(4) 0.099(7) Uani 1 1 d . . . C63 C -0.2587(8) 0.2449(5) -0.1022(3) 0.080(7) Uiso 1 1 d G . . H63A H -0.2462 0.2805 -0.0938 0.096 Uiso 1 1 calc R . . N8 N -0.2730(7) 0.1956(7) -0.0884(2) 0.068(5) Uiso 1 1 d G . . C60 C -0.2913(8) 0.1435(6) -0.1006(3) 0.078(7) Uiso 1 1 d G . . H60A H -0.3011 0.1098 -0.0912 0.094 Uiso 1 1 calc R . . C61 C -0.2952(8) 0.1408(6) -0.1266(3) 0.073(7) Uiso 1 1 d G . . H61A H -0.3077 0.1052 -0.1350 0.088 Uiso 1 1 calc R . . C62 C -0.2809(8) 0.1902(8) -0.1404(2) 0.082(8) Uiso 1 1 d G . . C64 C -0.2626(8) 0.2422(6) -0.1282(3) 0.082(8) Uiso 1 1 d G . . H64A H -0.2528 0.2759 -0.1376 0.099 Uiso 1 1 calc R . . C100 C 0.112(3) 0.156(4) -0.2286(13) 0.14(3) Uiso 0.50 1 d PD B -1 H10A H 0.0980 0.1699 -0.2426 0.170 Uiso 0.50 1 calc PR B -1 H10B H 0.0887 0.1138 -0.2279 0.170 Uiso 0.50 1 calc PR B -1 Cl1 Cl 0.184(4) 0.176(5) -0.2341(18) 0.55(7) Uiso 0.50 1 d PD B -1 Cl2 Cl 0.106(3) 0.185(3) -0.2007(11) 0.34(3) Uiso 0.50 1 d PD B -1 C101 C 0.015(3) 0.227(4) -0.2446(18) 0.14(3) Uiso 0.50 1 d PD C 2 H10C H 0.0198 0.2434 -0.2275 0.170 Uiso 0.50 1 calc PR C 2 H10F H 0.0422 0.2606 -0.2551 0.170 Uiso 0.50 1 calc PR C 2 Cl4 Cl -0.052(3) 0.217(3) -0.2537(14) 0.39(4) Uiso 0.50 1 d PD C 2 Cl3 Cl 0.051(5) 0.188(5) -0.242(2) 0.54(6) Uiso 0.50 1 d PD C 2 O40 O -0.3333 0.3333 -0.1667 0.018(5) Uiso 1 6 d SD . . H400 H -0.3608 0.3400 -0.1667 0.021 Uiso 0.17 1 d PRD . . H401 H -0.3100 0.3689 -0.1667 0.021 Uiso 0.17 1 d PRD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hg1 0.0699(7) 0.0651(7) 0.1392(11) -0.0096(7) -0.0087(7) 0.0440(6) I1 0.0641(10) 0.0658(10) 0.1035(12) -0.0110(9) -0.0097(9) 0.0435(9) I2 0.118(3) 0.0565(15) 0.090(2) -0.0048(14) -0.0119(18) 0.0469(16) Hg2 0.0777(7) 0.0493(6) 0.1105(9) 0.0031(6) 0.0080(6) 0.0288(5) I3 0.0656(10) 0.0459(8) 0.0917(12) 0.0028(8) -0.0068(9) 0.0193(8) I4 0.1115(18) 0.0789(14) 0.149(2) -0.0053(13) 0.0067(15) 0.0603(13) Hg3 0.117(2) 0.117(2) 0.273(7) 0.000 0.000 0.0586(11) I5 0.0937(19) 0.0937(19) 0.252(7) 0.000 0.000 0.0469(9) N1 0.082(15) 0.052(12) 0.14(2) 0.000(13) 0.025(14) 0.044(12) O1 0.098(15) 0.113(16) 0.115(15) 0.016(12) 0.017(12) 0.086(14) N2 0.051(13) 0.069(14) 0.098(17) 0.006(12) 0.011(12) 0.003(11) N3 0.120(19) 0.071(14) 0.077(14) 0.024(11) 0.031(13) 0.068(15) O2 0.13(2) 0.110(17) 0.137(18) 0.013(15) 0.002(15) 0.095(16) N4 0.044(11) 0.067(13) 0.060(12) 0.006(10) -0.007(9) 0.004(9) N5 0.057(12) 0.036(10) 0.088(14) -0.001(10) -0.003(10) 0.007(9) O3 0.068(11) 0.066(11) 0.115(15) -0.027(10) -0.013(11) 0.028(10) N6 0.083(16) 0.036(10) 0.101(16) -0.001(11) -0.030(13) 0.019(10) N7 0.043(12) 0.081(16) 0.14(2) 0.030(16) -0.030(13) -0.001(11) O4 0.060(11) 0.092(14) 0.103(15) -0.022(12) 0.007(11) 0.006(10) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N8 Hg1 N1 82(4) 7_444 . ? N8 Hg1 I1 101(5) 7_444 . ? N1 Hg1 I1 101.3(4) . . ? N8 Hg1 I2A 85(5) 7_444 . ? N1 Hg1 I2A 103.6(4) . . ? I1 Hg1 I2A 154.9(2) . . ? N8 Hg1 I2 104(5) 7_444 . ? N1 Hg1 I2 104.8(4) . . ? I1 Hg1 I2 145.83(11) . . ? I2A Hg1 I2 18.9(2) . . ? N4 Hg2 N5 82.8(5) . . ? N4 Hg2 I4 100.7(4) . . ? N5 Hg2 I4 104.6(4) . . ? N4 Hg2 I3 103.2(4) . . ? N5 Hg2 I3 97.8(4) . . ? I4 Hg2 I3 148.99(9) . . ? I5 Hg3 I5 180.0 . 13_344 ? C1 N1 C5 120.0 . . ? C1 N1 Hg1 117.0(9) . . ? C5 N1 Hg1 122.1(8) . . ? C2 C1 N1 120.0 . . ? C1 C2 C3 120.0 . . ? C2 C3 C4 120.0 . . ? C2 C3 C6 112.6(16) . . ? C4 C3 C6 127.2(16) . . ? C5 C4 C3 120.0 . . ? C4 C5 N1 120.0 . . ? O1 C6 N2 119(3) . . ? O1 C6 C3 122(2) . . ? N2 C6 C3 119(2) . . ? C6 N2 C7 121(2) . . ? N2 C7 C8 119(2) . . ? N2 C7 C16 119(2) . . ? C8 C7 C16 123(2) . . ? C9 C8 C7 123(3) . . ? C8 C9 C10 119(3) . . ? C11 C10 C9 114(2) . . ? C11 C10 C15 130(3) . . ? C9 C10 C15 116(2) . . ? C10 C11 C12 111(3) . . ? C13 C12 C11 125(4) . . ? C12 C13 C14 118(4) . . ? C13 C14 C15 123(3) . . ? C14 C15 C10 113(2) . . ? C14 C15 C16 118(2) . . ? C10 C15 C16 128(2) . . ? C7 C16 C15 112(2) . . ? C7 C16 C17 125.1(19) . . ? C15 C16 C17 122.2(19) . . ? C26 C17 C18 117.8(17) . . ? C26 C17 C16 120.9(18) . . ? C18 C17 C16 121.3(18) . . ? C23 C18 C19 113.6(19) . . ? C23 C18 C17 121.6(17) . . ? C19 C18 C17 124.7(18) . . ? C20 C19 C18 128(3) . . ? C19 C20 C21 112(3) . . ? C22 C21 C20 126(3) . . ? C21 C22 C23 116(2) . . ? C24 C23 C18 117.9(18) . . ? C24 C23 C22 118.2(18) . . ? C18 C23 C22 123.8(19) . . ? C25 C24 C23 123(2) . . ? C24 C25 C26 118(2) . . ? C17 C26 C25 122.4(19) . . ? C17 C26 N3 116.8(17) . . ? C25 C26 N3 120.8(17) . . ? C27 N3 C26 132(2) . . ? N3 C27 O2 122(3) . . ? N3 C27 C28 124(3) . . ? O2 C27 C28 114(3) . . ? C28 C31 C32 120.0 . . ? C29 C28 C31 120.0 . . ? C29 C28 C27 121.4(16) . . ? C31 C28 C27 118.6(16) . . ? C28 C29 C30 120.0 . . ? C29 C30 N4 120.0 . . ? C32 N4 C30 120.0 . . ? C32 N4 Hg2 119.4(7) . . ? C30 N4 Hg2 120.6(7) . . ? N4 C32 C31 120.0 . . ? C33 N5 C37 120.0 . . ? C33 N5 Hg2 116.0(8) . . ? C37 N5 Hg2 124.0(8) . . ? N5 C33 C34 120.0 . . ? C33 C34 C35 120.0 . . ? C36 C35 C34 120.0 . . ? C36 C35 C38 126.3(16) . . ? C34 C35 C38 113.7(16) . . ? C37 C36 C35 120.0 . . ? C36 C37 N5 120.0 . . ? N6 C38 O3 128(3) . . ? N6 C38 C35 114(3) . . ? O3 C38 C35 119(2) . . ? C38 N6 C39 119(3) . . ? C40 C39 C48 122(2) . . ? C40 C39 N6 119(2) . . ? C48 C39 N6 119(2) . . ? C41 C40 C39 122(3) . . ? C40 C41 C42 118(2) . . ? C47 C42 C41 118(2) . . ? C47 C42 C43 124(2) . . ? C41 C42 C43 119(2) . . ? C44 C43 C42 119(3) . . ? C43 C44 C45 119(3) . . ? C44 C45 C46 120(3) . . ? C45 C46 C47 122(3) . . ? C42 C47 C46 115(2) . . ? C42 C47 C48 126(2) . . ? C46 C47 C48 118(2) . . ? C49 C48 C39 123(2) . . ? C49 C48 C47 124(2) . . ? C39 C48 C47 114(2) . . ? C58 C49 C50 116(2) . . ? C58 C49 C48 121(2) . . ? C50 C49 C48 123(2) . . ? C51 C50 C49 123(2) . . ? C51 C50 C55 114(2) . . ? C49 C50 C55 124(2) . . ? C52 C51 C50 122(3) . . ? C51 C52 C53 125(3) . . ? C54 C53 C52 112(3) . . ? C53 C54 C55 124(3) . . ? C56 C55 C54 121(2) . . ? C56 C55 C50 117(2) . . ? C54 C55 C50 122(2) . . ? C55 C56 C57 123(2) . . ? C56 C57 C58 118(3) . . ? C49 C58 C57 123(3) . . ? C49 C58 N7 122(2) . . ? C57 C58 N7 115(2) . . ? C59 N7 C58 121(2) . . ? O4 C59 N7 122(3) . . ? O4 C59 C62 118(2) . . ? N7 C59 C62 119(3) . . ? N8 C63 C64 120.0 . . ? C60 N8 C63 120.0 . . ? C60 N8 Hg1 115.7(8) . 4 ? C63 N8 Hg1 124.0(8) . 4 ? N8 C60 C61 120.0 . . ? C62 C61 C60 120.0 . . ? C64 C62 C61 120.0 . . ? C64 C62 C59 118.8(16) . . ? C61 C62 C59 121.0(16) . . ? C62 C64 C63 120.0 . . ? Cl2 C100 Cl1 110.9(18) . . ? Cl4 C101 Cl3 138(8) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg1 N8 2.44(17) 7_444 ? Hg1 N1 2.447(13) . ? Hg1 I1 2.6196(19) . ? Hg1 I2A 2.631(10) . ? Hg1 I2 2.635(3) . ? Hg2 N4 2.442(10) . ? Hg2 N5 2.509(11) . ? Hg2 I4 2.640(2) . ? Hg2 I3 2.651(2) . ? Hg3 I5 2.575(7) . ? Hg3 I5 2.575(7) 13_344 ? N1 C1 1.3900 . ? N1 C5 1.3900 . ? C1 C2 1.3900 . ? C2 C3 1.3900 . ? C3 C4 1.3900 . ? C3 C6 1.54(3) . ? C4 C5 1.3900 . ? C6 O1 1.22(3) . ? C6 N2 1.31(3) . ? N2 C7 1.39(3) . ? C7 C8 1.399(15) . ? C7 C16 1.404(15) . ? C8 C9 1.389(16) . ? C9 C10 1.409(16) . ? C10 C11 1.396(16) . ? C10 C15 1.411(15) . ? C11 C12 1.400(16) . ? C12 C13 1.392(16) . ? C13 C14 1.393(16) . ? C14 C15 1.399(16) . ? C15 C16 1.418(15) . ? C16 C17 1.419(14) . ? C17 C26 1.390(14) . ? C17 C18 1.404(14) . ? C18 C23 1.395(14) . ? C18 C19 1.403(14) . ? C19 C20 1.394(15) . ? C20 C21 1.397(15) . ? C21 C22 1.392(15) . ? C22 C23 1.401(14) . ? C23 C24 1.389(14) . ? C24 C25 1.387(14) . ? C25 C26 1.396(14) . ? C26 N3 1.42(3) . ? N3 C27 1.25(3) . ? C27 O2 1.32(4) . ? C27 C28 1.47(3) . ? C31 C28 1.3900 . ? C31 C32 1.3900 . ? C28 C29 1.3900 . ? C29 C30 1.3900 . ? C30 N4 1.3900 . ? N4 C32 1.3900 . ? N5 C33 1.3900 . ? N5 C37 1.3900 . ? C33 C34 1.3900 . ? C34 C35 1.3900 . ? C35 C36 1.3900 . ? C35 C38 1.53(3) . ? C36 C37 1.3900 . ? C38 N6 1.25(3) . ? C38 O3 1.32(3) . ? N6 C39 1.45(3) . ? C39 C40 1.420(15) . ? C39 C48 1.426(15) . ? C40 C41 1.419(15) . ? C41 C42 1.428(15) . ? C42 C47 1.420(14) . ? C42 C43 1.433(15) . ? C43 C44 1.421(15) . ? C44 C45 1.424(16) . ? C45 C46 1.430(15) . ? C46 C47 1.435(15) . ? C47 C48 1.440(15) . ? C48 C49 1.400(15) . ? C49 C58 1.381(14) . ? C49 C50 1.389(14) . ? C50 C51 1.378(15) . ? C50 C55 1.393(14) . ? C51 C52 1.368(15) . ? C52 C53 1.390(15) . ? C53 C54 1.368(15) . ? C54 C55 1.391(14) . ? C55 C56 1.375(14) . ? C56 C57 1.375(14) . ? C57 C58 1.388(15) . ? C58 N7 1.48(4) . ? N7 C59 1.37(4) . ? C59 O4 1.27(3) . ? C59 C62 1.46(3) . ? C63 N8 1.3900 . ? C63 C64 1.3900 . ? N8 C60 1.3900 . ? N8 Hg1 2.445(11) 4 ? C60 C61 1.3900 . ? C61 C62 1.3900 . ? C62 C64 1.3900 . ? C100 Cl2 1.731(16) . ? C100 Cl1 1.736(16) . ? C101 Cl4 1.744(16) . ? C101 Cl3 1.746(16) . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2B O3 0.88 2.01 2.88(3) 173.6 15_454 N3 H3A O1 0.88 2.19 2.89(3) 136.2 . N6 H6A O4 0.88 2.03 2.82(3) 150.0 . N7 H7A O4 0.88 2.22 3.10(3) 177.0 18_554
1100735.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $ #$Revision: 176435 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100735.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100735 loop_ _publ_author_name 'Cheng Zhang' 'Robertha C. Howell' 'Qun-Hui Luo' 'Heidi L. Fieselmann' 'Louis J. Todaro' 'Lynn C. Francesconi' _publ_section_title ; Influence of Steric and Electronic Properties of the Defect Site, Lanthanide Ionic Radii, and Solution Conditions on the Composition of Lanthanide(III) \a1-P2W17O6110-Polyoxometalates ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3569 _journal_page_last 3578 _journal_paper_doi 10.1021/ic050103o _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'Cl3 Eu H82 K5 O155.5 P4 W34' _chemical_formula_weight 9399.25 _chemical_name_systematic ; ? ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 88.82(3) _cell_angle_beta 82.32(3) _cell_angle_gamma 69.61(3) _cell_formula_units_Z 2 _cell_length_a 16.432(3) _cell_length_b 21.204(4) _cell_length_c 25.860(5) _cell_measurement_temperature 100(2) _cell_volume 8367(3) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1603 _diffrn_reflns_av_sigmaI/netI 0.1544 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_number 117898 _diffrn_reflns_theta_full 27.49 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_theta_min 2.91 _exptl_absorpt_coefficient_mu 23.947 _exptl_absorpt_correction_T_max 0.5859 _exptl_absorpt_correction_T_min 0.0524 _exptl_absorpt_process_details 'Numerical absorption correction from indexed crystal faces' _exptl_crystal_density_diffrn 3.731 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8222 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.03 _refine_diff_density_max 25.827 _refine_diff_density_min -17.214 _refine_diff_density_rms 0.871 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 1047 _refine_ls_number_reflns 38252 _refine_ls_number_restraints 3 _refine_ls_restrained_S_all 1.053 _refine_ls_R_factor_all 0.1786 _refine_ls_R_factor_gt 0.1125 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1109P)^2^+2265.5039P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2761 _refine_ls_wR_factor_ref 0.3158 _reflns_number_gt 23456 _reflns_number_total 38252 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic050103osi20050113_051617.cif _cod_data_source_block Europium_a1P2W17O61_1to2 _cod_original_formula_sum 'H82 Cl3 Eu K5 O155.50 P4 W34' _cod_database_code 1100735 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W2 W 1.60235(9) 0.42693(7) 0.08682(5) 0.0164(3) Uani 1 1 d . . . W3 W 1.63657(9) 0.30437(8) -0.02448(5) 0.0174(3) Uani 1 1 d . . . W4 W 1.79477(9) 0.15284(8) -0.02059(5) 0.0184(3) Uani 1 1 d . . . W5 W 1.92202(9) 0.11399(7) 0.09065(5) 0.0167(3) Uani 1 1 d . . . W6 W 1.87347(9) 0.23646(7) 0.18554(5) 0.0160(3) Uani 1 1 d . . . W7 W 1.80013(10) 0.38378(8) -0.01442(5) 0.0188(3) Uani 1 1 d . . . W8 W 1.96051(10) 0.23304(8) -0.00924(6) 0.0206(3) Uani 1 1 d . . . W9 W 1.91500(9) 0.35276(8) 0.08979(6) 0.0195(3) Uani 1 1 d . . . W11 W 1.54897(9) 0.33331(7) 0.25247(5) 0.0157(3) Uani 1 1 d . . . W12 W 1.42917(9) 0.36378(8) 0.15474(5) 0.0168(3) Uani 1 1 d . . . W13 W 1.47120(9) 0.23920(8) 0.04730(5) 0.0192(3) Uani 1 1 d . . . W14 W 1.62752(9) 0.08732(8) 0.05179(5) 0.0196(3) Uani 1 1 d . . . W15 W 1.75669(9) 0.04578(7) 0.16178(5) 0.0173(3) Uani 1 1 d . . . W16 W 1.71673(9) 0.16269(7) 0.25689(5) 0.0160(3) Uani 1 1 d . . . W17 W 1.36570(9) 0.21257(8) 0.17768(6) 0.0207(3) Uani 1 1 d . . . W18 W 1.52301(10) 0.06031(8) 0.18322(6) 0.0220(3) Uani 1 1 d . . . W19 W 1.48418(9) 0.17908(8) 0.27987(5) 0.0186(3) Uani 1 1 d . . . W22 W 1.80339(16) 0.58815(13) 0.19043(6) 0.0484(6) Uani 1 1 d D . . W23 W 1.8369(2) 0.70019(16) 0.27132(7) 0.0701(9) Uani 1 1 d D . . W24 W 1.78923(16) 0.68258(14) 0.41314(7) 0.0532(7) Uani 1 1 d . . . W25 W 1.69903(11) 0.56801(10) 0.45793(6) 0.0292(4) Uani 1 1 d . . . W26 W 1.66715(10) 0.45420(8) 0.35849(5) 0.0215(3) Uani 1 1 d . . . W27 W 1.93744(12) 0.44292(15) 0.25544(7) 0.0524(7) Uani 1 1 d . . . W28 W 1.97907(15) 0.55096(18) 0.33854(8) 0.0701(10) Uani 1 1 d . . . W29 W 1.88982(12) 0.43692(13) 0.38761(7) 0.0456(6) Uani 1 1 d . . . W31 W 1.49106(11) 0.58703(8) 0.23221(5) 0.0243(3) Uani 1 1 d . . . W32 W 1.5799(2) 0.71906(11) 0.18554(7) 0.0546(7) Uani 1 1 d . . . W33 W 1.6086(2) 0.82589(12) 0.26800(8) 0.0719(9) Uani 1 1 d . . . W34 W 1.5595(2) 0.80762(12) 0.40980(8) 0.0637(8) Uani 1 1 d . . . W35 W 1.47269(14) 0.69312(10) 0.45387(6) 0.0381(4) Uani 1 1 d . . . W36 W 1.43862(11) 0.57888(10) 0.36001(6) 0.0290(4) Uani 1 1 d . . . W37 W 1.34653(19) 0.76954(11) 0.24104(8) 0.0632(8) Uani 1 1 d . . . W38 W 1.3763(3) 0.87629(13) 0.32770(10) 0.0846(11) Uani 1 1 d . . . W39 W 1.29356(18) 0.75903(14) 0.37152(8) 0.0696(9) Uani 1 1 d . . . Eu Eu 1.71615(12) 0.43115(10) 0.20841(6) 0.0178(4) Uani 1 1 d . . . P1 P 1.7613(5) 0.2728(5) 0.0778(3) 0.0131(17) Uani 1 1 d . . . P2 P 1.5855(6) 0.2022(5) 0.1567(3) 0.0168(18) Uani 1 1 d . . . P3 P 1.7591(8) 0.5718(7) 0.3253(4) 0.036(3) Uani 1 1 d . . . P4 P 1.5166(10) 0.7068(6) 0.3178(4) 0.044(3) Uani 1 1 d . . . O2 O 1.5323(16) 0.4980(14) 0.0606(10) 0.023(5) Uiso 1 1 d . . . O3 O 1.5817(18) 0.3421(15) -0.0755(11) 0.032(6) Uiso 1 1 d . . . O4 O 1.8397(16) 0.0906(13) -0.0677(9) 0.020(5) Uiso 1 1 d . . . O5 O 2.0098(16) 0.0392(13) 0.0773(9) 0.020(5) Uiso 1 1 d . . . O6 O 1.9409(17) 0.2298(14) 0.2338(10) 0.026(6) Uiso 1 1 d . . . O7 O 1.7918(17) 0.4449(14) -0.0604(10) 0.027(6) Uiso 1 1 d . . . O8 O 2.0531(19) 0.1942(16) -0.0517(11) 0.035(7) Uiso 1 1 d . . . O9 O 1.9959(18) 0.3825(15) 0.1020(11) 0.032(6) Uiso 1 1 d . . . O11 O 1.5218(16) 0.3716(13) 0.3144(10) 0.022(5) Uiso 1 1 d . . . O12 O 1.3355(17) 0.4301(14) 0.1475(10) 0.025(6) Uiso 1 1 d . . . O13 O 1.3864(18) 0.2665(15) 0.0106(11) 0.029(6) Uiso 1 1 d . . . O14 O 1.6459(17) 0.0156(14) 0.0163(10) 0.025(6) Uiso 1 1 d . . . O15 O 1.8179(17) -0.0387(14) 0.1606(10) 0.027(6) Uiso 1 1 d . . . O16 O 1.7511(16) 0.1506(13) 0.3169(10) 0.022(5) Uiso 1 1 d . . . O17 O 1.2563(18) 0.2306(15) 0.1782(11) 0.030(6) Uiso 1 1 d . . . O18 O 1.513(2) -0.0169(16) 0.1846(12) 0.037(7) Uiso 1 1 d . . . O19 O 1.4490(16) 0.1719(13) 0.3446(9) 0.021(5) Uiso 1 1 d . . . O22 O 1.842(2) 0.585(2) 0.1246(14) 0.053(9) Uiso 1 1 d . . . O23 O 1.888(3) 0.757(2) 0.2592(15) 0.060(10) Uiso 1 1 d . . . O24 O 1.828(3) 0.732(2) 0.4457(17) 0.068(11) Uiso 1 1 d . . . O25 O 1.6876(19) 0.5417(15) 0.5205(11) 0.032(7) Uiso 1 1 d . . . O26 O 1.6386(17) 0.3966(15) 0.4013(10) 0.027(6) Uiso 1 1 d . . . O27 O 2.022(2) 0.386(2) 0.2165(15) 0.057(10) Uiso 1 1 d . . . O28 O 2.071(3) 0.564(2) 0.3494(15) 0.061(10) Uiso 1 1 d . . . O29 O 1.933(2) 0.3684(18) 0.4266(13) 0.045(8) Uiso 1 1 d . . . O31 O 1.4531(17) 0.5618(14) 0.1812(10) 0.024(6) Uiso 1 1 d . . . O32 O 1.575(2) 0.7280(19) 0.1190(14) 0.052(9) Uiso 1 1 d . . . O33 O 1.631(3) 0.897(3) 0.256(2) 0.089(15) Uiso 1 1 d . . . O34 O 1.562(3) 0.876(2) 0.4427(18) 0.078(13) Uiso 1 1 d . . . O35 O 1.422(2) 0.6847(16) 0.5141(12) 0.037(7) Uiso 1 1 d . . . O36 O 1.3766(18) 0.5365(15) 0.3918(11) 0.031(6) Uiso 1 1 d . . . O37 O 1.274(3) 0.791(2) 0.1946(16) 0.067(11) Uiso 1 1 d . . . O38 O 1.326(3) 0.959(3) 0.3359(19) 0.084(14) Uiso 1 1 d . . . O39 O 1.190(3) 0.767(3) 0.407(2) 0.088(15) Uiso 1 1 d . . . O2E O 1.6402(16) 0.4635(14) 0.1359(10) 0.023(6) Uiso 1 1 d . . . O6E O 1.7891(15) 0.3108(12) 0.2028(9) 0.015(5) Uiso 1 1 d . . . O9E O 1.8210(15) 0.4034(13) 0.1307(9) 0.018(5) Uiso 1 1 d . . . O11E O 1.6095(15) 0.3764(12) 0.2190(9) 0.015(5) Uiso 1 1 d . . . O22E O 1.7429(18) 0.5347(15) 0.1944(11) 0.030(6) Uiso 1 1 d . . . O26E O 1.6915(16) 0.4102(14) 0.2983(10) 0.022(5) Uiso 1 1 d . . . O27E O 1.8459(18) 0.4203(15) 0.2446(11) 0.032(6) Uiso 1 1 d . . . O31E O 1.5871(15) 0.5206(13) 0.2396(9) 0.018(5) Uiso 1 1 d . . . O2P O 1.6899(15) 0.3312(13) 0.1065(9) 0.018(5) Uiso 1 1 d . . . O3P O 1.7277(13) 0.2420(11) 0.0368(8) 0.007(4) Uiso 1 1 d . . . O5P O 1.8093(14) 0.2200(12) 0.1147(8) 0.013(5) Uiso 1 1 d . . . O7P O 1.8330(15) 0.2991(13) 0.0480(9) 0.019(5) Uiso 1 1 d . . . O11P O 1.5571(14) 0.2770(12) 0.1721(8) 0.014(5) Uiso 1 1 d . . . O13P O 1.5874(14) 0.1898(12) 0.0982(8) 0.012(4) Uiso 1 1 d . . . O15P O 1.6721(14) 0.1619(11) 0.1751(8) 0.011(4) Uiso 1 1 d . . . O17P O 1.5159(16) 0.1729(13) 0.1872(10) 0.022(5) Uiso 1 1 d . . . O22P O 1.764(2) 0.6165(17) 0.2793(12) 0.042(8) Uiso 1 1 d . . . O24P O 1.7297(17) 0.6140(14) 0.3779(10) 0.027(6) Uiso 1 1 d . . . O26P O 1.7007(15) 0.5327(13) 0.3184(9) 0.019(5) Uiso 1 1 d . . . O27P O 1.8531(18) 0.5235(15) 0.3270(10) 0.028(6) Uiso 1 1 d . . . O31P O 1.5130(18) 0.6369(15) 0.3091(11) 0.031(6) Uiso 1 1 d . . . O34P O 1.542(2) 0.7125(17) 0.3734(12) 0.042(8) Uiso 1 1 d . . . O37P O 1.419(2) 0.7593(18) 0.3169(13) 0.043(8) Uiso 1 1 d . . . O32P O 1.575(2) 0.7277(19) 0.2749(14) 0.049(9) Uiso 1 1 d . . . O113 O 1.4421(15) 0.3803(13) 0.2244(9) 0.017(5) Uiso 1 1 d . . . O116 O 1.6475(14) 0.2544(12) 0.2627(9) 0.014(5) Uiso 1 1 d . . . O119 O 1.4843(15) 0.2654(13) 0.2761(9) 0.017(5) Uiso 1 1 d . . . O123 O 1.4502(15) 0.3176(13) 0.0878(9) 0.018(5) Uiso 1 1 d . . . O128 O 1.3763(14) 0.2993(12) 0.1790(9) 0.015(5) Uiso 1 1 d . . . O134 O 1.5249(17) 0.1453(14) 0.0262(10) 0.025(6) Uiso 1 1 d . . . O137 O 1.4095(17) 0.2089(15) 0.1039(10) 0.027(6) Uiso 1 1 d . . . O145 O 1.7190(16) 0.0574(13) 0.0953(9) 0.021(5) Uiso 1 1 d . . . O148 O 1.5523(17) 0.0696(14) 0.1108(10) 0.024(6) Uiso 1 1 d . . . O157 O 1.7665(17) 0.0693(14) 0.2315(10) 0.027(6) Uiso 1 1 d . . . O158 O 1.6450(17) 0.0384(14) 0.1889(10) 0.026(6) Uiso 1 1 d . . . O169 O 1.6066(14) 0.1447(12) 0.2774(8) 0.012(4) Uiso 1 1 d . . . O178 O 1.4025(19) 0.1163(16) 0.1744(11) 0.034(7) Uiso 1 1 d . . . O179 O 1.3751(16) 0.2041(14) 0.2506(10) 0.023(5) Uiso 1 1 d . . . O189 O 1.4961(17) 0.0865(14) 0.2548(10) 0.024(6) Uiso 1 1 d . . . O212 O 1.5105(16) 0.4039(13) 0.1284(9) 0.021(5) Uiso 1 1 d . . . O222 O 1.6883(17) 0.6752(14) 0.1862(17) 0.069(11) Uiso 1 1 d D . . O223 O 1.853(2) 0.6624(17) 0.2062(12) 0.040(7) Uiso 1 1 d . . . O227 O 1.902(2) 0.5244(18) 0.2182(13) 0.043(8) Uiso 1 1 d . . . O230 O 1.5878(15) 0.3681(12) 0.0272(9) 0.016(5) Uiso 1 1 d . . . O233 O 1.7097(16) 0.773(2) 0.263(2) 0.089(15) Uiso 1 1 d D . . O234 O 1.791(2) 0.7163(18) 0.3455(13) 0.045(8) Uiso 1 1 d . . . O238 O 1.9284(18) 0.6267(14) 0.2940(15) 0.061(10) Uiso 1 1 d D . . O244 O 1.660(2) 0.7449(16) 0.4226(12) 0.037(7) Uiso 1 1 d . . . O245 O 1.749(2) 0.6384(18) 0.4694(13) 0.046(8) Uiso 1 1 d . . . O248 O 1.893(2) 0.6150(17) 0.3929(12) 0.038(7) Uiso 1 1 d . . . O255 O 1.5874(19) 0.6445(15) 0.4643(11) 0.032(7) Uiso 1 1 d . . . O256 O 1.6537(16) 0.5195(14) 0.4219(10) 0.023(5) Uiso 1 1 d . . . O259 O 1.815(2) 0.5049(17) 0.4362(12) 0.039(7) Uiso 1 1 d . . . O266 O 1.5493(14) 0.5103(12) 0.3546(8) 0.014(5) Uiso 1 1 d . . . O269 O 1.7904(18) 0.4224(15) 0.3718(10) 0.028(6) Uiso 1 1 d . . . O270 O 1.7031(16) 0.4258(13) 0.0347(9) 0.020(5) Uiso 1 1 d . . . O278 O 2.015(3) 0.493(2) 0.2843(17) 0.073(12) Uiso 1 1 d . . . O279 O 1.951(2) 0.3980(19) 0.3220(14) 0.050(9) Uiso 1 1 d . . . O289 O 1.975(3) 0.483(2) 0.3866(15) 0.060(10) Uiso 1 1 d . . . O312 O 1.551(2) 0.6410(16) 0.1969(12) 0.037(7) Uiso 1 1 d . . . O313 O 1.5618(17) 0.2553(14) 0.0025(10) 0.025(6) Uiso 1 1 d . . . O316 O 1.4194(18) 0.5668(15) 0.2902(11) 0.029(6) Uiso 1 1 d . . . O317 O 1.385(2) 0.6784(17) 0.2398(12) 0.041(8) Uiso 1 1 d . . . O323 O 1.593(2) 0.803(2) 0.1978(15) 0.056(10) Uiso 1 1 d . . . O327 O 1.448(2) 0.7704(17) 0.2054(12) 0.039(7) Uiso 1 1 d . . . O334 O 1.603(3) 0.822(2) 0.3422(15) 0.061(10) Uiso 1 1 d . . . O338 O 1.476(2) 0.868(2) 0.2849(14) 0.052(9) Uiso 1 1 d . . . O340 O 1.7146(16) 0.2194(13) -0.0575(9) 0.020(5) Uiso 1 1 d . . . O345 O 1.497(2) 0.7734(19) 0.4629(14) 0.052(9) Uiso 1 1 d . . . O348 O 1.449(3) 0.851(2) 0.3815(18) 0.078(13) Uiso 1 1 d . . . O356 O 1.467(2) 0.6174(17) 0.4175(12) 0.038(7) Uiso 1 1 d . . . O359 O 1.369(2) 0.7460(19) 0.4243(13) 0.048(8) Uiso 1 1 d . . . O369 O 1.342(2) 0.6646(19) 0.3613(14) 0.050(9) Uiso 1 1 d . . . O370 O 1.7335(16) 0.3380(14) -0.0399(10) 0.023(5) Uiso 1 1 d . . . O378 O 1.320(2) 0.8604(18) 0.2697(13) 0.046(8) Uiso 1 1 d . . . O379 O 1.259(2) 0.770(2) 0.3036(15) 0.057(10) Uiso 1 1 d . . . O389 O 1.286(3) 0.848(2) 0.3718(17) 0.073(12) Uiso 1 1 d . . . O414 O 1.6948(14) 0.1241(12) 0.0086(9) 0.015(5) Uiso 1 1 d . . . O450 O 1.8494(16) 0.1125(13) 0.0382(10) 0.022(5) Uiso 1 1 d . . . O480 O 1.8786(15) 0.1947(12) -0.0332(9) 0.016(5) Uiso 1 1 d . . . O515 O 1.8462(16) 0.0777(14) 0.1351(10) 0.023(5) Uiso 1 1 d . . . O560 O 1.9533(15) 0.1461(13) 0.1466(9) 0.017(5) Uiso 1 1 d . . . O580 O 1.9691(16) 0.1663(14) 0.0415(10) 0.022(5) Uiso 1 1 d . . . O616 O 1.8059(16) 0.1831(13) 0.2186(9) 0.021(5) Uiso 1 1 d . . . O690 O 1.9361(15) 0.2751(13) 0.1318(9) 0.017(5) Uiso 1 1 d . . . O780 O 1.9029(19) 0.3114(16) -0.0460(11) 0.033(7) Uiso 1 1 d . . . O790 O 1.8779(17) 0.4018(14) 0.0254(10) 0.024(6) Uiso 1 1 d . . . O890 O 1.9998(17) 0.2829(14) 0.0316(10) 0.026(6) Uiso 1 1 d . . . K1 K 1.3586(6) 0.5461(5) 0.1092(3) 0.0261(18) Uani 1 1 d . . . K2 K 1.2469(7) 0.4139(6) 0.0510(4) 0.043(2) Uani 1 1 d . . . K3 K 2.0099(6) 0.0884(6) -0.1090(4) 0.043(3) Uani 1 1 d . . . K4 K 1.5851(7) 0.5991(5) 0.0919(3) 0.033(2) Uani 1 1 d . . . K5 K 1.4701(8) 0.4017(6) 0.4167(3) 0.044(3) Uani 1 1 d . . . Cl1 Cl 0.6942(19) 0.2638(10) 0.3809(9) 0.136(12) Uani 1 1 d . . . Cl2 Cl 1.6656(12) -0.0006(7) 0.2978(6) 0.063(4) Uani 1 1 d . . . Cl3 Cl 1.7681(11) 0.5014(15) 0.6113(5) 0.113(10) Uani 1 1 d . . . O901 O 0.3998(13) 0.9122(11) 0.1815(7) 0.006(4) Uiso 1 1 d . . . O902 O 0.7819(13) -0.1057(11) 0.0324(8) 0.010(4) Uiso 1 1 d . . . O903 O 0.6677(14) 0.4096(11) 0.5021(8) 0.011(4) Uiso 1 1 d . . . O904 O 1.3985(18) 0.4394(15) 0.0238(11) 0.029(6) Uiso 1 1 d . . . O905 O 1.0819(15) 0.2653(13) 0.1847(9) 0.019(5) Uiso 1 1 d . . . O906 O 0.1872(17) 0.4198(14) 0.2249(10) 0.026(6) Uiso 1 1 d . . . O907 O 1.0550(18) 0.3144(15) -0.1169(11) 0.030(6) Uiso 1 1 d . . . O908 O 0.4104(19) 0.0669(16) 0.0576(11) 0.035(7) Uiso 1 1 d . . . O909 O 0.411(2) 0.8413(18) 0.0924(13) 0.045(8) Uiso 1 1 d . . . O910 O 2.1056(18) 0.0337(15) -0.0269(11) 0.032(6) Uiso 1 1 d . . . O911 O 1.759(2) 0.5482(17) 0.0540(12) 0.039(7) Uiso 1 1 d . . . O912 O 0.659(3) 0.890(2) 0.1230(16) 0.063(11) Uiso 1 1 d . . . O913 O 1.5000 0.5000 0.5000 0.042(11) Uiso 1 2 d S . . O914 O 1.022(2) 0.4163(18) -0.0391(13) 0.047(8) Uiso 1 1 d . . . O915 O 0.978(2) 0.372(2) 0.5315(14) 0.053(9) Uiso 1 1 d . . . O916 O 0.853(3) 0.281(2) 0.3348(16) 0.063(11) Uiso 1 1 d . . . O917 O 0.537(2) 0.8731(18) 0.1364(13) 0.046(8) Uiso 1 1 d . . . O918 O 1.211(3) 0.609(2) 0.1838(16) 0.062(10) Uiso 1 1 d . . . O919 O 1.346(3) 0.357(2) 0.3726(18) 0.077(13) Uiso 1 1 d . . . O920 O 0.526(3) 0.929(3) 0.0501(19) 0.081(13) Uiso 1 1 d . . . O921 O 0.173(3) 0.739(2) 0.1432(15) 0.059(10) Uiso 1 1 d . . . O922 O 0.775(3) 0.377(2) 0.7142(18) 0.076(13) Uiso 1 1 d . . . O923 O 0.357(4) 0.258(3) 0.453(2) 0.098(16) Uiso 1 1 d . . . O924 O 1.103(3) 0.222(3) 0.223(2) 0.087(14) Uiso 1 1 d . . . O925 O 0.427(3) 0.114(2) 0.4404(18) 0.075(12) Uiso 1 1 d . . . O926 O 0.862(3) -0.140(2) 0.2416(16) 0.062(10) Uiso 1 1 d . . . O927 O 1.149(4) 0.344(3) 0.010(2) 0.12(2) Uiso 1 1 d . . . O928 O 1.122(4) 0.187(3) 0.110(2) 0.102(17) Uiso 1 1 d . . . O929 O 0.061(4) 0.574(3) 0.183(2) 0.107(18) Uiso 1 1 d . . . O930 O 1.702(3) 0.512(3) 0.718(2) 0.090(15) Uiso 1 1 d . . . O931 O 1.055(4) 0.489(3) 0.107(2) 0.102(17) Uiso 1 1 d . . . O932 O 0.784(4) 0.077(4) -0.167(3) 0.13(2) Uiso 1 1 d . . . O933 O 1.535(4) 0.263(3) 0.389(3) 0.12(2) Uiso 1 1 d . . . O934 O 0.549(4) 0.151(4) 0.440(3) 0.12(2) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W2 0.0201(7) 0.0121(7) 0.0116(6) 0.0038(5) 0.0018(5) -0.0004(6) W3 0.0210(7) 0.0155(7) 0.0107(6) 0.0038(5) 0.0000(5) -0.0010(6) W4 0.0222(7) 0.0154(7) 0.0130(6) 0.0019(5) -0.0001(5) -0.0015(6) W5 0.0173(7) 0.0139(7) 0.0159(6) 0.0032(5) 0.0006(5) -0.0028(6) W6 0.0160(6) 0.0165(7) 0.0149(6) 0.0042(5) -0.0017(5) -0.0054(6) W7 0.0245(7) 0.0146(7) 0.0131(6) 0.0054(5) 0.0051(5) -0.0044(6) W8 0.0210(7) 0.0157(8) 0.0188(7) 0.0045(6) 0.0065(5) -0.0023(6) W9 0.0204(7) 0.0173(8) 0.0199(7) 0.0035(6) 0.0035(5) -0.0080(6) W11 0.0195(7) 0.0160(7) 0.0102(6) 0.0022(5) 0.0010(5) -0.0056(6) W12 0.0158(6) 0.0170(8) 0.0130(6) 0.0044(5) -0.0005(5) -0.0009(6) W13 0.0172(7) 0.0241(8) 0.0139(6) 0.0016(6) -0.0034(5) -0.0036(6) W14 0.0203(7) 0.0205(8) 0.0182(6) -0.0015(6) -0.0031(5) -0.0070(6) W15 0.0203(7) 0.0129(7) 0.0174(6) 0.0047(5) -0.0015(5) -0.0047(6) W16 0.0186(7) 0.0165(7) 0.0123(6) 0.0064(5) -0.0023(5) -0.0058(6) W17 0.0151(7) 0.0272(9) 0.0206(7) 0.0037(6) -0.0012(5) -0.0090(6) W18 0.0225(7) 0.0205(8) 0.0256(7) 0.0029(6) -0.0012(6) -0.0117(7) W19 0.0212(7) 0.0197(8) 0.0151(6) 0.0051(6) 0.0016(5) -0.0091(6) W22 0.0846(15) 0.0719(16) 0.0142(7) -0.0081(8) 0.0134(8) -0.0658(14) W23 0.126(2) 0.109(2) 0.0203(9) -0.0128(11) 0.0174(11) -0.105(2) W24 0.0840(16) 0.0872(18) 0.0179(8) -0.0148(9) 0.0128(9) -0.0731(15) W25 0.0376(9) 0.0472(11) 0.0124(6) -0.0048(7) 0.0040(6) -0.0289(9) W26 0.0292(8) 0.0276(9) 0.0120(6) 0.0030(6) -0.0024(5) -0.0155(7) W27 0.0302(9) 0.112(2) 0.0234(8) -0.0265(11) 0.0087(7) -0.0380(12) W28 0.0461(12) 0.156(3) 0.0314(10) -0.0350(14) 0.0121(9) -0.0685(16) W29 0.0274(9) 0.0854(17) 0.0233(8) -0.0153(9) -0.0051(7) -0.0174(10) W31 0.0355(9) 0.0175(8) 0.0122(6) 0.0019(6) 0.0021(6) -0.0015(7) W32 0.124(2) 0.0266(11) 0.0192(8) 0.0032(8) 0.0048(10) -0.0393(13) W33 0.164(3) 0.0369(13) 0.0311(10) 0.0006(9) -0.0006(14) -0.0601(17) W34 0.134(2) 0.0373(13) 0.0267(9) -0.0119(9) 0.0081(12) -0.0451(15) W35 0.0579(12) 0.0353(11) 0.0153(7) -0.0082(7) 0.0078(7) -0.0132(9) W36 0.0297(8) 0.0405(11) 0.0123(6) -0.0018(7) 0.0040(6) -0.0091(8) W37 0.0969(19) 0.0282(11) 0.0334(10) -0.0073(9) -0.0153(11) 0.0198(12) W38 0.150(3) 0.0265(13) 0.0498(14) -0.0152(11) -0.0188(16) 0.0059(16) W39 0.0732(16) 0.0663(18) 0.0288(10) -0.0216(11) -0.0066(10) 0.0276(14) Eu 0.0209(9) 0.0177(9) 0.0141(8) 0.0007(7) 0.0008(6) -0.0071(8) P1 0.012(4) 0.013(4) 0.012(4) 0.004(3) -0.002(3) -0.002(4) P2 0.021(4) 0.017(5) 0.012(4) 0.006(4) 0.002(3) -0.008(4) P3 0.054(7) 0.054(8) 0.015(4) -0.006(5) 0.009(4) -0.041(7) P4 0.092(10) 0.014(6) 0.021(5) 0.001(4) 0.006(6) -0.017(6) K1 0.032(4) 0.025(5) 0.020(4) 0.004(3) -0.002(3) -0.009(4) K2 0.054(6) 0.034(6) 0.046(6) 0.013(5) -0.016(5) -0.020(5) K3 0.032(5) 0.055(7) 0.027(5) 0.002(5) 0.008(4) 0.000(5) K4 0.047(5) 0.033(5) 0.020(4) 0.005(4) -0.002(4) -0.017(5) K5 0.068(7) 0.066(8) 0.013(4) -0.004(4) 0.009(4) -0.048(6) Cl1 0.21(3) 0.059(12) 0.125(17) -0.071(12) 0.112(18) -0.077(15) Cl2 0.111(12) 0.040(8) 0.055(8) 0.016(6) -0.025(8) -0.042(9) Cl3 0.067(10) 0.29(3) 0.026(6) -0.012(11) 0.002(6) -0.118(15) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 W2 O2E 101.4(12) . . ? O2 W2 O212 95.4(11) . . ? O2E W2 O212 100.5(11) . . ? O2 W2 O270 92.2(11) . . ? O2E W2 O270 91.8(11) . . ? O212 W2 O270 163.9(10) . . ? O2 W2 O230 89.3(11) . . ? O2E W2 O230 166.7(11) . . ? O212 W2 O230 86.1(10) . . ? O270 W2 O230 79.8(9) . . ? O2 W2 O2P 170.2(10) . . ? O2E W2 O2P 87.6(11) . . ? O212 W2 O2P 86.6(10) . . ? O270 W2 O2P 83.6(10) . . ? O230 W2 O2P 81.2(9) . . ? O2 W2 K4 48.7(8) . . ? O2E W2 K4 55.6(9) . . ? O212 W2 K4 116.5(8) . . ? O270 W2 K4 79.0(8) . . ? O230 W2 K4 131.4(7) . . ? O2P W2 K4 138.2(6) . . ? O2 W2 K1 40.1(8) . . ? O2E W2 K1 97.3(8) . . ? O212 W2 K1 56.6(8) . . ? O270 W2 K1 132.4(7) . . ? O230 W2 K1 95.9(6) . . ? O2P W2 K1 143.1(6) . . ? K4 W2 K1 68.7(2) . . ? O3 W3 O230 101.9(12) . . ? O3 W3 O313 98.5(12) . . ? O230 W3 O313 91.3(11) . . ? O3 W3 O340 100.9(12) . . ? O230 W3 O340 157.2(10) . . ? O313 W3 O340 86.0(11) . . ? O3 W3 O370 96.5(12) . . ? O230 W3 O370 89.3(10) . . ? O313 W3 O370 164.5(11) . . ? O340 W3 O370 87.4(11) . . ? O3 W3 O3P 171.8(11) . . ? O230 W3 O3P 85.9(9) . . ? O313 W3 O3P 83.8(9) . . ? O340 W3 O3P 71.3(9) . . ? O370 W3 O3P 80.8(9) . . ? O3 W3 K1 47.0(10) . 2_865 ? O230 W3 K1 84.0(8) . 2_865 ? O313 W3 K1 142.4(8) . 2_865 ? O340 W3 K1 111.5(7) . 2_865 ? O370 W3 K1 53.0(8) . 2_865 ? O3P W3 K1 132.7(5) . 2_865 ? O3 W3 K4 26.4(10) . 2_865 ? O230 W3 K4 85.3(7) . 2_865 ? O313 W3 K4 78.4(8) . 2_865 ? O340 W3 K4 116.2(7) . 2_865 ? O370 W3 K4 117.0(8) . 2_865 ? O3P W3 K4 160.0(5) . 2_865 ? K1 W3 K4 64.04(19) 2_865 2_865 ? O4 W4 O480 97.8(11) . . ? O4 W4 O340 100.5(11) . . ? O480 W4 O340 92.0(10) . . ? O4 W4 O450 102.6(11) . . ? O480 W4 O450 88.1(10) . . ? O340 W4 O450 156.7(11) . . ? O4 W4 O414 96.6(10) . . ? O480 W4 O414 165.5(10) . . ? O340 W4 O414 87.5(10) . . ? O450 W4 O414 86.7(10) . . ? O4 W4 O3P 174.7(10) . . ? O480 W4 O3P 82.3(9) . . ? O340 W4 O3P 74.3(9) . . ? O450 W4 O3P 82.7(9) . . ? O414 W4 O3P 83.6(8) . . ? O4 W4 K3 45.5(8) . . ? O480 W4 K3 53.1(7) . . ? O340 W4 K3 107.2(7) . . ? O450 W4 K3 91.4(8) . . ? O414 W4 K3 140.5(7) . . ? O3P W4 K3 135.3(5) . . ? O5 W5 O560 100.6(11) . . ? O5 W5 O515 97.3(11) . . ? O560 W5 O515 91.7(10) . . ? O5 W5 O450 102.4(11) . . ? O560 W5 O450 157.0(11) . . ? O515 W5 O450 84.6(10) . . ? O5 W5 O580 95.5(11) . . ? O560 W5 O580 93.7(10) . . ? O515 W5 O580 165.0(11) . . ? O450 W5 O580 85.0(10) . . ? O5 W5 O5P 174.4(9) . . ? O560 W5 O5P 74.0(9) . . ? O515 W5 O5P 84.2(10) . . ? O450 W5 O5P 83.1(9) . . ? O580 W5 O5P 83.8(9) . . ? O5 W5 K3 38.5(8) . 2_955 ? O560 W5 K3 106.0(8) . 2_955 ? O515 W5 K3 59.4(8) . 2_955 ? O450 W5 K3 91.6(8) . 2_955 ? O580 W5 K3 131.8(8) . 2_955 ? O5P W5 K3 143.5(6) . 2_955 ? O6E W6 O6 102.5(12) . . ? O6E W6 O690 95.2(11) . . ? O6 W6 O690 97.6(11) . . ? O6E W6 O616 92.2(11) . . ? O6 W6 O616 98.0(11) . . ? O690 W6 O616 160.8(10) . . ? O6E W6 O560 162.6(9) . . ? O6 W6 O560 94.9(11) . . ? O690 W6 O560 82.7(10) . . ? O616 W6 O560 84.9(10) . . ? O6E W6 O5P 91.5(9) . . ? O6 W6 O5P 166.0(11) . . ? O690 W6 O5P 81.5(9) . . ? O616 W6 O5P 80.6(9) . . ? O560 W6 O5P 71.1(8) . . ? O7 W7 O270 101.8(12) . . ? O7 W7 O370 100.4(12) . . ? O270 W7 O370 87.3(11) . . ? O7 W7 O790 99.7(12) . . ? O270 W7 O790 92.9(11) . . ? O370 W7 O790 159.4(12) . . ? O7 W7 O780 101.3(13) . . ? O270 W7 O780 156.9(12) . . ? O370 W7 O780 86.9(12) . . ? O790 W7 O780 84.9(12) . . ? O7 W7 O7P 171.6(10) . . ? O270 W7 O7P 83.6(10) . . ? O370 W7 O7P 86.1(10) . . ? O790 W7 O7P 73.5(10) . . ? O780 W7 O7P 73.6(11) . . ? O7 W7 K1 47.9(9) . 2_865 ? O270 W7 K1 83.3(7) . 2_865 ? O370 W7 K1 55.6(8) . 2_865 ? O790 W7 K1 144.9(9) . 2_865 ? O780 W7 K1 111.4(8) . 2_865 ? O7P W7 K1 139.9(6) . 2_865 ? O8 W8 O890 101.0(13) . . ? O8 W8 O580 100.6(13) . . ? O890 W8 O580 92.5(11) . . ? O8 W8 O780 102.2(14) . . ? O890 W8 O780 90.5(12) . . ? O580 W8 O780 156.0(12) . . ? O8 W8 O480 101.0(12) . . ? O890 W8 O480 157.9(11) . . ? O580 W8 O480 82.0(10) . . ? O780 W8 O480 86.3(11) . . ? O8 W8 O7P 173.7(12) . . ? O890 W8 O7P 75.1(10) . . ? O580 W8 O7P 84.7(10) . . ? O780 W8 O7P 73.1(11) . . ? O480 W8 O7P 83.1(9) . . ? O8 W8 K3 50.1(10) . . ? O890 W8 K3 149.6(9) . . ? O580 W8 K3 85.2(8) . . ? O780 W8 K3 103.7(9) . . ? O480 W8 K3 51.6(7) . . ? O7P W8 K3 134.6(6) . . ? O9 W9 O9E 104.1(12) . . ? O9 W9 O690 102.4(12) . . ? O9E W9 O690 95.6(11) . . ? O9 W9 O790 101.2(12) . . ? O9E W9 O790 94.0(11) . . ? O690 W9 O790 151.4(10) . . ? O9 W9 O890 92.8(12) . . ? O9E W9 O890 162.9(10) . . ? O690 W9 O890 83.5(10) . . ? O790 W9 O890 79.6(11) . . ? O9 W9 O7P 162.1(11) . . ? O9E W9 O7P 92.6(9) . . ? O690 W9 O7P 82.1(9) . . ? O790 W9 O7P 70.6(10) . . ? O890 W9 O7P 70.4(9) . . ? O11E W11 O11 102.9(11) . . ? O11E W11 O113 96.1(10) . . ? O11 W11 O113 99.2(11) . . ? O11E W11 O116 95.7(10) . . ? O11 W11 O116 101.4(11) . . ? O113 W11 O116 153.4(10) . . ? O11E W11 O119 165.5(10) . . ? O11 W11 O119 91.5(11) . . ? O113 W11 O119 83.0(10) . . ? O116 W11 O119 79.7(9) . . ? O11E W11 O11P 87.8(9) . . ? O11 W11 O11P 167.7(10) . . ? O113 W11 O11P 73.3(9) . . ? O116 W11 O11P 83.4(9) . . ? O119 W11 O11P 78.1(8) . . ? O12 W12 O212 98.1(12) . . ? O12 W12 O113 100.3(11) . . ? O212 W12 O113 91.5(10) . . ? O12 W12 O128 98.4(11) . . ? O212 W12 O128 163.0(11) . . ? O113 W12 O128 89.7(10) . . ? O12 W12 O123 100.2(11) . . ? O212 W12 O123 88.4(10) . . ? O113 W12 O123 159.3(10) . . ? O128 W12 O123 84.6(10) . . ? O12 W12 O11P 174.8(10) . . ? O212 W12 O11P 81.8(10) . . ? O113 W12 O11P 74.5(9) . . ? O128 W12 O11P 82.2(9) . . ? O123 W12 O11P 84.9(9) . . ? O12 W12 K1 40.2(9) . . ? O212 W12 K1 57.9(8) . . ? O113 W12 K1 98.3(8) . . ? O128 W12 K1 138.6(7) . . ? O123 W12 K1 99.2(8) . . ? O11P W12 K1 139.1(6) . . ? O12 W12 K2 43.8(9) . . ? O212 W12 K2 104.5(8) . . ? O113 W12 K2 141.8(7) . . ? O128 W12 K2 84.7(7) . . ? O123 W12 K2 57.5(7) . . ? O11P W12 K2 141.2(6) . . ? K1 W12 K2 64.1(2) . . ? O13 W13 O313 101.4(12) . . ? O13 W13 O123 100.6(12) . . ? O313 W13 O123 91.7(11) . . ? O13 W13 O137 96.2(12) . . ? O313 W13 O137 162.1(11) . . ? O123 W13 O137 88.0(11) . . ? O13 W13 O134 102.2(12) . . ? O313 W13 O134 87.8(11) . . ? O123 W13 O134 156.8(10) . . ? O137 W13 O134 85.6(12) . . ? O13 W13 O13P 173.9(11) . . ? O313 W13 O13P 81.8(9) . . ? O123 W13 O13P 84.4(9) . . ? O137 W13 O13P 80.4(10) . . ? O134 W13 O13P 72.6(9) . . ? O14 W14 O414 99.1(11) . . ? O14 W14 O134 100.1(12) . . ? O414 W14 O134 90.5(11) . . ? O14 W14 O145 101.3(12) . . ? O414 W14 O145 89.2(10) . . ? O134 W14 O145 158.4(11) . . ? O14 W14 O148 97.2(12) . . ? O414 W14 O148 163.6(11) . . ? O134 W14 O148 88.3(11) . . ? O145 W14 O148 85.9(10) . . ? O14 W14 O13P 174.0(10) . . ? O414 W14 O13P 82.9(9) . . ? O134 W14 O13P 74.1(9) . . ? O145 W14 O13P 84.4(9) . . ? O148 W14 O13P 81.0(10) . . ? O15 W15 O515 98.3(12) . . ? O15 W15 O145 102.6(12) . . ? O515 W15 O145 88.1(11) . . ? O15 W15 O157 99.3(12) . . ? O515 W15 O157 90.3(11) . . ? O145 W15 O157 158.0(12) . . ? O15 W15 O158 97.2(12) . . ? O515 W15 O158 164.4(12) . . ? O145 W15 O158 87.8(11) . . ? O157 W15 O158 87.9(11) . . ? O15 W15 O15P 172.7(10) . . ? O515 W15 O15P 83.8(10) . . ? O145 W15 O15P 84.5(9) . . ? O157 W15 O15P 73.6(10) . . ? O158 W15 O15P 80.9(10) . . ? O15 W15 K3 37.1(9) . 2_955 ? O515 W15 K3 61.9(8) . 2_955 ? O145 W15 K3 93.5(8) . 2_955 ? O157 W15 K3 105.0(8) . 2_955 ? O158 W15 K3 133.4(9) . 2_955 ? O15P W15 K3 145.7(5) . 2_955 ? O16 W16 O616 101.4(11) . . ? O16 W16 O116 100.6(11) . . ? O616 W16 O116 90.2(11) . . ? O16 W16 O157 97.8(12) . . ? O616 W16 O157 91.5(11) . . ? O116 W16 O157 160.8(10) . . ? O16 W16 O169 96.2(10) . . ? O616 W16 O169 162.4(10) . . ? O116 W16 O169 86.5(10) . . ? O157 W16 O169 86.1(10) . . ? O16 W16 O15P 171.2(11) . . ? O616 W16 O15P 82.5(9) . . ? O116 W16 O15P 87.2(9) . . ? O157 W16 O15P 74.1(9) . . ? O169 W16 O15P 80.1(8) . . ? O17 W17 O128 103.3(12) . . ? O17 W17 O179 101.1(12) . . ? O128 W17 O179 90.6(10) . . ? O17 W17 O178 98.6(13) . . ? O128 W17 O178 158.1(11) . . ? O179 W17 O178 86.5(12) . . ? O17 W17 O137 103.3(12) . . ? O128 W17 O137 86.0(11) . . ? O179 W17 O137 155.5(11) . . ? O178 W17 O137 87.8(12) . . ? O17 W17 O17P 170.0(12) . . ? O128 W17 O17P 84.3(9) . . ? O179 W17 O17P 72.1(10) . . ? O178 W17 O17P 74.1(11) . . ? O137 W17 O17P 83.5(10) . . ? O18 W18 O148 101.7(13) . . ? O18 W18 O189 101.7(13) . . ? O148 W18 O189 156.6(12) . . ? O18 W18 O158 102.2(13) . . ? O148 W18 O158 87.1(11) . . ? O189 W18 O158 89.1(11) . . ? O18 W18 O178 99.5(14) . . ? O148 W18 O178 86.9(12) . . ? O189 W18 O178 88.2(12) . . ? O158 W18 O178 158.2(12) . . ? O18 W18 O17P 171.6(12) . . ? O148 W18 O17P 82.8(10) . . ? O189 W18 O17P 73.9(10) . . ? O158 W18 O17P 85.1(10) . . ? O178 W18 O17P 73.4(11) . . ? O19 W19 O119 103.6(11) . . ? O19 W19 O169 102.3(10) . . ? O119 W19 O169 91.1(10) . . ? O19 W19 O179 101.2(11) . . ? O119 W19 O179 91.7(11) . . ? O169 W19 O179 154.9(10) . . ? O19 W19 O189 98.0(11) . . ? O119 W19 O189 158.3(10) . . ? O169 W19 O189 85.8(10) . . ? O179 W19 O189 82.4(11) . . ? O19 W19 O17P 167.3(10) . . ? O119 W19 O17P 87.0(10) . . ? O169 W19 O17P 84.1(9) . . ? O179 W19 O17P 71.2(9) . . ? O189 W19 O17P 71.3(10) . . ? O22 W22 O22E 102.8(15) . . ? O22 W22 O227 102.2(16) . . ? O22E W22 O227 94.6(14) . . ? O22 W22 O223 92.9(15) . . ? O22E W22 O223 163.2(13) . . ? O227 W22 O223 87.7(13) . . ? O22 W22 O222 95.1(17) . . ? O22E W22 O222 91.9(15) . . ? O227 W22 O222 159.7(15) . . ? O223 W22 O222 80.8(15) . . ? O22 W22 O22P 165.1(15) . . ? O22E W22 O22P 91.7(12) . . ? O227 W22 O22P 79.6(13) . . ? O223 W22 O22P 72.4(12) . . ? O222 W22 O22P 81.0(14) . . ? O23 W23 O223 100.8(17) . . ? O23 W23 O238 100.6(18) . . ? O223 W23 O238 93.0(16) . . ? O23 W23 O234 103.0(17) . . ? O223 W23 O234 156.1(14) . . ? O238 W23 O234 85.0(16) . . ? O23 W23 O233 93(2) . . ? O223 W23 O233 94.1(17) . . ? O238 W23 O233 162.8(19) . . ? O234 W23 O233 82.1(17) . . ? O23 W23 O22P 174.2(15) . . ? O223 W23 O22P 73.6(13) . . ? O238 W23 O22P 81.0(14) . . ? O234 W23 O22P 82.7(13) . . ? O233 W23 O22P 86.1(16) . . ? O24 W24 O248 98.4(18) . . ? O24 W24 O234 102.6(18) . . ? O248 W24 O234 90.0(14) . . ? O24 W24 O245 100.3(18) . . ? O248 W24 O245 97.2(15) . . ? O234 W24 O245 154.7(14) . . ? O24 W24 O244 96.9(17) . . ? O248 W24 O244 164.5(13) . . ? O234 W24 O244 84.3(13) . . ? O245 W24 O244 82.5(14) . . ? O24 W24 O24P 173.8(16) . . ? O248 W24 O24P 84.2(12) . . ? O234 W24 O24P 83.0(12) . . ? O245 W24 O24P 73.7(12) . . ? O244 W24 O24P 80.9(11) . . ? O25 W25 O256 104.0(13) . . ? O25 W25 O259 97.3(14) . . ? O256 W25 O259 89.9(12) . . ? O25 W25 O255 96.7(13) . . ? O256 W25 O255 90.6(12) . . ? O259 W25 O255 165.4(13) . . ? O25 W25 O245 99.3(14) . . ? O256 W25 O245 156.5(13) . . ? O259 W25 O245 90.1(14) . . ? O255 W25 O245 83.6(13) . . ? O25 W25 O24P 169.8(12) . . ? O256 W25 O24P 86.1(10) . . ? O259 W25 O24P 80.9(12) . . ? O255 W25 O24P 84.6(11) . . ? O245 W25 O24P 70.7(12) . . ? O25 W25 K5 38.3(10) . 2_866 ? O256 W25 K5 96.9(8) . 2_866 ? O259 W25 K5 135.4(10) . 2_866 ? O255 W25 K5 58.9(9) . 2_866 ? O245 W25 K5 99.5(10) . 2_866 ? O24P W25 K5 143.4(7) . 2_866 ? O26E W26 O26 101.3(12) . . ? O26E W26 O266 99.9(10) . . ? O26 W26 O266 94.7(11) . . ? O26E W26 O269 93.9(11) . . ? O26 W26 O269 94.0(12) . . ? O266 W26 O269 161.9(11) . . ? O26E W26 O256 167.3(11) . . ? O26 W26 O256 90.8(11) . . ? O266 W26 O256 82.8(10) . . ? O269 W26 O256 81.2(10) . . ? O26E W26 O26P 88.0(11) . . ? O26 W26 O26P 170.6(11) . . ? O266 W26 O26P 85.0(10) . . ? O269 W26 O26P 83.8(10) . . ? O256 W26 O26P 79.8(10) . . ? O26E W26 Eu 23.9(9) . . ? O26 W26 Eu 124.6(9) . . ? O266 W26 Eu 91.5(7) . . ? O269 W26 Eu 96.6(8) . . ? O256 W26 Eu 144.5(7) . . ? O26P W26 Eu 64.8(6) . . ? O26E W26 K5 97.9(8) . . ? O26 W26 K5 37.5(9) . . ? O266 W26 K5 58.2(7) . . ? O269 W26 K5 131.4(8) . . ? O256 W26 K5 94.1(7) . . ? O26P W26 K5 143.2(7) . . ? Eu W26 K5 112.50(14) . . ? O27 W27 O27E 102.8(16) . . ? O27 W27 O227 106.8(17) . . ? O27E W27 O227 94.6(14) . . ? O27 W27 O279 99.9(17) . . ? O27E W27 O279 94.3(14) . . ? O227 W27 O279 149.0(15) . . ? O27 W27 O278 95.4(18) . . ? O27E W27 O278 161.7(16) . . ? O227 W27 O278 79.8(16) . . ? O279 W27 O278 82.4(16) . . ? O27 W27 O27P 161.8(14) . . ? O27E W27 O27P 93.5(11) . . ? O227 W27 O27P 79.4(12) . . ? O279 W27 O27P 70.5(13) . . ? O278 W27 O27P 68.4(14) . . ? O28 W28 O278 104(2) . . ? O28 W28 O289 102.3(18) . . ? O278 W28 O289 92.6(19) . . ? O28 W28 O238 101.1(18) . . ? O278 W28 O238 91.8(19) . . ? O289 W28 O238 154.5(16) . . ? O28 W28 O248 99.2(16) . . ? O278 W28 O248 156.8(16) . . ? O289 W28 O248 85.4(15) . . ? O238 W28 O248 80.8(14) . . ? O28 W28 O27P 175.0(16) . . ? O278 W28 O27P 75.4(16) . . ? O289 W28 O27P 73.0(13) . . ? O238 W28 O27P 83.9(13) . . ? O248 W28 O27P 82.0(11) . . ? O29 W29 O269 101.1(14) . . ? O29 W29 O279 98.8(16) . . ? O269 W29 O279 90.0(13) . . ? O29 W29 O259 103.6(15) . . ? O269 W29 O259 87.7(13) . . ? O279 W29 O259 157.5(15) . . ? O29 W29 O289 101.9(16) . . ? O269 W29 O289 157.0(15) . . ? O279 W29 O289 86.5(16) . . ? O259 W29 O289 87.0(15) . . ? O29 W29 O27P 171.1(13) . . ? O269 W29 O27P 84.1(11) . . ? O279 W29 O27P 73.8(13) . . ? O259 W29 O27P 83.7(12) . . ? O289 W29 O27P 73.0(13) . . ? O31 W31 O31E 104.3(12) . . ? O31 W31 O312 100.1(13) . . ? O31E W31 O312 94.0(12) . . ? O31 W31 O316 101.0(12) . . ? O31E W31 O316 96.6(12) . . ? O312 W31 O316 153.2(13) . . ? O31 W31 O317 91.3(12) . . ? O31E W31 O317 164.5(11) . . ? O312 W31 O317 82.6(13) . . ? O316 W31 O317 80.7(13) . . ? O31 W31 O31P 168.0(11) . . ? O31E W31 O31P 86.7(10) . . ? O312 W31 O31P 83.8(11) . . ? O316 W31 O31P 72.4(11) . . ? O317 W31 O31P 77.9(11) . . ? O31 W31 K4 58.1(9) . . ? O31E W31 K4 88.7(8) . . ? O312 W31 K4 45.2(9) . . ? O316 W31 K4 159.1(8) . . ? O317 W31 K4 99.2(9) . . ? O31P W31 K4 128.2(7) . . ? O222 W32 O32 101.3(19) . . ? O222 W32 O312 92.2(17) . . ? O32 W32 O312 100.6(15) . . ? O222 W32 O323 92.7(18) . . ? O32 W32 O323 96.6(17) . . ? O312 W32 O323 160.9(15) . . ? O222 W32 O327 165.1(17) . . ? O32 W32 O327 93.6(15) . . ? O312 W32 O327 85.1(13) . . ? O323 W32 O327 85.5(15) . . ? O222 W32 O32P 84.5(17) . . ? O32 W32 O32P 169.8(16) . . ? O312 W32 O32P 87.4(13) . . ? O323 W32 O32P 74.7(15) . . ? O327 W32 O32P 80.8(12) . . ? O222 W32 K4 86.7(14) . . ? O32 W32 K4 51.1(13) . . ? O312 W32 K4 52.3(9) . . ? O323 W32 K4 146.5(12) . . ? O327 W32 K4 102.9(9) . . ? O32P W32 K4 138.3(9) . . ? O233 W33 O33 98(3) . . ? O233 W33 O334 89(2) . . ? O33 W33 O334 102(2) . . ? O233 W33 O323 93(2) . . ? O33 W33 O323 100(2) . . ? O334 W33 O323 157.4(17) . . ? O233 W33 O338 163(2) . . ? O33 W33 O338 98(2) . . ? O334 W33 O338 82.9(16) . . ? O323 W33 O338 88.8(15) . . ? O233 W33 O32P 83(2) . . ? O33 W33 O32P 173.6(19) . . ? O334 W33 O32P 84.7(15) . . ? O323 W33 O32P 73.3(14) . . ? O338 W33 O32P 81.3(14) . . ? O34 W34 O244 100.8(19) . . ? O34 W34 O334 101(2) . . ? O244 W34 O334 94.6(16) . . ? O34 W34 O345 99.5(19) . . ? O244 W34 O345 90.2(15) . . ? O334 W34 O345 157.3(16) . . ? O34 W34 O348 98(2) . . ? O244 W34 O348 160.8(17) . . ? O334 W34 O348 80.2(18) . . ? O345 W34 O348 88.0(18) . . ? O34 W34 O34P 172.5(18) . . ? O244 W34 O34P 81.2(13) . . ? O334 W34 O34P 85.7(15) . . ? O345 W34 O34P 73.1(14) . . ? O348 W34 O34P 80.0(16) . . ? O35 W35 O255 98.1(14) . . ? O35 W35 O345 102.0(15) . . ? O255 W35 O345 88.2(14) . . ? O35 W35 O356 100.6(14) . . ? O255 W35 O356 90.3(13) . . ? O345 W35 O356 157.3(14) . . ? O35 W35 O359 97.5(15) . . ? O255 W35 O359 164.3(14) . . ? O345 W35 O359 88.7(15) . . ? O356 W35 O359 86.6(14) . . ? O35 W35 O34P 175.6(14) . . ? O255 W35 O34P 82.3(12) . . ? O345 W35 O34P 73.6(14) . . ? O356 W35 O34P 83.8(12) . . ? O359 W35 O34P 82.1(13) . . ? O35 W35 K5 40.5(11) . 2_866 ? O255 W35 K5 57.8(9) . 2_866 ? O345 W35 K5 103.0(11) . 2_866 ? O356 W35 K5 95.3(10) . 2_866 ? O359 W35 K5 137.7(11) . 2_866 ? O34P W35 K5 140.1(8) . 2_866 ? O36 W36 O266 99.3(12) . . ? O36 W36 O356 100.4(13) . . ? O266 W36 O356 89.3(12) . . ? O36 W36 O316 98.9(12) . . ? O266 W36 O316 95.3(11) . . ? O356 W36 O316 159.1(13) . . ? O36 W36 O369 94.8(15) . . ? O266 W36 O369 165.3(13) . . ? O356 W36 O369 84.2(14) . . ? O316 W36 O369 86.4(13) . . ? O36 W36 O31P 173.3(11) . . ? O266 W36 O31P 83.7(10) . . ? O356 W36 O31P 85.5(12) . . ? O316 W36 O31P 74.8(11) . . ? O369 W36 O31P 82.7(13) . . ? O36 W36 K5 41.2(10) . . ? O266 W36 K5 58.1(7) . . ? O356 W36 K5 97.8(10) . . ? O316 W36 K5 101.9(9) . . ? O369 W36 K5 135.8(11) . . ? O31P W36 K5 141.5(8) . . ? O37 W37 O327 103.4(17) . . ? O37 W37 O317 104.0(18) . . ? O327 W37 O317 91.9(15) . . ? O37 W37 O378 97.2(18) . . ? O327 W37 O378 91.3(14) . . ? O317 W37 O378 157.1(14) . . ? O37 W37 O379 98.0(18) . . ? O327 W37 O379 157.7(14) . . ? O317 W37 O379 88.8(15) . . ? O378 W37 O379 79.9(15) . . ? O37 W37 O37P 166.7(17) . . ? O327 W37 O37P 85.5(13) . . ? O317 W37 O37P 85.3(13) . . ? O378 W37 O37P 72.4(13) . . ? O379 W37 O37P 72.4(13) . . ? O38 W38 O338 104(2) . . ? O38 W38 O348 105(2) . . ? O338 W38 O348 85.6(18) . . ? O38 W38 O378 99(2) . . ? O338 W38 O378 92.0(15) . . ? O348 W38 O378 155.5(18) . . ? O38 W38 O389 98(2) . . ? O338 W38 O389 158.7(18) . . ? O348 W38 O389 89.3(19) . . ? O378 W38 O389 84.2(16) . . ? O38 W38 O37P 168.4(19) . . ? O338 W38 O37P 85.7(15) . . ? O348 W38 O37P 82.0(17) . . ? O378 W38 O37P 73.5(13) . . ? O389 W38 O37P 73.1(16) . . ? O39 W39 O389 100(2) . . ? O39 W39 O369 100(2) . . ? O389 W39 O369 159.9(18) . . ? O39 W39 O379 98(2) . . ? O389 W39 O379 89.1(18) . . ? O369 W39 O379 91.1(16) . . ? O39 W39 O359 103.8(19) . . ? O389 W39 O359 86.8(18) . . ? O369 W39 O359 85.6(15) . . ? O379 W39 O359 158.2(16) . . ? O39 W39 O37P 172.2(19) . . ? O389 W39 O37P 75.7(16) . . ? O369 W39 O37P 84.9(14) . . ? O379 W39 O37P 75.6(14) . . ? O359 W39 O37P 82.7(13) . . ? O2E Eu O31E 75.0(8) . . ? O2E Eu O26E 140.7(9) . . ? O31E Eu O26E 76.2(9) . . ? O2E Eu O27E 146.0(9) . . ? O31E Eu O27E 117.9(9) . . ? O26E Eu O27E 72.3(9) . . ? O2E Eu O22E 83.4(9) . . ? O31E Eu O22E 71.6(9) . . ? O26E Eu O22E 111.8(9) . . ? O27E Eu O22E 72.8(10) . . ? O2E Eu O11E 75.6(8) . . ? O31E Eu O11E 78.2(8) . . ? O26E Eu O11E 72.8(8) . . ? O27E Eu O11E 135.9(9) . . ? O22E Eu O11E 146.8(9) . . ? O2E Eu O9E 71.6(8) . . ? O31E Eu O9E 137.2(8) . . ? O26E Eu O9E 145.0(8) . . ? O27E Eu O9E 80.0(9) . . ? O22E Eu O9E 78.7(9) . . ? O11E Eu O9E 117.3(8) . . ? O2E Eu O6E 108.1(8) . . ? O31E Eu O6E 145.9(8) . . ? O26E Eu O6E 82.5(8) . . ? O27E Eu O6E 79.2(9) . . ? O22E Eu O6E 142.0(9) . . ? O11E Eu O6E 70.2(8) . . ? O9E Eu O6E 71.6(8) . . ? O2E Eu W26 138.1(6) . . ? O31E Eu W26 65.0(6) . . ? O26E Eu W26 17.5(6) . . ? O27E Eu W26 69.5(7) . . ? O22E Eu W26 94.9(7) . . ? O11E Eu W26 84.4(5) . . ? O9E Eu W26 149.3(5) . . ? O6E Eu W26 98.8(5) . . ? O2E Eu K4 30.4(7) . . ? O31E Eu K4 61.0(6) . . ? O26E Eu K4 137.1(6) . . ? O27E Eu K4 125.0(7) . . ? O22E Eu K4 54.2(7) . . ? O11E Eu K4 99.0(6) . . ? O9E Eu K4 76.7(6) . . ? O6E Eu K4 135.5(5) . . ? W26 Eu K4 123.66(13) . . ? O2P P1 O3P 111.8(13) . . ? O2P P1 O5P 112.3(13) . . ? O3P P1 O5P 111.6(13) . . ? O2P P1 O7P 108.6(14) . . ? O3P P1 O7P 106.7(12) . . ? O5P P1 O7P 105.4(13) . . ? O15P P2 O11P 111.4(13) . . ? O15P P2 O13P 111.4(13) . . ? O11P P2 O13P 113.4(13) . . ? O15P P2 O17P 105.1(13) . . ? O11P P2 O17P 108.0(14) . . ? O13P P2 O17P 107.0(13) . . ? O26P P3 O22P 111.2(17) . . ? O26P P3 O27P 109.9(17) . . ? O22P P3 O27P 105.9(17) . . ? O26P P3 O24P 111.8(15) . . ? O22P P3 O24P 110.9(18) . . ? O27P P3 O24P 106.8(15) . . ? O31P P4 O32P 114.2(19) . . ? O31P P4 O34P 110.0(18) . . ? O32P P4 O34P 112(2) . . ? O31P P4 O37P 106.5(18) . . ? O32P P4 O37P 106.3(19) . . ? O34P P4 O37P 107.4(18) . . ? W2 O2 K4 103.0(11) . . ? W2 O2 K1 116.3(12) . . ? K4 O2 K1 98.9(9) . . ? W3 O3 K4 136.9(15) . 2_865 ? W3 O3 K1 107.7(12) . 2_865 ? K4 O3 K1 97.2(10) 2_865 2_865 ? W4 O4 K3 109.2(11) . . ? W5 O5 K3 119.9(11) . 2_955 ? W7 O7 K2 132.0(13) . 2_865 ? W7 O7 K1 105.7(12) . 2_865 ? K2 O7 K1 95.9(9) 2_865 2_865 ? W8 O8 K3 104.4(13) . . ? W11 O11 K5 165.0(14) . . ? W12 O12 K1 116.1(12) . . ? W12 O12 K2 113.9(12) . . ? K1 O12 K2 91.8(8) . . ? W13 O13 K2 111.9(12) . . ? W15 O15 K3 121.2(13) . 2_955 ? W25 O25 K5 119.1(14) . 2_866 ? W26 O26 K5 119.0(13) . . ? W31 O31 K1 166.4(15) . . ? W31 O31 K4 95.3(10) . . ? K1 O31 K4 90.6(7) . . ? W32 O32 K4 99.8(16) . . ? W35 O35 K5 116.7(14) . 2_866 ? W36 O36 K5 115.5(13) . . ? W2 O2E Eu 139.6(15) . . ? W2 O2E K4 94.5(10) . . ? Eu O2E K4 125.8(10) . . ? W6 O6E Eu 156.3(13) . . ? W9 O9E Eu 155.5(14) . . ? W11 O11E Eu 155.1(12) . . ? W22 O22E Eu 156.5(16) . . ? W26 O26E Eu 138.6(14) . . ? W27 O27E Eu 155.7(17) . . ? W31 O31E Eu 153.8(13) . . ? P1 O2P W2 136.4(14) . . ? P1 O3P W4 132.2(12) . . ? P1 O3P W3 124.7(12) . . ? W4 O3P W3 92.4(7) . . ? P1 O5P W6 127.7(13) . . ? P1 O5P W5 126.8(12) . . ? W6 O5P W5 93.1(8) . . ? P1 O7P W7 122.4(13) . . ? P1 O7P W8 125.8(14) . . ? W7 O7P W8 90.3(8) . . ? P1 O7P W9 124.5(13) . . ? W7 O7P W9 91.7(9) . . ? W8 O7P W9 92.2(8) . . ? P2 O11P W12 127.1(12) . . ? P2 O11P W11 132.3(13) . . ? W12 O11P W11 89.2(8) . . ? P2 O13P W14 129.0(13) . . ? P2 O13P W13 126.8(13) . . ? W14 O13P W13 90.5(7) . . ? P2 O15P W16 129.3(13) . . ? P2 O15P W15 129.5(12) . . ? W16 O15P W15 91.2(8) . . ? P2 O17P W18 125.6(14) . . ? P2 O17P W17 123.8(14) . . ? W18 O17P W17 91.5(9) . . ? P2 O17P W19 122.0(13) . . ? W18 O17P W19 92.6(9) . . ? W17 O17P W19 92.0(9) . . ? P3 O22P W22 130(2) . . ? P3 O22P W23 126.8(18) . . ? W22 O22P W23 91.3(11) . . ? P3 O24P W24 130.2(15) . . ? P3 O24P W25 122.7(16) . . ? W24 O24P W25 93.9(9) . . ? P3 O26P W26 136.1(15) . . ? P3 O27P W29 123.0(15) . . ? P3 O27P W28 128.0(17) . . ? W29 O27P W28 90.9(9) . . ? P3 O27P W27 123.0(14) . . ? W29 O27P W27 90.1(10) . . ? W28 O27P W27 91.2(9) . . ? P4 O31P W36 129.8(17) . . ? P4 O31P W31 129.7(17) . . ? W36 O31P W31 89.9(10) . . ? P4 O34P W35 128.0(18) . . ? P4 O34P W34 126.3(19) . . ? W35 O34P W34 90.2(11) . . ? P4 O37P W39 125.9(19) . . ? P4 O37P W38 125.0(18) . . ? W39 O37P W38 91.0(12) . . ? P4 O37P W37 121.3(18) . . ? W39 O37P W37 91.7(11) . . ? W38 O37P W37 92.3(12) . . ? P4 O32P W32 128(2) . . ? P4 O32P W33 130(2) . . ? W32 O32P W33 91.9(13) . . ? W12 O113 W11 121.2(13) . . ? W16 O116 W11 155.9(13) . . ? W19 O119 W11 149.9(13) . . ? W13 O123 W12 151.0(14) . . ? W17 O128 W12 152.9(13) . . ? W14 O134 W13 122.4(13) . . ? W13 O137 W17 149.8(16) . . ? W15 O145 W14 150.9(14) . . ? W18 O148 W14 151.7(14) . . ? W15 O157 W16 120.6(14) . . ? W18 O158 W15 148.7(15) . . ? W19 O169 W16 145.3(13) . . ? W17 O178 W18 120.9(15) . . ? W17 O179 W19 124.6(13) . . ? W18 O189 W19 122.2(14) . . ? W12 O212 W2 164.7(15) . . ? W12 O212 K1 93.0(9) . . ? W2 O212 K1 93.7(9) . . ? W32 O222 W22 157(3) . . ? W23 O223 W22 122.7(17) . . ? W27 O227 W22 143.0(18) . . ? W3 O230 W2 149.7(13) . . ? W33 O233 W23 170(3) . . ? W24 O234 W23 148(2) . . ? W23 O238 W28 155(2) . . ? W34 O244 W24 160.9(18) . . ? W24 O245 W25 121.4(17) . . ? W24 O248 W28 151.5(18) . . ? W35 O255 W25 157.4(17) . . ? W35 O255 K5 93.9(11) . 2_866 ? W25 O255 K5 90.6(10) . 2_866 ? W25 O256 W26 149.4(14) . . ? W29 O259 W25 147.9(17) . . ? W36 O266 W26 167.4(13) . . ? W36 O266 K5 93.0(8) . . ? W26 O266 K5 92.5(9) . . ? W29 O269 W26 152.4(17) . . ? W7 O270 W2 153.5(15) . . ? W28 O278 W27 125(2) . . ? W29 O279 W27 125(2) . . ? W28 O289 W29 123(2) . . ? W32 O312 W31 155.5(18) . . ? W32 O312 K4 95.5(12) . . ? W31 O312 K4 106.0(13) . . ? W13 O313 W3 156.2(16) . . ? W36 O316 W31 120.2(14) . . ? W37 O317 W31 148.8(18) . . ? W32 O323 W33 119(2) . . ? W37 O327 W32 146.5(19) . . ? W34 O334 W33 157(2) . . ? W38 O338 W33 150(2) . . ? W4 O340 W3 122.0(12) . . ? W34 O345 W35 122.8(19) . . ? W38 O348 W34 155(3) . . ? W36 O356 W35 151.2(19) . . ? W39 O359 W35 150(2) . . ? W39 O369 W36 152(2) . . ? W7 O370 W3 146.7(14) . . ? W7 O370 K1 94.2(10) . 2_865 ? W3 O370 K1 96.6(9) . 2_865 ? W37 O378 W38 121.3(18) . . ? W39 O379 W37 120.3(19) . . ? W39 O389 W38 120(2) . . ? W14 O414 W4 160.8(13) . . ? W4 O450 W5 148.7(15) . . ? W4 O480 W8 151.6(13) . . ? W4 O480 K3 97.3(9) . . ? W8 O480 K3 97.9(9) . . ? W15 O515 W5 164.0(14) . . ? W5 O560 W6 121.8(12) . . ? W8 O580 W5 153.9(14) . . ? W16 O616 W6 159.9(16) . . ? W9 O690 W6 139.7(13) . . ? W8 O780 W7 122.7(15) . . ? W7 O790 W9 123.5(14) . . ? W8 O890 W9 122.3(13) . . ? O31 K1 O12 97.1(8) . . ? O31 K1 O2 75.0(8) . . ? O12 K1 O2 102.3(8) . . ? O31 K1 O918 85.7(10) . . ? O12 K1 O918 83.0(10) . . ? O2 K1 O918 160.4(10) . . ? O31 K1 O7 159.5(8) . 2_865 ? O12 K1 O7 81.9(8) . 2_865 ? O2 K1 O7 125.3(8) . 2_865 ? O918 K1 O7 73.9(10) . 2_865 ? O31 K1 O3 73.5(8) . 2_865 ? O12 K1 O3 168.3(8) . 2_865 ? O2 K1 O3 69.0(8) . 2_865 ? O918 K1 O3 102.7(11) . 2_865 ? O7 K1 O3 109.4(8) 2_865 2_865 ? O31 K1 O904 131.6(8) . . ? O12 K1 O904 68.1(8) . . ? O2 K1 O904 64.8(7) . . ? O918 K1 O904 133.7(10) . . ? O7 K1 O904 67.0(8) 2_865 . ? O3 K1 O904 112.9(8) 2_865 . ? O31 K1 O370 122.2(8) . 2_865 ? O12 K1 O370 137.2(8) . 2_865 ? O2 K1 O370 103.8(8) . 2_865 ? O918 K1 O370 83.6(10) . 2_865 ? O7 K1 O370 55.3(8) 2_865 2_865 ? O3 K1 O370 54.2(7) 2_865 2_865 ? O904 K1 O370 93.6(7) . 2_865 ? O31 K1 O212 69.4(7) . . ? O12 K1 O212 52.7(7) . . ? O2 K1 O212 52.6(7) . . ? O918 K1 O212 123.3(10) . . ? O7 K1 O212 123.2(8) 2_865 . ? O3 K1 O212 116.3(8) 2_865 . ? O904 K1 O212 65.3(7) . . ? O370 K1 O212 152.7(7) 2_865 . ? O31 K1 W7 151.3(7) . 2_865 ? O12 K1 W7 107.7(6) . 2_865 ? O2 K1 W7 112.4(6) . 2_865 ? O918 K1 W7 83.2(8) . 2_865 ? O7 K1 W7 26.5(6) 2_865 2_865 ? O3 K1 W7 83.3(6) 2_865 2_865 ? O904 K1 W7 72.9(5) . 2_865 ? O370 K1 W7 30.2(5) 2_865 2_865 ? O212 K1 W7 137.9(5) . 2_865 ? O31 K1 W3 98.4(6) . 2_865 ? O12 K1 W3 164.3(6) . 2_865 ? O2 K1 W3 79.4(6) . 2_865 ? O918 K1 W3 100.7(9) . 2_865 ? O7 K1 W3 84.5(6) 2_865 2_865 ? O3 K1 W3 25.4(5) 2_865 2_865 ? O904 K1 W3 99.3(6) . 2_865 ? O370 K1 W3 30.4(5) 2_865 2_865 ? O212 K1 W3 131.9(5) . 2_865 ? W7 K1 W3 58.12(13) 2_865 2_865 ? O31 K1 W12 83.6(6) . . ? O12 K1 W12 23.6(5) . . ? O2 K1 W12 80.1(6) . . ? O918 K1 W12 101.3(9) . . ? O7 K1 W12 101.3(6) 2_865 . ? O3 K1 W12 145.2(6) 2_865 . ? O904 K1 W12 64.6(6) . . ? O370 K1 W12 154.2(5) 2_865 . ? O212 K1 W12 29.1(4) . . ? W7 K1 W12 124.5(2) 2_865 . ? W3 K1 W12 158.0(3) 2_865 . ? O904 K2 O911 76.2(9) . 2_865 ? O904 K2 O7 71.7(9) . 2_865 ? O911 K2 O7 78.5(9) 2_865 2_865 ? O904 K2 O927 139.0(15) . . ? O911 K2 O927 74.8(15) 2_865 . ? O7 K2 O927 128.6(15) 2_865 . ? O904 K2 O12 67.0(8) . . ? O911 K2 O12 140.2(9) 2_865 . ? O7 K2 O12 76.1(8) 2_865 . ? O927 K2 O12 144.5(15) . . ? O904 K2 O931 138.4(13) . . ? O911 K2 O931 104.5(13) 2_865 . ? O7 K2 O931 67.9(12) 2_865 . ? O927 K2 O931 77.4(17) . . ? O12 K2 O931 93.7(12) . . ? O904 K2 O13 77.3(8) . . ? O911 K2 O13 88.8(9) 2_865 . ? O7 K2 O13 148.5(8) 2_865 . ? O927 K2 O13 73.7(14) . . ? O12 K2 O13 97.1(7) . . ? O931 K2 O13 143.6(12) . . ? O904 K2 W12 62.0(6) . . ? O911 K2 W12 137.4(7) 2_865 . ? O7 K2 W12 95.1(6) 2_865 . ? O927 K2 W12 133.5(14) . . ? O12 K2 W12 22.3(5) . . ? O931 K2 W12 112.0(11) . . ? O13 K2 W12 74.8(5) . . ? O904 K2 K1 45.5(6) . . ? O911 K2 K1 101.7(7) 2_865 . ? O7 K2 K1 42.3(6) 2_865 . ? O927 K2 K1 170.8(14) . . ? O12 K2 K1 40.6(5) . . ? O931 K2 K1 95.6(11) . . ? O13 K2 K1 115.0(6) . . ? W12 K2 K1 54.53(18) . . ? O904 K2 K4 45.9(6) . 2_865 ? O911 K2 K4 39.1(7) 2_865 2_865 ? O7 K2 K4 91.7(6) 2_865 2_865 ? O927 K2 K4 94.2(13) . 2_865 ? O12 K2 K4 111.7(6) . 2_865 ? O931 K2 K4 142.9(11) . 2_865 ? O13 K2 K4 61.8(5) . 2_865 ? W12 K2 K4 100.1(3) . 2_865 ? K1 K2 K4 87.8(3) . 2_865 ? O910 K3 O15 78.1(8) . 2_955 ? O910 K3 O4 101.7(8) . . ? O15 K3 O4 158.8(9) 2_955 . ? O910 K3 O5 68.7(8) . 2_955 ? O15 K3 O5 99.0(8) 2_955 2_955 ? O4 K3 O5 62.2(7) . 2_955 ? O910 K3 O480 89.3(8) . . ? O15 K3 O480 146.0(8) 2_955 . ? O4 K3 O480 54.5(7) . . ? O5 K3 O480 105.7(7) 2_955 . ? O910 K3 O8 68.1(9) . . ? O15 K3 O8 90.3(8) 2_955 . ? O4 K3 O8 109.4(8) . . ? O5 K3 O8 132.7(8) 2_955 . ? O480 K3 O8 55.7(7) . . ? O910 K3 W4 93.4(6) . . ? O15 K3 W4 171.1(6) 2_955 . ? O4 K3 W4 25.4(5) . . ? O5 K3 W4 80.0(5) 2_955 . ? O480 K3 W4 29.5(4) . . ? O8 K3 W4 84.1(6) . . ? O910 K3 W8 73.6(7) . . ? O15 K3 W8 115.7(7) 2_955 . ? O4 K3 W8 83.9(5) . . ? O5 K3 W8 121.0(5) 2_955 . ? O480 K3 W8 30.5(4) . . ? O8 K3 W8 25.5(6) . . ? W4 K3 W8 58.57(15) . . ? O910 K3 W15 68.8(6) . 2_955 ? O15 K3 W15 21.7(6) 2_955 2_955 ? O4 K3 W15 138.6(7) . 2_955 ? O5 K3 W15 77.3(5) 2_955 2_955 ? O480 K3 W15 155.4(5) . 2_955 ? O8 K3 W15 103.9(6) . 2_955 ? W4 K3 W15 155.1(3) . 2_955 ? W8 K3 W15 127.2(3) . 2_955 ? O910 K3 W5 63.1(6) . 2_955 ? O15 K3 W5 77.3(6) 2_955 2_955 ? O4 K3 W5 83.7(6) . 2_955 ? O5 K3 W5 21.7(5) 2_955 2_955 ? O480 K3 W5 124.6(5) . 2_955 ? O8 K3 W5 131.1(6) . 2_955 ? W4 K3 W5 101.2(3) . 2_955 ? W8 K3 W5 131.1(3) . 2_955 ? W15 K3 W5 55.66(15) 2_955 2_955 ? O3 K4 O911 149.9(9) 2_865 . ? O3 K4 O2 73.7(9) 2_865 . ? O911 K4 O2 100.1(9) . . ? O3 K4 O32 85.2(10) 2_865 . ? O911 K4 O32 98.4(10) . . ? O2 K4 O32 158.9(10) . . ? O3 K4 O312 93.7(9) 2_865 . ? O911 K4 O312 114.0(9) . . ? O2 K4 O312 120.0(9) . . ? O32 K4 O312 60.0(10) . . ? O3 K4 O2E 118.9(9) 2_865 . ? O911 K4 O2E 77.7(9) . . ? O2 K4 O2E 57.0(7) . . ? O32 K4 O2E 138.1(9) . . ? O312 K4 O2E 83.3(9) . . ? O3 K4 O904 80.1(8) 2_865 2_865 ? O911 K4 O904 72.1(8) . 2_865 ? O2 K4 O904 58.2(8) . 2_865 ? O32 K4 O904 119.2(10) . 2_865 ? O312 K4 O904 173.8(9) . 2_865 ? O2E K4 O904 99.5(8) . 2_865 ? O3 K4 O31 68.7(8) 2_865 . ? O911 K4 O31 137.0(9) . . ? O2 K4 O31 67.2(7) . . ? O32 K4 O31 105.1(9) . . ? O312 K4 O31 54.0(8) . . ? O2E K4 O31 60.8(7) . . ? O904 K4 O31 122.6(8) 2_865 . ? O3 K4 W32 95.6(7) 2_865 . ? O911 K4 W32 101.8(7) . . ? O2 K4 W32 151.0(6) . . ? O32 K4 W32 29.1(8) . . ? O312 K4 W32 32.2(7) . . ? O2E K4 W32 110.0(5) . . ? O904 K4 W32 147.9(6) 2_865 . ? O31 K4 W32 83.8(5) . . ? O3 K4 W2 99.7(7) 2_865 . ? O911 K4 W2 83.4(7) . . ? O2 K4 W2 28.3(5) . . ? O32 K4 W2 167.3(8) . . ? O312 K4 W2 107.8(7) . . ? O2E K4 W2 29.9(5) . . ? O904 K4 W2 73.4(6) 2_865 . ? O31 K4 W2 66.5(5) . . ? W32 K4 W2 138.3(3) . . ? O3 K4 W31 85.4(7) 2_865 . ? O911 K4 W31 124.5(7) . . ? O2 K4 W31 91.2(6) . . ? O32 K4 W31 86.6(8) . . ? O312 K4 W31 28.8(7) . . ? O2E K4 W31 63.9(5) . . ? O904 K4 W31 148.8(6) 2_865 . ? O31 K4 W31 26.6(4) . . ? W32 K4 W31 60.62(14) . . ? W2 K4 W31 82.12(19) . . ? O3 K4 W3 16.7(6) 2_865 2_865 ? O911 K4 W3 133.4(7) . 2_865 ? O2 K4 W3 75.0(6) . 2_865 ? O32 K4 W3 84.9(8) . 2_865 ? O312 K4 W3 107.7(7) . 2_865 ? O2E K4 W3 128.1(6) . 2_865 ? O904 K4 W3 66.2(5) 2_865 2_865 ? O31 K4 W3 84.7(5) . 2_865 ? W32 K4 W3 102.5(2) . 2_865 ? W2 K4 W3 103.1(2) . 2_865 ? W31 K4 W3 102.0(2) . 2_865 ? O11 K5 O26 75.6(8) . . ? O11 K5 O25 135.9(9) . 2_866 ? O26 K5 O25 143.2(9) . 2_866 ? O11 K5 O933 64.6(15) . . ? O26 K5 O933 87.2(15) . . ? O25 K5 O933 120.7(15) 2_866 . ? O11 K5 O36 89.4(9) . . ? O26 K5 O36 102.5(9) . . ? O25 K5 O36 66.5(9) 2_866 . ? O933 K5 O36 149.2(15) . . ? O11 K5 O35 115.9(9) . 2_866 ? O26 K5 O35 66.2(9) . 2_866 ? O25 K5 O35 102.8(9) 2_866 2_866 ? O933 K5 O35 64.1(15) . 2_866 ? O36 K5 O35 146.4(9) . 2_866 ? O11 K5 O919 69.6(11) . . ? O26 K5 O919 142.7(12) . . ? O25 K5 O919 74.0(11) 2_866 . ? O933 K5 O919 66.3(16) . . ? O36 K5 O919 90.1(12) . . ? O35 K5 O919 118.4(12) 2_866 . ? O11 K5 O913 135.4(6) . . ? O26 K5 O913 69.8(6) . . ? O25 K5 O913 73.4(6) 2_866 . ? O933 K5 O913 137.9(14) . . ? O36 K5 O913 72.2(6) . . ? O35 K5 O913 74.3(7) 2_866 . ? O919 K5 O913 147.0(10) . . ? O11 K5 O266 66.6(7) . . ? O26 K5 O266 52.3(7) . . ? O25 K5 O266 115.1(9) 2_866 . ? O933 K5 O266 122.5(14) . . ? O36 K5 O266 52.1(7) . . ? O35 K5 O266 116.0(8) 2_866 . ? O919 K5 O266 120.5(11) . . ? O913 K5 O266 70.2(4) . . ? O11 K5 O255 149.5(9) . 2_866 ? O26 K5 O255 112.6(8) . 2_866 ? O25 K5 O255 52.8(8) 2_866 2_866 ? O933 K5 O255 86.0(15) . 2_866 ? O36 K5 O255 115.7(8) . 2_866 ? O35 K5 O255 50.9(8) 2_866 2_866 ? O919 K5 O255 92.2(11) . 2_866 ? O913 K5 O255 72.1(5) . 2_866 ? O266 K5 O255 142.3(7) . 2_866 ? O11 K5 W25 152.6(6) . 2_866 ? O26 K5 W25 131.7(6) . 2_866 ? O25 K5 W25 22.6(6) 2_866 2_866 ? O933 K5 W25 108.8(14) . 2_866 ? O36 K5 W25 86.5(6) . 2_866 ? O35 K5 W25 80.2(6) 2_866 2_866 ? O919 K5 W25 83.4(9) . 2_866 ? O913 K5 W25 68.30(17) . 2_866 ? O266 K5 W25 128.4(5) . 2_866 ? O255 K5 W25 30.5(5) 2_866 2_866 ? O11 K5 W26 65.9(6) . . ? O26 K5 W26 23.5(6) . . ? O25 K5 W26 137.7(7) 2_866 . ? O933 K5 W26 101.2(14) . . ? O36 K5 W26 81.0(6) . . ? O35 K5 W26 89.4(7) 2_866 . ? O919 K5 W26 134.5(10) . . ? O913 K5 W26 71.29(19) . . ? O266 K5 W26 29.3(4) . . ? O255 K5 W26 131.8(6) 2_866 . ? W25 K5 W26 139.6(3) 2_866 . ? K2 O904 K1 94.6(9) . . ? K2 O904 K4 94.4(8) . 2_865 ? K1 O904 K4 150.0(11) . 2_865 ? K4 O911 K2 100.2(10) . 2_865 ? K5 O913 K5 180.000(1) . 2_866 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W2 O2 1.74(3) . ? W2 O2E 1.78(2) . ? W2 O212 1.93(2) . ? W2 O270 1.98(2) . ? W2 O230 2.09(2) . ? W2 O2P 2.14(2) . ? W2 K4 3.566(10) . ? W2 K1 3.893(9) . ? W3 O3 1.72(3) . ? W3 O230 1.81(2) . ? W3 O313 1.93(3) . ? W3 O340 1.94(3) . ? W3 O370 1.95(3) . ? W3 O3P 2.38(2) . ? W3 K1 3.833(9) 2_865 ? W3 K4 4.106(10) 2_865 ? W4 O4 1.71(2) . ? W4 O480 1.87(2) . ? W4 O340 1.90(2) . ? W4 O450 1.90(2) . ? W4 O414 2.00(2) . ? W4 O3P 2.28(2) . ? W4 K3 3.768(9) . ? W5 O5 1.73(3) . ? W5 O560 1.82(2) . ? W5 O515 1.93(3) . ? W5 O450 1.93(2) . ? W5 O580 1.93(3) . ? W5 O5P 2.39(2) . ? W5 K3 4.076(12) 2_955 ? W6 O6E 1.72(2) . ? W6 O6 1.75(3) . ? W6 O690 1.96(2) . ? W6 O616 1.96(3) . ? W6 O560 2.09(2) . ? W6 O5P 2.32(2) . ? W7 O7 1.72(3) . ? W7 O270 1.86(2) . ? W7 O370 1.88(2) . ? W7 O790 1.88(2) . ? W7 O780 1.94(3) . ? W7 O7P 2.36(2) . ? W7 K1 3.724(8) 2_865 ? W8 O8 1.71(3) . ? W8 O890 1.83(3) . ? W8 O580 1.89(3) . ? W8 O780 1.91(3) . ? W8 O480 1.97(2) . ? W8 O7P 2.40(2) . ? W8 K3 3.840(11) . ? W9 O9 1.72(3) . ? W9 O9E 1.76(2) . ? W9 O690 1.91(2) . ? W9 O790 1.99(3) . ? W9 O890 2.12(3) . ? W9 O7P 2.41(2) . ? W11 O11E 1.72(2) . ? W11 O11 1.74(2) . ? W11 O113 1.92(2) . ? W11 O116 1.92(2) . ? W11 O119 2.11(2) . ? W11 O11P 2.38(2) . ? W12 O12 1.71(3) . ? W12 O212 1.87(2) . ? W12 O113 1.89(2) . ? W12 O128 1.91(2) . ? W12 O123 1.94(2) . ? W12 O11P 2.35(2) . ? W12 K1 3.839(9) . ? W12 K2 4.136(10) . ? W13 O13 1.72(3) . ? W13 O313 1.88(3) . ? W13 O123 1.88(2) . ? W13 O137 1.90(3) . ? W13 O134 1.93(3) . ? W13 O13P 2.39(2) . ? W14 O14 1.71(3) . ? W14 O414 1.82(2) . ? W14 O134 1.90(3) . ? W14 O145 1.92(2) . ? W14 O148 1.95(3) . ? W14 O13P 2.34(2) . ? W15 O15 1.72(3) . ? W15 O515 1.87(3) . ? W15 O145 1.89(2) . ? W15 O157 1.92(3) . ? W15 O158 1.93(3) . ? W15 O15P 2.37(2) . ? W15 K3 3.979(10) 2_955 ? W16 O16 1.70(2) . ? W16 O616 1.83(2) . ? W16 O116 1.88(2) . ? W16 O157 1.95(3) . ? W16 O169 1.98(2) . ? W16 O15P 2.33(2) . ? W17 O17 1.70(3) . ? W17 O128 1.91(2) . ? W17 O179 1.91(2) . ? W17 O178 1.92(3) . ? W17 O137 1.94(3) . ? W17 O17P 2.36(2) . ? W18 O18 1.70(3) . ? W18 O148 1.89(3) . ? W18 O189 1.89(3) . ? W18 O158 1.92(3) . ? W18 O178 1.96(3) . ? W18 O17P 2.35(3) . ? W19 O19 1.72(2) . ? W19 O119 1.83(2) . ? W19 O169 1.88(2) . ? W19 O179 1.94(2) . ? W19 O189 2.01(3) . ? W19 O17P 2.38(2) . ? W22 O22 1.73(4) . ? W22 O22E 1.74(3) . ? W22 O227 1.93(3) . ? W22 O223 2.08(3) . ? W22 O222 2.147(10) . ? W22 O22P 2.34(3) . ? W23 O23 1.69(4) . ? W23 O223 1.83(3) . ? W23 O238 1.897(10) . ? W23 O234 1.95(3) . ? W23 O233 2.157(10) . ? W23 O22P 2.46(3) . ? W24 O24 1.70(4) . ? W24 O248 1.82(3) . ? W24 O234 1.88(3) . ? W24 O245 1.88(3) . ? W24 O244 2.05(3) . ? W24 O24P 2.28(3) . ? W25 O25 1.71(3) . ? W25 O256 1.80(2) . ? W25 O259 1.92(3) . ? W25 O255 1.97(3) . ? W25 O245 1.98(3) . ? W25 O24P 2.34(3) . ? W25 K5 3.884(9) 2_866 ? W26 O26E 1.76(2) . ? W26 O26 1.77(3) . ? W26 O266 1.90(2) . ? W26 O269 1.97(3) . ? W26 O256 2.11(3) . ? W26 O26P 2.14(3) . ? W26 Eu 3.863(2) . ? W26 K5 3.889(10) . ? W27 O27 1.70(4) . ? W27 O27E 1.79(3) . ? W27 O227 1.91(3) . ? W27 O279 1.95(4) . ? W27 O278 2.13(4) . ? W27 O27P 2.46(3) . ? W28 O28 1.69(4) . ? W28 O278 1.78(5) . ? W28 O289 1.91(4) . ? W28 O238 1.96(2) . ? W28 O248 2.01(3) . ? W28 O27P 2.39(3) . ? W29 O29 1.75(3) . ? W29 O269 1.86(3) . ? W29 O279 1.90(4) . ? W29 O259 1.90(3) . ? W29 O289 1.95(4) . ? W29 O27P 2.36(3) . ? W31 O31 1.70(2) . ? W31 O31E 1.74(2) . ? W31 O312 1.90(3) . ? W31 O316 1.92(3) . ? W31 O317 2.09(3) . ? W31 O31P 2.40(3) . ? W31 K4 3.789(9) . ? W32 O222 1.70(2) . ? W32 O32 1.74(4) . ? W32 O312 1.88(3) . ? W32 O323 1.90(4) . ? W32 O327 2.06(3) . ? W32 O32P 2.31(3) . ? W32 K4 3.519(9) . ? W33 O233 1.639(14) . ? W33 O33 1.70(5) . ? W33 O334 1.91(4) . ? W33 O323 1.96(4) . ? W33 O338 2.03(4) . ? W33 O32P 2.33(4) . ? W34 O34 1.71(5) . ? W34 O244 1.79(3) . ? W34 O334 1.86(4) . ? W34 O345 1.89(4) . ? W34 O348 1.96(5) . ? W34 O34P 2.37(3) . ? W35 O35 1.70(3) . ? W35 O255 1.86(3) . ? W35 O345 1.90(4) . ? W35 O356 1.91(3) . ? W35 O359 1.93(3) . ? W35 O34P 2.34(3) . ? W35 K5 3.921(11) 2_866 ? W36 O36 1.70(3) . ? W36 O266 1.88(2) . ? W36 O356 1.90(3) . ? W36 O316 1.91(3) . ? W36 O369 1.95(4) . ? W36 O31P 2.30(3) . ? W36 K5 3.892(12) . ? W37 O37 1.74(4) . ? W37 O327 1.80(3) . ? W37 O317 1.81(3) . ? W37 O378 1.96(4) . ? W37 O379 2.01(4) . ? W37 O37P 2.39(3) . ? W38 O38 1.67(5) . ? W38 O338 1.81(4) . ? W38 O348 1.90(5) . ? W38 O378 1.96(3) . ? W38 O389 2.00(5) . ? W38 O37P 2.34(3) . ? W39 O39 1.79(5) . ? W39 O389 1.86(5) . ? W39 O369 1.89(4) . ? W39 O379 1.90(4) . ? W39 O359 1.92(3) . ? W39 O37P 2.34(3) . ? Eu O2E 2.35(2) . ? Eu O31E 2.36(2) . ? Eu O26E 2.37(2) . ? Eu O27E 2.38(3) . ? Eu O22E 2.40(3) . ? Eu O11E 2.40(2) . ? Eu O9E 2.40(2) . ? Eu O6E 2.41(2) . ? Eu K4 4.727(10) . ? P1 O2P 1.50(3) . ? P1 O3P 1.51(2) . ? P1 O5P 1.53(2) . ? P1 O7P 1.58(3) . ? P2 O15P 1.52(2) . ? P2 O11P 1.53(3) . ? P2 O13P 1.53(2) . ? P2 O17P 1.60(3) . ? P3 O26P 1.50(3) . ? P3 O22P 1.51(4) . ? P3 O27P 1.53(3) . ? P3 O24P 1.57(3) . ? P4 O31P 1.53(3) . ? P4 O32P 1.53(4) . ? P4 O34P 1.56(3) . ? P4 O37P 1.61(4) . ? O2 K4 2.75(3) . ? O2 K1 2.80(3) . ? O3 K4 2.67(3) 2_865 ? O3 K1 2.94(3) 2_865 ? O4 K3 2.84(3) . ? O5 K3 2.92(3) 2_955 ? O7 K2 2.84(3) 2_865 ? O7 K1 2.87(3) 2_865 ? O8 K3 3.04(3) . ? O11 K5 2.69(3) . ? O12 K1 2.76(3) . ? O12 K2 3.13(3) . ? O13 K2 3.26(3) . ? O15 K3 2.81(3) 2_955 ? O25 K5 2.75(3) 2_866 ? O26 K5 2.71(3) . ? O31 K1 2.68(3) . ? O31 K4 3.23(3) . ? O32 K4 2.78(4) . ? O35 K5 2.85(3) 2_866 ? O36 K5 2.84(3) . ? O2E K4 2.95(3) . ? O212 K1 3.26(3) . ? O255 K5 3.33(3) 2_866 ? O266 K5 3.31(3) . ? O312 K4 2.80(3) . ? O370 K1 3.08(3) 2_865 ? O480 K3 3.04(3) . ? K1 O918 2.83(4) . ? K1 O7 2.87(3) 2_865 ? K1 O3 2.94(3) 2_865 ? K1 O904 3.04(3) . ? K1 O370 3.08(3) 2_865 ? K1 W7 3.724(8) 2_865 ? K1 W3 3.833(9) 2_865 ? K2 O904 2.73(3) . ? K2 O911 2.82(3) 2_865 ? K2 O7 2.84(3) 2_865 ? K2 O927 2.85(6) . ? K2 O931 3.16(6) . ? K2 K4 4.260(15) 2_865 ? K3 O910 2.80(3) . ? K3 O15 2.81(3) 2_955 ? K3 O5 2.92(3) 2_955 ? K3 W15 3.979(10) 2_955 ? K3 W5 4.076(12) 2_955 ? K4 O3 2.67(3) 2_865 ? K4 O911 2.73(3) . ? K4 O904 3.07(3) 2_865 ? K4 W3 4.106(10) 2_865 ? K5 O25 2.75(3) 2_866 ? K5 O933 2.83(7) . ? K5 O35 2.85(3) 2_866 ? K5 O919 2.90(5) . ? K5 O913 3.226(9) . ? K5 O255 3.33(3) 2_866 ? K5 W25 3.884(9) 2_866 ? O904 K4 3.07(3) 2_865 ? O905 O924 1.34(6) . ? O911 K2 2.82(3) 2_865 ? O913 K5 3.226(9) 2_866 ?
1100736.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100736.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100736 loop_ _publ_author_name 'Cheng Zhang' 'Robertha C. Howell' 'Qun-Hui Luo' 'Heidi L. Fieselmann' 'Louis J. Todaro' 'Lynn C. Francesconi' _publ_section_title ; Influence of Steric and Electronic Properties of the Defect Site, Lanthanide Ionic Radii, and Solution Conditions on the Composition of Lanthanide(III) \a1-P2W17O6110-Polyoxometalates ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3569 _journal_page_last 3578 _journal_paper_doi 10.1021/ic050103o _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'K14 La O158 P4 W34' _chemical_formula_weight 9589.09 _chemical_name_systematic ; ? ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 104.53(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 41.339(8) _cell_length_b 15.636(3) _cell_length_c 24.988(5) _cell_measurement_temperature 293(2) _cell_volume 15635(6) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0557 _diffrn_reflns_av_sigmaI/netI 0.0661 _diffrn_reflns_limit_h_max 53 _diffrn_reflns_limit_h_min -53 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_number 34400 _diffrn_reflns_theta_full 27.57 _diffrn_reflns_theta_max 27.57 _diffrn_reflns_theta_min 1.40 _exptl_absorpt_coefficient_mu 25.692 _exptl_crystal_density_diffrn 4.074 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 16652 _refine_diff_density_max 10.493 _refine_diff_density_min -7.549 _refine_diff_density_rms 0.997 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 568 _refine_ls_number_reflns 17934 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.070 _refine_ls_R_factor_all 0.1162 _refine_ls_R_factor_gt 0.0744 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1104P)^2^+2917.2334P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1953 _refine_ls_wR_factor_ref 0.2360 _reflns_number_gt 12594 _reflns_number_total 17934 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic050103osi20050113_051630.cif _cod_data_source_block Lanthanum_a1P2W17O61_1to2 _cod_original_cell_volume 15635(5) _cod_database_code 1100736 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.09244(2) 0.10038(7) 1.03130(4) 0.0233(2) Uani 1 1 d . . . W2 W 0.02275(2) 0.07338(7) 0.90275(3) 0.0202(2) Uani 1 1 d . . . W3 W 0.03694(3) 0.28133(7) 0.97872(4) 0.0289(2) Uani 1 1 d . . . W4 W 0.15812(2) 0.22013(8) 1.02124(4) 0.0311(3) Uani 1 1 d . . . W5 W 0.06439(2) -0.03596(7) 0.75190(4) 0.0252(2) Uani 1 1 d . . . W6 W 0.06519(3) -0.12746(7) 0.87213(4) 0.0271(2) Uani 1 1 d . . . W7 W 0.09266(2) 0.28184(8) 0.77711(4) 0.0315(3) Uani 1 1 d . . . W8 W 0.13867(2) 0.09160(9) 0.74297(4) 0.0372(3) Uani 1 1 d . . . W9 W 0.13498(3) -0.09488(8) 0.99606(4) 0.0323(3) Uani 1 1 d . . . W10 W 0.16004(3) 0.31633(10) 0.88759(5) 0.0441(3) Uani 1 1 d . . . W11 W 0.20082(2) 0.02205(10) 0.98638(4) 0.0391(3) Uani 1 1 d . . . W12 W 0.10232(3) 0.40277(8) 0.96772(5) 0.0387(3) Uani 1 1 d . . . La1 La 0.0000 0.16333(13) 0.7500 0.0197(4) Uani 1 2 d S . . W14 W 0.03575(3) 0.36980(7) 0.85322(4) 0.0320(3) Uani 1 1 d . . . W15 W 0.20337(3) 0.12006(11) 0.85343(4) 0.0494(4) Uani 1 1 d . . . W16 W 0.21317(3) -0.11506(12) 0.87055(5) 0.0591(5) Uani 1 1 d . . . W17 W 0.14704(4) -0.23373(10) 0.88149(5) 0.0518(4) Uani 1 1 d . . . W18 W 0.14724(3) -0.14194(11) 0.75775(4) 0.0486(4) Uani 1 1 d . . . P1 P 0.13602(15) -0.0126(5) 0.8656(3) 0.0307(16) Uani 1 1 d . . . P2 P 0.09041(14) 0.1969(5) 0.9054(2) 0.0263(14) Uani 1 1 d . . . O21 O -0.0048(4) 0.1044(11) 0.8395(7) 0.023(3) Uiso 1 1 d . . . O35 O 0.0602(4) 0.0551(10) 0.9748(6) 0.021(3) Uiso 1 1 d . . . O39 O 0.0589(4) 0.2124(11) 0.7603(7) 0.025(3) Uiso 1 1 d . . . O17 O -0.0058(4) 0.0241(11) 0.9329(7) 0.025(3) Uiso 1 1 d . . . O16 O 0.0400(5) -0.2065(13) 0.8863(8) 0.037(4) Uiso 1 1 d . . . O43 O 0.1854(5) 0.1209(13) 0.7764(8) 0.037(4) Uiso 1 1 d . . . O5 O 0.0688(4) 0.2066(10) 1.0255(6) 0.020(3) Uiso 1 1 d . . . O9 O 0.0131(4) 0.2807(12) 0.8188(7) 0.031(4) Uiso 1 1 d . . . O50 O 0.0429(4) -0.0623(11) 0.6854(6) 0.022(3) Uiso 1 1 d . . . O40 O 0.0933(4) -0.1055(11) 0.9437(7) 0.024(3) Uiso 1 1 d . . . O41 O 0.0508(4) -0.1264(11) 0.7948(7) 0.023(3) Uiso 1 1 d . . . O8 O 0.0703(5) 0.3612(13) 0.8156(8) 0.035(4) Uiso 1 1 d . . . O42 O 0.0963(4) 0.0448(11) 0.7369(7) 0.026(4) Uiso 1 1 d . . . O32 O 0.0634(4) 0.1337(11) 0.8793(7) 0.024(3) Uiso 1 1 d . . . O11 O 0.0396(4) -0.0307(10) 0.8802(6) 0.021(3) Uiso 1 1 d . . . O19 O 0.0888(5) 0.3408(13) 0.7176(8) 0.035(4) Uiso 1 1 d . . . O52 O 0.1913(5) 0.2581(14) 1.0725(8) 0.039(5) Uiso 1 1 d . . . O18 O 0.0816(4) 0.0637(12) 1.0891(7) 0.031(4) Uiso 1 1 d . . . O14 O 0.1790(5) 0.1102(12) 1.0139(7) 0.032(4) Uiso 1 1 d . . . O46 O 0.0703(5) 0.4456(14) 0.9106(8) 0.040(5) Uiso 1 1 d . . . O47 O 0.0169(5) 0.3567(12) 0.9177(8) 0.034(4) Uiso 1 1 d . . . O4 O 0.0190(4) 0.1843(11) 0.9380(7) 0.027(4) Uiso 1 1 d . . . O37 O 0.1707(5) 0.2593(13) 0.9584(8) 0.037(4) Uiso 1 1 d . . . O51 O 0.2396(5) 0.0314(13) 1.0324(8) 0.038(4) Uiso 1 1 d . . . O26 O 0.0731(4) 0.2796(11) 0.9198(7) 0.025(4) Uiso 1 1 d . . . O53 O 0.1032(5) -0.1214(13) 0.7497(8) 0.034(4) Uiso 1 1 d . . . O1 O 0.0097(5) 0.2954(13) 1.0207(8) 0.035(4) Uiso 1 1 d . . . O33 O 0.1809(5) -0.0612(13) 1.0242(8) 0.035(4) Uiso 1 1 d . . . O13 O 0.1218(4) 0.0040(11) 1.0240(7) 0.026(4) Uiso 1 1 d . . . O36 O 0.1339(4) 0.1638(11) 1.0656(7) 0.024(3) Uiso 1 1 d . . . O45 O 0.0691(5) 0.3725(12) 1.0055(8) 0.033(4) Uiso 1 1 d . . . O34 O 0.2538(6) -0.1484(17) 0.8816(10) 0.058(6) Uiso 1 1 d . . . O44 O 0.2065(5) 0.0948(14) 0.9282(9) 0.043(5) Uiso 1 1 d . . . O49 O 0.1369(5) 0.1113(13) 0.6753(8) 0.039(5) Uiso 1 1 d . . . O29 O 0.1480(4) 0.0661(12) 0.8374(7) 0.030(4) Uiso 1 1 d . . . O15 O 0.1304(5) -0.1652(14) 1.0469(8) 0.041(5) Uiso 1 1 d . . . O54 O 0.1014(4) -0.2024(12) 0.8656(7) 0.032(4) Uiso 1 1 d . . . O27 O 0.1463(4) -0.0035(12) 0.9291(7) 0.029(4) Uiso 1 1 d . . . O20 O 0.1937(6) 0.3872(16) 0.8973(10) 0.052(6) Uiso 1 1 d . . . O38 O 0.1360(5) 0.3427(13) 0.8179(8) 0.033(4) Uiso 1 1 d . . . O12 O 0.1813(5) 0.2223(13) 0.8581(8) 0.040(5) Uiso 1 1 d . . . O2 O 0.0128(5) 0.4567(14) 0.8208(9) 0.042(5) Uiso 1 1 d . . . O6 O 0.1307(5) 0.3143(13) 1.0149(8) 0.035(4) Uiso 1 1 d . . . O23 O 0.1552(5) -0.0281(13) 0.7430(8) 0.038(5) Uiso 1 1 d . . . O28 O 0.0982(4) -0.0272(11) 0.8441(7) 0.024(3) Uiso 1 1 d . . . O22 O 0.1503(5) -0.1801(13) 0.9506(8) 0.036(4) Uiso 1 1 d . . . O24 O 0.1446(5) -0.2442(15) 0.8041(9) 0.045(5) Uiso 1 1 d . . . O30 O 0.1117(4) 0.2258(11) 0.8660(7) 0.024(3) Uiso 1 1 d . . . O48 O 0.2431(6) 0.1622(15) 0.8559(9) 0.049(5) Uiso 1 1 d . . . O31 O 0.1129(4) 0.1614(11) 0.9598(6) 0.023(3) Uiso 1 1 d . . . O7 O 0.1328(5) 0.3846(13) 0.9209(8) 0.040(5) Uiso 1 1 d . . . O25 O 0.1542(5) -0.0965(13) 0.8502(8) 0.039(5) Uiso 1 1 d . . . O3 O 0.1191(6) 0.4937(16) 1.0031(9) 0.050(5) Uiso 1 1 d . . . O59 O 0.2123(5) -0.0685(14) 0.9412(9) 0.043(5) Uiso 1 1 d . . . O55 O 0.1963(5) -0.1496(14) 0.7968(8) 0.042(5) Uiso 1 1 d . . . O57 O 0.1501(6) -0.1955(16) 0.6986(10) 0.052(6) Uiso 1 1 d . . . O56 O 0.1948(6) -0.2188(15) 0.8936(9) 0.049(5) Uiso 1 1 d . . . O58 O 0.1460(7) -0.3443(18) 0.8982(11) 0.063(7) Uiso 1 1 d . . . O60 O 0.2137(5) -0.0011(14) 0.8475(9) 0.044(5) Uiso 1 1 d . . . O10 O 0.1239(4) 0.1967(12) 0.7620(7) 0.028(4) Uiso 1 1 d . . . K2 K 0.2436(2) 0.1565(9) 1.1188(4) 0.088(3) Uani 1 1 d . . . K1 K -0.0623(3) 0.2823(9) 0.9856(6) 0.106(4) Uani 1 1 d . . . O61 O 0.0384(4) 0.0418(10) 0.7702(6) 0.019(3) Uiso 1 1 d . . . K4 K 0.06700(13) -0.0891(4) 1.1265(2) 0.0320(13) Uani 1 1 d . . . K5 K 0.01881(15) -0.1464(5) 0.5904(2) 0.0368(14) Uani 1 1 d . . . K6 K 0.1119(5) 0.3179(12) 1.1200(7) 0.139(6) Uani 1 1 d . . . O62 O 0.0507(5) -0.2599(15) 1.1214(9) 0.045(5) Uiso 1 1 d . . . O63 O -0.0414(5) 0.1166(13) 0.9937(8) 0.039(5) Uiso 1 1 d . . . O64 O 0.1840(5) 0.0467(14) 1.1366(9) 0.042(5) Uiso 1 1 d . . . O65 O 0.1954(7) 0.3404(18) 1.1778(11) 0.064(7) Uiso 1 1 d . . . O66 O 0.2869(9) -0.084(2) 1.0962(14) 0.090(10) Uiso 1 1 d . . . O67 O 0.0019(10) -0.362(3) 0.8537(16) 0.104(11) Uiso 1 1 d . . . O68 O 0.3079(9) -0.022(2) 1.0385(15) 0.094(10) Uiso 1 1 d . . . O69 O 0.2199(9) -0.224(2) 1.0195(14) 0.092(10) Uiso 1 1 d . . . K7 K 0.0000 -0.254(3) 0.7500 0.29(2) Uani 1 2 d S . . O71 O -0.0533(7) 0.507(2) 0.7726(12) 0.074(8) Uiso 1 1 d . . . O72 O 0.2279(7) -0.002(2) 1.2333(12) 0.069(7) Uiso 1 1 d . . . K8 K 0.2500 0.2500 1.0000 0.28(3) Uani 1 2 d S . . O74 O 0.0595(11) -0.262(3) 0.6599(18) 0.125(14) Uiso 1 1 d . . . O75 O 0.2383(16) 0.198(4) 1.234(2) 0.16(2) Uiso 1 1 d . . . O76 O 0.2145(19) 0.221(5) 1.192(3) 0.20(3) Uiso 1 1 d . . . O77 O 0.1086(11) 0.521(3) 0.8208(17) 0.114(13) Uiso 1 1 d . . . O78 O 0.212(2) -0.115(6) 1.144(4) 0.26(4) Uiso 1 1 d . . . O79 O 0.272(2) 0.012(6) 1.172(3) 0.24(3) Uiso 1 1 d . . . O80 O 0.264(4) 0.141(11) 1.217(6) 0.39(8) Uiso 1 1 d . . . O81 O -0.043(3) 0.436(7) 0.941(4) 0.30(5) Uiso 1 1 d . . . K3 K 0.267(5) 0.406(10) 0.809(8) 0.72(16) Uani 0.63(3) 1 d P . 1 K3 K 0.2815(4) 0.1007(14) 0.9733(7) 0.043(7) Uani 0.37(3) 1 d P . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.0148(4) 0.0402(6) 0.0132(4) -0.0011(4) 0.0003(3) -0.0023(4) W2 0.0118(4) 0.0338(6) 0.0140(4) -0.0007(4) 0.0012(3) -0.0019(4) W3 0.0262(5) 0.0362(6) 0.0210(5) -0.0073(4) -0.0006(4) 0.0049(4) W4 0.0165(4) 0.0534(7) 0.0191(5) 0.0008(4) -0.0037(3) -0.0087(4) W5 0.0187(4) 0.0425(6) 0.0134(4) 0.0012(4) 0.0021(3) 0.0091(4) W6 0.0321(5) 0.0317(6) 0.0156(4) 0.0005(4) 0.0024(4) 0.0060(4) W7 0.0205(5) 0.0476(7) 0.0217(5) 0.0067(4) -0.0031(4) -0.0122(4) W8 0.0134(4) 0.0818(9) 0.0154(5) 0.0047(5) 0.0020(3) 0.0019(5) W9 0.0311(5) 0.0481(7) 0.0148(4) 0.0029(4) 0.0006(4) 0.0132(5) W10 0.0244(5) 0.0769(10) 0.0247(5) 0.0098(5) -0.0058(4) -0.0224(6) W11 0.0179(5) 0.0794(9) 0.0169(5) 0.0028(5) -0.0018(4) 0.0137(5) W12 0.0411(6) 0.0364(7) 0.0288(6) -0.0015(5) -0.0098(5) -0.0090(5) La1 0.0107(7) 0.0303(11) 0.0162(8) 0.000 -0.0004(6) 0.000 W14 0.0339(5) 0.0294(6) 0.0255(5) -0.0015(4) -0.0061(4) 0.0002(4) W15 0.0125(4) 0.1140(13) 0.0197(5) 0.0064(6) 0.0004(4) -0.0033(6) W16 0.0304(6) 0.1203(14) 0.0227(6) -0.0038(7) -0.0009(4) 0.0421(8) W17 0.0607(8) 0.0671(10) 0.0212(5) -0.0017(5) -0.0015(5) 0.0435(7) W18 0.0357(6) 0.0883(11) 0.0189(5) -0.0038(6) 0.0016(4) 0.0370(7) P1 0.016(3) 0.056(5) 0.018(3) -0.001(3) 0.000(2) 0.013(3) P2 0.015(3) 0.049(4) 0.013(3) -0.003(3) -0.001(2) -0.006(3) K2 0.045(5) 0.146(11) 0.066(6) -0.010(6) 0.004(4) -0.012(6) K1 0.063(6) 0.129(11) 0.123(10) -0.049(8) 0.018(6) 0.017(7) K4 0.020(2) 0.053(4) 0.019(2) 0.001(2) -0.0013(19) -0.003(2) K5 0.030(3) 0.055(4) 0.025(3) -0.005(3) 0.005(2) 0.003(3) K6 0.140(14) 0.139(14) 0.135(13) -0.016(11) 0.032(11) 0.010(11) K7 0.34(7) 0.21(4) 0.31(6) 0.000 0.07(5) 0.000 K8 0.16(3) 0.19(4) 0.47(8) -0.08(5) 0.03(4) -0.04(3) K3 0.7(3) 0.5(2) 1.0(4) -0.4(2) 0.5(3) -0.3(2) K3 0.018(8) 0.077(15) 0.027(9) 0.015(8) -0.006(6) -0.025(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O18 W1 O35 103.2(8) . . ? O18 W1 O5 96.8(8) . . ? O35 W1 O5 91.1(7) . . ? O18 W1 O13 96.8(8) . . ? O35 W1 O13 88.8(7) . . ? O5 W1 O13 166.1(7) . . ? O18 W1 O36 100.6(8) . . ? O35 W1 O36 156.1(7) . . ? O5 W1 O36 88.1(7) . . ? O13 W1 O36 86.4(7) . . ? O18 W1 O31 172.4(7) . . ? O35 W1 O31 84.3(6) . . ? O5 W1 O31 82.2(6) . . ? O13 W1 O31 83.9(6) . . ? O36 W1 O31 71.9(6) . . ? O18 W1 K5 47.7(6) . 6_556 ? O35 W1 K5 82.7(5) . 6_556 ? O5 W1 K5 54.4(5) . 6_556 ? O13 W1 K5 139.2(5) . 6_556 ? O36 W1 K5 115.5(5) . 6_556 ? O31 W1 K5 134.2(4) . 6_556 ? O18 W1 K6 82.9(7) . . ? O35 W1 K6 139.5(6) . . ? O5 W1 K6 48.4(5) . . ? O13 W1 K6 130.8(6) . . ? O36 W1 K6 46.1(6) . . ? O31 W1 K6 90.9(5) . . ? K5 W1 K6 72.1(3) 6_556 . ? O18 W1 K4 27.1(6) . . ? O35 W1 K4 85.7(5) . . ? O5 W1 K4 118.1(5) . . ? O13 W1 K4 75.8(5) . . ? O36 W1 K4 115.5(5) . . ? O31 W1 K4 157.5(4) . . ? K5 W1 K4 63.93(13) 6_556 . ? K6 W1 K4 109.6(3) . . ? O17 W2 O21 98.9(8) . . ? O17 W2 O11 95.0(7) . . ? O21 W2 O11 99.8(7) . . ? O17 W2 O4 93.4(7) . . ? O21 W2 O4 93.1(7) . . ? O11 W2 O4 163.3(7) . . ? O17 W2 O35 90.2(7) . . ? O21 W2 O35 169.8(7) . . ? O11 W2 O35 83.7(6) . . ? O4 W2 O35 81.9(7) . . ? O17 W2 O32 170.3(7) . . ? O21 W2 O32 90.4(7) . . ? O11 W2 O32 85.7(7) . . ? O4 W2 O32 83.6(7) . . ? O35 W2 O32 80.3(6) . . ? O17 W2 K4 48.7(6) . 5_557 ? O21 W2 K4 53.2(5) . 5_557 ? O11 W2 K4 115.6(5) . 5_557 ? O4 W2 K4 80.7(5) . 5_557 ? O35 W2 K4 133.7(4) . 5_557 ? O32 W2 K4 139.1(5) . 5_557 ? O17 W2 K5 39.3(6) . 2_556 ? O21 W2 K5 95.2(6) . 2_556 ? O11 W2 K5 57.0(5) . 2_556 ? O4 W2 K5 132.7(5) . 2_556 ? O35 W2 K5 94.8(5) . 2_556 ? O32 W2 K5 142.6(5) . 2_556 ? K4 W2 K5 67.87(14) 5_557 2_556 ? O1 W3 O4 101.7(8) . . ? O1 W3 O5 99.1(8) . . ? O4 W3 O5 87.5(7) . . ? O1 W3 O47 100.6(8) . . ? O4 W3 O47 91.8(8) . . ? O5 W3 O47 160.0(7) . . ? O1 W3 O45 100.9(9) . . ? O4 W3 O45 157.2(8) . . ? O5 W3 O45 86.1(7) . . ? O47 W3 O45 86.9(8) . . ? O1 W3 O26 173.3(8) . . ? O4 W3 O26 83.0(7) . . ? O5 W3 O26 85.8(6) . . ? O47 W3 O26 74.3(7) . . ? O45 W3 O26 74.8(7) . . ? O1 W3 K5 48.3(7) . 6_556 ? O4 W3 K5 79.7(5) . 6_556 ? O5 W3 K5 55.7(5) . 6_556 ? O47 W3 K5 143.8(6) . 6_556 ? O45 W3 K5 113.9(6) . 6_556 ? O26 W3 K5 138.0(4) . 6_556 ? O1 W3 K6 85.8(7) . . ? O4 W3 K6 133.6(6) . . ? O5 W3 K6 46.2(5) . . ? O47 W3 K6 132.2(6) . . ? O45 W3 K6 45.7(6) . . ? O26 W3 K6 94.5(5) . . ? K5 W3 K6 71.6(3) 6_556 . ? O52 W4 O6 98.4(9) . . ? O52 W4 O37 100.0(9) . . ? O6 W4 O37 87.7(8) . . ? O52 W4 O36 99.5(8) . . ? O6 W4 O36 91.0(8) . . ? O37 W4 O36 160.5(8) . . ? O52 W4 O14 94.9(9) . . ? O6 W4 O14 166.7(8) . . ? O37 W4 O14 89.3(8) . . ? O36 W4 O14 87.5(7) . . ? O52 W4 O31 174.4(8) . . ? O6 W4 O31 83.2(7) . . ? O37 W4 O31 85.5(7) . . ? O36 W4 O31 75.0(6) . . ? O14 W4 O31 83.7(7) . . ? O52 W4 K3 46.9(7) . 7_557 ? O6 W4 K3 78.1(7) . 7_557 ? O37 W4 K3 57.5(7) . 7_557 ? O36 W4 K3 141.0(6) . 7_557 ? O14 W4 K3 110.9(6) . 7_557 ? O31 W4 K3 138.7(5) . 7_557 ? O52 W4 K6 79.4(7) . . ? O6 W4 K6 48.4(6) . . ? O37 W4 K6 134.6(7) . . ? O36 W4 K6 51.6(6) . . ? O14 W4 K6 136.1(6) . . ? O31 W4 K6 97.9(5) . . ? K3 W4 K6 96.6(4) 7_557 . ? O52 W4 K2 36.5(7) . . ? O6 W4 K2 134.6(6) . . ? O37 W4 K2 102.1(6) . . ? O36 W4 K2 92.6(5) . . ? O14 W4 K2 58.6(6) . . ? O31 W4 K2 141.1(5) . . ? K3 W4 K2 71.0(3) 7_557 . ? K6 W4 K2 102.8(3) . . ? O52 W4 K8 56.9(7) . . ? O6 W4 K8 118.7(6) . . ? O37 W4 K8 51.6(6) . . ? O36 W4 K8 142.7(5) . . ? O14 W4 K8 68.4(5) . . ? O31 W4 K8 127.0(4) . . ? K3 W4 K8 42.9(3) 7_557 . ? K6 W4 K8 133.6(3) . . ? K2 W4 K8 50.78(17) . . ? O50 W5 O61 102.4(7) . . ? O50 W5 O42 100.5(7) . . ? O61 W5 O42 95.2(7) . . ? O50 W5 O41 101.9(7) . . ? O61 W5 O41 94.5(7) . . ? O42 W5 O41 153.0(7) . . ? O50 W5 O53 92.0(7) . . ? O61 W5 O53 165.6(7) . . ? O42 W5 O53 81.2(7) . . ? O41 W5 O53 83.2(7) . . ? O50 W5 O28 168.8(7) . . ? O61 W5 O28 87.5(6) . . ? O42 W5 O28 83.5(6) . . ? O41 W5 O28 71.8(6) . . ? O53 W5 O28 78.2(6) . . ? O50 W5 K4 55.4(5) . 6 ? O61 W5 K4 90.3(5) . 6 ? O42 W5 K4 47.7(5) . 6 ? O41 W5 K4 157.3(5) . 6 ? O53 W5 K4 97.4(5) . 6 ? O28 W5 K4 130.7(4) . 6 ? O16 W6 O41 99.6(8) . . ? O16 W6 O11 99.8(8) . . ? O41 W6 O11 93.5(7) . . ? O16 W6 O40 101.3(8) . . ? O41 W6 O40 158.2(7) . . ? O11 W6 O40 88.9(7) . . ? O16 W6 O54 95.9(9) . . ? O41 W6 O54 88.3(7) . . ? O11 W6 O54 163.6(7) . . ? O40 W6 O54 83.5(7) . . ? O16 W6 O28 174.0(8) . . ? O41 W6 O28 74.8(6) . . ? O11 W6 O28 82.9(6) . . ? O40 W6 O28 84.0(7) . . ? O54 W6 O28 81.8(7) . . ? O16 W6 K5 42.0(7) . 2_556 ? O41 W6 K5 100.4(5) . 2_556 ? O11 W6 K5 57.9(5) . 2_556 ? O40 W6 K5 99.3(5) . 2_556 ? O54 W6 K5 137.8(6) . 2_556 ? O28 W6 K5 140.4(4) . 2_556 ? O16 W6 K7 58.4(8) . . ? O41 W6 K7 41.2(7) . . ? O11 W6 K7 100.9(7) . . ? O40 W6 K7 158.6(8) . . ? O54 W6 K7 91.3(7) . . ? O28 W6 K7 115.9(6) . . ? K5 W6 K7 70.94(12) 2_556 . ? O19 W7 O39 103.3(8) . . ? O19 W7 O8 97.6(9) . . ? O39 W7 O8 93.9(8) . . ? O19 W7 O10 97.0(8) . . ? O39 W7 O10 93.2(8) . . ? O8 W7 O10 161.9(7) . . ? O19 W7 O38 93.5(8) . . ? O39 W7 O38 163.1(8) . . ? O8 W7 O38 85.5(8) . . ? O10 W7 O38 82.8(7) . . ? O19 W7 O30 163.5(8) . . ? O39 W7 O30 93.1(7) . . ? O8 W7 O30 81.8(7) . . ? O10 W7 O30 81.1(6) . . ? O38 W7 O30 70.0(7) . . ? O49 W8 O10 99.2(9) . . ? O49 W8 O42 100.6(9) . . ? O10 W8 O42 90.3(8) . . ? O49 W8 O43 100.0(9) . . ? O10 W8 O43 92.1(8) . . ? O42 W8 O43 158.6(8) . . ? O49 W8 O23 95.7(9) . . ? O10 W8 O23 165.1(8) . . ? O42 W8 O23 87.0(8) . . ? O43 W8 O23 85.3(8) . . ? O49 W8 O29 173.3(8) . . ? O10 W8 O29 82.7(7) . . ? O42 W8 O29 85.9(7) . . ? O43 W8 O29 73.4(7) . . ? O23 W8 O29 82.5(7) . . ? O49 W8 K4 51.4(7) . 6 ? O10 W8 K4 87.7(5) . 6 ? O42 W8 K4 50.6(5) . 6 ? O43 W8 K4 150.8(6) . 6 ? O23 W8 K4 101.7(6) . 6 ? O29 W8 K4 135.4(4) . 6 ? O15 W9 O13 99.1(9) . . ? O15 W9 O40 101.8(9) . . ? O13 W9 O40 91.8(7) . . ? O15 W9 O33 100.7(9) . . ? O13 W9 O33 89.5(8) . . ? O40 W9 O33 157.0(8) . . ? O15 W9 O22 96.0(9) . . ? O13 W9 O22 164.9(8) . . ? O40 W9 O22 84.8(8) . . ? O33 W9 O22 88.0(8) . . ? O15 W9 O27 174.8(8) . . ? O13 W9 O27 83.7(7) . . ? O40 W9 O27 82.5(7) . . ? O33 W9 O27 74.8(7) . . ? O22 W9 O27 81.3(7) . . ? O20 W10 O38 102.3(10) . . ? O20 W10 O7 97.1(10) . . ? O38 W10 O7 92.9(9) . . ? O20 W10 O37 100.1(10) . . ? O38 W10 O37 157.6(9) . . ? O7 W10 O37 83.2(9) . . ? O20 W10 O12 96.4(10) . . ? O38 W10 O12 89.9(8) . . ? O7 W10 O12 165.3(9) . . ? O37 W10 O12 88.7(8) . . ? O20 W10 O30 174.6(9) . . ? O38 W10 O30 72.2(7) . . ? O7 W10 O30 83.0(8) . . ? O37 W10 O30 85.3(7) . . ? O12 W10 O30 84.1(7) . . ? O20 W10 K3 51.3(8) . 7_557 ? O38 W10 K3 147.0(7) . 7_557 ? O7 W10 K3 74.1(7) . 7_557 ? O37 W10 K3 52.6(7) . 7_557 ? O12 W10 K3 110.4(7) . 7_557 ? O30 W10 K3 133.5(4) . 7_557 ? O20 W10 K2 35.1(8) . 7_557 ? O38 W10 K2 104.2(6) . 7_557 ? O7 W10 K2 131.2(7) . 7_557 ? O37 W10 K2 94.9(6) . 7_557 ? O12 W10 K2 61.5(6) . 7_557 ? O30 W10 K2 145.6(4) . 7_557 ? K3 W10 K2 66.9(3) 7_557 7_557 ? O51 W11 O14 98.3(9) . . ? O51 W11 O44 100.7(9) . . ? O14 W11 O44 90.3(9) . . ? O51 W11 O33 99.8(9) . . ? O14 W11 O33 90.7(8) . . ? O44 W11 O33 159.1(9) . . ? O51 W11 O59 97.3(9) . . ? O14 W11 O59 164.1(8) . . ? O44 W11 O59 84.1(9) . . ? O33 W11 O59 89.4(9) . . ? O51 W11 O27 173.7(8) . . ? O14 W11 O27 82.8(7) . . ? O44 W11 O27 85.5(8) . . ? O33 W11 O27 73.9(7) . . ? O59 W11 O27 82.0(8) . . ? O51 W11 K3 46.8(7) . . ? O14 W11 K3 108.7(7) . . ? O44 W11 K3 55.9(7) . . ? O33 W11 K3 142.3(6) . . ? O59 W11 K3 80.3(7) . . ? O27 W11 K3 138.8(5) . . ? O51 W11 K2 41.5(7) . . ? O14 W11 K2 56.9(6) . . ? O44 W11 K2 101.9(7) . . ? O33 W11 K2 96.1(6) . . ? O59 W11 K2 138.8(6) . . ? O27 W11 K2 138.7(5) . . ? K3 W11 K2 70.6(3) . . ? O51 W11 K8 60.7(7) . . ? O14 W11 K8 66.5(6) . . ? O44 W11 K8 52.2(7) . . ? O33 W11 K8 145.3(6) . . ? O59 W11 K8 119.8(6) . . ? O27 W11 K8 125.1(4) . . ? K3 W11 K8 42.6(4) . . ? K2 W11 K8 49.80(19) . . ? O3 W12 O46 102.7(10) . . ? O3 W12 O45 101.5(10) . . ? O46 W12 O45 90.4(9) . . ? O3 W12 O7 100.9(10) . . ? O46 W12 O7 92.1(9) . . ? O45 W12 O7 156.3(9) . . ? O3 W12 O6 99.6(10) . . ? O46 W12 O6 157.7(9) . . ? O45 W12 O6 85.8(8) . . ? O7 W12 O6 83.1(8) . . ? O3 W12 O26 174.0(9) . . ? O46 W12 O26 74.4(8) . . ? O45 W12 O26 73.5(7) . . ? O7 W12 O26 84.5(7) . . ? O6 W12 O26 83.5(7) . . ? O3 W12 K6 81.6(8) . . ? O46 W12 K6 139.3(7) . . ? O45 W12 K6 49.7(6) . . ? O7 W12 K6 127.3(7) . . ? O6 W12 K6 45.4(6) . . ? O26 W12 K6 97.2(5) . . ? O61 La1 O61 78.0(7) . 2_556 ? O61 La1 O21 72.7(5) . 2_556 ? O61 La1 O21 73.6(5) 2_556 2_556 ? O61 La1 O21 73.6(5) . . ? O61 La1 O21 72.7(5) 2_556 . ? O21 La1 O21 136.2(8) 2_556 . ? O61 La1 O9 114.4(6) . . ? O61 La1 O9 137.4(5) 2_556 . ? O21 La1 O9 148.2(6) 2_556 . ? O21 La1 O9 72.6(6) . . ? O61 La1 O9 137.4(5) . 2_556 ? O61 La1 O9 114.4(6) 2_556 2_556 ? O21 La1 O9 72.6(6) 2_556 2_556 ? O21 La1 O9 148.2(6) . 2_556 ? O9 La1 O9 84.6(8) . 2_556 ? O61 La1 O39 69.7(5) . . ? O61 La1 O39 145.3(5) 2_556 . ? O21 La1 O39 84.9(5) 2_556 . ? O21 La1 O39 108.5(5) . . ? O9 La1 O39 70.4(6) . . ? O9 La1 O39 83.3(6) 2_556 . ? O61 La1 O39 145.3(5) . 2_556 ? O61 La1 O39 69.7(5) 2_556 2_556 ? O21 La1 O39 108.5(5) 2_556 2_556 ? O21 La1 O39 84.9(5) . 2_556 ? O9 La1 O39 83.3(6) . 2_556 ? O9 La1 O39 70.4(6) 2_556 2_556 ? O39 La1 O39 144.4(8) . 2_556 ? O2 W14 O9 103.2(9) . . ? O2 W14 O8 102.4(9) . . ? O9 W14 O8 94.3(8) . . ? O2 W14 O47 100.4(9) . . ? O9 W14 O47 92.6(8) . . ? O8 W14 O47 153.9(8) . . ? O2 W14 O46 94.3(9) . . ? O9 W14 O46 162.2(8) . . ? O8 W14 O46 84.9(8) . . ? O47 W14 O46 81.0(8) . . ? O2 W14 O26 163.1(8) . . ? O9 W14 O26 92.5(7) . . ? O8 W14 O26 82.5(7) . . ? O47 W14 O26 72.1(7) . . ? O46 W14 O26 69.8(7) . . ? O48 W15 O12 98.3(10) . . ? O48 W15 O44 102.3(10) . . ? O12 W15 O44 91.8(9) . . ? O48 W15 O43 99.1(9) . . ? O12 W15 O43 89.1(9) . . ? O44 W15 O43 158.2(9) . . ? O48 W15 O60 98.5(10) . . ? O12 W15 O60 163.2(9) . . ? O44 W15 O60 84.8(9) . . ? O43 W15 O60 88.1(9) . . ? O48 W15 O29 172.5(8) . . ? O12 W15 O29 81.3(8) . . ? O44 W15 O29 85.2(8) . . ? O43 W15 O29 73.4(7) . . ? O60 W15 O29 82.1(8) . . ? O48 W15 K3 53.4(8) . . ? O12 W15 K3 110.5(7) . . ? O44 W15 K3 51.1(7) . . ? O43 W15 K3 147.2(7) . . ? O60 W15 K3 79.9(7) . . ? O29 W15 K3 133.8(5) . . ? O48 W15 K2 38.4(8) . 7_557 ? O12 W15 K2 60.4(7) . 7_557 ? O44 W15 K2 96.3(7) . 7_557 ? O43 W15 K2 103.0(6) . 7_557 ? O60 W15 K2 136.3(7) . 7_557 ? O29 W15 K2 141.6(5) . 7_557 ? K3 W15 K2 67.9(3) . 7_557 ? O34 W16 O60 104.7(11) . . ? O34 W16 O55 100.3(11) . . ? O60 W16 O55 90.1(9) . . ? O34 W16 O59 102.2(11) . . ? O60 W16 O59 85.8(9) . . ? O55 W16 O59 157.5(9) . . ? O34 W16 O56 98.0(11) . . ? O60 W16 O56 157.2(9) . . ? O55 W16 O56 88.5(9) . . ? O59 W16 O56 86.8(9) . . ? O34 W16 O25 169.0(10) . . ? O60 W16 O25 84.7(8) . . ? O55 W16 O25 73.5(8) . . ? O59 W16 O25 84.0(8) . . ? O56 W16 O25 73.1(9) . . ? O58 W17 O54 102.7(10) . . ? O58 W17 O22 102.5(10) . . ? O54 W17 O22 85.2(8) . . ? O58 W17 O24 98.9(11) . . ? O54 W17 O24 90.7(8) . . ? O22 W17 O24 158.5(9) . . ? O58 W17 O56 99.4(11) . . ? O54 W17 O56 157.8(9) . . ? O22 W17 O56 88.1(9) . . ? O24 W17 O56 87.8(9) . . ? O58 W17 O25 170.3(10) . . ? O54 W17 O25 84.0(8) . . ? O22 W17 O25 84.9(8) . . ? O24 W17 O25 73.7(9) . . ? O56 W17 O25 74.4(9) . . ? O57 W18 O53 105.8(10) . . ? O57 W18 O23 103.9(10) . . ? O53 W18 O23 91.8(9) . . ? O57 W18 O24 97.7(10) . . ? O53 W18 O24 90.4(9) . . ? O23 W18 O24 156.8(9) . . ? O57 W18 O55 96.3(10) . . ? O53 W18 O55 157.5(8) . . ? O23 W18 O55 86.9(9) . . ? O24 W18 O55 82.3(9) . . ? O57 W18 O25 164.4(10) . . ? O53 W18 O25 85.9(8) . . ? O23 W18 O25 85.5(8) . . ? O24 W18 O25 71.6(8) . . ? O55 W18 O25 71.6(8) . . ? O28 P1 O27 111.4(10) . . ? O28 P1 O29 111.7(10) . . ? O27 P1 O29 110.9(11) . . ? O28 P1 O25 106.9(11) . . ? O27 P1 O25 107.3(10) . . ? O29 P1 O25 108.4(10) . . ? O32 P2 O30 113.3(9) . . ? O32 P2 O31 111.2(10) . . ? O30 P2 O31 110.7(9) . . ? O32 P2 O26 108.0(10) . . ? O30 P2 O26 105.8(10) . . ? O31 P2 O26 107.6(9) . . ? W2 O21 La1 137.1(8) . . ? W2 O21 K4 97.7(6) . 5_557 ? La1 O21 K4 124.8(6) . 5_557 ? W1 O35 W2 149.1(9) . . ? W7 O39 La1 156.7(9) . . ? W2 O17 K5 117.2(8) . 2_556 ? W2 O17 K4 103.4(7) . 5_557 ? K5 O17 K4 97.9(5) 2_556 5_557 ? W6 O16 K5 113.9(9) . 2_556 ? W6 O16 K1 114.9(9) . 5_557 ? K5 O16 K1 88.0(5) 2_556 5_557 ? W15 O43 W8 121.9(10) . . ? W1 O5 W3 146.3(9) . . ? W1 O5 K5 95.3(6) . 6_556 ? W3 O5 K5 93.3(6) . 6_556 ? W1 O5 K6 104.1(7) . . ? W3 O5 K6 107.3(7) . . ? K5 O5 K6 95.9(6) 6_556 . ? W14 O9 La1 156.0(10) . . ? W5 O50 K5 163.3(9) . . ? W5 O50 K4 97.2(7) . 6 ? K5 O50 K4 92.6(5) . 6 ? W9 O40 W6 154.3(10) . . ? W6 O41 W5 121.0(9) . . ? W6 O41 K7 113.7(8) . . ? W5 O41 K7 124.6(8) . . ? W14 O8 W7 143.2(11) . . ? W8 O42 W5 155.9(10) . . ? W8 O42 K4 98.5(7) . 6 ? W5 O42 K4 101.8(7) . 6 ? P2 O32 W2 136.0(10) . . ? W6 O11 W2 166.2(9) . . ? W6 O11 K5 92.7(6) . 2_556 ? W2 O11 K5 93.5(6) . 2_556 ? W4 O52 K2 121.1(10) . . ? W4 O52 K3 106.8(9) . 7_557 ? K2 O52 K3 105.9(8) . 7_557 ? W4 O52 K8 97.7(8) . . ? K2 O52 K8 66.5(5) . . ? K3 O52 K8 53.4(5) 7_557 . ? W1 O18 K4 136.0(9) . . ? W1 O18 K5 106.4(8) . 6_556 ? K4 O18 K5 96.4(6) . 6_556 ? W11 O14 W4 161.5(11) . . ? W11 O14 K2 94.9(7) . . ? W4 O14 K2 91.2(7) . . ? W12 O46 W14 124.2(11) . . ? W3 O47 W14 121.8(10) . . ? W3 O4 W2 153.1(10) . . ? W4 O37 W10 150.5(11) . . ? W4 O37 K3 92.3(8) . 7_557 ? W10 O37 K3 98.2(8) . 7_557 ? W4 O37 K8 101.0(7) . . ? W10 O37 K8 107.4(8) . . ? K3 O37 K8 53.1(5) 7_557 . ? W11 O51 K3 106.1(9) . . ? W11 O51 K2 115.1(9) . . ? K3 O51 K2 102.0(8) . . ? P2 O26 W3 123.7(10) . . ? P2 O26 W14 125.0(9) . . ? W3 O26 W14 91.5(6) . . ? P2 O26 W12 124.9(9) . . ? W3 O26 W12 89.9(6) . . ? W14 O26 W12 91.7(6) . . ? W18 O53 W5 149.8(11) . . ? W3 O1 K5 104.9(9) . 6_556 ? W3 O1 K1 125.6(9) . . ? K5 O1 K1 95.4(7) 6_556 . ? W11 O33 W9 120.9(10) . . ? W9 O13 W1 158.1(10) . . ? W4 O36 W1 120.6(8) . . ? W4 O36 K6 99.0(8) . . ? W1 O36 K6 105.6(7) . . ? W12 O45 W3 121.6(10) . . ? W12 O45 K6 102.1(8) . . ? W3 O45 K6 107.4(8) . . ? W15 O44 W11 153.0(13) . . ? W15 O44 K3 100.0(9) . . ? W11 O44 K3 92.6(8) . . ? W15 O44 K8 106.3(9) . . ? W11 O44 K8 100.4(8) . . ? K3 O44 K8 53.3(6) . . ? W8 O49 K4 100.9(9) . 6 ? P1 O29 W8 127.1(10) . . ? P1 O29 W15 127.2(10) . . ? W8 O29 W15 91.0(6) . . ? W9 O15 K1 114.7(9) . 5_557 ? W17 O54 W6 152.6(11) . . ? P1 O27 W9 128.9(11) . . ? P1 O27 W11 127.4(10) . . ? W9 O27 W11 90.1(6) . . ? W10 O20 K2 123.9(12) . 7_557 ? W10 O20 K3 102.9(10) . 7_557 ? K2 O20 K3 95.1(8) 7_557 7_557 ? W10 O38 W7 124.5(10) . . ? W15 O12 W10 161.2(12) . . ? W4 O6 W12 149.7(11) . . ? W4 O6 K6 103.6(9) . . ? W12 O6 K6 105.6(8) . . ? W18 O23 W8 145.0(11) . . ? P1 O28 W6 128.6(10) . . ? P1 O28 W5 130.2(9) . . ? W6 O28 W5 90.4(6) . . ? W17 O22 W9 150.6(11) . . ? W17 O24 W18 121.4(12) . . ? P2 O30 W7 127.3(9) . . ? P2 O30 W10 127.3(9) . . ? W7 O30 W10 93.2(6) . . ? W15 O48 K2 119.7(11) . 7_557 ? W15 O48 K3 99.7(9) . . ? K2 O48 K3 94.1(8) 7_557 . ? P2 O31 W4 130.9(10) . . ? P2 O31 W1 124.1(9) . . ? W4 O31 W1 92.4(6) . . ? W10 O7 W12 153.6(12) . . ? P1 O25 W17 124.5(11) . . ? P1 O25 W18 122.0(11) . . ? W17 O25 W18 93.2(7) . . ? P1 O25 W16 124.4(11) . . ? W17 O25 W16 91.5(7) . . ? W18 O25 W16 92.3(7) . . ? W16 O59 W11 151.0(12) . . ? W16 O55 W18 122.5(11) . . ? W18 O57 K6 139.0(12) . 6 ? W17 O56 W16 121.0(12) . . ? W16 O60 W15 151.5(12) . . ? W8 O10 W7 158.0(10) . . ? K3 K2 O80 37(4) 7_557 . ? K3 K2 O76 51(5) 7_557 . ? O80 K2 O76 55(4) . . ? K3 K2 O52 108(5) 7_557 . ? O80 K2 O52 122(4) . . ? O76 K2 O52 67.6(19) . . ? K3 K2 O79 52(5) 7_557 . ? O80 K2 O79 55(5) . . ? O76 K2 O79 101(3) . . ? O52 K2 O79 153(2) . . ? K3 K2 O20 113(5) 7_557 7_557 ? O80 K2 O20 92(4) . 7_557 ? O76 K2 O20 142.4(19) . 7_557 ? O52 K2 O20 138.7(8) . 7_557 ? O79 K2 O20 64.6(19) . 7_557 ? K3 K2 O51 109(3) 7_557 . ? O80 K2 O51 130(4) . . ? O76 K2 O51 146.1(18) . . ? O52 K2 O51 100.9(7) . . ? O79 K2 O51 74.9(19) . . ? O20 K2 O51 67.0(7) 7_557 . ? K3 K2 O48 109(3) 7_557 7_557 ? O80 K2 O48 83(4) . 7_557 ? O76 K2 O48 64.8(18) . 7_557 ? O52 K2 O48 67.0(7) . 7_557 ? O79 K2 O48 131.6(19) . 7_557 ? O20 K2 O48 97.8(7) 7_557 7_557 ? O51 K2 O48 142.2(7) . 7_557 ? K3 K2 O75 40(4) 7_557 . ? O80 K2 O75 30(4) . . ? O76 K2 O75 25.2(17) . . ? O52 K2 O75 92.3(14) . . ? O79 K2 O75 81(2) . . ? O20 K2 O75 118.8(14) 7_557 . ? O51 K2 O75 149.0(14) . . ? O48 K2 O75 68.8(13) 7_557 . ? K3 K2 O64 46(4) 7_557 . ? O80 K2 O64 83(4) . . ? O76 K2 O64 66.2(18) . . ? O52 K2 O64 79.0(6) . . ? O79 K2 O64 74.4(19) . . ? O20 K2 O64 132.5(8) 7_557 . ? O51 K2 O64 80.5(6) . . ? O48 K2 O64 127.9(7) 7_557 . ? O75 K2 O64 74.6(12) . . ? K3 K2 O14 105(4) 7_557 . ? O80 K2 O14 142(4) . . ? O76 K2 O14 102.6(18) . . ? O52 K2 O14 52.4(6) . . ? O79 K2 O14 111.3(19) . . ? O20 K2 O14 115.0(7) 7_557 . ? O51 K2 O14 51.5(5) . . ? O48 K2 O14 116.9(7) 7_557 . ? O75 K2 O14 124.4(13) . . ? O64 K2 O14 59.0(5) . . ? K3 K2 K8 173(5) 7_557 . ? O80 K2 K8 149(4) . . ? O76 K2 K8 126.8(18) . . ? O52 K2 K8 66.4(5) . . ? O79 K2 K8 131.9(19) . . ? O20 K2 K8 72.6(5) 7_557 . ? O51 K2 K8 68.8(5) . . ? O48 K2 K8 73.7(5) 7_557 . ? O75 K2 K8 141.8(13) . . ? O64 K2 K8 126.9(5) . . ? O14 K2 K8 68.0(4) . . ? O63 K1 O81 136(2) . . ? O63 K1 O62 80.1(7) . 5_557 ? O81 K1 O62 67(2) . 5_557 ? O63 K1 O1 76.2(7) . . ? O81 K1 O1 72(2) . . ? O62 K1 O1 83.7(7) 5_557 . ? O63 K1 O15 74.0(7) . 5_557 ? O81 K1 O15 133(2) . 5_557 ? O62 K1 O15 92.0(7) 5_557 5_557 ? O1 K1 O15 150.2(7) . 5_557 ? O63 K1 O16 65.3(6) . 5_557 ? O81 K1 O16 130(2) . 5_557 ? O62 K1 O16 142.1(7) 5_557 5_557 ? O1 K1 O16 73.6(6) . 5_557 ? O15 K1 O16 93.1(6) 5_557 5_557 ? O63 K1 K4 46.2(5) . 5_557 ? O81 K1 K4 109(2) . 5_557 ? O62 K1 K4 42.1(5) 5_557 5_557 ? O1 K1 K4 97.4(5) . 5_557 ? O15 K1 K4 61.9(4) 5_557 5_557 ? O16 K1 K4 110.6(5) 5_557 5_557 ? O63 K1 K5 45.1(5) . 6_556 ? O81 K1 K5 114(2) . 6_556 ? O62 K1 K5 102.9(5) 5_557 6_556 ? O1 K1 K5 42.1(4) . 6_556 ? O15 K1 K5 111.5(6) 5_557 6_556 ? O16 K1 K5 41.0(4) 5_557 6_556 ? K4 K1 K5 87.0(3) 5_557 6_556 ? W5 O61 La1 153.0(8) . . ? O18 K4 O62 157.0(6) . . ? O18 K4 O17 75.1(5) . 5_557 ? O62 K4 O17 98.7(6) . 5_557 ? O18 K4 O42 92.5(6) . 6_556 ? O62 K4 O42 109.0(6) . 6_556 ? O17 K4 O42 123.0(5) 5_557 6_556 ? O18 K4 O49 88.0(6) . 6_556 ? O62 K4 O49 96.4(6) . 6_556 ? O17 K4 O49 163.1(6) 5_557 6_556 ? O42 K4 O49 58.0(5) 6_556 6_556 ? O18 K4 O21 117.8(6) . 5_557 ? O62 K4 O21 73.1(6) . 5_557 ? O17 K4 O21 55.6(5) 5_557 5_557 ? O42 K4 O21 85.9(5) 6_556 5_557 ? O49 K4 O21 137.4(5) 6_556 5_557 ? O18 K4 O63 80.2(6) . 5_557 ? O62 K4 O63 77.9(6) . 5_557 ? O17 K4 O63 57.7(5) 5_557 5_557 ? O42 K4 O63 172.3(6) 6_556 5_557 ? O49 K4 O63 118.8(6) 6_556 5_557 ? O21 K4 O63 99.6(5) 5_557 5_557 ? O18 K4 O50 67.2(5) . 6_556 ? O62 K4 O50 131.6(6) . 6_556 ? O17 K4 O50 67.4(5) 5_557 6_556 ? O42 K4 O50 56.8(5) 6_556 6_556 ? O49 K4 O50 107.6(5) 6_556 6_556 ? O21 K4 O50 60.6(5) 5_557 6_556 ? O63 K4 O50 121.4(5) 5_557 6_556 ? O18 K4 W8 94.6(4) . 6_556 ? O62 K4 W8 99.7(5) . 6_556 ? O17 K4 W8 152.9(4) 5_557 6_556 ? O42 K4 W8 30.9(3) 6_556 6_556 ? O49 K4 W8 27.7(4) 6_556 6_556 ? O21 K4 W8 111.8(4) 5_557 6_556 ? O63 K4 W8 146.4(4) 5_557 6_556 ? O50 K4 W8 85.5(3) 6_556 6_556 ? O18 K4 W2 100.3(4) . 5_557 ? O62 K4 W2 80.2(5) . 5_557 ? O17 K4 W2 27.9(3) 5_557 5_557 ? O42 K4 W2 110.6(4) 6_556 5_557 ? O49 K4 W2 166.5(4) 6_556 5_557 ? O21 K4 W2 29.1(3) 5_557 5_557 ? O63 K4 W2 73.5(4) 5_557 5_557 ? O50 K4 W2 66.7(3) 6_556 5_557 ? W8 K4 W2 139.67(16) 6_556 5_557 ? O18 K4 W5 83.2(4) . 6_556 ? O62 K4 W5 119.4(5) . 6_556 ? O17 K4 W5 92.5(4) 5_557 6_556 ? O42 K4 W5 30.6(4) 6_556 6_556 ? O49 K4 W5 86.8(4) 6_556 6_556 ? O21 K4 W5 65.4(3) 5_557 6_556 ? O63 K4 W5 148.7(5) 5_557 6_556 ? O50 K4 W5 27.4(3) 6_556 6_556 ? W8 K4 W5 61.04(9) 6_556 6_556 ? W2 K4 W5 83.65(12) 5_557 6_556 ? O18 K4 K1 113.2(5) . 5_557 ? O62 K4 K1 44.1(5) . 5_557 ? O17 K4 K1 91.3(4) 5_557 5_557 ? O42 K4 K1 142.1(5) 6_556 5_557 ? O49 K4 K1 94.1(5) 6_556 5_557 ? O21 K4 K1 104.2(4) 5_557 5_557 ? O63 K4 K1 41.7(5) 5_557 5_557 ? O50 K4 K1 158.2(4) 6_556 5_557 ? W8 K4 K1 115.7(2) 6_556 5_557 ? W2 K4 K1 92.4(2) 5_557 5_557 ? W5 K4 K1 163.6(3) 6_556 5_557 ? O50 K5 O17 73.9(5) . 2_556 ? O50 K5 O74 74.5(10) . . ? O17 K5 O74 145.3(11) 2_556 . ? O50 K5 O16 97.4(5) . 2_556 ? O17 K5 O16 103.6(6) 2_556 2_556 ? O74 K5 O16 94.1(10) . 2_556 ? O50 K5 O1 153.8(6) . 6 ? O17 K5 O1 131.9(6) 2_556 6 ? O74 K5 O1 79.4(11) . 6 ? O16 K5 O1 82.3(6) 2_556 6 ? O50 K5 O18 70.0(5) . 6 ? O17 K5 O18 72.2(5) 2_556 6 ? O74 K5 O18 84.0(10) . 6 ? O16 K5 O18 167.3(6) 2_556 6 ? O1 K5 O18 109.6(6) 6 6 ? O50 K5 O63 132.7(6) . 6 ? O17 K5 O63 66.8(5) 2_556 6 ? O74 K5 O63 147.8(11) . 6 ? O16 K5 O63 68.7(6) 2_556 6 ? O1 K5 O63 71.7(6) 6 6 ? O18 K5 O63 118.6(6) 6 6 ? O50 K5 O5 117.9(5) . 6 ? O17 K5 O5 107.8(5) 2_556 6 ? O74 K5 O5 75.4(10) . 6 ? O16 K5 O5 137.7(6) 2_556 6 ? O1 K5 O5 55.7(5) 6 6 ? O18 K5 O5 53.9(5) 6 6 ? O63 K5 O5 98.8(5) 6 6 ? O50 K5 O11 70.0(5) . 2_556 ? O17 K5 O11 52.5(5) 2_556 2_556 ? O74 K5 O11 126.3(10) . 2_556 ? O16 K5 O11 53.6(5) 2_556 2_556 ? O1 K5 O11 126.6(5) 6 2_556 ? O18 K5 O11 118.2(5) 6 2_556 ? O63 K5 O11 65.6(5) 6 2_556 ? O5 K5 O11 157.9(5) 6 2_556 ? O50 K5 W3 147.5(4) . 6 ? O17 K5 W3 117.1(4) 2_556 6 ? O74 K5 W3 83.9(9) . 6 ? O16 K5 W3 108.3(4) 2_556 6 ? O1 K5 W3 26.8(4) 6 6 ? O18 K5 W3 84.0(4) 6 6 ? O63 K5 W3 76.7(4) 6 6 ? O5 K5 W3 31.0(3) 6 6 ? O11 K5 W3 141.9(3) 2_556 6 ? O50 K5 W1 95.6(4) . 6 ? O17 K5 W1 82.3(4) 2_556 6 ? O74 K5 W1 87.0(9) . 6 ? O16 K5 W1 166.8(5) 2_556 6 ? O1 K5 W1 85.0(4) 6 6 ? O18 K5 W1 25.9(4) 6 6 ? O63 K5 W1 103.9(4) 6 6 ? O5 K5 W1 30.4(3) 6 6 ? O11 K5 W1 134.6(4) 2_556 6 ? W3 K5 W1 58.70(9) 6 6 ? O50 K5 W6 84.4(4) . 2_556 ? O17 K5 W6 80.6(4) 2_556 2_556 ? O74 K5 W6 110.0(9) . 2_556 ? O16 K5 W6 24.1(4) 2_556 2_556 ? O1 K5 W6 102.8(4) 6 2_556 ? O18 K5 W6 146.7(4) 6 2_556 ? O63 K5 W6 64.5(4) 6 2_556 ? O5 K5 W6 157.4(4) 6 2_556 ? O11 K5 W6 29.5(3) 2_556 2_556 ? W3 K5 W6 126.36(17) 6 2_556 ? W1 K5 W6 162.2(2) 6 2_556 ? O74 K6 O57 83.7(12) 6_556 6_556 ? O74 K6 O6 137.2(13) 6_556 . ? O57 K6 O6 111.9(8) 6_556 . ? O74 K6 O36 105.4(12) 6_556 . ? O57 K6 O36 66.8(7) 6_556 . ? O6 K6 O36 53.2(6) . . ? O74 K6 O45 95.9(12) 6_556 . ? O57 K6 O45 153.8(9) 6_556 . ? O6 K6 O45 52.5(6) . . ? O36 K6 O45 88.3(7) . . ? O74 K6 O5 75.2(11) 6_556 . ? O57 K6 O5 104.8(8) 6_556 . ? O6 K6 O5 62.4(6) . . ? O36 K6 O5 52.4(5) . . ? O45 K6 O5 50.5(6) . . ? O74 K6 O65 133.4(12) 6_556 . ? O57 K6 O65 57.4(7) 6_556 . ? O6 K6 O65 85.0(7) . . ? O36 K6 O65 83.5(7) . . ? O45 K6 O65 130.5(9) . . ? O5 K6 O65 134.9(8) . . ? O74 K6 W4 132.9(12) 6_556 . ? O57 K6 W4 84.1(6) 6_556 . ? O6 K6 W4 28.1(4) . . ? O36 K6 W4 29.4(4) . . ? O45 K6 W4 76.9(5) . . ? O5 K6 W4 64.3(4) . . ? O65 K6 W4 72.3(6) . . ? O74 K6 W12 123.9(11) 6_556 . ? O57 K6 W12 141.0(7) 6_556 . ? O6 K6 W12 29.1(4) . . ? O36 K6 W12 78.6(5) . . ? O45 K6 W12 28.2(4) . . ? O5 K6 W12 63.7(4) . . ? O65 K6 W12 102.6(7) . . ? W4 K6 W12 57.0(3) . . ? O74 K6 W1 82.3(11) 6_556 . ? O57 K6 W1 79.4(6) 6_556 . ? O6 K6 W1 63.3(5) . . ? O36 K6 W1 28.2(4) . . ? O45 K6 W1 74.6(5) . . ? O5 K6 W1 27.4(3) . . ? O65 K6 W1 111.2(7) . . ? W4 K6 W1 50.7(2) . . ? W12 K6 W1 78.2(3) . . ? O74 K6 W3 77.0(10) 6_556 . ? O57 K6 W3 130.8(8) 6_556 . ? O6 K6 W3 62.5(5) . . ? O36 K6 W3 75.5(5) . . ? O45 K6 W3 26.9(4) . . ? O5 K6 W3 26.5(3) . . ? O65 K6 W3 147.4(7) . . ? W4 K6 W3 77.3(3) . . ? W12 K6 W3 49.3(2) . . ? W1 K6 W3 53.6(2) . . ? O74 K6 K5 33.7(10) 6_556 6_556 ? O57 K6 K5 90.9(7) 6_556 6_556 ? O6 K6 K5 104.2(6) . 6_556 ? O36 K6 K5 78.2(5) . 6_556 ? O45 K6 K5 75.5(5) . 6_556 ? O5 K6 K5 41.8(4) . 6_556 ? O65 K6 K5 147.8(7) . 6_556 ? W4 K6 K5 101.4(4) . 6_556 ? W12 K6 K5 99.4(4) . 6_556 ? W1 K6 K5 51.3(2) . 6_556 ? W3 K6 K5 50.2(2) . 6_556 ? K4 O62 K1 93.8(7) . 5_557 ? K1 O63 K4 92.1(7) . 5_557 ? K1 O63 K5 95.5(7) . 6_556 ? K4 O63 K5 147.5(8) 5_557 6_556 ? K3 O64 K2 44(5) 7_557 . ? O41 K7 O41 93.3(16) . 2_556 ? O41 K7 O67 124.3(8) . 2_556 ? O41 K7 O67 100.9(8) 2_556 2_556 ? O41 K7 O67 100.9(8) . . ? O41 K7 O67 124.3(8) 2_556 . ? O67 K7 O67 114(2) 2_556 . ? O41 K7 W6 25.1(3) . . ? O41 K7 W6 103.5(13) 2_556 . ? O67 K7 W6 140.8(7) 2_556 . ? O67 K7 W6 76.2(7) . . ? O41 K7 W6 103.5(13) . 2_556 ? O41 K7 W6 25.1(3) 2_556 2_556 ? O67 K7 W6 76.2(7) 2_556 2_556 ? O67 K7 W6 140.8(7) . 2_556 ? W6 K7 W6 121.4(13) . 2_556 ? O41 K7 K5 79.6(7) . . ? O41 K7 K5 71.1(6) 2_556 . ? O67 K7 K5 56.0(8) 2_556 . ? O67 K7 K5 164.3(13) . . ? W6 K7 K5 104.5(8) . . ? W6 K7 K5 52.3(3) 2_556 . ? O41 K7 K5 71.1(6) . 2_556 ? O41 K7 K5 79.6(7) 2_556 2_556 ? O67 K7 K5 164.3(13) 2_556 2_556 ? O67 K7 K5 56.0(8) . 2_556 ? W6 K7 K5 52.3(3) . 2_556 ? W6 K7 K5 104.5(8) 2_556 2_556 ? K5 K7 K5 136.8(12) . 2_556 ? K3 K8 K3 180.0(6) . 7_557 ? K3 K8 O37 62.8(5) . 7_557 ? K3 K8 O37 117.2(5) 7_557 7_557 ? K3 K8 O37 117.2(5) . . ? K3 K8 O37 62.8(5) 7_557 . ? O37 K8 O37 180.0(2) 7_557 . ? K3 K8 O44 121.2(5) . 7_557 ? K3 K8 O44 58.8(5) 7_557 7_557 ? O37 K8 O44 58.4(5) 7_557 7_557 ? O37 K8 O44 121.6(5) . 7_557 ? K3 K8 O44 58.8(5) . . ? K3 K8 O44 121.2(5) 7_557 . ? O37 K8 O44 121.6(5) 7_557 . ? O37 K8 O44 58.4(5) . . ? O44 K8 O44 180.0(5) 7_557 . ? K3 K8 O52 53.7(5) . 7_557 ? K3 K8 O52 126.3(5) 7_557 7_557 ? O37 K8 O52 49.7(5) 7_557 7_557 ? O37 K8 O52 130.3(5) . 7_557 ? O44 K8 O52 87.3(5) 7_557 7_557 ? O44 K8 O52 92.7(5) . 7_557 ? K3 K8 O52 126.3(5) . . ? K3 K8 O52 53.7(5) 7_557 . ? O37 K8 O52 130.3(5) 7_557 . ? O37 K8 O52 49.7(5) . . ? O44 K8 O52 92.7(5) 7_557 . ? O44 K8 O52 87.3(5) . . ? O52 K8 O52 180.000(3) 7_557 . ? K3 K8 K2 90.4(4) . 7_557 ? K3 K8 K2 89.6(4) 7_557 7_557 ? O37 K8 K2 90.3(4) 7_557 7_557 ? O37 K8 K2 89.7(4) . 7_557 ? O44 K8 K2 90.5(4) 7_557 7_557 ? O44 K8 K2 89.5(4) . 7_557 ? O52 K8 K2 47.1(4) 7_557 7_557 ? O52 K8 K2 132.9(4) . 7_557 ? K3 K8 K2 89.6(4) . . ? K3 K8 K2 90.4(4) 7_557 . ? O37 K8 K2 89.7(4) 7_557 . ? O37 K8 K2 90.3(4) . . ? O44 K8 K2 89.5(4) 7_557 . ? O44 K8 K2 90.5(4) . . ? O52 K8 K2 132.9(4) 7_557 . ? O52 K8 K2 47.1(4) . . ? K2 K8 K2 180.000(2) 7_557 . ? K3 K8 W4 63.7(3) . 7_557 ? K3 K8 W4 116.3(3) 7_557 7_557 ? O37 K8 W4 27.5(3) 7_557 7_557 ? O37 K8 W4 152.5(3) . 7_557 ? O44 K8 W4 65.0(4) 7_557 7_557 ? O44 K8 W4 115.0(4) . 7_557 ? O52 K8 W4 25.4(3) 7_557 7_557 ? O52 K8 W4 154.6(3) . 7_557 ? K2 K8 W4 62.97(16) 7_557 7_557 ? K2 K8 W4 117.03(16) . 7_557 ? K3 K8 W4 116.3(3) . . ? K3 K8 W4 63.7(3) 7_557 . ? O37 K8 W4 152.5(3) 7_557 . ? O37 K8 W4 27.5(3) . . ? O44 K8 W4 115.0(4) 7_557 . ? O44 K8 W4 65.0(4) . . ? O52 K8 W4 154.6(3) 7_557 . ? O52 K8 W4 25.4(3) . . ? K2 K8 W4 117.03(16) 7_557 . ? K2 K8 W4 62.97(16) . . ? W4 K8 W4 180.0 7_557 . ? K6 O74 K5 112.9(16) 6 . ? O76 O75 O80 113(8) . . ? O76 O75 K3 80(8) . 7_557 ? O80 O75 K3 49(7) . 7_557 ? O76 O75 K2 61(4) . . ? O80 O75 K2 52(6) . . ? K3 O75 K2 47(5) 7_557 . ? O75 O76 K3 64(7) . 7_557 ? O75 O76 K2 94(5) . . ? K3 O76 K2 53(5) 7_557 . ? K3 O79 K2 52(5) 7_557 . ? K3 O80 O75 81(10) 7_557 . ? K3 O80 K2 63(10) 7_557 . ? O75 O80 K2 98(8) . . ? O80 K3 O72 110(10) 7_557 7_557 ? O80 K3 O75 50(8) 7_557 7_557 ? O72 K3 O75 112(9) 7_557 7_557 ? O80 K3 O76 78(10) 7_557 7_557 ? O72 K3 O76 130(8) 7_557 7_557 ? O75 K3 O76 36(4) 7_557 7_557 ? O80 K3 K2 79(9) 7_557 7_557 ? O72 K3 K2 154(8) 7_557 7_557 ? O75 K3 K2 93(7) 7_557 7_557 ? O76 K3 K2 75(7) 7_557 7_557 ? O80 K3 O79 78(10) 7_557 7_557 ? O72 K3 O79 81(8) 7_557 7_557 ? O75 K3 O79 128(9) 7_557 7_557 ? O76 K3 O79 146(8) 7_557 7_557 ? K2 K3 O79 77(5) 7_557 7_557 ? O80 K3 O64 167(10) 7_557 7_557 ? O72 K3 O64 83(5) 7_557 7_557 ? O75 K3 O64 125(10) 7_557 7_557 ? O76 K3 O64 93(9) 7_557 7_557 ? K2 K3 O64 89(8) 7_557 7_557 ? O79 K3 O64 106(6) 7_557 7_557 ? O68 K3 O51 66.0(10) . . ? O68 K3 K8 127.7(10) . . ? O51 K3 K8 79.0(7) . . ? O68 K3 O52 133.2(11) . 7_557 ? O51 K3 O52 152.0(11) . 7_557 ? K8 K3 O52 72.9(7) . 7_557 ? O68 K3 O44 116.5(11) . . ? O51 K3 O44 57.7(6) . . ? K8 K3 O44 67.9(6) . . ? O52 K3 O44 110.2(8) 7_557 . ? O68 K3 O48 149.3(12) . . ? O51 K3 O48 112.6(8) . . ? K8 K3 O48 79.1(6) . . ? O52 K3 O48 62.7(7) 7_557 . ? O44 K3 O48 54.9(6) . . ? O68 K3 O20 54.4(10) . 7_557 ? O51 K3 O20 63.9(7) . 7_557 ? K8 K3 O20 76.0(7) . 7_557 ? O52 K3 O20 107.9(8) 7_557 7_557 ? O44 K3 O20 115.1(8) . 7_557 ? O48 K3 O20 155.1(10) . 7_557 ? O68 K3 O37 93.8(10) . 7_557 ? O51 K3 O37 112.0(8) . 7_557 ? K8 K3 O37 64.1(6) . 7_557 ? O52 K3 O37 54.6(6) 7_557 7_557 ? O44 K3 O37 132.0(9) . 7_557 ? O48 K3 O37 113.4(8) . 7_557 ? O20 K3 O37 53.3(6) 7_557 7_557 ? O68 K3 W11 86.8(9) . . ? O51 K3 W11 27.1(4) . . ? K8 K3 W11 76.8(4) . . ? O52 K3 W11 139.5(8) 7_557 . ? O44 K3 W11 31.5(4) . . ? O48 K3 W11 85.8(5) . . ? O20 K3 W11 89.8(6) 7_557 . ? O37 K3 W11 130.5(7) 7_557 . ? O68 K3 W4 111.3(9) . 7_557 ? O51 K3 W4 141.0(8) . 7_557 ? K8 K3 W4 73.5(4) . 7_557 ? O52 K3 W4 26.3(4) 7_557 7_557 ? O44 K3 W4 130.6(8) . 7_557 ? O48 K3 W4 88.9(6) . 7_557 ? O20 K3 W4 82.8(6) 7_557 7_557 ? O37 K3 W4 30.2(4) 7_557 7_557 ? W11 K3 W4 150.3(7) . 7_557 ? O68 K3 W15 134.0(10) . . ? O51 K3 W15 86.0(5) . . ? K8 K3 W15 76.8(4) . . ? O52 K3 W15 88.0(6) 7_557 . ? O44 K3 W15 28.9(4) . . ? O48 K3 W15 26.9(4) . . ? O20 K3 W15 142.5(7) 7_557 . ? O37 K3 W15 131.4(7) 7_557 . ? W11 K3 W15 59.0(2) . . ? W4 K3 W15 113.3(5) 7_557 . ? O68 K3 W10 67.5(9) . 7_557 ? O51 K3 W10 89.1(6) . 7_557 ? K8 K3 W10 74.7(4) . 7_557 ? O52 K3 W10 83.2(6) 7_557 7_557 ? O44 K3 W10 133.4(7) . 7_557 ? O48 K3 W10 141.9(8) . 7_557 ? O20 K3 W10 25.7(5) 7_557 7_557 ? O37 K3 W10 29.1(4) 7_557 7_557 ? W11 K3 W10 113.9(4) . 7_557 ? W4 K3 W10 57.4(2) 7_557 7_557 ? W15 K3 W10 151.5(7) . 7_557 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 O18 1.715(18) . ? W1 O35 1.823(16) . ? W1 O5 1.914(16) . ? W1 O13 1.971(17) . ? W1 O36 1.978(17) . ? W1 O31 2.359(16) . ? W1 K5 3.770(6) 6_556 ? W1 K6 4.029(18) . ? W1 K4 4.099(6) . ? W2 O17 1.733(16) . ? W2 O21 1.768(16) . ? W2 O11 1.910(16) . ? W2 O4 1.968(18) . ? W2 O35 2.079(15) . ? W2 O32 2.132(17) . ? W2 K4 3.605(5) 5_557 ? W2 K5 3.864(7) 2_556 ? W3 O1 1.734(19) . ? W3 O4 1.874(18) . ? W3 O5 1.922(16) . ? W3 O47 1.941(19) . ? W3 O45 1.948(19) . ? W3 O26 2.348(16) . ? W3 K5 3.721(6) 6_556 ? W3 K6 4.112(19) . ? W4 O52 1.73(2) . ? W4 O6 1.84(2) . ? W4 O37 1.876(19) . ? W4 O36 1.888(16) . ? W4 O14 1.952(19) . ? W4 O31 2.293(16) . ? W4 K3 3.732(16) 7_557 ? W4 K6 3.801(17) . ? W4 K2 3.885(10) . ? W4 K8 3.9921(13) . ? W5 O50 1.725(15) . ? W5 O61 1.759(15) . ? W5 O42 1.930(17) . ? W5 O41 1.941(17) . ? W5 O53 2.101(19) . ? W5 O28 2.379(16) . ? W5 K4 3.717(6) 6 ? W6 O16 1.71(2) . ? W6 O41 1.874(16) . ? W6 O11 1.886(16) . ? W6 O40 1.904(16) . ? W6 O54 1.939(18) . ? W6 O28 2.299(17) . ? W6 K5 3.828(6) 2_556 ? W6 K7 4.05(3) . ? W7 O19 1.722(19) . ? W7 O39 1.733(17) . ? W7 O8 1.940(19) . ? W7 O10 1.957(18) . ? W7 O38 2.060(19) . ? W7 O30 2.334(16) . ? W8 O49 1.70(2) . ? W8 O10 1.856(18) . ? W8 O42 1.868(17) . ? W8 O43 1.96(2) . ? W8 O23 1.99(2) . ? W8 O29 2.328(17) . ? W8 K4 3.595(5) 6 ? W9 O15 1.73(2) . ? W9 O13 1.835(18) . ? W9 O40 1.892(16) . ? W9 O33 1.925(19) . ? W9 O22 1.96(2) . ? W9 O27 2.334(18) . ? W10 O20 1.75(2) . ? W10 O38 1.821(18) . ? W10 O7 1.89(2) . ? W10 O37 1.931(19) . ? W10 O12 1.95(2) . ? W10 O30 2.396(17) . ? W10 K3 3.924(16) 7_557 ? W10 K2 4.050(10) 7_557 ? W11 O51 1.73(2) . ? W11 O14 1.871(19) . ? W11 O44 1.91(2) . ? W11 O33 1.913(19) . ? W11 O59 1.94(2) . ? W11 O27 2.382(17) . ? W11 K3 3.646(14) . ? W11 K2 3.945(11) . ? W11 K8 4.0750(16) . ? W12 O3 1.73(2) . ? W12 O46 1.81(2) . ? W12 O45 1.913(19) . ? W12 O7 1.94(2) . ? W12 O6 1.996(19) . ? W12 O26 2.423(17) . ? W12 K6 3.956(19) . ? La1 O61 2.445(16) . ? La1 O61 2.445(16) 2_556 ? La1 O21 2.471(16) 2_556 ? La1 O21 2.471(16) . ? La1 O9 2.480(19) . ? La1 O9 2.480(19) 2_556 ? La1 O39 2.506(16) . ? La1 O39 2.506(16) 2_556 ? W14 O2 1.74(2) . ? W14 O9 1.776(19) . ? W14 O8 1.902(19) . ? W14 O47 1.969(18) . ? W14 O46 2.11(2) . ? W14 O26 2.420(17) . ? W15 O48 1.76(2) . ? W15 O12 1.86(2) . ? W15 O44 1.88(2) . ? W15 O43 1.882(19) . ? W15 O60 1.96(2) . ? W15 O29 2.379(18) . ? W15 K3 3.826(14) . ? W15 K2 4.091(13) 7_557 ? W16 O34 1.71(3) . ? W16 O60 1.87(2) . ? W16 O55 1.88(2) . ? W16 O59 1.92(2) . ? W16 O56 1.94(2) . ? W16 O25 2.38(2) . ? W17 O58 1.78(3) . ? W17 O54 1.894(18) . ? W17 O22 1.894(19) . ? W17 O24 1.92(2) . ? W17 O56 1.94(2) . ? W17 O25 2.33(2) . ? W18 O57 1.73(2) . ? W18 O53 1.807(19) . ? W18 O23 1.86(2) . ? W18 O24 1.99(2) . ? W18 O55 2.02(2) . ? W18 O25 2.37(2) . ? P1 O28 1.539(17) . ? P1 O27 1.543(18) . ? P1 O29 1.56(2) . ? P1 O25 1.61(2) . ? P2 O32 1.511(18) . ? P2 O30 1.545(17) . ? P2 O31 1.546(17) . ? P2 O26 1.563(19) . ? O21 K4 2.915(17) 5_557 ? O17 K5 2.752(19) 2_556 ? O17 K4 2.784(17) 5_557 ? O16 K5 2.80(2) 2_556 ? O16 K1 3.32(2) 5_557 ? O5 K5 3.078(16) 6_556 ? O5 K6 3.11(2) . ? O50 K5 2.679(17) . ? O50 K4 3.083(17) 6 ? O41 K7 2.91(4) . ? O42 K4 2.807(17) 6 ? O11 K5 3.245(17) 2_556 ? O52 K2 2.70(2) . ? O52 K3 2.84(3) 7_557 ? O52 K8 3.38(2) . ? O18 K4 2.69(2) . ? O18 K5 2.908(19) 6_556 ? O14 K2 3.32(2) . ? O37 K3 3.15(3) 7_557 ? O37 K8 3.19(2) . ? O51 K3 2.76(2) . ? O51 K2 2.89(2) . ? O1 K5 2.88(2) 6_556 ? O1 K1 2.89(2) . ? O36 K6 3.02(2) . ? O45 K6 3.08(3) . ? O44 K3 3.02(3) . ? O44 K8 3.27(2) . ? O49 K4 2.86(2) 6 ? O15 K1 3.28(2) 5_557 ? O20 K2 2.81(3) 7_557 ? O20 K3 3.14(3) 7_557 ? O6 K6 2.92(3) . ? O48 K2 2.93(3) 7_557 ? O48 K3 3.12(3) . ? O57 K6 2.91(3) 6 ? K2 K3 2.19(18) 7_557 ? K2 O80 2.41(15) . ? K2 O76 2.64(8) . ? K2 O79 2.72(9) . ? K2 O20 2.81(3) 7_557 ? K2 O48 2.93(3) 7_557 ? K2 O75 3.01(6) . ? K2 O64 3.12(2) . ? K2 K8 3.379(12) . ? K1 O63 2.72(3) . ? K1 O81 2.85(11) . ? K1 O62 2.86(2) 5_557 ? K1 O15 3.28(2) 5_557 ? K1 O16 3.32(2) 5_557 ? K1 K4 4.092(13) 5_557 ? K1 K5 4.267(15) 6_556 ? K4 O62 2.75(2) . ? K4 O17 2.784(17) 5_557 ? K4 O42 2.807(17) 6_556 ? K4 O49 2.86(2) 6_556 ? K4 O21 2.915(17) 5_557 ? K4 O63 2.96(2) 5_557 ? K4 O50 3.083(17) 6_556 ? K4 W8 3.595(5) 6_556 ? K4 W2 3.605(5) 5_557 ? K4 W5 3.717(6) 6_556 ? K4 K1 4.092(13) 5_557 ? K5 O17 2.752(19) 2_556 ? K5 O74 2.77(5) . ? K5 O16 2.80(2) 2_556 ? K5 O1 2.88(2) 6 ? K5 O18 2.908(19) 6 ? K5 O63 3.04(2) 6 ? K5 O5 3.078(16) 6 ? K5 O11 3.245(17) 2_556 ? K5 W3 3.721(6) 6 ? K5 W1 3.770(6) 6 ? K5 W6 3.828(6) 2_556 ? K6 O74 2.74(5) 6_556 ? K6 O57 2.91(3) 6_556 ? K6 O65 3.41(3) . ? K6 K5 4.60(2) 6_556 ? O62 K1 2.86(2) 5_557 ? O63 K4 2.96(2) 5_557 ? O63 K5 3.04(2) 6_556 ? O64 K3 2.25(17) 7_557 ? O67 K7 3.08(5) . ? O68 K3 2.58(4) . ? K7 O41 2.91(4) 2_556 ? K7 O67 3.08(5) 2_556 ? K7 W6 4.05(3) 2_556 ? K7 K5 4.57(2) 2_556 ? O72 K3 1.87(18) 7_557 ? K8 K3 2.83(2) . ? K8 K3 2.83(2) 7_557 ? K8 O37 3.19(2) 7_557 ? K8 O44 3.27(2) 7_557 ? K8 O52 3.38(2) 7_557 ? K8 K2 3.379(12) 7_557 ? K8 W4 3.9921(13) 7_557 ? O74 K6 2.74(5) 6 ? O75 O76 1.28(8) . ? O75 O80 1.51(16) . ? O75 K3 1.94(14) 7_557 ? O76 K3 2.13(19) 7_557 ? O79 K3 2.19(18) 7_557 ? O80 K3 1.48(18) 7_557 ? K3 O80 1.48(18) 7_557 ? K3 O72 1.87(18) 7_557 ? K3 O75 1.94(14) 7_557 ? K3 O76 2.13(19) 7_557 ? K3 K2 2.19(18) 7_557 ? K3 O79 2.19(18) 7_557 ? K3 O64 2.25(17) 7_557 ? K3 O52 2.84(3) 7_557 ? K3 O20 3.14(3) 7_557 ? K3 O37 3.15(3) 7_557 ? K3 W4 3.732(16) 7_557 ? K3 W10 3.924(16) 7_557 ?
1100737.cif	#------------------------------------------------------------------------------ #$Date: 2016-09-20 14:11:36 +0300 (Tue, 20 Sep 2016) $ #$Revision: 186650 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/10/07/1100737.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100737 loop_ _publ_author_name 'Cheng Zhang' 'Robertha C. Howell' 'Qun-Hui Luo' 'Heidi L. Fieselmann' 'Louis J. Todaro' 'Lynn C. Francesconi' _publ_section_title ; Influence of Steric and Electronic Properties of the Defect Site, Lanthanide Ionic Radii, and Solution Conditions on the Composition of Lanthanide(III) \a1-P2W17O6110-Polyoxometalates ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3569 _journal_page_last 3578 _journal_paper_doi 10.1021/ic050103o _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'Cl4 H92 K4 Na6 Nd O162 P4 W34' _chemical_formula_weight 9593.92 _chemical_name_systematic ; ? ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 104.63(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 41.072(8) _cell_length_b 16.152(3) _cell_length_c 24.933(5) _cell_measurement_temperature 100(2) _cell_volume 16004(6) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.957 _diffrn_measured_fraction_theta_max 0.957 _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.2791 _diffrn_reflns_av_sigmaI/netI 0.2139 _diffrn_reflns_limit_h_max 52 _diffrn_reflns_limit_h_min -52 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_number 59874 _diffrn_reflns_theta_full 27.32 _diffrn_reflns_theta_max 27.32 _diffrn_reflns_theta_min 2.90 _exptl_absorpt_coefficient_mu 24.980 _exptl_absorpt_correction_T_max 0.1890 _exptl_absorpt_correction_T_min 0.0314 _exptl_absorpt_process_details 'Numerical absorption correction from indexed crystal faces' _exptl_crystal_density_diffrn 3.982 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 16848 _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.10 _refine_diff_density_max 6.177 _refine_diff_density_min -6.372 _refine_diff_density_rms 1.162 _refine_ls_extinction_coef 0.000070(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 540 _refine_ls_number_reflns 17288 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.044 _refine_ls_R_factor_all 0.1846 _refine_ls_R_factor_gt 0.1221 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1544P)^2^+9812.2217P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2982 _refine_ls_wR_factor_ref 0.3469 _reflns_number_gt 10779 _reflns_number_total 17288 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic050103osi20050113_051640.cif _cod_data_source_block Neodymium_a1P2W17O61_1to2 _cod_original_formula_sum 'H46 Cl2 K2 Na2 Nd0.50 O81 P2 W17' _cod_database_code 1100737 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W2 W 0.02270(4) 0.56841(11) 0.40168(7) 0.0096(4) Uani 1 1 d . . . W3 W 0.09232(4) 0.59860(11) 0.53174(8) 0.0116(4) Uani 1 1 d . . . W4 W 0.15712(4) 0.72008(11) 0.52242(8) 0.0131(4) Uani 1 1 d . . . W5 W 0.15760(4) 0.81552(11) 0.38859(8) 0.0151(4) Uani 1 1 d . . . W6 W 0.09019(4) 0.77867(11) 0.27754(8) 0.0128(4) Uani 1 1 d . . . W7 W 0.03437(4) 0.76844(12) 0.47874(8) 0.0150(4) Uani 1 1 d . . . W8 W 0.09838(5) 0.89270(12) 0.46842(9) 0.0191(4) Uani 1 1 d . . . W9 W 0.03186(4) 0.85611(11) 0.35282(9) 0.0161(4) Uani 1 1 d . . . W11 W 0.06532(4) 0.46914(11) 0.25318(8) 0.0102(4) Uani 1 1 d . . . W12 W 0.06768(4) 0.37699(11) 0.37328(8) 0.0108(4) Uani 1 1 d . . . W13 W 0.13763(4) 0.41360(11) 0.49766(8) 0.0120(4) Uani 1 1 d . . . W14 W 0.20245(4) 0.53280(11) 0.48785(8) 0.0114(4) Uani 1 1 d . . . W15 W 0.20360(4) 0.63112(11) 0.35479(8) 0.0126(4) Uani 1 1 d . . . W16 W 0.13873(4) 0.59932(11) 0.24381(8) 0.0107(4) Uani 1 1 d . . . W17 W 0.15184(4) 0.28391(11) 0.38250(8) 0.0150(4) Uani 1 1 d . . . W18 W 0.21669(4) 0.40525(12) 0.37114(8) 0.0148(4) Uani 1 1 d . . . W19 W 0.15010(4) 0.37458(12) 0.25831(8) 0.0140(4) Uani 1 1 d . . . Nd Nd 0.0000 0.6565(2) 0.2500 0.0097(6) Uani 1 2 d S . . P1 P 0.0898(2) 0.6937(7) 0.4060(5) 0.008(2) Uiso 1 1 d . . . P2 P 0.1377(3) 0.4969(7) 0.3676(5) 0.010(2) Uiso 1 1 d . . . O2 O -0.0053(7) 0.5210(19) 0.4334(13) 0.013(6) Uiso 1 1 d . . . O3 O 0.0822(8) 0.562(2) 0.5893(15) 0.021(7) Uiso 1 1 d . . . O4 O 0.1908(8) 0.759(2) 0.5755(15) 0.019(7) Uiso 1 1 d . . . O5 O 0.1894(9) 0.882(2) 0.4008(16) 0.027(8) Uiso 1 1 d . . . O6 O 0.0848(8) 0.836(2) 0.2184(15) 0.024(8) Uiso 1 1 d . . . O7 O 0.0067(8) 0.780(2) 0.5196(15) 0.024(8) Uiso 1 1 d . . . O8 O 0.1147(11) 0.984(3) 0.503(2) 0.046(11) Uiso 1 1 d . . . O9 O 0.0089(7) 0.940(2) 0.3245(14) 0.017(7) Uiso 1 1 d . . . O11 O 0.0435(6) 0.4426(16) 0.1862(11) 0.002(5) Uiso 1 1 d . . . O12 O 0.0430(8) 0.302(2) 0.3902(16) 0.024(8) Uiso 1 1 d . . . O13 O 0.1341(8) 0.344(2) 0.5457(16) 0.026(8) Uiso 1 1 d . . . O14 O 0.2415(7) 0.5451(19) 0.5349(13) 0.013(6) Uiso 1 1 d . . . O15 O 0.2406(7) 0.6717(19) 0.3558(13) 0.013(6) Uiso 1 1 d . . . O16 O 0.1358(8) 0.620(2) 0.1768(15) 0.021(7) Uiso 1 1 d . . . O17 O 0.1511(10) 0.180(3) 0.3978(18) 0.036(9) Uiso 1 1 d . . . O18 O 0.2578(8) 0.379(2) 0.3796(16) 0.026(8) Uiso 1 1 d . . . O19 O 0.1525(9) 0.327(2) 0.1970(16) 0.027(8) Uiso 1 1 d . . . O2N O -0.0041(7) 0.5988(19) 0.3397(13) 0.012(6) Uiso 1 1 d . . . O6N O 0.0575(7) 0.7073(19) 0.2620(13) 0.013(6) Uiso 1 1 d . . . O9N O 0.0124(6) 0.7712(17) 0.3180(12) 0.006(5) Uiso 1 1 d . . . O11N O 0.0382(9) 0.544(3) 0.2721(18) 0.033(9) Uiso 1 1 d . . . O2P O 0.0629(6) 0.6290(16) 0.3775(11) 0.003(5) Uiso 1 1 d . . . O3P O 0.1121(7) 0.6625(18) 0.4584(12) 0.009(6) Uiso 1 1 d . . . O5P O 0.1101(7) 0.7266(18) 0.3645(13) 0.011(6) Uiso 1 1 d . . . O7P O 0.0704(8) 0.771(2) 0.4219(15) 0.024(8) Uiso 1 1 d . . . O11P O 0.1000(7) 0.4811(19) 0.3462(14) 0.015(7) Uiso 1 1 d . . . O13P O 0.1483(8) 0.506(2) 0.4296(14) 0.019(7) Uiso 1 1 d . . . O15P O 0.1481(6) 0.5740(17) 0.3374(12) 0.006(5) Uiso 1 1 d . . . O17P O 0.1563(7) 0.4192(19) 0.3524(13) 0.012(6) Uiso 1 1 d . . . O112 O 0.0525(7) 0.3819(19) 0.2940(13) 0.012(6) Uiso 1 1 d . . . O116 O 0.0967(7) 0.552(2) 0.2378(14) 0.016(7) Uiso 1 1 d . . . O119 O 0.1057(9) 0.395(2) 0.2497(17) 0.031(9) Uiso 1 1 d . . . O123 O 0.0946(7) 0.3987(19) 0.4455(14) 0.014(6) Uiso 1 1 d . . . O127 O 0.1063(7) 0.3134(18) 0.3637(12) 0.009(6) Uiso 1 1 d . . . O134 O 0.1839(7) 0.449(2) 0.5254(14) 0.018(7) Uiso 1 1 d . . . O137 O 0.1542(7) 0.334(2) 0.4525(14) 0.016(7) Uiso 1 1 d . . . O145 O 0.2070(8) 0.608(2) 0.4297(15) 0.020(7) Uiso 1 1 d . . . O148 O 0.2133(6) 0.4486(17) 0.4424(12) 0.005(5) Uiso 1 1 d . . . O156 O 0.1853(8) 0.630(2) 0.2758(14) 0.018(7) Uiso 1 1 d . . . O158 O 0.2160(7) 0.5215(19) 0.3461(14) 0.014(6) Uiso 1 1 d . . . O169 O 0.1563(8) 0.486(2) 0.2435(15) 0.019(7) Uiso 1 1 d . . . O178 O 0.2003(7) 0.3031(19) 0.3926(13) 0.012(6) Uiso 1 1 d . . . O179 O 0.1475(8) 0.274(2) 0.3053(14) 0.019(7) Uiso 1 1 d . . . O189 O 0.1999(8) 0.376(2) 0.2969(15) 0.022(7) Uiso 1 1 d . . . O212 O 0.0409(7) 0.4702(19) 0.3800(14) 0.013(6) Uiso 1 1 d . . . O230 O 0.0602(6) 0.5533(16) 0.4748(12) 0.004(5) Uiso 1 1 d . . . O270 O 0.0171(7) 0.6762(19) 0.4370(13) 0.013(6) Uiso 1 1 d . . . O313 O 0.1227(7) 0.5104(18) 0.5256(12) 0.008(6) Uiso 1 1 d . . . O340 O 0.1330(8) 0.662(2) 0.5675(16) 0.025(8) Uiso 1 1 d . . . O370 O 0.0677(8) 0.699(2) 0.5239(14) 0.018(7) Uiso 1 1 d . . . O414 O 0.1796(6) 0.6170(17) 0.5140(12) 0.007(6) Uiso 1 1 d . . . O450 O 0.1692(7) 0.7544(19) 0.4583(13) 0.012(6) Uiso 1 1 d . . . O480 O 0.1281(9) 0.814(2) 0.5137(17) 0.029(8) Uiso 1 1 d . . . O515 O 0.1792(7) 0.7267(19) 0.3604(13) 0.012(6) Uiso 1 1 d . . . O560 O 0.1331(6) 0.8446(17) 0.3206(12) 0.005(5) Uiso 1 1 d . . . O580 O 0.1292(8) 0.876(2) 0.4231(15) 0.020(7) Uiso 1 1 d . . . O616 O 0.1227(7) 0.7007(18) 0.2618(13) 0.010(6) Uiso 1 1 d . . . O690 O 0.0687(7) 0.853(2) 0.3177(14) 0.015(6) Uiso 1 1 d . . . O780 O 0.0640(8) 0.861(2) 0.5048(15) 0.022(7) Uiso 1 1 d . . . O790 O 0.0142(7) 0.8388(18) 0.4181(12) 0.009(6) Uiso 1 1 d . . . O890 O 0.0661(8) 0.932(2) 0.4064(15) 0.023(7) Uiso 1 1 d . . . K1 K 0.0673(2) 0.5830(7) 0.1269(4) 0.019(2) Uani 1 1 d . . . K2 K -0.0180(2) 0.3552(7) 0.4069(5) 0.019(2) Uani 1 1 d . . . Cl1 Cl 0.2444(3) 0.6557(8) 0.6211(5) 0.022(2) Uani 1 1 d . . . Cl2 Cl 0.0661(4) 0.7675(12) 0.0149(8) 0.050(5) Uani 1 1 d . . . Na1 Na 0.2838(6) 0.6131(14) 0.4717(12) 0.042(6) Uani 1 1 d . . . Na2 Na 0.1995(6) 1.0495(15) 0.3964(11) 0.038(5) Uiso 1 1 d . . . O901 O 0.1998(8) 0.386(2) 0.6391(15) 0.020(7) Uiso 1 1 d . . . O902 O 0.1138(11) 0.188(3) 0.125(2) 0.043(11) Uiso 1 1 d . . . O903 O 0.0517(8) 0.745(2) 0.1230(15) 0.021(7) Uiso 1 1 d . . . O904 O 0.2258(10) 0.480(3) 0.7283(19) 0.039(10) Uiso 1 1 d . . . O905 O 0.1873(9) 0.557(3) 0.6330(18) 0.034(9) Uiso 1 1 d . . . O906 O 0.0402(8) 0.609(2) 0.0037(15) 0.023(7) Uiso 1 1 d . . . O907 O 0.1952(11) 0.166(3) 0.178(2) 0.050(12) Uiso 1 1 d . . . O908 O 0.2201(12) 0.966(3) 0.311(2) 0.059(14) Uiso 1 1 d . . . O909 O 0.2358(12) 0.301(3) 0.232(2) 0.052(12) Uiso 1 1 d . . . O910 O -0.0673(13) 0.266(4) 0.334(2) 0.064(15) Uiso 1 1 d . . . O911 O 0.1092(14) 0.853(4) -0.028(3) 0.074(17) Uiso 1 1 d . . . O912 O 0.2233(15) 0.289(4) 0.523(3) 0.082(18) Uiso 1 1 d . . . O913 O -0.0371(17) 1.033(5) 0.242(3) 0.09(2) Uiso 1 1 d . . . O914 O 0.0427(15) 0.917(4) 0.047(3) 0.078(18) Uiso 1 1 d . . . O915 O 0.1622(17) 0.888(5) 0.223(3) 0.09(2) Uiso 1 1 d . . . O916 O 0.051(2) 0.928(6) 0.606(4) 0.12(3) Uiso 1 1 d . . . O917 O 0.0255(19) 1.072(5) 0.444(4) 0.11(3) Uiso 1 1 d . . . O918 O 0.118(2) 1.018(6) 0.326(4) 0.14(3) Uiso 1 1 d . . . O919 O 0.0779(19) 0.197(5) 0.266(4) 0.11(2) Uiso 1 1 d . . . O920 O 0.2500 0.7500 0.5000 0.046(16) Uiso 1 2 d S . . O921 O 0.0000 2.272(6) 0.2500 0.08(3) Uiso 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W2 0.0030(7) 0.0156(9) 0.0081(9) 0.0010(7) -0.0024(6) 0.0006(6) W3 0.0061(7) 0.0175(9) 0.0090(9) -0.0016(7) -0.0022(6) 0.0016(6) W4 0.0077(7) 0.0135(9) 0.0132(10) -0.0055(8) -0.0064(7) 0.0000(6) W5 0.0087(7) 0.0121(8) 0.0182(10) -0.0003(8) -0.0084(7) -0.0028(7) W6 0.0072(7) 0.0119(8) 0.0149(10) 0.0009(7) -0.0052(7) -0.0015(6) W7 0.0115(8) 0.0166(9) 0.0141(10) -0.0043(8) -0.0023(7) 0.0067(7) W8 0.0176(8) 0.0106(9) 0.0230(11) -0.0057(8) -0.0057(8) 0.0027(7) W9 0.0132(8) 0.0104(8) 0.0191(10) -0.0035(8) -0.0061(7) 0.0047(7) W11 0.0055(7) 0.0133(8) 0.0102(9) 0.0006(7) -0.0014(6) -0.0004(6) W12 0.0089(7) 0.0107(8) 0.0116(9) 0.0013(7) 0.0002(7) -0.0005(6) W13 0.0096(7) 0.0132(9) 0.0107(9) 0.0009(7) -0.0020(7) 0.0021(6) W14 0.0056(7) 0.0142(9) 0.0110(9) 0.0003(7) -0.0040(6) 0.0018(6) W15 0.0044(7) 0.0167(9) 0.0141(9) 0.0012(8) -0.0027(7) -0.0016(6) W16 0.0045(7) 0.0157(9) 0.0091(9) 0.0027(7) -0.0036(6) -0.0012(6) W17 0.0177(8) 0.0088(8) 0.0169(10) 0.0016(7) 0.0010(8) 0.0051(7) W18 0.0097(7) 0.0182(9) 0.0152(10) 0.0010(8) 0.0011(7) 0.0071(7) W19 0.0124(8) 0.0147(9) 0.0133(10) -0.0015(8) 0.0005(7) 0.0059(7) Nd 0.0025(12) 0.0142(16) 0.0096(16) 0.000 -0.0036(12) 0.000 K1 0.011(4) 0.030(6) 0.011(5) 0.002(4) -0.007(4) 0.005(4) K2 0.009(4) 0.031(6) 0.020(6) -0.005(5) 0.005(4) 0.001(4) Cl1 0.020(5) 0.021(6) 0.022(6) 0.000(5) 0.001(5) 0.000(5) Cl2 0.039(8) 0.058(11) 0.059(12) -0.015(9) 0.022(8) -0.029(8) Na1 0.033(12) 0.027(12) 0.062(19) 0.007(12) 0.005(12) -0.016(10) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2N W2 O2 100.8(14) . . ? O2N W2 O212 101.0(14) . . ? O2 W2 O212 96.7(13) . . ? O2N W2 O270 91.6(14) . . ? O2 W2 O270 91.1(13) . . ? O212 W2 O270 163.6(12) . . ? O2N W2 O230 168.6(12) . . ? O2 W2 O230 88.8(12) . . ? O212 W2 O230 83.9(12) . . ? O270 W2 O230 81.9(12) . . ? O2N W2 O2P 88.9(12) . . ? O2 W2 O2P 169.6(13) . . ? O212 W2 O2P 85.0(11) . . ? O270 W2 O2P 84.8(11) . . ? O230 W2 O2P 81.2(10) . . ? O2N W2 K1 54.0(9) . 2 ? O2 W2 K1 49.5(10) . 2 ? O212 W2 K1 117.4(9) . 2 ? O270 W2 K1 78.6(8) . 2 ? O230 W2 K1 132.7(7) . 2 ? O2P W2 K1 138.2(7) . 2 ? O2N W2 K2 95.8(10) . . ? O2 W2 K2 40.8(10) . . ? O212 W2 K2 57.6(9) . . ? O270 W2 K2 131.9(8) . . ? O230 W2 K2 95.6(7) . . ? O2P W2 K2 142.6(7) . . ? K1 W2 K2 68.4(2) 2 . ? O3 W3 O230 103.6(14) . . ? O3 W3 O370 98.5(15) . . ? O230 W3 O370 90.1(13) . . ? O3 W3 O313 96.5(14) . . ? O230 W3 O313 89.8(12) . . ? O370 W3 O313 164.7(13) . . ? O3 W3 O340 99.1(16) . . ? O230 W3 O340 157.2(13) . . ? O370 W3 O340 88.4(14) . . ? O313 W3 O340 85.7(13) . . ? O3 W3 O3P 172.2(14) . . ? O230 W3 O3P 84.1(11) . . ? O370 W3 O3P 80.1(12) . . ? O313 W3 O3P 84.6(11) . . ? O340 W3 O3P 73.2(13) . . ? O3 W3 K2 48.6(11) . 5_566 ? O230 W3 K2 84.1(8) . 5_566 ? O370 W3 K2 54.2(10) . 5_566 ? O313 W3 K2 141.0(9) . 5_566 ? O340 W3 K2 113.0(10) . 5_566 ? O3P W3 K2 132.6(7) . 5_566 ? O3 W3 K1 26.3(12) . 6_566 ? O230 W3 K1 85.7(8) . 6_566 ? O370 W3 K1 118.1(10) . 6_566 ? O313 W3 K1 77.2(9) . 6_566 ? O340 W3 K1 114.9(11) . 6_566 ? O3P W3 K1 159.2(7) . 6_566 ? K2 W3 K1 64.0(2) 5_566 6_566 ? O4 W4 O450 101.9(14) . . ? O4 W4 O480 98.7(16) . . ? O450 W4 O480 87.8(15) . . ? O4 W4 O340 99.1(15) . . ? O450 W4 O340 158.6(15) . . ? O480 W4 O340 93.2(15) . . ? O4 W4 O414 94.7(13) . . ? O450 W4 O414 85.8(12) . . ? O480 W4 O414 166.1(15) . . ? O340 W4 O414 88.4(13) . . ? O4 W4 O3P 175.4(13) . . ? O450 W4 O3P 82.5(12) . . ? O480 W4 O3P 82.7(14) . . ? O340 W4 O3P 76.5(13) . . ? O414 W4 O3P 84.3(11) . . ? O4 W4 Na1 46.6(12) . 7_566 ? O450 W4 Na1 59.5(10) . 7_566 ? O480 W4 Na1 78.8(12) . 7_566 ? O340 W4 Na1 141.6(12) . 7_566 ? O414 W4 Na1 108.2(9) . 7_566 ? O3P W4 Na1 137.9(9) . 7_566 ? O5 W5 O560 103.4(16) . . ? O5 W5 O580 97.3(16) . . ? O560 W5 O580 91.7(13) . . ? O5 W5 O515 97.9(15) . . ? O560 W5 O515 92.9(13) . . ? O580 W5 O515 162.6(13) . . ? O5 W5 O450 99.1(16) . . ? O560 W5 O450 157.4(12) . . ? O580 W5 O450 84.1(14) . . ? O515 W5 O450 85.2(13) . . ? O5 W5 O5P 175.4(15) . . ? O560 W5 O5P 72.0(11) . . ? O580 W5 O5P 82.4(12) . . ? O515 W5 O5P 83.1(11) . . ? O450 W5 O5P 85.4(11) . . ? O6 W6 O6N 104.0(16) . . ? O6 W6 O690 98.0(15) . . ? O6N W6 O690 95.6(13) . . ? O6 W6 O616 97.0(15) . . ? O6N W6 O616 93.3(13) . . ? O690 W6 O616 160.3(13) . . ? O6 W6 O560 94.4(14) . . ? O6N W6 O560 161.6(13) . . ? O690 W6 O560 81.6(11) . . ? O616 W6 O560 84.4(11) . . ? O6 W6 O5P 163.8(14) . . ? O6N W6 O5P 92.2(13) . . ? O690 W6 O5P 80.5(12) . . ? O616 W6 O5P 81.5(12) . . ? O560 W6 O5P 69.3(10) . . ? O7 W7 O270 101.9(15) . . ? O7 W7 O790 100.5(14) . . ? O270 W7 O790 90.4(13) . . ? O7 W7 O370 101.6(16) . . ? O270 W7 O370 88.6(14) . . ? O790 W7 O370 157.6(12) . . ? O7 W7 O780 99.6(16) . . ? O270 W7 O780 158.5(13) . . ? O790 W7 O780 85.2(14) . . ? O370 W7 O780 87.6(14) . . ? O7 W7 O7P 172.4(15) . . ? O270 W7 O7P 83.2(13) . . ? O790 W7 O7P 73.7(12) . . ? O370 W7 O7P 84.0(13) . . ? O780 W7 O7P 75.3(14) . . ? O7 W7 K2 47.5(12) . 5_566 ? O270 W7 K2 83.0(10) . 5_566 ? O790 W7 K2 144.1(8) . 5_566 ? O370 W7 K2 57.8(10) . 5_566 ? O780 W7 K2 112.4(11) . 5_566 ? O7P W7 K2 139.5(9) . 5_566 ? O8 W8 O890 102.6(19) . . ? O8 W8 O480 99.3(19) . . ? O890 W8 O480 157.3(16) . . ? O8 W8 O580 100.1(18) . . ? O890 W8 O580 89.8(15) . . ? O480 W8 O580 80.8(15) . . ? O8 W8 O780 103.3(18) . . ? O890 W8 O780 91.7(15) . . ? O480 W8 O780 88.8(15) . . ? O580 W8 O780 155.7(15) . . ? O8 W8 O7P 174.4(16) . . ? O890 W8 O7P 74.5(14) . . ? O480 W8 O7P 84.1(14) . . ? O580 W8 O7P 84.9(13) . . ? O780 W8 O7P 72.2(13) . . ? O9 W9 O9N 106.7(14) . . ? O9 W9 O690 104.5(14) . . ? O9N W9 O690 93.8(13) . . ? O9 W9 O790 100.1(14) . . ? O9N W9 O790 94.8(12) . . ? O690 W9 O790 150.3(13) . . ? O9 W9 O890 90.6(15) . . ? O9N W9 O890 162.6(13) . . ? O690 W9 O890 80.1(13) . . ? O790 W9 O890 83.3(13) . . ? O9 W9 O7P 159.1(14) . . ? O9N W9 O7P 92.3(12) . . ? O690 W9 O7P 82.1(12) . . ? O790 W9 O7P 69.2(11) . . ? O890 W9 O7P 70.8(13) . . ? O11 W11 O11N 102.4(16) . . ? O11 W11 O112 100.8(13) . . ? O11N W11 O112 94.7(16) . . ? O11 W11 O116 100.7(13) . . ? O11N W11 O116 94.6(16) . . ? O112 W11 O116 154.2(13) . . ? O11 W11 O119 92.3(14) . . ? O11N W11 O119 164.9(17) . . ? O112 W11 O119 85.6(14) . . ? O116 W11 O119 79.3(14) . . ? O11 W11 O11P 169.5(11) . . ? O11N W11 O11P 87.1(15) . . ? O112 W11 O11P 73.6(12) . . ? O116 W11 O11P 82.8(12) . . ? O119 W11 O11P 78.5(13) . . ? O11 W11 K1 54.3(8) . . ? O11N W11 K1 92.3(13) . . ? O112 W11 K1 155.0(10) . . ? O116 W11 K1 48.1(10) . . ? O119 W11 K1 93.7(11) . . ? O11P W11 K1 130.7(8) . . ? O12 W12 O123 97.9(16) . . ? O12 W12 O212 98.6(15) . . ? O123 W12 O212 88.9(13) . . ? O12 W12 O112 103.0(15) . . ? O123 W12 O112 158.9(12) . . ? O212 W12 O112 90.8(13) . . ? O12 W12 O127 102.0(14) . . ? O123 W12 O127 85.3(12) . . ? O212 W12 O127 159.1(12) . . ? O112 W12 O127 87.6(12) . . ? O12 W12 O11P 177.5(15) . . ? O123 W12 O11P 84.5(12) . . ? O212 W12 O11P 80.7(12) . . ? O112 W12 O11P 74.6(12) . . ? O127 W12 O11P 78.8(11) . . ? O12 W12 K2 40.8(12) . . ? O123 W12 K2 99.0(9) . . ? O212 W12 K2 57.9(9) . . ? O112 W12 K2 98.7(8) . . ? O127 W12 K2 142.8(8) . . ? O11P W12 K2 138.3(8) . . ? O13 W13 O313 101.4(15) . . ? O13 W13 O137 94.5(16) . . ? O313 W13 O137 164.0(13) . . ? O13 W13 O123 99.6(15) . . ? O313 W13 O123 91.4(12) . . ? O137 W13 O123 85.5(13) . . ? O13 W13 O134 101.3(16) . . ? O313 W13 O134 90.4(13) . . ? O137 W13 O134 86.8(13) . . ? O123 W13 O134 158.2(14) . . ? O13 W13 O13P 174.0(14) . . ? O313 W13 O13P 82.9(12) . . ? O137 W13 O13P 81.2(13) . . ? O123 W13 O13P 84.3(12) . . ? O134 W13 O13P 74.4(13) . . ? O14 W14 O414 98.1(13) . . ? O14 W14 O148 99.7(13) . . ? O414 W14 O148 161.8(12) . . ? O14 W14 O134 99.4(14) . . ? O414 W14 O134 92.8(13) . . ? O148 W14 O134 88.0(13) . . ? O14 W14 O145 100.7(14) . . ? O414 W14 O145 87.6(13) . . ? O148 W14 O145 85.4(13) . . ? O134 W14 O145 159.6(14) . . ? O14 W14 O13P 174.6(13) . . ? O414 W14 O13P 82.4(12) . . ? O148 W14 O13P 80.2(11) . . ? O134 W14 O13P 75.2(13) . . ? O145 W14 O13P 84.7(13) . . ? O14 W14 Na1 47.9(11) . . ? O414 W14 Na1 109.4(9) . . ? O148 W14 Na1 80.3(9) . . ? O134 W14 Na1 141.6(10) . . ? O145 W14 Na1 55.8(10) . . ? O13P W14 Na1 137.0(9) . . ? O15 W15 O145 103.2(15) . . ? O15 W15 O515 100.4(14) . . ? O145 W15 O515 89.8(14) . . ? O15 W15 O158 95.8(14) . . ? O145 W15 O158 88.4(14) . . ? O515 W15 O158 163.7(12) . . ? O15 W15 O156 97.9(14) . . ? O145 W15 O156 158.6(13) . . ? O515 W15 O156 90.2(14) . . ? O158 W15 O156 85.5(14) . . ? O15 W15 O15P 170.8(13) . . ? O145 W15 O15P 86.1(12) . . ? O515 W15 O15P 80.0(11) . . ? O158 W15 O15P 83.7(11) . . ? O156 W15 O15P 72.9(11) . . ? O16 W16 O616 97.3(15) . . ? O16 W16 O116 99.8(15) . . ? O616 W16 O116 90.3(13) . . ? O16 W16 O156 99.9(15) . . ? O616 W16 O156 92.6(13) . . ? O116 W16 O156 159.5(14) . . ? O16 W16 O169 96.4(15) . . ? O616 W16 O169 166.3(14) . . ? O116 W16 O169 87.0(13) . . ? O156 W16 O169 85.4(13) . . ? O16 W16 O15P 174.6(12) . . ? O616 W16 O15P 83.7(12) . . ? O116 W16 O15P 85.5(12) . . ? O156 W16 O15P 74.7(12) . . ? O169 W16 O15P 82.6(12) . . ? O16 W16 K1 50.7(11) . . ? O616 W16 K1 89.6(9) . . ? O116 W16 K1 49.6(10) . . ? O156 W16 K1 150.6(10) . . ? O169 W16 K1 98.8(10) . . ? O15P W16 K1 134.7(6) . . ? O17 W17 O127 103.4(16) . . ? O17 W17 O137 102.3(18) . . ? O127 W17 O137 86.4(13) . . ? O17 W17 O179 98.2(18) . . ? O127 W17 O179 86.3(13) . . ? O137 W17 O179 159.4(14) . . ? O17 W17 O178 101.5(16) . . ? O127 W17 O178 155.1(13) . . ? O137 W17 O178 90.0(13) . . ? O179 W17 O178 88.5(13) . . ? O17 W17 O17P 172.2(16) . . ? O127 W17 O17P 80.6(11) . . ? O137 W17 O17P 84.5(13) . . ? O179 W17 O17P 75.2(13) . . ? O178 W17 O17P 74.6(11) . . ? O18 W18 O189 99.5(16) . . ? O18 W18 O178 99.0(15) . . ? O189 W18 O178 89.4(14) . . ? O18 W18 O148 106.0(15) . . ? O189 W18 O148 154.6(12) . . ? O178 W18 O148 86.7(12) . . ? O18 W18 O158 102.3(15) . . ? O189 W18 O158 87.4(14) . . ? O178 W18 O158 158.7(12) . . ? O148 W18 O158 87.1(12) . . ? O18 W18 O17P 170.0(15) . . ? O189 W18 O17P 74.2(12) . . ? O178 W18 O17P 73.6(11) . . ? O148 W18 O17P 80.6(11) . . ? O158 W18 O17P 85.3(11) . . ? O19 W19 O119 104.8(17) . . ? O19 W19 O169 102.2(17) . . ? O119 W19 O169 89.3(16) . . ? O19 W19 O179 100.2(16) . . ? O119 W19 O179 90.8(15) . . ? O169 W19 O179 156.8(15) . . ? O19 W19 O189 98.4(15) . . ? O119 W19 O189 156.8(16) . . ? O169 W19 O189 85.0(14) . . ? O179 W19 O189 85.8(13) . . ? O19 W19 O17P 167.3(14) . . ? O119 W19 O17P 85.3(15) . . ? O169 W19 O17P 85.4(13) . . ? O179 W19 O17P 71.5(12) . . ? O189 W19 O17P 71.8(12) . . ? O11N Nd O11N 79.7(19) 2 . ? O11N Nd O6N 147.7(12) 2 . ? O11N Nd O6N 70.7(12) . . ? O11N Nd O6N 70.7(12) 2 2 ? O11N Nd O6N 147.7(12) . 2 ? O6N Nd O6N 140.8(14) . 2 ? O11N Nd O9N 138.0(11) 2 . ? O11N Nd O9N 113.9(12) . . ? O6N Nd O9N 68.9(9) . . ? O6N Nd O9N 81.9(9) 2 . ? O11N Nd O9N 113.9(12) 2 2 ? O11N Nd O9N 138.0(11) . 2 ? O6N Nd O9N 81.9(9) . 2 ? O6N Nd O9N 68.9(9) 2 2 ? O9N Nd O9N 83.1(13) . 2 ? O11N Nd O2N 72.1(12) 2 2 ? O11N Nd O2N 74.2(12) . 2 ? O6N Nd O2N 87.3(10) . 2 ? O6N Nd O2N 107.5(10) 2 2 ? O9N Nd O2N 148.6(9) . 2 ? O9N Nd O2N 73.2(10) 2 2 ? O11N Nd O2N 74.2(12) 2 . ? O11N Nd O2N 72.1(12) . . ? O6N Nd O2N 107.5(10) . . ? O6N Nd O2N 87.3(10) 2 . ? O9N Nd O2N 73.2(10) . . ? O9N Nd O2N 148.6(9) 2 . ? O2N Nd O2N 135.6(14) 2 . ? O3P P1 O7P 106.6(19) . . ? O3P P1 O2P 112.5(16) . . ? O7P P1 O2P 107.3(17) . . ? O3P P1 O5P 112.4(16) . . ? O7P P1 O5P 106.5(18) . . ? O2P P1 O5P 111.1(16) . . ? O13P P2 O11P 112.4(18) . . ? O13P P2 O15P 111.6(18) . . ? O11P P2 O15P 109.8(17) . . ? O13P P2 O17P 107.4(18) . . ? O11P P2 O17P 107.2(17) . . ? O15P P2 O17P 108.2(16) . . ? W2 O2 K2 115.2(14) . . ? W2 O2 K1 102.5(14) . 2 ? K2 O2 K1 97.3(10) . 2 ? W3 O3 K1 137.2(18) . 6_566 ? W3 O3 K2 106.2(15) . 5_566 ? K1 O3 K2 95.7(10) 6_566 5_566 ? W4 O4 Na1 105.0(16) . 7_566 ? W5 O5 Na2 138.6(19) . . ? W7 O7 K2 105.8(15) . 5_566 ? W11 O11 K2 162.1(14) . 2 ? W11 O11 K1 97.7(10) . . ? K2 O11 K1 94.4(8) 2 . ? W12 O12 K2 115.5(17) . . ? W14 O14 Na1 104.9(15) . . ? W14 O14 Na2 142.9(16) . 7_566 ? Na1 O14 Na2 89.7(10) . 7_566 ? W16 O16 K1 102.0(14) . . ? W17 O17 Na2 130.9(19) . 1_545 ? W2 O2N Nd 138.1(14) . . ? W2 O2N K1 97.5(12) . 2 ? Nd O2N K1 124.0(11) . 2 ? W6 O6N Nd 156.6(16) . . ? W9 O9N Nd 159.6(14) . . ? W11 O11N Nd 151(2) . . ? P1 O2P W2 133.7(16) . . ? P1 O3P W4 132.9(17) . . ? P1 O3P W3 124.3(15) . . ? W4 O3P W3 90.7(10) . . ? P1 O5P W6 128.8(16) . . ? P1 O5P W5 125.1(17) . . ? W6 O5P W5 95.3(11) . . ? P1 O7P W7 126(2) . . ? P1 O7P W9 123(2) . . ? W7 O7P W9 92.4(12) . . ? P1 O7P W8 123.4(18) . . ? W7 O7P W8 91.1(13) . . ? W9 O7P W8 91.3(12) . . ? P2 O11P W12 128.1(19) . . ? P2 O11P W11 130.8(18) . . ? W12 O11P W11 88.8(10) . . ? P2 O13P W14 129.1(18) . . ? P2 O13P W13 127.6(19) . . ? W14 O13P W13 89.4(12) . . ? P2 O15P W16 129.1(16) . . ? P2 O15P W15 125.5(15) . . ? W16 O15P W15 91.2(9) . . ? P2 O17P W17 126.1(16) . . ? P2 O17P W19 122.6(17) . . ? W17 O17P W19 92.1(11) . . ? P2 O17P W18 124.7(17) . . ? W17 O17P W18 90.6(10) . . ? W19 O17P W18 90.7(10) . . ? W12 O112 W11 121.5(16) . . ? W16 O116 W11 155.3(19) . . ? W16 O116 K1 99.6(13) . . ? W11 O116 K1 100.2(12) . . ? W19 O119 W11 153(2) . . ? W12 O123 W13 151.7(17) . . ? W17 O127 W12 153.3(17) . . ? W14 O134 W13 120.6(17) . . ? W17 O137 W13 150.5(18) . . ? W15 O145 W14 151(2) . . ? W14 O148 W18 152.3(16) . . ? W16 O156 W15 120.7(16) . . ? W15 O158 W18 147.6(18) . . ? W19 O169 W16 145.8(18) . . ? W18 O178 W17 121.2(15) . . ? W17 O179 W19 121.2(17) . . ? W18 O189 W19 123.2(17) . . ? W12 O212 W2 166.3(19) . . ? W12 O212 K2 92.4(11) . . ? W2 O212 K2 92.9(10) . . ? W3 O230 W2 149.5(15) . . ? W7 O270 W2 151.7(16) . . ? W13 O313 W3 157.7(17) . . ? W4 O340 W3 119.6(19) . . ? W3 O370 W7 148(2) . . ? W3 O370 K2 96.2(12) . 5_566 ? W7 O370 K2 91.1(11) . 5_566 ? W14 O414 W4 163.8(17) . . ? W4 O450 W5 148.4(16) . . ? W8 O480 W4 152(2) . . ? W15 O515 W5 163.2(19) . . ? W5 O560 W6 123.0(14) . . ? W5 O580 W8 156(2) . . ? W16 O616 W6 157.0(16) . . ? W6 O690 W9 140.7(17) . . ? W8 O780 W7 121.3(18) . . ? W7 O790 W9 124.4(14) . . ? W8 O890 W9 123.2(18) . . ? O3 K1 O903 157.0(12) 6_565 . ? O3 K1 O116 96.4(11) 6_565 . ? O903 K1 O116 104.7(11) . . ? O3 K1 O2 75.7(10) 6_565 2 ? O903 K1 O2 98.7(10) . 2 ? O116 K1 O2 125.4(10) . 2 ? O3 K1 O16 92.7(10) 6_565 . ? O903 K1 O16 90.8(10) . . ? O116 K1 O16 57.8(10) . . ? O2 K1 O16 168.1(10) 2 . ? O3 K1 O2N 118.6(10) 6_565 2 ? O903 K1 O2N 72.9(9) . 2 ? O116 K1 O2N 85.8(9) . 2 ? O2 K1 O2N 55.4(9) 2 2 ? O16 K1 O2N 135.1(10) . 2 ? O3 K1 O11 68.9(9) 6_565 . ? O903 K1 O11 130.4(9) . . ? O116 K1 O11 59.0(8) . . ? O2 K1 O11 68.2(8) 2 . ? O16 K1 O11 110.6(9) . . ? O2N K1 O11 60.3(8) 2 . ? O3 K1 O906 79.9(10) 6_565 . ? O903 K1 O906 78.6(11) . . ? O116 K1 O906 175.2(10) . . ? O2 K1 O906 56.8(9) 2 . ? O16 K1 O906 119.1(10) . . ? O2N K1 O906 98.7(9) 2 . ? O11 K1 O906 121.6(9) . . ? O3 K1 W16 97.9(8) 6_565 . ? O903 K1 W16 95.6(8) . . ? O116 K1 W16 30.8(6) . . ? O2 K1 W16 155.6(7) 2 . ? O16 K1 W16 27.2(7) . . ? O2N K1 W16 111.4(7) 2 . ? O11 K1 W16 87.5(5) . . ? O906 K1 W16 146.3(7) . . ? O3 K1 W2 100.9(7) 6_565 2 ? O903 K1 W2 80.3(7) . 2 ? O116 K1 W2 110.7(7) . 2 ? O2 K1 W2 28.0(6) 2 2 ? O16 K1 W2 163.3(8) . 2 ? O2N K1 W2 28.5(6) 2 2 ? O11 K1 W2 66.5(5) . 2 ? O906 K1 W2 73.2(6) . 2 ? W16 K1 W2 139.1(3) . 2 ? O3 K1 W11 85.3(8) 6_565 . ? O903 K1 W11 117.6(8) . . ? O116 K1 W11 31.7(6) . . ? O2 K1 W11 93.8(7) 2 . ? O16 K1 W11 87.9(8) . . ? O2N K1 W11 65.5(6) 2 . ? O11 K1 W11 28.0(5) . . ? O906 K1 W11 149.5(7) . . ? W16 K1 W11 61.95(17) . . ? W2 K1 W11 83.8(2) 2 . ? O3 K1 W3 16.5(8) 6_565 6_565 ? O903 K1 W3 140.7(9) . 6_565 ? O116 K1 W3 109.9(7) . 6_565 ? O2 K1 W3 76.0(7) 2 6_565 ? O16 K1 W3 92.2(7) . 6_565 ? O2N K1 W3 127.0(7) 2 6_565 ? O11 K1 W3 84.5(5) . 6_565 ? O906 K1 W3 65.9(7) . 6_565 ? W16 K1 W3 104.6(2) . 6_565 ? W2 K1 W3 103.6(3) 2 6_565 ? W11 K1 W3 101.7(3) . 6_565 ? O11 K2 O910 69.2(14) 2 . ? O11 K2 O12 101.8(10) 2 . ? O910 K2 O12 106.3(14) . . ? O11 K2 O2 73.0(9) 2 . ? O910 K2 O2 136.2(14) . . ? O12 K2 O2 102.3(10) . . ? O11 K2 O7 158.8(10) 2 5_566 ? O910 K2 O7 89.7(14) . 5_566 ? O12 K2 O7 81.3(10) . 5_566 ? O2 K2 O7 127.2(11) . 5_566 ? O11 K2 O3 68.8(9) 2 5_566 ? O910 K2 O3 75.2(13) . 5_566 ? O12 K2 O3 169.5(11) . 5_566 ? O2 K2 O3 71.0(9) . 5_566 ? O7 K2 O3 109.2(10) 5_566 5_566 ? O11 K2 O906 130.8(9) 2 6_566 ? O910 K2 O906 159.1(15) . 6_566 ? O12 K2 O906 67.3(10) . 6_566 ? O2 K2 O906 63.9(9) . 6_566 ? O7 K2 O906 69.9(10) 5_566 6_566 ? O3 K2 O906 114.9(10) 5_566 6_566 ? O11 K2 O370 117.3(8) 2 5_566 ? O910 K2 O370 75.0(13) . 5_566 ? O12 K2 O370 137.5(10) . 5_566 ? O2 K2 O370 104.4(9) . 5_566 ? O7 K2 O370 56.2(9) 5_566 5_566 ? O3 K2 O370 53.0(9) 5_566 5_566 ? O906 K2 O370 96.2(9) 6_566 5_566 ? O11 K2 O212 70.8(8) 2 . ? O910 K2 O212 128.6(14) . . ? O12 K2 O212 53.2(9) . . ? O2 K2 O212 52.6(8) . . ? O7 K2 O212 124.7(9) 5_566 . ? O3 K2 O212 117.5(9) 5_566 . ? O906 K2 O212 64.8(9) 6_566 . ? O370 K2 O212 154.3(9) 5_566 . ? O11 K2 W7 147.6(6) 2 5_566 ? O910 K2 W7 88.8(12) . 5_566 ? O12 K2 W7 107.2(8) . 5_566 ? O2 K2 W7 113.5(7) . 5_566 ? O7 K2 W7 26.7(7) 5_566 5_566 ? O3 K2 W7 83.2(7) 5_566 5_566 ? O906 K2 W7 75.1(7) 6_566 5_566 ? O370 K2 W7 31.1(6) 5_566 5_566 ? O212 K2 W7 139.6(7) . 5_566 ? O11 K2 W3 93.8(6) 2 5_566 ? O910 K2 W3 80.5(11) . 5_566 ? O12 K2 W3 164.4(9) . 5_566 ? O2 K2 W3 80.6(6) . 5_566 ? O7 K2 W3 84.7(7) 5_566 5_566 ? O3 K2 W3 25.2(7) 5_566 5_566 ? O906 K2 W3 101.2(7) 6_566 5_566 ? O370 K2 W3 29.6(6) 5_566 5_566 ? O212 K2 W3 133.1(6) . 5_566 ? W7 K2 W3 58.27(15) 5_566 5_566 ? O11 K2 W12 86.7(5) 2 . ? O910 K2 W12 117.9(12) . . ? O12 K2 W12 23.7(7) . . ? O2 K2 W12 80.6(6) . . ? O7 K2 W12 101.8(7) 5_566 . ? O3 K2 W12 146.6(8) 5_566 . ? O906 K2 W12 64.5(7) 6_566 . ? O370 K2 W12 156.0(7) 5_566 . ? O212 K2 W12 29.6(5) . . ? W7 K2 W12 125.2(3) 5_566 . ? W3 K2 W12 160.2(3) 5_566 . ? O4 Na1 O920 77.1(9) 7_566 . ? O4 Na1 O14 152.9(14) 7_566 . ? O920 Na1 O14 75.8(9) . . ? O4 Na1 W4 28.3(8) 7_566 7_566 ? O920 Na1 W4 76.7(5) . 7_566 ? O14 Na1 W4 139.9(12) . 7_566 ? O4 Na1 W14 140.4(11) 7_566 . ? O920 Na1 W14 74.4(5) . . ? O14 Na1 W14 27.1(7) . . ? W4 Na1 W14 151.0(8) 7_566 . ? O4 Na1 Na2 145.6(11) 7_566 7_566 ? O920 Na1 Na2 107.2(9) . 7_566 ? O14 Na1 Na2 46.7(8) . 7_566 ? W4 Na1 Na2 117.9(7) 7_566 7_566 ? W14 Na1 Na2 70.3(5) . 7_566 ? O5 Na2 O908 68.7(15) . . ? O5 Na2 O17 127.3(13) . 1_565 ? O908 Na2 O17 133.8(17) . 1_565 ? O5 Na2 O14 65.4(11) . 7_566 ? O908 Na2 O14 80.5(14) . 7_566 ? O17 Na2 O14 144.9(14) 1_565 7_566 ? O5 Na2 Na1 48.5(10) . 7_566 ? O908 Na2 Na1 106.0(14) . 7_566 ? O17 Na2 Na1 115.5(12) 1_565 7_566 ? O14 Na2 Na1 43.5(7) 7_566 7_566 ? K2 O906 K1 149.6(12) 6_565 . ? Na1 O920 Na1 180.0(11) . 7_566 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W2 O2N 1.73(3) . ? W2 O2 1.73(3) . ? W2 O212 1.89(3) . ? W2 O270 1.99(3) . ? W2 O230 2.08(3) . ? W2 O2P 2.13(2) . ? W2 K1 3.592(9) 2 ? W2 K2 3.844(11) . ? W3 O3 1.70(3) . ? W3 O230 1.83(3) . ? W3 O370 1.90(3) . ? W3 O313 1.93(3) . ? W3 O340 1.97(4) . ? W3 O3P 2.41(3) . ? W3 K2 3.819(9) 5_566 ? W3 K1 4.065(11) 6_566 ? W4 O4 1.77(3) . ? W4 O450 1.87(3) . ? W4 O480 1.91(4) . ? W4 O340 1.92(4) . ? W4 O414 1.94(3) . ? W4 O3P 2.31(3) . ? W4 Na1 3.61(2) 7_566 ? W5 O5 1.66(4) . ? W5 O560 1.80(3) . ? W5 O580 1.89(3) . ? W5 O515 1.91(3) . ? W5 O450 1.95(3) . ? W5 O5P 2.37(3) . ? W6 O6 1.70(4) . ? W6 O6N 1.74(3) . ? W6 O690 1.91(3) . ? W6 O616 1.95(3) . ? W6 O560 2.11(3) . ? W6 O5P 2.28(3) . ? W7 O7 1.72(3) . ? W7 O270 1.85(3) . ? W7 O790 1.91(3) . ? W7 O370 1.90(3) . ? W7 O780 1.93(3) . ? W7 O7P 2.29(3) . ? W7 K2 3.681(11) 5_566 ? W8 O8 1.74(5) . ? W8 O890 1.88(4) . ? W8 O480 1.92(4) . ? W8 O580 1.92(3) . ? W8 O780 1.93(3) . ? W8 O7P 2.42(4) . ? W9 O9 1.69(3) . ? W9 O9N 1.71(3) . ? W9 O690 1.93(3) . ? W9 O790 1.96(3) . ? W9 O890 2.08(4) . ? W9 O7P 2.45(4) . ? W11 O11 1.74(3) . ? W11 O11N 1.78(4) . ? W11 O112 1.89(3) . ? W11 O116 1.96(3) . ? W11 O119 2.07(4) . ? W11 O11P 2.40(3) . ? W11 K1 3.664(11) . ? W12 O12 1.70(3) . ? W12 O123 1.89(3) . ? W12 O212 1.90(3) . ? W12 O112 1.92(3) . ? W12 O127 1.96(3) . ? W12 O11P 2.34(3) . ? W12 K2 3.833(9) . ? W13 O13 1.67(4) . ? W13 O313 1.88(3) . ? W13 O137 1.94(3) . ? W13 O123 1.93(3) . ? W13 O134 1.94(3) . ? W13 O13P 2.39(3) . ? W14 O14 1.74(3) . ? W14 O414 1.86(3) . ? W14 O148 1.89(3) . ? W14 O134 1.91(3) . ? W14 O145 1.93(3) . ? W14 O13P 2.37(3) . ? W14 Na1 3.70(2) . ? W15 O15 1.65(3) . ? W15 O145 1.88(3) . ? W15 O515 1.87(3) . ? W15 O158 1.87(3) . ? W15 O156 1.92(3) . ? W15 O15P 2.40(3) . ? W16 O16 1.68(4) . ? W16 O616 1.86(3) . ? W16 O116 1.86(3) . ? W16 O156 1.94(3) . ? W16 O169 1.98(3) . ? W16 O15P 2.30(3) . ? W16 K1 3.584(10) . ? W17 O17 1.72(4) . ? W17 O127 1.87(3) . ? W17 O137 1.91(3) . ? W17 O179 1.90(3) . ? W17 O178 1.97(3) . ? W17 O17P 2.33(3) . ? W18 O18 1.70(3) . ? W18 O189 1.87(4) . ? W18 O178 1.91(3) . ? W18 O148 1.95(3) . ? W18 O158 1.98(3) . ? W18 O17P 2.41(3) . ? W19 O19 1.74(4) . ? W19 O119 1.81(4) . ? W19 O169 1.86(3) . ? W19 O179 2.02(3) . ? W19 O189 2.03(3) . ? W19 O17P 2.40(3) . ? Nd O11N 2.38(4) 2 ? Nd O11N 2.38(4) . ? Nd O6N 2.45(3) . ? Nd O6N 2.45(3) 2 ? Nd O9N 2.47(3) . ? Nd O9N 2.47(3) 2 ? Nd O2N 2.47(3) 2 ? Nd O2N 2.47(3) . ? P1 O3P 1.48(3) . ? P1 O7P 1.58(4) . ? P1 O2P 1.56(3) . ? P1 O5P 1.58(3) . ? P2 O13P 1.50(4) . ? P2 O11P 1.53(3) . ? P2 O15P 1.57(3) . ? P2 O17P 1.57(3) . ? O2 K2 2.78(3) . ? O2 K1 2.80(3) 2 ? O3 K1 2.65(4) 6_566 ? O3 K2 2.98(3) 5_566 ? O4 Na1 2.71(4) 7_566 ? O5 Na2 2.74(5) . ? O7 K2 2.82(4) 5_566 ? O11 K2 2.69(3) 2 ? O11 K1 3.00(3) . ? O12 K2 2.78(3) . ? O14 Na1 2.84(4) . ? O14 Na2 3.01(4) 7_566 ? O16 K1 2.84(3) . ? O17 Na2 2.91(5) 1_545 ? O2N K1 2.93(3) 2 ? O116 K1 2.77(4) . ? O212 K2 3.25(3) . ? O370 K2 3.12(3) 5_566 ? K1 O3 2.65(4) 6_565 ? K1 O903 2.68(4) . ? K1 O2 2.80(3) 2 ? K1 O2N 2.93(3) 2 ? K1 O906 3.02(4) . ? K1 W2 3.592(9) 2 ? K1 W3 4.065(11) 6_565 ? K2 O11 2.69(3) 2 ? K2 O910 2.75(6) . ? K2 O7 2.82(4) 5_566 ? K2 O3 2.98(3) 5_566 ? K2 O906 2.99(4) 6_566 ? K2 O370 3.12(3) 5_566 ? K2 W7 3.681(11) 5_566 ? K2 W3 3.819(9) 5_566 ? Na1 O4 2.71(4) 7_566 ? Na1 O920 2.79(3) . ? Na1 W4 3.61(2) 7_566 ? Na1 Na2 4.13(4) 7_566 ? Na2 O908 2.81(6) . ? Na2 O17 2.91(5) 1_565 ? Na2 O14 3.01(4) 7_566 ? Na2 Na1 4.13(4) 7_566 ? O906 K2 2.99(4) 6_565 ? O920 Na1 2.79(3) 7_566 ?
1100738.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $ #$Revision: 176435 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100738.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100738 loop_ _publ_author_name 'Yutaka Hitomi' 'Akira Ando' 'Hajime Matsui' 'Tomoyuki Ito' 'Tsunehiro Tanaka' 'Seiji Ogo' 'Takuzo Funabiki' _publ_contact_author_email hitomi@moleng.kyoto-u.ac.jp _publ_contact_author_fax +81-75-383-2563 _publ_contact_author_name 'Yutaka Hitomi' _publ_contact_author_phone +81-75-383-2563 _publ_section_title ; Aerobic Catechol Oxidation Catalyzed by a Bis(\m-oxo)dimanganese(III,III) Complex via a Manganese(II)-Semiquinonate Complex ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3473 _journal_page_last 3478 _journal_paper_doi 10.1021/ic050109d _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C58 H61 B Mn N5 O2' _chemical_formula_weight 925.90 _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _cell_angle_alpha 94.841(3) _cell_angle_beta 101.952(4) _cell_angle_gamma 97.012(4) _cell_formula_units_Z 2 _cell_length_a 13.236(2) _cell_length_b 13.659(2) _cell_length_c 14.778(2) _cell_measurement_reflns_used 12071 _cell_measurement_temperature 223.2 _cell_measurement_theta_max 27.5 _cell_measurement_theta_min 3.0 _cell_volume 2577.7(6) _computing_cell_refinement CRYSTALCLEAR _computing_data_collection CRYSTALCLEAR _computing_data_reduction 'teXsan Ver. 1.11' _computing_publication_material 'teXsan Ver. 1.11' _computing_structure_refinement 'teXsan Ver. 1.10' _computing_structure_solution SIR92 _diffrn_detector_area_resol_mean 14.71 _diffrn_measured_fraction_theta_full 0.9696 _diffrn_measured_fraction_theta_max 0.9696 _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents 0.025 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 27791 _diffrn_reflns_theta_full 27.49 _diffrn_reflns_theta_max 27.49 _exptl_absorpt_coefficient_mu 0.302 _exptl_absorpt_correction_T_max 0.941 _exptl_absorpt_correction_T_min 0.725 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details RICABA _exptl_crystal_colour green _exptl_crystal_density_diffrn 1.193 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Prism _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.150 _refine_diff_density_max 0.62 _refine_diff_density_min -0.38 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.618 _refine_ls_hydrogen_treatment noref _refine_ls_number_parameters 604 _refine_ls_number_reflns 8632 _refine_ls_R_factor_gt 0.0554 _refine_ls_shift/su_max 0.0009 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.03000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.1279 _reflns_number_gt 8632 _reflns_number_total 11438 _reflns_threshold_expression F^2^>2.0\s(F^2^) _cod_data_source_file ic050109dsi20050124_043757_1.cif _cod_data_source_block '_nstr654_MnTPA35DBSQBPh4_M' _cod_original_cell_volume 2577.7(7) _cod_original_sg_symbol_H-M 'P -1 ' _cod_original_formula_sum 'C58 H61 B N5 Mn O2 ' _cod_database_code 1100738 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn(1) Mn 0.26390(3) 0.26719(3) 0.27575(3) 0.0353(1) Uani 1.00 d . . . O(1) O 0.1132(1) 0.2111(1) 0.2895(1) 0.0446(5) Uani 1.00 d . . . O(2) O 0.2818(1) 0.1309(1) 0.3407(1) 0.0406(5) Uani 1.00 d . . . N(1) N 0.3803(1) 0.3785(1) 0.2189(1) 0.0324(5) Uani 1.00 d . . . N(2) N 0.1865(1) 0.4047(1) 0.2435(1) 0.0381(6) Uani 1.00 d . . . N(3) N 0.2807(1) 0.1935(1) 0.1422(1) 0.0349(6) Uani 1.00 d . . . N(4) N 0.4079(2) 0.3204(2) 0.3906(1) 0.0475(7) Uani 1.00 d . . . N(5) N 0.1772(7) 0.462(1) 0.5164(10) 0.542(9) Uani 1.00 d . . . C(1) C 0.1017(2) 0.1227(2) 0.3127(2) 0.0342(7) Uani 1.00 d . . . C(2) C 0.1957(2) 0.0783(2) 0.3427(2) 0.0310(6) Uani 1.00 d . . . C(3) C 0.1871(2) -0.0192(2) 0.3724(2) 0.0321(6) Uani 1.00 d . . . C(4) C 0.0880(2) -0.0668(2) 0.3653(2) 0.0352(7) Uani 1.00 d . . . C(5) C -0.0053(2) -0.0257(2) 0.3331(2) 0.0330(6) Uani 1.00 d . . . C(6) C 0.0025(2) 0.0680(2) 0.3082(2) 0.0373(7) Uani 1.00 d . . . C(7) C -0.1108(2) -0.0892(2) 0.3261(2) 0.0407(7) Uani 1.00 d . . . C(8) C -0.2017(2) -0.0310(2) 0.2970(2) 0.0612(10) Uani 1.00 d . . . C(9) C -0.1173(2) -0.1239(2) 0.4199(2) 0.063(1) Uani 1.00 d . . . C(10) C -0.1219(2) -0.1766(3) 0.2524(3) 0.082(1) Uani 1.00 d . . . C(11) C 0.2851(2) -0.0645(2) 0.4097(2) 0.0417(7) Uani 1.00 d . . . C(12) C 0.2586(2) -0.1666(2) 0.4416(3) 0.073(1) Uani 1.00 d . . . C(13) C 0.3526(2) 0.0025(2) 0.4935(2) 0.0488(8) Uani 1.00 d . . . C(14) C 0.3483(2) -0.0765(2) 0.3338(2) 0.064(1) Uani 1.00 d . . . C(15) C 0.3628(2) 0.4799(2) 0.2478(2) 0.0384(7) Uani 1.00 d . . . C(16) C 0.3581(2) 0.3561(2) 0.1173(2) 0.0366(7) Uani 1.00 d . . . C(17) C 0.4854(2) 0.3622(2) 0.2623(2) 0.0404(7) Uani 1.00 d . . . C(18) C 0.2492(2) 0.4881(2) 0.2393(2) 0.0342(7) Uani 1.00 d . . . C(19) C 0.2124(2) 0.5779(2) 0.2287(2) 0.0426(8) Uani 1.00 d . . . C(20) C 0.1079(2) 0.5821(2) 0.2217(2) 0.0503(9) Uani 1.00 d . . . C(21) C 0.0422(2) 0.4963(2) 0.2231(2) 0.0493(8) Uani 1.00 d . . . C(22) C 0.0845(2) 0.4096(2) 0.2338(2) 0.0453(8) Uani 1.00 d . . . C(23) C 0.3294(2) 0.2464(2) 0.0872(2) 0.0331(6) Uani 1.00 d . . . C(24) C 0.3489(2) 0.2036(2) 0.0058(2) 0.0400(7) Uani 1.00 d . . . C(25) C 0.3172(2) 0.1034(2) -0.0206(2) 0.0452(8) Uani 1.00 d . . . C(26) C 0.2668(2) 0.0483(2) 0.0349(2) 0.0429(7) Uani 1.00 d . . . C(27) C 0.2506(2) 0.0958(2) 0.1149(2) 0.0407(7) Uani 1.00 d . . . C(28) C 0.4953(2) 0.3575(2) 0.3652(2) 0.0422(7) Uani 1.00 d . . . C(29) C 0.5882(2) 0.3867(2) 0.4289(2) 0.0547(9) Uani 1.00 d . . . C(30) C 0.5931(3) 0.3757(2) 0.5209(2) 0.067(1) Uani 1.00 d . . . C(31) C 0.5056(3) 0.3361(2) 0.5479(2) 0.067(1) Uani 1.00 d . . . C(32) C 0.4149(3) 0.3095(2) 0.4812(2) 0.0620(10) Uani 1.00 d . . . C(33) C 0.3796(2) -0.2806(2) 0.0518(2) 0.0329(6) Uani 1.00 d . . . C(34) C 0.4191(2) -0.1940(2) 0.1134(2) 0.0420(7) Uani 1.00 d . . . C(35) C 0.5048(2) -0.1877(2) 0.1866(2) 0.0524(9) Uani 1.00 d . . . C(36) C 0.5563(2) -0.2682(3) 0.2016(2) 0.0539(9) Uani 1.00 d . . . C(37) C 0.5218(2) -0.3549(2) 0.1422(2) 0.0512(9) Uani 1.00 d . . . C(38) C 0.4349(2) -0.3600(2) 0.0695(2) 0.0406(7) Uani 1.00 d . . . C(39) C 0.2278(2) -0.4056(2) -0.0605(2) 0.0335(6) Uani 1.00 d . . . C(40) C 0.1551(2) -0.4482(2) -0.0122(2) 0.0367(7) Uani 1.00 d . . . C(41) C 0.1199(2) -0.5488(2) -0.0223(2) 0.0415(7) Uani 1.00 d . . . C(42) C 0.1540(2) -0.6130(2) -0.0827(2) 0.0472(8) Uani 1.00 d . . . C(43) C 0.2235(2) -0.5748(2) -0.1324(2) 0.0539(9) Uani 1.00 d . . . C(44) C 0.2599(2) -0.4733(2) -0.1208(2) 0.0474(8) Uani 1.00 d . . . C(45) C 0.3163(2) -0.2408(2) -0.1245(2) 0.0361(7) Uani 1.00 d . . . C(46) C 0.2656(2) -0.2701(2) -0.2171(2) 0.0470(8) Uani 1.00 d . . . C(47) C 0.2945(2) -0.2257(3) -0.2909(2) 0.0584(10) Uani 1.00 d . . . C(48) C 0.3764(3) -0.1504(3) -0.2758(2) 0.062(1) Uani 1.00 d . . . C(49) C 0.4293(2) -0.1189(2) -0.1849(2) 0.0565(10) Uani 1.00 d . . . C(50) C 0.3994(2) -0.1637(2) -0.1118(2) 0.0433(8) Uani 1.00 d . . . C(51) C 0.1871(2) -0.2258(2) -0.0084(2) 0.0306(6) Uani 1.00 d . . . C(52) C 0.1118(2) -0.1939(2) -0.0763(2) 0.0385(7) Uani 1.00 d . . . C(53) C 0.0313(2) -0.1473(2) -0.0561(2) 0.0474(8) Uani 1.00 d . . . C(54) C 0.0214(2) -0.1290(2) 0.0347(2) 0.0462(8) Uani 1.00 d . . . C(55) C 0.0940(2) -0.1591(2) 0.1050(2) 0.0411(7) Uani 1.00 d . . . C(56) C 0.1740(2) -0.2070(2) 0.0825(2) 0.0349(7) Uani 1.00 d . . . C(57) C -0.0121(6) 0.3405(5) 0.4427(5) 0.180(3) Uani 1.00 d . . . C(58) C 0.1006(8) 0.4048(7) 0.4819(5) 0.191(4) Uani 1.00 d . . . B(1) B 0.2784(2) -0.2877(2) -0.0357(2) 0.0319(7) Uani 1.00 d . . . H(1) H 0.0808 -0.1321 0.3831 0.0422 Uiso 1.00 calc . . . H(2) H -0.0589 0.0969 0.2878 0.0447 Uiso 1.00 calc . . . H(3) H 0.2588 0.6360 0.2263 0.0512 Uiso 1.00 calc . . . H(4) H 0.0814 0.6433 0.2159 0.0604 Uiso 1.00 calc . . . H(5) H -0.0306 0.4968 0.2169 0.0591 Uiso 1.00 calc . . . H(6) H 0.0389 0.3503 0.2343 0.0544 Uiso 1.00 calc . . . H(7) H 0.3838 0.2427 -0.0317 0.0479 Uiso 1.00 calc . . . H(8) H 0.3301 0.0729 -0.0765 0.0542 Uiso 1.00 calc . . . H(9) H 0.2438 -0.0207 0.0181 0.0514 Uiso 1.00 calc . . . H(10) H 0.2163 0.0576 0.1534 0.0488 Uiso 1.00 calc . . . H(11) H 0.6484 0.4144 0.4092 0.0656 Uiso 1.00 calc . . . H(12) H 0.6567 0.3954 0.5656 0.0804 Uiso 1.00 calc . . . H(13) H 0.5075 0.3272 0.6112 0.0798 Uiso 1.00 calc . . . H(14) H 0.3540 0.2821 0.5000 0.0744 Uiso 1.00 calc . . . H(15) H 0.3853 -0.1369 0.1044 0.0504 Uiso 1.00 calc . . . H(16) H 0.5281 -0.1274 0.2267 0.0629 Uiso 1.00 calc . . . H(17) H 0.6148 -0.2644 0.2520 0.0647 Uiso 1.00 calc . . . H(18) H 0.5573 -0.4109 0.1509 0.0614 Uiso 1.00 calc . . . H(19) H 0.4121 -0.4206 0.0300 0.0487 Uiso 1.00 calc . . . H(20) H 0.1292 -0.4058 0.0291 0.0440 Uiso 1.00 calc . . . H(21) H 0.0719 -0.5740 0.0127 0.0499 Uiso 1.00 calc . . . H(22) H 0.1299 -0.6822 -0.0898 0.0566 Uiso 1.00 calc . . . H(23) H 0.2471 -0.6178 -0.1750 0.0647 Uiso 1.00 calc . . . H(24) H 0.3087 -0.4493 -0.1555 0.0569 Uiso 1.00 calc . . . H(25) H 0.2088 -0.3227 -0.2303 0.0564 Uiso 1.00 calc . . . H(26) H 0.2568 -0.2479 -0.3527 0.0700 Uiso 1.00 calc . . . H(27) H 0.3965 -0.1206 -0.3263 0.0740 Uiso 1.00 calc . . . H(28) H 0.4861 -0.0664 -0.1726 0.0678 Uiso 1.00 calc . . . H(29) H 0.4373 -0.1409 -0.0502 0.0520 Uiso 1.00 calc . . . H(30) H 0.1164 -0.2050 -0.1396 0.0462 Uiso 1.00 calc . . . H(31) H -0.0180 -0.1275 -0.1051 0.0569 Uiso 1.00 calc . . . H(32) H -0.0338 -0.0964 0.0488 0.0555 Uiso 1.00 calc . . . H(33) H 0.0891 -0.1471 0.1681 0.0493 Uiso 1.00 calc . . . H(34) H 0.2222 -0.2279 0.1315 0.0419 Uiso 1.00 calc . . . H(35) H -0.1967 0.0238 0.3425 0.0735 Uiso 1.00 calc . . . H(36) H -0.1992 -0.0077 0.2386 0.0735 Uiso 1.00 calc . . . H(37) H -0.2658 -0.0732 0.2918 0.0735 Uiso 1.00 calc . . . H(38) H -0.1105 -0.0679 0.4646 0.0753 Uiso 1.00 calc . . . H(39) H -0.1827 -0.1637 0.4148 0.0753 Uiso 1.00 calc . . . H(40) H -0.0627 -0.1619 0.4389 0.0753 Uiso 1.00 calc . . . H(41) H -0.1875 -0.2165 0.2464 0.0990 Uiso 1.00 calc . . . H(42) H -0.1177 -0.1529 0.1945 0.0990 Uiso 1.00 calc . . . H(43) H -0.0675 -0.2152 0.2702 0.0990 Uiso 1.00 calc . . . H(44) H 0.2203 -0.1603 0.4890 0.0878 Uiso 1.00 calc . . . H(45) H 0.2178 -0.2106 0.3903 0.0878 Uiso 1.00 calc . . . H(46) H 0.3212 -0.1921 0.4653 0.0878 Uiso 1.00 calc . . . H(47) H 0.4136 -0.0259 0.5163 0.0585 Uiso 1.00 calc . . . H(48) H 0.3718 0.0660 0.4754 0.0585 Uiso 1.00 calc . . . H(49) H 0.3144 0.0091 0.5409 0.0585 Uiso 1.00 calc . . . H(50) H 0.4090 -0.1049 0.3578 0.0767 Uiso 1.00 calc . . . H(51) H 0.3067 -0.1187 0.2816 0.0767 Uiso 1.00 calc . . . H(52) H 0.3681 -0.0133 0.3153 0.0767 Uiso 1.00 calc . . . H(53) H -0.0600 0.3825 0.4168 0.2166 Uiso 1.00 calc . . . H(54) H -0.0076 0.2901 0.3959 0.2166 Uiso 1.00 calc . . . H(55) H -0.0354 0.3110 0.4920 0.2166 Uiso 1.00 calc . . . H(56) H 0.3983 0.4983 0.3108 0.0461 Uiso 1.00 calc . . . H(57) H 0.3904 0.5240 0.2096 0.0461 Uiso 1.00 calc . . . H(58) H 0.3017 0.3890 0.0907 0.0440 Uiso 1.00 calc . . . H(59) H 0.4184 0.3797 0.0956 0.0440 Uiso 1.00 calc . . . H(60) H 0.4995 0.3015 0.2346 0.0485 Uiso 1.00 calc . . . H(61) H 0.5343 0.4154 0.2530 0.0485 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Mn(1) 0.0376(2) 0.0321(2) 0.0372(2) 0.0005(2) 0.0112(2) 0.0089(2) O(1) 0.0381(9) 0.038(1) 0.061(1) 0.0047(8) 0.0119(8) 0.0204(9) O(2) 0.0307(9) 0.044(1) 0.047(1) -0.0001(7) 0.0092(8) 0.0162(8) N(1) 0.033(1) 0.030(1) 0.034(1) 0.0026(8) 0.0063(8) 0.0043(9) N(2) 0.038(1) 0.033(1) 0.045(1) 0.0030(9) 0.0111(9) 0.0108(9) N(3) 0.037(1) 0.032(1) 0.036(1) 0.0007(9) 0.0092(9) 0.0077(9) N(4) 0.061(1) 0.039(1) 0.037(1) -0.007(1) 0.005(1) 0.007(1) N(5) 0.205(9) 0.68(2) 0.60(2) -0.25(1) 0.10(1) -0.25(2) C(1) 0.034(1) 0.034(1) 0.035(1) 0.001(1) 0.007(1) 0.010(1) C(2) 0.033(1) 0.032(1) 0.028(1) 0.0003(10) 0.0093(10) 0.0052(10) C(3) 0.035(1) 0.032(1) 0.030(1) 0.0043(10) 0.0089(10) 0.005(1) C(4) 0.043(1) 0.028(1) 0.036(1) 0.001(1) 0.012(1) 0.005(1) C(5) 0.033(1) 0.034(1) 0.029(1) -0.0025(10) 0.0067(10) 0.000(1) C(6) 0.029(1) 0.045(1) 0.037(1) 0.003(1) 0.004(1) 0.011(1) C(7) 0.038(1) 0.038(1) 0.043(2) -0.006(1) 0.012(1) -0.004(1) C(8) 0.036(1) 0.066(2) 0.076(2) -0.007(1) 0.007(1) 0.010(2) C(9) 0.053(2) 0.067(2) 0.073(2) -0.004(2) 0.027(2) 0.019(2) C(10) 0.058(2) 0.073(2) 0.105(3) -0.028(2) 0.038(2) -0.046(2) C(11) 0.041(1) 0.042(1) 0.046(2) 0.013(1) 0.014(1) 0.009(1) C(12) 0.061(2) 0.052(2) 0.113(3) 0.023(2) 0.016(2) 0.035(2) C(13) 0.036(1) 0.069(2) 0.044(2) 0.017(1) 0.007(1) 0.015(1) C(14) 0.060(2) 0.081(2) 0.058(2) 0.032(2) 0.020(2) 0.000(2) C(15) 0.043(1) 0.029(1) 0.044(2) 0.000(1) 0.013(1) 0.006(1) C(16) 0.040(1) 0.035(1) 0.034(1) -0.001(1) 0.010(1) 0.007(1) C(17) 0.033(1) 0.040(1) 0.046(2) 0.003(1) 0.006(1) 0.003(1) C(18) 0.040(1) 0.032(1) 0.031(1) 0.004(1) 0.006(1) 0.007(1) C(19) 0.051(2) 0.033(1) 0.044(2) 0.006(1) 0.007(1) 0.009(1) C(20) 0.056(2) 0.042(2) 0.055(2) 0.017(1) 0.007(1) 0.011(1) C(21) 0.044(2) 0.053(2) 0.054(2) 0.017(1) 0.009(1) 0.014(1) C(22) 0.037(1) 0.046(2) 0.054(2) 0.006(1) 0.009(1) 0.015(1) C(23) 0.030(1) 0.035(1) 0.034(1) 0.0020(10) 0.0041(10) 0.009(1) C(24) 0.042(1) 0.044(2) 0.035(1) 0.002(1) 0.013(1) 0.006(1) C(25) 0.046(2) 0.050(2) 0.037(2) 0.005(1) 0.007(1) -0.002(1) C(26) 0.045(1) 0.034(1) 0.045(2) 0.002(1) 0.005(1) -0.002(1) C(27) 0.042(1) 0.034(1) 0.044(2) -0.001(1) 0.010(1) 0.007(1) C(28) 0.046(1) 0.034(1) 0.042(2) 0.007(1) 0.000(1) 0.000(1) C(29) 0.048(2) 0.057(2) 0.052(2) 0.015(1) -0.003(1) -0.010(1) C(30) 0.072(2) 0.063(2) 0.053(2) 0.024(2) -0.014(2) -0.015(2) C(31) 0.097(3) 0.053(2) 0.037(2) 0.006(2) -0.008(2) 0.000(1) C(32) 0.090(2) 0.051(2) 0.039(2) -0.009(2) 0.011(2) 0.006(1) C(33) 0.029(1) 0.034(1) 0.036(1) 0.0028(10) 0.0105(10) 0.007(1) C(34) 0.035(1) 0.048(2) 0.042(2) 0.007(1) 0.007(1) 0.000(1) C(35) 0.036(1) 0.073(2) 0.043(2) -0.001(1) 0.008(1) -0.006(1) C(36) 0.029(1) 0.089(2) 0.045(2) 0.001(1) 0.005(1) 0.028(2) C(37) 0.031(1) 0.058(2) 0.068(2) 0.006(1) 0.009(1) 0.035(2) C(38) 0.030(1) 0.038(1) 0.056(2) 0.002(1) 0.011(1) 0.016(1) C(39) 0.028(1) 0.032(1) 0.039(1) 0.0084(10) 0.002(1) 0.001(1) C(40) 0.039(1) 0.033(1) 0.036(1) 0.006(1) 0.005(1) 0.002(1) C(41) 0.040(1) 0.037(1) 0.046(2) 0.002(1) 0.005(1) 0.008(1) C(42) 0.038(1) 0.030(1) 0.067(2) 0.004(1) 0.000(1) -0.001(1) C(43) 0.045(2) 0.038(2) 0.077(2) 0.008(1) 0.019(1) -0.016(1) C(44) 0.038(1) 0.039(1) 0.066(2) 0.004(1) 0.020(1) -0.008(1) C(45) 0.033(1) 0.038(1) 0.039(1) 0.013(1) 0.006(1) 0.006(1) C(46) 0.046(2) 0.057(2) 0.040(2) 0.015(1) 0.008(1) 0.005(1) C(47) 0.068(2) 0.080(2) 0.035(2) 0.036(2) 0.013(1) 0.016(2) C(48) 0.070(2) 0.073(2) 0.059(2) 0.032(2) 0.030(2) 0.036(2) C(49) 0.057(2) 0.053(2) 0.071(2) 0.015(1) 0.026(2) 0.030(2) C(50) 0.046(1) 0.040(1) 0.047(2) 0.011(1) 0.011(1) 0.014(1) C(51) 0.030(1) 0.023(1) 0.037(1) 0.0021(9) 0.0052(10) 0.0019(10) C(52) 0.038(1) 0.041(1) 0.035(1) 0.012(1) 0.003(1) -0.001(1) C(53) 0.038(1) 0.056(2) 0.047(2) 0.019(1) 0.000(1) 0.004(1) C(54) 0.038(1) 0.046(2) 0.059(2) 0.018(1) 0.014(1) 0.004(1) C(55) 0.047(1) 0.039(1) 0.041(2) 0.009(1) 0.017(1) 0.006(1) C(56) 0.035(1) 0.034(1) 0.038(1) 0.009(1) 0.009(1) 0.009(1) C(57) 0.186(6) 0.129(5) 0.205(7) -0.002(5) -0.006(6) 0.057(5) C(58) 0.232(9) 0.213(8) 0.149(7) 0.087(7) 0.057(6) 0.015(6) B(1) 0.031(1) 0.031(1) 0.033(2) 0.006(1) 0.006(1) 0.003(1) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; B B 0.001 0.001 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Mn Mn 0.337 0.728 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(1) Mn(1) O(2) 74.86(6) . . . yes O(1) Mn(1) N(1) 152.04(7) . . . yes O(1) Mn(1) N(2) 82.19(7) . . . yes O(1) Mn(1) N(3) 105.42(7) . . . yes O(1) Mn(1) N(4) 127.97(8) . . . yes O(2) Mn(1) N(1) 132.62(6) . . . yes O(2) Mn(1) N(2) 154.05(7) . . . yes O(2) Mn(1) N(3) 90.80(7) . . . yes O(2) Mn(1) N(4) 79.69(7) . . . yes N(1) Mn(1) N(2) 71.84(7) . . . yes N(1) Mn(1) N(3) 73.60(7) . . . yes N(1) Mn(1) N(4) 70.95(7) . . . yes N(2) Mn(1) N(3) 107.07(7) . . . yes N(2) Mn(1) N(4) 106.05(8) . . . yes N(3) Mn(1) N(4) 119.67(8) . . . yes Mn(1) O(1) C(1) 115.9(1) . . . yes Mn(1) O(2) C(2) 114.3(1) . . . yes Mn(1) N(1) C(15) 107.4(1) . . . yes Mn(1) N(1) C(16) 107.8(1) . . . yes Mn(1) N(1) C(17) 106.8(1) . . . yes C(15) N(1) C(16) 112.1(2) . . . yes C(15) N(1) C(17) 110.6(2) . . . yes C(16) N(1) C(17) 111.9(2) . . . yes Mn(1) N(2) C(18) 117.2(2) . . . yes Mn(1) N(2) C(22) 125.1(2) . . . yes C(18) N(2) C(22) 117.7(2) . . . yes Mn(1) N(3) C(23) 119.0(2) . . . yes Mn(1) N(3) C(27) 123.5(2) . . . yes C(23) N(3) C(27) 117.4(2) . . . yes Mn(1) N(4) C(28) 117.5(2) . . . yes Mn(1) N(4) C(32) 124.8(2) . . . yes C(28) N(4) C(32) 117.4(2) . . . yes O(1) C(1) C(2) 117.3(2) . . . yes O(1) C(1) C(6) 122.6(2) . . . yes C(2) C(1) C(6) 120.1(2) . . . yes O(2) C(2) C(1) 116.1(2) . . . yes O(2) C(2) C(3) 124.5(2) . . . yes C(1) C(2) C(3) 119.4(2) . . . yes C(2) C(3) C(4) 116.4(2) . . . yes C(2) C(3) C(11) 120.2(2) . . . yes C(4) C(3) C(11) 123.4(2) . . . yes C(3) C(4) C(5) 124.9(2) . . . yes C(4) C(5) C(6) 118.9(2) . . . yes C(4) C(5) C(7) 119.0(2) . . . yes C(6) C(5) C(7) 122.2(2) . . . yes C(1) C(6) C(5) 120.2(2) . . . yes C(5) C(7) C(8) 111.8(2) . . . yes C(5) C(7) C(9) 110.0(2) . . . yes C(5) C(7) C(10) 108.2(2) . . . yes C(8) C(7) C(9) 107.7(2) . . . yes C(8) C(7) C(10) 108.0(2) . . . yes C(9) C(7) C(10) 111.2(3) . . . yes C(3) C(11) C(12) 111.7(2) . . . yes C(3) C(11) C(13) 109.8(2) . . . yes C(3) C(11) C(14) 110.2(2) . . . yes C(12) C(11) C(13) 107.5(2) . . . yes C(12) C(11) C(14) 108.4(2) . . . yes C(13) C(11) C(14) 109.1(2) . . . yes N(1) C(15) C(18) 112.4(2) . . . yes N(1) C(16) C(23) 111.9(2) . . . yes N(1) C(17) C(28) 110.3(2) . . . yes N(2) C(18) C(15) 116.5(2) . . . yes N(2) C(18) C(19) 122.3(2) . . . yes C(15) C(18) C(19) 121.2(2) . . . yes C(18) C(19) C(20) 119.2(2) . . . yes C(19) C(20) C(21) 119.1(2) . . . yes C(20) C(21) C(22) 118.5(2) . . . yes N(2) C(22) C(21) 123.3(2) . . . yes N(3) C(23) C(16) 116.3(2) . . . yes N(3) C(23) C(24) 122.0(2) . . . yes C(16) C(23) C(24) 121.7(2) . . . yes C(23) C(24) C(25) 119.4(2) . . . yes C(24) C(25) C(26) 119.2(2) . . . yes C(25) C(26) C(27) 118.1(2) . . . yes N(3) C(27) C(26) 123.8(2) . . . yes N(4) C(28) C(17) 115.6(2) . . . yes N(4) C(28) C(29) 122.0(3) . . . yes C(17) C(28) C(29) 122.4(3) . . . yes C(28) C(29) C(30) 119.4(3) . . . yes C(29) C(30) C(31) 119.4(3) . . . yes C(30) C(31) C(32) 118.4(3) . . . yes N(4) C(32) C(31) 123.3(3) . . . yes C(34) C(33) C(38) 114.4(2) . . . yes C(34) C(33) B(1) 123.2(2) . . . yes C(38) C(33) B(1) 122.4(2) . . . yes C(33) C(34) C(35) 123.2(3) . . . yes C(34) C(35) C(36) 120.2(3) . . . yes C(35) C(36) C(37) 119.0(2) . . . yes C(36) C(37) C(38) 119.9(3) . . . yes C(33) C(38) C(37) 123.3(3) . . . yes C(40) C(39) C(44) 114.4(2) . . . yes C(40) C(39) B(1) 120.8(2) . . . yes C(44) C(39) B(1) 124.4(2) . . . yes C(39) C(40) C(41) 123.1(2) . . . yes C(40) C(41) C(42) 120.5(2) . . . yes C(41) C(42) C(43) 118.6(2) . . . yes C(42) C(43) C(44) 120.6(3) . . . yes C(39) C(44) C(43) 122.9(2) . . . yes C(46) C(45) C(50) 114.6(2) . . . yes C(46) C(45) B(1) 123.5(2) . . . yes C(50) C(45) B(1) 121.9(2) . . . yes C(45) C(46) C(47) 122.9(3) . . . yes C(46) C(47) C(48) 120.9(3) . . . yes C(47) C(48) C(49) 118.4(3) . . . yes C(48) C(49) C(50) 120.2(3) . . . yes C(45) C(50) C(49) 123.2(3) . . . yes C(52) C(51) C(56) 114.5(2) . . . yes C(52) C(51) B(1) 122.0(2) . . . yes C(56) C(51) B(1) 123.4(2) . . . yes C(51) C(52) C(53) 123.3(2) . . . yes C(52) C(53) C(54) 120.6(2) . . . yes C(53) C(54) C(55) 118.6(2) . . . yes C(54) C(55) C(56) 119.6(2) . . . yes C(51) C(56) C(55) 123.4(2) . . . yes N(5) C(58) C(57) 171(1) . . . yes C(33) B(1) C(39) 107.1(2) . . . yes C(33) B(1) C(45) 109.4(2) . . . yes C(33) B(1) C(51) 112.1(2) . . . yes C(39) B(1) C(45) 112.5(2) . . . yes C(39) B(1) C(51) 107.6(2) . . . yes C(45) B(1) C(51) 108.2(2) . . . yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn(1) O(1) 2.104(2) . . yes Mn(1) O(2) 2.181(2) . . yes Mn(1) N(1) 2.359(2) . . yes Mn(1) N(2) 2.285(2) . . yes Mn(1) N(3) 2.204(2) . . yes Mn(1) N(4) 2.271(2) . . yes O(1) C(1) 1.283(3) . . yes O(2) C(2) 1.278(2) . . yes N(1) C(15) 1.475(3) . . yes N(1) C(16) 1.468(3) . . yes N(1) C(17) 1.459(3) . . yes N(2) C(18) 1.340(3) . . yes N(2) C(22) 1.339(3) . . yes N(3) C(23) 1.343(3) . . yes N(3) C(27) 1.348(3) . . yes N(4) C(28) 1.344(3) . . yes N(4) C(32) 1.344(3) . . yes N(5) C(58) 1.192(10) . . yes C(1) C(2) 1.454(3) . . yes C(1) C(6) 1.416(3) . . yes C(2) C(3) 1.435(3) . . yes C(3) C(4) 1.370(3) . . yes C(3) C(11) 1.526(3) . . yes C(4) C(5) 1.428(3) . . yes C(5) C(6) 1.359(3) . . yes C(5) C(7) 1.530(3) . . yes C(7) C(8) 1.530(4) . . yes C(7) C(9) 1.517(4) . . yes C(7) C(10) 1.519(4) . . yes C(11) C(12) 1.532(4) . . yes C(11) C(13) 1.523(4) . . yes C(11) C(14) 1.541(4) . . yes C(15) C(18) 1.502(3) . . yes C(16) C(23) 1.505(3) . . yes C(17) C(28) 1.506(4) . . yes C(18) C(19) 1.382(3) . . yes C(19) C(20) 1.374(4) . . yes C(20) C(21) 1.375(4) . . yes C(21) C(22) 1.377(4) . . yes C(23) C(24) 1.378(3) . . yes C(24) C(25) 1.379(3) . . yes C(25) C(26) 1.376(4) . . yes C(26) C(27) 1.369(4) . . yes C(28) C(29) 1.377(3) . . yes C(29) C(30) 1.371(4) . . yes C(30) C(31) 1.365(5) . . yes C(31) C(32) 1.374(4) . . yes C(33) C(34) 1.404(3) . . yes C(33) C(38) 1.393(3) . . yes C(33) B(1) 1.645(3) . . yes C(34) C(35) 1.385(4) . . yes C(35) C(36) 1.373(4) . . yes C(36) C(37) 1.381(4) . . yes C(37) C(38) 1.392(3) . . yes C(39) C(40) 1.410(3) . . yes C(39) C(44) 1.395(3) . . yes C(39) B(1) 1.646(3) . . yes C(40) C(41) 1.382(3) . . yes C(41) C(42) 1.379(4) . . yes C(42) C(43) 1.373(4) . . yes C(43) C(44) 1.395(4) . . yes C(45) C(46) 1.395(3) . . yes C(45) C(50) 1.396(3) . . yes C(45) B(1) 1.649(4) . . yes C(46) C(47) 1.390(4) . . yes C(47) C(48) 1.368(4) . . yes C(48) C(49) 1.385(4) . . yes C(49) C(50) 1.389(4) . . yes C(51) C(52) 1.398(3) . . yes C(51) C(56) 1.396(3) . . yes C(51) B(1) 1.653(4) . . yes C(52) C(53) 1.377(3) . . yes C(53) C(54) 1.380(4) . . yes C(54) C(55) 1.388(4) . . yes C(55) C(56) 1.392(3) . . yes C(57) C(58) 1.60(1) . . yes loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(1) C(57) 3.549(8) . . ? O(1) C(53) 3.560(3) . 2_555 ? N(5) C(29) 3.418(7) . 2_666 ? C(8) C(48) 3.580(4) . 2_555 ? C(10) C(42) 3.573(4) . 2_545 ? C(15) C(37) 3.570(3) . 1_565 ? C(19) C(40) 3.461(4) . 1_565 ? C(21) C(41) 3.468(4) . 2_555 ? C(21) C(40) 3.582(4) . 2_555 ? C(21) C(42) 3.596(4) . 2_555 ? C(24) C(50) 3.503(4) . 2_655 ? C(29) C(47) 3.577(4) . 2_655 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Mn(1) O(1) C(1) C(2) 10.7(3) . . . . yes Mn(1) O(1) C(1) C(6) -168.2(2) . . . . yes Mn(1) O(2) C(2) C(1) -7.4(3) . . . . yes Mn(1) O(2) C(2) C(3) 172.8(2) . . . . yes Mn(1) N(1) C(15) C(18) -40.3(2) . . . . yes Mn(1) N(1) C(16) C(23) -36.8(2) . . . . yes Mn(1) N(1) C(17) C(28) -46.3(2) . . . . yes Mn(1) N(2) C(18) C(15) 5.2(3) . . . . yes Mn(1) N(2) C(18) C(19) -174.0(2) . . . . yes Mn(1) N(2) C(22) C(21) 173.6(2) . . . . yes Mn(1) N(3) C(23) C(16) -6.8(3) . . . . yes Mn(1) N(3) C(23) C(24) 175.5(2) . . . . yes Mn(1) N(3) C(27) C(26) -175.7(2) . . . . yes Mn(1) N(4) C(28) C(17) 2.0(3) . . . . yes Mn(1) N(4) C(28) C(29) -176.4(2) . . . . yes Mn(1) N(4) C(32) C(31) 175.1(2) . . . . yes O(1) Mn(1) O(2) C(2) 9.6(2) . . . . yes O(1) Mn(1) N(1) C(15) 54.2(2) . . . . yes O(1) Mn(1) N(1) C(16) -66.8(2) . . . . yes O(1) Mn(1) N(1) C(17) 172.8(2) . . . . yes O(1) Mn(1) N(2) C(18) 169.7(2) . . . . yes O(1) Mn(1) N(2) C(22) -6.3(2) . . . . yes O(1) Mn(1) N(3) C(23) 140.3(2) . . . . yes O(1) Mn(1) N(3) C(27) -44.3(2) . . . . yes O(1) Mn(1) N(4) C(28) -177.1(2) . . . . yes O(1) Mn(1) N(4) C(32) 9.1(3) . . . . yes O(1) C(1) C(2) O(2) -2.0(3) . . . . yes O(1) C(1) C(2) C(3) 177.9(2) . . . . yes O(1) C(1) C(6) C(5) 179.6(2) . . . . yes O(2) Mn(1) O(1) C(1) -10.7(2) . . . . yes O(2) Mn(1) N(1) C(15) -138.3(1) . . . . yes O(2) Mn(1) N(1) C(16) 100.8(2) . . . . yes O(2) Mn(1) N(1) C(17) -19.6(2) . . . . yes O(2) Mn(1) N(2) C(18) 141.9(2) . . . . yes O(2) Mn(1) N(2) C(22) -34.2(3) . . . . yes O(2) Mn(1) N(3) C(23) -145.1(2) . . . . yes O(2) Mn(1) N(3) C(27) 30.2(2) . . . . yes O(2) Mn(1) N(4) C(28) 121.5(2) . . . . yes O(2) Mn(1) N(4) C(32) -52.3(2) . . . . yes O(2) C(2) C(1) C(6) 176.9(2) . . . . yes O(2) C(2) C(3) C(4) -176.7(2) . . . . yes O(2) C(2) C(3) C(11) 3.6(4) . . . . yes N(1) Mn(1) O(1) C(1) 159.8(2) . . . . yes N(1) Mn(1) O(2) C(2) -164.4(1) . . . . yes N(1) Mn(1) N(2) C(18) -20.8(2) . . . . yes N(1) Mn(1) N(2) C(22) 163.2(2) . . . . yes N(1) Mn(1) N(3) C(23) -10.6(2) . . . . yes N(1) Mn(1) N(3) C(27) 164.8(2) . . . . yes N(1) Mn(1) N(4) C(28) -20.8(2) . . . . yes N(1) Mn(1) N(4) C(32) 165.4(3) . . . . yes N(1) C(15) C(18) N(2) 25.1(3) . . . . yes N(1) C(15) C(18) C(19) -155.7(2) . . . . yes N(1) C(16) C(23) N(3) 30.8(3) . . . . yes N(1) C(16) C(23) C(24) -151.5(2) . . . . yes N(1) C(17) C(28) N(4) 31.3(3) . . . . yes N(1) C(17) C(28) C(29) -150.2(2) . . . . yes N(2) Mn(1) O(1) C(1) -178.5(2) . . . . yes N(2) Mn(1) O(2) C(2) 38.2(2) . . . . yes N(2) Mn(1) N(1) C(15) 31.5(1) . . . . yes N(2) Mn(1) N(1) C(16) -89.4(2) . . . . yes N(2) Mn(1) N(1) C(17) 150.2(2) . . . . yes N(2) Mn(1) N(3) C(23) 53.9(2) . . . . yes N(2) Mn(1) N(3) C(27) -130.7(2) . . . . yes N(2) Mn(1) N(4) C(28) -84.6(2) . . . . yes N(2) Mn(1) N(4) C(32) 101.6(2) . . . . yes N(2) C(18) C(19) C(20) -0.4(4) . . . . yes N(2) C(22) C(21) C(20) 0.5(4) . . . . yes N(3) Mn(1) O(1) C(1) 75.8(2) . . . . yes N(3) Mn(1) O(2) C(2) -96.2(2) . . . . yes N(3) Mn(1) N(1) C(15) 146.3(2) . . . . yes N(3) Mn(1) N(1) C(16) 25.3(1) . . . . yes N(3) Mn(1) N(1) C(17) -95.1(2) . . . . yes N(3) Mn(1) N(2) C(18) -86.4(2) . . . . yes N(3) Mn(1) N(2) C(22) 97.5(2) . . . . yes N(3) Mn(1) N(4) C(28) 36.5(2) . . . . yes N(3) Mn(1) N(4) C(32) -137.3(2) . . . . yes N(3) C(23) C(24) C(25) 0.3(4) . . . . yes N(3) C(27) C(26) C(25) 0.5(4) . . . . yes N(4) Mn(1) O(1) C(1) -74.2(2) . . . . yes N(4) Mn(1) O(2) C(2) 143.8(2) . . . . yes N(4) Mn(1) N(1) C(15) -83.4(1) . . . . yes N(4) Mn(1) N(1) C(16) 155.7(2) . . . . yes N(4) Mn(1) N(1) C(17) 35.3(1) . . . . yes N(4) Mn(1) N(2) C(18) 42.4(2) . . . . yes N(4) Mn(1) N(2) C(22) -133.7(2) . . . . yes N(4) Mn(1) N(3) C(23) -66.6(2) . . . . yes N(4) Mn(1) N(3) C(27) 108.8(2) . . . . yes N(4) C(28) C(29) C(30) 1.7(4) . . . . yes N(4) C(32) C(31) C(30) 0.1(5) . . . . yes C(1) C(2) C(3) C(4) 3.5(3) . . . . yes C(1) C(2) C(3) C(11) -176.3(2) . . . . yes C(1) C(6) C(5) C(4) 1.2(4) . . . . yes C(1) C(6) C(5) C(7) -177.7(2) . . . . yes C(2) C(1) C(6) C(5) 0.8(4) . . . . yes C(2) C(3) C(4) C(5) -1.6(4) . . . . yes C(2) C(3) C(11) C(12) 177.3(2) . . . . yes C(2) C(3) C(11) C(13) 58.1(3) . . . . yes C(2) C(3) C(11) C(14) -62.1(3) . . . . yes C(3) C(2) C(1) C(6) -3.2(3) . . . . yes C(3) C(4) C(5) C(6) -0.8(4) . . . . yes C(3) C(4) C(5) C(7) 178.1(2) . . . . yes C(4) C(3) C(11) C(12) -2.5(4) . . . . yes C(4) C(3) C(11) C(13) -121.6(3) . . . . yes C(4) C(3) C(11) C(14) 118.2(3) . . . . yes C(4) C(5) C(7) C(8) 176.1(2) . . . . yes C(4) C(5) C(7) C(9) 56.5(3) . . . . yes C(4) C(5) C(7) C(10) -65.1(3) . . . . yes C(5) C(4) C(3) C(11) 178.2(2) . . . . yes C(6) C(5) C(7) C(8) -5.0(3) . . . . yes C(6) C(5) C(7) C(9) -124.6(3) . . . . yes C(6) C(5) C(7) C(10) 113.8(3) . . . . yes C(15) N(1) C(16) C(23) -154.8(2) . . . . yes C(15) N(1) C(17) C(28) 70.2(2) . . . . yes C(15) C(18) N(2) C(22) -178.4(2) . . . . yes C(15) C(18) C(19) C(20) -179.6(2) . . . . yes C(16) N(1) C(15) C(18) 77.9(2) . . . . yes C(16) N(1) C(17) C(28) -164.0(2) . . . . yes C(16) C(23) N(3) C(27) 177.6(2) . . . . yes C(16) C(23) C(24) C(25) -177.3(2) . . . . yes C(17) N(1) C(15) C(18) -156.4(2) . . . . yes C(17) N(1) C(16) C(23) 80.3(2) . . . . yes C(17) C(28) N(4) C(32) 176.3(2) . . . . yes C(17) C(28) C(29) C(30) -176.7(3) . . . . yes C(18) N(2) C(22) C(21) -2.4(4) . . . . yes C(18) C(19) C(20) C(21) -1.5(4) . . . . yes C(19) C(18) N(2) C(22) 2.4(4) . . . . yes C(19) C(20) C(21) C(22) 1.5(4) . . . . yes C(23) N(3) C(27) C(26) -0.2(4) . . . . yes C(23) C(24) C(25) C(26) 0.0(4) . . . . yes C(24) C(23) N(3) C(27) -0.2(3) . . . . yes C(24) C(25) C(26) C(27) -0.3(4) . . . . yes C(28) N(4) C(32) C(31) 1.3(5) . . . . yes C(28) C(29) C(30) C(31) -0.2(5) . . . . yes C(29) C(28) N(4) C(32) -2.2(4) . . . . yes C(29) C(30) C(31) C(32) -0.7(5) . . . . yes C(33) C(34) C(35) C(36) 0.5(4) . . . . yes C(33) C(38) C(37) C(36) 0.8(4) . . . . yes C(33) B(1) C(39) C(40) 85.4(3) . . . . yes C(33) B(1) C(39) C(44) -87.0(3) . . . . yes C(33) B(1) C(45) C(46) 152.4(2) . . . . yes C(33) B(1) C(45) C(50) -31.3(3) . . . . yes C(33) B(1) C(51) C(52) 158.8(2) . . . . yes C(33) B(1) C(51) C(56) -25.7(3) . . . . yes C(34) C(33) C(38) C(37) 0.2(4) . . . . yes C(34) C(33) B(1) C(39) -156.0(2) . . . . yes C(34) C(33) B(1) C(45) 81.7(3) . . . . yes C(34) C(33) B(1) C(51) -38.3(3) . . . . yes C(34) C(35) C(36) C(37) 0.5(4) . . . . yes C(35) C(34) C(33) C(38) -0.8(4) . . . . yes C(35) C(34) C(33) B(1) -179.4(2) . . . . yes C(35) C(36) C(37) C(38) -1.1(4) . . . . yes C(37) C(38) C(33) B(1) 178.8(2) . . . . yes C(38) C(33) B(1) C(39) 25.5(3) . . . . yes C(38) C(33) B(1) C(45) -96.7(3) . . . . yes C(38) C(33) B(1) C(51) 143.3(2) . . . . yes C(39) C(40) C(41) C(42) -1.2(4) . . . . yes C(39) C(44) C(43) C(42) -0.9(5) . . . . yes C(39) B(1) C(45) C(46) 33.5(3) . . . . yes C(39) B(1) C(45) C(50) -150.2(2) . . . . yes C(39) B(1) C(51) C(52) -83.7(3) . . . . yes C(39) B(1) C(51) C(56) 91.8(2) . . . . yes C(40) C(39) C(44) C(43) -0.1(4) . . . . yes C(40) C(39) B(1) C(45) -154.3(2) . . . . yes C(40) C(39) B(1) C(51) -35.2(3) . . . . yes C(40) C(41) C(42) C(43) 0.1(4) . . . . yes C(41) C(40) C(39) C(44) 1.1(4) . . . . yes C(41) C(40) C(39) B(1) -172.0(2) . . . . yes C(41) C(42) C(43) C(44) 0.9(4) . . . . yes C(43) C(44) C(39) B(1) 172.7(2) . . . . yes C(44) C(39) B(1) C(45) 33.3(3) . . . . yes C(44) C(39) B(1) C(51) 152.4(2) . . . . yes C(45) C(46) C(47) C(48) 0.7(5) . . . . yes C(45) C(50) C(49) C(48) -0.4(4) . . . . yes C(45) B(1) C(51) C(52) 38.1(3) . . . . yes C(45) B(1) C(51) C(56) -146.4(2) . . . . yes C(46) C(45) C(50) C(49) 0.4(4) . . . . yes C(46) C(45) B(1) C(51) -85.2(3) . . . . yes C(46) C(47) C(48) C(49) -0.6(5) . . . . yes C(47) C(46) C(45) C(50) -0.6(4) . . . . yes C(47) C(46) C(45) B(1) 175.9(2) . . . . yes C(47) C(48) C(49) C(50) 0.5(5) . . . . yes C(49) C(50) C(45) B(1) -176.1(2) . . . . yes C(50) C(45) B(1) C(51) 91.1(3) . . . . yes C(51) C(52) C(53) C(54) 0.4(4) . . . . yes C(51) C(56) C(55) C(54) 1.0(4) . . . . yes C(52) C(51) C(56) C(55) -1.0(3) . . . . yes C(52) C(53) C(54) C(55) -0.4(4) . . . . yes C(53) C(52) C(51) C(56) 0.3(3) . . . . yes C(53) C(52) C(51) B(1) 176.1(2) . . . . yes C(53) C(54) C(55) C(56) -0.2(4) . . . . yes C(55) C(56) C(51) B(1) -176.7(2) . . . . yes C(55) C(56) C(51) B(1) -176.7(2) . . . . yes
1100739.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $ #$Revision: 176435 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100739.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100739 loop_ _publ_author_name 'Yutaka Hitomi' 'Akira Ando' 'Hajime Matsui' 'Tomoyuki Ito' 'Tsunehiro Tanaka' 'Seiji Ogo' 'Takuzo Funabiki' _publ_contact_author_email hitomi@moleng.kyoto-u.ac.jp _publ_contact_author_fax +81-75-383-2563 _publ_contact_author_name 'Yutaka Hitomi' _publ_contact_author_phone +81-75-383-2563 _publ_section_title ; Aerobic Catechol Oxidation Catalyzed by a Bis(\m-oxo)dimanganese(III,III) Complex via a Manganese(II)-Semiquinonate Complex ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3473 _journal_page_last 3478 _journal_paper_doi 10.1021/ic050109d _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C84 H76 B2 Mn2 N8 O2' _chemical_formula_weight 1361.07 _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_Int_Tables_number 15 _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _cell_angle_alpha 90 _cell_angle_beta 105.370(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 19.474(2) _cell_length_b 14.884(2) _cell_length_c 24.538(3) _cell_measurement_reflns_used 13782 _cell_measurement_temperature 243.2 _cell_measurement_theta_max 27.5 _cell_measurement_theta_min 3.1 _cell_volume 6858.0(14) _computing_cell_refinement CRYSTALCLEAR _computing_data_collection CRYSTALCLEAR _computing_data_reduction 'teXsan Ver. 1.11' _computing_publication_material 'teXsan Ver. 1.11' _computing_structure_refinement 'teXsan Ver. 1.10' _computing_structure_solution SIR97 _diffrn_detector_area_resol_mean 14.71 _diffrn_measured_fraction_theta_full 0.9847 _diffrn_measured_fraction_theta_max 0.9847 _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents 0.052 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_number 37881 _diffrn_reflns_theta_full 27.48 _diffrn_reflns_theta_max 27.48 _exptl_absorpt_coefficient_mu 0.425 _exptl_absorpt_correction_T_max 0.919 _exptl_absorpt_correction_T_min 0.623 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details RICABA _exptl_crystal_colour brown _exptl_crystal_density_diffrn 1.318 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Prism _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.150 _refine_diff_density_max 1.85 _refine_diff_density_min -0.91 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_hydrogen_treatment noref _refine_ls_number_parameters 442 _refine_ls_number_reflns 4372 _refine_ls_R_factor_gt 0.0660 _refine_ls_shift/su_max 0.0005 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.03000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.1797 _reflns_number_gt 3277 _reflns_number_total 7748 _reflns_threshold_expression F^2^>2.0\s(F^2^) _cod_data_source_file ic050109dsi20050124_043757_2.cif _cod_data_source_block '_str863_MnTPA35DTBSQBPh4_O' _cod_original_cell_volume 6858.3(1) _cod_original_formula_sum 'C84 H76 B2 N8 Mn2 O2 ' _cod_database_code 1100739 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y,1/2-z -x,-y,-z x,-y,1/2+z 1/2+x,1/2+y,z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn(1) Mn 0.24091(4) -0.17227(5) 0.52373(3) 0.0382(3) Uani 1.00 d . . . O(1) O 0.2229(2) -0.2927(2) 0.5360(1) 0.036(1) Uani 1.00 d . . . N(1) N 0.2584(2) -0.0298(3) 0.5153(2) 0.036(1) Uani 1.00 d . . . N(2) N 0.1333(2) -0.1163(3) 0.4684(2) 0.049(2) Uani 1.00 d . . . N(3) N 0.3492(2) -0.1397(3) 0.5863(2) 0.044(2) Uani 1.00 d . . . N(4) N 0.2024(2) -0.1239(3) 0.5894(2) 0.040(1) Uani 1.00 d . . . C(1) C 0.2144(3) -0.0024(3) 0.4574(2) 0.050(2) Uani 1.00 d . . . C(2) C 0.3350(3) -0.0189(3) 0.5198(2) 0.050(2) Uani 1.00 d . . . C(3) C 0.2364(3) 0.0217(3) 0.5594(2) 0.044(2) Uani 1.00 d . . . C(4) C 0.1399(3) -0.0326(4) 0.4528(2) 0.049(2) Uani 1.00 d . . . C(5) C 0.0795(4) 0.0215(4) 0.4312(3) 0.067(2) Uani 1.00 d . . . C(6) C 0.0155(4) -0.0142(6) 0.4297(3) 0.077(3) Uani 1.00 d . . . C(7) C 0.0073(4) -0.1011(5) 0.4449(3) 0.075(3) Uani 1.00 d . . . C(8) C 0.0693(4) -0.1494(4) 0.4643(3) 0.058(2) Uani 1.00 d . . . C(9) C 0.3763(3) -0.0616(4) 0.5743(2) 0.040(2) Uani 1.00 d . . . C(10) C 0.4370(3) -0.0251(4) 0.6124(3) 0.051(2) Uani 1.00 d . . . C(11) C 0.4687(3) -0.0704(5) 0.6598(3) 0.059(2) Uani 1.00 d . . . C(12) C 0.4402(3) -0.1500(4) 0.6720(2) 0.054(2) Uani 1.00 d . . . C(13) C 0.3806(3) -0.1834(4) 0.6326(3) 0.053(2) Uani 1.00 d . . . C(14) C 0.2043(3) -0.0351(4) 0.5986(2) 0.042(2) Uani 1.00 d . . . C(15) C 0.1824(3) 0.0036(4) 0.6421(3) 0.045(2) Uani 1.00 d . . . C(16) C 0.1540(3) -0.0516(5) 0.6743(2) 0.057(2) Uani 1.00 d . . . C(17) C 0.1509(3) -0.1428(4) 0.6644(3) 0.059(2) Uani 1.00 d . . . C(18) C 0.1751(3) -0.1763(3) 0.6217(3) 0.047(2) Uani 1.00 d . . . C(19) C 0.2739(3) 0.3213(4) 0.6601(2) 0.044(2) Uani 1.00 d . . . C(20) C 0.3072(3) 0.2395(4) 0.6555(2) 0.047(2) Uani 1.00 d . . . C(21) C 0.3798(4) 0.2296(4) 0.6670(3) 0.057(2) Uani 1.00 d . . . C(22) C 0.4236(3) 0.3018(5) 0.6839(2) 0.055(2) Uani 1.00 d . . . C(23) C 0.3938(3) 0.3835(4) 0.6883(3) 0.059(2) Uani 1.00 d . . . C(24) C 0.3201(3) 0.3931(4) 0.6777(2) 0.045(2) Uani 1.00 d . . . C(25) C 0.1653(3) 0.4259(3) 0.6722(2) 0.037(2) Uani 1.00 d . . . C(26) C 0.1443(3) 0.5004(4) 0.6360(2) 0.045(2) Uani 1.00 d . . . C(27) C 0.1216(3) 0.5818(4) 0.6539(2) 0.051(2) Uani 1.00 d . . . C(28) C 0.1227(3) 0.5943(4) 0.7090(3) 0.046(2) Uani 1.00 d . . . C(29) C 0.1450(3) 0.5235(4) 0.7465(2) 0.047(2) Uani 1.00 d . . . C(30) C 0.1647(3) 0.4425(4) 0.7277(2) 0.040(2) Uani 1.00 d . . . C(31) C 0.1614(3) 0.2508(3) 0.6877(2) 0.040(2) Uani 1.00 d . . . C(32) C 0.2066(3) 0.2169(4) 0.7370(2) 0.048(2) Uani 1.00 d . . . C(33) C 0.1857(4) 0.1580(4) 0.7757(2) 0.055(2) Uani 1.00 d . . . C(34) C 0.1155(4) 0.1294(4) 0.7605(3) 0.058(2) Uani 1.00 d . . . C(35) C 0.0682(3) 0.1595(4) 0.7118(3) 0.061(2) Uani 1.00 d . . . C(36) C 0.0918(3) 0.2182(4) 0.6762(2) 0.041(2) Uani 1.00 d . . . C(37) C 0.1443(3) 0.3144(3) 0.5810(2) 0.031(1) Uani 1.00 d . . . C(38) C 0.0739(3) 0.3421(4) 0.5616(2) 0.049(2) Uani 1.00 d . . . C(39) C 0.0366(3) 0.3300(4) 0.5061(3) 0.049(2) Uani 1.00 d . . . C(40) C 0.0666(3) 0.2880(4) 0.4669(2) 0.051(2) Uani 1.00 d . . . C(41) C 0.1354(3) 0.2605(4) 0.4860(2) 0.050(2) Uani 1.00 d . . . C(42) C 0.1740(3) 0.2723(3) 0.5419(2) 0.043(2) Uani 1.00 d . . . B(1) B 0.1874(3) 0.3287(4) 0.6497(3) 0.036(2) Uani 1.00 d . . . H(1) H 0.2158 0.0609 0.4533 0.0603 Uiso 1.00 calc . . . H(2) H 0.2321 -0.0306 0.4291 0.0603 Uiso 1.00 calc . . . H(3) H 0.3464 -0.0475 0.4887 0.0603 Uiso 1.00 calc . . . H(4) H 0.3464 0.0432 0.5198 0.0603 Uiso 1.00 calc . . . H(5) H 0.2771 0.0518 0.5819 0.0523 Uiso 1.00 calc . . . H(6) H 0.2019 0.0647 0.5412 0.0523 Uiso 1.00 calc . . . H(7) H 0.0838 0.0808 0.4182 0.0803 Uiso 1.00 calc . . . H(8) H -0.0257 0.0225 0.4176 0.0927 Uiso 1.00 calc . . . H(9) H -0.0382 -0.1265 0.4422 0.0898 Uiso 1.00 calc . . . H(10) H 0.0657 -0.2100 0.4753 0.0701 Uiso 1.00 calc . . . H(11) H 0.4555 0.0312 0.6048 0.0613 Uiso 1.00 calc . . . H(12) H 0.5109 -0.0474 0.6849 0.0706 Uiso 1.00 calc . . . H(13) H 0.4607 -0.1812 0.7062 0.0646 Uiso 1.00 calc . . . H(14) H 0.3619 -0.2399 0.6396 0.0640 Uiso 1.00 calc . . . H(15) H 0.1870 0.0663 0.6493 0.0534 Uiso 1.00 calc . . . H(16) H 0.1361 -0.0274 0.7036 0.0681 Uiso 1.00 calc . . . H(17) H 0.1320 -0.1819 0.6874 0.0711 Uiso 1.00 calc . . . H(18) H 0.1724 -0.2391 0.6148 0.0565 Uiso 1.00 calc . . . H(19) H 0.2782 0.1881 0.6438 0.0569 Uiso 1.00 calc . . . H(20) H 0.3997 0.1723 0.6633 0.0679 Uiso 1.00 calc . . . H(21) H 0.4738 0.2953 0.6923 0.0659 Uiso 1.00 calc . . . H(22) H 0.4236 0.4346 0.6988 0.0711 Uiso 1.00 calc . . . H(23) H 0.3009 0.4503 0.6827 0.0535 Uiso 1.00 calc . . . H(24) H 0.1456 0.4951 0.5977 0.0541 Uiso 1.00 calc . . . H(25) H 0.1052 0.6286 0.6273 0.0616 Uiso 1.00 calc . . . H(26) H 0.1086 0.6500 0.7216 0.0550 Uiso 1.00 calc . . . H(27) H 0.1466 0.5308 0.7853 0.0560 Uiso 1.00 calc . . . H(28) H 0.1787 0.3953 0.7544 0.0484 Uiso 1.00 calc . . . H(29) H 0.2552 0.2344 0.7458 0.0573 Uiso 1.00 calc . . . H(30) H 0.2182 0.1394 0.8100 0.0664 Uiso 1.00 calc . . . H(31) H 0.0997 0.0882 0.7842 0.0695 Uiso 1.00 calc . . . H(32) H 0.0199 0.1405 0.7025 0.0732 Uiso 1.00 calc . . . H(33) H 0.0586 0.2370 0.6423 0.0491 Uiso 1.00 calc . . . H(34) H 0.0511 0.3697 0.5870 0.0592 Uiso 1.00 calc . . . H(35) H -0.0111 0.3510 0.4939 0.0584 Uiso 1.00 calc . . . H(36) H 0.0402 0.2791 0.4287 0.0618 Uiso 1.00 calc . . . H(37) H 0.1577 0.2325 0.4604 0.0595 Uiso 1.00 calc . . . H(38) H 0.2217 0.2513 0.5538 0.0512 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Mn(1) 0.0470(6) 0.0260(4) 0.0435(5) -0.0061(4) 0.0153(4) -0.0003(4) O(1) 0.045(2) 0.028(2) 0.035(2) -0.002(2) 0.011(2) -0.011(2) N(1) 0.034(3) 0.032(2) 0.036(3) -0.002(2) -0.001(2) 0.005(2) N(2) 0.046(3) 0.039(3) 0.063(3) -0.005(2) 0.015(3) 0.007(3) N(3) 0.041(3) 0.030(2) 0.065(4) 0.000(2) 0.021(3) 0.001(2) N(4) 0.046(3) 0.026(3) 0.044(3) -0.009(2) 0.005(2) -0.001(2) C(1) 0.055(4) 0.039(3) 0.046(4) -0.007(3) -0.005(3) 0.014(3) C(2) 0.055(4) 0.034(3) 0.063(4) -0.012(3) 0.019(3) 0.005(3) C(3) 0.037(3) 0.034(3) 0.059(4) 0.000(3) 0.010(3) 0.006(3) C(4) 0.054(4) 0.043(4) 0.043(4) -0.006(3) -0.002(3) 0.008(3) C(5) 0.055(5) 0.062(5) 0.068(5) -0.002(4) -0.011(4) 0.012(4) C(6) 0.058(5) 0.087(6) 0.064(5) 0.011(4) -0.025(4) -0.011(4) C(7) 0.050(5) 0.073(5) 0.091(6) -0.014(4) 0.000(4) -0.017(5) C(8) 0.040(4) 0.052(4) 0.077(5) -0.012(3) 0.005(3) -0.004(3) C(9) 0.031(3) 0.038(3) 0.046(4) 0.004(3) 0.006(3) -0.007(3) C(10) 0.041(4) 0.049(4) 0.059(4) -0.003(3) 0.007(3) -0.006(3) C(11) 0.038(4) 0.072(5) 0.061(4) 0.005(3) 0.002(3) -0.019(4) C(12) 0.059(4) 0.072(5) 0.020(3) 0.014(4) -0.007(3) 0.005(3) C(13) 0.058(4) 0.036(4) 0.068(5) 0.009(3) 0.019(4) 0.006(3) C(14) 0.046(4) 0.034(3) 0.042(3) 0.002(3) 0.005(3) -0.004(3) C(15) 0.029(3) 0.042(3) 0.059(4) 0.000(3) 0.006(3) -0.009(3) C(16) 0.051(4) 0.065(5) 0.048(4) 0.009(3) 0.003(3) -0.011(4) C(17) 0.076(5) 0.052(4) 0.056(4) 0.008(4) 0.028(4) 0.015(3) C(18) 0.046(4) 0.037(3) 0.059(4) -0.001(3) 0.015(3) 0.001(3) C(19) 0.044(4) 0.036(3) 0.058(4) -0.005(3) 0.024(3) -0.001(3) C(20) 0.040(4) 0.039(3) 0.067(4) -0.002(3) 0.022(3) 0.002(3) C(21) 0.058(5) 0.054(4) 0.067(5) 0.004(3) 0.031(4) -0.002(3) C(22) 0.050(4) 0.076(5) 0.046(4) 0.008(4) 0.025(3) 0.004(4) C(23) 0.054(4) 0.068(5) 0.056(4) -0.015(4) 0.016(3) -0.006(4) C(24) 0.036(4) 0.047(3) 0.053(4) -0.007(3) 0.016(3) -0.009(3) C(25) 0.041(3) 0.036(3) 0.032(3) -0.008(3) 0.008(3) -0.005(3) C(26) 0.056(4) 0.046(4) 0.030(3) -0.011(3) 0.006(3) -0.003(3) C(27) 0.070(5) 0.033(3) 0.048(4) -0.002(3) 0.011(3) 0.004(3) C(28) 0.052(4) 0.042(4) 0.045(4) -0.015(3) 0.015(3) -0.020(3) C(29) 0.047(4) 0.052(4) 0.041(4) -0.002(3) 0.012(3) -0.008(3) C(30) 0.047(4) 0.044(3) 0.025(3) 0.003(3) 0.001(3) -0.004(3) C(31) 0.051(4) 0.036(3) 0.029(3) -0.005(3) 0.006(3) -0.013(3) C(32) 0.065(4) 0.050(4) 0.033(3) -0.003(3) 0.022(3) -0.003(3) C(33) 0.071(5) 0.053(4) 0.048(4) 0.010(3) 0.026(4) 0.006(3) C(34) 0.073(5) 0.038(4) 0.074(5) 0.007(3) 0.038(4) 0.009(3) C(35) 0.056(4) 0.048(4) 0.088(5) -0.007(3) 0.037(4) -0.001(4) C(36) 0.040(4) 0.052(4) 0.033(3) 0.006(3) 0.013(3) 0.002(3) C(37) 0.026(3) 0.044(3) 0.019(3) -0.005(2) 0.000(2) -0.003(2) C(38) 0.068(4) 0.054(4) 0.034(3) -0.004(3) 0.028(3) -0.009(3) C(39) 0.049(4) 0.049(4) 0.049(4) -0.002(3) 0.015(3) 0.002(3) C(40) 0.059(4) 0.054(4) 0.038(3) -0.018(3) 0.007(3) -0.001(3) C(41) 0.055(4) 0.042(4) 0.047(4) -0.006(3) 0.004(3) -0.007(3) C(42) 0.040(4) 0.037(3) 0.053(4) 0.004(3) 0.015(3) 0.007(3) B(1) 0.032(4) 0.029(3) 0.051(4) -0.002(3) 0.015(3) -0.002(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; B B 0.001 0.001 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Mn Mn 0.337 0.728 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Mn(1) Mn(1) O(1) 44.48(9) 7_546 . . yes Mn(1) Mn(1) O(1) 44.6(1) 7_546 . 7_546 yes Mn(1) Mn(1) N(1) 140.2(1) 7_546 . . yes Mn(1) Mn(1) N(2) 105.0(1) 7_546 . . yes Mn(1) Mn(1) N(3) 105.7(1) 7_546 . . yes Mn(1) Mn(1) N(4) 139.4(1) 7_546 . . yes O(1) Mn(1) O(1) 89.1(1) . . 7_546 yes O(1) Mn(1) N(1) 175.3(2) . . . yes O(1) Mn(1) N(2) 105.0(2) . . . yes O(1) Mn(1) N(3) 105.8(2) . . . yes O(1) Mn(1) N(4) 94.9(1) . . . yes O(1) Mn(1) N(1) 95.6(2) 7_546 . . yes O(1) Mn(1) N(2) 96.4(1) 7_546 . . yes O(1) Mn(1) N(3) 96.5(1) 7_546 . . yes O(1) Mn(1) N(4) 176.0(1) 7_546 . . yes N(1) Mn(1) N(2) 74.6(2) . . . yes N(1) Mn(1) N(3) 73.7(2) . . . yes N(1) Mn(1) N(4) 80.4(2) . . . yes N(2) Mn(1) N(3) 146.7(2) . . . yes N(2) Mn(1) N(4) 82.8(2) . . . yes N(3) Mn(1) N(4) 82.2(2) . . . yes Mn(1) O(1) Mn(1) 90.9(1) . . 7_546 yes Mn(1) N(1) C(1) 106.8(3) . . . yes Mn(1) N(1) C(2) 106.4(3) . . . yes Mn(1) N(1) C(3) 110.8(3) . . . yes C(1) N(1) C(2) 110.5(4) . . . yes C(1) N(1) C(3) 110.3(4) . . . yes C(2) N(1) C(3) 111.8(4) . . . yes Mn(1) N(2) C(4) 111.4(4) . . . yes Mn(1) N(2) C(8) 126.7(4) . . . yes C(4) N(2) C(8) 119.6(5) . . . yes Mn(1) N(3) C(9) 112.2(4) . . . yes Mn(1) N(3) C(13) 127.4(4) . . . yes C(9) N(3) C(13) 120.0(5) . . . yes Mn(1) N(4) C(14) 118.1(4) . . . yes Mn(1) N(4) C(18) 123.1(4) . . . yes C(14) N(4) C(18) 118.7(5) . . . yes N(1) C(1) C(4) 106.7(4) . . . yes N(1) C(2) C(9) 108.1(4) . . . yes N(1) C(3) C(14) 114.7(4) . . . yes N(2) C(4) C(1) 115.5(5) . . . yes N(2) C(4) C(5) 120.8(6) . . . yes C(1) C(4) C(5) 123.6(5) . . . yes C(4) C(5) C(6) 117.4(6) . . . yes C(5) C(6) C(7) 122.6(7) . . . yes C(6) C(7) C(8) 115.7(6) . . . yes N(2) C(8) C(7) 123.8(6) . . . yes N(3) C(9) C(2) 114.4(5) . . . yes N(3) C(9) C(10) 119.9(5) . . . yes C(2) C(9) C(10) 125.7(5) . . . yes C(9) C(10) C(11) 119.5(6) . . . yes C(10) C(11) C(12) 120.1(6) . . . yes C(11) C(12) C(13) 118.0(5) . . . yes N(3) C(13) C(12) 122.4(5) . . . yes N(4) C(14) C(3) 115.9(5) . . . yes N(4) C(14) C(15) 122.8(5) . . . yes C(3) C(14) C(15) 121.2(5) . . . yes C(14) C(15) C(16) 117.2(5) . . . yes C(15) C(16) C(17) 120.0(5) . . . yes C(16) C(17) C(18) 119.4(6) . . . yes N(4) C(18) C(17) 121.7(5) . . . yes C(20) C(19) C(24) 114.8(5) . . . yes C(20) C(19) B(1) 121.7(5) . . . yes C(24) C(19) B(1) 123.4(5) . . . yes C(19) C(20) C(21) 123.5(5) . . . yes C(20) C(21) C(22) 120.1(6) . . . yes C(21) C(22) C(23) 118.8(6) . . . yes C(22) C(23) C(24) 121.0(6) . . . yes C(19) C(24) C(23) 121.8(5) . . . yes C(26) C(25) C(30) 113.6(5) . . . yes C(26) C(25) B(1) 122.6(4) . . . yes C(30) C(25) B(1) 123.8(5) . . . yes C(25) C(26) C(27) 123.1(5) . . . yes C(26) C(27) C(28) 120.5(5) . . . yes C(27) C(28) C(29) 118.3(5) . . . yes C(28) C(29) C(30) 120.4(5) . . . yes C(25) C(30) C(29) 124.0(5) . . . yes C(32) C(31) C(36) 114.0(5) . . . yes C(32) C(31) B(1) 122.0(5) . . . yes C(36) C(31) B(1) 123.8(5) . . . yes C(31) C(32) C(33) 125.1(5) . . . yes C(32) C(33) C(34) 116.4(6) . . . yes C(33) C(34) C(35) 121.4(5) . . . yes C(34) C(35) C(36) 119.4(6) . . . yes C(31) C(36) C(35) 123.6(5) . . . yes C(38) C(37) C(42) 116.7(5) . . . yes C(38) C(37) B(1) 119.3(4) . . . yes C(42) C(37) B(1) 123.9(5) . . . yes C(37) C(38) C(39) 121.0(5) . . . yes C(38) C(39) C(40) 122.2(5) . . . yes C(39) C(40) C(41) 116.7(5) . . . yes C(40) C(41) C(42) 121.9(5) . . . yes C(37) C(42) C(41) 121.5(5) . . . yes C(19) B(1) C(25) 110.8(4) . . . yes C(19) B(1) C(31) 108.7(4) . . . yes C(19) B(1) C(37) 111.5(4) . . . yes C(25) B(1) C(31) 106.4(4) . . . yes C(25) B(1) C(37) 110.0(4) . . . yes C(31) B(1) C(37) 109.3(4) . . . yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn(1) Mn(1) 2.656(2) . 7_546 yes Mn(1) O(1) 1.866(3) . . yes Mn(1) O(1) 1.861(3) . 7_546 yes Mn(1) N(1) 2.166(4) . . yes Mn(1) N(2) 2.328(5) . . yes Mn(1) N(3) 2.308(5) . . yes Mn(1) N(4) 2.079(4) . . yes N(1) C(1) 1.507(6) . . yes N(1) C(2) 1.475(6) . . yes N(1) C(3) 1.479(6) . . yes N(2) C(4) 1.320(6) . . yes N(2) C(8) 1.319(6) . . yes N(3) C(9) 1.342(6) . . yes N(3) C(13) 1.311(7) . . yes N(4) C(14) 1.340(6) . . yes N(4) C(18) 1.320(6) . . yes C(1) C(4) 1.494(7) . . yes C(2) C(9) 1.507(7) . . yes C(3) C(14) 1.532(7) . . yes C(4) C(5) 1.409(8) . . yes C(5) C(6) 1.347(8) . . yes C(6) C(7) 1.366(9) . . yes C(7) C(8) 1.377(8) . . yes C(9) C(10) 1.408(7) . . yes C(10) C(11) 1.344(8) . . yes C(11) C(12) 1.374(8) . . yes C(12) C(13) 1.390(8) . . yes C(14) C(15) 1.376(7) . . yes C(15) C(16) 1.355(7) . . yes C(16) C(17) 1.378(8) . . yes C(17) C(18) 1.351(7) . . yes C(19) C(20) 1.398(6) . . yes C(19) C(24) 1.389(7) . . yes C(19) B(1) 1.641(7) . . yes C(20) C(21) 1.374(7) . . yes C(21) C(22) 1.366(7) . . yes C(22) C(23) 1.363(8) . . yes C(23) C(24) 1.397(7) . . yes C(25) C(26) 1.412(7) . . yes C(25) C(30) 1.389(6) . . yes C(25) B(1) 1.645(7) . . yes C(26) C(27) 1.399(7) . . yes C(27) C(28) 1.360(7) . . yes C(28) C(29) 1.392(7) . . yes C(29) C(30) 1.380(7) . . yes C(31) C(32) 1.390(7) . . yes C(31) C(36) 1.397(7) . . yes C(31) B(1) 1.649(7) . . yes C(32) C(33) 1.429(7) . . yes C(33) C(34) 1.385(8) . . yes C(34) C(35) 1.376(8) . . yes C(35) C(36) 1.397(7) . . yes C(37) C(38) 1.390(7) . . yes C(37) C(42) 1.393(6) . . yes C(37) B(1) 1.684(8) . . yes C(38) C(39) 1.375(7) . . yes C(39) C(40) 1.398(7) . . yes C(40) C(41) 1.360(7) . . yes C(41) C(42) 1.390(7) . . yes loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Mn(1) Mn(1) 2.656(2) . 7_546 ? C(1) C(24) 3.594(7) . 7_556 ? C(5) C(23) 3.417(9) . 7_556 ? C(7) C(36) 3.543(8) . 3_556 ? C(8) C(39) 3.579(8) . 3_556 ? C(12) C(36) 3.522(8) . 5_545 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Mn(1) Mn(1) N(1) C(1) -61.5(4) . 7_546 7_546 7_546 yes Mn(1) Mn(1) N(1) C(2) 56.6(4) . 7_546 7_546 7_546 yes Mn(1) Mn(1) N(1) C(3) 178.3(2) . 7_546 7_546 7_546 yes Mn(1) Mn(1) N(2) C(4) 129.1(4) . 7_546 7_546 7_546 yes Mn(1) Mn(1) N(2) C(8) -68.8(5) . 7_546 7_546 7_546 yes Mn(1) Mn(1) N(3) C(9) -120.3(3) . 7_546 7_546 7_546 yes Mn(1) Mn(1) N(3) C(13) 66.8(5) . 7_546 7_546 7_546 yes Mn(1) Mn(1) N(4) C(14) -179.5(3) . 7_546 7_546 7_546 yes Mn(1) Mn(1) N(4) C(18) 1.7(5) . 7_546 7_546 7_546 yes Mn(1) O(1) Mn(1) O(1) 0.0000(1) . . 7_546 7_546 yes Mn(1) O(1) Mn(1) N(1) -180.0(1) . . 7_546 7_546 yes Mn(1) O(1) Mn(1) N(2) 105.0(2) . . 7_546 7_546 yes Mn(1) O(1) Mn(1) N(3) -105.8(2) . . 7_546 7_546 yes Mn(1) O(1) Mn(1) N(4) -177(2) . . 7_546 7_546 yes Mn(1) O(1) Mn(1) O(1) 0.0000(1) . 7_546 7_546 . yes Mn(1) O(1) Mn(1) N(1) 179(1) . 7_546 7_546 7_546 yes Mn(1) O(1) Mn(1) N(2) -96.4(2) . 7_546 7_546 7_546 yes Mn(1) O(1) Mn(1) N(3) 96.5(1) . 7_546 7_546 7_546 yes Mn(1) O(1) Mn(1) N(4) 179.8(2) . 7_546 7_546 7_546 yes Mn(1) N(1) C(1) C(4) 53.6(4) . . . . yes Mn(1) N(1) C(2) C(9) -54.9(4) . . . . yes Mn(1) N(1) C(3) C(14) -2.3(5) . . . . yes Mn(1) N(2) C(4) C(1) 18.2(6) . . . . yes Mn(1) N(2) C(4) C(5) -164.5(5) . . . . yes Mn(1) N(2) C(8) C(7) 160.2(5) . . . . yes Mn(1) N(3) C(9) C(2) -6.7(5) . . . . yes Mn(1) N(3) C(9) C(10) 171.2(4) . . . . yes Mn(1) N(3) C(13) C(12) -169.5(4) . . . . yes Mn(1) N(4) C(14) C(3) -0.9(6) . . . . yes Mn(1) N(4) C(14) C(15) -177.7(4) . . . . yes Mn(1) N(4) C(18) C(17) 179.5(4) . . . . yes O(1) Mn(1) Mn(1) O(1) 180.0 . . 7_546 7_546 yes O(1) Mn(1) Mn(1) N(1) 0.1(2) . . 7_546 7_546 yes O(1) Mn(1) Mn(1) N(2) -83.8(2) . . 7_546 7_546 yes O(1) Mn(1) Mn(1) N(3) 83.2(2) . . 7_546 7_546 yes O(1) Mn(1) Mn(1) N(4) 179.7(2) . . 7_546 7_546 yes O(1) Mn(1) O(1) Mn(1) 0.0 . . 7_546 7_546 yes O(1) Mn(1) N(1) C(1) -119(1) . . . . yes O(1) Mn(1) N(1) C(2) 122(1) . . . . yes O(1) Mn(1) N(1) C(3) 1(1) . . . . yes O(1) Mn(1) N(2) C(4) -175.2(4) . . . . yes O(1) Mn(1) N(2) C(8) 22.6(5) . . . . yes O(1) Mn(1) N(3) C(9) 166.7(3) . . . . yes O(1) Mn(1) N(3) C(13) -20.5(5) . . . . yes O(1) Mn(1) N(4) C(14) 179.7(4) . . . . yes O(1) Mn(1) N(4) C(18) -1.5(4) . . . . yes O(1) Mn(1) Mn(1) O(1) -180.0 . 7_546 . 7_546 yes O(1) Mn(1) Mn(1) N(1) 179.9(2) . 7_546 . . yes O(1) Mn(1) Mn(1) N(2) -96.2(2) . 7_546 . . yes O(1) Mn(1) Mn(1) N(3) 96.8(2) . 7_546 . . yes O(1) Mn(1) Mn(1) N(4) 0.3(2) . 7_546 . . yes O(1) Mn(1) O(1) Mn(1) 0.0 . 7_546 7_546 . yes O(1) Mn(1) N(1) C(1) -61.4(3) . 7_546 7_546 7_546 yes O(1) Mn(1) N(1) C(2) 56.7(3) . 7_546 7_546 7_546 yes O(1) Mn(1) N(1) C(3) 178.4(3) . 7_546 7_546 7_546 yes O(1) Mn(1) N(2) C(4) 84.4(4) . 7_546 7_546 7_546 yes O(1) Mn(1) N(2) C(8) -113.4(5) . 7_546 7_546 7_546 yes O(1) Mn(1) N(3) C(9) -75.8(3) . 7_546 7_546 7_546 yes O(1) Mn(1) N(3) C(13) 111.4(5) . 7_546 7_546 7_546 yes O(1) Mn(1) N(4) C(14) -2(2) . 7_546 7_546 7_546 yes O(1) Mn(1) N(4) C(18) 178(2) . 7_546 7_546 7_546 yes N(1) Mn(1) Mn(1) N(1) 180.0 . . 7_546 7_546 yes N(1) Mn(1) Mn(1) N(2) 96.2(2) . . 7_546 7_546 yes N(1) Mn(1) Mn(1) N(3) -96.8(2) . . 7_546 7_546 yes N(1) Mn(1) Mn(1) N(4) -0.4(3) . . 7_546 7_546 yes N(1) Mn(1) N(2) C(4) 9.7(4) . . . . yes N(1) Mn(1) N(2) C(8) -152.5(5) . . . . yes N(1) Mn(1) N(3) C(9) -18.2(3) . . . . yes N(1) Mn(1) N(3) C(13) 154.6(5) . . . . yes N(1) Mn(1) N(4) C(14) -0.3(4) . . . . yes N(1) Mn(1) N(4) C(18) 178.5(4) . . . . yes N(1) C(1) C(4) N(2) -48.2(6) . . . . yes N(1) C(1) C(4) C(5) 134.6(6) . . . . yes N(1) C(2) C(9) N(3) 40.7(6) . . . . yes N(1) C(2) C(9) C(10) -137.0(5) . . . . yes N(1) C(3) C(14) N(4) 2.2(7) . . . . yes N(1) C(3) C(14) C(15) 179.1(4) . . . . yes N(2) Mn(1) Mn(1) N(2) 180.0 . . 7_546 7_546 yes N(2) Mn(1) Mn(1) N(3) -13.0(2) . . 7_546 7_546 yes N(2) Mn(1) Mn(1) N(4) 83.5(2) . . 7_546 7_546 yes N(2) Mn(1) N(1) C(1) -33.7(3) . . . . yes N(2) Mn(1) N(1) C(2) -151.8(3) . . . . yes N(2) Mn(1) N(1) C(3) 86.5(3) . . . . yes N(2) Mn(1) N(3) C(9) -36.4(5) . . . . yes N(2) Mn(1) N(3) C(13) 136.4(4) . . . . yes N(2) Mn(1) N(4) C(14) -75.8(4) . . . . yes N(2) Mn(1) N(4) C(18) 103.0(4) . . . . yes N(2) C(4) C(5) C(6) 3.2(9) . . . . yes N(2) C(8) C(7) C(6) 0(1) . . . . yes N(3) Mn(1) Mn(1) N(3) -180.0 . . 7_546 7_546 yes N(3) Mn(1) Mn(1) N(4) -83.6(2) . . 7_546 7_546 yes N(3) Mn(1) N(1) C(1) 156.6(3) . . . . yes N(3) Mn(1) N(1) C(2) 38.5(3) . . . . yes N(3) Mn(1) N(1) C(3) -83.3(3) . . . . yes N(3) Mn(1) N(2) C(4) 27.7(5) . . . . yes N(3) Mn(1) N(2) C(8) -134.4(5) . . . . yes N(3) Mn(1) N(4) C(14) 74.4(4) . . . . yes N(3) Mn(1) N(4) C(18) -106.8(4) . . . . yes N(3) C(9) C(10) C(11) 2.2(8) . . . . yes N(3) C(13) C(12) C(11) -3.3(9) . . . . yes N(4) Mn(1) Mn(1) N(4) 180.0 . . 7_546 7_546 yes N(4) Mn(1) N(1) C(1) -118.8(3) . . . . yes N(4) Mn(1) N(1) C(2) 123.1(3) . . . . yes N(4) Mn(1) N(1) C(3) 1.4(3) . . . . yes N(4) Mn(1) N(2) C(4) 91.6(4) . . . . yes N(4) Mn(1) N(2) C(8) -70.6(5) . . . . yes N(4) Mn(1) N(3) C(9) -100.4(3) . . . . yes N(4) Mn(1) N(3) C(13) 72.4(5) . . . . yes N(4) C(14) C(15) C(16) -4.0(8) . . . . yes N(4) C(18) C(17) C(16) 0.7(9) . . . . yes C(1) N(1) C(2) C(9) -170.5(4) . . . . yes C(1) N(1) C(3) C(14) 115.8(5) . . . . yes C(1) C(4) N(2) C(8) -178.2(5) . . . . yes C(1) C(4) C(5) C(6) -179.7(6) . . . . yes C(2) N(1) C(1) C(4) 168.9(4) . . . . yes C(2) N(1) C(3) C(14) -120.8(5) . . . . yes C(2) C(9) N(3) C(13) 179.9(5) . . . . yes C(2) C(9) C(10) C(11) 179.8(5) . . . . yes C(3) N(1) C(1) C(4) -66.9(5) . . . . yes C(3) N(1) C(2) C(9) 66.2(5) . . . . yes C(3) C(14) N(4) C(18) -179.8(5) . . . . yes C(3) C(14) C(15) C(16) 179.3(5) . . . . yes C(4) N(2) C(8) C(7) -0.7(10) . . . . yes C(4) C(5) C(6) C(7) -4(1) . . . . yes C(5) C(4) N(2) C(8) -0.9(9) . . . . yes C(5) C(6) C(7) C(8) 2(1) . . . . yes C(9) N(3) C(13) C(12) 2.8(8) . . . . yes C(9) C(10) C(11) C(12) -2.7(9) . . . . yes C(10) C(9) N(3) C(13) -2.2(8) . . . . yes C(10) C(11) C(12) C(13) 3.2(9) . . . . yes C(14) N(4) C(18) C(17) -1.7(8) . . . . yes C(14) C(15) C(16) C(17) 3.0(8) . . . . yes C(15) C(14) N(4) C(18) 3.4(8) . . . . yes C(15) C(16) C(17) C(18) -1.4(9) . . . . yes C(19) C(20) C(21) C(22) -0.2(9) . . . . yes C(19) C(24) C(23) C(22) -2.6(9) . . . . yes C(19) B(1) C(25) C(26) 95.4(6) . . . . yes C(19) B(1) C(25) C(30) -85.4(6) . . . . yes C(19) B(1) C(31) C(32) 26.7(7) . . . . yes C(19) B(1) C(31) C(36) -158.5(5) . . . . yes C(19) B(1) C(37) C(38) -162.5(4) . . . . yes C(19) B(1) C(37) C(42) 20.3(6) . . . . yes C(20) C(19) C(24) C(23) 1.6(8) . . . . yes C(20) C(19) B(1) C(25) 166.7(5) . . . . yes C(20) C(19) B(1) C(31) 50.1(7) . . . . yes C(20) C(19) B(1) C(37) -70.4(6) . . . . yes C(20) C(21) C(22) C(23) -0.7(9) . . . . yes C(21) C(20) C(19) C(24) -0.3(8) . . . . yes C(21) C(20) C(19) B(1) -176.2(5) . . . . yes C(21) C(22) C(23) C(24) 2.1(9) . . . . yes C(23) C(24) C(19) B(1) 177.4(5) . . . . yes C(24) C(19) B(1) C(25) -8.8(7) . . . . yes C(24) C(19) B(1) C(31) -125.4(5) . . . . yes C(24) C(19) B(1) C(37) 114.0(6) . . . . yes C(25) C(26) C(27) C(28) 3.8(9) . . . . yes C(25) C(30) C(29) C(28) 1.2(8) . . . . yes C(25) B(1) C(31) C(32) -92.7(6) . . . . yes C(25) B(1) C(31) C(36) 82.1(6) . . . . yes C(25) B(1) C(37) C(38) -39.2(6) . . . . yes C(25) B(1) C(37) C(42) 143.6(5) . . . . yes C(26) C(25) C(30) C(29) 0.5(8) . . . . yes C(26) C(25) B(1) C(31) -146.5(5) . . . . yes C(26) C(25) B(1) C(37) -28.3(6) . . . . yes C(26) C(27) C(28) C(29) -1.8(8) . . . . yes C(27) C(26) C(25) C(30) -3.0(8) . . . . yes C(27) C(26) C(25) B(1) 176.3(5) . . . . yes C(27) C(28) C(29) C(30) -0.6(8) . . . . yes C(29) C(30) C(25) B(1) -178.7(5) . . . . yes C(30) C(25) B(1) C(31) 32.7(7) . . . . yes C(30) C(25) B(1) C(37) 150.9(5) . . . . yes C(31) C(32) C(33) C(34) 3.6(8) . . . . yes C(31) C(36) C(35) C(34) -1.6(9) . . . . yes C(31) B(1) C(37) C(38) 77.2(6) . . . . yes C(31) B(1) C(37) C(42) -99.9(5) . . . . yes C(32) C(31) C(36) C(35) 2.3(8) . . . . yes C(32) C(31) B(1) C(37) 148.6(5) . . . . yes C(32) C(33) C(34) C(35) -2.5(9) . . . . yes C(33) C(32) C(31) C(36) -3.4(8) . . . . yes C(33) C(32) C(31) B(1) 171.9(5) . . . . yes C(33) C(34) C(35) C(36) 1.7(9) . . . . yes C(35) C(36) C(31) B(1) -172.8(5) . . . . yes C(36) C(31) B(1) C(37) -36.6(6) . . . . yes C(37) C(38) C(39) C(40) 1.4(9) . . . . yes C(37) C(42) C(41) C(40) -1.0(9) . . . . yes C(38) C(37) C(42) C(41) 1.3(7) . . . . yes C(38) C(39) C(40) C(41) -1.0(9) . . . . yes C(39) C(38) C(37) C(42) -1.5(8) . . . . yes C(39) C(38) C(37) B(1) -178.8(5) . . . . yes C(39) C(40) C(41) C(42) 0.8(8) . . . . yes C(41) C(42) C(37) B(1) 178.5(5) . . . . yes C(41) C(42) C(37) B(1) 178.5(5) . . . . yes
1100740.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100740.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100740 loop_ _publ_author_name 'St\'ephane A. Baudron' 'Narcis Avarvari' 'Patrick Batail' _publ_contact_author ; Dr Patrick Batail Laboratoire Chimie Ing\'enierie Mol\'eculaires et Mat\'eriaux d'Angers, UMR 6200 CNRS-Universit\'e d'Angers, Bat. K, 2, Boulevard Lavoisier, Angers, France ; _publ_contact_author_email patrick.batail@univ-angers.fr _publ_contact_author_fax '33 2 41 73 50 11' _publ_contact_author_phone '33 2 41 73 52 64' _publ_section_title ; A Straightforward Synthesis of Diverse Nickel Dithiolene Complexes Appended with Hydrogen-Bond Donor/Acceptor Groups ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3380 _journal_page_last 3382 _journal_paper_doi 10.1021/ic050174n _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C32 H22 N2 Ni O4 P S4' _chemical_formula_weight 716.44 _chemical_name_common (PPh4)[Ni(midt)2] _chemical_name_systematic ; ? ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 77.422(16) _cell_angle_beta 76.190(17) _cell_angle_gamma 74.858(17) _cell_formula_units_Z 2 _cell_length_a 10.9413(17) _cell_length_b 11.9501(17) _cell_length_c 13.0235(16) _cell_measurement_reflns_used 7685 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 52.1 _cell_measurement_theta_min 3.3 _cell_volume 1574.1(4) _computing_cell_refinement 'SELECT, CELL (STOE-IPDS)' _computing_data_collection 'EXPOSE, (STOE-IPDS)' _computing_data_reduction 'INTEGRATE (STOE-IPDS)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 6.66 _diffrn_measured_fraction_theta_full 0.915 _diffrn_measured_fraction_theta_max 0.915 _diffrn_measurement_device_type STOE-IPDS _diffrn_measurement_method 'Oscillation, Phi. incr. = 1.8' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0608 _diffrn_reflns_av_sigmaI/netI 0.1016 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 15845 _diffrn_reflns_theta_full 25.98 _diffrn_reflns_theta_max 25.98 _diffrn_reflns_theta_min 1.97 _exptl_absorpt_coefficient_mu 0.973 _exptl_absorpt_correction_T_max 0.7483 _exptl_absorpt_correction_T_min 0.5358 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'FACEIT, STOE-IPDS' _exptl_crystal_colour black _exptl_crystal_density_diffrn 1.512 _exptl_crystal_density_meas ? _exptl_crystal_density_method . _exptl_crystal_description prism _exptl_crystal_F_000 734 _exptl_crystal_size_max 0.693 _exptl_crystal_size_mid 0.5775 _exptl_crystal_size_min 0.2694 _refine_diff_density_max 0.458 _refine_diff_density_min -0.209 _refine_diff_density_rms 0.062 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.781 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 397 _refine_ls_number_reflns 5657 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.781 _refine_ls_R_factor_all 0.0872 _refine_ls_R_factor_gt 0.0396 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0240P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0702 _refine_ls_wR_factor_ref 0.0783 _reflns_number_gt 3057 _reflns_number_total 5657 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic050174nsi20050201_114424.cif _cod_data_source_block sb30p3 _cod_database_code 1100740 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.66767(5) 0.94764(4) 0.70560(4) 0.04092(14) Uani 1 1 d . . . S1 S 0.67352(10) 0.83794(8) 0.86200(7) 0.0480(3) Uani 1 1 d . . . S2 S 0.65111(10) 1.10817(7) 0.76522(8) 0.0476(3) Uani 1 1 d . . . S3 S 0.69541(13) 0.78562(8) 0.64504(8) 0.0682(4) Uani 1 1 d . . . S4 S 0.65844(10) 1.05725(7) 0.54931(7) 0.0470(3) Uani 1 1 d . . . C1 C 0.6825(3) 0.9201(3) 1.0509(3) 0.0400(9) Uani 1 1 d . . . C2 C 0.6705(3) 0.9383(3) 0.9378(3) 0.0362(9) Uani 1 1 d . . . C3 C 0.6619(3) 1.0539(3) 0.8953(3) 0.0367(9) Uani 1 1 d . . . C4 C 0.6709(3) 1.1155(3) 0.9801(3) 0.0437(9) Uani 1 1 d . . . C5 C 0.6984(5) 0.7724(3) 0.4263(3) 0.0672(14) Uani 1 1 d . . . C6 C 0.6900(4) 0.8375(3) 0.5141(3) 0.0483(10) Uani 1 1 d . . . C7 C 0.6740(3) 0.9534(3) 0.4725(3) 0.0389(9) Uani 1 1 d . . . C8 C 0.6761(3) 0.9685(3) 0.3558(3) 0.0415(9) Uani 1 1 d . . . O1 O 0.6940(3) 0.8298(2) 1.1163(2) 0.0572(8) Uani 1 1 d . . . O2 O 0.6738(3) 1.2163(2) 0.9751(2) 0.0656(8) Uani 1 1 d . . . O3 O 0.7083(4) 0.6700(2) 0.4303(2) 0.1163(16) Uani 1 1 d . . . O4 O 0.6651(3) 1.0575(2) 0.2899(2) 0.0542(7) Uani 1 1 d . . . N1 N 0.6833(3) 1.0297(2) 1.0694(2) 0.0462(8) Uani 1 1 d . . . H1 H 0.6906 1.0429 1.1298 0.055 Uiso 1 1 calc R . . N2 N 0.6923(3) 0.8567(2) 0.3352(2) 0.0533(9) Uani 1 1 d . . . H2 H 0.6979 0.8410 0.2726 0.064 Uiso 1 1 calc R . . P1 P 0.84342(9) 1.36932(7) 0.27465(8) 0.0380(2) Uani 1 1 d . . . C9 C 0.8103(4) 1.3775(3) 0.4143(3) 0.0439(9) Uani 1 1 d . . . C10 C 0.6868(4) 1.3837(3) 0.4732(3) 0.0554(11) Uani 1 1 d . . . H10 H 0.6197 1.3841 0.4406 0.066 Uiso 1 1 calc R . . C11 C 0.6635(5) 1.3894(4) 0.5816(4) 0.0771(15) Uani 1 1 d . . . H11 H 0.5803 1.3941 0.6219 0.093 Uiso 1 1 calc R . . C12 C 0.7617(7) 1.3882(5) 0.6292(4) 0.0935(18) Uani 1 1 d . . . H12 H 0.7453 1.3920 0.7019 0.112 Uiso 1 1 calc R . . C13 C 0.8835(6) 1.3815(4) 0.5716(4) 0.0937(17) Uani 1 1 d . . . H13 H 0.9498 1.3811 0.6051 0.112 Uiso 1 1 calc R . . C14 C 0.9102(5) 1.3754(4) 0.4630(4) 0.0704(13) Uani 1 1 d . . . H14 H 0.9940 1.3700 0.4237 0.084 Uiso 1 1 calc R . . C15 C 0.9071(3) 1.2191(3) 0.2555(3) 0.0447(9) Uani 1 1 d . . . C16 C 0.9231(4) 1.1900(4) 0.1556(4) 0.0719(13) Uani 1 1 d . . . H16 H 0.8984 1.2473 0.0989 0.086 Uiso 1 1 calc R . . C17 C 0.9760(5) 1.0755(5) 0.1403(5) 0.0950(18) Uani 1 1 d . . . H17 H 0.9886 1.0555 0.0729 0.114 Uiso 1 1 calc R . . C18 C 1.0100(5) 0.9915(4) 0.2242(6) 0.0874(19) Uani 1 1 d . . . H18 H 1.0456 0.9143 0.2134 0.105 Uiso 1 1 calc R . . C19 C 0.9925(4) 1.0189(4) 0.3229(5) 0.0805(15) Uani 1 1 d . . . H19 H 1.0148 0.9606 0.3796 0.097 Uiso 1 1 calc R . . C20 C 0.9415(4) 1.1334(3) 0.3395(4) 0.0576(11) Uani 1 1 d . . . H20 H 0.9305 1.1525 0.4071 0.069 Uiso 1 1 calc R . . C21 C 0.6995(3) 1.4259(3) 0.2204(3) 0.0353(8) Uani 1 1 d . . . C22 C 0.6252(4) 1.3524(3) 0.2134(3) 0.0590(11) Uani 1 1 d . . . H22 H 0.6478 1.2722 0.2386 0.071 Uiso 1 1 calc R . . C23 C 0.5162(4) 1.3990(4) 0.1684(4) 0.0725(14) Uani 1 1 d . . . H23 H 0.4660 1.3495 0.1627 0.087 Uiso 1 1 calc R . . C24 C 0.4817(4) 1.5169(4) 0.1324(3) 0.0594(12) Uani 1 1 d . . . H24 H 0.4091 1.5470 0.1013 0.071 Uiso 1 1 calc R . . C25 C 0.5528(4) 1.5898(3) 0.1420(3) 0.0569(11) Uani 1 1 d . . . H25 H 0.5274 1.6704 0.1198 0.068 Uiso 1 1 calc R . . C26 C 0.6619(4) 1.5450(3) 0.1843(3) 0.0505(10) Uani 1 1 d . . . H26 H 0.7117 1.5955 0.1888 0.061 Uiso 1 1 calc R . . C27 C 0.9590(3) 1.4564(3) 0.2084(3) 0.0428(9) Uani 1 1 d . . . C28 C 0.9386(4) 1.5695(3) 0.2272(3) 0.0594(11) Uani 1 1 d . . . H28 H 0.8676 1.5982 0.2775 0.071 Uiso 1 1 calc R . . C29 C 1.0221(6) 1.6406(4) 0.1724(4) 0.0817(16) Uani 1 1 d . . . H29 H 1.0063 1.7177 0.1840 0.098 Uiso 1 1 calc R . . C30 C 1.1282(5) 1.5973(6) 0.1010(5) 0.0899(19) Uani 1 1 d . . . H30 H 1.1848 1.6450 0.0638 0.108 Uiso 1 1 calc R . . C31 C 1.1514(5) 1.4862(6) 0.0839(4) 0.0891(17) Uani 1 1 d . . . H31 H 1.2255 1.4569 0.0368 0.107 Uiso 1 1 calc R . . C32 C 1.0672(4) 1.4155(4) 0.1351(3) 0.0656(12) Uani 1 1 d . . . H32 H 1.0829 1.3396 0.1206 0.079 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0495(3) 0.0389(2) 0.0302(3) -0.00738(18) -0.0042(2) -0.0047(2) S1 0.0721(7) 0.0362(5) 0.0349(6) -0.0060(4) -0.0084(5) -0.0123(5) S2 0.0671(7) 0.0358(5) 0.0358(6) -0.0027(4) -0.0129(5) -0.0045(5) S3 0.1254(11) 0.0373(5) 0.0327(6) -0.0047(4) -0.0093(7) -0.0084(6) S4 0.0693(7) 0.0376(5) 0.0352(6) -0.0057(4) -0.0122(5) -0.0119(5) C1 0.041(2) 0.038(2) 0.040(2) -0.0084(18) -0.0052(19) -0.0075(17) C2 0.033(2) 0.0385(19) 0.036(2) -0.0088(16) -0.0058(18) -0.0057(16) C3 0.038(2) 0.0341(19) 0.037(2) -0.0056(16) -0.0096(18) -0.0027(16) C4 0.046(2) 0.044(2) 0.041(2) -0.0070(18) -0.012(2) -0.0057(18) C5 0.116(4) 0.041(2) 0.033(2) -0.0111(19) -0.005(3) -0.003(2) C6 0.069(3) 0.037(2) 0.032(2) -0.0071(17) -0.004(2) -0.0063(19) C7 0.043(2) 0.038(2) 0.034(2) -0.0070(16) -0.0081(18) -0.0054(17) C8 0.046(2) 0.040(2) 0.038(2) -0.0093(18) -0.006(2) -0.0086(18) O1 0.095(2) 0.0414(14) 0.0361(16) -0.0017(12) -0.0195(16) -0.0149(14) O2 0.107(2) 0.0380(15) 0.0615(19) -0.0050(13) -0.0306(18) -0.0213(16) O3 0.249(5) 0.0380(17) 0.049(2) -0.0126(14) -0.019(3) -0.015(2) O4 0.086(2) 0.0403(14) 0.0368(16) 0.0013(12) -0.0181(15) -0.0144(14) N1 0.063(2) 0.0409(17) 0.0383(19) -0.0073(14) -0.0176(17) -0.0097(15) N2 0.085(3) 0.0442(18) 0.0280(18) -0.0091(14) -0.0073(18) -0.0094(17) P1 0.0402(6) 0.0386(5) 0.0340(6) -0.0061(4) -0.0059(5) -0.0075(4) C9 0.050(3) 0.042(2) 0.039(2) -0.0049(16) -0.007(2) -0.0115(18) C10 0.064(3) 0.055(2) 0.040(2) -0.0039(18) -0.006(2) -0.008(2) C11 0.088(4) 0.070(3) 0.050(3) -0.006(2) 0.013(3) -0.005(3) C12 0.123(5) 0.114(4) 0.039(3) -0.016(3) -0.002(4) -0.028(4) C13 0.123(5) 0.129(5) 0.049(3) -0.020(3) -0.029(4) -0.048(4) C14 0.066(3) 0.104(3) 0.049(3) -0.013(3) -0.014(3) -0.030(3) C15 0.042(2) 0.043(2) 0.048(3) -0.0083(18) -0.013(2) -0.0045(18) C16 0.084(4) 0.067(3) 0.063(3) -0.028(2) -0.019(3) 0.005(3) C17 0.083(4) 0.098(4) 0.114(5) -0.071(4) -0.008(4) -0.003(3) C18 0.054(3) 0.057(3) 0.150(6) -0.038(4) -0.017(4) 0.005(2) C19 0.071(4) 0.044(3) 0.122(5) 0.000(3) -0.035(3) -0.001(2) C20 0.052(3) 0.046(2) 0.073(3) -0.003(2) -0.020(2) -0.006(2) C21 0.041(2) 0.0339(19) 0.033(2) -0.0069(15) -0.0041(17) -0.0130(16) C22 0.061(3) 0.044(2) 0.077(3) -0.003(2) -0.024(3) -0.016(2) C23 0.061(3) 0.081(3) 0.091(4) -0.016(3) -0.028(3) -0.029(3) C24 0.043(3) 0.074(3) 0.062(3) -0.014(2) -0.020(2) -0.002(2) C25 0.053(3) 0.044(2) 0.071(3) -0.014(2) -0.018(2) 0.004(2) C26 0.049(3) 0.044(2) 0.063(3) -0.0108(19) -0.018(2) -0.0094(19) C27 0.043(2) 0.049(2) 0.037(2) 0.0013(17) -0.015(2) -0.0117(18) C28 0.061(3) 0.061(2) 0.066(3) -0.009(2) -0.014(2) -0.027(2) C29 0.094(4) 0.069(3) 0.099(4) 0.012(3) -0.041(4) -0.048(3) C30 0.060(4) 0.124(5) 0.082(4) 0.046(4) -0.031(3) -0.050(4) C31 0.045(3) 0.123(4) 0.078(4) 0.009(3) 0.005(3) -0.017(3) C32 0.046(3) 0.078(3) 0.062(3) -0.002(2) -0.005(2) -0.007(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S3 Ni1 S2 176.91(6) . . ? S3 Ni1 S1 86.15(4) . . ? S2 Ni1 S1 93.62(4) . . ? S3 Ni1 S4 93.66(4) . . ? S2 Ni1 S4 86.62(4) . . ? S1 Ni1 S4 179.03(5) . . ? C2 S1 Ni1 101.16(13) . . ? C3 S2 Ni1 100.74(11) . . ? C6 S3 Ni1 101.07(12) . . ? C7 S4 Ni1 100.68(12) . . ? O1 C1 N1 125.2(3) . . ? O1 C1 C2 129.6(3) . . ? N1 C1 C2 105.2(3) . . ? C3 C2 C1 109.1(3) . . ? C3 C2 S1 121.5(3) . . ? C1 C2 S1 129.3(3) . . ? C2 C3 C4 107.9(3) . . ? C2 C3 S2 122.8(3) . . ? C4 C3 S2 129.2(3) . . ? O2 C4 N1 124.8(3) . . ? O2 C4 C3 129.7(3) . . ? N1 C4 C3 105.4(3) . . ? O3 C5 N2 125.5(4) . . ? O3 C5 C6 129.0(4) . . ? N2 C5 C6 105.4(3) . . ? C7 C6 C5 108.0(3) . . ? C7 C6 S3 122.6(3) . . ? C5 C6 S3 129.4(3) . . ? C6 C7 C8 108.8(3) . . ? C6 C7 S4 122.0(3) . . ? C8 C7 S4 129.2(3) . . ? O4 C8 N2 125.2(3) . . ? O4 C8 C7 129.6(3) . . ? N2 C8 C7 105.2(3) . . ? C4 N1 C1 112.4(3) . . ? C8 N2 C5 112.5(3) . . ? C9 P1 C27 107.77(17) . . ? C9 P1 C21 110.53(17) . . ? C27 P1 C21 109.29(16) . . ? C9 P1 C15 109.77(17) . . ? C27 P1 C15 110.26(17) . . ? C21 P1 C15 109.20(16) . . ? C10 C9 C14 120.3(4) . . ? C10 C9 P1 120.4(3) . . ? C14 C9 P1 119.3(3) . . ? C9 C10 C11 119.3(4) . . ? C12 C11 C10 120.2(5) . . ? C13 C12 C11 120.6(5) . . ? C12 C13 C14 120.7(5) . . ? C9 C14 C13 118.8(4) . . ? C20 C15 C16 119.9(4) . . ? C20 C15 P1 120.5(3) . . ? C16 C15 P1 119.6(3) . . ? C17 C16 C15 119.5(5) . . ? C18 C17 C16 120.0(5) . . ? C19 C18 C17 120.9(5) . . ? C18 C19 C20 120.1(5) . . ? C15 C20 C19 119.7(4) . . ? C22 C21 C26 119.0(3) . . ? C22 C21 P1 120.9(3) . . ? C26 C21 P1 120.1(3) . . ? C21 C22 C23 119.3(4) . . ? C24 C23 C22 120.6(4) . . ? C25 C24 C23 120.1(4) . . ? C24 C25 C26 119.9(4) . . ? C25 C26 C21 121.0(3) . . ? C28 C27 C32 118.2(3) . . ? C28 C27 P1 119.6(3) . . ? C32 C27 P1 122.1(3) . . ? C29 C28 C27 120.7(4) . . ? C30 C29 C28 119.5(5) . . ? C31 C30 C29 120.5(5) . . ? C30 C31 C32 120.8(5) . . ? C31 C32 C27 120.2(4) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 S3 2.1695(11) . ? Ni1 S2 2.1716(10) . ? Ni1 S1 2.1741(12) . ? Ni1 S4 2.1764(12) . ? S1 C2 1.701(3) . ? S2 C3 1.698(4) . ? S3 C6 1.693(4) . ? S4 C7 1.708(3) . ? C1 O1 1.219(4) . ? C1 N1 1.385(4) . ? C1 C2 1.475(5) . ? C2 C3 1.359(4) . ? C3 C4 1.487(5) . ? C4 O2 1.201(4) . ? C4 N1 1.381(4) . ? C5 O3 1.190(4) . ? C5 N2 1.381(5) . ? C5 C6 1.490(5) . ? C6 C7 1.353(4) . ? C7 C8 1.487(5) . ? C8 O4 1.211(4) . ? C8 N2 1.378(4) . ? P1 C9 1.786(4) . ? P1 C27 1.789(3) . ? P1 C21 1.790(4) . ? P1 C15 1.797(3) . ? C9 C10 1.377(5) . ? C9 C14 1.382(5) . ? C10 C11 1.388(6) . ? C11 C12 1.359(7) . ? C12 C13 1.355(7) . ? C13 C14 1.388(6) . ? C15 C20 1.376(5) . ? C15 C16 1.379(5) . ? C16 C17 1.378(6) . ? C17 C18 1.364(7) . ? C18 C19 1.353(7) . ? C19 C20 1.379(5) . ? C21 C22 1.372(4) . ? C21 C26 1.383(4) . ? C22 C23 1.386(6) . ? C23 C24 1.366(5) . ? C24 C25 1.352(5) . ? C25 C26 1.367(5) . ? C27 C28 1.378(5) . ? C27 C32 1.383(5) . ? C28 C29 1.377(5) . ? C29 C30 1.365(7) . ? C30 C31 1.342(6) . ? C31 C32 1.370(6) . ?
1100741.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100741.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100741 loop_ _publ_author_name 'St\'ephane A. Baudron' 'Narcis Avarvari' 'Patrick Batail' _publ_contact_author ; Dr Patrick Batail Laboratoire Chimie Ing\'enierie Mol\'eculaires et Mat\'eriaux d'Angers, UMR 6200 CNRS-Universit\'e d'Angers, Bat. K, 2, Boulevard Lavoisier, Angers, France ; _publ_contact_author_email patrick.batail@univ-angers.fr _publ_contact_author_fax '33 2 41 73 50 11' _publ_contact_author_phone '33 2 41 73 52 64' _publ_section_title ; A Straightforward Synthesis of Diverse Nickel Dithiolene Complexes Appended with Hydrogen-Bond Donor/Acceptor Groups ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3380 _journal_page_last 3382 _journal_paper_doi 10.1021/ic050174n _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C58 H45 N3 Ni O4 P2 S4' _chemical_formula_weight 1096.86 _chemical_name_common '(PPh4)2 Ni(midt)2 CH3CN' _chemical_name_systematic ; ? ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 93.924(11) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 13.0034(12) _cell_length_b 18.3544(14) _cell_length_c 22.048(2) _cell_measurement_reflns_used 7998 _cell_measurement_temperature 200(2) _cell_measurement_theta_max 52.1 _cell_measurement_theta_min 3.3 _cell_volume 5249.9(8) _computing_cell_refinement 'SELECT, CELL [STOE-IPDS]' _computing_data_collection 'EXPOSE [STOE-IPDS]' _computing_data_reduction 'INTEGRATE [STOE-IPDS]' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 200(2) _diffrn_detector_area_resol_mean 6.66 _diffrn_measured_fraction_theta_full 0.961 _diffrn_measured_fraction_theta_max 0.961 _diffrn_measurement_device_type STOE-IPDS _diffrn_measurement_method 'Oscillation, Phi. incr. = 1.1' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0612 _diffrn_reflns_av_sigmaI/netI 0.1008 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 42496 _diffrn_reflns_theta_full 25.96 _diffrn_reflns_theta_max 25.96 _diffrn_reflns_theta_min 1.85 _exptl_absorpt_coefficient_mu 0.640 _exptl_absorpt_correction_T_max 0.9582 _exptl_absorpt_correction_T_min 0.8498 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'FACEIT, STOE-IPDS' _exptl_crystal_colour black _exptl_crystal_density_diffrn 1.388 _exptl_crystal_density_meas ? _exptl_crystal_density_method . _exptl_crystal_description rod _exptl_crystal_F_000 2272 _exptl_crystal_size_max 0.5774 _exptl_crystal_size_mid 0.1156 _exptl_crystal_size_min 0.077 _refine_diff_density_max 0.390 _refine_diff_density_min -0.320 _refine_diff_density_rms 0.062 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.711 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 650 _refine_ls_number_reflns 9871 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.711 _refine_ls_R_factor_all 0.0670 _refine_ls_R_factor_gt 0.0291 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0488 _refine_ls_wR_factor_ref 0.0585 _reflns_number_gt 5803 _reflns_number_total 9871 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic050174nsi20050201_114447.cif _cod_data_source_block sb24p4f _cod_database_code 1100741 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.24542(2) 0.227568(18) 0.016087(14) 0.02289(8) Uani 1 1 d . . . S1 S 0.34317(5) 0.25941(4) 0.09754(3) 0.02684(15) Uani 1 1 d . . . S4 S 0.14794(5) 0.17660(4) -0.05781(3) 0.02947(16) Uani 1 1 d . . . S3 S 0.11322(5) 0.26466(4) 0.06598(3) 0.02976(15) Uani 1 1 d . . . S2 S 0.37750(5) 0.20876(4) -0.04040(3) 0.02869(16) Uani 1 1 d . . . N2 N -0.14615(15) 0.21759(12) -0.03274(9) 0.0313(5) Uani 1 1 d . . . H2 H -0.2115 0.2183 -0.0419 0.038 Uiso 1 1 calc R . . C3 C 0.47778(17) 0.23004(14) 0.01208(11) 0.0249(6) Uani 1 1 d . . . C7 C 0.02806(18) 0.19980(13) -0.03576(11) 0.0240(6) Uani 1 1 d . . . C6 C 0.01261(17) 0.23630(14) 0.01626(11) 0.0246(6) Uani 1 1 d . . . C2 C 0.46283(17) 0.25205(13) 0.06972(11) 0.0236(6) Uani 1 1 d . . . N1 N 0.63773(15) 0.25179(12) 0.05904(9) 0.0336(6) Uani 1 1 d . . . H1 H 0.7034 0.2544 0.0665 0.040 Uiso 1 1 calc R . . C1 C 0.56539(19) 0.26810(15) 0.10092(11) 0.0299(6) Uani 1 1 d . . . C5 C -0.09854(18) 0.24864(13) 0.01933(11) 0.0259(6) Uani 1 1 d . . . C8 C -0.07442(19) 0.18530(14) -0.06815(12) 0.0297(6) Uani 1 1 d . . . C4 C 0.58952(19) 0.23072(14) 0.00349(11) 0.0275(6) Uani 1 1 d . . . O2 O 0.63433(13) 0.21710(11) -0.04180(8) 0.0382(5) Uani 1 1 d . . . O3 O -0.14473(12) 0.27997(10) 0.05827(8) 0.0356(4) Uani 1 1 d . . . O4 O -0.09492(14) 0.15168(11) -0.11451(9) 0.0459(5) Uani 1 1 d . . . O1 O 0.58615(14) 0.29111(11) 0.15233(8) 0.0445(5) Uani 1 1 d . . . P1A P 0.25902(5) 0.53733(4) 0.12069(3) 0.02648(16) Uani 1 1 d . . . C1A C 0.2969(2) 0.62679(14) 0.14633(11) 0.0308(6) Uani 1 1 d . . . C2A C 0.3995(2) 0.64812(16) 0.14411(13) 0.0411(7) Uani 1 1 d . . . H2A H 0.4454 0.6189 0.1246 0.049 Uiso 1 1 calc R . . C3A C 0.4328(3) 0.71254(17) 0.17090(15) 0.0533(9) Uani 1 1 d . . . H3A H 0.5012 0.7266 0.1693 0.064 Uiso 1 1 calc R . . C4A C 0.3663(3) 0.75592(17) 0.19980(14) 0.0550(9) Uani 1 1 d . . . H4A H 0.3897 0.7991 0.2181 0.066 Uiso 1 1 calc R . . C5A C 0.2643(3) 0.73567(17) 0.20184(14) 0.0568(9) Uani 1 1 d . . . H5A H 0.2190 0.7657 0.2211 0.068 Uiso 1 1 calc R . . C6A C 0.2293(2) 0.67154(16) 0.17569(13) 0.0440(7) Uani 1 1 d . . . H6A H 0.1606 0.6580 0.1776 0.053 Uiso 1 1 calc R . . C7A C 0.29653(19) 0.47626(14) 0.18223(11) 0.0290(6) Uani 1 1 d . . . C8A C 0.2429(2) 0.47959(16) 0.23493(13) 0.0416(7) Uani 1 1 d . . . H8A H 0.1840 0.5082 0.2354 0.050 Uiso 1 1 calc R . . C9A C 0.2762(2) 0.44106(17) 0.28620(13) 0.0485(8) Uani 1 1 d . . . H9A H 0.2399 0.4436 0.3210 0.058 Uiso 1 1 calc R . . C10A C 0.3637(2) 0.39869(16) 0.28555(14) 0.0445(8) Uani 1 1 d . . . H10A H 0.3872 0.3734 0.3203 0.053 Uiso 1 1 calc R . . C11A C 0.4161(2) 0.39381(16) 0.23374(14) 0.0459(8) Uani 1 1 d . . . H11A H 0.4735 0.3636 0.2331 0.055 Uiso 1 1 calc R . . C12A C 0.3841(2) 0.43362(15) 0.18209(13) 0.0380(7) Uani 1 1 d . . . H12A H 0.4215 0.4315 0.1477 0.046 Uiso 1 1 calc R . . C13A C 0.31748(18) 0.51391(13) 0.05156(11) 0.0273(6) Uani 1 1 d . . . C14A C 0.3221(2) 0.44106(14) 0.03433(12) 0.0332(6) Uani 1 1 d . . . H14A H 0.3046 0.4047 0.0611 0.040 Uiso 1 1 calc R . . C15A C 0.3529(2) 0.42281(16) -0.02255(13) 0.0395(7) Uani 1 1 d . . . H15A H 0.3574 0.3741 -0.0337 0.047 Uiso 1 1 calc R . . C16A C 0.3770(2) 0.47672(16) -0.06283(13) 0.0402(7) Uani 1 1 d . . . H16A H 0.3968 0.4643 -0.1012 0.048 Uiso 1 1 calc R . . C17A C 0.3716(2) 0.54863(17) -0.04635(13) 0.0445(8) Uani 1 1 d . . . H17A H 0.3883 0.5848 -0.0736 0.053 Uiso 1 1 calc R . . C18A C 0.3416(2) 0.56780(15) 0.01080(12) 0.0365(7) Uani 1 1 d . . . H18A H 0.3376 0.6166 0.0217 0.044 Uiso 1 1 calc R . . C19A C 0.12221(19) 0.53231(14) 0.10346(11) 0.0265(6) Uani 1 1 d . . . C20A C 0.0696(2) 0.59107(15) 0.07564(11) 0.0317(6) Uani 1 1 d . . . H20A H 0.1030 0.6353 0.0712 0.038 Uiso 1 1 calc R . . C21A C -0.0327(2) 0.58308(16) 0.05470(12) 0.0373(7) Uani 1 1 d . . . H21A H -0.0686 0.6224 0.0370 0.045 Uiso 1 1 calc R . . C22A C -0.0813(2) 0.51691(17) 0.06005(12) 0.0382(7) Uani 1 1 d . . . H22A H -0.1500 0.5118 0.0461 0.046 Uiso 1 1 calc R . . C23A C -0.0285(2) 0.45794(16) 0.08601(12) 0.0372(7) Uani 1 1 d . . . H23A H -0.0613 0.4131 0.0886 0.045 Uiso 1 1 calc R . . C24A C 0.0731(2) 0.46580(14) 0.10812(11) 0.0305(6) Uani 1 1 d . . . H24A H 0.1084 0.4264 0.1261 0.037 Uiso 1 1 calc R . . P1B P 0.12659(5) 0.02771(4) 0.18886(3) 0.02647(16) Uani 1 1 d . . . C1B C 0.0083(2) 0.05343(14) 0.14670(12) 0.0312(6) Uani 1 1 d . . . C2B C -0.0238(2) 0.01646(16) 0.09372(13) 0.0462(8) Uani 1 1 d . . . H2B H 0.0175 -0.0196 0.0785 0.055 Uiso 1 1 calc R . . C3B C -0.1180(3) 0.03374(19) 0.06370(15) 0.0597(10) Uani 1 1 d . . . H3B H -0.1400 0.0090 0.0284 0.072 Uiso 1 1 calc R . . C4B C -0.1784(2) 0.08699(18) 0.08598(16) 0.0543(9) Uani 1 1 d . . . H4B H -0.2413 0.0982 0.0656 0.065 Uiso 1 1 calc R . . C5B C -0.1476(2) 0.12408(17) 0.13789(16) 0.0527(9) Uani 1 1 d . . . H5B H -0.1893 0.1602 0.1526 0.063 Uiso 1 1 calc R . . C6B C -0.0530(2) 0.10737(15) 0.16873(14) 0.0412(7) Uani 1 1 d . . . H6B H -0.0315 0.1325 0.2040 0.049 Uiso 1 1 calc R . . C7B C 0.10302(19) -0.04986(13) 0.23562(11) 0.0255(6) Uani 1 1 d . . . C8B C 0.0122(2) -0.08920(14) 0.22676(11) 0.0302(6) Uani 1 1 d . . . H8B H -0.0385 -0.0743 0.1976 0.036 Uiso 1 1 calc R . . C9B C -0.0027(2) -0.15086(15) 0.26155(12) 0.0372(7) Uani 1 1 d . . . H9B H -0.0638 -0.1771 0.2556 0.045 Uiso 1 1 calc R . . C10B C 0.0719(2) -0.17359(14) 0.30471(12) 0.0362(7) Uani 1 1 d . . . H10B H 0.0608 -0.2145 0.3283 0.043 Uiso 1 1 calc R . . C11B C 0.1636(2) -0.13539(15) 0.31296(12) 0.0354(7) Uani 1 1 d . . . H11B H 0.2148 -0.1516 0.3412 0.042 Uiso 1 1 calc R . . C12B C 0.1794(2) -0.07299(14) 0.27928(11) 0.0316(6) Uani 1 1 d . . . H12B H 0.2403 -0.0467 0.2856 0.038 Uiso 1 1 calc R . . C13B C 0.16807(19) 0.10304(13) 0.23680(11) 0.0264(6) Uani 1 1 d . . . C14B C 0.1467(2) 0.10580(15) 0.29749(12) 0.0428(8) Uani 1 1 d . . . H14B H 0.1110 0.0679 0.3145 0.051 Uiso 1 1 calc R . . C15B C 0.1786(3) 0.16497(16) 0.33257(13) 0.0535(9) Uani 1 1 d . . . H15B H 0.1645 0.1666 0.3733 0.064 Uiso 1 1 calc R . . C16B C 0.2308(2) 0.22142(16) 0.30787(12) 0.0419(7) Uani 1 1 d . . . H16B H 0.2522 0.2609 0.3319 0.050 Uiso 1 1 calc R . . C17B C 0.2515(2) 0.21969(15) 0.24767(12) 0.0388(7) Uani 1 1 d . . . H17B H 0.2864 0.2582 0.2309 0.047 Uiso 1 1 calc R . . C18B C 0.2203(2) 0.16056(14) 0.21195(12) 0.0328(6) Uani 1 1 d . . . H18B H 0.2344 0.1594 0.1712 0.039 Uiso 1 1 calc R . . C19B C 0.2237(2) 0.00663(13) 0.13698(11) 0.0293(6) Uani 1 1 d . . . C20B C 0.2881(2) -0.05325(14) 0.14720(12) 0.0318(6) Uani 1 1 d . . . H20B H 0.2795 -0.0837 0.1802 0.038 Uiso 1 1 calc R . . C21B C 0.3647(2) -0.06770(16) 0.10858(13) 0.0401(7) Uani 1 1 d . . . H21B H 0.4075 -0.1078 0.1156 0.048 Uiso 1 1 calc R . . C22B C 0.3778(2) -0.02248(16) 0.05940(13) 0.0427(7) Uani 1 1 d . . . H22B H 0.4296 -0.0323 0.0335 0.051 Uiso 1 1 calc R . . C23B C 0.3147(2) 0.03680(16) 0.04876(13) 0.0457(8) Uani 1 1 d . . . H23B H 0.3244 0.0672 0.0159 0.055 Uiso 1 1 calc R . . C24B C 0.2368(2) 0.05145(14) 0.08661(11) 0.0357(7) Uani 1 1 d . . . H24B H 0.1931 0.0909 0.0787 0.043 Uiso 1 1 calc R . . N1C N 0.5875(2) 0.53784(17) 0.22233(14) 0.0630(8) Uani 1 1 d . . . C2C C 0.5502(3) 0.56662(18) 0.26060(17) 0.0506(9) Uani 1 1 d . . . C1C C 0.5017(3) 0.6028(2) 0.30984(17) 0.0739(11) Uani 1 1 d . . . H1C1 H 0.4759 0.6494 0.2962 0.111 Uiso 1 1 calc R . . H1C2 H 0.5514 0.6093 0.3436 0.111 Uiso 1 1 calc R . . H1C3 H 0.4457 0.5735 0.3222 0.111 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.01705(16) 0.02769(18) 0.02404(16) 0.00052(15) 0.00221(13) -0.00077(14) S1 0.0201(3) 0.0365(4) 0.0241(3) 0.0009(3) 0.0028(3) -0.0022(3) S4 0.0198(3) 0.0391(4) 0.0298(4) -0.0080(3) 0.0037(3) -0.0002(3) S3 0.0185(3) 0.0425(4) 0.0282(3) -0.0085(3) 0.0007(3) 0.0011(3) S2 0.0180(3) 0.0418(4) 0.0264(3) -0.0041(3) 0.0029(3) -0.0023(3) N2 0.0155(11) 0.0474(14) 0.0309(12) -0.0116(11) 0.0003(9) -0.0010(10) C3 0.0170(12) 0.0270(14) 0.0308(14) 0.0039(12) 0.0016(11) -0.0012(11) C7 0.0196(13) 0.0273(14) 0.0253(13) 0.0009(11) 0.0037(11) -0.0018(10) C6 0.0174(12) 0.0305(15) 0.0261(13) 0.0007(12) 0.0034(11) -0.0013(11) C2 0.0182(12) 0.0281(14) 0.0243(13) 0.0037(11) 0.0012(11) -0.0026(10) N1 0.0146(11) 0.0550(16) 0.0312(12) -0.0066(11) 0.0006(10) -0.0017(10) C1 0.0243(14) 0.0358(16) 0.0295(14) 0.0039(13) 0.0025(12) 0.0004(12) C5 0.0213(13) 0.0299(15) 0.0268(14) -0.0036(11) 0.0040(12) -0.0009(11) C8 0.0240(14) 0.0342(16) 0.0310(15) -0.0032(13) 0.0022(12) -0.0025(12) C4 0.0225(13) 0.0289(14) 0.0307(14) -0.0016(12) -0.0002(12) 0.0008(12) O2 0.0235(10) 0.0585(13) 0.0332(10) -0.0128(10) 0.0063(9) 0.0003(9) O3 0.0211(9) 0.0522(12) 0.0340(10) -0.0154(10) 0.0045(8) -0.0003(9) O4 0.0286(11) 0.0673(15) 0.0414(12) -0.0260(11) -0.0005(9) -0.0032(10) O1 0.0309(11) 0.0754(15) 0.0271(10) -0.0096(10) 0.0018(9) -0.0074(10) P1A 0.0259(4) 0.0254(4) 0.0281(4) 0.0004(3) 0.0018(3) -0.0001(3) C1A 0.0332(16) 0.0296(15) 0.0286(15) 0.0030(12) -0.0050(13) 0.0008(12) C2A 0.0361(17) 0.0385(17) 0.0478(18) -0.0030(14) -0.0043(14) -0.0012(13) C3A 0.050(2) 0.043(2) 0.064(2) 0.0052(17) -0.0180(18) -0.0134(16) C4A 0.075(3) 0.0354(19) 0.051(2) -0.0050(15) -0.0235(19) -0.0076(18) C5A 0.078(3) 0.041(2) 0.051(2) -0.0175(16) 0.0015(19) 0.0056(18) C6A 0.0443(18) 0.0419(18) 0.0461(18) -0.0112(15) 0.0059(15) -0.0004(15) C7A 0.0287(14) 0.0272(15) 0.0304(15) -0.0007(12) -0.0036(12) -0.0038(12) C8A 0.0372(17) 0.0505(19) 0.0376(16) 0.0058(14) 0.0064(14) 0.0072(14) C9A 0.046(2) 0.065(2) 0.0338(17) 0.0134(16) 0.0024(15) -0.0020(17) C10A 0.0477(19) 0.0435(19) 0.0398(18) 0.0131(15) -0.0145(16) -0.0085(15) C11A 0.0391(18) 0.0472(19) 0.050(2) 0.0054(15) -0.0094(16) 0.0093(14) C12A 0.0347(16) 0.0413(17) 0.0376(16) 0.0022(14) 0.0000(14) 0.0031(13) C13A 0.0222(14) 0.0280(15) 0.0313(15) 0.0037(12) 0.0000(12) 0.0010(11) C14A 0.0351(16) 0.0314(16) 0.0329(15) 0.0028(13) 0.0007(13) 0.0014(12) C15A 0.0415(17) 0.0399(17) 0.0368(16) -0.0046(14) -0.0007(14) 0.0085(14) C16A 0.0345(16) 0.052(2) 0.0350(16) -0.0010(15) 0.0090(14) 0.0077(14) C17A 0.0475(19) 0.047(2) 0.0402(18) 0.0096(15) 0.0131(15) -0.0020(15) C18A 0.0405(17) 0.0301(16) 0.0400(17) 0.0016(13) 0.0094(14) -0.0016(13) C19A 0.0284(14) 0.0290(15) 0.0222(13) -0.0012(11) 0.0030(11) 0.0025(12) C20A 0.0310(15) 0.0363(16) 0.0283(15) 0.0022(12) 0.0045(13) 0.0012(12) C21A 0.0344(16) 0.0502(19) 0.0277(15) 0.0040(13) 0.0039(13) 0.0127(14) C22A 0.0250(15) 0.065(2) 0.0247(15) -0.0051(14) 0.0010(12) 0.0009(15) C23A 0.0328(16) 0.0498(19) 0.0298(15) -0.0005(14) 0.0066(13) -0.0111(14) C24A 0.0331(15) 0.0332(16) 0.0255(14) 0.0012(12) 0.0042(12) 0.0017(12) P1B 0.0309(4) 0.0254(4) 0.0231(3) 0.0015(3) 0.0013(3) -0.0009(3) C1B 0.0364(16) 0.0257(15) 0.0313(15) 0.0079(12) -0.0005(13) -0.0011(12) C2B 0.054(2) 0.0426(18) 0.0402(17) -0.0056(15) -0.0117(16) 0.0069(15) C3B 0.062(2) 0.064(2) 0.049(2) -0.0023(18) -0.0247(18) 0.0035(19) C4B 0.0426(19) 0.051(2) 0.066(2) 0.0158(18) -0.0196(18) 0.0039(16) C5B 0.0419(19) 0.045(2) 0.070(2) 0.0012(17) -0.0023(17) 0.0104(15) C6B 0.0405(17) 0.0372(17) 0.0453(18) -0.0031(14) -0.0023(15) 0.0047(14) C7B 0.0286(14) 0.0270(14) 0.0212(13) -0.0012(11) 0.0038(11) 0.0013(11) C8B 0.0311(15) 0.0315(16) 0.0280(14) 0.0005(12) 0.0021(12) -0.0013(12) C9B 0.0409(17) 0.0327(16) 0.0389(17) -0.0033(13) 0.0099(14) -0.0106(13) C10B 0.0521(19) 0.0265(15) 0.0314(16) 0.0064(12) 0.0124(14) -0.0005(14) C11B 0.0429(17) 0.0368(17) 0.0267(14) 0.0045(13) 0.0047(13) 0.0070(13) C12B 0.0322(15) 0.0345(16) 0.0284(15) 0.0015(12) 0.0038(13) -0.0024(12) C13B 0.0289(14) 0.0266(14) 0.0240(14) 0.0023(11) 0.0022(12) 0.0016(11) C14B 0.065(2) 0.0341(17) 0.0310(16) -0.0021(13) 0.0131(15) -0.0146(14) C15B 0.092(3) 0.045(2) 0.0254(15) -0.0060(14) 0.0162(17) -0.0188(18) C16B 0.060(2) 0.0336(17) 0.0329(15) -0.0108(14) 0.0061(14) -0.0135(15) C17B 0.0503(17) 0.0309(16) 0.0364(16) -0.0034(14) 0.0115(14) -0.0123(14) C18B 0.0418(17) 0.0322(16) 0.0254(14) 0.0008(12) 0.0079(13) -0.0050(13) C19B 0.0384(16) 0.0244(14) 0.0247(14) -0.0013(11) -0.0017(12) -0.0042(12) C20B 0.0366(16) 0.0301(15) 0.0289(14) 0.0023(12) 0.0037(13) -0.0009(12) C21B 0.0395(17) 0.0421(18) 0.0396(17) -0.0029(14) 0.0086(15) 0.0033(14) C22B 0.0445(18) 0.0463(19) 0.0397(17) -0.0078(15) 0.0205(15) -0.0038(15) C23B 0.069(2) 0.0423(19) 0.0278(16) 0.0041(14) 0.0189(16) -0.0059(17) C24B 0.0528(18) 0.0282(15) 0.0265(14) 0.0029(12) 0.0061(14) -0.0001(13) N1C 0.0509(19) 0.073(2) 0.064(2) -0.0081(17) -0.0055(16) 0.0043(16) C2C 0.044(2) 0.050(2) 0.056(2) 0.0021(18) -0.0165(18) -0.0016(16) C1C 0.080(3) 0.078(3) 0.063(2) -0.009(2) -0.002(2) 0.009(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S4 Ni1 S1 169.89(3) . . ? S4 Ni1 S3 94.08(3) . . ? S1 Ni1 S3 86.43(3) . . ? S4 Ni1 S2 86.96(3) . . ? S1 Ni1 S2 94.20(3) . . ? S3 Ni1 S2 170.52(3) . . ? C2 S1 Ni1 100.03(8) . . ? C7 S4 Ni1 99.95(8) . . ? C6 S3 Ni1 99.92(8) . . ? C3 S2 Ni1 99.60(8) . . ? C5 N2 C8 111.2(2) . . ? C2 C3 C4 108.8(2) . . ? C2 C3 S2 122.91(18) . . ? C4 C3 S2 128.28(19) . . ? C6 C7 C8 108.3(2) . . ? C6 C7 S4 123.51(18) . . ? C8 C7 S4 128.20(19) . . ? C7 C6 C5 108.6(2) . . ? C7 C6 S3 122.41(18) . . ? C5 C6 S3 128.96(19) . . ? C3 C2 C1 108.1(2) . . ? C3 C2 S1 123.25(17) . . ? C1 C2 S1 128.68(19) . . ? C4 N1 C1 111.0(2) . . ? O1 C1 N1 124.9(2) . . ? O1 C1 C2 129.2(2) . . ? N1 C1 C2 106.0(2) . . ? O3 C5 N2 124.1(2) . . ? O3 C5 C6 129.5(2) . . ? N2 C5 C6 106.4(2) . . ? O4 C8 N2 125.1(2) . . ? O4 C8 C7 129.4(2) . . ? N2 C8 C7 105.5(2) . . ? O2 C4 N1 124.6(2) . . ? O2 C4 C3 129.3(2) . . ? N1 C4 C3 106.1(2) . . ? C1A P1A C19A 111.12(12) . . ? C1A P1A C13A 111.22(12) . . ? C19A P1A C13A 106.15(11) . . ? C1A P1A C7A 106.12(12) . . ? C19A P1A C7A 109.92(12) . . ? C13A P1A C7A 112.38(12) . . ? C2A C1A C6A 119.1(3) . . ? C2A C1A P1A 119.3(2) . . ? C6A C1A P1A 121.1(2) . . ? C3A C2A C1A 119.9(3) . . ? C4A C3A C2A 120.7(3) . . ? C3A C4A C5A 119.9(3) . . ? C6A C5A C4A 120.6(3) . . ? C5A C6A C1A 119.8(3) . . ? C12A C7A C8A 119.0(2) . . ? C12A C7A P1A 122.1(2) . . ? C8A C7A P1A 118.3(2) . . ? C9A C8A C7A 120.9(3) . . ? C8A C9A C10A 119.6(3) . . ? C11A C10A C9A 120.2(3) . . ? C10A C11A C12A 120.6(3) . . ? C7A C12A C11A 119.7(3) . . ? C18A C13A C14A 119.5(2) . . ? C18A C13A P1A 120.4(2) . . ? C14A C13A P1A 119.24(19) . . ? C15A C14A C13A 120.0(3) . . ? C16A C15A C14A 120.2(3) . . ? C17A C16A C15A 120.1(3) . . ? C16A C17A C18A 120.4(3) . . ? C13A C18A C17A 119.8(3) . . ? C24A C19A C20A 119.9(2) . . ? C24A C19A P1A 118.98(19) . . ? C20A C19A P1A 120.14(19) . . ? C21A C20A C19A 119.7(3) . . ? C22A C21A C20A 120.0(3) . . ? C21A C22A C23A 120.5(2) . . ? C22A C23A C24A 119.9(3) . . ? C23A C24A C19A 120.0(2) . . ? C7B P1B C13B 109.13(11) . . ? C7B P1B C19B 110.39(12) . . ? C13B P1B C19B 110.03(12) . . ? C7B P1B C1B 109.28(12) . . ? C13B P1B C1B 108.18(12) . . ? C19B P1B C1B 109.78(12) . . ? C6B C1B C2B 119.9(3) . . ? C6B C1B P1B 119.9(2) . . ? C2B C1B P1B 120.1(2) . . ? C3B C2B C1B 119.6(3) . . ? C4B C3B C2B 120.1(3) . . ? C3B C4B C5B 121.0(3) . . ? C4B C5B C6B 119.7(3) . . ? C1B C6B C5B 119.8(3) . . ? C8B C7B C12B 119.7(2) . . ? C8B C7B P1B 120.59(19) . . ? C12B C7B P1B 119.58(19) . . ? C7B C8B C9B 119.8(2) . . ? C10B C9B C8B 120.7(3) . . ? C9B C10B C11B 119.8(2) . . ? C10B C11B C12B 120.4(2) . . ? C11B C12B C7B 119.6(2) . . ? C14B C13B C18B 119.3(2) . . ? C14B C13B P1B 121.5(2) . . ? C18B C13B P1B 119.16(19) . . ? C15B C14B C13B 119.8(3) . . ? C16B C15B C14B 120.6(3) . . ? C15B C16B C17B 120.1(3) . . ? C16B C17B C18B 119.9(3) . . ? C17B C18B C13B 120.2(2) . . ? C20B C19B C24B 119.2(3) . . ? C20B C19B P1B 120.5(2) . . ? C24B C19B P1B 120.3(2) . . ? C21B C20B C19B 120.3(3) . . ? C20B C21B C22B 120.1(3) . . ? C23B C22B C21B 120.3(3) . . ? C22B C23B C24B 120.4(3) . . ? C23B C24B C19B 119.8(3) . . ? N1C C2C C1C 179.3(4) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 S4 2.2032(7) . ? Ni1 S1 2.2068(7) . ? Ni1 S3 2.2107(7) . ? Ni1 S2 2.2165(8) . ? S1 C2 1.717(2) . ? S4 C7 1.718(2) . ? S3 C6 1.729(2) . ? S2 C3 1.728(2) . ? N2 C5 1.389(3) . ? N2 C8 1.389(3) . ? C3 C2 1.360(3) . ? C3 C4 1.478(3) . ? C7 C6 1.355(3) . ? C7 C8 1.492(3) . ? C6 C5 1.469(3) . ? C2 C1 1.488(3) . ? N1 C4 1.392(3) . ? N1 C1 1.395(3) . ? C1 O1 1.222(3) . ? C5 O3 1.224(3) . ? C8 O4 1.208(3) . ? C4 O2 1.216(3) . ? P1A C1A 1.795(3) . ? P1A C19A 1.796(3) . ? P1A C13A 1.801(3) . ? P1A C7A 1.801(3) . ? C1A C2A 1.394(4) . ? C1A C6A 1.395(4) . ? C2A C3A 1.378(4) . ? C3A C4A 1.364(5) . ? C4A C5A 1.381(5) . ? C5A C6A 1.375(4) . ? C7A C12A 1.382(4) . ? C7A C8A 1.396(4) . ? C8A C9A 1.378(4) . ? C9A C10A 1.378(4) . ? C10A C11A 1.373(4) . ? C11A C12A 1.392(4) . ? C13A C18A 1.386(4) . ? C13A C14A 1.393(3) . ? C14A C15A 1.383(4) . ? C15A C16A 1.380(4) . ? C16A C17A 1.372(4) . ? C17A C18A 1.390(4) . ? C19A C24A 1.385(3) . ? C19A C20A 1.397(3) . ? C20A C21A 1.385(4) . ? C21A C22A 1.378(4) . ? C22A C23A 1.384(4) . ? C23A C24A 1.384(3) . ? P1B C7B 1.796(3) . ? P1B C13B 1.801(3) . ? P1B C19B 1.803(3) . ? P1B C1B 1.804(3) . ? C1B C6B 1.380(4) . ? C1B C2B 1.390(4) . ? C2B C3B 1.388(4) . ? C3B C4B 1.366(5) . ? C4B C5B 1.368(4) . ? C5B C6B 1.398(4) . ? C7B C8B 1.386(3) . ? C7B C12B 1.401(3) . ? C8B C9B 1.388(4) . ? C9B C10B 1.377(4) . ? C10B C11B 1.384(4) . ? C11B C12B 1.388(4) . ? C13B C14B 1.386(4) . ? C13B C18B 1.388(3) . ? C14B C15B 1.380(4) . ? C15B C16B 1.372(4) . ? C16B C17B 1.373(4) . ? C17B C18B 1.385(4) . ? C19B C20B 1.391(3) . ? C19B C24B 1.402(3) . ? C20B C21B 1.380(4) . ? C21B C22B 1.385(4) . ? C22B C23B 1.374(4) . ? C23B C24B 1.382(4) . ? N1C C2C 1.132(4) . ? C2C C1C 1.453(5) . ?
1100742.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100742.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100742 loop_ _publ_author_name 'St\'ephane A. Baudron' 'Narcis Avarvari' 'Patrick Batail' _publ_contact_author ; Dr Patrick Batail Laboratoire Chimie Ing\'enierie Mol\'eculaires et Mat\'eriaux d'Angers, UMR 6200 CNRS-Universit\'e d'Angers, Bat. K, 2, Boulevard Lavoisier, Angers, France ; _publ_contact_author_email patrick.batail@univ-angers.fr _publ_contact_author_fax '33 2 41 73 50 11' _publ_contact_author_phone '33 2 41 73 52 64' _publ_section_title ; A Straightforward Synthesis of Diverse Nickel Dithiolene Complexes Appended with Hydrogen-Bond Donor/Acceptor Groups ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3380 _journal_page_last 3382 _journal_paper_doi 10.1021/ic050174n _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C40 H74 N4 Ni O4 S4' _chemical_formula_weight 861.98 _chemical_name_common (n-Bu4N)2(Ni(midt)2) _chemical_name_systematic ; ? ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.929(16) _cell_angle_beta 108.964(14) _cell_angle_gamma 113.839(14) _cell_formula_units_Z 2 _cell_length_a 13.0984(16) _cell_length_b 13.3622(19) _cell_length_c 15.772(2) _cell_measurement_reflns_used 8000 _cell_measurement_temperature 200(2) _cell_measurement_theta_max 52.1 _cell_measurement_theta_min 3.3 _cell_volume 2352.9(7) _computing_cell_refinement 'SELECT, CELL (STOE-IPDS)' _computing_data_collection 'EXPOSE, (STOE-IPDS)' _computing_data_reduction 'INTEGRATE (STOE-IPDS)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 200(2) _diffrn_detector_area_resol_mean 6.66 _diffrn_measured_fraction_theta_full 0.925 _diffrn_measured_fraction_theta_max 0.925 _diffrn_measurement_device_type STOE-IPDS _diffrn_measurement_method 'Oscillation, Phi. incr. = 1.5' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0457 _diffrn_reflns_av_sigmaI/netI 0.0718 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 23581 _diffrn_reflns_theta_full 25.95 _diffrn_reflns_theta_max 25.95 _diffrn_reflns_theta_min 1.82 _exptl_absorpt_coefficient_mu 0.630 _exptl_absorpt_correction_T_max 0.9544 _exptl_absorpt_correction_T_min 0.8627 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'FACEIT, STOE-IPDS' _exptl_crystal_colour black _exptl_crystal_density_diffrn 1.217 _exptl_crystal_density_meas ? _exptl_crystal_density_method . _exptl_crystal_description rod _exptl_crystal_F_000 932 _exptl_crystal_size_max 0.4620 _exptl_crystal_size_mid 0.1232 _exptl_crystal_size_min 0.0770 _refine_diff_density_max 0.726 _refine_diff_density_min -0.423 _refine_diff_density_rms 0.052 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.854 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 473 _refine_ls_number_reflns 8516 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.854 _refine_ls_R_factor_all 0.0678 _refine_ls_R_factor_gt 0.0354 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0375P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0734 _refine_ls_wR_factor_ref 0.0793 _reflns_number_gt 5413 _reflns_number_total 8516 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic050174nsi20050201_114507.cif _cod_data_source_block sb28p4 _cod_original_cell_volume 2352.9(5) _cod_database_code 1100742 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.01543(3) 0.11816(3) 0.27399(2) 0.01946(8) Uani 1 1 d . . . S1 S -0.15089(6) -0.03533(5) 0.24378(5) 0.02655(15) Uani 1 1 d . . . S2 S -0.06675(5) 0.22716(5) 0.29627(4) 0.02429(15) Uani 1 1 d . . . S3 S 0.09976(6) 0.01035(5) 0.25407(5) 0.02768(16) Uani 1 1 d . . . S4 S 0.17948(6) 0.27260(5) 0.30088(4) 0.02555(15) Uani 1 1 d . . . C1 C 0.4031(2) 0.2815(2) 0.30269(17) 0.0278(6) Uani 1 1 d . . . C2 C 0.2758(2) 0.21983(19) 0.29077(16) 0.0233(6) Uani 1 1 d . . . C3 C 0.2425(2) 0.1096(2) 0.27200(16) 0.0223(6) Uani 1 1 d . . . C4 C 0.3478(2) 0.0941(2) 0.27075(17) 0.0258(6) Uani 1 1 d . . . C5 C -0.3139(2) 0.1459(2) 0.28025(17) 0.0261(6) Uani 1 1 d . . . C6 C -0.2109(2) 0.12929(19) 0.27629(16) 0.0216(5) Uani 1 1 d . . . C7 C -0.2462(2) 0.01882(19) 0.25452(16) 0.0211(5) Uani 1 1 d . . . C8 C -0.3740(2) -0.0412(2) 0.24216(17) 0.0251(6) Uani 1 1 d . . . O1 O 0.46742(16) 0.38095(14) 0.32113(14) 0.0402(5) Uani 1 1 d . . . O2 O 0.35700(16) 0.00817(14) 0.25740(13) 0.0342(4) Uani 1 1 d . . . O3 O -0.32110(16) 0.23217(14) 0.29769(13) 0.0349(5) Uani 1 1 d . . . O4 O -0.44085(16) -0.14015(14) 0.22143(13) 0.0362(5) Uani 1 1 d . . . N1 N 0.4410(2) 0.20066(17) 0.28880(15) 0.0329(5) Uani 1 1 d . . . H1 H 0.5120 0.2146 0.2911 0.040 Uiso 1 1 calc R . . N2 N -0.40979(19) 0.04020(17) 0.25872(15) 0.0301(5) Uani 1 1 d . . . H2 H -0.4807 0.0272 0.2561 0.036 Uiso 1 1 calc R . . N1B N -0.17533(18) 0.20824(16) -0.00758(13) 0.0251(5) Uani 1 1 d . . . C1B C -0.2481(2) 0.1102(2) 0.02898(17) 0.0305(6) Uani 1 1 d . . . H1B1 H -0.1938 0.1000 0.0831 0.037 Uiso 1 1 calc R . . H1B2 H -0.3030 0.1289 0.0472 0.037 Uiso 1 1 calc R . . C2B C -0.3197(3) 0.0005(2) -0.03661(19) 0.0357(7) Uani 1 1 d . . . H2B1 H -0.2655 -0.0222 -0.0521 0.043 Uiso 1 1 calc R . . H2B2 H -0.3724 0.0099 -0.0922 0.043 Uiso 1 1 calc R . . C3B C -0.3939(3) -0.0893(2) 0.00537(19) 0.0404(7) Uani 1 1 d . . . H3B1 H -0.3405 -0.0997 0.0600 0.048 Uiso 1 1 calc R . . H3B2 H -0.4454 -0.0647 0.0230 0.048 Uiso 1 1 calc R . . C4B C -0.4704(3) -0.1997(2) -0.0590(2) 0.0568(9) Uani 1 1 d . . . H4B1 H -0.5154 -0.2530 -0.0296 0.085 Uiso 1 1 calc R . . H4B2 H -0.4197 -0.2255 -0.0755 0.085 Uiso 1 1 calc R . . H4B3 H -0.5244 -0.1902 -0.1128 0.085 Uiso 1 1 calc R . . C5B C -0.0841(2) 0.1864(2) -0.03508(17) 0.0304(6) Uani 1 1 d . . . H5B1 H -0.1269 0.1208 -0.0819 0.036 Uiso 1 1 calc R . . H5B2 H -0.0448 0.2483 -0.0621 0.036 Uiso 1 1 calc R . . C6B C 0.0108(3) 0.1699(3) 0.0394(2) 0.0467(8) Uani 1 1 d . . . H6B1 H -0.0268 0.1064 0.0657 0.056 Uiso 1 1 calc R . . H6B2 H 0.0546 0.2348 0.0870 0.056 Uiso 1 1 calc R . . C7B C 0.0980(3) 0.1511(3) 0.0034(2) 0.0487(8) Uani 1 1 d . . . H7B1 H 0.1538 0.1353 0.0525 0.058 Uiso 1 1 calc R . . H7B2 H 0.0530 0.0859 -0.0439 0.058 Uiso 1 1 calc R . . C8B C 0.1682(4) 0.2456(4) -0.0343(3) 0.0997(15) Uiso 1 1 d . . . H8B1 H 0.2201 0.2264 -0.0552 0.150 Uiso 1 1 calc R . . H8B2 H 0.2153 0.3104 0.0122 0.150 Uiso 1 1 calc R . . H8B3 H 0.1143 0.2609 -0.0843 0.150 Uiso 1 1 calc R . . C9B C -0.2588(2) 0.2278(2) -0.09151(16) 0.0275(6) Uani 1 1 d . . . H9B1 H -0.3301 0.2197 -0.0803 0.033 Uiso 1 1 calc R . . H9B2 H -0.2835 0.1704 -0.1421 0.033 Uiso 1 1 calc R . . C10B C -0.2057(2) 0.3411(2) -0.11971(18) 0.0329(6) Uani 1 1 d . . . H10A H -0.1891 0.3991 -0.0725 0.040 Uiso 1 1 calc R . . H10B H -0.1306 0.3530 -0.1261 0.040 Uiso 1 1 calc R . . C11B C -0.2909(3) 0.3483(2) -0.20902(19) 0.0393(7) Uani 1 1 d . . . H11A H -0.3705 0.3221 -0.2066 0.047 Uiso 1 1 calc R . . H11B H -0.2953 0.3003 -0.2582 0.047 Uiso 1 1 calc R . . C12B C -0.2505(3) 0.4668(2) -0.2285(2) 0.0427(7) Uani 1 1 d . . . H12A H -0.3066 0.4684 -0.2850 0.064 Uiso 1 1 calc R . . H12B H -0.1727 0.4923 -0.2326 0.064 Uiso 1 1 calc R . . H12C H -0.2469 0.5144 -0.1803 0.064 Uiso 1 1 calc R . . C13B C -0.1090(2) 0.3091(2) 0.06793(17) 0.0297(6) Uani 1 1 d . . . H13A H -0.0566 0.3701 0.0474 0.036 Uiso 1 1 calc R . . H13B H -0.0587 0.2920 0.1202 0.036 Uiso 1 1 calc R . . C14B C -0.1880(2) 0.3480(2) 0.09853(18) 0.0333(6) Uani 1 1 d . . . H14A H -0.2510 0.3494 0.0457 0.040 Uiso 1 1 calc R . . H14B H -0.2252 0.2966 0.1340 0.040 Uiso 1 1 calc R . . C15B C -0.1129(3) 0.4633(2) 0.1556(2) 0.0441(8) Uani 1 1 d . . . H15A H -0.0438 0.4635 0.2033 0.053 Uiso 1 1 calc R . . H15B H -0.0840 0.5157 0.1175 0.053 Uiso 1 1 calc R . . C16B C -0.1822(3) 0.5010(3) 0.1984(2) 0.0600(10) Uani 1 1 d . . . H16A H -0.1312 0.5741 0.2336 0.090 Uiso 1 1 calc R . . H16B H -0.2095 0.4504 0.2372 0.090 Uiso 1 1 calc R . . H16C H -0.2499 0.5025 0.1514 0.090 Uiso 1 1 calc R . . N1C N 0.26107(18) 0.32467(15) 0.60095(13) 0.0234(5) Uani 1 1 d . . . C1C C 0.3562(2) 0.3337(2) 0.56267(17) 0.0268(6) Uani 1 1 d . . . H1C1 H 0.4289 0.3994 0.5964 0.032 Uiso 1 1 calc R . . H1C2 H 0.3298 0.3446 0.5000 0.032 Uiso 1 1 calc R . . C2C C 0.3860(3) 0.2347(2) 0.5653(2) 0.0383(7) Uani 1 1 d . . . H2C1 H 0.4017 0.2164 0.6260 0.046 Uiso 1 1 calc R . . H2C2 H 0.3178 0.1710 0.5235 0.046 Uiso 1 1 calc R . . C3C C 0.4941(3) 0.2590(2) 0.5395(2) 0.0402(7) Uani 1 1 d . . . H3C1 H 0.5633 0.3187 0.5844 0.048 Uiso 1 1 calc R . . H3C2 H 0.4810 0.2844 0.4813 0.048 Uiso 1 1 calc R . . C4C C 0.5212(3) 0.1599(3) 0.5327(3) 0.0603(10) Uani 1 1 d . . . H4C1 H 0.5904 0.1807 0.5161 0.091 Uiso 1 1 calc R . . H4C2 H 0.4539 0.1009 0.4873 0.091 Uiso 1 1 calc R . . H4C3 H 0.5365 0.1353 0.5905 0.091 Uiso 1 1 calc R . . C5C C 0.1440(2) 0.22261(19) 0.54693(17) 0.0265(6) Uani 1 1 d . . . H5C1 H 0.1306 0.2219 0.4827 0.032 Uiso 1 1 calc R . . H5C2 H 0.1544 0.1565 0.5625 0.032 Uiso 1 1 calc R . . C6C C 0.0330(2) 0.2152(2) 0.56166(18) 0.0305(6) Uani 1 1 d . . . H6C1 H 0.0135 0.2741 0.5373 0.037 Uiso 1 1 calc R . . H6C2 H 0.0481 0.2251 0.6264 0.037 Uiso 1 1 calc R . . C7C C -0.0729(2) 0.1025(2) 0.51491(18) 0.0300(6) Uani 1 1 d . . . H7C1 H -0.0776 0.0865 0.4532 0.036 Uiso 1 1 calc R . . H7C2 H -0.0594 0.0451 0.5471 0.036 Uiso 1 1 calc R . . C8C C -0.1903(3) 0.0995(2) 0.5124(2) 0.0448(8) Uani 1 1 d . . . H8C1 H -0.2539 0.0276 0.4829 0.067 Uiso 1 1 calc R . . H8C2 H -0.2051 0.1550 0.4793 0.067 Uiso 1 1 calc R . . H8C3 H -0.1865 0.1142 0.5734 0.067 Uiso 1 1 calc R . . C9C C 0.2448(2) 0.43154(19) 0.59409(16) 0.0252(6) Uani 1 1 d . . . H9C1 H 0.1889 0.4285 0.6231 0.030 Uiso 1 1 calc R . . H9C2 H 0.3211 0.4933 0.6286 0.030 Uiso 1 1 calc R . . C10C C 0.2001(2) 0.4563(2) 0.49875(17) 0.0312(6) Uani 1 1 d . . . H10C H 0.2597 0.4693 0.4712 0.037 Uiso 1 1 calc R . . H10D H 0.1271 0.3930 0.4614 0.037 Uiso 1 1 calc R . . C11C C 0.1762(3) 0.5580(2) 0.50309(19) 0.0414(7) Uani 1 1 d . . . H11C H 0.1198 0.5458 0.5337 0.050 Uiso 1 1 calc R . . H11D H 0.2502 0.6214 0.5387 0.050 Uiso 1 1 calc R . . C12C C 0.1260(3) 0.5838(3) 0.4094(2) 0.0530(9) Uani 1 1 d . . . H12D H 0.1124 0.6485 0.4154 0.080 Uiso 1 1 calc R . . H12E H 0.0518 0.5219 0.3743 0.080 Uiso 1 1 calc R . . H12F H 0.1822 0.5974 0.3793 0.080 Uiso 1 1 calc R . . C13C C 0.2973(2) 0.31129(19) 0.70061(16) 0.0252(6) Uani 1 1 d . . . H13C H 0.2359 0.3107 0.7224 0.030 Uiso 1 1 calc R . . H13D H 0.2986 0.2394 0.7042 0.030 Uiso 1 1 calc R . . C14C C 0.4171(2) 0.3988(2) 0.76442(17) 0.0332(6) Uani 1 1 d . . . H14C H 0.4804 0.3976 0.7459 0.040 Uiso 1 1 calc R . . H14D H 0.4183 0.4716 0.7609 0.040 Uiso 1 1 calc R . . C15C C 0.4396(2) 0.3781(2) 0.86138(17) 0.0320(6) Uani 1 1 d . . . H15C H 0.4344 0.3038 0.8639 0.038 Uiso 1 1 calc R . . H15D H 0.3777 0.3820 0.8803 0.038 Uiso 1 1 calc R . . C16C C 0.5613(3) 0.4613(3) 0.9272(2) 0.0482(8) Uani 1 1 d . . . H16D H 0.5713 0.4451 0.9876 0.072 Uiso 1 1 calc R . . H16E H 0.5664 0.5349 0.9257 0.072 Uiso 1 1 calc R . . H16F H 0.6231 0.4564 0.9097 0.072 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.01503(17) 0.01878(15) 0.02329(17) 0.00406(12) 0.00671(13) 0.00625(12) S1 0.0179(4) 0.0196(3) 0.0421(4) 0.0041(3) 0.0121(3) 0.0071(3) S2 0.0167(3) 0.0205(3) 0.0329(4) 0.0024(3) 0.0074(3) 0.0067(3) S3 0.0182(4) 0.0202(3) 0.0430(4) 0.0018(3) 0.0124(3) 0.0058(3) S4 0.0197(4) 0.0192(3) 0.0366(4) 0.0036(3) 0.0113(3) 0.0064(3) C1 0.0211(15) 0.0280(14) 0.0319(15) 0.0059(12) 0.0105(12) 0.0077(12) C2 0.0152(14) 0.0258(13) 0.0264(14) 0.0053(11) 0.0098(11) 0.0046(11) C3 0.0186(14) 0.0255(13) 0.0225(14) 0.0029(10) 0.0094(11) 0.0079(11) C4 0.0189(15) 0.0290(14) 0.0270(15) 0.0014(11) 0.0098(11) 0.0068(12) C5 0.0176(15) 0.0295(14) 0.0275(15) 0.0030(11) 0.0060(11) 0.0085(12) C6 0.0172(14) 0.0260(13) 0.0202(13) 0.0046(10) 0.0051(11) 0.0092(11) C7 0.0158(14) 0.0250(13) 0.0229(14) 0.0059(10) 0.0075(11) 0.0087(11) C8 0.0206(15) 0.0275(14) 0.0256(14) 0.0062(11) 0.0070(11) 0.0099(12) O1 0.0246(11) 0.0262(10) 0.0636(14) 0.0065(9) 0.0173(10) 0.0043(9) O2 0.0249(11) 0.0288(10) 0.0505(12) -0.0020(9) 0.0170(9) 0.0110(9) O3 0.0250(11) 0.0274(10) 0.0524(13) -0.0004(9) 0.0135(9) 0.0122(8) O4 0.0228(11) 0.0247(10) 0.0554(13) 0.0049(9) 0.0147(9) 0.0045(8) N1 0.0177(13) 0.0312(12) 0.0507(15) 0.0039(11) 0.0168(11) 0.0081(10) N2 0.0138(12) 0.0301(12) 0.0458(14) 0.0027(10) 0.0111(10) 0.0086(10) N1B 0.0229(12) 0.0275(11) 0.0223(11) 0.0044(9) 0.0063(9) 0.0098(9) C1B 0.0302(17) 0.0328(14) 0.0282(15) 0.0114(11) 0.0125(12) 0.0114(12) C2B 0.0339(17) 0.0338(15) 0.0348(16) 0.0092(12) 0.0117(13) 0.0108(13) C3B 0.0376(19) 0.0358(15) 0.0415(18) 0.0159(13) 0.0124(14) 0.0110(13) C4B 0.045(2) 0.0436(18) 0.054(2) 0.0167(16) 0.0050(16) 0.0027(15) C5B 0.0267(16) 0.0315(14) 0.0316(15) 0.0014(11) 0.0109(12) 0.0113(12) C6B 0.052(2) 0.061(2) 0.0405(18) 0.0082(15) 0.0124(15) 0.0402(18) C7B 0.046(2) 0.0542(19) 0.055(2) 0.0056(16) 0.0143(16) 0.0332(17) C9B 0.0245(15) 0.0285(13) 0.0246(14) 0.0064(11) 0.0054(11) 0.0093(11) C10B 0.0281(16) 0.0303(14) 0.0349(16) 0.0085(12) 0.0095(12) 0.0088(12) C11B 0.0364(18) 0.0357(15) 0.0383(17) 0.0140(13) 0.0084(14) 0.0121(13) C12B 0.0403(19) 0.0365(15) 0.0488(19) 0.0173(14) 0.0152(15) 0.0145(14) C13B 0.0265(16) 0.0288(13) 0.0270(14) 0.0007(11) 0.0053(12) 0.0091(12) C14B 0.0309(17) 0.0392(15) 0.0321(15) 0.0061(12) 0.0117(12) 0.0172(13) C15B 0.045(2) 0.0428(17) 0.0442(18) -0.0038(14) 0.0146(15) 0.0198(15) C16B 0.064(3) 0.061(2) 0.062(2) -0.0079(18) 0.0243(19) 0.034(2) N1C 0.0216(12) 0.0194(10) 0.0250(11) 0.0015(8) 0.0075(9) 0.0058(9) C1C 0.0244(15) 0.0294(13) 0.0258(14) 0.0065(11) 0.0110(11) 0.0092(11) C2C 0.0381(18) 0.0382(16) 0.0488(18) 0.0100(14) 0.0222(15) 0.0210(14) C3C 0.0361(19) 0.0505(18) 0.0382(17) 0.0071(14) 0.0146(14) 0.0220(15) C4C 0.053(2) 0.064(2) 0.083(3) 0.0056(19) 0.035(2) 0.0347(19) C5C 0.0252(15) 0.0199(12) 0.0277(14) -0.0021(10) 0.0068(11) 0.0057(11) C6C 0.0234(15) 0.0295(13) 0.0339(15) -0.0020(11) 0.0088(12) 0.0085(12) C7C 0.0268(16) 0.0226(13) 0.0324(15) 0.0031(11) 0.0073(12) 0.0055(11) C8C 0.0271(18) 0.0410(17) 0.056(2) 0.0056(15) 0.0108(15) 0.0081(14) C9C 0.0258(15) 0.0184(12) 0.0278(14) 0.0000(10) 0.0070(11) 0.0083(11) C10C 0.0368(17) 0.0253(13) 0.0280(15) 0.0014(11) 0.0094(12) 0.0119(12) C11C 0.056(2) 0.0409(16) 0.0348(17) 0.0060(13) 0.0131(14) 0.0302(15) C12C 0.077(3) 0.0533(19) 0.048(2) 0.0162(16) 0.0215(18) 0.047(2) C13C 0.0281(15) 0.0229(12) 0.0244(14) 0.0053(10) 0.0099(11) 0.0104(11) C14C 0.0245(16) 0.0364(15) 0.0318(15) 0.0085(12) 0.0074(12) 0.0089(12) C15C 0.0375(17) 0.0320(14) 0.0258(15) 0.0018(11) 0.0089(12) 0.0165(13) C16C 0.0389(19) 0.065(2) 0.0328(17) -0.0003(15) 0.0046(14) 0.0213(16) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S4 Ni1 S1 178.55(3) . . ? S4 Ni1 S3 93.71(3) . . ? S1 Ni1 S3 86.80(3) . . ? S4 Ni1 S2 85.81(3) . . ? S1 Ni1 S2 93.70(3) . . ? S3 Ni1 S2 179.05(3) . . ? C7 S1 Ni1 100.53(8) . . ? C6 S2 Ni1 100.24(8) . . ? C3 S3 Ni1 100.05(8) . . ? C2 S4 Ni1 100.57(8) . . ? O1 C1 N1 124.2(3) . . ? O1 C1 C2 130.2(2) . . ? N1 C1 C2 105.6(2) . . ? C3 C2 C1 109.4(2) . . ? C3 C2 S4 122.62(19) . . ? C1 C2 S4 127.97(18) . . ? C2 C3 C4 108.1(2) . . ? C2 C3 S3 123.04(19) . . ? C4 C3 S3 128.89(18) . . ? O2 C4 N1 124.4(2) . . ? O2 C4 C3 129.4(2) . . ? N1 C4 C3 106.1(2) . . ? O3 C5 N2 123.8(2) . . ? O3 C5 C6 129.8(2) . . ? N2 C5 C6 106.4(2) . . ? C7 C6 C5 108.3(2) . . ? C7 C6 S2 122.82(19) . . ? C5 C6 S2 128.89(18) . . ? C6 C7 C8 108.9(2) . . ? C6 C7 S1 122.71(19) . . ? C8 C7 S1 128.34(18) . . ? O4 C8 N2 123.6(2) . . ? O4 C8 C7 130.5(2) . . ? N2 C8 C7 105.9(2) . . ? C4 N1 C1 110.8(2) . . ? C8 N2 C5 110.5(2) . . ? C5B N1B C9B 107.82(19) . . ? C5B N1B C13B 108.77(18) . . ? C9B N1B C13B 111.48(18) . . ? C5B N1B C1B 111.50(19) . . ? C9B N1B C1B 109.53(19) . . ? C13B N1B C1B 107.77(19) . . ? C2B C1B N1B 115.6(2) . . ? C1B C2B C3B 110.9(2) . . ? C4B C3B C2B 112.8(3) . . ? C6B C5B N1B 116.4(2) . . ? C5B C6B C7B 111.2(2) . . ? C8B C7B C6B 115.4(3) . . ? N1B C9B C10B 115.2(2) . . ? C11B C10B C9B 111.3(2) . . ? C10B C11B C12B 111.7(2) . . ? N1B C13B C14B 115.5(2) . . ? C15B C14B C13B 109.8(2) . . ? C16B C15B C14B 112.5(3) . . ? C1C N1C C13C 111.85(18) . . ? C1C N1C C9C 108.09(18) . . ? C13C N1C C9C 108.23(17) . . ? C1C N1C C5C 109.23(18) . . ? C13C N1C C5C 108.07(18) . . ? C9C N1C C5C 111.40(18) . . ? N1C C1C C2C 115.6(2) . . ? C3C C2C C1C 111.4(2) . . ? C2C C3C C4C 113.6(3) . . ? C6C C5C N1C 116.10(19) . . ? C5C C6C C7C 110.6(2) . . ? C8C C7C C6C 112.2(2) . . ? C10C C9C N1C 116.50(19) . . ? C11C C10C C9C 109.9(2) . . ? C12C C11C C10C 112.3(2) . . ? C14C C13C N1C 116.3(2) . . ? C15C C14C C13C 110.8(2) . . ? C14C C15C C16C 112.5(2) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 S4 2.2024(9) . ? Ni1 S1 2.2049(9) . ? Ni1 S3 2.2116(8) . ? Ni1 S2 2.2135(7) . ? S1 C7 1.725(2) . ? S2 C6 1.726(3) . ? S3 C3 1.724(3) . ? S4 C2 1.720(2) . ? C1 O1 1.218(3) . ? C1 N1 1.399(3) . ? C1 C2 1.476(4) . ? C2 C3 1.353(3) . ? C3 C4 1.481(3) . ? C4 O2 1.225(3) . ? C4 N1 1.398(3) . ? C5 O3 1.228(3) . ? C5 N2 1.400(3) . ? C5 C6 1.473(3) . ? C6 C7 1.356(3) . ? C7 C8 1.477(3) . ? C8 O4 1.219(3) . ? C8 N2 1.397(3) . ? N1B C5B 1.522(3) . ? N1B C9B 1.523(3) . ? N1B C13B 1.523(3) . ? N1B C1B 1.527(3) . ? C1B C2B 1.519(3) . ? C2B C3B 1.524(4) . ? C3B C4B 1.519(4) . ? C5B C6B 1.501(4) . ? C6B C7B 1.529(4) . ? C7B C8B 1.496(5) . ? C9B C10B 1.532(3) . ? C10B C11B 1.520(4) . ? C11B C12B 1.526(4) . ? C13B C14B 1.524(3) . ? C14B C15B 1.519(4) . ? C15B C16B 1.513(4) . ? N1C C1C 1.517(3) . ? N1C C13C 1.523(3) . ? N1C C9C 1.527(3) . ? N1C C5C 1.536(3) . ? C1C C2C 1.521(3) . ? C2C C3C 1.511(4) . ? C3C C4C 1.513(4) . ? C5C C6C 1.511(4) . ? C6C C7C 1.532(3) . ? C7C C8C 1.509(4) . ? C9C C10C 1.521(3) . ? C10C C11C 1.519(3) . ? C11C C12C 1.517(4) . ? C13C C14C 1.515(3) . ? C14C C15C 1.513(4) . ? C15C C16C 1.520(4) . ?
1100743.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100743.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100743 loop_ _publ_author_name 'St\'ephane A. Baudron' 'Narcis Avarvari' 'Patrick Batail' _publ_contact_author ; Dr Patrick Batail Laboratoire Chimie Ing\'enierie Mol\'eculaires et Mat\'eriaux d'Angers, UMR 6200 CNRS-Universit\'e d'Angers, Bat. K, 2, Boulevard Lavoisier, Angers, France ; _publ_contact_author_email patrick.batail@univ-angers.fr _publ_contact_author_fax '33 2 41 73 50 11' _publ_contact_author_phone '33 2 41 73 52 64' _publ_section_title ; A Straightforward Synthesis of Diverse Nickel Dithiolene Complexes Appended with Hydrogen-Bond Donor/Acceptor Groups ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3380 _journal_page_last 3382 _journal_paper_doi 10.1021/ic050174n _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C32 H24 N4 Ni O5 P S4' _chemical_formula_weight 762.47 _chemical_name_common (PPh4)[Ni(madt)2](H2O) _chemical_name_systematic ; ? ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 114.341(15) _cell_angle_beta 94.651(16) _cell_angle_gamma 101.106(17) _cell_formula_units_Z 2 _cell_length_a 10.3180(14) _cell_length_b 13.0706(19) _cell_length_c 15.399(2) _cell_measurement_reflns_used 8000 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 23.6 _cell_measurement_theta_min 2.1 _cell_volume 1826.6(5) _computing_cell_refinement 'SELECT, CELL [STOE-IPDS]' _computing_data_collection 'EXPOSE [STOE-IPDS]' _computing_data_reduction 'INTEGRATE [STOE-IPDS]' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 6.66 _diffrn_measured_fraction_theta_full 0.929 _diffrn_measured_fraction_theta_max 0.929 _diffrn_measurement_device_type STOE-IPDS _diffrn_measurement_method 'Rotation, Phi. incr. = 1.5' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0613 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 6595 _diffrn_reflns_theta_full 25.89 _diffrn_reflns_theta_max 25.89 _diffrn_reflns_theta_min 2.04 _exptl_absorpt_coefficient_mu 0.847 _exptl_absorpt_correction_T_max 0.8960 _exptl_absorpt_correction_T_min 0.7774 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'FACEIT, STOE-IPDS' _exptl_crystal_colour black _exptl_crystal_density_diffrn 1.386 _exptl_crystal_density_meas ? _exptl_crystal_density_method . _exptl_crystal_description prism _exptl_crystal_F_000 782 _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _refine_diff_density_max 1.507 _refine_diff_density_min -0.558 _refine_diff_density_rms 0.124 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 416 _refine_ls_number_reflns 6595 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.993 _refine_ls_R_factor_all 0.0803 _refine_ls_R_factor_gt 0.0549 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1276P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1789 _refine_ls_wR_factor_ref 0.1938 _reflns_number_gt 4416 _reflns_number_total 6595 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic050174nsi20050201_114526.cif _cod_data_source_block sb658e _cod_original_cell_volume 1826.5(4) _cod_database_code 1100743 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.24112(6) 0.00835(4) 0.01236(4) 0.0327(2) Uani 1 1 d . . . S3 S 0.22068(13) -0.12485(9) 0.06109(9) 0.0420(3) Uani 1 1 d . . . S1 S 0.41266(14) 0.10623(10) 0.12638(9) 0.0429(3) Uani 1 1 d . . . S2 S 0.25988(12) 0.14376(9) -0.03411(9) 0.0367(3) Uani 1 1 d . . . S4 S 0.07840(13) -0.09553(9) -0.10753(9) 0.0370(3) Uani 1 1 d . . . C5 C 0.0527(5) -0.3463(4) -0.0117(4) 0.0367(11) Uani 1 1 d . . . C4 C 0.4451(5) 0.3562(3) 0.0292(3) 0.0300(10) Uani 1 1 d . . . C6 C 0.0923(5) -0.2376(4) -0.0243(3) 0.0333(10) Uani 1 1 d . . . C3 C 0.4010(4) 0.2481(3) 0.0428(3) 0.0282(9) Uani 1 1 d . . . C1 C 0.5833(5) 0.3206(4) 0.1887(4) 0.0375(11) Uani 1 1 d . . . C7 C 0.0315(5) -0.2243(3) -0.0991(3) 0.0318(10) Uani 1 1 d . . . C2 C 0.4680(4) 0.2313(3) 0.1132(3) 0.0298(10) Uani 1 1 d . . . C8 C -0.0625(5) -0.3233(4) -0.1856(4) 0.0434(12) Uani 1 1 d . . . C24A C 0.8528(8) -0.0175(6) 0.6714(5) 0.0709(19) Uani 1 1 d . . . H24A H 0.9165 0.0459 0.7188 0.085 Uiso 1 1 calc R . . O2 O 0.5659(3) 0.4008(3) 0.0385(3) 0.0425(8) Uani 1 1 d . . . N2 N 0.3488(4) 0.3991(3) 0.0061(3) 0.0401(10) Uani 1 1 d . . . H2A H 0.3690 0.4604 -0.0031 0.048 Uiso 1 1 calc R . . H2B H 0.2660 0.3657 0.0003 0.048 Uiso 1 1 calc R . . N1 N 0.7021(4) 0.2982(4) 0.1804(4) 0.0544(12) Uani 1 1 d . . . H1A H 0.7719 0.3457 0.2220 0.065 Uiso 1 1 calc R . . H1B H 0.7098 0.2360 0.1333 0.065 Uiso 1 1 calc R . . N4 N -0.1842(5) -0.3128(4) -0.2042(4) 0.0559(12) Uani 1 1 d . . . H4A H -0.2394 -0.3654 -0.2547 0.067 Uiso 1 1 calc R . . H4B H -0.2088 -0.2534 -0.1658 0.067 Uiso 1 1 calc R . . O1 O 0.5648(5) 0.4074(3) 0.2538(3) 0.0713(13) Uani 1 1 d . . . O4 O -0.0207(5) -0.4058(4) -0.2372(4) 0.0856(16) Uani 1 1 d . . . O3 O -0.0666(3) -0.3999(3) -0.0317(3) 0.0526(10) Uani 1 1 d . . . N3 N 0.1499(4) -0.3791(3) 0.0229(4) 0.0503(12) Uani 1 1 d . . . H3A H 0.1315 -0.4402 0.0325 0.060 Uiso 1 1 calc R . . H3B H 0.2316 -0.3393 0.0359 0.060 Uiso 1 1 calc R . . P1 P 0.79199(14) 0.13460(11) 0.60204(9) 0.0390(3) Uani 1 1 d . . . C1A C 0.7558(5) 0.1174(5) 0.4801(4) 0.0426(12) Uani 1 1 d . . . C13A C 0.6792(6) 0.2038(4) 0.6744(4) 0.0453(12) Uani 1 1 d . . . C19A C 0.7758(5) -0.0057(4) 0.5979(4) 0.0441(12) Uani 1 1 d . . . C7A C 0.9568(6) 0.2271(5) 0.6576(4) 0.0493(13) Uani 1 1 d . . . C16A C 0.5180(9) 0.3184(8) 0.7920(5) 0.087(2) Uani 1 1 d . . . H16A H 0.4612 0.3568 0.8301 0.105 Uiso 1 1 calc R . . C11A C 1.1682(8) 0.3386(7) 0.6530(6) 0.090(2) Uani 1 1 d . . . H11A H 1.2279 0.3596 0.6176 0.108 Uiso 1 1 calc R . . C23A C 0.8323(10) -0.1245(7) 0.6721(6) 0.094(3) Uani 1 1 d . . . H23A H 0.8839 -0.1330 0.7199 0.112 Uiso 1 1 calc R . . C2A C 0.6713(7) 0.1761(6) 0.4555(4) 0.0598(16) Uani 1 1 d . . . H2A H 0.6307 0.2244 0.5021 0.072 Uiso 1 1 calc R . . C21A C 0.6628(7) -0.2078(6) 0.5309(6) 0.080(2) Uani 1 1 d . . . H21A H 0.5997 -0.2718 0.4836 0.096 Uiso 1 1 calc R . . C14A C 0.5889(6) 0.1440(5) 0.7108(4) 0.0593(15) Uani 1 1 d . . . H14A H 0.5825 0.0664 0.6956 0.071 Uiso 1 1 calc R . . C10A C 1.2000(8) 0.3868(6) 0.7524(6) 0.079(2) Uani 1 1 d . . . H10A H 1.2820 0.4399 0.7846 0.095 Uiso 1 1 calc R . . C4A C 0.7057(7) 0.0915(7) 0.2918(5) 0.0719(19) Uani 1 1 d . . . H4A H 0.6913 0.0860 0.2295 0.086 Uiso 1 1 calc R . . C6A C 0.8111(7) 0.0419(6) 0.4080(4) 0.0652(17) Uani 1 1 d . . . H6A H 0.8657 0.0007 0.4234 0.078 Uiso 1 1 calc R . . C15A C 0.5086(7) 0.2056(7) 0.7709(5) 0.082(2) Uani 1 1 d . . . H15A H 0.4480 0.1686 0.7967 0.098 Uiso 1 1 calc R . . C8A C 0.9915(9) 0.2786(7) 0.7572(5) 0.095(3) Uani 1 1 d . . . H8A H 0.9327 0.2602 0.7943 0.114 Uiso 1 1 calc R . . C20A C 0.6823(7) -0.1007(5) 0.5285(5) 0.0625(16) Uani 1 1 d . . . H20A H 0.6318 -0.0934 0.4795 0.075 Uiso 1 1 calc R . . C3A C 0.6489(7) 0.1619(6) 0.3619(5) 0.0707(19) Uani 1 1 d . . . H3A H 0.5930 0.2017 0.3457 0.085 Uiso 1 1 calc R . . C9A C 1.1138(9) 0.3572(7) 0.8015(6) 0.100(3) Uani 1 1 d . . . H9A H 1.1362 0.3908 0.8687 0.120 Uiso 1 1 calc R . . C22A C 0.7373(8) -0.2186(7) 0.6037(7) 0.083(2) Uani 1 1 d . . . H22A H 0.7232 -0.2896 0.6065 0.100 Uiso 1 1 calc R . . C12A C 1.0462(7) 0.2582(6) 0.6060(5) 0.074(2) Uani 1 1 d . . . H12A H 1.0247 0.2250 0.5387 0.088 Uiso 1 1 calc R . . C5A C 0.7848(7) 0.0282(7) 0.3133(4) 0.0720(19) Uani 1 1 d . . . H5A H 0.8202 -0.0232 0.2649 0.086 Uiso 1 1 calc R . . C18A C 0.6870(9) 0.3201(6) 0.6996(5) 0.083(2) Uani 1 1 d . . . H18A H 0.7474 0.3591 0.6751 0.100 Uiso 1 1 calc R . . C17A C 0.6106(8) 0.3776(6) 0.7579(5) 0.103(3) Uani 1 1 d . . . H17A H 0.6193 0.4561 0.7754 0.123 Uiso 1 1 calc R . . O5 O 0.4026(8) 0.4958(6) 0.3838(5) 0.249(5) Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni 0.0356(4) 0.0218(3) 0.0399(3) 0.0192(2) -0.0034(3) -0.0037(2) S3 0.0480(8) 0.0279(6) 0.0485(7) 0.0252(5) -0.0090(6) -0.0062(5) S1 0.0443(8) 0.0328(6) 0.0518(7) 0.0293(6) -0.0123(6) -0.0062(5) S2 0.0389(7) 0.0266(5) 0.0423(6) 0.0217(5) -0.0080(5) -0.0061(5) S4 0.0385(7) 0.0284(6) 0.0433(7) 0.0221(5) -0.0048(5) -0.0032(5) C5 0.035(3) 0.026(2) 0.054(3) 0.023(2) 0.009(2) 0.0051(19) C4 0.033(3) 0.0215(19) 0.036(2) 0.0150(17) 0.005(2) 0.0019(17) C6 0.030(3) 0.023(2) 0.049(3) 0.021(2) 0.007(2) 0.0007(17) C3 0.028(3) 0.022(2) 0.035(2) 0.0156(18) 0.0042(19) 0.0014(16) C1 0.036(3) 0.031(2) 0.041(3) 0.017(2) 0.000(2) -0.0002(19) C7 0.027(3) 0.025(2) 0.041(2) 0.0154(19) 0.004(2) 0.0011(17) C2 0.029(3) 0.024(2) 0.038(2) 0.0173(18) 0.006(2) 0.0020(17) C8 0.040(3) 0.030(2) 0.051(3) 0.017(2) -0.001(3) -0.003(2) C24A 0.088(6) 0.070(4) 0.062(4) 0.039(3) -0.003(4) 0.018(4) O2 0.030(2) 0.0344(17) 0.070(2) 0.0345(17) 0.0046(17) -0.0021(14) N2 0.027(2) 0.033(2) 0.072(3) 0.036(2) 0.006(2) 0.0027(16) N1 0.033(3) 0.047(3) 0.070(3) 0.018(2) -0.005(2) 0.003(2) N4 0.039(3) 0.052(3) 0.065(3) 0.024(2) -0.011(2) -0.002(2) O1 0.069(3) 0.049(2) 0.060(3) -0.006(2) 0.010(2) 0.005(2) O4 0.079(4) 0.050(2) 0.083(3) -0.010(2) -0.010(3) 0.017(2) O3 0.031(2) 0.0397(19) 0.102(3) 0.048(2) 0.011(2) 0.0035(15) N3 0.034(3) 0.038(2) 0.092(4) 0.045(2) 0.004(2) 0.0010(18) P1 0.0375(8) 0.0459(7) 0.0323(6) 0.0160(5) 0.0041(6) 0.0110(5) C1A 0.041(3) 0.054(3) 0.034(3) 0.021(2) 0.005(2) 0.012(2) C13A 0.050(3) 0.050(3) 0.038(3) 0.017(2) 0.009(2) 0.020(2) C19A 0.043(3) 0.048(3) 0.047(3) 0.024(2) 0.011(3) 0.016(2) C7A 0.048(4) 0.051(3) 0.041(3) 0.015(2) 0.003(3) 0.008(2) C16A 0.092(6) 0.102(6) 0.062(4) 0.012(4) 0.020(4) 0.062(5) C11A 0.065(5) 0.086(5) 0.095(6) 0.032(5) 0.007(4) -0.012(4) C23A 0.121(8) 0.098(6) 0.087(6) 0.064(5) 0.003(5) 0.034(6) C2A 0.066(4) 0.077(4) 0.047(3) 0.031(3) 0.014(3) 0.033(3) C21A 0.062(5) 0.053(4) 0.111(6) 0.027(4) 0.000(4) 0.010(3) C14A 0.049(4) 0.062(4) 0.054(3) 0.014(3) 0.015(3) 0.009(3) C10A 0.060(5) 0.059(4) 0.091(6) 0.021(4) -0.010(4) -0.009(3) C4A 0.066(5) 0.116(6) 0.046(3) 0.046(4) 0.007(3) 0.025(4) C6A 0.059(4) 0.098(5) 0.042(3) 0.025(3) 0.007(3) 0.039(4) C15A 0.052(4) 0.104(6) 0.067(4) 0.020(4) 0.024(4) 0.005(4) C8A 0.084(6) 0.120(7) 0.048(4) 0.027(4) -0.006(4) -0.021(5) C20A 0.059(4) 0.052(3) 0.070(4) 0.026(3) -0.007(3) 0.009(3) C3A 0.071(5) 0.094(5) 0.065(4) 0.049(4) 0.006(4) 0.030(4) C9A 0.091(7) 0.105(6) 0.061(5) 0.020(4) -0.027(4) -0.019(5) C22A 0.078(6) 0.081(5) 0.117(7) 0.065(5) 0.023(5) 0.029(4) C12A 0.065(5) 0.081(5) 0.054(4) 0.019(3) 0.013(3) -0.003(3) C5A 0.070(5) 0.109(5) 0.037(3) 0.026(3) 0.016(3) 0.034(4) C18A 0.138(7) 0.065(4) 0.075(5) 0.040(4) 0.061(5) 0.053(5) C17A 0.175(10) 0.092(6) 0.080(5) 0.046(5) 0.067(6) 0.084(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S3 Ni S2 178.87(6) . . ? S3 Ni S4 91.49(5) . . ? S2 Ni S4 88.83(5) . . ? S3 Ni S1 88.15(5) . . ? S2 Ni S1 91.60(5) . . ? S4 Ni S1 176.15(6) . . ? C6 S3 Ni 104.36(15) . . ? C2 S1 Ni 104.37(16) . . ? C3 S2 Ni 104.07(14) . . ? C7 S4 Ni 104.46(17) . . ? O3 C5 N3 123.0(4) . . ? O3 C5 C6 120.1(4) . . ? N3 C5 C6 116.8(4) . . ? O2 C4 N2 122.7(4) . . ? O2 C4 C3 120.8(4) . . ? N2 C4 C3 116.5(4) . . ? C7 C6 C5 122.5(4) . . ? C7 C6 S3 119.4(3) . . ? C5 C6 S3 118.1(4) . . ? C2 C3 C4 121.7(4) . . ? C2 C3 S2 120.0(3) . . ? C4 C3 S2 118.3(3) . . ? O1 C1 N1 123.6(5) . . ? O1 C1 C2 120.7(5) . . ? N1 C1 C2 115.7(4) . . ? C6 C7 C8 123.0(4) . . ? C6 C7 S4 120.2(3) . . ? C8 C7 S4 116.1(3) . . ? C3 C2 C1 123.9(4) . . ? C3 C2 S1 120.0(3) . . ? C1 C2 S1 115.9(3) . . ? O4 C8 N4 123.4(5) . . ? O4 C8 C7 119.5(5) . . ? N4 C8 C7 117.0(5) . . ? C23A C24A C19A 119.0(7) . . ? C19A P1 C13A 109.1(2) . . ? C19A P1 C7A 112.4(3) . . ? C13A P1 C7A 106.4(3) . . ? C19A P1 C1A 108.2(3) . . ? C13A P1 C1A 111.7(2) . . ? C7A P1 C1A 109.1(3) . . ? C2A C1A C6A 119.3(5) . . ? C2A C1A P1 121.2(4) . . ? C6A C1A P1 119.5(4) . . ? C18A C13A C14A 119.7(5) . . ? C18A C13A P1 119.6(5) . . ? C14A C13A P1 120.6(4) . . ? C20A C19A C24A 119.5(5) . . ? C20A C19A P1 121.1(4) . . ? C24A C19A P1 119.2(4) . . ? C12A C7A C8A 118.1(6) . . ? C12A C7A P1 122.7(5) . . ? C8A C7A P1 118.9(5) . . ? C15A C16A C17A 121.2(7) . . ? C10A C11A C12A 119.4(7) . . ? C22A C23A C24A 121.4(7) . . ? C3A C2A C1A 119.0(6) . . ? C22A C21A C20A 119.7(7) . . ? C13A C14A C15A 117.4(6) . . ? C9A C10A C11A 119.5(7) . . ? C3A C4A C5A 119.9(6) . . ? C5A C6A C1A 120.2(6) . . ? C16A C15A C14A 120.8(7) . . ? C9A C8A C7A 119.6(7) . . ? C19A C20A C21A 120.6(6) . . ? C4A C3A C2A 122.2(6) . . ? C10A C9A C8A 122.5(8) . . ? C23A C22A C21A 119.9(7) . . ? C7A C12A C11A 120.8(7) . . ? C4A C5A C6A 119.4(6) . . ? C17A C18A C13A 122.0(7) . . ? C18A C17A C16A 118.8(7) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni S3 2.1446(12) . ? Ni S2 2.1487(12) . ? Ni S4 2.1503(14) . ? Ni S1 2.1504(15) . ? S3 C6 1.739(5) . ? S1 C2 1.723(4) . ? S2 C3 1.734(4) . ? S4 C7 1.720(4) . ? C5 O3 1.236(6) . ? C5 N3 1.319(6) . ? C5 C6 1.497(6) . ? C4 O2 1.239(5) . ? C4 N2 1.323(6) . ? C4 C3 1.502(5) . ? C6 C7 1.357(7) . ? C3 C2 1.355(6) . ? C1 O1 1.227(6) . ? C1 N1 1.318(6) . ? C1 C2 1.501(6) . ? C7 C8 1.509(7) . ? C8 O4 1.227(6) . ? C8 N4 1.311(7) . ? C24A C23A 1.378(9) . ? C24A C19A 1.408(8) . ? P1 C19A 1.782(5) . ? P1 C13A 1.789(5) . ? P1 C7A 1.790(6) . ? P1 C1A 1.795(5) . ? C1A C2A 1.391(8) . ? C1A C6A 1.395(8) . ? C13A C18A 1.389(8) . ? C13A C14A 1.399(8) . ? C19A C20A 1.376(8) . ? C7A C12A 1.374(8) . ? C7A C8A 1.379(9) . ? C16A C15A 1.354(11) . ? C16A C17A 1.385(11) . ? C11A C10A 1.375(11) . ? C11A C12A 1.389(10) . ? C23A C22A 1.373(11) . ? C2A C3A 1.370(8) . ? C21A C22A 1.379(10) . ? C21A C20A 1.391(9) . ? C14A C15A 1.400(9) . ? C10A C9A 1.316(11) . ? C4A C3A 1.359(9) . ? C4A C5A 1.379(9) . ? C6A C5A 1.391(8) . ? C8A C9A 1.377(10) . ? C18A C17A 1.334(9) . ?
1100744.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100744.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100744 loop_ _publ_author_name 'St\'ephane A. Baudron' 'Narcis Avarvari' 'Patrick Batail' _publ_contact_author ; Dr Patrick Batail Laboratoire Chimie Ing\'enierie Mol\'eculaires et Mat\'eriaux d'Angers, UMR 6200 CNRS-Universit\'e d'Angers, Bat. K, 2, Boulevard Lavoisier, Angers, France ; _publ_contact_author_email patrick.batail@univ-angers.fr _publ_contact_author_fax '33 2 41 73 50 11' _publ_contact_author_phone '33 2 41 73 52 64' _publ_section_title ; A Straightforward Synthesis of Diverse Nickel Dithiolene Complexes Appended with Hydrogen-Bond Donor/Acceptor Groups ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3380 _journal_page_last 3382 _journal_paper_doi 10.1021/ic050174n _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C40 H76 N6 Ni O2 S4' _chemical_formula_weight 860.02 _chemical_name_common (n-Bu4N)[Ni(mant)2] _chemical_name_systematic ; ? ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 70.09(3) _cell_angle_beta 77.79(2) _cell_angle_gamma 76.68(3) _cell_formula_units_Z 1 _cell_length_a 9.1252(17) _cell_length_b 11.804(3) _cell_length_c 12.478(3) _cell_measurement_reflns_used 3495 _cell_measurement_temperature 200(2) _cell_measurement_theta_max 23.6 _cell_measurement_theta_min 2.1 _cell_volume 1216.7(5) _computing_cell_refinement 'SELECT, CELL [STOE-IPDS]' _computing_data_collection 'EXPOSE [STOE-IPDS]' _computing_data_reduction 'INTEGRATE [STOE-IPDS]' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 200(2) _diffrn_detector_area_resol_mean 6.66 _diffrn_measured_fraction_theta_full 0.907 _diffrn_measured_fraction_theta_max 0.907 _diffrn_measurement_device_type STOE-IPDS _diffrn_measurement_method 'Oscillation, Phi. incr. = 1.9' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1174 _diffrn_reflns_av_sigmaI/netI 0.2538 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 12471 _diffrn_reflns_theta_full 26.23 _diffrn_reflns_theta_max 26.23 _diffrn_reflns_theta_min 1.86 _exptl_absorpt_coefficient_mu 0.607 _exptl_absorpt_correction_T_max 0.9860 _exptl_absorpt_correction_T_min 0.9061 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'FACEIT, STOE-IPDS' _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.174 _exptl_crystal_density_meas ? _exptl_crystal_density_method . _exptl_crystal_description platelet _exptl_crystal_F_000 466 _exptl_crystal_size_max 0.2694 _exptl_crystal_size_mid 0.1156 _exptl_crystal_size_min 0.0230 _refine_diff_density_max 0.285 _refine_diff_density_min -0.240 _refine_diff_density_rms 0.048 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.592 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 241 _refine_ls_number_reflns 4462 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.592 _refine_ls_R_factor_all 0.1528 _refine_ls_R_factor_gt 0.0414 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0625 _refine_ls_wR_factor_ref 0.0874 _reflns_number_gt 1579 _reflns_number_total 4462 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic050174nsi20050201_114543.cif _cod_data_source_block sb687e _cod_original_cell_volume 1216.6(4) _cod_database_code 1100744 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.0000 0.0000 0.0000 0.0402(3) Uani 1 2 d S . . S1 S 0.05150(13) -0.09573(10) 0.17306(11) 0.0479(4) Uani 1 1 d . . . S2 S 0.16269(14) -0.13469(10) -0.06560(11) 0.0476(4) Uani 1 1 d . . . C1 C 0.2218(5) -0.3105(4) 0.2675(5) 0.0499(14) Uani 1 1 d . . . C2 C 0.1793(5) -0.2270(4) 0.1604(4) 0.0423(13) Uani 1 1 d . . . C3 C 0.2308(5) -0.2429(4) 0.0535(4) 0.0408(12) Uani 1 1 d . . . C4 C 0.3448(5) -0.3529(4) 0.0397(4) 0.0408(12) Uani 1 1 d . . . O1 O 0.4011(3) -0.4343(3) 0.1195(3) 0.0548(10) Uani 1 1 d . . . N1 N 0.2470(5) -0.3697(4) 0.3581(4) 0.0698(14) Uani 1 1 d . . . N2 N 0.3883(5) -0.3558(3) -0.0701(4) 0.0638(13) Uani 1 1 d . . . H2A H 0.4559 -0.4149 -0.0846 0.077 Uiso 1 1 calc R . . H2B H 0.3485 -0.2986 -0.1254 0.077 Uiso 1 1 calc R . . N1B N 0.7164(4) -0.3439(3) 0.2453(3) 0.0369(9) Uani 1 1 d . . . C1B C 0.8283(5) -0.3383(4) 0.1345(3) 0.0427(12) Uani 1 1 d . . . H1B1 H 0.8673 -0.2622 0.1096 0.051 Uiso 1 1 calc R . . H1B2 H 0.9136 -0.4047 0.1515 0.051 Uiso 1 1 calc R . . C2B C 0.7628(5) -0.3466(4) 0.0350(4) 0.0513(13) Uani 1 1 d . . . H2B1 H 0.6716 -0.2855 0.0215 0.062 Uiso 1 1 calc R . . H2B2 H 0.7351 -0.4266 0.0549 0.062 Uiso 1 1 calc R . . C3B C 0.8796(5) -0.3258(4) -0.0745(4) 0.0583(14) Uani 1 1 d . . . H3B1 H 0.9039 -0.2445 -0.0956 0.070 Uiso 1 1 calc R . . H3B2 H 0.9724 -0.3844 -0.0593 0.070 Uiso 1 1 calc R . . C4B C 0.8215(5) -0.3388(5) -0.1742(4) 0.0656(15) Uani 1 1 d . . . H4B1 H 0.8976 -0.3244 -0.2412 0.098 Uiso 1 1 calc R . . H4B2 H 0.7303 -0.2802 -0.1901 0.098 Uiso 1 1 calc R . . H4B3 H 0.8000 -0.4199 -0.1545 0.098 Uiso 1 1 calc R . . C5B C 0.6524(5) -0.4624(4) 0.2900(3) 0.0431(11) Uani 1 1 d . . . H5B1 H 0.5834 -0.4624 0.3608 0.052 Uiso 1 1 calc R . . H5B2 H 0.5926 -0.4624 0.2343 0.052 Uiso 1 1 calc R . . C6B C 0.7670(5) -0.5809(4) 0.3138(4) 0.0529(13) Uani 1 1 d . . . H6B1 H 0.8272 -0.5890 0.2419 0.063 Uiso 1 1 calc R . . H6B2 H 0.8353 -0.5793 0.3629 0.063 Uiso 1 1 calc R . . C7B C 0.6849(6) -0.6895(4) 0.3723(4) 0.0668(15) Uani 1 1 d . . . H7B1 H 0.6084 -0.6845 0.3268 0.080 Uiso 1 1 calc R . . H7B2 H 0.6327 -0.6841 0.4471 0.080 Uiso 1 1 calc R . . C8B C 0.7889(7) -0.8133(5) 0.3887(5) 0.101(2) Uani 1 1 d . . . H8B1 H 0.7297 -0.8772 0.4263 0.151 Uiso 1 1 calc R . . H8B2 H 0.8639 -0.8200 0.4351 0.151 Uiso 1 1 calc R . . H8B3 H 0.8387 -0.8208 0.3149 0.151 Uiso 1 1 calc R . . C9B C 0.8043(5) -0.3328(4) 0.3307(3) 0.0434(12) Uani 1 1 d . . . H9B1 H 0.8408 -0.2554 0.2989 0.052 Uiso 1 1 calc R . . H9B2 H 0.8927 -0.3974 0.3389 0.052 Uiso 1 1 calc R . . C10B C 0.7154(6) -0.3397(4) 0.4499(4) 0.0599(14) Uani 1 1 d . . . H10A H 0.6918 -0.4214 0.4877 0.072 Uiso 1 1 calc R . . H10B H 0.6201 -0.2826 0.4424 0.072 Uiso 1 1 calc R . . C11B C 0.8060(7) -0.3096(5) 0.5239(4) 0.0725(16) Uani 1 1 d . . . H11A H 0.7635 -0.3400 0.6044 0.087 Uiso 1 1 calc R . . H11B H 0.9105 -0.3512 0.5145 0.087 Uiso 1 1 calc R . . C12B C 0.8043(8) -0.1741(5) 0.4926(5) 0.106(2) Uani 1 1 d . . . H12A H 0.8636 -0.1598 0.5402 0.159 Uiso 1 1 calc R . . H12B H 0.7013 -0.1327 0.5045 0.159 Uiso 1 1 calc R . . H12C H 0.8468 -0.1436 0.4132 0.159 Uiso 1 1 calc R . . C13B C 0.5808(5) -0.2416(4) 0.2237(4) 0.0457(12) Uani 1 1 d . . . H13A H 0.5136 -0.2476 0.2962 0.055 Uiso 1 1 calc R . . H13B H 0.5256 -0.2553 0.1720 0.055 Uiso 1 1 calc R . . C14B C 0.6136(5) -0.1117(4) 0.1731(4) 0.0580(14) Uani 1 1 d . . . H14A H 0.6744 -0.0977 0.2210 0.070 Uiso 1 1 calc R . . H14B H 0.6719 -0.1013 0.0968 0.070 Uiso 1 1 calc R . . C15B C 0.4672(5) -0.0185(4) 0.1654(4) 0.0639(16) Uani 1 1 d . . . H15A H 0.4011 -0.0397 0.1263 0.077 Uiso 1 1 calc R . . H15B H 0.4911 0.0614 0.1193 0.077 Uiso 1 1 calc R . . C16B C 0.3822(7) -0.0111(5) 0.2822(5) 0.104(2) Uani 1 1 d . . . H16A H 0.2909 0.0488 0.2717 0.156 Uiso 1 1 calc R . . H16B H 0.4457 0.0120 0.3207 0.156 Uiso 1 1 calc R . . H16C H 0.3561 -0.0894 0.3279 0.156 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0343(6) 0.0301(5) 0.0527(6) -0.0113(5) -0.0054(5) -0.0018(5) S1 0.0412(8) 0.0412(7) 0.0568(9) -0.0166(7) -0.0072(7) 0.0040(6) S2 0.0442(8) 0.0375(7) 0.0563(9) -0.0144(6) -0.0096(6) 0.0041(6) C1 0.038(3) 0.040(3) 0.062(4) -0.008(3) -0.006(3) -0.001(2) C2 0.030(3) 0.035(3) 0.056(3) -0.001(2) -0.019(2) -0.002(2) C3 0.031(3) 0.027(2) 0.067(3) -0.017(2) -0.013(2) -0.001(2) C4 0.034(3) 0.037(3) 0.055(3) -0.016(3) -0.015(3) -0.004(2) O1 0.050(2) 0.0421(19) 0.073(2) -0.0214(18) -0.0266(18) 0.0142(17) N1 0.068(3) 0.062(3) 0.067(3) -0.010(3) -0.011(3) 0.001(3) N2 0.065(3) 0.054(3) 0.070(3) -0.031(2) -0.013(2) 0.018(2) N1B 0.028(2) 0.048(2) 0.034(2) -0.0107(18) -0.0029(17) -0.0075(18) C1B 0.043(3) 0.046(3) 0.037(3) -0.010(2) -0.001(2) -0.012(2) C2B 0.048(3) 0.071(3) 0.039(3) -0.020(3) -0.004(3) -0.016(3) C3B 0.058(3) 0.084(4) 0.038(3) -0.022(3) 0.000(3) -0.026(3) C4B 0.065(4) 0.089(4) 0.049(3) -0.028(3) -0.001(3) -0.021(3) C5B 0.041(3) 0.049(3) 0.036(3) -0.009(2) 0.002(2) -0.015(2) C6B 0.054(3) 0.051(3) 0.047(3) -0.012(2) 0.006(2) -0.013(3) C7B 0.082(4) 0.050(3) 0.057(3) -0.008(3) 0.007(3) -0.017(3) C8B 0.131(6) 0.056(4) 0.097(5) -0.021(3) 0.014(4) -0.013(4) C9B 0.042(3) 0.048(3) 0.040(3) -0.009(2) -0.015(2) -0.006(2) C10B 0.077(4) 0.067(3) 0.034(3) -0.006(3) -0.012(3) -0.021(3) C11B 0.092(4) 0.092(4) 0.043(3) -0.023(3) -0.018(3) -0.024(3) C12B 0.171(7) 0.099(5) 0.069(4) -0.041(4) 0.001(4) -0.059(5) C13B 0.039(3) 0.053(3) 0.042(3) -0.014(2) -0.011(2) 0.000(2) C14B 0.063(4) 0.048(3) 0.058(3) -0.005(3) -0.015(3) -0.010(3) C15B 0.059(3) 0.051(3) 0.071(4) -0.011(3) -0.015(3) 0.005(3) C16B 0.120(6) 0.087(5) 0.094(5) -0.043(4) -0.005(4) 0.017(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 Ni1 S1 180.00(6) . 2 ? S1 Ni1 S2 88.90(5) . 2 ? S1 Ni1 S2 91.10(5) 2 2 ? S1 Ni1 S2 91.10(5) . . ? S1 Ni1 S2 88.90(5) 2 . ? S2 Ni1 S2 180.00(9) 2 . ? C2 S1 Ni1 104.18(17) . . ? C3 S2 Ni1 105.32(15) . . ? N1 C1 C2 173.5(5) . . ? C3 C2 C1 125.7(4) . . ? C3 C2 S1 120.0(3) . . ? C1 C2 S1 114.3(3) . . ? C2 C3 C4 121.1(4) . . ? C2 C3 S2 119.2(3) . . ? C4 C3 S2 119.7(3) . . ? O1 C4 N2 120.5(4) . . ? O1 C4 C3 124.4(4) . . ? N2 C4 C3 115.0(4) . . ? C13B N1B C9B 111.3(3) . . ? C13B N1B C5B 106.0(3) . . ? C9B N1B C5B 111.7(3) . . ? C13B N1B C1B 110.7(3) . . ? C9B N1B C1B 106.1(3) . . ? C5B N1B C1B 111.1(3) . . ? C2B C1B N1B 115.2(4) . . ? C1B C2B C3B 110.4(4) . . ? C4B C3B C2B 112.1(4) . . ? C6B C5B N1B 116.8(3) . . ? C7B C6B C5B 110.2(4) . . ? C6B C7B C8B 114.1(4) . . ? N1B C9B C10B 115.4(4) . . ? C9B C10B C11B 111.3(4) . . ? C12B C11B C10B 112.5(4) . . ? N1B C13B C14B 117.0(4) . . ? C15B C14B C13B 111.2(4) . . ? C14B C15B C16B 113.4(4) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 S1 2.1640(14) . ? Ni1 S1 2.1640(14) 2 ? Ni1 S2 2.1648(12) 2 ? Ni1 S2 2.1648(12) . ? S1 C2 1.744(4) . ? S2 C3 1.720(5) . ? C1 N1 1.148(5) . ? C1 C2 1.433(6) . ? C2 C3 1.379(6) . ? C3 C4 1.500(5) . ? C4 O1 1.231(4) . ? C4 N2 1.353(5) . ? N1B C13B 1.514(4) . ? N1B C9B 1.518(5) . ? N1B C5B 1.522(5) . ? N1B C1B 1.527(5) . ? C1B C2B 1.526(5) . ? C2B C3B 1.529(6) . ? C3B C4B 1.516(6) . ? C5B C6B 1.521(5) . ? C6B C7B 1.520(6) . ? C7B C8B 1.522(6) . ? C9B C10B 1.521(6) . ? C10B C11B 1.532(6) . ? C11B C12B 1.508(6) . ? C13B C14B 1.521(6) . ? C14B C15B 1.520(6) . ? C15B C16B 1.520(6) . ?
1100745.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100745.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100745 loop_ _publ_author_name 'St\'ephane A. Baudron' 'Narcis Avarvari' 'Patrick Batail' _publ_contact_author ; Dr Patrick Batail Laboratoire Chimie Ing\'enierie Mol\'eculaires et Mat\'eriaux d'Angers, UMR 6200 CNRS-Universit\'e d'Angers, Bat. K, 2, Boulevard Lavoisier, Angers, France ; _publ_contact_author_email patrick.batail@univ-angers.fr _publ_contact_author_fax '33 2 41 73 50 11' _publ_contact_author_phone '33 2 41 73 52 64' _publ_section_title ; A Straightforward Synthesis of Diverse Nickel Dithiolene Complexes Appended with Hydrogen-Bond Donor/Acceptor Groups ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3380 _journal_page_last 3382 _journal_paper_doi 10.1021/ic050174n _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C32 H24 N4 Ni O2 P S4' _chemical_formula_weight 714.47 _chemical_name_common (n-Bu4N)2[Ni(mant)2] _chemical_name_systematic ; ? ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 72.019(16) _cell_angle_beta 70.639(17) _cell_angle_gamma 77.020(17) _cell_formula_units_Z 2 _cell_length_a 10.1114(16) _cell_length_b 13.1679(17) _cell_length_c 14.002(2) _cell_measurement_reflns_used 4419 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 25.1 _cell_measurement_theta_min 1.95 _cell_volume 1657.4(5) _computing_cell_refinement 'SELECT, CELL [STOE-IPDS]' _computing_data_collection 'EXPOSE [STOE-IPDS]' _computing_data_reduction 'INTEGRATE [STOE-IPDS]' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 6.66 _diffrn_measured_fraction_theta_full 0.915 _diffrn_measured_fraction_theta_max 0.915 _diffrn_measurement_device_type STOE-IPDS _diffrn_measurement_method 'Oscillation, Phi. incr. = 1.7' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1411 _diffrn_reflns_av_sigmaI/netI 0.2303 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 16291 _diffrn_reflns_theta_full 25.92 _diffrn_reflns_theta_max 25.92 _diffrn_reflns_theta_min 1.98 _exptl_absorpt_coefficient_mu 0.921 _exptl_absorpt_correction_type none _exptl_crystal_colour black _exptl_crystal_density_diffrn 1.432 _exptl_crystal_density_meas ? _exptl_crystal_density_method . _exptl_crystal_description prism _exptl_crystal_F_000 734 _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.451 _refine_diff_density_min -0.294 _refine_diff_density_rms 0.077 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.728 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 400 _refine_ls_number_reflns 5918 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.728 _refine_ls_R_factor_all 0.1752 _refine_ls_R_factor_gt 0.0515 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0311P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0911 _refine_ls_wR_factor_ref 0.1162 _reflns_number_gt 2096 _reflns_number_total 5918 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic050174nsi20050201_114605.cif _cod_data_source_block sb7 _cod_original_cell_volume 1657.3(4) _cod_database_code 1100745 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.0000 0.0000 0.0000 0.0320(4) Uani 1 2 d S . . S1 S 0.1868(2) -0.01059(14) -0.12753(17) 0.0447(6) Uani 1 1 d . . . S2 S 0.01160(19) -0.17213(14) 0.05456(17) 0.0397(6) Uani 1 1 d . . . C1 C 0.2396(7) -0.1471(6) -0.1101(6) 0.035(2) Uani 1 1 d . . . C2 C 0.1623(7) -0.2187(5) -0.0304(6) 0.0296(19) Uani 1 1 d . . . C3 C 0.3649(9) -0.1788(6) -0.1866(7) 0.051(2) Uani 1 1 d . . . C4 C 0.2020(7) -0.3376(6) -0.0153(6) 0.0275(19) Uani 1 1 d . . . N1 N 0.4649(9) -0.1991(7) -0.2460(7) 0.112(4) Uani 1 1 d . . . O2 O 0.3270(5) -0.3792(4) -0.0277(5) 0.0519(17) Uani 1 1 d . . . N2 N 0.0983(6) -0.3942(4) 0.0105(5) 0.0359(17) Uani 1 1 d . . . H2A H 0.1160 -0.4629 0.0194 0.043 Uiso 1 1 calc R . . H2B H 0.0126 -0.3625 0.0184 0.043 Uiso 1 1 calc R . . Ni2 Ni 0.5000 0.0000 0.0000 0.0345(4) Uani 1 2 d S . . S3 S 0.4968(2) 0.17082(15) -0.03842(17) 0.0427(6) Uani 1 1 d . . . S4 S 0.2932(2) 0.00845(14) 0.10952(18) 0.0445(6) Uani 1 1 d . . . C5 C 0.3336(7) 0.2169(6) 0.0351(6) 0.031(2) Uani 1 1 d . . . C6 C 0.2426(7) 0.1454(6) 0.1022(6) 0.0315(19) Uani 1 1 d . . . C7 C 0.2947(9) 0.3369(6) 0.0229(6) 0.0310(19) Uani 1 1 d . . . C8 C 0.1065(9) 0.1743(6) 0.1695(7) 0.049(2) Uani 1 1 d . . . O3 O 0.1704(5) 0.3774(4) 0.0325(5) 0.0502(17) Uani 1 1 d . . . N3 N 0.3987(6) 0.3912(5) -0.0007(5) 0.0446(19) Uani 1 1 d . . . H3A H 0.3827 0.4601 -0.0108 0.053 Uiso 1 1 calc R . . H3B H 0.4836 0.3583 -0.0064 0.053 Uiso 1 1 calc R . . N4 N -0.0014(8) 0.1878(6) 0.2217(6) 0.075(2) Uani 1 1 d . . . P1 P 0.22166(19) 0.67447(16) -0.53070(16) 0.0451(5) Uani 1 1 d . . . C9 C 0.3612(7) 0.7506(6) -0.5626(7) 0.0458(19) Uani 1 1 d . . . C10 C 0.4130(9) 0.7632(7) -0.4868(7) 0.066(3) Uani 1 1 d . . . H10 H 0.3834 0.7236 -0.4177 0.079 Uiso 1 1 calc R . . C11 C 0.5084(10) 0.8348(9) -0.5151(8) 0.082(3) Uani 1 1 d . . . H11 H 0.5409 0.8436 -0.4636 0.099 Uiso 1 1 calc R . . C12 C 0.5565(9) 0.8927(8) -0.6150(9) 0.068(3) Uani 1 1 d . . . H12 H 0.6210 0.9403 -0.6320 0.082 Uiso 1 1 calc R . . C13 C 0.5085(8) 0.8799(7) -0.6904(8) 0.070(3) Uani 1 1 d . . . H13 H 0.5413 0.9190 -0.7594 0.084 Uiso 1 1 calc R . . C14 C 0.4121(8) 0.8099(7) -0.6658(7) 0.061(2) Uani 1 1 d . . . H14 H 0.3809 0.8020 -0.7183 0.074 Uiso 1 1 calc R . . C15 C 0.2202(7) 0.5683(5) -0.4118(6) 0.0423(18) Uani 1 1 d . . . C16 C 0.2480(7) 0.4597(6) -0.4139(7) 0.054(2) Uani 1 1 d . . . H16 H 0.2659 0.4423 -0.4769 0.065 Uiso 1 1 calc R . . C17 C 0.2493(9) 0.3804(7) -0.3267(8) 0.065(3) Uani 1 1 d . . . H17 H 0.2662 0.3089 -0.3299 0.078 Uiso 1 1 calc R . . C18 C 0.2259(9) 0.4037(7) -0.2323(7) 0.070(3) Uani 1 1 d . . . H18 H 0.2298 0.3485 -0.1725 0.084 Uiso 1 1 calc R . . C19 C 0.1966(9) 0.5095(7) -0.2281(7) 0.063(3) Uani 1 1 d . . . H19 H 0.1813 0.5261 -0.1650 0.076 Uiso 1 1 calc R . . C20 C 0.1899(8) 0.5906(6) -0.3157(7) 0.058(2) Uani 1 1 d . . . H20 H 0.1649 0.6616 -0.3108 0.070 Uiso 1 1 calc R . . C21 C 0.2486(8) 0.6131(7) -0.6335(7) 0.050(2) Uani 1 1 d . . . C22 C 0.3802(9) 0.5553(7) -0.6713(7) 0.070(3) Uani 1 1 d . . . H22 H 0.4580 0.5577 -0.6510 0.084 Uiso 1 1 calc R . . C23 C 0.3925(11) 0.4947(8) -0.7390(7) 0.087(3) Uani 1 1 d . . . H23 H 0.4797 0.4561 -0.7643 0.104 Uiso 1 1 calc R . . C24 C 0.2814(15) 0.4900(10) -0.7698(8) 0.102(4) Uani 1 1 d . . . H24 H 0.2917 0.4481 -0.8151 0.122 Uiso 1 1 calc R . . C25 C 0.1522(13) 0.5483(10) -0.7329(8) 0.100(4) Uani 1 1 d . . . H25 H 0.0750 0.5452 -0.7536 0.119 Uiso 1 1 calc R . . C26 C 0.1360(10) 0.6109(7) -0.6660(7) 0.073(3) Uani 1 1 d . . . H26 H 0.0493 0.6514 -0.6432 0.088 Uiso 1 1 calc R . . C27 C 0.0598(8) 0.7632(7) -0.5130(7) 0.058(2) Uani 1 1 d . . . C28 C 0.0490(10) 0.8626(8) -0.5818(12) 0.128(6) Uani 1 1 d . . . H28 H 0.1262 0.8825 -0.6388 0.154 Uiso 1 1 calc R . . C29 C -0.0736(13) 0.9330(8) -0.5679(12) 0.137(6) Uani 1 1 d . . . H29 H -0.0809 0.9991 -0.6166 0.165 Uiso 1 1 calc R . . C30 C -0.1877(11) 0.9050(11) -0.4803(14) 0.123(5) Uani 1 1 d . . . H30 H -0.2685 0.9550 -0.4682 0.148 Uiso 1 1 calc R . . C31 C -0.1827(11) 0.8079(12) -0.4139(11) 0.131(5) Uani 1 1 d . . . H31 H -0.2607 0.7877 -0.3578 0.157 Uiso 1 1 calc R . . C32 C -0.0581(9) 0.7381(9) -0.4309(9) 0.098(4) Uani 1 1 d . . . H32 H -0.0538 0.6704 -0.3843 0.118 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0312(8) 0.0148(8) 0.0384(10) -0.0064(7) 0.0039(7) -0.0016(6) S1 0.0423(12) 0.0209(10) 0.0473(15) -0.0042(10) 0.0135(11) -0.0044(9) S2 0.0358(11) 0.0161(10) 0.0487(15) -0.0073(10) 0.0091(10) -0.0008(9) C1 0.024(4) 0.022(4) 0.041(5) -0.003(4) 0.006(4) 0.003(3) C2 0.032(4) 0.017(4) 0.040(6) -0.009(4) -0.010(4) -0.001(4) C3 0.047(5) 0.023(4) 0.063(7) -0.003(4) -0.001(5) 0.004(4) C4 0.017(4) 0.025(4) 0.040(5) -0.010(4) -0.007(4) 0.000(4) N1 0.096(6) 0.075(6) 0.092(7) -0.013(5) 0.035(6) 0.030(5) O2 0.028(3) 0.022(3) 0.101(5) -0.015(3) -0.016(3) 0.001(2) N2 0.025(3) 0.013(3) 0.066(5) -0.013(3) -0.009(3) 0.004(3) Ni2 0.0413(9) 0.0158(8) 0.0428(10) -0.0121(7) -0.0100(8) 0.0071(7) S3 0.0396(11) 0.0231(11) 0.0553(16) -0.0137(11) -0.0021(11) 0.0035(9) S4 0.0477(12) 0.0182(10) 0.0556(16) -0.0098(10) -0.0043(11) 0.0038(9) C5 0.033(5) 0.021(4) 0.040(6) -0.013(4) -0.013(4) 0.007(4) C6 0.031(4) 0.024(4) 0.037(5) -0.010(4) -0.011(4) 0.006(4) C7 0.042(5) 0.019(4) 0.031(5) -0.008(4) -0.008(4) -0.004(4) C8 0.040(5) 0.037(5) 0.058(6) -0.013(5) -0.007(5) 0.007(4) O3 0.034(3) 0.022(3) 0.093(5) -0.014(3) -0.023(3) 0.005(3) N3 0.032(4) 0.020(4) 0.084(6) -0.023(4) -0.016(4) 0.004(3) N4 0.056(5) 0.075(5) 0.071(6) -0.012(5) 0.007(5) -0.010(4) P1 0.0347(10) 0.0554(11) 0.0432(14) -0.0097(11) -0.0075(10) -0.0115(9) C9 0.037(4) 0.056(4) 0.046(6) -0.003(4) -0.016(4) -0.016(4) C10 0.072(6) 0.081(6) 0.047(7) -0.009(5) -0.002(5) -0.052(5) C11 0.105(8) 0.116(9) 0.045(7) -0.014(7) -0.018(6) -0.066(7) C12 0.060(6) 0.081(7) 0.074(8) -0.009(6) -0.024(6) -0.038(5) C13 0.053(5) 0.085(6) 0.065(7) 0.014(5) -0.017(5) -0.042(5) C14 0.051(5) 0.083(6) 0.048(6) -0.004(5) -0.013(5) -0.025(5) C15 0.039(4) 0.047(4) 0.037(5) -0.005(4) -0.008(4) -0.012(3) C16 0.052(5) 0.056(5) 0.053(6) -0.019(5) -0.009(4) -0.004(4) C17 0.075(6) 0.041(5) 0.058(7) -0.001(5) -0.001(6) -0.008(5) C18 0.075(6) 0.068(6) 0.049(7) -0.002(5) -0.013(5) -0.002(5) C19 0.086(7) 0.072(6) 0.031(6) -0.015(5) -0.007(5) -0.021(6) C20 0.062(5) 0.055(5) 0.050(6) -0.024(5) 0.005(5) -0.011(4) C21 0.041(4) 0.076(6) 0.041(6) -0.007(5) -0.011(4) -0.032(4) C22 0.055(5) 0.101(7) 0.054(6) -0.027(6) 0.001(5) -0.025(5) C23 0.102(8) 0.123(8) 0.042(6) -0.043(6) 0.008(6) -0.040(7) C24 0.136(10) 0.156(12) 0.045(8) -0.050(8) 0.001(8) -0.086(10) C25 0.107(9) 0.155(11) 0.056(8) -0.026(8) -0.011(7) -0.073(8) C26 0.076(6) 0.095(7) 0.051(7) -0.011(6) -0.010(5) -0.041(5) C27 0.046(5) 0.058(5) 0.071(7) -0.018(5) -0.013(5) -0.016(4) C28 0.044(6) 0.065(7) 0.242(17) -0.001(9) -0.041(9) 0.005(6) C29 0.085(8) 0.064(6) 0.229(18) 0.032(8) -0.060(11) -0.018(7) C30 0.044(6) 0.104(9) 0.233(18) -0.078(11) -0.042(9) 0.024(7) C31 0.047(7) 0.167(13) 0.158(13) -0.028(11) -0.035(8) 0.017(8) C32 0.043(6) 0.134(9) 0.102(10) -0.028(8) -0.019(6) 0.010(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 Ni1 S1 180.00(15) 2 . ? S1 Ni1 S2 87.92(7) 2 . ? S1 Ni1 S2 92.08(7) . . ? S1 Ni1 S2 92.08(7) 2 2 ? S1 Ni1 S2 87.92(7) . 2 ? S2 Ni1 S2 180.0 . 2 ? C1 S1 Ni1 103.5(3) . . ? C2 S2 Ni1 104.1(3) . . ? C2 C1 C3 123.3(7) . . ? C2 C1 S1 120.8(5) . . ? C3 C1 S1 115.9(6) . . ? C1 C2 C4 122.2(6) . . ? C1 C2 S2 119.5(5) . . ? C4 C2 S2 118.3(6) . . ? N1 C3 C1 176.4(10) . . ? O2 C4 N2 122.5(7) . . ? O2 C4 C2 120.9(7) . . ? N2 C4 C2 116.6(6) . . ? S3 Ni2 S3 180.0 2_655 . ? S3 Ni2 S4 87.99(7) 2_655 . ? S3 Ni2 S4 92.01(7) . . ? S3 Ni2 S4 92.01(7) 2_655 2_655 ? S3 Ni2 S4 87.99(7) . 2_655 ? S4 Ni2 S4 180.00(16) . 2_655 ? C5 S3 Ni2 104.5(3) . . ? C6 S4 Ni2 104.2(3) . . ? C6 C5 C7 121.8(6) . . ? C6 C5 S3 120.1(5) . . ? C7 C5 S3 118.1(6) . . ? C5 C6 C8 124.9(7) . . ? C5 C6 S4 119.1(5) . . ? C8 C6 S4 116.0(6) . . ? O3 C7 N3 124.3(7) . . ? O3 C7 C5 119.4(7) . . ? N3 C7 C5 116.3(7) . . ? N4 C8 C6 173.5(10) . . ? C9 P1 C21 109.0(4) . . ? C9 P1 C27 108.0(3) . . ? C21 P1 C27 111.5(4) . . ? C9 P1 C15 110.5(4) . . ? C21 P1 C15 107.9(4) . . ? C27 P1 C15 109.9(4) . . ? C10 C9 C14 117.9(7) . . ? C10 C9 P1 122.5(6) . . ? C14 C9 P1 119.3(6) . . ? C11 C10 C9 119.5(9) . . ? C12 C11 C10 122.3(9) . . ? C11 C12 C13 118.8(9) . . ? C12 C13 C14 121.0(9) . . ? C13 C14 C9 120.4(8) . . ? C20 C15 C16 117.5(7) . . ? C20 C15 P1 121.8(6) . . ? C16 C15 P1 120.7(6) . . ? C17 C16 C15 121.3(8) . . ? C16 C17 C18 120.7(8) . . ? C19 C18 C17 119.1(8) . . ? C20 C19 C18 120.6(8) . . ? C19 C20 C15 120.7(7) . . ? C26 C21 C22 119.9(8) . . ? C26 C21 P1 119.7(7) . . ? C22 C21 P1 119.9(6) . . ? C23 C22 C21 118.8(9) . . ? C24 C23 C22 121.8(10) . . ? C23 C24 C25 119.0(10) . . ? C26 C25 C24 121.0(10) . . ? C21 C26 C25 119.5(9) . . ? C28 C27 C32 116.8(9) . . ? C28 C27 P1 120.2(8) . . ? C32 C27 P1 122.9(7) . . ? C29 C28 C27 121.0(11) . . ? C28 C29 C30 119.5(11) . . ? C31 C30 C29 121.0(10) . . ? C30 C31 C32 117.9(13) . . ? C27 C32 C31 123.5(11) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 S1 2.139(2) 2 ? Ni1 S1 2.139(2) . ? Ni1 S2 2.1461(18) . ? Ni1 S2 2.1461(18) 2 ? S1 C1 1.721(7) . ? S2 C2 1.715(7) . ? C1 C2 1.360(9) . ? C1 C3 1.437(10) . ? C2 C4 1.492(9) . ? C3 N1 1.115(9) . ? C4 O2 1.237(7) . ? C4 N2 1.311(8) . ? Ni2 S3 2.1405(19) 2_655 ? Ni2 S3 2.1405(19) . ? Ni2 S4 2.147(2) . ? Ni2 S4 2.147(2) 2_655 ? S3 C5 1.720(7) . ? S4 C6 1.741(7) . ? C5 C6 1.373(10) . ? C5 C7 1.510(9) . ? C6 C8 1.433(10) . ? C7 O3 1.231(8) . ? C7 N3 1.299(9) . ? C8 N4 1.104(9) . ? P1 C9 1.771(7) . ? P1 C21 1.776(8) . ? P1 C27 1.777(8) . ? P1 C15 1.812(7) . ? C9 C10 1.395(10) . ? C9 C14 1.397(10) . ? C10 C11 1.378(11) . ? C11 C12 1.353(12) . ? C12 C13 1.366(11) . ? C13 C14 1.380(11) . ? C15 C20 1.387(10) . ? C15 C16 1.401(9) . ? C16 C17 1.341(11) . ? C17 C18 1.381(11) . ? C18 C19 1.374(11) . ? C19 C20 1.365(11) . ? C21 C26 1.368(10) . ? C21 C22 1.399(10) . ? C22 C23 1.377(11) . ? C23 C24 1.349(13) . ? C24 C25 1.382(14) . ? C25 C26 1.378(12) . ? C27 C28 1.371(13) . ? C27 C32 1.373(12) . ? C28 C29 1.367(13) . ? C29 C30 1.394(17) . ? C30 C31 1.331(17) . ? C31 C32 1.380(12) . ?
1100746.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100746.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100746 loop_ _publ_author_name 'Natasha J. Lundin' 'Penny J. Walsh' 'Sarah L. Howell' 'John J. McGarvey' 'Allan G. Blackman' 'Keith C. Gordon' _publ_contact_author_address ;Department of Chemistry University of Otago P.O. Box 56 Dunedin New Zealand ; _publ_contact_author_email kgordon@alkali.otago.ac.nz _publ_contact_author_fax '+64 3 479 7906' _publ_contact_author_name 'Keith Gordon' _publ_contact_author_phone '+64 3 479 7599' _publ_section_title ; Complexes of Functionalized Dipyrido[3,2-a:2',3'-c]-phenazine: A Synthetic, Spectroscopic, Structural, and Density Functional Theory Study ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3551 _journal_page_last 3560 _journal_paper_doi 10.1021/ic050179k _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C24 H14 Cl N4 O5 Re' _chemical_formula_weight 660.04 _chemical_name_systematic ; ? ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_creation_date 2005-02-03T10:11:14-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _cell_angle_alpha 84.087(5) _cell_angle_beta 84.161(5) _cell_angle_gamma 79.369(5) _cell_formula_units_Z 2 _cell_length_a 6.403(5) _cell_length_b 10.388(5) _cell_length_c 16.976(5) _cell_measurement_reflns_used 7292 _cell_measurement_temperature 176(2) _cell_measurement_theta_max 26.35 _cell_measurement_theta_min 2.25 _cell_volume 1099.9(11) _computing_cell_refinement 'Bruker SMART (Bruker, 1997)' _computing_data_collection 'Bruker SMART (Bruker, 1997)' _computing_data_reduction 'Bruker SAINT (Bruker, 1997)' _computing_molecular_graphics 'WinGX (Farrugia, 1999)' _computing_publication_material 'WinGX (Farrugia, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _diffrn_ambient_temperature 176(2) _diffrn_measured_fraction_theta_full 0.966 _diffrn_measured_fraction_theta_max 0.937 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.0421 _diffrn_reflns_av_unetI/netI 0.0451 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 13073 _diffrn_reflns_theta_full 25 _diffrn_reflns_theta_max 26.44 _diffrn_reflns_theta_min 2 _exptl_absorpt_coefficient_mu 5.692 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_correction_T_min 0.611769 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Bruker, 1997)' _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.993 _exptl_crystal_density_meas ? _exptl_crystal_density_method . _exptl_crystal_description needle _exptl_crystal_F_000 636 _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _refine_diff_density_max 2.823 _refine_diff_density_min -1.861 _refine_diff_density_rms 0.187 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 317 _refine_ls_number_reflns 4234 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.089 _refine_ls_R_factor_all 0.0536 _refine_ls_R_factor_gt 0.041 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0548P)^2^+3.7060P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0928 _refine_ls_wR_factor_ref 0.0978 _reflns_number_gt 3658 _reflns_number_total 4234 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic050179ksi20050202_061130.cif _cod_data_source_block njla _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_database_code 1100746 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.83062(5) 0.43270(3) 0.342091(17) 0.01787(11) Uani 1 1 d . . . Cl1 Cl 0.6892(3) 0.29143(17) 0.25983(11) 0.0237(4) Uani 1 1 d . . . N1 N 0.9997(9) 0.4888(5) 0.2301(3) 0.0179(12) Uani 1 1 d . . . N3 N 0.4717(10) 0.8188(6) 0.0299(3) 0.0195(12) Uani 1 1 d . . . C18 C 1.2913(12) 0.4721(7) 0.1297(4) 0.0229(16) Uani 1 1 d . . . H18 H 1.4312 0.4357 0.1138 0.027 Uiso 1 1 calc R . . O5 O 0.4325(9) 1.0327(5) -0.3072(3) 0.0309(13) Uani 1 1 d . . . C16 C 0.9625(12) 0.6123(7) 0.1026(4) 0.0209(15) Uani 1 1 d . . . C21 C 0.6077(12) 0.7476(7) 0.0775(4) 0.0221(15) Uani 1 1 d . . . C19 C 1.2010(11) 0.4391(7) 0.2059(4) 0.0211(15) Uani 1 1 d . . . H19 H 1.2834 0.381 0.2407 0.025 Uiso 1 1 calc R . . C20 C 0.8244(12) 0.7017(6) 0.0512(4) 0.0194(15) Uani 1 1 d . . . O3 O 0.9929(9) 0.6204(5) 0.4390(3) 0.0245(11) Uani 1 1 d . . . C27 C 0.7690(12) 0.8121(7) -0.0697(4) 0.0214(15) Uani 1 1 d . . . C3 C 0.9319(11) 0.5482(7) 0.4020(4) 0.0201(15) Uani 1 1 d . . . C13 C 0.5306(11) 0.7144(6) 0.1599(4) 0.0169(14) Uani 1 1 d . . . O2 O 0.5438(10) 0.3500(5) 0.4874(3) 0.0310(13) Uani 1 1 d . . . O4 O 0.1587(9) 1.0805(6) -0.2148(3) 0.0334(13) Uani 1 1 d . . . N4 N 0.9044(10) 0.7364(6) -0.0214(3) 0.0213(13) Uani 1 1 d . . . C28 C 0.3391(13) 1.0273(7) -0.2331(4) 0.0256(17) Uani 1 1 d . . . C26 C 0.8471(12) 0.8468(7) -0.1489(4) 0.0238(16) Uani 1 1 d . . . H26 H 0.9912 0.8239 -0.1652 0.029 Uiso 1 1 calc R . . C10 C 0.4093(12) 0.6389(7) 0.3148(4) 0.0203(15) Uani 1 1 d . . . H10 H 0.366 0.6137 0.3672 0.024 Uiso 1 1 calc R . . O1 O 1.1799(10) 0.2093(6) 0.4001(4) 0.0409(15) Uani 1 1 d . . . C17 C 1.1721(12) 0.5578(7) 0.0794(4) 0.0230(16) Uani 1 1 d . . . H17 H 1.231 0.5805 0.0287 0.028 Uiso 1 1 calc R . . C2 C 0.6503(12) 0.3820(6) 0.4336(5) 0.0223(16) Uani 1 1 d . . . C11 C 0.2691(12) 0.7288(7) 0.2702(4) 0.0210(15) Uani 1 1 d . . . H11 H 0.1354 0.7642 0.2932 0.025 Uiso 1 1 calc R . . C23 C 0.4104(13) 0.9229(7) -0.1004(4) 0.0240(16) Uani 1 1 d . . . H23 H 0.267 0.9501 -0.0846 0.029 Uiso 1 1 calc R . . C15 C 0.8825(12) 0.5748(6) 0.1792(4) 0.0193(15) Uani 1 1 d . . . N2 N 0.6030(9) 0.5881(5) 0.2848(3) 0.0181(12) Uani 1 1 d . . . C29 C 0.3067(16) 1.0997(10) -0.3698(5) 0.046(2) Uani 1 1 d . . . H29A H 0.209 1.1739 -0.3492 0.055 Uiso 1 1 calc R . . H29B H 0.4006 1.1338 -0.4121 0.055 Uiso 1 1 calc R . . C1 C 1.0492(13) 0.2930(8) 0.3785(5) 0.0277(17) Uani 1 1 d . . . C25 C 0.7086(13) 0.9139(7) -0.2007(4) 0.0250(16) Uani 1 1 d . . . H25 H 0.759 0.9349 -0.2529 0.03 Uiso 1 1 calc R . . C24 C 0.4891(12) 0.9527(6) -0.1768(4) 0.0205(15) Uani 1 1 d . . . C14 C 0.6661(11) 0.6274(6) 0.2083(4) 0.0159(14) Uani 1 1 d . . . C12 C 0.3279(12) 0.7651(7) 0.1926(4) 0.0219(15) Uani 1 1 d . . . H12 H 0.2333 0.8232 0.162 0.026 Uiso 1 1 calc R . . C30 C 0.190(3) 1.0188(14) -0.4013(10) 0.124(8) Uani 1 1 d . . . H30A H 0.2839 0.9601 -0.4347 0.186 Uiso 1 1 calc R . . H30B H 0.0828 1.072 -0.4321 0.186 Uiso 1 1 calc R . . H30C H 0.1225 0.9686 -0.3587 0.186 Uiso 1 1 calc R . . C22 C 0.5506(12) 0.8497(6) -0.0454(4) 0.0204(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.02063(16) 0.01599(15) 0.01696(15) 0.00097(9) -0.00215(10) -0.00412(10) Cl1 0.0231(9) 0.0213(8) 0.0279(9) -0.0044(7) -0.0023(7) -0.0058(7) N1 0.022(3) 0.014(3) 0.021(3) -0.001(2) -0.005(2) -0.009(2) N3 0.020(3) 0.020(3) 0.019(3) -0.001(2) -0.005(2) -0.005(2) C18 0.020(4) 0.023(4) 0.028(4) -0.005(3) 0.001(3) -0.008(3) O5 0.039(3) 0.034(3) 0.017(3) 0.005(2) -0.003(2) -0.004(3) C16 0.025(4) 0.017(3) 0.024(4) -0.006(3) -0.006(3) -0.008(3) C21 0.027(4) 0.020(4) 0.021(4) 0.000(3) -0.007(3) -0.004(3) C19 0.017(4) 0.017(3) 0.031(4) -0.003(3) 0.000(3) -0.008(3) C20 0.027(4) 0.015(3) 0.019(3) -0.004(3) 0.000(3) -0.009(3) O3 0.031(3) 0.022(3) 0.021(3) 0.005(2) -0.005(2) -0.009(2) C27 0.027(4) 0.016(3) 0.024(4) -0.003(3) -0.002(3) -0.008(3) C3 0.012(3) 0.027(4) 0.016(3) 0.012(3) 0.008(3) -0.002(3) C13 0.024(4) 0.012(3) 0.017(3) -0.004(3) -0.004(3) -0.007(3) O2 0.042(4) 0.031(3) 0.020(3) 0.003(2) 0.010(3) -0.016(3) O4 0.033(3) 0.034(3) 0.030(3) 0.002(2) -0.007(3) 0.002(3) N4 0.025(3) 0.020(3) 0.019(3) 0.000(2) 0.000(3) -0.007(3) C28 0.035(5) 0.018(4) 0.026(4) 0.000(3) -0.007(3) -0.007(3) C26 0.023(4) 0.022(4) 0.025(4) 0.002(3) 0.003(3) -0.008(3) C10 0.023(4) 0.016(3) 0.021(4) 0.002(3) 0.000(3) -0.005(3) O1 0.038(4) 0.033(3) 0.045(4) 0.007(3) -0.008(3) 0.008(3) C17 0.024(4) 0.025(4) 0.024(4) -0.007(3) 0.002(3) -0.013(3) C2 0.028(4) 0.010(3) 0.030(4) 0.000(3) -0.010(3) -0.005(3) C11 0.018(4) 0.020(3) 0.025(4) -0.001(3) -0.001(3) -0.005(3) C23 0.025(4) 0.020(4) 0.026(4) -0.003(3) -0.004(3) -0.002(3) C15 0.027(4) 0.013(3) 0.020(3) 0.000(3) -0.002(3) -0.010(3) N2 0.019(3) 0.014(3) 0.022(3) -0.001(2) -0.006(2) -0.001(2) C29 0.050(6) 0.056(6) 0.027(5) 0.003(4) -0.009(4) 0.006(5) C1 0.025(4) 0.027(4) 0.032(4) -0.007(3) 0.003(3) -0.007(3) C25 0.034(4) 0.020(4) 0.021(4) 0.001(3) -0.002(3) -0.007(3) C24 0.027(4) 0.010(3) 0.024(4) 0.000(3) -0.007(3) -0.003(3) C14 0.019(4) 0.008(3) 0.022(3) 0.000(3) -0.006(3) -0.006(3) C12 0.024(4) 0.017(3) 0.026(4) 0.002(3) -0.008(3) -0.004(3) C30 0.22(2) 0.076(10) 0.101(12) 0.033(9) -0.111(15) -0.050(12) C22 0.028(4) 0.013(3) 0.023(4) 0.000(3) -0.003(3) -0.010(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.231 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Re1 C1 89.4(3) . . ? C3 Re1 C2 90.0(3) . . ? C1 Re1 C2 87.5(3) . . ? C3 Re1 N1 95.8(2) . . ? C1 Re1 N1 97.2(3) . . ? C2 Re1 N1 172.6(3) . . ? C3 Re1 N2 94.1(2) . . ? C1 Re1 N2 172.3(3) . . ? C2 Re1 N2 99.4(3) . . ? N1 Re1 N2 75.6(2) . . ? C3 Re1 Cl1 177.1(2) . . ? C1 Re1 Cl1 93.3(2) . . ? C2 Re1 Cl1 91.1(2) . . ? N1 Re1 Cl1 82.99(15) . . ? N2 Re1 Cl1 83.12(16) . . ? C19 N1 C15 118.4(6) . . ? C19 N1 Re1 125.7(5) . . ? C15 N1 Re1 115.6(5) . . ? C21 N3 C22 116.4(6) . . ? C17 C18 C19 119.0(7) . . ? C17 C18 H18 120.5 . . ? C19 C18 H18 120.5 . . ? C28 O5 C29 118.0(7) . . ? C17 C16 C15 117.2(7) . . ? C17 C16 C20 123.7(7) . . ? C15 C16 C20 119.1(7) . . ? N3 C21 C20 122.3(7) . . ? N3 C21 C13 118.3(7) . . ? C20 C21 C13 119.4(6) . . ? N1 C19 C18 121.9(7) . . ? N1 C19 H19 119.1 . . ? C18 C19 H19 119.1 . . ? N4 C20 C21 121.4(6) . . ? N4 C20 C16 118.0(7) . . ? C21 C20 C16 120.6(6) . . ? N4 C27 C22 121.8(7) . . ? N4 C27 C26 118.3(7) . . ? C22 C27 C26 119.7(7) . . ? O3 C3 Re1 179.4(6) . . ? C12 C13 C14 118.0(6) . . ? C12 C13 C21 123.2(6) . . ? C14 C13 C21 118.8(6) . . ? C20 N4 C27 116.7(6) . . ? O4 C28 O5 124.0(7) . . ? O4 C28 C24 125.1(7) . . ? O5 C28 C24 110.9(7) . . ? C25 C26 C27 119.2(7) . . ? C25 C26 H26 120.4 . . ? C27 C26 H26 120.4 . . ? N2 C10 C11 121.9(7) . . ? N2 C10 H10 119.1 . . ? C11 C10 H10 119.1 . . ? C18 C17 C16 120.9(7) . . ? C18 C17 H17 119.6 . . ? C16 C17 H17 119.6 . . ? O2 C2 Re1 178.9(6) . . ? C12 C11 C10 119.9(7) . . ? C12 C11 H11 120 . . ? C10 C11 H11 120 . . ? C24 C23 C22 119.3(7) . . ? C24 C23 H23 120.4 . . ? C22 C23 H23 120.4 . . ? N1 C15 C16 122.7(7) . . ? N1 C15 C14 116.5(6) . . ? C16 C15 C14 120.8(6) . . ? C10 N2 C14 118.6(6) . . ? C10 N2 Re1 126.6(5) . . ? C14 N2 Re1 114.6(4) . . ? C30 C29 O5 113.1(9) . . ? C30 C29 H29A 109 . . ? O5 C29 H29A 109 . . ? C30 C29 H29B 109 . . ? O5 C29 H29B 109 . . ? H29A C29 H29B 107.8 . . ? O1 C1 Re1 179.9(7) . . ? C26 C25 C24 121.5(7) . . ? C26 C25 H25 119.3 . . ? C24 C25 H25 119.3 . . ? C23 C24 C25 120.5(6) . . ? C23 C24 C28 118.1(7) . . ? C25 C24 C28 121.3(7) . . ? N2 C14 C13 122.1(6) . . ? N2 C14 C15 116.8(6) . . ? C13 C14 C15 121.0(6) . . ? C11 C12 C13 119.3(6) . . ? C11 C12 H12 120.3 . . ? C13 C12 H12 120.3 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N3 C22 C27 121.1(6) . . ? N3 C22 C23 119.1(7) . . ? C27 C22 C23 119.8(7) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 C3 1.890(8) . ? Re1 C1 1.921(8) . ? Re1 C2 1.927(8) . ? Re1 N1 2.170(6) . ? Re1 N2 2.185(5) . ? Re1 Cl1 2.4683(19) . ? N1 C19 1.337(9) . ? N1 C15 1.355(9) . ? N3 C21 1.320(9) . ? N3 C22 1.355(9) . ? C18 C17 1.352(10) . ? C18 C19 1.398(11) . ? C18 H18 0.93 . ? O5 C28 1.337(10) . ? O5 C29 1.442(10) . ? C16 C17 1.391(10) . ? C16 C15 1.392(10) . ? C16 C20 1.447(10) . ? C21 C20 1.423(10) . ? C21 C13 1.464(10) . ? C19 H19 0.93 . ? C20 N4 1.326(9) . ? O3 C3 1.167(9) . ? C27 N4 1.342(9) . ? C27 C22 1.412(11) . ? C27 C26 1.422(10) . ? C13 C12 1.390(10) . ? C13 C14 1.396(9) . ? O2 C2 1.143(9) . ? O4 C28 1.209(10) . ? C28 C24 1.481(10) . ? C26 C25 1.359(10) . ? C26 H26 0.93 . ? C10 N2 1.328(9) . ? C10 C11 1.391(10) . ? C10 H10 0.93 . ? O1 C1 1.148(9) . ? C17 H17 0.93 . ? C11 C12 1.367(10) . ? C11 H11 0.93 . ? C23 C24 1.368(11) . ? C23 C22 1.423(10) . ? C23 H23 0.93 . ? C15 C14 1.449(10) . ? N2 C14 1.363(9) . ? C29 C30 1.400(18) . ? C29 H29A 0.97 . ? C29 H29B 0.97 . ? C25 C24 1.418(11) . ? C25 H25 0.93 . ? C12 H12 0.93 . ? C30 H30A 0.96 . ? C30 H30B 0.96 . ? C30 H30C 0.96 . ?
1100747.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100747.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100747 loop_ _publ_author_name 'Natasha J. Lundin' 'Penny J. Walsh' 'Sarah L. Howell' 'John J. McGarvey' 'Allan G. Blackman' 'Keith C. Gordon' _publ_contact_author_address ;Department of Chemistry University of Otago P.O. Box 56 Dunedin New Zealand ; _publ_contact_author_email kgordon@alkali.otago.ac.nz _publ_contact_author_fax '+64 3 479 7906' _publ_contact_author_name 'Keith Gordon' _publ_contact_author_phone '+64 3 479 7599' _publ_section_title ; Complexes of Functionalized Dipyrido[3,2-a:2',3'-c]-phenazine: A Synthetic, Spectroscopic, Structural, and Density Functional Theory Study ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3551 _journal_page_last 3560 _journal_paper_doi 10.1021/ic050179k _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C22 H12 Br Cl N4 O4 Re' _chemical_formula_weight 697.92 _chemical_name_systematic ; ? ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_creation_date 2004-08-30T13:27:07-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _cell_angle_alpha 90.000 _cell_angle_beta 114.936(5) _cell_angle_gamma 90.000 _cell_formula_units_Z 8 _cell_length_a 19.506(5) _cell_length_b 18.043(5) _cell_length_c 13.320(5) _cell_measurement_reflns_used 9837 _cell_measurement_temperature 164(2) _cell_measurement_theta_max 26.51 _cell_measurement_theta_min 2.3 _cell_volume 4251(2) _computing_cell_refinement 'Bruker SMART (Bruker, 1997)' _computing_data_collection 'Bruker SMART (Bruker, 1997)' _computing_data_reduction 'Bruker SAINT (Bruker, 1997)' _computing_molecular_graphics 'WinGX (Farrugia, 1999)' _computing_publication_material 'WinGX (Farrugia, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SIR-97 (Altomare et al, 1997)' _diffrn_ambient_temperature 164(2) _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.0316 _diffrn_reflns_av_unetI/netI 0.0202 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 26269 _diffrn_reflns_theta_full 26.54 _diffrn_reflns_theta_max 26.54 _diffrn_reflns_theta_min 1.95 _exptl_absorpt_coefficient_mu 7.762 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_correction_T_min 0.709676 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Bruker, 1997)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 2.181 _exptl_crystal_density_meas ? _exptl_crystal_density_method . _exptl_crystal_description block _exptl_crystal_F_000 2648 _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _refine_diff_density_max 2.203 _refine_diff_density_min -1.684 _refine_diff_density_rms 0.134 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 310 _refine_ls_number_reflns 4381 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.067 _refine_ls_R_factor_all 0.0345 _refine_ls_R_factor_gt 0.0298 _refine_ls_shift/su_max 0.016 _refine_ls_shift/su_mean 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0411P)^2^+40.1104P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0791 _refine_ls_wR_factor_ref 0.0827 _reflns_number_gt 3956 _reflns_number_total 4381 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic050179ksi20050202_061153.cif _cod_data_source_block njldm _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_database_code 1100747 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.656870(10) 0.154175(10) 0.580330(16) 0.02564(8) Uani 1 1 d . . . Br1 Br 1.26297(6) -0.10104(8) 1.06764(9) 0.0443(4) Uani 0.501(2) 1 d P A 1 Br1A Br 1.17956(9) -0.23632(9) 1.02240(13) 0.0662(6) Uani 0.499(2) 1 d P A 2 Cl1 Cl 0.69696(9) 0.10626(7) 0.44017(11) 0.0382(3) Uani 1 1 d . . . N2 N 0.7769(2) 0.1700(2) 0.6792(3) 0.0238(8) Uani 1 1 d . . . C300 C 0.5538(3) 0.1330(3) 0.4888(6) 0.0441(15) Uani 1 1 d . . . C3 C 0.7672(3) -0.0910(3) 0.7238(4) 0.0312(11) Uani 1 1 d . . . H3 H 0.7898 -0.137 0.7467 0.037 Uiso 1 1 calc R . . C6 C 0.8167(3) 0.1079(3) 0.7227(4) 0.0235(9) Uani 1 1 d . . . C100 C 0.6356(3) 0.2527(3) 0.5228(4) 0.0301(11) Uani 1 1 d . . . N1 N 0.6984(2) 0.0460(2) 0.6512(3) 0.0249(8) Uani 1 1 d . . . N3 N 1.0084(2) 0.0420(3) 0.8774(3) 0.0285(9) Uani 1 1 d . A . N4 N 0.9273(2) -0.0933(3) 0.8293(4) 0.0315(9) Uani 1 1 d . . . C4 C 0.8111(3) -0.0272(3) 0.7429(4) 0.0250(10) Uani 1 1 d . . . C7 C 0.8950(3) 0.1086(3) 0.7828(4) 0.0256(10) Uani 1 1 d . . . C10 C 0.8131(3) 0.2340(3) 0.6954(4) 0.0311(11) Uani 1 1 d . . . H10 H 0.7857 0.2769 0.6654 0.037 Uiso 1 1 calc R . . C11 C 0.9342(3) 0.0393(3) 0.8228(4) 0.0266(10) Uani 1 1 d . . . C9 C 0.8914(3) 0.2389(3) 0.7565(5) 0.0351(12) Uani 1 1 d . . . H9 H 0.9156 0.2846 0.7665 0.042 Uiso 1 1 calc R . . C13 C 1.0039(3) -0.0911(3) 0.8829(4) 0.0339(12) Uani 1 1 d . A . C200 C 0.6287(4) 0.1859(3) 0.6939(6) 0.0436(14) Uani 1 1 d . . . C2 C 0.6904(3) -0.0847(3) 0.6708(5) 0.0373(13) Uani 1 1 d . . . H2 H 0.66 -0.1265 0.6582 0.045 Uiso 1 1 calc R . . O3 O 0.4914(2) 0.1209(3) 0.4307(5) 0.0685(16) Uani 1 1 d . . . C16 C 1.1601(3) -0.0903(4) 0.9951(5) 0.0476(17) Uani 1 1 d . . . O1 O 0.6229(2) 0.3118(2) 0.4898(4) 0.0399(9) Uani 1 1 d . . . C8 C 0.9319(3) 0.1770(3) 0.8008(4) 0.0314(11) Uani 1 1 d . . . H8 H 0.9838 0.1799 0.8429 0.038 Uiso 1 1 calc R . . C1 C 0.6579(3) -0.0155(3) 0.6359(4) 0.0314(11) Uani 1 1 d . . . H1 H 0.6055 -0.0122 0.6002 0.038 Uiso 1 1 calc R . . C15 C 1.1203(4) -0.1577(4) 0.9683(6) 0.0523(18) Uani 1 1 d . A . C17 C 1.1237(3) -0.0243(4) 0.9661(4) 0.0384(13) Uani 1 1 d . A . H17 H 1.1508 0.0199 0.9839 0.046 Uiso 1 1 calc R . . O2 O 0.6084(4) 0.2074(3) 0.7563(5) 0.0702(16) Uani 1 1 d . . . C12 C 0.8931(3) -0.0287(3) 0.8000(4) 0.0241(9) Uani 1 1 d . . . C18 C 1.0440(3) -0.0237(3) 0.9084(4) 0.0319(11) Uani 1 1 d . . . C5 C 0.7743(3) 0.0399(3) 0.7051(4) 0.0227(9) Uani 1 1 d . . . C14 C 1.0440(4) -0.1583(4) 0.9132(5) 0.0450(15) Uani 1 1 d . . . H14 H 1.0182 -0.2032 0.8954 0.054 Uiso 1 1 calc R A . O4 O 0.53070(19) -0.0542(2) 0.3695(2) 0.0268(7) Uani 1 1 d . . . H4 H 0.5488 -0.0955 0.3901 0.04 Uiso 1 1 calc R . . C19 C 0.5659(7) -0.0218(6) 0.3155(9) 0.109(5) Uani 1 1 d . . . H19A H 0.6011 0.0141 0.3628 0.164 Uiso 1 1 calc R . . H19B H 0.5295 0.0025 0.2509 0.164 Uiso 1 1 calc R . . H19C H 0.5926 -0.0585 0.2937 0.164 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.01763(11) 0.02622(12) 0.02963(13) 0.00241(7) 0.00663(8) -0.00129(7) Br1 0.0238(5) 0.0731(9) 0.0316(6) 0.0084(5) 0.0075(4) 0.0153(5) Br1A 0.0549(9) 0.0684(10) 0.0531(9) -0.0035(7) 0.0012(6) 0.0380(7) Cl1 0.0509(8) 0.0319(6) 0.0329(7) 0.0014(5) 0.0187(6) -0.0021(6) N2 0.0206(19) 0.026(2) 0.023(2) -0.0015(16) 0.0081(16) -0.0027(16) C300 0.027(3) 0.035(3) 0.059(4) 0.015(3) 0.007(3) 0.000(2) C3 0.030(3) 0.027(2) 0.033(3) 0.007(2) 0.010(2) -0.003(2) C6 0.021(2) 0.030(2) 0.020(2) -0.0024(18) 0.0091(18) -0.0049(18) C100 0.018(2) 0.036(3) 0.032(3) 0.001(2) 0.0055(19) -0.001(2) N1 0.0183(18) 0.030(2) 0.024(2) 0.0036(16) 0.0060(15) -0.0027(16) N3 0.0192(19) 0.046(3) 0.0195(19) 0.0039(18) 0.0071(16) -0.0006(18) N4 0.027(2) 0.041(2) 0.025(2) 0.0052(18) 0.0104(18) 0.0044(19) C4 0.021(2) 0.033(3) 0.021(2) 0.0051(19) 0.0086(18) -0.0020(19) C7 0.020(2) 0.035(3) 0.021(2) -0.0015(19) 0.0078(18) -0.0045(19) C10 0.030(2) 0.027(2) 0.035(3) -0.003(2) 0.012(2) -0.006(2) C11 0.021(2) 0.041(3) 0.019(2) -0.002(2) 0.0092(18) -0.002(2) C9 0.032(3) 0.032(3) 0.038(3) -0.005(2) 0.012(2) -0.011(2) C13 0.026(2) 0.052(3) 0.025(2) 0.009(2) 0.012(2) 0.010(2) C200 0.044(3) 0.038(3) 0.062(4) 0.008(3) 0.036(3) 0.007(3) C2 0.027(3) 0.035(3) 0.039(3) 0.010(2) 0.003(2) -0.010(2) O3 0.023(2) 0.056(3) 0.095(4) 0.018(3) -0.005(2) -0.009(2) C16 0.031(3) 0.085(5) 0.030(3) 0.018(3) 0.017(2) 0.023(3) O1 0.036(2) 0.030(2) 0.049(2) 0.0077(18) 0.0132(18) 0.0082(16) C8 0.021(2) 0.042(3) 0.027(3) -0.005(2) 0.007(2) -0.010(2) C1 0.019(2) 0.036(3) 0.032(3) 0.007(2) 0.003(2) -0.009(2) C15 0.042(3) 0.079(5) 0.038(3) 0.020(3) 0.019(3) 0.029(3) C17 0.022(2) 0.069(4) 0.023(2) 0.008(3) 0.008(2) 0.006(2) O2 0.092(4) 0.067(3) 0.079(4) 0.006(3) 0.063(4) 0.017(3) C12 0.021(2) 0.033(3) 0.018(2) 0.0049(19) 0.0079(18) 0.0020(19) C18 0.019(2) 0.057(3) 0.021(2) 0.005(2) 0.0108(19) 0.004(2) C5 0.021(2) 0.028(2) 0.019(2) -0.0004(18) 0.0082(17) -0.0060(18) C14 0.040(3) 0.056(4) 0.038(3) 0.016(3) 0.016(3) 0.015(3) O4 0.0300(17) 0.041(2) 0.0071(14) -0.0046(13) 0.0055(13) -0.0209(15) C19 0.175(11) 0.097(7) 0.104(8) -0.057(6) 0.106(8) -0.086(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.231 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C300 Re1 C200 89.4(3) . . ? C300 Re1 C100 86.4(2) . . ? C200 Re1 C100 87.3(2) . . ? C300 Re1 N2 175.1(2) . . ? C200 Re1 N2 94.4(2) . . ? C100 Re1 N2 96.76(18) . . ? C300 Re1 N1 101.4(2) . . ? C200 Re1 N1 96.0(2) . . ? C100 Re1 N1 171.51(17) . . ? N2 Re1 N1 75.21(15) . . ? C300 Re1 Cl1 91.8(2) . . ? C200 Re1 Cl1 176.46(19) . . ? C100 Re1 Cl1 96.14(16) . . ? N2 Re1 Cl1 84.26(11) . . ? N1 Re1 Cl1 80.51(11) . . ? C10 N2 C6 119.0(4) . . ? C10 N2 Re1 125.4(3) . . ? C6 N2 Re1 115.5(3) . . ? O3 C300 Re1 178.1(6) . . ? C2 C3 C4 118.8(5) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? N2 C6 C7 122.2(4) . . ? N2 C6 C5 116.8(4) . . ? C7 C6 C5 121.0(5) . . ? O1 C100 Re1 179.0(5) . . ? C1 N1 C5 117.5(4) . . ? C1 N1 Re1 126.6(3) . . ? C5 N1 Re1 115.4(3) . . ? C11 N3 C18 116.1(5) . . ? C12 N4 C13 115.9(5) . . ? C5 C4 C3 118.1(4) . . ? C5 C4 C12 119.5(4) . . ? C3 C4 C12 122.5(5) . . ? C6 C7 C8 117.9(5) . . ? C6 C7 C11 119.0(4) . . ? C8 C7 C11 123.2(4) . . ? N2 C10 C9 121.8(5) . . ? N2 C10 H10 119.1 . . ? C9 C10 H10 119.1 . . ? N3 C11 C12 122.5(5) . . ? N3 C11 C7 117.3(5) . . ? C12 C11 C7 120.2(4) . . ? C8 C9 C10 119.7(5) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? N4 C13 C18 121.9(5) . . ? N4 C13 C14 118.8(6) . . ? C18 C13 C14 119.3(5) . . ? O2 C200 Re1 175.6(6) . . ? C3 C2 C1 119.7(5) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C17 C16 C15 121.4(6) . . ? C17 C16 Br1 124.5(6) . . ? C15 C16 Br1 114.0(5) . . ? C9 C8 C7 119.4(5) . . ? C9 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? N1 C1 C2 122.8(4) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C14 C15 C16 120.6(6) . . ? C14 C15 Br1A 126.2(6) . . ? C16 C15 Br1A 113.1(5) . . ? C16 C17 C18 118.9(6) . . ? C16 C17 H17 120.5 . . ? C18 C17 H17 120.5 . . ? N4 C12 C11 121.9(4) . . ? N4 C12 C4 118.6(4) . . ? C11 C12 C4 119.4(4) . . ? N3 C18 C13 121.6(4) . . ? N3 C18 C17 118.6(5) . . ? C13 C18 C17 119.8(5) . . ? N1 C5 C4 123.1(4) . . ? N1 C5 C6 116.2(4) . . ? C4 C5 C6 120.6(4) . . ? C15 C14 C13 120.0(7) . . ? C15 C14 H14 120 . . ? C13 C14 H14 120 . . ? C19 O4 H4 109.5 . . ? O4 C19 H19A 109.5 . . ? O4 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O4 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 C300 1.900(6) . ? Re1 C200 1.902(6) . ? Re1 C100 1.911(5) . ? Re1 N2 2.168(4) . ? Re1 N1 2.171(4) . ? Re1 Cl1 2.4648(15) . ? Br1 C16 1.834(6) . ? Br1A C15 1.779(6) . ? N2 C10 1.323(6) . ? N2 C6 1.346(6) . ? C300 O3 1.154(7) . ? C3 C2 1.365(7) . ? C3 C4 1.393(7) . ? C3 H3 0.93 . ? C6 C7 1.394(6) . ? C6 C5 1.442(6) . ? C100 O1 1.141(7) . ? N1 C1 1.327(6) . ? N1 C5 1.352(6) . ? N3 C11 1.319(6) . ? N3 C18 1.347(7) . ? N4 C12 1.318(7) . ? N4 C13 1.357(7) . ? C4 C5 1.389(7) . ? C4 C12 1.454(6) . ? C7 C8 1.397(7) . ? C7 C11 1.446(7) . ? C10 C9 1.399(7) . ? C10 H10 0.93 . ? C11 C12 1.425(7) . ? C9 C8 1.351(8) . ? C9 H9 0.93 . ? C13 C18 1.406(8) . ? C13 C14 1.408(8) . ? C200 O2 1.131(8) . ? C2 C1 1.388(8) . ? C2 H2 0.93 . ? C16 C17 1.356(9) . ? C16 C15 1.404(11) . ? C8 H8 0.93 . ? C1 H1 0.93 . ? C15 C14 1.353(9) . ? C17 C18 1.416(7) . ? C17 H17 0.93 . ? C14 H14 0.93 . ? O4 C19 1.321(9) . ? O4 H4 0.82 . ? C19 H19A 0.96 . ? C19 H19B 0.96 . ? C19 H19C 0.96 . ?
1100748.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100748.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100748 loop_ _publ_author_name 'Theocharis C. Stamatatos' 'Stavroula Dionyssopoulou' 'Georgios Efthymiou' 'Panayotis Kyritsis' 'Catherine P. Raptopoulou' 'Aris Terzis' 'Ramon Vicente' 'Albert Escuer' 'Spyros P. Perlepes' _publ_section_title ; The First Cobalt Metallacrowns: Preparation and Characterization of Mixed-Valence Cobalt(II/III), Inverse 12-Metallacrown-4 Complexes ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3374 _journal_page_last 3376 _journal_paper_doi 10.1021/ic050208r _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C54 H70.16 Cl2 Co4 N12 O27.08' _chemical_formula_weight 1627.28 _chemical_name_systematic ; ? ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL _cell_angle_alpha 110.15(1) _cell_angle_beta 95.25(2) _cell_angle_gamma 92.05(2) _cell_formula_units_Z 1 _cell_length_a 10.523(5) _cell_length_b 13.556(5) _cell_length_c 12.465(5) _cell_measurement_reflns_used 25 _cell_measurement_temperature 298 _cell_measurement_theta_max 11.7 _cell_measurement_theta_min 5.3 _cell_volume 1658.0(12) _computing_cell_refinement 'Program LEAST (UCLA Cryst.package C.E.Strouse 1994)' _computing_data_collection 'Program COLLECT (UCLA Cryst.package C.E.Strouse 1994)' _computing_data_reduction 'Program REDUCE (UCLA Cryst.package C.E.Strouse 1994)' _computing_molecular_graphics ORTEP _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _diffrn_ambient_temperature 298 _diffrn_measurement_device 'Crystal Logic Dual Goniometer' _diffrn_measurement_method 'theta-2theta scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0220 _diffrn_reflns_av_sigmaI/netI 0.0530 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 5936 _diffrn_reflns_theta_max 24.75 _diffrn_reflns_theta_min 1.92 _diffrn_standards_decay_% -2.9 _diffrn_standards_interval_count 97 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.157 _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.630 _exptl_crystal_density_meas 1.62 _exptl_crystal_density_method 'floating method' _exptl_crystal_description parallelipiped _exptl_crystal_F_000 837 _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.928 _refine_diff_density_min -0.507 _refine_diff_density_rms 0.095 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 1.093 _refine_ls_goodness_of_fit_obs 1.136 _refine_ls_matrix_type full _refine_ls_number_parameters 497 _refine_ls_number_reflns 5653 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.094 _refine_ls_restrained_S_obs 1.136 _refine_ls_R_factor_all 0.0785 _refine_ls_R_factor_obs 0.0596 _refine_ls_shift/esd_max 0.146 _refine_ls_shift/esd_mean 0.004 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0817P)^2^+2.8053P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.1696 _refine_ls_wR_factor_obs 0.1546 _reflns_number_observed 4454 _reflns_number_total 5654 _reflns_observed_criterion >2sigma(I) _cod_data_source_file ic050208rsi20050207_081321.cif _cod_data_source_block pexs532 _cod_depositor_comments ; The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w=1/[\s^2^(Fo^2^)+(0.0817P)^2^+2.8053P] where P=(Fo^2^+2Fc^2^)/3' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w=1/[\s^2^(Fo^2^)+(0.0817P)^2^+2.8053P] where P=(Fo^2^+2Fc^2^)/3'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_cell_volume 1657.8(2) _cod_database_code 1100748 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0370(4) 0.0358(3) 0.0308(3) 0.0077(3) 0.0037(2) -0.0057(3) Co2 0.0355(4) 0.0393(4) 0.0413(4) 0.0099(3) 0.0014(3) -0.0046(3) O1 0.044(2) 0.039(2) 0.033(2) 0.0077(14) 0.0062(14) -0.0023(14) N1 0.045(2) 0.040(2) 0.033(2) 0.005(2) 0.006(2) -0.006(2) N2 0.035(2) 0.036(2) 0.033(2) 0.008(2) 0.004(2) -0.008(2) N3 0.038(2) 0.049(2) 0.040(2) 0.017(2) -0.001(2) -0.004(2) O11 0.041(2) 0.043(2) 0.040(2) 0.0034(14) 0.0045(14) -0.0116(15) N11 0.040(2) 0.038(2) 0.038(2) 0.012(2) 0.004(2) -0.006(2) N12 0.036(2) 0.036(2) 0.035(2) 0.008(2) 0.001(2) -0.008(2) O21 0.041(2) 0.043(2) 0.040(2) 0.013(2) 0.0054(14) -0.007(2) O31 0.047(2) 0.042(2) 0.049(2) 0.015(2) 0.001(2) -0.0010(15) O32 0.064(3) 0.047(2) 0.074(3) 0.028(2) -0.016(2) -0.009(2) OM1 0.055(3) 0.091(4) 0.094(4) 0.008(3) 0.023(3) 0.010(3) C1 0.067(4) 0.049(3) 0.043(3) 0.009(2) 0.007(3) 0.006(3) C2 0.103(6) 0.053(4) 0.052(4) -0.003(3) 0.014(3) 0.016(4) C3 0.119(6) 0.073(4) 0.038(3) 0.004(3) 0.005(4) 0.013(4) C4 0.090(5) 0.067(4) 0.035(3) 0.013(3) 0.005(3) 0.009(3) C5 0.050(3) 0.047(3) 0.032(2) 0.007(2) 0.004(2) -0.006(2) C6 0.040(3) 0.044(3) 0.037(2) 0.015(2) 0.001(2) -0.006(2) C7 0.041(3) 0.049(3) 0.031(2) 0.009(2) 0.004(2) -0.001(2) C8 0.056(3) 0.055(4) 0.045(3) 0.011(3) -0.006(2) -0.005(3) C9 0.056(4) 0.079(5) 0.046(3) 0.004(3) -0.014(3) 0.001(3) C10 0.061(4) 0.074(4) 0.050(3) 0.015(3) -0.011(3) 0.015(3) C11 0.059(3) 0.052(3) 0.045(3) 0.016(3) 0.001(3) 0.002(3) C21 0.058(3) 0.044(3) 0.039(3) 0.006(2) 0.005(2) -0.013(2) C22 0.059(4) 0.051(3) 0.065(4) 0.013(3) 0.005(3) -0.025(3) C23 0.059(4) 0.074(4) 0.056(4) 0.015(3) 0.012(3) -0.030(3) C24 0.057(4) 0.064(4) 0.045(3) 0.010(3) 0.016(3) -0.016(3) C25 0.044(3) 0.041(3) 0.037(3) 0.012(2) 0.005(2) -0.007(2) C26 0.038(2) 0.039(2) 0.034(2) 0.009(2) 0.000(2) -0.005(2) C27 0.040(3) 0.060(3) 0.033(2) 0.005(2) 0.005(2) -0.008(2) C28 0.069(4) 0.065(4) 0.051(3) 0.004(3) 0.017(3) -0.004(3) C29 0.095(6) 0.072(5) 0.069(5) -0.007(4) 0.026(4) -0.008(4) C30 0.067(4) 0.113(7) 0.053(4) -0.013(4) 0.020(3) -0.017(4) C31 0.073(5) 0.115(7) 0.045(3) 0.022(4) 0.012(3) -0.013(4) N13 0.068(3) 0.085(4) 0.036(2) 0.013(2) 0.008(2) -0.020(3) C41 0.053(3) 0.044(3) 0.059(3) 0.020(3) 0.000(3) -0.001(2) C42 0.068(4) 0.059(4) 0.116(6) 0.036(4) -0.016(4) -0.001(3) CM1 0.132(11) 0.215(15) 0.251(18) 0.106(14) 0.111(12) 0.033(11) Cl1 0.168(2) 0.0705(11) 0.0491(9) 0.0106(8) 0.0087(11) -0.0150(13) O41 0.238(10) 0.095(5) 0.104(5) -0.029(4) 0.013(6) -0.028(5) O42 0.405(20) 0.198(10) 0.133(8) -0.026(7) 0.130(11) -0.160(13) O43 0.495(22) 0.232(11) 0.074(5) 0.041(6) 0.007(8) -0.211(14) O44 0.514(34) 0.249(16) 0.304(22) 0.034(15) -0.114(21) 0.203(21) loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co1 Co 0.40826(6) 0.28287(5) 0.94904(5) 0.0358(2) Uani 1 d . . Co2 Co 0.68396(6) 0.40240(5) 1.05880(6) 0.0402(2) Uani 1 d . . O1 O 0.2752(3) 0.4630(2) 0.9780(3) 0.0401(7) Uani 1 d . . N1 N 0.3724(4) 0.1968(3) 0.7883(3) 0.0417(9) Uani 1 d . . N2 N 0.3043(4) 0.3751(3) 0.9028(3) 0.0360(8) Uani 1 d . . N3 N 0.1957(4) 0.5145(3) 0.7877(3) 0.0427(9) Uani 1 d . . O11 O 0.5232(3) 0.4534(3) 1.1445(3) 0.0448(8) Uani 1 d . . N11 N 0.2609(4) 0.2288(3) 0.9987(3) 0.0391(9) Uani 1 d . . N12 N 0.4304(4) 0.3764(3) 1.1055(3) 0.0374(9) Uani 1 d . . O21 O 0.5568(3) 0.3432(3) 0.9150(3) 0.0416(8) Uani 1 d . . O31 O 0.5033(3) 0.1725(3) 0.9782(3) 0.0465(8) Uani 1 d . . O32 O 0.6744(4) 0.2651(3) 1.0927(4) 0.0615(11) Uani 1 d . . OM1 O 0.8396(6) 0.3373(5) 0.9694(6) 0.085(2) Uani 1 d . . C1 C 0.4156(6) 0.1017(4) 0.7364(5) 0.0549(14) Uani 1 d . . C2 C 0.3932(8) 0.0505(5) 0.6191(6) 0.074(2) Uani 1 d . . C3 C 0.3300(8) 0.1003(6) 0.5532(6) 0.081(2) Uani 1 d . . C4 C 0.2867(7) 0.1979(5) 0.6053(5) 0.065(2) Uani 1 d . . C5 C 0.3055(5) 0.2450(4) 0.7241(4) 0.0451(12) Uani 1 d . . C6 C 0.2620(5) 0.3459(4) 0.7935(4) 0.0406(11) Uani 1 d . . C7 C 0.1751(5) 0.4084(4) 0.7464(4) 0.0418(11) Uani 1 d . . C8 C 0.0749(6) 0.3589(5) 0.6632(5) 0.0547(14) Uani 1 d . . C9 C -0.0017(6) 0.4182(6) 0.6175(5) 0.066(2) Uani 1 d . . C10 C 0.0218(6) 0.5246(6) 0.6554(5) 0.064(2) Uani 1 d . . C11 C 0.1203(6) 0.5702(5) 0.7416(5) 0.0528(13) Uani 1 d . . C21 C 0.1742(6) 0.1517(4) 0.9358(5) 0.0495(13) Uani 1 d . . C22 C 0.0713(6) 0.1220(5) 0.9790(6) 0.061(2) Uani 1 d . . C23 C 0.0558(6) 0.1733(5) 1.0928(5) 0.065(2) Uani 1 d . . C24 C 0.1451(6) 0.2527(5) 1.1594(5) 0.058(2) Uani 1 d . . C25 C 0.2473(5) 0.2802(4) 1.1113(4) 0.0418(11) Uani 1 d . . C26 C 0.3468(4) 0.3655(4) 1.1699(4) 0.0387(10) Uani 1 d . . C27 C 0.3453(5) 0.4365(4) 1.2919(4) 0.0476(12) Uani 1 d . . C28 C 0.3539(7) 0.5448(5) 1.3209(6) 0.066(2) Uani 1 d . . C29 C 0.3498(8) 0.6091(7) 1.4342(7) 0.086(2) Uani 1 d . . C30 C 0.3382(7) 0.5617(8) 1.5138(6) 0.088(3) Uani 1 d . . C31 C 0.3293(8) 0.4567(8) 1.4801(6) 0.079(2) Uani 1 d . . N13 N 0.3332(5) 0.3911(4) 1.3695(4) 0.0660(14) Uani 1 d . . C41 C 0.6110(5) 0.1815(4) 1.0373(5) 0.0522(13) Uani 1 d . . C42 C 0.6659(7) 0.0798(5) 1.0368(7) 0.081(2) Uani 1 d . . H42A H 0.5974(7) 0.0273(15) 1.0254(53) 0.126(20) Uiso 1 calc R . H42B H 0.7159(49) 0.0915(13) 1.1090(21) 0.126(20) Uiso 1 calc R . H42C H 0.7192(46) 0.0562(25) 0.9756(33) 0.126(20) Uiso 1 calc R . CM1 C 0.9481(13) 0.3793(12) 0.9472(14) 0.186(7) Uani 1 d . . HM1A H 0.9771(63) 0.3311(42) 0.8790(58) 0.242 Uiso 1 calc R . HM1B H 1.0129(36) 0.3923(85) 1.0109(44) 0.242 Uiso 1 calc R . HM1C H 0.9315(29) 0.4444(49) 0.9359(101) 0.242 Uiso 1 calc R . Cl1 Cl -0.0938(3) 0.1526(2) 0.3711(2) 0.0995(7) Uani 1 d . . O41 O -0.1144(10) 0.0645(6) 0.2775(6) 0.164(4) Uani 1 d . . O42 O 0.0103(17) 0.2161(10) 0.3753(9) 0.265(9) Uani 1 d . . O43 O -0.1153(17) 0.1503(10) 0.4683(7) 0.278(9) Uani 1 d . . O44 O -0.1836(26) 0.2125(15) 0.3510(16) 0.378(15) Uani 1 d . . OM2 O 0.3833(12) 0.1789(9) 0.3291(10) 0.194(4) Uiso 1 d . . CM2 C 0.4868(16) 0.1690(12) 0.2849(13) 0.162(5) Uiso 1 d . . OM3 O 0.2289(16) 0.8382(13) 0.2114(15) 0.271(7) Uiso 1 d . . CM3 C 0.2881(22) 0.7946(17) 0.2866(19) 0.232(9) Uiso 1 d . . OW1 O 0.2089(15) 0.0182(12) 0.2491(13) 0.249(6) Uiso 1 d . . OW2 O -0.0161(18) 0.1024(14) 0.6611(16) 0.171(11) Uiso 0.54(3) d P . HOM1 H 0.8073(112) 0.3194(93) 0.9181(90) 0.123(50) Uiso 1 d . . H1 H 0.4632(52) 0.0722(41) 0.7857(47) 0.046(14) Uiso 1 d . . H2 H 0.4197(53) -0.0123(47) 0.5896(48) 0.049(15) Uiso 1 d . . H3 H 0.3090(62) 0.0609(53) 0.4728(60) 0.073(19) Uiso 1 d . . H4 H 0.2471(61) 0.2352(49) 0.5684(54) 0.061(18) Uiso 1 d . . H8 H 0.0662(68) 0.2970(57) 0.6578(60) 0.074(22) Uiso 1 d . . H9 H -0.0641(81) 0.3930(65) 0.5679(72) 0.101(27) Uiso 1 d . . H10 H -0.0252(59) 0.5578(46) 0.6223(52) 0.056(17) Uiso 1 d . . H11 H 0.1358(63) 0.6367(54) 0.7692(56) 0.068(20) Uiso 1 d . . H21 H 0.1845(54) 0.1240(44) 0.8673(51) 0.050(16) Uiso 1 d . . H22 H 0.0133(68) 0.0665(56) 0.9345(60) 0.080(21) Uiso 1 d . . H23 H -0.0070(63) 0.1598(48) 1.1235(53) 0.062(18) Uiso 1 d . . H24 H 0.1427(62) 0.2838(51) 1.2241(57) 0.063(20) Uiso 1 d . . H28 H 0.3545(75) 0.5765(60) 1.2625(69) 0.093(25) Uiso 1 d . . H29 H 0.3365(73) 0.6813(65) 1.4399(66) 0.089(24) Uiso 1 d . . H30 H 0.3167(66) 0.6114(55) 1.5914(62) 0.080(20) Uiso 1 d . . H31 H 0.3254(86) 0.4160(69) 1.5143(76) 0.103(32) Uiso 1 d . . HO21 H 0.5445(46) 0.3868(37) 0.9028(41) 0.019(14) Uiso 1 d . . loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O21 Co1 N2 91.5(2) . . ? O21 Co1 N12 92.2(2) . . ? N2 Co1 N12 92.2(2) . . ? O21 Co1 N11 174.7(2) . . ? N2 Co1 N11 89.5(2) . . ? N12 Co1 N11 82.6(2) . . ? O21 Co1 N1 89.2(2) . . ? N2 Co1 N1 82.3(2) . . ? N12 Co1 N1 174.3(2) . . ? N11 Co1 N1 96.1(2) . . ? O21 Co1 O31 91.5(2) . . ? N2 Co1 O31 172.10(15) . . ? N12 Co1 O31 95.0(2) . . ? N11 Co1 O31 88.2(2) . . ? N1 Co1 O31 90.4(2) . . ? O21 Co2 O32 93.0(2) . . ? O21 Co2 O1 91.41(15) . 2_667 ? O32 Co2 O1 170.6(2) . 2_667 ? O21 Co2 O11 85.24(14) . . ? O32 Co2 O11 91.6(2) . . ? O1 Co2 O11 97.03(13) 2_667 . ? O21 Co2 OM1 92.7(2) . . ? O32 Co2 OM1 84.0(2) . . ? O1 Co2 OM1 87.6(2) 2_667 . ? O11 Co2 OM1 175.0(2) . . ? O21 Co2 N3 171.6(2) . 2_667 ? O32 Co2 N3 93.9(2) . 2_667 ? O1 Co2 N3 82.46(14) 2_667 2_667 ? O11 Co2 N3 89.75(15) . 2_667 ? OM1 Co2 N3 92.8(2) . 2_667 ? N2 O1 Co2 115.5(3) . 2_667 ? C1 N1 C5 119.7(4) . . ? C1 N1 Co1 126.4(4) . . ? C5 N1 Co1 113.7(3) . . ? O1 N2 C6 122.2(4) . . ? O1 N2 Co1 120.6(3) . . ? C6 N2 Co1 117.1(3) . . ? C11 N3 C7 118.2(5) . . ? C11 N3 Co2 117.8(4) . 2_667 ? C7 N3 Co2 122.9(3) . 2_667 ? N12 O11 Co2 108.6(3) . . ? C21 N11 C25 119.1(4) . . ? C21 N11 Co1 127.9(4) . . ? C25 N11 Co1 113.0(3) . . ? C26 N12 O11 121.1(4) . . ? C26 N12 Co1 116.8(3) . . ? O11 N12 Co1 122.0(3) . . ? Co1 O21 Co2 110.0(2) . . ? C41 O31 Co1 128.3(3) . . ? C41 O32 Co2 128.6(4) . . ? CM1 OM1 Co2 133.7(8) . . ? N1 C1 C2 121.8(6) . . ? C3 C2 C1 118.9(6) . . ? C4 C3 C2 119.7(6) . . ? C3 C4 C5 119.9(6) . . ? N1 C5 C4 119.9(5) . . ? N1 C5 C6 113.0(4) . . ? C4 C5 C6 127.1(5) . . ? N2 C6 C5 113.5(4) . . ? N2 C6 C7 122.7(4) . . ? C5 C6 C7 123.7(4) . . ? N3 C7 C8 121.1(5) . . ? N3 C7 C6 118.4(4) . . ? C8 C7 C6 120.5(5) . . ? C9 C8 C7 119.5(6) . . ? C10 C9 C8 119.6(6) . . ? C9 C10 C11 118.5(6) . . ? N3 C11 C10 123.0(6) . . ? N11 C21 C22 122.9(5) . . ? C21 C22 C23 118.8(5) . . ? C22 C23 C24 119.1(6) . . ? C25 C24 C23 119.8(6) . . ? N11 C25 C24 120.2(5) . . ? N11 C25 C26 113.7(4) . . ? C24 C25 C26 126.0(5) . . ? N12 C26 C25 114.0(4) . . ? N12 C26 C27 123.5(4) . . ? C25 C26 C27 122.4(4) . . ? N13 C27 C28 122.0(5) . . ? N13 C27 C26 117.2(5) . . ? C28 C27 C26 120.7(5) . . ? C27 C28 C29 119.8(7) . . ? C30 C29 C28 117.8(8) . . ? C31 C30 C29 119.5(7) . . ? C30 C31 N13 124.3(8) . . ? C27 N13 C31 116.6(6) . . ? O32 C41 O31 125.8(5) . . ? O32 C41 C42 118.0(5) . . ? O31 C41 C42 116.1(5) . . ? O43 Cl1 O44 102.1(14) . . ? O43 Cl1 O41 120.0(6) . . ? O44 Cl1 O41 102.6(9) . . ? O43 Cl1 O42 113.5(7) . . ? O44 Cl1 O42 98.4(13) . . ? O41 Cl1 O42 115.7(6) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O21 1.887(4) . ? Co1 N2 1.890(4) . ? Co1 N12 1.912(4) . ? Co1 N11 1.932(4) . ? Co1 N1 1.934(4) . ? Co1 O31 1.946(4) . ? Co2 O21 2.035(4) . ? Co2 O32 2.046(4) . ? Co2 O1 2.068(3) 2_667 ? Co2 O11 2.094(3) . ? Co2 OM1 2.113(5) . ? Co2 N3 2.122(4) 2_667 ? O1 N2 1.304(5) . ? O1 Co2 2.068(3) 2_667 ? N1 C1 1.344(7) . ? N1 C5 1.361(7) . ? N2 C6 1.310(6) . ? N3 C11 1.337(7) . ? N3 C7 1.352(6) . ? N3 Co2 2.122(4) 2_667 ? O11 N12 1.331(5) . ? N11 C21 1.332(6) . ? N11 C25 1.359(6) . ? N12 C26 1.282(6) . ? O31 C41 1.272(6) . ? O32 C41 1.237(6) . ? OM1 CM1 1.351(13) . ? C1 C2 1.380(8) . ? C2 C3 1.374(10) . ? C3 C4 1.373(10) . ? C4 C5 1.388(7) . ? C5 C6 1.459(7) . ? C6 C7 1.483(7) . ? C7 C8 1.381(7) . ? C8 C9 1.379(9) . ? C9 C10 1.359(10) . ? C10 C11 1.380(8) . ? C21 C22 1.360(8) . ? C22 C23 1.376(9) . ? C23 C24 1.378(8) . ? C24 C25 1.378(7) . ? C25 C26 1.469(6) . ? C26 C27 1.496(6) . ? C27 N13 1.326(7) . ? C27 C28 1.383(9) . ? C28 C29 1.386(9) . ? C29 C30 1.367(12) . ? C30 C31 1.335(13) . ? C31 N13 1.364(9) . ? C41 C42 1.511(8) . ? Cl1 O43 1.264(8) . ? Cl1 O44 1.329(14) . ? Cl1 O41 1.345(6) . ? Cl1 O42 1.354(11) . ? OM2 CM2 1.26(2) . ? OM3 CM3 1.38(2) . ?
1100749.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $ #$Revision: 176435 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100749.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100749 loop_ _publ_author_name 'Theocharis C. Stamatatos' 'Stavroula Dionyssopoulou' 'Georgios Efthymiou' 'Panayotis Kyritsis' 'Catherine P. Raptopoulou' 'Aris Terzis' 'Ramon Vicente' 'Albert Escuer' 'Spyros P. Perlepes' _publ_section_title ; The First Cobalt Metallacrowns: Preparation and Characterization of Mixed-Valence Cobalt(II/III), Inverse 12-Metallacrown-4 Complexes ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3374 _journal_page_last 3376 _journal_paper_doi 10.1021/ic050208r _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C59.6 H78.4 Co4 F12 N12 O17.6 P2' _chemical_formula_weight 1770.20 _chemical_name_systematic ; ? ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 70.09(1) _cell_angle_beta 80.60(1) _cell_angle_gamma 69.86(1) _cell_formula_units_Z 1 _cell_length_a 11.867(4) _cell_length_b 14.534(6) _cell_length_c 12.289(5) _cell_measurement_reflns_used 25 _cell_measurement_temperature 298 _cell_measurement_theta_max 11.6 _cell_measurement_theta_min 5.4 _cell_volume 1868.5(13) _computing_cell_refinement 'Program LEAST (UCLA Cryst.package C.E.Strouse 1994)' _computing_data_collection 'Program COLLECT (UCLA Cryst.package C.E.Strouse 1994)' _computing_data_reduction 'Program REDUCE (UCLA Cryst.package C.E.Strouse 1994)' _computing_molecular_graphics ORTEP _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _diffrn_ambient_temperature 298 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Crystal Logic Dual Goniometer' _diffrn_measurement_method 'theta-2theta scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0172 _diffrn_reflns_av_sigmaI/netI 0.0606 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 6364 _diffrn_reflns_theta_full 24.25 _diffrn_reflns_theta_max 24.25 _diffrn_reflns_theta_min 1.76 _diffrn_standards_decay_% 0.1 _diffrn_standards_interval_count 97 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.018 _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.575 _exptl_crystal_density_meas 1.56 _exptl_crystal_density_method 'floating method' _exptl_crystal_description parallelipiped _exptl_crystal_F_000 907 _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.629 _refine_diff_density_min -0.694 _refine_diff_density_rms 0.089 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 548 _refine_ls_number_reflns 6046 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.068 _refine_ls_R_factor_all 0.0838 _refine_ls_R_factor_gt 0.0544 _refine_ls_shift/su_max 0.569 _refine_ls_shift/su_mean 0.023 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0673P)^2^+3.2720P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1390 _refine_ls_wR_factor_ref 0.1602 _reflns_number_gt 4376 _reflns_number_total 6046 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic050208rsi20050207_081352.cif _cod_data_source_block pesd185 _cod_original_cell_volume 1868.3(1) _cod_original_formula_sum 'C59.60 H78.40 Co4 F12 N12 O17.60 P2' _cod_database_code 1100749 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co -0.13924(6) 0.10415(5) 0.63492(6) 0.0393(2) Uani 1 1 d . . . Co2 Co 0.16158(6) 0.10824(5) 0.36788(6) 0.0377(2) Uani 1 1 d . . . O1 O 0.0217(3) 0.1228(3) 0.5710(3) 0.0513(9) Uani 1 1 d . . . N1 N 0.0918(4) 0.2369(3) 0.2480(3) 0.0431(10) Uani 1 1 d . . . N2 N 0.0303(4) 0.1676(3) 0.4592(3) 0.0411(9) Uani 1 1 d . . . N3 N -0.2054(4) 0.2619(3) 0.5616(4) 0.0457(10) Uani 1 1 d . . . O11 O 0.1742(3) -0.0915(2) 0.5121(3) 0.0441(8) Uani 1 1 d . . . N11 N 0.2655(4) 0.1515(3) 0.4331(4) 0.0446(10) Uani 1 1 d . . . N12 N 0.2170(3) -0.0142(3) 0.4915(3) 0.0396(9) Uani 1 1 d . . . O21 O -0.3004(3) 0.0947(3) 0.7102(3) 0.0510(9) Uani 1 1 d . . . O22 O -0.2946(3) -0.0674(3) 0.7371(3) 0.0460(8) Uani 1 1 d . . . OM1 O 0.0701(3) 0.0464(3) 0.3174(3) 0.0456(8) Uani 1 1 d . . . OE1 O -0.1016(4) 0.1254(4) 0.7806(4) 0.0744(13) Uani 1 1 d . . . C1 C 0.1292(6) 0.2632(5) 0.1368(5) 0.0560(15) Uani 1 1 d . . . C2 C 0.0598(7) 0.3421(5) 0.0544(6) 0.0682(19) Uani 1 1 d . . . C3 C -0.0540(6) 0.3941(5) 0.0860(5) 0.0657(17) Uani 1 1 d . . . C4 C -0.0940(6) 0.3693(4) 0.2006(5) 0.0538(14) Uani 1 1 d . . . C5 C -0.0188(5) 0.2921(4) 0.2813(4) 0.0442(12) Uani 1 1 d . . . C6 C -0.0476(5) 0.2548(4) 0.4072(4) 0.0424(11) Uani 1 1 d . . . C7 C -0.1495(5) 0.3143(4) 0.4672(4) 0.0473(12) Uani 1 1 d . . . C8 C -0.1861(6) 0.4209(5) 0.4295(6) 0.0617(16) Uani 1 1 d . . . C9 C -0.2866(7) 0.4753(5) 0.4842(6) 0.0720(19) Uani 1 1 d . . . C10 C -0.3427(7) 0.4212(6) 0.5774(7) 0.073(2) Uani 1 1 d . . . C11 C -0.2999(5) 0.3165(5) 0.6132(6) 0.0590(15) Uani 1 1 d . . . C21 C 0.2846(6) 0.2424(5) 0.3941(6) 0.0578(15) Uani 1 1 d . . . C22 C 0.3617(7) 0.2655(6) 0.4459(7) 0.0728(19) Uani 1 1 d . . . C23 C 0.4226(7) 0.1900(6) 0.5393(7) 0.080(2) Uani 1 1 d . . . H23 H 0.4760 0.2032 0.5750 0.10(3) Uiso 1 1 calc R . . C24 C 0.4044(7) 0.0963(6) 0.5789(6) 0.0700(18) Uani 1 1 d . . . C25 C 0.3229(5) 0.0777(4) 0.5263(5) 0.0493(13) Uani 1 1 d . . . C26 C 0.2928(4) -0.0188(4) 0.5612(4) 0.0438(12) Uani 1 1 d . . . C27 C 0.3367(5) -0.1083(5) 0.6632(5) 0.0609(16) Uani 1 1 d . . . C28 C 0.3499(7) -0.2110(5) 0.6651(7) 0.084(2) Uani 1 1 d . . . H28 H 0.3296 -0.2224 0.6019 0.16(2) Uiso 1 1 calc R . . C29 C 0.3934(8) -0.2931(7) 0.7629(8) 0.109(3) Uani 1 1 d . . . H29 H 0.4056 -0.3611 0.7678 0.16(2) Uiso 1 1 calc R . . C30 C 0.4180(10) -0.2654(9) 0.8552(8) 0.133(4) Uani 1 1 d . . . H30 H 0.4390 -0.3152 0.9262 0.16(2) Uiso 1 1 calc R . . C31 C 0.4113(14) -0.1731(9) 0.8408(10) 0.175(7) Uani 1 1 d . . . H31 H 0.4372 -0.1601 0.8999 0.16(2) Uiso 1 1 calc R . . N13 N 0.3702(9) -0.0932(6) 0.7482(6) 0.136(4) Uani 1 1 d . . . C41 C -0.3348(4) 0.0177(4) 0.7594(4) 0.0437(12) Uani 1 1 d . . . C42 C -0.4318(5) 0.0239(5) 0.8529(5) 0.0642(17) Uani 1 1 d . . . H42A H -0.4920 -0.0010 0.8399 0.132(19) Uiso 1 1 calc R . . H42B H -0.4675 0.0941 0.8525 0.132(19) Uiso 1 1 calc R . . H42C H -0.3983 -0.0175 0.9266 0.132(19) Uiso 1 1 calc R . . CM1 C -0.0254(14) 0.0960(11) 0.2438(18) 0.231(9) Uani 1 1 d . . . HM1A H -0.0710 0.0503 0.2532 0.278 Uiso 1 1 calc R . . HM1B H 0.0054 0.1151 0.1649 0.278 Uiso 1 1 calc R . . HM1C H -0.0763 0.1566 0.2626 0.278 Uiso 1 1 calc R . . CE1A C -0.118(2) 0.071(2) 0.878(2) 0.110(7) Uani 0.50 1 d P . . CE2A C -0.1159(18) -0.0190(17) 0.9040(14) 0.099(6) Uani 0.50 1 d P . . CE1B C -0.175(2) 0.130(2) 0.8920(19) 0.125(10) Uani 0.50 1 d P . . CE2B C -0.123(4) 0.123(3) 0.963(3) 0.198(15) Uani 0.50 1 d P . . P1 P 0.38668(16) 0.34844(14) 0.84663(15) 0.0678(5) Uani 1 1 d . . . F1 F 0.3994(5) 0.4558(4) 0.7625(5) 0.1149(17) Uani 1 1 d . . . F2 F 0.2493(4) 0.3899(4) 0.8170(4) 0.0998(14) Uani 1 1 d . . . F3 F 0.4214(5) 0.3051(4) 0.7408(4) 0.1080(16) Uani 1 1 d . . . F4 F 0.3510(6) 0.3930(5) 0.9507(5) 0.152(2) Uani 1 1 d . . . F5 F 0.5236(4) 0.3087(5) 0.8734(5) 0.134(2) Uani 1 1 d . . . F6 F 0.3699(5) 0.2445(4) 0.9292(5) 0.133(2) Uani 1 1 d . . . H1 H 0.196(5) 0.226(4) 0.128(5) 0.053(17) Uiso 1 1 d . . . H2 H 0.083(8) 0.351(6) -0.014(7) 0.11(3) Uiso 1 1 d . . . H3 H -0.105(5) 0.447(5) 0.036(5) 0.064(18) Uiso 1 1 d . . . H4 H -0.168(5) 0.401(4) 0.222(4) 0.045(15) Uiso 1 1 d . . . H8 H -0.145(6) 0.454(5) 0.365(6) 0.07(2) Uiso 1 1 d . . . H9 H -0.310(6) 0.550(5) 0.467(6) 0.08(2) Uiso 1 1 d . . . H10 H -0.400(6) 0.453(5) 0.607(5) 0.059(18) Uiso 1 1 d . . . H11 H -0.336(5) 0.269(4) 0.680(5) 0.054(16) Uiso 1 1 d . . . H21 H 0.242(5) 0.288(4) 0.330(5) 0.045(15) Uiso 1 1 d . . . H22 H 0.369(7) 0.348(6) 0.407(7) 0.11(3) Uiso 1 1 d . . . H24 H 0.446(6) 0.053(5) 0.636(6) 0.07(2) Uiso 1 1 d . . . OM2 O -0.0819(19) 0.8514(15) 0.1264(18) 0.172(7) Uiso 0.50 1 d P . . CM2 C -0.194(3) 0.846(3) 0.197(3) 0.166(11) Uiso 0.50 1 d P . . OM2A O -0.1582(19) 0.9110(17) 0.1817(19) 0.175(7) Uiso 0.50 1 d P . . CM2A C -0.216(4) 0.871(3) 0.121(4) 0.203(15) Uiso 0.50 1 d P . . OM3 O 0.294(2) 0.5322(17) 0.1449(18) 0.192(8) Uiso 0.50 1 d P . . CM3 C 0.263(2) 0.4587(19) 0.154(2) 0.128(7) Uiso 0.50 1 d P . . OM3A O 0.174(2) 0.4956(17) 0.209(2) 0.206(9) Uiso 0.50 1 d P . . CM3A C 0.086(4) 0.495(3) 0.319(4) 0.206(14) Uiso 0.50 1 d P . . OM4 O -0.067(3) 0.649(3) 0.378(3) 0.204(11) Uiso 0.40 1 d P . . CM4 C 0.028(3) 0.676(3) 0.298(3) 0.154(11) Uiso 0.40 1 d P . . OM4A O 0.009(4) 0.570(4) 0.363(4) 0.251(15) Uiso 0.40 1 d P . . CM4A C 0.003(4) 0.614(4) 0.256(4) 0.203(17) Uiso 0.40 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0371(4) 0.0407(4) 0.0361(4) -0.0117(3) 0.0025(3) -0.0092(3) Co2 0.0341(4) 0.0391(4) 0.0368(4) -0.0120(3) 0.0035(3) -0.0096(3) O1 0.047(2) 0.056(2) 0.0317(18) -0.0069(16) 0.0028(15) -0.0013(17) N1 0.046(2) 0.040(2) 0.039(2) -0.0090(18) 0.0052(18) -0.0139(19) N2 0.040(2) 0.039(2) 0.037(2) -0.0095(18) 0.0035(17) -0.0084(18) N3 0.039(2) 0.049(2) 0.046(2) -0.019(2) 0.0027(19) -0.0084(19) O11 0.051(2) 0.0408(19) 0.0391(18) -0.0049(15) -0.0120(15) -0.0161(16) N11 0.042(2) 0.052(3) 0.046(2) -0.021(2) 0.0052(19) -0.019(2) N12 0.035(2) 0.046(2) 0.038(2) -0.0151(18) 0.0019(17) -0.0110(18) O21 0.043(2) 0.047(2) 0.059(2) -0.0193(18) 0.0118(17) -0.0123(17) O22 0.0398(18) 0.048(2) 0.045(2) -0.0154(16) 0.0097(15) -0.0124(16) OM1 0.0407(19) 0.046(2) 0.047(2) -0.0099(16) -0.0089(16) -0.0108(16) OE1 0.076(3) 0.091(3) 0.054(3) -0.019(3) 0.002(2) -0.028(3) C1 0.052(4) 0.054(3) 0.046(3) -0.005(3) 0.011(3) -0.013(3) C2 0.076(4) 0.064(4) 0.044(3) -0.003(3) 0.015(3) -0.018(3) C3 0.074(4) 0.051(3) 0.051(4) 0.001(3) -0.007(3) -0.008(3) C4 0.051(3) 0.049(3) 0.049(3) -0.008(3) -0.002(3) -0.007(3) C5 0.048(3) 0.040(3) 0.040(3) -0.012(2) 0.002(2) -0.011(2) C6 0.045(3) 0.037(3) 0.039(3) -0.011(2) 0.004(2) -0.009(2) C7 0.049(3) 0.045(3) 0.044(3) -0.019(2) -0.001(2) -0.005(2) C8 0.068(4) 0.049(3) 0.058(4) -0.018(3) 0.004(3) -0.007(3) C9 0.087(5) 0.047(4) 0.068(4) -0.027(3) -0.004(4) 0.006(3) C10 0.065(4) 0.070(4) 0.075(5) -0.046(4) 0.012(4) 0.006(3) C11 0.046(3) 0.063(4) 0.067(4) -0.034(3) 0.011(3) -0.008(3) C21 0.057(4) 0.056(4) 0.066(4) -0.021(3) 0.002(3) -0.024(3) C22 0.076(5) 0.073(4) 0.085(5) -0.030(4) -0.001(4) -0.039(4) C23 0.081(5) 0.105(6) 0.080(5) -0.038(4) -0.001(4) -0.054(5) C24 0.069(4) 0.091(5) 0.061(4) -0.019(4) -0.007(3) -0.042(4) C25 0.040(3) 0.067(4) 0.045(3) -0.024(3) 0.006(2) -0.020(3) C26 0.041(3) 0.056(3) 0.034(3) -0.013(2) 0.000(2) -0.016(2) C27 0.056(3) 0.073(4) 0.050(3) -0.004(3) -0.014(3) -0.024(3) C28 0.078(5) 0.067(4) 0.089(5) 0.000(4) -0.032(4) -0.013(4) C29 0.098(6) 0.085(6) 0.121(7) 0.018(5) -0.048(6) -0.032(5) C30 0.166(10) 0.142(9) 0.089(7) 0.033(6) -0.070(7) -0.083(8) C31 0.325(19) 0.112(8) 0.118(8) 0.027(7) -0.142(11) -0.105(11) N13 0.246(11) 0.099(5) 0.087(5) 0.011(4) -0.096(6) -0.085(6) C41 0.032(2) 0.053(3) 0.039(3) -0.013(2) 0.001(2) -0.005(2) C42 0.053(3) 0.078(4) 0.065(4) -0.033(3) 0.020(3) -0.023(3) CM1 0.169(15) 0.149(13) 0.39(3) -0.079(15) -0.052(17) -0.055(11) CE1A 0.088(15) 0.13(2) 0.12(2) -0.049(17) -0.033(14) -0.023(14) CE2A 0.130(16) 0.135(16) 0.060(9) -0.039(10) 0.009(9) -0.075(14) CE1B 0.121(19) 0.17(2) 0.066(12) -0.066(15) 0.008(12) 0.002(16) CE2B 0.25(4) 0.23(4) 0.13(2) -0.10(3) 0.02(3) -0.07(3) P1 0.0582(10) 0.0700(11) 0.0575(10) -0.0198(8) 0.0022(8) -0.0005(8) F1 0.110(4) 0.090(3) 0.135(4) -0.018(3) 0.000(3) -0.039(3) F2 0.063(2) 0.099(3) 0.106(3) -0.012(3) -0.003(2) -0.008(2) F3 0.112(4) 0.125(4) 0.084(3) -0.059(3) 0.003(3) -0.011(3) F4 0.151(5) 0.204(7) 0.111(4) -0.105(5) 0.001(4) -0.014(5) F5 0.070(3) 0.201(6) 0.102(4) -0.040(4) -0.021(3) -0.006(3) F6 0.130(4) 0.089(3) 0.115(4) 0.012(3) 0.013(3) -0.008(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag OM1 Co1 O11 85.71(14) 2_556 2_556 ? OM1 Co1 O21 91.43(15) 2_556 . ? O11 Co1 O21 92.61(15) 2_556 . ? OM1 Co1 O1 91.90(15) 2_556 . ? O11 Co1 O1 92.98(15) 2_556 . ? O21 Co1 O1 173.69(16) . . ? OM1 Co1 OE1 97.13(18) 2_556 . ? O11 Co1 OE1 176.59(17) 2_556 . ? O21 Co1 OE1 89.22(18) . . ? O1 Co1 OE1 85.05(17) . . ? OM1 Co1 N3 172.10(16) 2_556 . ? O11 Co1 N3 87.35(15) 2_556 . ? O21 Co1 N3 92.66(15) . . ? O1 Co1 N3 84.68(15) . . ? OE1 Co1 N3 89.69(19) . . ? N12 Co2 N2 93.28(17) . . ? N12 Co2 OM1 90.30(16) . . ? N2 Co2 OM1 92.96(17) . . ? N12 Co2 O22 93.74(16) . 2_556 ? N2 Co2 O22 171.97(16) . 2_556 ? OM1 Co2 O22 90.89(16) . 2_556 ? N12 Co2 N11 81.73(18) . . ? N2 Co2 N11 89.27(18) . . ? OM1 Co2 N11 171.84(17) . . ? O22 Co2 N11 87.89(17) 2_556 . ? N12 Co2 N1 175.21(17) . . ? N2 Co2 N1 82.12(17) . . ? OM1 Co2 N1 88.60(17) . . ? O22 Co2 N1 90.94(16) 2_556 . ? N11 Co2 N1 99.48(18) . . ? N2 O1 Co1 115.7(3) . . ? C1 N1 C5 119.1(5) . . ? C1 N1 Co2 126.7(4) . . ? C5 N1 Co2 112.8(3) . . ? C6 N2 O1 122.1(4) . . ? C6 N2 Co2 117.7(3) . . ? O1 N2 Co2 120.1(3) . . ? C11 N3 C7 118.0(5) . . ? C11 N3 Co1 119.6(4) . . ? C7 N3 Co1 122.2(3) . . ? N12 O11 Co1 111.3(3) . 2_556 ? C21 N11 C25 120.1(5) . . ? C21 N11 Co2 126.3(4) . . ? C25 N11 Co2 113.5(3) . . ? C26 N12 O11 120.1(4) . . ? C26 N12 Co2 119.0(3) . . ? O11 N12 Co2 120.7(3) . . ? C41 O21 Co1 130.2(3) . . ? C41 O22 Co2 127.7(3) . 2_556 ? CM1 OM1 Co2 127.6(6) . . ? CM1 OM1 Co1 120.5(6) . 2_556 ? Co2 OM1 Co1 111.51(17) . 2_556 ? CE1A OE1 CE1B 38.2(13) . . ? CE1A OE1 Co1 122.5(12) . . ? CE1B OE1 Co1 130.9(12) . . ? N1 C1 C2 122.3(6) . . ? C1 C2 C3 118.9(6) . . ? C2 C3 C4 119.8(6) . . ? C5 C4 C3 119.2(6) . . ? N1 C5 C4 120.6(5) . . ? N1 C5 C6 113.1(4) . . ? C4 C5 C6 126.3(5) . . ? N2 C6 C7 124.3(4) . . ? N2 C6 C5 112.8(4) . . ? C7 C6 C5 122.8(4) . . ? N3 C7 C8 120.9(5) . . ? N3 C7 C6 118.5(4) . . ? C8 C7 C6 120.7(5) . . ? C7 C8 C9 119.4(6) . . ? C10 C9 C8 118.7(6) . . ? C11 C10 C9 119.2(6) . . ? N3 C11 C10 123.8(6) . . ? N11 C21 C22 122.0(6) . . ? C21 C22 C23 118.2(6) . . ? C24 C23 C22 120.0(7) . . ? C23 C24 C25 119.7(7) . . ? N11 C25 C24 119.8(6) . . ? N11 C25 C26 114.6(5) . . ? C24 C25 C26 125.5(6) . . ? N12 C26 C25 111.0(4) . . ? N12 C26 C27 123.4(5) . . ? C25 C26 C27 125.5(5) . . ? N13 C27 C28 120.4(6) . . ? N13 C27 C26 118.2(6) . . ? C28 C27 C26 121.3(6) . . ? C29 C28 C27 119.0(8) . . ? C28 C29 C30 115.1(9) . . ? C31 C30 C29 120.2(8) . . ? C30 C31 N13 125.5(9) . . ? C27 N13 C31 119.2(8) . . ? O21 C41 O22 125.9(5) . . ? O21 C41 C42 118.4(5) . . ? O22 C41 C42 115.7(5) . . ? CE1B CE1A OE1 88(3) . . ? CE1B CE1A CE2A 133(4) . . ? OE1 CE1A CE2A 125(2) . . ? CE1B CE1A CE2B 49(3) . . ? OE1 CE1A CE2B 110(3) . . ? CE2A CE1A CE2B 124(3) . . ? CE1A CE2A CE1B 19.9(16) . . ? CE1A CE1B CE2B 92(4) . . ? CE1A CE1B OE1 54(2) . . ? CE2B CE1B OE1 114(3) . . ? CE1A CE1B CE2A 27(2) . . ? CE2B CE1B CE2A 97(3) . . ? OE1 CE1B CE2A 75.6(12) . . ? CE1B CE2B CE1A 39.3(17) . . ? F4 P1 F6 89.2(4) . . ? F4 P1 F3 179.2(4) . . ? F6 P1 F3 91.4(3) . . ? F4 P1 F5 91.3(3) . . ? F6 P1 F5 90.8(3) . . ? F3 P1 F5 89.2(3) . . ? F4 P1 F2 89.3(3) . . ? F6 P1 F2 90.3(3) . . ? F3 P1 F2 90.1(3) . . ? F5 P1 F2 178.8(3) . . ? F4 P1 F1 90.4(4) . . ? F6 P1 F1 178.3(3) . . ? F3 P1 F1 89.1(3) . . ? F5 P1 F1 90.9(3) . . ? F2 P1 F1 88.1(3) . . ? OM2A OM2 CM2 46.7(15) . . ? OM2A OM2 CM2A 61.2(19) . . ? CM2 OM2 CM2A 36.0(18) . . ? CM2A CM2 OM2A 90(4) . . ? CM2A CM2 OM2 75(4) . . ? OM2A CM2 OM2 58(2) . . ? CM2 OM2A OM2 75(2) . . ? CM2 OM2A CM2A 40(2) . . ? OM2 OM2A CM2A 67.0(19) . . ? CM2 CM2A OM2A 50(3) . . ? CM2 CM2A OM2 69(4) . . ? OM2A CM2A OM2 51.8(17) . . ? CM3 OM3 OM3A 46.6(15) . . ? OM3A CM3 OM3 87(2) . . ? CM3 OM3A CM3A 154(3) . . ? CM3 OM3A OM3 46.3(15) . . ? CM3A OM3A OM3 142(2) . . ? OM4A CM3A OM3A 135(4) . . ? OM4A CM3A CM4A 48(2) . . ? OM3A CM3A CM4A 92(3) . . ? OM4A OM4 CM4 70(3) . . ? OM4A OM4 CM4A 46(2) . . ? CM4 OM4 CM4A 48(2) . . ? CM4A CM4 OM4 78(3) . . ? CM4A CM4 OM4A 51(3) . . ? OM4 CM4 OM4A 49(2) . . ? CM4A OM4A OM4 88(4) . . ? CM4A OM4A CM3A 77(4) . . ? OM4 OM4A CM3A 166(5) . . ? CM4A OM4A CM4 55(3) . . ? OM4 OM4A CM4 61(3) . . ? CM3A OM4A CM4 111(4) . . ? OM4A CM4A CM4 74(4) . . ? OM4A CM4A OM4 45(3) . . ? CM4 CM4A OM4 54(2) . . ? OM4A CM4A CM3A 55(3) . . ? CM4 CM4A CM3A 108(4) . . ? OM4 CM4A CM3A 100(3) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 OM1 1.962(4) 2_556 ? Co1 O11 1.999(3) 2_556 ? Co1 O21 2.012(4) . ? Co1 O1 2.015(4) . ? Co1 OE1 2.058(5) . ? Co1 N3 2.066(4) . ? Co2 N12 1.894(4) . ? Co2 N2 1.896(4) . ? Co2 OM1 1.908(4) . ? Co2 O22 1.929(3) 2_556 ? Co2 N11 1.938(4) . ? Co2 N1 1.951(4) . ? O1 N2 1.309(5) . ? N1 C1 1.333(7) . ? N1 C5 1.362(6) . ? N2 C6 1.305(6) . ? N3 C11 1.336(7) . ? N3 C7 1.365(7) . ? O11 N12 1.318(5) . ? O11 Co1 1.999(3) 2_556 ? N11 C21 1.329(7) . ? N11 C25 1.357(7) . ? N12 C26 1.312(6) . ? O21 C41 1.248(6) . ? O22 C41 1.269(6) . ? O22 Co2 1.929(3) 2_556 ? OM1 CM1 1.397(16) . ? OM1 Co1 1.962(4) 2_556 ? OE1 CE1A 1.22(3) . ? OE1 CE1B 1.50(2) . ? C1 C2 1.360(9) . ? C2 C3 1.368(9) . ? C3 C4 1.376(8) . ? C4 C5 1.371(7) . ? C5 C6 1.479(7) . ? C6 C7 1.476(7) . ? C7 C8 1.384(8) . ? C8 C9 1.396(9) . ? C9 C10 1.367(10) . ? C10 C11 1.361(9) . ? C21 C22 1.379(9) . ? C22 C23 1.382(10) . ? C23 C24 1.362(10) . ? C24 C25 1.389(8) . ? C25 C26 1.470(7) . ? C26 C27 1.473(7) . ? C27 N13 1.284(9) . ? C27 C28 1.439(10) . ? C28 C29 1.392(10) . ? C29 C30 1.425(14) . ? C30 C31 1.268(14) . ? C31 N13 1.331(11) . ? C41 C42 1.490(7) . ? CE1A CE1B 0.93(3) . ? CE1A CE2A 1.23(3) . ? CE1A CE2B 1.47(4) . ? CE2A CE1B 1.99(4) . ? CE1B CE2B 1.11(4) . ? P1 F4 1.560(5) . ? P1 F6 1.564(5) . ? P1 F3 1.569(5) . ? P1 F5 1.576(5) . ? P1 F2 1.587(4) . ? P1 F1 1.593(5) . ? OM2 OM2A 1.30(2) . ? OM2 CM2 1.48(4) . ? OM2 CM2A 1.52(4) . ? CM2 CM2A 0.93(5) . ? CM2 OM2A 1.11(3) . ? OM2A CM2A 1.45(4) . ? OM3 CM3 1.21(3) . ? OM3 OM3A 1.67(3) . ? CM3 OM3A 1.22(3) . ? OM3A CM3A 1.56(4) . ? CM3A OM4A 1.38(5) . ? CM3A CM4A 1.65(6) . ? OM4 OM4A 1.23(4) . ? OM4 CM4 1.44(4) . ? OM4 CM4A 1.73(6) . ? CM4 CM4A 1.31(5) . ? CM4 OM4A 1.54(5) . ? OM4A CM4A 1.25(5) . ?
1100750.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100750.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100750 loop_ _publ_author_name 'Xunhua Mo' 'Erin Ferguson' 'Shiou-Jyh Hwu' _publ_section_title ; Salt-Inclusion Synthesis of Two New Polar Solids, Ba6Mn4Si12O34Cl3 and Ba6Fe5Si11O34Cl3 ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3121 _journal_page_last 3126 _journal_paper_doi 10.1021/ic050228t _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'Ba6 Cl3 Mn4 O34 Si12' _chemical_formula_weight 2031.23 _chemical_name_systematic ; ? ; _space_group_IT_number 26 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'P 2c -2' _symmetry_space_group_name_H-M 'P m c 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 1 _cell_length_a 6.8211(14) _cell_length_b 9.6203(19) _cell_length_c 13.172(3) _cell_measurement_temperature 293(2) _cell_volume 864.4(3) _computing_cell_refinement 'Bruker XSCANS' _computing_data_collection 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0641 _diffrn_reflns_av_sigmaI/netI 0.0481 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 8188 _diffrn_reflns_theta_full 26.47 _diffrn_reflns_theta_max 26.47 _diffrn_reflns_theta_min 3.66 _exptl_absorpt_coefficient_mu 8.890 _exptl_absorpt_correction_T_max 0.8422 _exptl_absorpt_correction_T_min 0.2242 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ;Jacobson, R.A. REQAB, subroutine of Crystal Clear;Rigaku/MSC: The Woodlands, TX, 1999. ; _exptl_crystal_colour orange _exptl_crystal_density_diffrn 3.902 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 927 _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _refine_diff_density_max 2.587 _refine_diff_density_min -1.101 _refine_diff_density_rms 0.225 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.04(4) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 158 _refine_ls_number_reflns 1936 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.001 _refine_ls_R_factor_all 0.0474 _refine_ls_R_factor_gt 0.0405 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0407P)^2^+10.3635P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0868 _refine_ls_wR_factor_ref 0.0906 _reflns_number_gt 1769 _reflns_number_total 1936 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic050228tsi20050214_023827_1.cif _cod_data_source_block Ba6Mn4Si12O34Cl3(1) _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_database_code 1100750 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x, -y, z+1/2' '-x, y, z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ba1 Ba 0.0000 0.64346(9) 0.02471(7) 0.0172(2) Uani 1 2 d S . . Ba2 Ba -0.5000 0.97244(11) 0.07799(8) 0.0272(3) Uani 1 2 d S . . Ba3 Ba -0.5000 0.50960(13) -0.24520(12) 0.0378(4) Uani 1 2 d S . . Mn1 Mn 0.0000 1.0190(2) -0.01459(18) 0.0167(5) Uani 1 2 d S . . Mn2 Mn 0.0000 0.3689(2) 0.20921(17) 0.0118(5) Uani 1 2 d S . . Si1 Si -0.2689(4) 0.8429(3) -0.1703(2) 0.0121(6) Uani 1 1 d . . . Si2 Si -0.7326(4) 1.3011(3) 0.0141(2) 0.0132(6) Uani 1 1 d . . . Si3 Si -1.0000 1.3291(4) -0.1634(3) 0.0107(8) Uani 1 2 d S . . Si4 Si 0.0000 1.0482(4) -0.2737(3) 0.0106(8) Uani 1 2 d S . . O1 O -0.7999(11) 1.1433(7) 0.0240(7) 0.0240(15) Uani 1 1 d . . . O2 O -0.5000 0.838(2) -0.1951(16) 0.061(5) Uiso 1 2 d S . . O3 O 0.0000 0.8874(11) 0.1159(9) 0.029(3) Uani 1 2 d S . . O4 O -0.1933(13) 0.9500(9) -0.2577(6) 0.033(2) Uani 1 1 d . . . O5 O 0.0000 1.1591(11) -0.1792(8) 0.011(2) Uiso 1 2 d S . . O6 O -0.1999(18) 0.8925(9) -0.0633(6) 0.044(3) Uani 1 1 d . . . O7 O -0.2012(18) 0.6883(9) -0.1929(9) 0.054(3) Uani 1 1 d . . . O8 O -1.0000 1.4145(11) -0.2650(8) 0.021(2) Uani 1 2 d S . . O9 O -0.5000 1.3006(15) 0.0080(14) 0.052(5) Uani 1 2 d S . . O10 O -0.7977(15) 1.3978(9) 0.1070(7) 0.036(2) Uani 1 1 d . . . O11 O -0.8131(17) 1.3688(8) -0.0921(7) 0.040(3) Uani 1 1 d . . . Cl1 Cl -0.5000 0.1987(10) -0.2314(8) 0.034(2) Uani 0.50 2 d SP . . Cl2 Cl -0.5000 0.6776(16) 0.086(2) 0.035(5) Uani 0.34(4) 2 d SP . . Cl3 Cl -0.5000 0.6439(12) 0.0218(15) 0.042(5) Uani 0.66(4) 2 d SP . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ba1 0.0256(5) 0.0103(4) 0.0156(4) -0.0005(4) 0.000 0.000 Ba2 0.0182(5) 0.0324(6) 0.0311(6) 0.0019(5) 0.000 0.000 Ba3 0.0189(5) 0.0226(5) 0.0718(10) 0.0058(6) 0.000 0.000 Mn1 0.0277(12) 0.0079(10) 0.0145(11) -0.0003(9) 0.000 0.000 Mn2 0.0147(11) 0.0112(11) 0.0095(11) 0.0023(8) 0.000 0.000 Si1 0.0056(13) 0.0156(14) 0.0152(13) -0.0025(11) -0.0017(11) -0.0031(11) Si2 0.0095(12) 0.0144(12) 0.0157(14) 0.0015(13) 0.0008(12) 0.0004(10) Si3 0.019(2) 0.0071(18) 0.0056(17) -0.0019(13) 0.000 0.000 Si4 0.0116(18) 0.0099(17) 0.0102(18) -0.0005(15) 0.000 0.000 O1 0.031(4) 0.019(3) 0.022(3) 0.006(3) -0.002(4) -0.005(3) O3 0.060(9) 0.006(5) 0.022(6) 0.001(4) 0.000 0.000 O4 0.037(5) 0.042(5) 0.018(4) 0.002(4) 0.001(4) -0.028(4) O6 0.093(8) 0.026(5) 0.013(4) 0.007(3) -0.014(5) -0.026(5) O7 0.068(8) 0.020(4) 0.075(8) -0.023(5) 0.050(7) -0.019(5) O8 0.037(7) 0.017(5) 0.009(5) -0.006(4) 0.000 0.000 O9 0.004(5) 0.063(9) 0.088(13) -0.039(10) 0.000 0.000 O10 0.037(5) 0.030(5) 0.040(6) -0.009(4) 0.022(4) -0.001(4) O11 0.063(7) 0.016(4) 0.039(5) 0.019(4) -0.030(5) -0.015(4) Cl1 0.033(5) 0.021(4) 0.047(6) -0.008(4) 0.000 0.000 Cl2 0.051(9) 0.021(7) 0.033(13) -0.007(7) 0.000 0.000 Cl3 0.024(3) 0.030(5) 0.073(13) 0.030(7) 0.000 0.000 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Ba1 O8 74.3(3) . 2_475 ? O3 Ba1 O10 123.1(3) . 4_445 ? O8 Ba1 O10 58.7(2) 2_475 4_445 ? O3 Ba1 O10 123.1(3) . 1_645 ? O8 Ba1 O10 58.7(2) 2_475 1_645 ? O10 Ba1 O10 55.9(4) 4_445 1_645 ? O3 Ba1 O6 57.6(3) . 4 ? O8 Ba1 O6 122.6(3) 2_475 4 ? O10 Ba1 O6 178.7(3) 4_445 4 ? O10 Ba1 O6 124.9(3) 1_645 4 ? O3 Ba1 O6 57.6(3) . . ? O8 Ba1 O6 122.6(3) 2_475 . ? O10 Ba1 O6 124.9(3) 4_445 . ? O10 Ba1 O6 178.7(3) 1_645 . ? O6 Ba1 O6 54.3(4) 4 . ? O3 Ba1 O7 106.7(3) . . ? O8 Ba1 O7 154.52(19) 2_475 . ? O10 Ba1 O7 103.7(2) 4_445 . ? O10 Ba1 O7 129.6(2) 1_645 . ? O6 Ba1 O7 75.0(3) 4 . ? O6 Ba1 O7 49.5(2) . . ? O3 Ba1 O7 106.7(3) . 4 ? O8 Ba1 O7 154.52(19) 2_475 4 ? O10 Ba1 O7 129.6(2) 4_445 4 ? O10 Ba1 O7 103.7(2) 1_645 4 ? O6 Ba1 O7 49.5(2) 4 4 ? O6 Ba1 O7 75.0(3) . 4 ? O7 Ba1 O7 50.7(4) . 4 ? O3 Ba1 O11 157.17(18) . 4_445 ? O8 Ba1 O11 107.3(2) 2_475 4_445 ? O10 Ba1 O11 49.5(2) 4_445 4_445 ? O10 Ba1 O11 73.2(2) 1_645 4_445 ? O6 Ba1 O11 129.4(2) 4 4_445 ? O6 Ba1 O11 106.5(2) . 4_445 ? O7 Ba1 O11 61.8(2) . 4_445 ? O7 Ba1 O11 81.8(2) 4 4_445 ? O3 Ba1 O11 157.17(18) . 1_645 ? O8 Ba1 O11 107.3(2) 2_475 1_645 ? O10 Ba1 O11 73.2(2) 4_445 1_645 ? O10 Ba1 O11 49.5(2) 1_645 1_645 ? O6 Ba1 O11 106.5(2) 4 1_645 ? O6 Ba1 O11 129.4(2) . 1_645 ? O7 Ba1 O11 81.8(2) . 1_645 ? O7 Ba1 O11 61.8(2) 4 1_645 ? O11 Ba1 O11 45.3(4) 4_445 1_645 ? O3 Ba1 Cl3 90.2(3) . 1_655 ? O8 Ba1 Cl3 90.6(3) 2_475 1_655 ? O10 Ba1 Cl3 118.3(2) 4_445 1_655 ? O10 Ba1 Cl3 62.4(2) 1_645 1_655 ? O6 Ba1 Cl3 62.5(2) 4 1_655 ? O6 Ba1 Cl3 116.8(2) . 1_655 ? O7 Ba1 Cl3 114.7(4) . 1_655 ? O7 Ba1 Cl3 64.0(4) 4 1_655 ? O11 Ba1 Cl3 112.4(4) 4_445 1_655 ? O11 Ba1 Cl3 67.1(4) 1_645 1_655 ? O3 Ba1 Cl3 90.2(3) . . ? O8 Ba1 Cl3 90.6(3) 2_475 . ? O10 Ba1 Cl3 62.4(2) 4_445 . ? O10 Ba1 Cl3 118.3(2) 1_645 . ? O6 Ba1 Cl3 116.8(2) 4 . ? O6 Ba1 Cl3 62.5(2) . . ? O7 Ba1 Cl3 64.0(4) . . ? O7 Ba1 Cl3 114.7(4) 4 . ? O11 Ba1 Cl3 67.1(4) 4_445 . ? O11 Ba1 Cl3 112.4(4) 1_645 . ? Cl3 Ba1 Cl3 178.7(6) 1_655 . ? O1 Ba2 O1 97.6(3) 4_455 . ? O1 Ba2 Cl2 127.9(2) 4_455 . ? O1 Ba2 Cl2 127.9(2) . . ? O1 Ba2 O6 121.9(3) 4_455 4_455 ? O1 Ba2 O6 57.1(2) . 4_455 ? Cl2 Ba2 O6 75.9(4) . 4_455 ? O1 Ba2 O6 57.1(2) 4_455 . ? O1 Ba2 O6 121.9(3) . . ? Cl2 Ba2 O6 75.9(4) . . ? O6 Ba2 O6 90.9(4) 4_455 . ? O1 Ba2 Cl1 123.4(2) 4_455 2_465 ? O1 Ba2 Cl1 123.4(2) . 2_465 ? Cl2 Ba2 Cl1 54.6(6) . 2_465 ? O6 Ba2 Cl1 113.3(2) 4_455 2_465 ? O6 Ba2 Cl1 113.3(2) . 2_465 ? O1 Ba2 O4 61.9(3) 4_455 3_575 ? O1 Ba2 O4 123.0(2) . 3_575 ? Cl2 Ba2 O4 102.4(4) . 3_575 ? O6 Ba2 O4 176.1(3) 4_455 3_575 ? O6 Ba2 O4 92.1(2) . 3_575 ? Cl1 Ba2 O4 63.2(2) 2_465 3_575 ? O1 Ba2 O4 123.0(2) 4_455 2_475 ? O1 Ba2 O4 61.9(3) . 2_475 ? Cl2 Ba2 O4 102.4(4) . 2_475 ? O6 Ba2 O4 92.1(2) 4_455 2_475 ? O6 Ba2 O4 176.1(3) . 2_475 ? Cl1 Ba2 O4 63.2(2) 2_465 2_475 ? O4 Ba2 O4 84.8(3) 3_575 2_475 ? O1 Ba2 Cl3 122.0(2) 4_455 . ? O1 Ba2 Cl3 122.0(2) . . ? Cl2 Ba2 Cl3 15.3(4) . . ? O6 Ba2 Cl3 65.9(3) 4_455 . ? O6 Ba2 Cl3 65.9(3) . . ? Cl1 Ba2 Cl3 69.9(4) 2_465 . ? O4 Ba2 Cl3 113.2(3) 3_575 . ? O4 Ba2 Cl3 113.2(3) 2_475 . ? O1 Ba2 O9 49.17(16) 4_455 . ? O1 Ba2 O9 49.17(16) . . ? Cl2 Ba2 O9 165.9(6) . . ? O6 Ba2 O9 94.3(3) 4_455 . ? O6 Ba2 O9 94.3(3) . . ? Cl1 Ba2 O9 139.5(4) 2_465 . ? O4 Ba2 O9 88.0(3) 3_575 . ? O4 Ba2 O9 88.0(3) 2_475 . ? Cl3 Ba2 O9 150.5(4) . . ? O1 Ba2 Si2 23.85(16) 4_455 4_455 ? O1 Ba2 Si2 75.05(16) . 4_455 ? Cl2 Ba2 Si2 151.4(2) . 4_455 ? O6 Ba2 Si2 113.21(18) 4_455 4_455 ? O6 Ba2 Si2 76.82(17) . 4_455 ? Cl1 Ba2 Si2 132.09(16) 2_465 4_455 ? O4 Ba2 Si2 69.99(17) 3_575 4_455 ? O4 Ba2 Si2 104.27(16) 2_475 4_455 ? Cl3 Ba2 Si2 142.6(2) . 4_455 ? O9 Ba2 Si2 25.91(4) . 4_455 ? O1 Ba2 Si2 75.05(16) 4_455 . ? O1 Ba2 Si2 23.85(16) . . ? Cl2 Ba2 Si2 151.4(2) . . ? O6 Ba2 Si2 76.82(17) 4_455 . ? O6 Ba2 Si2 113.21(18) . . ? Cl1 Ba2 Si2 132.09(16) 2_465 . ? O4 Ba2 Si2 104.27(16) 3_575 . ? O4 Ba2 Si2 69.99(17) 2_475 . ? Cl3 Ba2 Si2 142.6(2) . . ? O9 Ba2 Si2 25.91(4) . . ? Si2 Ba2 Si2 51.75(8) 4_455 . ? O7 Ba3 O7 95.5(5) . 4_455 ? O7 Ba3 Cl2 126.0(3) . 2_464 ? O7 Ba3 Cl2 126.0(3) 4_455 2_464 ? O7 Ba3 O10 119.1(3) . 3_574 ? O7 Ba3 O10 57.8(3) 4_455 3_574 ? Cl2 Ba3 O10 71.2(4) 2_464 3_574 ? O7 Ba3 O10 57.8(3) . 2_474 ? O7 Ba3 O10 119.1(3) 4_455 2_474 ? Cl2 Ba3 O10 71.2(4) 2_464 2_474 ? O10 Ba3 O10 87.0(3) 3_574 2_474 ? O7 Ba3 Cl1 127.4(3) . . ? O7 Ba3 Cl1 127.4(3) 4_455 . ? Cl2 Ba3 Cl1 54.5(5) 2_464 . ? O10 Ba3 Cl1 110.0(2) 3_574 . ? O10 Ba3 Cl1 110.0(2) 2_474 . ? O7 Ba3 O2 48.5(2) . . ? O7 Ba3 O2 48.5(2) 4_455 . ? Cl2 Ba3 O2 140.8(6) 2_464 . ? O10 Ba3 O2 80.8(3) 3_574 . ? O10 Ba3 O2 80.8(3) 2_474 . ? Cl1 Ba3 O2 164.7(4) . . ? O7 Ba3 O11 67.5(3) . 4_445 ? O7 Ba3 O11 126.5(3) 4_455 4_445 ? Cl2 Ba3 O11 102.7(4) 2_464 4_445 ? O10 Ba3 O11 172.8(3) 3_574 4_445 ? O10 Ba3 O11 94.8(2) 2_474 4_445 ? Cl1 Ba3 O11 62.9(2) . 4_445 ? O2 Ba3 O11 106.4(3) . 4_445 ? O7 Ba3 O11 126.5(3) . 1_545 ? O7 Ba3 O11 67.5(3) 4_455 1_545 ? Cl2 Ba3 O11 102.7(4) 2_464 1_545 ? O10 Ba3 O11 94.8(2) 3_574 1_545 ? O10 Ba3 O11 172.8(3) 2_474 1_545 ? Cl1 Ba3 O11 62.9(2) . 1_545 ? O2 Ba3 O11 106.4(3) . 1_545 ? O11 Ba3 O11 82.6(3) 4_445 1_545 ? O7 Ba3 Cl3 119.7(3) . 2_464 ? O7 Ba3 Cl3 119.7(3) 4_455 2_464 ? Cl2 Ba3 Cl3 13.3(3) 2_464 2_464 ? O10 Ba3 Cl3 62.4(3) 3_574 2_464 ? O10 Ba3 Cl3 62.4(3) 2_474 2_464 ? Cl1 Ba3 Cl3 67.8(4) . 2_464 ? O2 Ba3 Cl3 127.5(5) . 2_464 ? O11 Ba3 Cl3 112.3(3) 4_445 2_464 ? O11 Ba3 Cl3 112.3(3) 1_545 2_464 ? O7 Ba3 Mn2 31.9(2) . 2_564 ? O7 Ba3 Mn2 122.1(3) 4_455 2_564 ? Cl2 Ba3 Mn2 94.23(17) 2_464 2_564 ? O10 Ba3 Mn2 115.93(17) 3_574 2_564 ? O10 Ba3 Mn2 32.10(17) 2_474 2_564 ? Cl1 Ba3 Mn2 109.22(5) . 2_564 ? O2 Ba3 Mn2 73.77(10) . 2_564 ? O11 Ba3 Mn2 67.69(17) 4_445 2_564 ? O11 Ba3 Mn2 148.48(17) 1_545 2_564 ? Cl3 Ba3 Mn2 89.46(11) 2_464 2_564 ? O7 Ba3 Mn2 122.1(3) . 2_464 ? O7 Ba3 Mn2 31.9(2) 4_455 2_464 ? Cl2 Ba3 Mn2 94.23(17) 2_464 2_464 ? O10 Ba3 Mn2 32.10(17) 3_574 2_464 ? O10 Ba3 Mn2 115.93(17) 2_474 2_464 ? Cl1 Ba3 Mn2 109.22(5) . 2_464 ? O2 Ba3 Mn2 73.77(10) . 2_464 ? O11 Ba3 Mn2 148.48(17) 4_445 2_464 ? O11 Ba3 Mn2 67.69(17) 1_545 2_464 ? Cl3 Ba3 Mn2 89.46(11) 2_464 2_464 ? Mn2 Ba3 Mn2 137.85(8) 2_564 2_464 ? O1 Mn1 O1 92.8(5) 1_655 4_455 ? O1 Mn1 O6 176.3(4) 1_655 . ? O1 Mn1 O6 88.8(4) 4_455 . ? O1 Mn1 O6 88.8(4) 1_655 4 ? O1 Mn1 O6 176.3(4) 4_455 4 ? O6 Mn1 O6 89.5(7) . 4 ? O1 Mn1 O3 99.2(3) 1_655 . ? O1 Mn1 O3 99.2(3) 4_455 . ? O6 Mn1 O3 83.9(3) . . ? O6 Mn1 O3 83.9(3) 4 . ? O1 Mn1 Ba1 126.2(2) 1_655 . ? O1 Mn1 Ba1 126.2(2) 4_455 . ? O6 Mn1 Ba1 54.9(3) . . ? O6 Mn1 Ba1 54.9(3) 4 . ? O3 Mn1 Ba1 45.5(3) . . ? O1 Mn1 Ba2 46.4(2) 1_655 1_655 ? O1 Mn1 Ba2 131.7(3) 4_455 1_655 ? O6 Mn1 Ba2 133.7(3) . 1_655 ? O6 Mn1 Ba2 51.4(3) 4 1_655 ? O3 Mn1 Ba2 70.01(5) . 1_655 ? Ba1 Mn1 Ba2 80.28(4) . 1_655 ? O1 Mn1 Ba2 131.7(3) 1_655 . ? O1 Mn1 Ba2 46.4(2) 4_455 . ? O6 Mn1 Ba2 51.4(3) . . ? O6 Mn1 Ba2 133.7(3) 4 . ? O3 Mn1 Ba2 70.01(5) . . ? Ba1 Mn1 Ba2 80.28(4) . . ? Ba2 Mn1 Ba2 138.29(7) 1_655 . ? O10 Mn2 O10 90.2(6) 4_445 1_645 ? O10 Mn2 O7 171.9(4) 4_445 2_565 ? O10 Mn2 O7 89.9(5) 1_645 2_565 ? O10 Mn2 O7 89.9(5) 4_445 3_565 ? O10 Mn2 O7 171.9(4) 1_645 3_565 ? O7 Mn2 O7 88.8(8) 2_565 3_565 ? O10 Mn2 O8 88.3(3) 4_445 2_475 ? O10 Mn2 O8 88.3(3) 1_645 2_475 ? O7 Mn2 O8 99.8(4) 2_565 2_475 ? O7 Mn2 O8 99.8(4) 3_565 2_475 ? O10 Mn2 Ba1 55.0(3) 4_445 . ? O10 Mn2 Ba1 55.0(3) 1_645 . ? O7 Mn2 Ba1 130.6(3) 2_565 . ? O7 Mn2 Ba1 130.6(3) 3_565 . ? O8 Mn2 Ba1 51.9(3) 2_475 . ? O10 Mn2 Ba3 136.8(3) 4_445 2_565 ? O10 Mn2 Ba3 53.6(3) 1_645 2_565 ? O7 Mn2 Ba3 47.8(3) 2_565 2_565 ? O7 Mn2 Ba3 129.4(4) 3_565 2_565 ? O8 Mn2 Ba3 69.99(5) 2_475 2_565 ? Ba1 Mn2 Ba3 82.87(4) . 2_565 ? O10 Mn2 Ba3 53.6(3) 4_445 2_465 ? O10 Mn2 Ba3 136.8(3) 1_645 2_465 ? O7 Mn2 Ba3 129.4(4) 2_565 2_465 ? O7 Mn2 Ba3 47.8(3) 3_565 2_465 ? O8 Mn2 Ba3 69.99(5) 2_475 2_465 ? Ba1 Mn2 Ba3 82.87(4) . 2_465 ? Ba3 Mn2 Ba3 137.85(8) 2_565 2_465 ? O6 Si1 O7 111.6(6) . . ? O6 Si1 O2 119.2(9) . . ? O7 Si1 O2 102.6(8) . . ? O6 Si1 O4 110.4(4) . . ? O7 Si1 O4 111.6(5) . . ? O2 Si1 O4 100.7(8) . . ? O6 Si1 Ba1 51.8(4) . . ? O7 Si1 Ba1 59.9(5) . . ? O2 Si1 Ba1 127.7(7) . . ? O4 Si1 Ba1 131.5(4) . . ? O6 Si1 Ba3 129.3(3) . . ? O7 Si1 Ba3 42.5(5) . . ? O2 Si1 Ba3 60.2(7) . . ? O4 Si1 Ba3 119.6(3) . . ? Ba1 Si1 Ba3 86.97(7) . . ? O6 Si1 Ba2 41.9(5) . . ? O7 Si1 Ba2 125.8(4) . . ? O2 Si1 Ba2 77.4(7) . . ? O4 Si1 Ba2 121.8(3) . . ? Ba1 Si1 Ba2 77.30(6) . . ? Ba3 Si1 Ba2 109.46(8) . . ? O9 Si2 O1 106.8(6) . . ? O9 Si2 O10 108.6(7) . . ? O1 Si2 O10 114.3(5) . . ? O9 Si2 O11 107.0(8) . . ? O1 Si2 O11 110.6(5) . . ? O10 Si2 O11 109.2(5) . . ? O9 Si2 Ba2 64.7(6) . . ? O1 Si2 Ba2 43.7(3) . . ? O10 Si2 Ba2 116.7(4) . . ? O11 Si2 Ba2 133.6(4) . . ? O9 Si2 Ba1 119.2(6) . 1_465 ? O1 Si2 Ba1 133.7(3) . 1_465 ? O10 Si2 Ba1 47.9(4) . 1_465 ? O11 Si2 Ba1 61.4(4) . 1_465 ? Ba2 Si2 Ba1 164.33(10) . 1_465 ? O8 Si3 O11 111.6(4) . . ? O8 Si3 O11 111.6(4) . 4_355 ? O11 Si3 O11 103.0(8) . 4_355 ? O8 Si3 O5 114.3(6) . 1_455 ? O11 Si3 O5 107.8(4) . 1_455 ? O11 Si3 O5 107.8(4) 4_355 1_455 ? O3 Si4 O4 110.2(4) 2_574 . ? O3 Si4 O4 110.2(4) 2_574 4 ? O4 Si4 O4 107.4(7) . 4 ? O3 Si4 O5 116.3(6) 2_574 . ? O4 Si4 O5 106.1(4) . . ? O4 Si4 O5 106.1(4) 4 . ? Si2 O1 Mn1 142.4(5) . 1_455 ? Si2 O1 Ba2 112.4(4) . . ? Mn1 O1 Ba2 103.4(3) 1_455 . ? Si1 O2 Si1 156.3(15) . 4_455 ? Si1 O2 Ba3 94.1(7) . . ? Si1 O2 Ba3 94.1(7) 4_455 . ? Si4 O3 Mn1 120.6(6) 2_575 . ? Si4 O3 Ba1 140.2(6) 2_575 . ? Mn1 O3 Ba1 99.3(4) . . ? Si1 O4 Si4 135.4(6) . . ? Si1 O4 Ba2 115.6(4) . 2_474 ? Si4 O4 Ba2 108.3(4) . 2_474 ? Si4 O5 Si3 137.8(7) . 1_655 ? Si1 O6 Mn1 134.7(6) . . ? Si1 O6 Ba2 116.9(6) . . ? Mn1 O6 Ba2 96.8(4) . . ? Si1 O6 Ba1 104.1(5) . . ? Mn1 O6 Ba1 93.1(4) . . ? Ba2 O6 Ba1 106.8(3) . . ? Si1 O7 Mn2 126.2(6) . 2_564 ? Si1 O7 Ba3 114.6(6) . . ? Mn2 O7 Ba3 100.3(4) 2_564 . ? Si1 O7 Ba1 94.7(5) . . ? Mn2 O7 Ba1 104.5(5) 2_564 . ? Ba3 O7 Ba1 117.1(3) . . ? Si3 O8 Mn2 130.8(6) . 2_474 ? Si3 O8 Ba1 137.0(6) . 2_474 ? Mn2 O8 Ba1 92.1(4) 2_474 2_474 ? Si2 O9 Si2 174.1(14) . 4_455 ? Si2 O9 Ba2 89.4(6) . . ? Si2 O9 Ba2 89.4(6) 4_455 . ? Si2 O10 Mn2 130.0(6) . 1_465 ? Si2 O10 Ba1 108.4(5) . 1_465 ? Mn2 O10 Ba1 92.1(3) 1_465 1_465 ? Si2 O10 Ba3 119.3(5) . 2_475 ? Mn2 O10 Ba3 94.3(4) 1_465 2_475 ? Ba1 O10 Ba3 108.9(3) 1_465 2_475 ? Si3 O11 Si2 131.4(6) . . ? Si3 O11 Ba3 104.8(4) . 1_565 ? Si2 O11 Ba3 118.5(5) . 1_565 ? Si3 O11 Ba1 98.8(5) . 1_465 ? Si2 O11 Ba1 92.8(4) . 1_465 ? Ba3 O11 Ba1 102.1(2) 1_565 1_465 ? Ba3 Cl1 Ba2 119.8(3) . 2_464 ? Cl3 Cl2 Ba2 108.8(14) . . ? Cl3 Cl2 Ba3 120.0(12) . 2_465 ? Ba2 Cl2 Ba3 131.2(10) . 2_465 ? Cl3 Cl2 Ba1 75.7(4) . 1_455 ? Ba2 Cl2 Ba1 94.9(3) . 1_455 ? Ba3 Cl2 Ba1 96.9(3) 2_465 1_455 ? Cl3 Cl2 Ba1 75.7(4) . . ? Ba2 Cl2 Ba1 94.9(3) . . ? Ba3 Cl2 Ba1 96.9(3) 2_465 . ? Ba1 Cl2 Ba1 151.3(9) 1_455 . ? Cl2 Cl3 Ba2 55.8(12) . . ? Cl2 Cl3 Ba3 46.7(10) . 2_465 ? Ba2 Cl3 Ba3 102.5(6) . 2_465 ? Cl2 Cl3 Ba1 89.4(4) . . ? Ba2 Cl3 Ba1 89.9(2) . . ? Ba3 Cl3 Ba1 89.4(3) 2_465 . ? Cl2 Cl3 Ba1 89.4(4) . 1_455 ? Ba2 Cl3 Ba1 89.9(2) . 1_455 ? Ba3 Cl3 Ba1 89.4(3) 2_465 1_455 ? Ba1 Cl3 Ba1 178.7(6) . 1_455 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ba1 O3 2.637(11) . ? Ba1 O8 2.826(10) 2_475 ? Ba1 O10 2.943(10) 4_445 ? Ba1 O10 2.943(10) 1_645 ? Ba1 O6 2.990(10) 4 ? Ba1 O6 2.990(10) . ? Ba1 O7 3.208(14) . ? Ba1 O7 3.208(14) 4 ? Ba1 O11 3.313(10) 4_445 ? Ba1 O11 3.313(10) 1_645 ? Ba1 Cl3 3.4108(7) 1_655 ? Ba1 Cl3 3.4108(7) . ? Ba2 O1 2.719(8) 4_455 ? Ba2 O1 2.719(8) . ? Ba2 Cl2 2.838(15) . ? Ba2 O6 2.872(12) 4_455 ? Ba2 O6 2.872(12) . ? Ba2 Cl1 3.003(10) 2_465 ? Ba2 O4 3.102(9) 3_575 ? Ba2 O4 3.102(9) 2_475 ? Ba2 Cl3 3.246(15) . ? Ba2 O9 3.289(17) . ? Ba2 Si2 3.636(3) 4_455 ? Ba2 Si2 3.636(3) . ? Ba3 O7 2.754(11) . ? Ba3 O7 2.754(11) 4_455 ? Ba3 Cl2 2.86(2) 2_464 ? Ba3 O10 2.951(10) 3_574 ? Ba3 O10 2.951(10) 2_474 ? Ba3 Cl1 2.996(9) . ? Ba3 O2 3.225(19) . ? Ba3 O11 3.235(10) 4_445 ? Ba3 O11 3.235(10) 1_545 ? Ba3 Cl3 3.406(15) 2_464 ? Ba3 Mn2 3.6550(11) 2_564 ? Ba3 Mn2 3.6550(11) 2_464 ? Mn1 O1 1.885(8) 1_655 ? Mn1 O1 1.885(8) 4_455 ? Mn1 O6 1.937(10) . ? Mn1 O6 1.937(10) 4 ? Mn1 O3 2.135(12) . ? Mn1 Ba2 3.6496(11) 1_655 ? Mn2 O10 1.947(9) 4_445 ? Mn2 O10 1.947(9) 1_645 ? Mn2 O7 1.962(10) 2_565 ? Mn2 O7 1.962(10) 3_565 ? Mn2 O8 2.111(11) 2_475 ? Mn2 Ba3 3.6550(11) 2_565 ? Mn2 Ba3 3.6550(11) 2_465 ? Si1 O6 1.560(9) . ? Si1 O7 1.586(10) . ? Si1 O2 1.610(5) . ? Si1 O4 1.629(8) . ? Si2 O9 1.589(3) . ? Si2 O1 1.591(7) . ? Si2 O10 1.600(9) . ? Si2 O11 1.638(8) . ? Si2 Ba1 3.767(3) 1_465 ? Si3 O8 1.571(11) . ? Si3 O11 1.629(10) . ? Si3 O11 1.629(10) 4_355 ? Si3 O5 1.648(11) 1_455 ? Si4 O3 1.580(12) 2_574 ? Si4 O4 1.636(8) . ? Si4 O4 1.636(8) 4 ? Si4 O5 1.640(11) . ? O1 Mn1 1.885(8) 1_455 ? O2 Si1 1.610(5) 4_455 ? O3 Si4 1.580(12) 2_575 ? O4 Ba2 3.102(9) 2_474 ? O5 Si3 1.648(11) 1_655 ? O7 Mn2 1.962(10) 2_564 ? O8 Mn2 2.111(11) 2_474 ? O8 Ba1 2.826(10) 2_474 ? O9 Si2 1.589(3) 4_455 ? O10 Mn2 1.947(9) 1_465 ? O10 Ba1 2.943(10) 1_465 ? O10 Ba3 2.951(10) 2_475 ? O11 Ba3 3.235(10) 1_565 ? O11 Ba1 3.313(10) 1_465 ? Cl1 Ba2 3.003(10) 2_464 ? Cl2 Cl3 0.907(18) . ? Cl2 Ba3 2.86(2) 2_465 ? Cl2 Ba1 3.520(7) 1_455 ? Cl3 Ba3 3.406(15) 2_465 ? Cl3 Ba1 3.4108(7) 1_455 ?
1100751.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100751.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100751 loop_ _publ_author_name 'Xunhua Mo' 'Erin Ferguson' 'Shiou-Jyh Hwu' _publ_section_title ; Salt-Inclusion Synthesis of Two New Polar Solids, Ba6Mn4Si12O34Cl3 and Ba6Fe5Si11O34Cl3 ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3121 _journal_page_last 3126 _journal_paper_doi 10.1021/ic050228t _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'Ba6 Cl3 Fe5 O34 Si11' _chemical_formula_weight 2062.63 _chemical_name_systematic ; ? ; _space_group_IT_number 26 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'P 2c -2' _symmetry_space_group_name_H-M 'P m c 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 1 _cell_length_a 6.8782(14) _cell_length_b 9.6635(19) _cell_length_c 13.098(3) _cell_measurement_temperature 298(2) _cell_volume 870.6(3) _computing_cell_refinement 'Bruker XSCANS' _computing_data_collection 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 298(2) _diffrn_measured_fraction_theta_full 0.969 _diffrn_measured_fraction_theta_max 0.969 _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0285 _diffrn_reflns_av_sigmaI/netI 0.0225 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 8568 _diffrn_reflns_theta_full 28.45 _diffrn_reflns_theta_max 28.45 _diffrn_reflns_theta_min 2.96 _exptl_absorpt_coefficient_mu 9.407 _exptl_absorpt_correction_T_max 0.7047 _exptl_absorpt_correction_T_min 0.2111 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ;Jacobson, R.A. REQAB, subroutine of Crystal Clear;Rigaku/MSC: The Woodlands, TX, 1999. ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 3.934 _exptl_crystal_density_method 'not measured' _exptl_crystal_description column _exptl_crystal_F_000 943 _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _refine_diff_density_max 2.046 _refine_diff_density_min -1.095 _refine_diff_density_rms 0.172 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.32(2) _refine_ls_extinction_coef 0.0012(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 173 _refine_ls_number_reflns 2195 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.073 _refine_ls_R_factor_all 0.0270 _refine_ls_R_factor_gt 0.0260 _refine_ls_shift/su_max 0.044 _refine_ls_shift/su_mean 0.004 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0177P)^2^+5.3028P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0557 _refine_ls_wR_factor_ref 0.0561 _reflns_number_gt 2135 _reflns_number_total 2195 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic050228tsi20050214_023827_2.cif _cod_data_source_block Ba6Fe5Si11O34Cl3(2) _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_database_code 1100751 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x, -y, z+1/2' '-x, y, z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ba1 Ba 0.0000 0.64563(5) 0.02160(4) 0.01945(12) Uani 1 2 d S . . Ba2 Ba 0.5000 0.98042(6) 0.07570(4) 0.02731(15) Uani 1 2 d S . . Ba3 Ba 0.5000 0.50429(8) -0.23036(8) 0.04077(19) Uani 1 2 d S . . Fe1 Fe 0.0000 0.01795(12) -0.01001(9) 0.0168(3) Uani 1 2 d S . . Fe2 Fe 0.0000 0.38939(12) 0.21452(9) 0.0137(2) Uani 1 2 d S . . Si1 Si -0.2697(2) 0.83213(15) -0.16870(12) 0.0108(3) Uani 1 1 d . . . Si2 Si -0.72949(19) 0.30506(14) 0.01903(13) 0.0137(3) Uani 1 1 d . . . Fe3 Fe 0.0000 0.31980(17) -0.15886(12) 0.0265(4) Uani 0.50 2 d SP . . Si3 Si 0.0000 0.31980(17) -0.15886(12) 0.0265(4) Uani 0.50 2 d SP . . Si4 Si 0.0000 0.0307(2) -0.27180(17) 0.0130(4) Uani 1 2 d S . . O1 O -0.7956(6) 0.1464(4) 0.0220(4) 0.0260(8) Uani 1 1 d . . . O2 O 0.5000 0.8293(11) -0.1867(8) 0.054(3) Uani 1 2 d S . . O3 O 0.0000 0.9026(6) 0.1188(4) 0.0174(12) Uani 1 2 d S . . O4 O -0.1921(8) 0.9338(5) -0.2591(3) 0.0337(12) Uani 1 1 d . . . O5 O 0.0000 0.1397(6) -0.1755(5) 0.0171(13) Uani 1 2 d S . . O6 O -0.2052(8) 0.8885(4) -0.0612(3) 0.0286(11) Uani 1 1 d . . . O7 O -0.1957(8) 0.6764(5) -0.1853(4) 0.0349(12) Uani 1 1 d . . . O8 O 0.0000 0.4151(6) -0.2665(5) 0.0339(18) Uani 1 2 d S . . O9 O 0.5000 0.300(2) 0.051(4) 0.030(10) Uani 0.44(8) 2 d SP . 1 O9A O 0.5000 0.315(3) -0.012(4) 0.044(12) Uani 0.56(8) 2 d SP . 2 O10 O -0.8001(11) 0.3976(6) 0.1114(5) 0.0514(18) Uani 1 1 d . . . O11 O -0.8028(13) 0.3750(6) -0.0868(5) 0.062(2) Uani 1 1 d . . . Cl1 Cl 0.5000 0.1839(9) -0.2238(7) 0.079(3) Uani 0.50 2 d SP . . Cl2 Cl 0.5000 0.6788(7) 0.0906(11) 0.059(4) Uani 0.64(2) 2 d SP . 1 Cl3 Cl 0.5000 0.6423(8) 0.0270(10) 0.024(3) Uani 0.36(2) 2 d SP . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ba1 0.0279(2) 0.0145(2) 0.0159(2) 0.0022(2) 0.000 0.000 Ba2 0.0160(3) 0.0361(3) 0.0298(3) -0.0016(3) 0.000 0.000 Ba3 0.0191(3) 0.0216(3) 0.0815(5) 0.0015(3) 0.000 0.000 Fe1 0.0165(5) 0.0132(5) 0.0208(7) -0.0073(5) 0.000 0.000 Fe2 0.0202(6) 0.0096(5) 0.0113(5) 0.0008(4) 0.000 0.000 Si1 0.0082(6) 0.0119(6) 0.0124(6) -0.0008(6) 0.0009(5) -0.0006(5) Si2 0.0082(6) 0.0137(6) 0.0191(7) 0.0055(7) 0.0006(7) 0.0003(5) Fe3 0.0612(12) 0.0078(7) 0.0104(8) 0.0008(6) 0.000 0.000 Si3 0.0612(12) 0.0078(7) 0.0104(8) 0.0008(6) 0.000 0.000 Si4 0.0127(9) 0.0153(10) 0.0111(10) 0.0004(8) 0.000 0.000 O1 0.032(2) 0.0217(17) 0.0246(19) 0.0068(19) -0.010(2) -0.0138(18) O2 0.003(3) 0.078(6) 0.081(7) 0.044(6) 0.000 0.000 O3 0.036(4) 0.014(3) 0.002(2) -0.004(2) 0.000 0.000 O4 0.042(3) 0.044(3) 0.015(2) 0.0038(19) 0.002(2) -0.025(2) O5 0.018(3) 0.025(3) 0.008(2) -0.010(2) 0.000 0.000 O6 0.049(3) 0.020(2) 0.017(2) 0.0012(17) -0.008(2) -0.019(2) O7 0.033(3) 0.017(2) 0.055(3) -0.014(2) 0.019(2) 0.001(2) O8 0.075(5) 0.011(3) 0.016(3) 0.002(2) 0.000 0.000 O9 0.002(6) 0.034(10) 0.05(3) 0.020(11) 0.000 0.000 O9A 0.014(6) 0.046(12) 0.07(3) -0.025(15) 0.000 0.000 O10 0.067(4) 0.037(3) 0.050(3) -0.017(3) 0.037(3) -0.027(3) O11 0.108(6) 0.037(3) 0.042(3) 0.026(3) -0.029(4) -0.015(4) Cl1 0.118(8) 0.054(4) 0.064(6) -0.009(4) 0.000 0.000 Cl2 0.046(3) 0.029(3) 0.102(10) 0.026(4) 0.000 0.000 Cl3 0.030(3) 0.015(3) 0.027(5) 0.005(3) 0.000 0.000 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Ba1 O8 74.80(16) . 2_565 ? O3 Ba1 O6 57.25(12) . . ? O8 Ba1 O6 121.69(14) 2_565 . ? O3 Ba1 O6 57.25(12) . 4 ? O8 Ba1 O6 121.69(14) 2_565 4 ? O6 Ba1 O6 57.26(19) . 4 ? O3 Ba1 O10 122.11(15) . 4_455 ? O8 Ba1 O10 56.74(14) 2_565 4_455 ? O6 Ba1 O10 124.11(15) . 4_455 ? O6 Ba1 O10 178.19(14) 4 4_455 ? O3 Ba1 O10 122.11(15) . 1_655 ? O8 Ba1 O10 56.74(14) 2_565 1_655 ? O6 Ba1 O10 178.19(14) . 1_655 ? O6 Ba1 O10 124.11(15) 4 1_655 ? O10 Ba1 O10 54.5(2) 4_455 1_655 ? O3 Ba1 O7 108.63(13) . . ? O8 Ba1 O7 153.16(10) 2_565 . ? O6 Ba1 O7 51.80(11) . . ? O6 Ba1 O7 78.80(13) 4 . ? O10 Ba1 O7 102.98(14) 4_455 . ? O10 Ba1 O7 129.05(14) 1_655 . ? O3 Ba1 O7 108.63(13) . 4 ? O8 Ba1 O7 153.16(10) 2_565 4 ? O6 Ba1 O7 78.80(13) . 4 ? O6 Ba1 O7 51.80(11) 4 4 ? O10 Ba1 O7 129.05(14) 4_455 4 ? O10 Ba1 O7 102.98(13) 1_655 4 ? O7 Ba1 O7 52.55(18) . 4 ? O3 Ba1 O11 155.47(14) . 4_455 ? O8 Ba1 O11 105.04(15) 2_565 4_455 ? O6 Ba1 O11 106.16(14) . 4_455 ? O6 Ba1 O11 132.51(14) 4 4_455 ? O10 Ba1 O11 48.86(13) 4_455 4_455 ? O10 Ba1 O11 73.85(15) 1_655 4_455 ? O7 Ba1 O11 60.50(13) . 4_455 ? O7 Ba1 O11 82.80(13) 4 4_455 ? O3 Ba1 O11 155.47(14) . 1_655 ? O8 Ba1 O11 105.04(15) 2_565 1_655 ? O6 Ba1 O11 132.51(14) . 1_655 ? O6 Ba1 O11 106.16(14) 4 1_655 ? O10 Ba1 O11 73.85(15) 4_455 1_655 ? O10 Ba1 O11 48.86(13) 1_655 1_655 ? O7 Ba1 O11 82.80(13) . 1_655 ? O7 Ba1 O11 60.50(13) 4 1_655 ? O11 Ba1 O11 49.0(3) 4_455 1_655 ? O3 Ba1 Cl3 89.95(19) . 1_455 ? O8 Ba1 Cl3 88.7(2) 2_565 1_455 ? O6 Ba1 Cl3 62.36(15) . 1_455 ? O6 Ba1 Cl3 119.61(15) 4 1_455 ? O10 Ba1 Cl3 61.75(16) 4_455 1_455 ? O10 Ba1 Cl3 116.24(16) 1_655 1_455 ? O7 Ba1 Cl3 64.9(2) . 1_455 ? O7 Ba1 Cl3 117.5(2) 4 1_455 ? O11 Ba1 Cl3 65.6(2) 4_455 1_455 ? O11 Ba1 Cl3 114.6(2) 1_655 1_455 ? O3 Ba1 Cl3 89.95(19) . . ? O8 Ba1 Cl3 88.7(2) 2_565 . ? O6 Ba1 Cl3 119.61(15) . . ? O6 Ba1 Cl3 62.36(15) 4 . ? O10 Ba1 Cl3 116.24(16) 4_455 . ? O10 Ba1 Cl3 61.75(16) 1_655 . ? O7 Ba1 Cl3 117.5(2) . . ? O7 Ba1 Cl3 64.9(2) 4 . ? O11 Ba1 Cl3 114.6(2) 4_455 . ? O11 Ba1 Cl3 65.6(2) 1_655 . ? Cl3 Ba1 Cl3 177.4(4) 1_455 . ? O1 Ba2 O1 98.51(17) 4_565 1_665 ? O1 Ba2 O6 124.09(15) 4_565 4 ? O1 Ba2 O6 58.82(13) 1_665 4 ? O1 Ba2 O6 58.82(13) 4_565 1_655 ? O1 Ba2 O6 124.09(15) 1_665 1_655 ? O6 Ba2 O6 90.74(18) 4 1_655 ? O1 Ba2 Cl2 127.87(11) 4_565 . ? O1 Ba2 Cl2 127.87(11) 1_665 . ? O6 Ba2 Cl2 74.4(2) 4 . ? O6 Ba2 Cl2 74.4(2) 1_655 . ? O1 Ba2 Cl1 122.25(14) 4_565 2_665 ? O1 Ba2 Cl1 122.25(14) 1_665 2_665 ? O6 Ba2 Cl1 112.16(14) 4 2_665 ? O6 Ba2 Cl1 112.16(14) 1_655 2_665 ? Cl2 Ba2 Cl1 55.0(3) . 2_665 ? O1 Ba2 O9 51.6(3) 4_565 1_565 ? O1 Ba2 O9 51.6(3) 1_665 1_565 ? O6 Ba2 O9 104.2(7) 4 1_565 ? O6 Ba2 O9 104.2(7) 1_655 1_565 ? Cl2 Ba2 O9 177.9(11) . 1_565 ? Cl1 Ba2 O9 127.1(11) 2_665 1_565 ? O1 Ba2 O4 60.77(15) 4_565 3_675 ? O1 Ba2 O4 122.27(13) 1_665 3_675 ? O6 Ba2 O4 175.13(13) 4 3_675 ? O6 Ba2 O4 92.08(12) 1_655 3_675 ? Cl2 Ba2 O4 102.6(2) . 3_675 ? Cl1 Ba2 O4 63.05(15) 2_665 3_675 ? O9 Ba2 O4 79.0(8) 1_565 3_675 ? O1 Ba2 O4 122.27(13) 4_565 2_575 ? O1 Ba2 O4 60.77(15) 1_665 2_575 ? O6 Ba2 O4 92.08(12) 4 2_575 ? O6 Ba2 O4 175.13(13) 1_655 2_575 ? Cl2 Ba2 O4 102.6(2) . 2_575 ? Cl1 Ba2 O4 63.05(15) 2_665 2_575 ? O9 Ba2 O4 79.0(8) 1_565 2_575 ? O4 Ba2 O4 84.85(17) 3_675 2_575 ? O1 Ba2 Cl3 122.44(13) 4_565 . ? O1 Ba2 Cl3 122.44(13) 1_665 . ? O6 Ba2 Cl3 64.74(15) 4 . ? O6 Ba2 Cl3 64.74(15) 1_655 . ? Cl2 Ba2 Cl3 14.9(2) . . ? Cl1 Ba2 Cl3 69.9(3) 2_665 . ? O9 Ba2 Cl3 163.0(11) 1_565 . ? O4 Ba2 Cl3 113.04(17) 3_675 . ? O4 Ba2 Cl3 113.04(17) 2_575 . ? O1 Ba2 Si2 24.52(8) 4_565 4_565 ? O1 Ba2 Si2 75.91(9) 1_665 4_565 ? O6 Ba2 Si2 117.09(9) 4 4_565 ? O6 Ba2 Si2 80.18(9) 1_655 4_565 ? Cl2 Ba2 Si2 152.35(9) . 4_565 ? Cl1 Ba2 Si2 128.99(14) 2_665 4_565 ? O9 Ba2 Si2 27.0(3) 1_565 4_565 ? O4 Ba2 Si2 67.36(10) 3_675 4_565 ? O4 Ba2 Si2 102.03(9) 2_575 4_565 ? Cl3 Ba2 Si2 144.90(14) . 4_565 ? O1 Ba2 Si2 75.91(9) 4_565 1_665 ? O1 Ba2 Si2 24.52(8) 1_665 1_665 ? O6 Ba2 Si2 80.18(9) 4 1_665 ? O6 Ba2 Si2 117.09(9) 1_655 1_665 ? Cl2 Ba2 Si2 152.35(9) . 1_665 ? Cl1 Ba2 Si2 128.99(14) 2_665 1_665 ? O9 Ba2 Si2 27.0(3) 1_565 1_665 ? O4 Ba2 Si2 102.03(9) 3_675 1_665 ? O4 Ba2 Si2 67.36(10) 2_575 1_665 ? Cl3 Ba2 Si2 144.90(14) . 1_665 ? Si2 Ba2 Si2 52.17(4) 4_565 1_665 ? O7 Ba3 O7 99.7(2) 1_655 4 ? O7 Ba3 Cl2 122.54(14) 1_655 2_664 ? O7 Ba3 Cl2 122.54(14) 4 2_664 ? O7 Ba3 O11 66.21(18) 1_655 4 ? O7 Ba3 O11 129.31(17) 4 4 ? Cl2 Ba3 O11 104.1(2) 2_664 4 ? O7 Ba3 O11 129.31(17) 1_655 1_655 ? O7 Ba3 O11 66.21(18) 4 1_655 ? Cl2 Ba3 O11 104.1(2) 2_664 1_655 ? O11 Ba3 O11 85.4(3) 4 1_655 ? O7 Ba3 O10 118.12(17) 1_655 3_664 ? O7 Ba3 O10 56.27(15) 4 3_664 ? Cl2 Ba3 O10 69.4(2) 2_664 3_664 ? O11 Ba3 O10 173.32(18) 4 3_664 ? O11 Ba3 O10 94.74(15) 1_655 3_664 ? O7 Ba3 O10 56.27(15) 1_655 2_564 ? O7 Ba3 O10 118.12(17) 4 2_564 ? Cl2 Ba3 O10 69.4(2) 2_664 2_564 ? O11 Ba3 O10 94.74(15) 4 2_564 ? O11 Ba3 O10 173.32(18) 1_655 2_564 ? O10 Ba3 O10 84.3(2) 3_664 2_564 ? O7 Ba3 Cl1 126.96(12) 1_655 . ? O7 Ba3 Cl1 126.96(12) 4 . ? Cl2 Ba3 Cl1 54.6(3) 2_664 . ? O11 Ba3 Cl1 64.94(17) 4 . ? O11 Ba3 Cl1 64.94(17) 1_655 . ? O10 Ba3 Cl1 109.08(17) 3_664 . ? O10 Ba3 Cl1 109.08(17) 2_564 . ? O7 Ba3 O2 50.48(10) 1_655 . ? O7 Ba3 O2 50.48(10) 4 . ? Cl2 Ba3 O2 137.3(3) 2_664 . ? O11 Ba3 O2 106.88(18) 4 . ? O11 Ba3 O2 106.88(18) 1_655 . ? O10 Ba3 O2 79.49(18) 3_664 . ? O10 Ba3 O2 79.49(18) 2_564 . ? Cl1 Ba3 O2 168.1(2) . . ? O7 Ba3 Cl3 116.37(14) 1_655 2_664 ? O7 Ba3 Cl3 116.37(14) 4 2_664 ? Cl2 Ba3 Cl3 13.00(17) 2_664 2_664 ? O11 Ba3 Cl3 113.18(18) 4 2_664 ? O11 Ba3 Cl3 113.18(18) 1_655 2_664 ? O10 Ba3 Cl3 60.65(16) 3_664 2_664 ? O10 Ba3 Cl3 60.65(16) 2_564 2_664 ? Cl1 Ba3 Cl3 67.6(2) . 2_664 ? O2 Ba3 Cl3 124.3(3) . 2_664 ? O7 Ba3 Cl3 64.92(12) 1_655 . ? O7 Ba3 Cl3 64.92(12) 4 . ? Cl2 Ba3 Cl3 164.6(3) 2_664 . ? O11 Ba3 Cl3 65.19(14) 4 . ? O11 Ba3 Cl3 65.19(14) 1_655 . ? O10 Ba3 Cl3 120.88(12) 3_664 . ? O10 Ba3 Cl3 120.88(12) 2_564 . ? Cl1 Ba3 Cl3 110.0(2) . . ? O2 Ba3 Cl3 58.1(2) . . ? Cl3 Ba3 Cl3 177.56(16) 2_664 . ? O7 Ba3 Si1 24.35(10) 1_655 1_655 ? O7 Ba3 Si1 75.85(10) 4 1_655 ? Cl2 Ba3 Si1 134.6(2) 2_664 1_655 ? O11 Ba3 Si1 85.58(13) 4 1_655 ? O11 Ba3 Si1 120.95(13) 1_655 1_655 ? O10 Ba3 Si1 100.01(13) 3_664 1_655 ? O10 Ba3 Si1 65.69(11) 2_564 1_655 ? Cl1 Ba3 Si1 149.94(9) . 1_655 ? O2 Ba3 Si1 26.13(3) . 1_655 ? Cl3 Ba3 Si1 123.92(16) 2_664 1_655 ? Cl3 Ba3 Si1 58.16(9) . 1_655 ? O1 Fe1 O1 94.0(3) 1_655 4_455 ? O1 Fe1 O6 173.0(2) 1_655 1_545 ? O1 Fe1 O6 87.8(2) 4_455 1_545 ? O1 Fe1 O6 87.8(2) 1_655 4_545 ? O1 Fe1 O6 173.0(2) 4_455 4_545 ? O6 Fe1 O6 89.6(3) 1_545 4_545 ? O1 Fe1 O3 100.02(19) 1_655 1_545 ? O1 Fe1 O3 100.02(19) 4_455 1_545 ? O6 Fe1 O3 86.28(16) 1_545 1_545 ? O6 Fe1 O3 86.28(16) 4_545 1_545 ? O1 Fe1 Ba1 128.08(13) 1_655 1_545 ? O1 Fe1 Ba1 128.08(13) 4_455 1_545 ? O6 Fe1 Ba1 54.36(14) 1_545 1_545 ? O6 Fe1 Ba1 54.36(14) 4_545 1_545 ? O3 Fe1 Ba1 49.98(15) 1_545 1_545 ? O1 Fe1 Ba2 45.98(13) 1_655 1_545 ? O1 Fe1 Ba2 133.56(16) 4_455 1_545 ? O6 Fe1 Ba2 135.07(16) 1_545 1_545 ? O6 Fe1 Ba2 51.27(15) 4_545 1_545 ? O3 Fe1 Ba2 71.78(2) 1_545 1_545 ? Ba1 Fe1 Ba2 82.28(2) 1_545 1_545 ? O1 Fe1 Ba2 133.56(16) 1_655 1_445 ? O1 Fe1 Ba2 45.98(13) 4_455 1_445 ? O6 Fe1 Ba2 51.27(15) 1_545 1_445 ? O6 Fe1 Ba2 135.07(16) 4_545 1_445 ? O3 Fe1 Ba2 71.78(2) 1_545 1_445 ? Ba1 Fe1 Ba2 82.28(2) 1_545 1_445 ? Ba2 Fe1 Ba2 142.13(4) 1_545 1_445 ? O8 Fe2 O10 92.9(2) 2_565 4_455 ? O8 Fe2 O10 92.9(2) 2_565 1_655 ? O10 Fe2 O10 90.9(5) 4_455 1_655 ? O8 Fe2 O7 103.4(2) 2_565 2_565 ? O10 Fe2 O7 163.7(2) 4_455 2_565 ? O10 Fe2 O7 89.6(3) 1_655 2_565 ? O8 Fe2 O7 103.4(2) 2_565 3_565 ? O10 Fe2 O7 89.6(3) 4_455 3_565 ? O10 Fe2 O7 163.7(2) 1_655 3_565 ? O7 Fe2 O7 85.4(3) 2_565 3_565 ? O8 Fe2 Ba1 53.06(19) 2_565 . ? O10 Fe2 Ba1 58.1(2) 4_455 . ? O10 Fe2 Ba1 58.1(2) 1_655 . ? O7 Fe2 Ba1 134.15(14) 2_565 . ? O7 Fe2 Ba1 134.15(14) 3_565 . ? O8 Fe2 Ba3 72.31(4) 2_565 2_665 ? O10 Fe2 Ba3 142.8(2) 4_455 2_665 ? O10 Fe2 Ba3 57.1(2) 1_655 2_665 ? O7 Fe2 Ba3 47.34(14) 2_565 2_665 ? O7 Fe2 Ba3 126.64(17) 3_565 2_665 ? Ba1 Fe2 Ba3 86.81(2) . 2_665 ? O8 Fe2 Ba3 72.31(4) 2_565 2_565 ? O10 Fe2 Ba3 57.1(2) 4_455 2_565 ? O10 Fe2 Ba3 142.8(2) 1_655 2_565 ? O7 Fe2 Ba3 126.64(17) 2_565 2_565 ? O7 Fe2 Ba3 47.34(14) 3_565 2_565 ? Ba1 Fe2 Ba3 86.81(2) . 2_565 ? Ba3 Fe2 Ba3 139.88(4) 2_665 2_565 ? O6 Si1 O2 114.6(5) . 1_455 ? O6 Si1 O7 110.9(3) . . ? O2 Si1 O7 106.1(4) 1_455 . ? O6 Si1 O4 110.4(2) . . ? O2 Si1 O4 103.2(4) 1_455 . ? O7 Si1 O4 111.3(3) . . ? O6 Si1 Ba1 53.63(18) . . ? O2 Si1 Ba1 127.2(3) 1_455 . ? O7 Si1 Ba1 57.3(2) . . ? O4 Si1 Ba1 129.6(2) . . ? O6 Si1 Ba3 128.59(16) . 1_455 ? O2 Si1 Ba3 61.4(4) 1_455 1_455 ? O7 Si1 Ba3 44.75(19) . 1_455 ? O4 Si1 Ba3 120.49(18) . 1_455 ? Ba1 Si1 Ba3 86.67(4) . 1_455 ? O10 Si2 O1 115.9(3) . . ? O10 Si2 O11 108.8(4) . . ? O1 Si2 O11 109.4(3) . . ? O10 Si2 O9A 117.3(10) . 1_455 ? O1 Si2 O9A 109.6(10) . 1_455 ? O11 Si2 O9A 93(2) . 1_455 ? O10 Si2 O9 96.7(19) . 1_455 ? O1 Si2 O9 103.7(8) . 1_455 ? O11 Si2 O9 122.3(16) . 1_455 ? O9A Si2 O9 30.0(7) 1_455 1_455 ? O10 Si2 Ba2 118.1(3) . 1_445 ? O1 Si2 Ba2 44.13(15) . 1_445 ? O11 Si2 Ba2 132.6(3) . 1_445 ? O9A Si2 Ba2 71.1(15) 1_455 1_445 ? O9 Si2 Ba2 59.6(7) 1_455 1_445 ? O10 Si2 Ba1 49.4(3) . 1_455 ? O1 Si2 Ba1 133.97(17) . 1_455 ? O11 Si2 Ba1 59.5(3) . 1_455 ? O9A Si2 Ba1 115.4(12) 1_455 1_455 ? O9 Si2 Ba1 120.1(10) 1_455 1_455 ? Ba2 Si2 Ba1 167.25(5) 1_445 1_455 ? O8 Fe3 O11 106.7(2) . 1_655 ? O8 Fe3 O11 106.7(2) . 4_455 ? O11 Fe3 O11 102.7(6) 1_655 4_455 ? O8 Fe3 O5 116.0(3) . . ? O11 Fe3 O5 111.9(2) 1_655 . ? O11 Fe3 O5 111.9(2) 4_455 . ? O3 Si4 O4 109.2(2) 2_564 1_545 ? O3 Si4 O4 109.2(2) 2_564 4_545 ? O4 Si4 O4 108.5(4) 1_545 4_545 ? O3 Si4 O5 115.9(3) 2_564 . ? O4 Si4 O5 106.9(2) 1_545 . ? O4 Si4 O5 106.9(2) 4_545 . ? Si2 O1 Fe1 145.3(3) . 1_455 ? Si2 O1 Ba2 111.3(2) . 1_445 ? Fe1 O1 Ba2 103.02(16) 1_455 1_445 ? Si1 O2 Si1 163.0(8) 1_655 4 ? Si1 O2 Ba3 92.5(4) 1_655 . ? Si1 O2 Ba3 92.5(4) 4 . ? Si4 O3 Fe1 122.3(3) 2_565 1_565 ? Si4 O3 Ba1 141.3(3) 2_565 . ? Fe1 O3 Ba1 96.3(2) 1_565 . ? Si4 O4 Si1 133.4(3) 1_565 . ? Si4 O4 Ba2 109.0(2) 1_565 2_574 ? Si1 O4 Ba2 116.1(2) . 2_574 ? Si4 O5 Fe3 137.0(4) . . ? Si1 O6 Fe1 135.7(3) . 1_565 ? Si1 O6 Ba2 118.1(3) . 1_455 ? Fe1 O6 Ba2 95.49(17) 1_565 1_455 ? Si1 O6 Ba1 100.9(2) . . ? Fe1 O6 Ba1 92.10(18) 1_565 . ? Ba2 O6 Ba1 110.95(14) 1_455 . ? Si1 O7 Fe2 127.3(3) . 2_564 ? Si1 O7 Ba3 110.9(3) . 1_455 ? Fe2 O7 Ba3 100.45(18) 2_564 1_455 ? Si1 O7 Ba1 96.4(2) . . ? Fe2 O7 Ba1 104.9(2) 2_564 . ? Ba3 O7 Ba1 118.11(18) 1_455 . ? Fe3 O8 Fe2 130.6(4) . 2_564 ? Fe3 O8 Ba1 134.9(3) . 2_564 ? Fe2 O8 Ba1 94.5(2) 2_564 2_564 ? Si2 O9 Si2 150(4) 4 1_655 ? Si2 O9 Ba2 93.4(9) 4 1_545 ? Si2 O9 Ba2 93.4(9) 1_655 1_545 ? Si2 O9A Si2 150(4) 4 1_655 ? Si2 O10 Fe2 137.0(3) . 1_455 ? Si2 O10 Ba1 107.0(3) . 1_455 ? Fe2 O10 Ba1 88.9(3) 1_455 1_455 ? Si2 O10 Ba3 118.9(4) . 2_565 ? Fe2 O10 Ba3 91.1(2) 1_455 2_565 ? Ba1 O10 Ba3 108.99(17) 1_455 2_565 ? Si2 O11 Si3 125.4(4) . 1_455 ? Si2 O11 Fe3 125.4(4) . 1_455 ? Si3 O11 Fe3 0.00(9) 1_455 1_455 ? Si2 O11 Ba3 118.8(4) . 1_455 ? Si3 O11 Ba3 108.8(3) 1_455 1_455 ? Fe3 O11 Ba3 108.8(3) 1_455 1_455 ? Si2 O11 Ba1 95.2(3) . 1_455 ? Si3 O11 Ba1 99.1(3) 1_455 1_455 ? Fe3 O11 Ba1 99.1(3) 1_455 1_455 ? Ba3 O11 Ba1 102.81(16) 1_455 1_455 ? Ba2 Cl1 Ba3 119.6(3) 2_664 . ? Ba2 Cl2 Ba3 130.8(5) . 2_665 ? Ba2 Cl2 Ba1 94.17(8) . . ? Ba3 Cl2 Ba1 98.51(10) 2_665 . ? Ba2 Cl2 Ba1 94.17(8) . 1_655 ? Ba3 Cl2 Ba1 98.51(10) 2_665 1_655 ? Ba1 Cl2 Ba1 148.9(5) . 1_655 ? Ba2 Cl3 Ba1 89.69(15) . 1_655 ? Ba2 Cl3 Ba1 89.70(15) . . ? Ba1 Cl3 Ba1 177.4(4) 1_655 . ? Ba2 Cl3 Ba3 103.0(4) . 2_665 ? Ba1 Cl3 Ba3 91.29(18) 1_655 2_665 ? Ba1 Cl3 Ba3 91.29(18) . 2_665 ? Ba2 Cl3 Ba3 122.6(3) . . ? Ba1 Cl3 Ba3 89.1(2) 1_655 . ? Ba1 Cl3 Ba3 89.1(2) . . ? Ba3 Cl3 Ba3 134.4(2) 2_665 . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ba1 O3 2.791(5) . ? Ba1 O8 2.836(6) 2_565 ? Ba1 O6 2.945(5) . ? Ba1 O6 2.945(5) 4 ? Ba1 O10 3.003(8) 4_455 ? Ba1 O10 3.003(8) 1_655 ? Ba1 O7 3.041(6) . ? Ba1 O7 3.041(6) 4 ? Ba1 O11 3.270(8) 4_455 ? Ba1 O11 3.270(8) 1_655 ? Ba1 Cl3 3.4400(7) 1_455 ? Ba1 Cl3 3.4400(7) . ? Ba2 O1 2.683(4) 4_565 ? Ba2 O1 2.683(4) 1_665 ? Ba2 O6 2.849(5) 4 ? Ba2 O6 2.849(5) 1_655 ? Ba2 Cl2 2.922(6) . ? Ba2 Cl1 3.069(9) 2_665 ? Ba2 O9 3.10(2) 1_565 ? Ba2 O4 3.140(5) 3_675 ? Ba2 O4 3.140(5) 2_575 ? Ba2 Cl3 3.329(9) . ? Ba2 Si2 3.5895(15) 4_565 ? Ba2 Si2 3.5895(15) 1_665 ? Ba3 O7 2.738(5) 1_655 ? Ba3 O7 2.738(5) 4 ? Ba3 Cl2 2.938(9) 2_664 ? Ba3 O11 3.072(7) 4 ? Ba3 O11 3.072(7) 1_655 ? Ba3 O10 3.074(7) 3_664 ? Ba3 O10 3.074(7) 2_564 ? Ba3 Cl1 3.097(9) . ? Ba3 O2 3.193(11) . ? Ba3 Cl3 3.480(11) 2_664 ? Ba3 Cl3 3.625(14) . ? Ba3 Si1 3.6329(17) 1_655 ? Fe1 O1 1.922(4) 1_655 ? Fe1 O1 1.922(4) 4_455 ? Fe1 O6 2.002(4) 1_545 ? Fe1 O6 2.002(4) 4_545 ? Fe1 O3 2.022(6) 1_545 ? Fe1 Ba1 3.6217(15) 1_545 ? Fe1 Ba2 3.6358(8) 1_545 ? Fe1 Ba2 3.6358(8) 1_445 ? Fe2 O8 1.906(6) 2_565 ? Fe2 O10 1.929(5) 4_455 ? Fe2 O10 1.929(5) 1_655 ? Fe2 O7 1.984(5) 2_565 ? Fe2 O7 1.984(5) 3_565 ? Fe2 Ba3 3.6612(8) 2_665 ? Fe2 Ba3 3.6612(8) 2_565 ? Si1 O6 1.573(4) . ? Si1 O2 1.602(2) 1_455 ? Si1 O7 1.603(5) . ? Si1 O4 1.628(5) . ? Si1 Ba3 3.6329(17) 1_455 ? Si2 O10 1.582(5) . ? Si2 O1 1.600(4) . ? Si2 O11 1.623(6) . ? Si2 O9A 1.634(15) 1_455 ? Si2 O9 1.635(14) 1_455 ? Si2 Ba2 3.5895(15) 1_445 ? Si2 Ba1 3.7808(15) 1_455 ? Fe3 O8 1.684(6) . ? Fe3 O11 1.736(7) 1_655 ? Fe3 O11 1.736(7) 4_455 ? Fe3 O5 1.754(6) . ? Si4 O3 1.571(5) 2_564 ? Si4 O4 1.628(5) 1_545 ? Si4 O4 1.628(5) 4_545 ? Si4 O5 1.644(6) . ? O1 Fe1 1.922(4) 1_455 ? O1 Ba2 2.683(4) 1_445 ? O2 Si1 1.602(2) 1_655 ? O2 Si1 1.602(2) 4 ? O3 Si4 1.571(5) 2_565 ? O3 Fe1 2.022(6) 1_565 ? O4 Si4 1.628(5) 1_565 ? O4 Ba2 3.140(5) 2_574 ? O6 Fe1 2.002(4) 1_565 ? O6 Ba2 2.849(5) 1_455 ? O7 Fe2 1.984(5) 2_564 ? O7 Ba3 2.738(5) 1_455 ? O8 Fe2 1.906(6) 2_564 ? O8 Ba1 2.836(6) 2_564 ? O9 Si2 1.635(14) 4 ? O9 Si2 1.635(14) 1_655 ? O9 Ba2 3.10(2) 1_545 ? O9A Si2 1.634(15) 4 ? O9A Si2 1.634(15) 1_655 ? O10 Fe2 1.929(5) 1_455 ? O10 Ba1 3.003(8) 1_455 ? O10 Ba3 3.074(7) 2_565 ? O11 Si3 1.736(7) 1_455 ? O11 Fe3 1.736(7) 1_455 ? O11 Ba3 3.072(7) 1_455 ? O11 Ba1 3.270(8) 1_455 ? Cl1 Ba2 3.069(9) 2_664 ? Cl2 Ba3 2.938(9) 2_665 ? Cl2 Ba1 3.570(4) 1_655 ? Cl3 Ba1 3.4400(7) 1_655 ? Cl3 Ba3 3.480(11) 2_665 ?
1100752.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $ #$Revision: 176432 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100752.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100752 loop_ _publ_author_name 'Jian-Kai Cheng' 'Yu-Biao Chen' 'Ling Wu' 'Jian Zhang' 'Yi-Hang Wen' 'Zhao-Ji Li' 'Yuan-Gen Yao' _publ_contact_author_address ; The State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, the Chinese Academy of Sciences, Fuzhou, Fujian 350002, P. R. China ; _publ_contact_author_email yyg@fjirsm.ac.cn _publ_contact_author_fax 86-591-83714946 _publ_contact_author_name 'Yuan-Gen Yao' _publ_contact_author_phone 86-591-83711523 _publ_section_title ; A 3-D Noninterpenetrating Diamondoid Network of a Decanuclear Copper(I) Complex ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3386 _journal_page_last 3388 _journal_paper_doi 10.1021/ic050301f _journal_volume 44 _journal_year 2005 _chemical_formula_moiety 'C10 H10 Cl5 Cu5 N2 S2 ' _chemical_formula_sum 'C10 H10 Cl5 Cu5 N2 S2' _chemical_formula_weight 717.27 _chemical_name_systematic ; ? ; _space_group_IT_number 88 _symmetry_cell_setting tetragonal _symmetry_space_group_name_Hall '-I 4ad' _symmetry_space_group_name_H-M 'I 41/a :2' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 17.5832(4) _cell_length_b 17.5832(4) _cell_length_c 12.1881(6) _cell_measurement_temperature 293(2) _cell_measurement_theta_max 24.99 _cell_measurement_theta_min 2.03 _cell_volume 3768.2(2) _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_collection 'Siemens SMART' _computing_data_reduction 'Siemens XPREP' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_structure_solution 'Siemens SHELXTL' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.990 _diffrn_measured_fraction_theta_max 0.990 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0522 _diffrn_reflns_av_sigmaI/netI 0.0618 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_number 4467 _diffrn_reflns_theta_full 24.99 _diffrn_reflns_theta_max 24.99 _diffrn_reflns_theta_min 2.03 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time . _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 6.478 _exptl_absorpt_correction_T_max 0.355 _exptl_absorpt_correction_T_min 0.230 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_crystal_colour red _exptl_crystal_density_diffrn 2.529 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 2768 _exptl_crystal_size_max .26 _exptl_crystal_size_mid .20 _exptl_crystal_size_min .16 _refine_diff_density_max 0.864 _refine_diff_density_min -0.882 _refine_diff_density_rms 0.128 _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 112 _refine_ls_number_reflns 1670 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.063 _refine_ls_R_factor_gt 0.0559 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0314P)^2^+54.1553P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1001 _refine_ls_wR_factor_ref 0.1216 _reflns_number_gt 1045 _reflns_number_total 1670 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic050301fsi20050228_040827.cif _cod_data_source_block 1 _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_sg_symbol_Hall '-I 4ad ' _cod_original_sg_symbol_H-M 'I 41/a' _cod_database_code 1100752 #BEGIN Tags that were not found in dictionaries: _refine_ls_r_factor_ref 0.1112 #END Tags that were not found in dictionaries loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.0000 0.7500 0.09016(13) 0.0405(5) Uani 1 2 d S . . Cu2 Cu 0.14046(7) 0.80280(7) -0.12705(10) 0.0496(4) Uani 1 1 d . . . S1 S 0.09773(11) 0.70730(11) -0.01972(16) 0.0223(5) Uani 1 1 d . . . Cl3 Cl 0.2500 0.7500 -0.2500 0.0368(7) Uani 1 2 d S . . Cl1 Cl 0.04812(12) 0.84903(12) 0.20431(18) 0.0388(6) Uani 1 1 d . . . Cl2 Cl 0.20213(12) 0.90588(12) -0.0395(2) 0.0443(6) Uani 1 1 d . . . Cu3 Cu 0.34074(9) 0.84439(8) -0.19317(12) 0.0657(5) Uani 1 1 d . . . C5 C 0.1596(5) 0.6087(5) 0.1312(7) 0.039(2) Uani 1 1 d . . . H5A H 0.1144 0.5814 0.1269 0.047 Uiso 1 1 calc R . . C2 C 0.2378(5) 0.7140(5) 0.0784(7) 0.040(2) Uani 1 1 d . . . H2A H 0.2463 0.7575 0.0368 0.048 Uiso 1 1 calc R . . C1 C 0.1689(4) 0.6752(4) 0.0699(6) 0.0224(18) Uani 1 1 d . . . N1 N 0.2812(4) 0.6244(5) 0.2043(6) 0.048(2) Uani 1 1 d . . . H1A H 0.3165 0.6085 0.2474 0.057 Uiso 1 1 calc R . . C3 C 0.2928(5) 0.6882(6) 0.1476(8) 0.051(3) Uani 1 1 d . . . H3A H 0.3381 0.7149 0.1553 0.061 Uiso 1 1 calc R . . C4 C 0.2167(5) 0.5841(6) 0.1969(8) 0.047(3) Uani 1 1 d . . . H4A H 0.2111 0.5394 0.2368 0.057 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0314(9) 0.0499(11) 0.0402(10) 0.000 0.000 0.0102(8) Cu2 0.0447(8) 0.0477(8) 0.0563(8) 0.0226(6) -0.0182(6) -0.0116(6) S1 0.0197(10) 0.0230(11) 0.0243(10) -0.0001(9) -0.0034(9) 0.0013(8) Cl3 0.0291(16) 0.0357(17) 0.0456(19) -0.0092(15) 0.0044(14) -0.0023(13) Cl1 0.0372(12) 0.0393(13) 0.0398(13) -0.0047(11) -0.0101(11) 0.0000(10) Cl2 0.0304(12) 0.0346(13) 0.0679(17) -0.0127(12) -0.0042(12) -0.0048(10) Cu3 0.0835(11) 0.0528(9) 0.0607(9) 0.0028(7) -0.0041(8) 0.0000(8) C5 0.032(5) 0.042(6) 0.043(6) 0.014(5) -0.002(5) -0.006(4) C2 0.036(5) 0.039(5) 0.045(6) 0.021(5) -0.011(5) -0.008(4) C1 0.024(4) 0.018(4) 0.025(4) -0.002(4) -0.001(4) 0.006(3) N1 0.040(5) 0.061(5) 0.042(5) 0.019(4) -0.018(4) 0.008(4) C3 0.038(6) 0.059(7) 0.056(7) 0.016(6) -0.024(5) -0.008(5) C4 0.040(6) 0.050(6) 0.051(6) 0.021(5) -0.007(5) 0.003(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 Cu1 S1 108.93(11) 6_464 . ? S1 Cu1 Cl1 111.46(7) 6_464 . ? S1 Cu1 Cl1 108.21(7) . . ? S1 Cu1 Cl1 108.21(7) 6_464 6_464 ? S1 Cu1 Cl1 111.46(7) . 6_464 ? Cl1 Cu1 Cl1 108.60(13) . 6_464 ? S1 Cu2 S1 109.13(10) . 16_665 ? S1 Cu2 Cl2 117.44(10) . . ? S1 Cu2 Cl2 109.28(9) 16_665 . ? S1 Cu2 Cl3 108.28(7) . . ? S1 Cu2 Cl3 111.34(7) 16_665 . ? Cl2 Cu2 Cl3 101.14(7) . . ? S1 Cu2 Cu3 86.67(7) . 8_354 ? S1 Cu2 Cu3 89.57(7) 16_665 8_354 ? Cl2 Cu2 Cu3 46.83(7) . 8_354 ? Cl3 Cu2 Cu3 147.28(5) . 8_354 ? C1 S1 Cu2 111.2(3) . . ? C1 S1 Cu2 110.5(2) . 11_565 ? Cu2 S1 Cu2 110.96(8) . 11_565 ? C1 S1 Cu1 105.9(3) . . ? Cu2 S1 Cu1 110.04(9) . . ? Cu2 S1 Cu1 108.00(9) 11_565 . ? Cu3 Cl3 Cu3 180.00(7) 13_564 . ? Cu3 Cl3 Cu2 94.52(4) 13_564 13_564 ? Cu3 Cl3 Cu2 85.48(4) . 13_564 ? Cu3 Cl3 Cu2 85.48(4) 13_564 . ? Cu3 Cl3 Cu2 94.51(4) . . ? Cu2 Cl3 Cu2 180.0 13_564 . ? Cu3 Cl1 Cu1 90.34(9) 8_354 . ? Cu3 Cl2 Cu2 82.45(9) 8_354 . ? Cl2 Cu3 Cl1 135.95(11) 7_554 7_554 ? Cl2 Cu3 Cl3 116.92(9) 7_554 . ? Cl1 Cu3 Cl3 107.11(8) 7_554 . ? Cl2 Cu3 Cu2 50.73(7) 7_554 7_554 ? Cl1 Cu3 Cu2 113.50(8) 7_554 7_554 ? Cl3 Cu3 Cu2 112.42(6) . 7_554 ? C4 C5 C1 119.8(8) . . ? C4 C5 H5A 120.1 . . ? C1 C5 H5A 120.1 . . ? C3 C2 C1 120.1(8) . . ? C3 C2 H2A 120.0 . . ? C1 C2 H2A 120.0 . . ? C2 C1 C5 118.0(7) . . ? C2 C1 S1 120.7(6) . . ? C5 C1 S1 121.2(6) . . ? C3 N1 C4 122.6(8) . . ? C3 N1 H1A 118.7 . . ? C4 N1 H1A 118.7 . . ? N1 C3 C2 119.5(9) . . ? N1 C3 H3A 120.2 . . ? C2 C3 H3A 120.2 . . ? N1 C4 C5 119.9(9) . . ? N1 C4 H4A 120.1 . . ? C5 C4 H4A 120.1 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 S1 2.304(2) 6_464 ? Cu1 S1 2.304(2) . ? Cu1 Cl1 2.384(2) . ? Cu1 Cl1 2.384(2) 6_464 ? Cu2 S1 2.257(2) . ? Cu2 S1 2.272(2) 16_665 ? Cu2 Cl2 2.366(2) . ? Cu2 Cl3 2.6109(14) . ? Cu2 Cu3 3.030(2) 8_354 ? S1 C1 1.754(8) . ? S1 Cu2 2.272(2) 11_565 ? Cl3 Cu3 2.4042(14) 13_564 ? Cl3 Cu3 2.4042(14) . ? Cl3 Cu2 2.6109(14) 13_564 ? Cl1 Cu3 2.239(3) 8_354 ? Cl2 Cu3 2.229(3) 8_354 ? Cu3 Cl2 2.229(3) 7_554 ? Cu3 Cl1 2.239(3) 7_554 ? Cu3 Cu2 3.030(2) 7_554 ? C5 C4 1.355(12) . ? C5 C1 1.398(11) . ? C5 H5A 0.9300 . ? C2 C3 1.360(11) . ? C2 C1 1.394(11) . ? C2 H2A 0.9300 . ? N1 C3 1.333(11) . ? N1 C4 1.340(11) . ? N1 H1A 0.8600 . ? C3 H3A 0.9300 . ? C4 H4A 0.9300 . ?
1100753.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100753.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100753 loop_ _publ_author_name 'James D. Crowley' 'Ian M. Steele' 'B. Bosnich' _publ_section_title ; Supramolecular Recognition Forces: An Examination of Weak Metal-Metal Interactions in Host-Guest Formation ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 2989 _journal_page_last 2991 _journal_paper_doi 10.1021/ic0481531 _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C92 H118 Cl2 F12 N16 O9 Pt2 Sb2' _chemical_formula_weight 2524.60 _chemical_name_systematic ; ? ; _space_group_IT_number 2 _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 91.11(5) _cell_angle_beta 93.27(5) _cell_angle_gamma 90.39(5) _cell_formula_units_Z 2 _cell_length_a 13.90(4) _cell_length_b 18.83(5) _cell_length_c 19.15(5) _cell_measurement_temperature 108(2) _cell_volume 5003(2) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 108(2) _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0327 _diffrn_reflns_av_sigmaI/netI 0.0417 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 47859 _diffrn_reflns_theta_full 25.03 _diffrn_reflns_theta_max 25.03 _diffrn_reflns_theta_min 1.47 _exptl_absorpt_coefficient_mu 3.459 _exptl_absorpt_correction_T_max 0.354 _exptl_absorpt_correction_T_min 0.266 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; absorption corrections were made based on correspondance of equivalent intensities usingprogram SADABS (G. Sheldrick, Bruker Analytical X-ray Systems, Madison, WI) ; _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.675 _exptl_crystal_density_method 'not measured' _exptl_crystal_description fragment _exptl_crystal_F_000 2508 _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _refine_diff_density_max 7.527 _refine_diff_density_min -2.665 _refine_diff_density_rms 0.206 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 1240 _refine_ls_number_reflns 17626 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.075 _refine_ls_R_factor_all 0.0793 _refine_ls_R_factor_gt 0.0678 _refine_ls_shift/su_max 2.489 _refine_ls_shift/su_mean 0.015 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0917P)^2^+46.6967P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1767 _refine_ls_wR_factor_ref 0.1830 _reflns_number_gt 14417 _reflns_number_total 17626 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic0481531si20041231_115410_1.cif _cod_data_source_block 1-Ptreceptor _cod_original_cell_volume 5005.0(24) _cod_database_code 1100753 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6844(7) 0.0402(6) 0.6488(5) 0.037(2) Uani 1 1 d . . . H1 H 0.6909 0.0018 0.6801 0.044 Uiso 1 1 calc R . . C2 C 0.7036(7) 0.1088(6) 0.6735(5) 0.042(3) Uani 1 1 d . . . H2 H 0.7217 0.1170 0.7216 0.051 Uiso 1 1 calc R . . C3 C 0.6967(7) 0.1641(6) 0.6294(5) 0.039(2) Uani 1 1 d . . . H3 H 0.7102 0.2112 0.6462 0.046 Uiso 1 1 calc R . . C4 C 0.6696(6) 0.1511(5) 0.5590(5) 0.033(2) Uani 1 1 d . . . H4 H 0.6645 0.1891 0.5271 0.039 Uiso 1 1 calc R . . C5 C 0.6510(6) 0.0840(5) 0.5368(5) 0.030(2) Uani 1 1 d . . . C6 C 0.6208(6) 0.0627(5) 0.4629(5) 0.033(2) Uani 1 1 d . . . C7 C 0.5782(7) -0.2127(5) 0.4683(6) 0.041(2) Uani 1 1 d . . . H7 H 0.5905 -0.2316 0.5135 0.049 Uiso 1 1 calc R . . C8 C 0.5525(8) -0.2577(6) 0.4130(7) 0.054(3) Uani 1 1 d . . . H8 H 0.5477 -0.3073 0.4204 0.064 Uiso 1 1 calc R . . C9 C 0.5338(8) -0.2318(6) 0.3474(7) 0.051(3) Uani 1 1 d . . . H9 H 0.5161 -0.2631 0.3093 0.062 Uiso 1 1 calc R . . C10 C 0.5410(7) -0.1597(6) 0.3376(6) 0.040(2) Uani 1 1 d . . . H10 H 0.5288 -0.1406 0.2924 0.048 Uiso 1 1 calc R . . C11 C 0.5665(6) -0.1150(5) 0.3946(5) 0.034(2) Uani 1 1 d . . . C12 C 0.5779(6) -0.0369(5) 0.3912(5) 0.031(2) Uani 1 1 d . . . C13 C 0.6112(6) 0.1092(6) 0.4080(5) 0.034(2) Uani 1 1 d . . . H13 H 0.6211 0.1589 0.4146 0.041 Uiso 1 1 calc R . . C14 C 0.5853(6) 0.0778(5) 0.3401(5) 0.030(2) Uani 1 1 d . . . C15 C 0.5671(6) 0.0057(5) 0.3325(5) 0.032(2) Uani 1 1 d . . . H15 H 0.5475 -0.0145 0.2881 0.038 Uiso 1 1 calc R . . C16 C 0.5803(6) 0.1246(5) 0.2792(5) 0.030(2) Uani 1 1 d . . . C17 C 0.6488(7) 0.1789(5) 0.2740(5) 0.030(2) Uani 1 1 d . . . H17 H 0.6981 0.1858 0.3099 0.036 Uiso 1 1 calc R . . C18 C 0.6446(7) 0.2227(5) 0.2164(5) 0.033(2) Uani 1 1 d . . . C19 C 0.5720(7) 0.2135(6) 0.1640(5) 0.039(2) Uani 1 1 d . . . C20 C 0.5054(7) 0.1606(6) 0.1701(5) 0.039(2) Uani 1 1 d . . . H20 H 0.4553 0.1549 0.1345 0.047 Uiso 1 1 calc R . . C21 C 0.5081(7) 0.1154(5) 0.2257(5) 0.035(2) Uani 1 1 d . . . H21 H 0.4616 0.0784 0.2279 0.042 Uiso 1 1 calc R . . C22 C 0.5718(8) 0.2615(7) 0.1018(6) 0.053(3) Uani 1 1 d . . . H22A H 0.6153 0.2418 0.0673 0.063 Uiso 1 1 calc R . . H22B H 0.5060 0.2629 0.0793 0.063 Uiso 1 1 calc R . . C23 C 0.6034(8) 0.3346(6) 0.1221(6) 0.050(3) Uani 1 1 d . . . H23A H 0.5535 0.3574 0.1496 0.060 Uiso 1 1 calc R . . H23B H 0.6101 0.3625 0.0793 0.060 Uiso 1 1 calc R . . C24 C 0.6980(7) 0.3355(5) 0.1647(5) 0.037(2) Uani 1 1 d . . . C25 C 0.7182(7) 0.2788(5) 0.2102(5) 0.033(2) Uani 1 1 d . . . C26 C 0.7674(7) 0.3880(6) 0.1601(5) 0.039(2) Uani 1 1 d . . . C27 C 0.8549(7) 0.3848(6) 0.2007(5) 0.039(2) Uani 1 1 d . . . C28 C 0.8676(7) 0.3262(5) 0.2441(5) 0.034(2) Uani 1 1 d . . . C29 C 0.9335(8) 0.4378(6) 0.1961(6) 0.048(3) Uani 1 1 d . . . H29A H 0.9058 0.4835 0.1806 0.058 Uiso 1 1 calc R . . H29B H 0.9780 0.4214 0.1606 0.058 Uiso 1 1 calc R . . C30 C 0.9899(8) 0.4491(6) 0.2662(6) 0.048(3) Uani 1 1 d . . . H30A H 1.0479 0.4784 0.2596 0.058 Uiso 1 1 calc R . . H30B H 0.9494 0.4749 0.2991 0.058 Uiso 1 1 calc R . . C31 C 1.0196(7) 0.3783(6) 0.2965(6) 0.042(2) Uani 1 1 d . . . C32 C 0.9602(7) 0.3198(5) 0.2871(5) 0.036(2) Uani 1 1 d . . . C33 C 1.1066(8) 0.3722(6) 0.3381(6) 0.047(3) Uani 1 1 d . . . H33 H 1.1494 0.4117 0.3434 0.056 Uiso 1 1 calc R . . C34 C 1.1295(8) 0.3103(6) 0.3704(6) 0.046(3) Uani 1 1 d . . . H34 H 1.1872 0.3077 0.3993 0.055 Uiso 1 1 calc R . . C35 C 1.0693(6) 0.2505(5) 0.3618(5) 0.035(2) Uani 1 1 d . . . C36 C 0.9838(6) 0.2567(5) 0.3185(5) 0.034(2) Uani 1 1 d . . . H36 H 0.9422 0.2167 0.3110 0.041 Uiso 1 1 calc R . . C37 C 1.0910(6) 0.1835(5) 0.3970(5) 0.031(2) Uani 1 1 d . . . C38 C 1.1252(6) 0.1857(6) 0.4665(5) 0.039(2) Uani 1 1 d . . . H38 H 1.1399 0.2294 0.4905 0.047 Uiso 1 1 calc R . . C39 C 1.0747(6) 0.1186(6) 0.3614(5) 0.038(2) Uani 1 1 d . . . H39 H 1.0550 0.1182 0.3130 0.045 Uiso 1 1 calc R . . C40 C 1.1374(6) 0.1197(6) 0.5001(5) 0.036(2) Uani 1 1 d . . . C41 C 1.1694(6) 0.1071(6) 0.5743(5) 0.042(3) Uani 1 1 d . . . C42 C 1.1983(7) 0.1623(7) 0.6209(5) 0.044(3) Uani 1 1 d . . . H42 H 1.1989 0.2104 0.6068 0.053 Uiso 1 1 calc R . . C43 C 1.2273(7) 0.1427(8) 0.6914(6) 0.052(3) Uani 1 1 d . . . H43 H 1.2488 0.1780 0.7249 0.062 Uiso 1 1 calc R . . C44 C 1.2237(7) 0.0746(7) 0.7092(6) 0.049(3) Uani 1 1 d . . . H44 H 1.2412 0.0616 0.7559 0.058 Uiso 1 1 calc R . . C45 C 1.1948(7) 0.0229(7) 0.6602(6) 0.050(3) Uani 1 1 d . . . H45 H 1.1930 -0.0252 0.6742 0.060 Uiso 1 1 calc R . . C46 C 1.0870(6) 0.0543(6) 0.3959(5) 0.038(2) Uani 1 1 d . . . C47 C 1.0722(7) -0.0177(6) 0.3691(5) 0.038(2) Uani 1 1 d . . . C48 C 1.0426(7) -0.0348(6) 0.3017(5) 0.039(2) Uani 1 1 d . . . H48 H 1.0318 0.0015 0.2684 0.047 Uiso 1 1 calc R . . C49 C 1.0285(7) -0.1054(6) 0.2821(6) 0.046(3) Uani 1 1 d . . . H49 H 1.0078 -0.1181 0.2354 0.056 Uiso 1 1 calc R . . C50 C 1.0447(7) -0.1568(6) 0.3311(6) 0.047(3) Uani 1 1 d . . . H50 H 1.0349 -0.2056 0.3189 0.056 Uiso 1 1 calc R . . C51 C 1.0754(7) -0.1366(6) 0.3983(6) 0.045(3) Uani 1 1 d . . . H51 H 1.0881 -0.1725 0.4316 0.053 Uiso 1 1 calc R . . C52 C 0.7458(7) 0.4507(5) 0.1131(5) 0.038(2) Uani 1 1 d . . . C53 C 0.6823(7) 0.5010(6) 0.1343(5) 0.040(2) Uani 1 1 d . . . H53 H 0.6572 0.4982 0.1793 0.048 Uiso 1 1 calc R . . C54 C 0.6539(7) 0.5568(6) 0.0902(6) 0.042(2) Uani 1 1 d . . . C55 C 0.6928(7) 0.5581(6) 0.0251(5) 0.042(2) Uani 1 1 d . . . H55 H 0.6742 0.5950 -0.0058 0.051 Uiso 1 1 calc R . . C56 C 0.7573(8) 0.5080(6) 0.0033(6) 0.042(2) Uani 1 1 d . . . C57 C 0.7821(8) 0.4528(5) 0.0481(6) 0.042(2) Uani 1 1 d . . . H57 H 0.8243 0.4166 0.0336 0.051 Uiso 1 1 calc R . . C58 C 0.5813(8) 0.6128(6) 0.1116(6) 0.047(3) Uani 1 1 d . . . C59 C 0.5358(9) 0.5955(7) 0.1806(6) 0.057(3) Uani 1 1 d . . . H59A H 0.5036 0.5491 0.1761 0.086 Uiso 1 1 calc R . . H59B H 0.4885 0.6320 0.1912 0.086 Uiso 1 1 calc R . . H59C H 0.5861 0.5945 0.2185 0.086 Uiso 1 1 calc R . . C60 C 0.6339(10) 0.6846(7) 0.1222(8) 0.065(4) Uani 1 1 d . . . H60A H 0.6822 0.6815 0.1613 0.097 Uiso 1 1 calc R . . H60B H 0.5873 0.7216 0.1325 0.097 Uiso 1 1 calc R . . H60C H 0.6658 0.6963 0.0795 0.097 Uiso 1 1 calc R . . C61 C 0.5016(9) 0.6178(8) 0.0532(7) 0.067(4) Uani 1 1 d . . . H61A H 0.5297 0.6326 0.0100 0.100 Uiso 1 1 calc R . . H61B H 0.4538 0.6528 0.0668 0.100 Uiso 1 1 calc R . . H61C H 0.4703 0.5713 0.0456 0.100 Uiso 1 1 calc R . . C62 C 0.7941(10) 0.5106(7) -0.0723(6) 0.055(3) Uani 1 1 d . . . C63 C 0.8345(12) 0.5833(7) -0.0858(9) 0.078(5) Uani 1 1 d . . . H63A H 0.8972 0.5892 -0.0602 0.117 Uiso 1 1 calc R . . H63B H 0.7902 0.6196 -0.0700 0.117 Uiso 1 1 calc R . . H63C H 0.8425 0.5881 -0.1360 0.117 Uiso 1 1 calc R . . C64 C 0.7044(15) 0.5040(14) -0.1258(9) 0.132(9) Uani 1 1 d . . . H64A H 0.7256 0.5075 -0.1735 0.198 Uiso 1 1 calc R . . H64B H 0.6592 0.5424 -0.1167 0.198 Uiso 1 1 calc R . . H64C H 0.6725 0.4580 -0.1205 0.198 Uiso 1 1 calc R . . C65 C 0.863(2) 0.4586(12) -0.0859(10) 0.169(14) Uani 1 1 d . . . H65A H 0.9172 0.4628 -0.0507 0.253 Uiso 1 1 calc R . . H65B H 0.8870 0.4655 -0.1325 0.253 Uiso 1 1 calc R . . H65C H 0.8339 0.4113 -0.0839 0.253 Uiso 1 1 calc R . . C66 C 0.2740(15) 0.6958(14) 0.2407(13) 0.120(8) Uani 1 1 d . . . H66 H 0.2270 0.6741 0.2676 0.144 Uiso 1 1 calc R . . C67 C 0.1412(12) 0.7400(11) 0.1641(14) 0.134(10) Uani 1 1 d . . . H67A H 0.1026 0.7160 0.1979 0.201 Uiso 1 1 calc R . . H67B H 0.1259 0.7198 0.1172 0.201 Uiso 1 1 calc R . . H67C H 0.1266 0.7908 0.1646 0.201 Uiso 1 1 calc R . . C68 C 0.3116(18) 0.7609(11) 0.1380(16) 0.161(13) Uani 1 1 d . . . H68A H 0.2943 0.8103 0.1289 0.242 Uiso 1 1 calc R . . H68B H 0.3105 0.7338 0.0937 0.242 Uiso 1 1 calc R . . H68C H 0.3764 0.7593 0.1609 0.242 Uiso 1 1 calc R . . C69 C 0.1291(8) 0.9003(6) 0.8089(5) 0.044(3) Uani 1 1 d . . . H69 H 0.1680 0.8616 0.7954 0.053 Uiso 1 1 calc R . . C70 C 0.2704(9) 0.9433(7) 0.8787(7) 0.061(3) Uani 1 1 d . . . H70A H 0.2742 0.9426 0.9299 0.091 Uiso 1 1 calc R . . H70B H 0.3069 0.9842 0.8630 0.091 Uiso 1 1 calc R . . H70C H 0.2978 0.8994 0.8603 0.091 Uiso 1 1 calc R . . C71 C 0.1159(8) 1.0088(6) 0.8780(6) 0.049(3) Uani 1 1 d . . . H71A H 0.0484 1.0045 0.8604 0.073 Uiso 1 1 calc R . . H71B H 0.1436 1.0529 0.8611 0.073 Uiso 1 1 calc R . . H71C H 0.1193 1.0098 0.9292 0.073 Uiso 1 1 calc R . . C72 C 0.135(2) 0.7916(15) 0.9810(15) 0.152(11) Uani 1 1 d . . . H72 H 0.1608 0.8308 1.0081 0.182 Uiso 1 1 calc R . . C73 C 0.0150(16) 0.7495(10) 0.8989(10) 0.111(7) Uani 1 1 d . . . H73A H 0.0581 0.7085 0.8973 0.166 Uiso 1 1 calc R . . H73B H 0.0097 0.7714 0.8528 0.166 Uiso 1 1 calc R . . H73C H -0.0489 0.7337 0.9116 0.166 Uiso 1 1 calc R . . C74 C 0.0000(16) 0.8631(9) 0.9613(12) 0.117(8) Uani 1 1 d . . . H74A H 0.0377 0.8955 0.9930 0.176 Uiso 1 1 calc R . . H74B H -0.0606 0.8509 0.9821 0.176 Uiso 1 1 calc R . . H74C H -0.0140 0.8862 0.9165 0.176 Uiso 1 1 calc R . . C75 C 0.1139(10) 0.2499(8) 0.8179(9) 0.075(4) Uani 1 1 d . . . H75 H 0.1151 0.2636 0.7704 0.090 Uiso 1 1 calc R . . C76 C 0.1021(15) 0.2855(12) 0.9355(10) 0.113(7) Uani 1 1 d . . . H76A H 0.1534 0.2520 0.9485 0.170 Uiso 1 1 calc R . . H76B H 0.0395 0.2648 0.9451 0.170 Uiso 1 1 calc R . . H76C H 0.1122 0.3298 0.9628 0.170 Uiso 1 1 calc R . . C77 C 0.0993(13) 0.3738(8) 0.8467(13) 0.112(7) Uani 1 1 d . . . H77A H 0.0948 0.3809 0.7961 0.168 Uiso 1 1 calc R . . H77B H 0.1574 0.3975 0.8673 0.168 Uiso 1 1 calc R . . H77C H 0.0424 0.3939 0.8675 0.168 Uiso 1 1 calc R . . C78 C 0.4565(10) 0.0885(9) 0.8630(7) 0.074(4) Uani 1 1 d . . . H78 H 0.5216 0.0737 0.8614 0.088 Uiso 1 1 calc R . . C79 C 0.4898(16) 0.101(2) 0.9888(9) 0.198(17) Uani 1 1 d . . . H79A H 0.4511 0.1054 1.0298 0.297 Uiso 1 1 calc R . . H79B H 0.5379 0.1397 0.9903 0.297 Uiso 1 1 calc R . . H79C H 0.5226 0.0554 0.9889 0.297 Uiso 1 1 calc R . . C80 C 0.3328(12) 0.1326(8) 0.9351(7) 0.077(5) Uani 1 1 d . . . H80A H 0.3002 0.1403 0.8892 0.116 Uiso 1 1 calc R . . H80B H 0.3369 0.1775 0.9618 0.116 Uiso 1 1 calc R . . H80C H 0.2963 0.0977 0.9605 0.116 Uiso 1 1 calc R . . C81 C 0.4307(13) 0.6856(8) 0.6035(8) 0.075(4) Uani 1 1 d . . . H81 H 0.4968 0.6916 0.6180 0.090 Uiso 1 1 calc R . . C82 C 0.4314(16) 0.5898(8) 0.6829(8) 0.098(6) Uani 1 1 d . . . H82A H 0.5014 0.5970 0.6865 0.147 Uiso 1 1 calc R . . H82B H 0.4166 0.5409 0.6672 0.147 Uiso 1 1 calc R . . H82C H 0.4054 0.5984 0.7288 0.147 Uiso 1 1 calc R . . C83 C 0.2860(13) 0.6295(14) 0.6121(12) 0.127(8) Uani 1 1 d . . . H83A H 0.2541 0.6758 0.6110 0.191 Uiso 1 1 calc R . . H83B H 0.2561 0.5993 0.6460 0.191 Uiso 1 1 calc R . . H83C H 0.2792 0.6069 0.5655 0.191 Uiso 1 1 calc R . . C84 C 0.6461(14) 0.5507(16) 0.5769(16) 0.147(10) Uani 1 1 d . . . H84 H 0.6458 0.5673 0.5303 0.176 Uiso 1 1 calc R . . C85 C 0.613(3) 0.4269(17) 0.550(3) 0.30(3) Uani 1 1 d . . . H85A H 0.6732 0.4095 0.5325 0.456 Uiso 1 1 calc R . . H85B H 0.5714 0.4442 0.5107 0.456 Uiso 1 1 calc R . . H85C H 0.5795 0.3882 0.5725 0.456 Uiso 1 1 calc R . . C86 C 0.637(3) 0.465(2) 0.6676(14) 0.25(2) Uani 1 1 d . . . H86A H 0.5725 0.4633 0.6849 0.381 Uiso 1 1 calc R . . H86B H 0.6760 0.5011 0.6941 0.381 Uiso 1 1 calc R . . H86C H 0.6677 0.4184 0.6733 0.381 Uiso 1 1 calc R . . C87 C 0.2772(10) 0.2423(7) 0.1024(7) 0.058(3) Uani 1 1 d . . . H87 H 0.2362 0.2070 0.0802 0.070 Uiso 1 1 calc R . . C88 C 0.2024(16) 0.2114(9) 0.2105(9) 0.103(6) Uani 1 1 d . . . H88A H 0.1480 0.1955 0.1792 0.154 Uiso 1 1 calc R . . H88B H 0.1789 0.2414 0.2481 0.154 Uiso 1 1 calc R . . H88C H 0.2351 0.1699 0.2306 0.154 Uiso 1 1 calc R . . C89 C 0.3333(13) 0.3022(9) 0.2103(9) 0.091(5) Uani 1 1 d . . . H89A H 0.3889 0.2770 0.2311 0.137 Uiso 1 1 calc R . . H89B H 0.2980 0.3251 0.2473 0.137 Uiso 1 1 calc R . . H89C H 0.3556 0.3384 0.1787 0.137 Uiso 1 1 calc R . . C90 C 0.8617(19) 0.3181(10) 0.5496(12) 0.123(8) Uani 1 1 d . . . H90 H 0.8574 0.2828 0.5134 0.148 Uiso 1 1 calc R . . C91 C 0.8974(11) 0.4399(7) 0.5837(9) 0.075(4) Uani 1 1 d . . . H91A H 0.8552 0.4296 0.6216 0.112 Uiso 1 1 calc R . . H91B H 0.8735 0.4815 0.5584 0.112 Uiso 1 1 calc R . . H91C H 0.9629 0.4495 0.6034 0.112 Uiso 1 1 calc R . . C92 C 0.9472(13) 0.3888(10) 0.4734(9) 0.091(5) Uani 1 1 d . . . H92A H 0.9387 0.3461 0.4435 0.137 Uiso 1 1 calc R . . H92B H 1.0160 0.3969 0.4850 0.137 Uiso 1 1 calc R . . H92C H 0.9203 0.4298 0.4485 0.137 Uiso 1 1 calc R . . Cl1 Cl 0.65267(18) -0.13980(15) 0.62730(14) 0.0458(6) Uani 1 1 d . . . Cl2 Cl 1.14575(17) -0.13494(16) 0.57155(14) 0.0488(7) Uani 1 1 d . . . F1 F 0.1728(8) 0.9110(5) 0.1584(5) 0.108(4) Uani 1 1 d . . . F2 F 0.2878(8) 0.9392(5) 0.0582(5) 0.101(3) Uani 1 1 d . . . F3 F 0.1326(7) 1.0100(10) 0.0669(6) 0.169(7) Uani 1 1 d . . . F4 F 0.2974(9) 1.0710(5) 0.1016(5) 0.115(4) Uani 1 1 d . . . F5 F 0.1812(8) 1.0429(5) 0.2005(5) 0.107(4) Uani 1 1 d . . . F6 F 0.3372(7) 0.9730(7) 0.1903(5) 0.107(4) Uani 1 1 d . . . F7 F 0.0982(7) 0.3566(7) 0.6416(8) 0.136(5) Uani 1 1 d . . . F8 F 0.2298(8) 0.3252(5) 0.5508(5) 0.103(3) Uani 1 1 d . . . F9 F 0.2721(6) 0.3196(5) 0.6854(4) 0.078(2) Uani 1 1 d . . . F10 F 0.3316(12) 0.4195(4) 0.6018(7) 0.170(7) Uani 1 1 d . . . F11 F 0.1713(8) 0.4566(5) 0.5655(6) 0.116(4) Uani 1 1 d . . . F12 F 0.2216(8) 0.4551(6) 0.7004(6) 0.106(3) Uani 1 1 d . . . N1 N 0.6569(5) 0.0273(4) 0.5815(4) 0.0307(17) Uani 1 1 d . . . N2 N 0.6043(5) -0.0072(4) 0.4534(4) 0.0276(16) Uani 1 1 d . . . N3 N 0.5861(5) -0.1426(4) 0.4595(4) 0.0324(17) Uani 1 1 d . . . N4 N 0.8010(6) 0.2746(4) 0.2491(4) 0.0363(19) Uani 1 1 d . . . N5 N 1.0879(5) -0.0696(5) 0.4183(4) 0.037(2) Uani 1 1 d . . . N6 N 1.1196(5) 0.0588(5) 0.4650(4) 0.0359(19) Uani 1 1 d . . . N7 N 1.1688(5) 0.0383(5) 0.5928(4) 0.037(2) Uani 1 1 d . . . N8 N 0.2434(11) 0.7301(8) 0.1830(10) 0.099(5) Uani 1 1 d . . . N9 N 0.1696(6) 0.9488(5) 0.8530(5) 0.044(2) Uani 1 1 d . . . N10 N 0.0534(12) 0.8005(7) 0.9501(8) 0.084(4) Uani 1 1 d . . . N11 N 0.1039(7) 0.3007(5) 0.8601(6) 0.055(3) Uani 1 1 d . . . N12 N 0.4280(8) 0.1064(8) 0.9260(5) 0.078(4) Uani 1 1 d . . . N13 N 0.3875(9) 0.6394(6) 0.6324(6) 0.065(3) Uani 1 1 d . . . N14 N 0.6317(11) 0.4817(10) 0.5979(9) 0.103(5) Uani 1 1 d . . . N15 N 0.2699(9) 0.2519(5) 0.1710(6) 0.062(3) Uani 1 1 d . . . N16 N 0.8985(8) 0.3793(5) 0.5361(6) 0.056(3) Uani 1 1 d . . . O1 O 0.3581(10) 0.6907(10) 0.2605(8) 0.139(6) Uani 1 1 d . . . O2 O 0.0460(6) 0.9014(5) 0.7845(4) 0.057(2) Uani 1 1 d . . . O3 O 0.1867(19) 0.7353(12) 0.9798(12) 0.217(11) Uani 1 1 d . . . O4 O 0.1222(7) 0.1864(5) 0.8263(5) 0.066(2) Uani 1 1 d . . . O5 O 0.4118(6) 0.0886(5) 0.8090(4) 0.057(2) Uani 1 1 d . . . O6 O 0.3991(9) 0.7260(5) 0.5571(5) 0.077(3) Uani 1 1 d . . . O7 O 0.6612(15) 0.5909(17) 0.639(2) 0.34(3) Uani 1 1 d . . . O8 O 0.3297(7) 0.2730(5) 0.0654(5) 0.069(3) Uani 1 1 d . . . O9 O 0.8308(15) 0.3025(8) 0.6090(8) 0.151(7) Uani 1 1 d . . . Pt1 Pt 0.62565(2) -0.06758(2) 0.533218(19) 0.03159(12) Uani 1 1 d . . . Pt2 Pt 1.12998(2) -0.02938(2) 0.51401(2) 0.03835(13) Uani 1 1 d . . . Sb1 Sb 0.23262(5) 0.99192(4) 0.12774(4) 0.0469(2) Uani 1 1 d . . . Sb2 Sb 0.22306(7) 0.38940(5) 0.62609(6) 0.0698(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.026(5) 0.059(7) 0.027(5) 0.011(5) 0.006(4) 0.007(4) C2 0.026(5) 0.073(8) 0.029(5) 0.003(5) 0.002(4) 0.005(5) C3 0.027(5) 0.055(6) 0.034(5) 0.002(5) 0.000(4) 0.007(4) C4 0.026(5) 0.047(6) 0.026(5) 0.011(4) 0.002(4) 0.003(4) C5 0.017(4) 0.037(5) 0.036(5) 0.008(4) 0.006(4) 0.007(4) C6 0.022(5) 0.049(6) 0.028(5) 0.005(4) 0.003(4) 0.009(4) C7 0.031(5) 0.034(5) 0.060(7) 0.013(5) 0.013(5) 0.001(4) C8 0.046(7) 0.043(6) 0.073(9) 0.009(6) 0.018(6) 0.000(5) C9 0.033(6) 0.048(7) 0.074(8) -0.013(6) 0.011(5) -0.002(5) C10 0.021(5) 0.055(7) 0.044(6) 0.005(5) 0.007(4) -0.001(4) C11 0.017(4) 0.045(6) 0.041(6) 0.007(4) 0.008(4) 0.005(4) C12 0.018(4) 0.044(6) 0.033(5) 0.003(4) 0.004(4) -0.002(4) C13 0.018(4) 0.049(6) 0.035(5) 0.024(4) -0.002(4) -0.006(4) C14 0.015(4) 0.042(5) 0.033(5) 0.005(4) 0.005(3) 0.005(4) C15 0.016(4) 0.045(6) 0.035(5) 0.006(4) 0.004(4) -0.001(4) C16 0.017(4) 0.044(5) 0.029(5) 0.010(4) -0.004(3) 0.001(4) C17 0.029(5) 0.035(5) 0.026(5) 0.009(4) -0.005(4) 0.001(4) C18 0.028(5) 0.043(6) 0.029(5) 0.008(4) -0.002(4) -0.003(4) C19 0.032(5) 0.050(6) 0.033(5) 0.013(4) -0.007(4) -0.002(4) C20 0.028(5) 0.053(6) 0.035(5) 0.008(5) -0.009(4) -0.004(4) C21 0.029(5) 0.044(6) 0.032(5) 0.010(4) 0.000(4) -0.007(4) C22 0.036(6) 0.068(8) 0.052(7) 0.026(6) -0.017(5) -0.011(5) C23 0.043(6) 0.056(7) 0.048(6) 0.029(5) -0.017(5) -0.009(5) C24 0.032(5) 0.038(5) 0.040(6) 0.014(4) -0.007(4) -0.004(4) C25 0.027(5) 0.043(6) 0.030(5) 0.011(4) -0.002(4) -0.003(4) C26 0.034(5) 0.045(6) 0.037(5) 0.020(4) -0.003(4) 0.007(4) C27 0.028(5) 0.048(6) 0.042(6) 0.010(5) -0.005(4) 0.003(4) C28 0.026(5) 0.042(5) 0.033(5) 0.008(4) -0.003(4) -0.005(4) C29 0.044(6) 0.045(6) 0.054(7) 0.020(5) -0.008(5) -0.014(5) C30 0.038(6) 0.046(6) 0.061(7) 0.015(5) -0.010(5) -0.007(5) C31 0.035(5) 0.045(6) 0.044(6) 0.006(5) -0.001(4) -0.008(5) C32 0.032(5) 0.043(6) 0.034(5) 0.004(4) 0.000(4) -0.001(4) C33 0.034(6) 0.049(6) 0.057(7) -0.001(5) -0.007(5) -0.008(5) C34 0.034(6) 0.060(7) 0.042(6) 0.003(5) -0.011(5) -0.001(5) C35 0.022(5) 0.047(6) 0.036(5) 0.008(4) -0.003(4) -0.002(4) C36 0.022(5) 0.046(6) 0.033(5) 0.006(4) -0.003(4) -0.003(4) C37 0.012(4) 0.041(5) 0.041(5) 0.002(4) 0.003(4) -0.004(4) C38 0.016(4) 0.057(7) 0.044(6) 0.003(5) -0.007(4) -0.003(4) C39 0.019(4) 0.064(7) 0.030(5) 0.015(5) 0.000(4) 0.003(4) C40 0.014(4) 0.056(6) 0.037(5) 0.011(5) -0.001(4) 0.003(4) C41 0.016(4) 0.073(8) 0.036(6) 0.004(5) 0.000(4) 0.008(5) C42 0.019(5) 0.078(8) 0.035(6) 0.013(5) -0.002(4) 0.008(5) C43 0.020(5) 0.097(10) 0.039(6) -0.003(6) 0.002(4) 0.008(5) C44 0.024(5) 0.086(9) 0.036(6) 0.021(6) 0.002(4) 0.013(5) C45 0.024(5) 0.090(9) 0.036(6) 0.017(6) 0.002(4) 0.015(5) C46 0.012(4) 0.067(7) 0.037(5) 0.016(5) 0.004(4) 0.005(4) C47 0.020(5) 0.059(7) 0.037(6) 0.009(5) 0.006(4) 0.006(4) C48 0.022(5) 0.058(7) 0.040(6) 0.010(5) 0.004(4) 0.006(4) C49 0.029(5) 0.065(8) 0.045(6) -0.006(5) 0.003(5) -0.004(5) C50 0.031(5) 0.049(6) 0.060(7) 0.011(5) 0.003(5) 0.001(5) C51 0.031(5) 0.052(7) 0.052(7) 0.011(5) 0.004(5) 0.005(5) C52 0.032(5) 0.037(5) 0.045(6) 0.021(5) -0.011(4) -0.002(4) C53 0.035(5) 0.047(6) 0.038(6) 0.022(5) -0.004(4) -0.004(5) C54 0.033(5) 0.049(6) 0.044(6) 0.015(5) -0.006(4) -0.007(5) C55 0.036(6) 0.052(6) 0.039(6) 0.022(5) -0.001(4) -0.004(5) C56 0.043(6) 0.039(6) 0.044(6) 0.009(5) -0.003(5) -0.001(5) C57 0.046(6) 0.034(5) 0.047(6) 0.013(5) 0.002(5) 0.001(5) C58 0.038(6) 0.058(7) 0.046(6) 0.019(5) 0.004(5) 0.003(5) C59 0.044(7) 0.077(9) 0.052(7) 0.022(6) 0.007(5) 0.016(6) C60 0.069(9) 0.049(7) 0.081(9) 0.014(6) 0.027(7) 0.013(6) C61 0.045(7) 0.096(11) 0.060(8) 0.027(7) -0.001(6) 0.017(7) C62 0.072(8) 0.053(7) 0.044(7) 0.014(5) 0.016(6) 0.002(6) C63 0.086(11) 0.065(9) 0.089(11) 0.021(8) 0.045(9) 0.014(8) C64 0.107(15) 0.24(3) 0.051(10) 0.012(13) 0.000(9) -0.070(17) C65 0.28(3) 0.138(18) 0.104(15) 0.084(14) 0.124(19) 0.14(2) C66 0.073(13) 0.16(2) 0.127(19) -0.053(17) -0.004(13) -0.005(13) C67 0.045(9) 0.106(15) 0.25(3) -0.059(17) -0.013(13) 0.009(9) C68 0.15(2) 0.080(14) 0.27(3) 0.025(17) 0.12(2) 0.033(14) C69 0.049(7) 0.050(6) 0.034(5) 0.005(5) -0.002(5) 0.018(5) C70 0.044(7) 0.065(8) 0.072(9) 0.003(7) -0.008(6) 0.004(6) C71 0.045(6) 0.052(7) 0.049(7) 0.011(5) 0.003(5) 0.003(5) C72 0.17(3) 0.12(2) 0.15(2) -0.035(18) -0.02(2) 0.04(2) C73 0.16(2) 0.075(12) 0.105(14) -0.008(11) 0.047(14) -0.009(12) C74 0.147(19) 0.068(11) 0.143(18) -0.026(11) 0.072(15) -0.022(12) C75 0.062(9) 0.069(10) 0.094(12) 0.001(9) 0.002(8) 0.009(7) C76 0.113(16) 0.139(18) 0.089(13) 0.003(12) 0.024(12) -0.011(14) C77 0.070(11) 0.057(10) 0.21(2) 0.003(12) 0.043(13) 0.000(8) C78 0.045(7) 0.128(14) 0.049(8) -0.022(8) 0.015(6) -0.018(8) C79 0.091(15) 0.45(5) 0.050(11) -0.05(2) -0.010(10) -0.04(2) C80 0.116(13) 0.062(9) 0.058(8) -0.008(7) 0.038(9) -0.010(8) C81 0.110(13) 0.054(8) 0.065(9) 0.001(7) 0.020(9) 0.000(8) C82 0.172(19) 0.064(10) 0.060(9) 0.022(7) 0.016(11) 0.016(11) C83 0.074(13) 0.18(2) 0.128(18) -0.048(16) 0.005(12) -0.002(13) C84 0.060(12) 0.18(3) 0.20(3) 0.04(2) 0.000(14) -0.046(15) C85 0.22(4) 0.16(3) 0.54(8) -0.23(4) 0.19(5) -0.07(3) C86 0.32(5) 0.35(5) 0.11(2) 0.12(3) 0.11(3) 0.22(4) C87 0.071(9) 0.056(7) 0.049(7) 0.012(6) 0.003(6) 0.023(6) C88 0.161(19) 0.086(12) 0.065(10) 0.022(9) 0.025(11) 0.002(12) C89 0.104(14) 0.083(11) 0.086(12) -0.015(9) 0.007(10) 0.010(10) C90 0.19(2) 0.065(12) 0.111(17) 0.014(11) -0.016(16) -0.010(13) C91 0.072(10) 0.054(8) 0.099(12) 0.012(8) 0.011(8) 0.017(7) C92 0.091(12) 0.102(13) 0.080(11) 0.009(9) 0.000(9) 0.029(10) Cl1 0.0363(13) 0.0555(16) 0.0469(15) 0.0211(12) 0.0045(11) 0.0139(11) Cl2 0.0254(12) 0.0726(19) 0.0498(15) 0.0265(13) 0.0045(11) 0.0065(12) F1 0.122(8) 0.104(7) 0.102(7) -0.016(6) 0.048(6) -0.063(6) F2 0.119(8) 0.106(7) 0.080(6) -0.026(5) 0.044(6) -0.022(6) F3 0.065(6) 0.34(2) 0.100(8) 0.088(11) -0.013(6) 0.049(9) F4 0.154(10) 0.089(7) 0.107(8) 0.024(6) 0.065(7) -0.039(7) F5 0.139(9) 0.074(6) 0.115(8) -0.021(5) 0.081(7) -0.021(6) F6 0.077(6) 0.184(11) 0.061(5) 0.048(6) 0.004(4) 0.006(6) F7 0.065(6) 0.145(10) 0.195(13) 0.047(9) -0.035(7) 0.008(6) F8 0.161(10) 0.068(5) 0.072(6) -0.002(4) -0.047(6) 0.016(6) F9 0.078(6) 0.084(6) 0.070(5) 0.000(4) -0.021(4) 0.022(4) F10 0.331(19) 0.034(4) 0.163(11) 0.000(5) 0.179(13) 0.013(7) F11 0.124(9) 0.089(7) 0.131(9) 0.031(6) -0.043(7) 0.038(6) F12 0.105(7) 0.102(7) 0.110(8) -0.032(6) -0.002(6) 0.040(6) N1 0.020(4) 0.040(4) 0.032(4) 0.012(3) 0.006(3) 0.005(3) N2 0.016(3) 0.033(4) 0.034(4) 0.012(3) 0.001(3) 0.004(3) N3 0.022(4) 0.040(5) 0.036(4) 0.004(3) 0.006(3) 0.007(3) N4 0.028(4) 0.045(5) 0.035(4) 0.013(4) -0.009(3) 0.000(4) N5 0.016(4) 0.060(6) 0.035(4) 0.014(4) 0.003(3) 0.007(4) N6 0.018(4) 0.063(6) 0.027(4) 0.007(4) 0.007(3) 0.001(4) N7 0.020(4) 0.062(6) 0.030(4) 0.017(4) 0.002(3) 0.009(4) N8 0.077(10) 0.076(9) 0.140(15) -0.028(10) -0.011(10) 0.006(8) N9 0.034(5) 0.053(6) 0.044(5) 0.005(4) 0.004(4) 0.002(4) N10 0.100(11) 0.063(8) 0.091(10) 0.001(7) 0.016(8) -0.002(8) N11 0.047(6) 0.050(6) 0.070(7) -0.003(5) 0.012(5) -0.006(5) N12 0.051(7) 0.141(12) 0.041(6) -0.013(7) 0.005(5) -0.033(7) N13 0.064(7) 0.062(7) 0.069(7) 0.002(6) 0.004(6) -0.004(6) N14 0.089(11) 0.119(13) 0.101(12) -0.024(10) 0.035(9) -0.028(10) N15 0.086(8) 0.046(6) 0.055(6) 0.013(5) 0.016(6) 0.018(6) N16 0.064(7) 0.047(6) 0.058(6) 0.006(5) 0.005(5) 0.008(5) O1 0.069(8) 0.215(18) 0.130(12) -0.058(12) -0.017(8) 0.008(10) O2 0.048(5) 0.067(5) 0.054(5) 0.000(4) -0.021(4) 0.008(4) O3 0.26(3) 0.177(19) 0.21(2) -0.052(16) -0.023(19) 0.123(19) O4 0.067(6) 0.046(5) 0.083(7) -0.001(4) -0.002(5) -0.004(4) O5 0.055(5) 0.080(6) 0.035(4) 0.000(4) 0.005(4) -0.007(4) O6 0.126(9) 0.053(5) 0.051(5) 0.014(4) 0.003(5) 0.003(5) O7 0.125(16) 0.36(4) 0.54(5) -0.36(4) 0.11(2) -0.12(2) O8 0.066(6) 0.082(7) 0.060(6) 0.022(5) 0.017(5) 0.020(5) O9 0.24(2) 0.114(11) 0.101(11) 0.018(9) 0.039(12) -0.068(12) Pt1 0.01909(18) 0.0416(2) 0.0350(2) 0.01283(16) 0.00512(14) 0.00820(14) Pt2 0.01761(18) 0.0633(3) 0.0351(2) 0.01638(18) 0.00363(14) 0.00856(16) Sb1 0.0407(4) 0.0606(5) 0.0400(4) 0.0113(3) 0.0045(3) -0.0056(3) Sb2 0.0598(6) 0.0666(6) 0.0800(7) -0.0012(5) -0.0234(5) 0.0194(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 121.1(9) . . ? C3 C2 C1 120.3(10) . . ? C2 C3 C4 119.0(10) . . ? C5 C4 C3 119.1(9) . . ? C4 C5 N1 122.2(9) . . ? C4 C5 C6 124.6(9) . . ? N1 C5 C6 113.1(8) . . ? N2 C6 C13 121.5(9) . . ? N2 C6 C5 114.0(8) . . ? C13 C6 C5 124.5(9) . . ? N3 C7 C8 121.1(11) . . ? C9 C8 C7 120.7(11) . . ? C8 C9 C10 119.0(11) . . ? C9 C10 C11 119.3(11) . . ? N3 C11 C10 120.3(9) . . ? N3 C11 C12 114.8(9) . . ? C10 C11 C12 124.8(9) . . ? N2 C12 C15 119.5(9) . . ? N2 C12 C11 112.4(8) . . ? C15 C12 C11 128.0(9) . . ? C6 C13 C14 116.1(9) . . ? C15 C14 C13 120.7(9) . . ? C15 C14 C16 121.2(9) . . ? C13 C14 C16 118.1(9) . . ? C14 C15 C12 118.9(9) . . ? C17 C16 C21 119.0(8) . . ? C17 C16 C14 120.1(8) . . ? C21 C16 C14 120.9(8) . . ? C18 C17 C16 120.1(8) . . ? C19 C18 C17 120.3(9) . . ? C19 C18 C25 119.7(9) . . ? C17 C18 C25 120.0(8) . . ? C20 C19 C18 118.9(9) . . ? C20 C19 C22 122.8(9) . . ? C18 C19 C22 118.2(9) . . ? C19 C20 C21 122.4(9) . . ? C20 C21 C16 119.2(9) . . ? C23 C22 C19 111.9(10) . . ? C22 C23 C24 111.9(9) . . ? C26 C24 C25 118.2(9) . . ? C26 C24 C23 123.4(9) . . ? C25 C24 C23 118.4(9) . . ? N4 C25 C24 122.5(9) . . ? N4 C25 C18 118.6(8) . . ? C24 C25 C18 118.9(8) . . ? C24 C26 C27 120.3(9) . . ? C24 C26 C52 118.9(9) . . ? C27 C26 C52 120.7(9) . . ? C28 C27 C26 116.8(9) . . ? C28 C27 C29 120.2(9) . . ? C26 C27 C29 122.9(9) . . ? N4 C28 C27 123.6(9) . . ? N4 C28 C32 117.7(8) . . ? C27 C28 C32 118.6(9) . . ? C27 C29 C30 111.7(9) . . ? C31 C30 C29 110.2(9) . . ? C32 C31 C33 118.9(10) . . ? C32 C31 C30 120.5(9) . . ? C33 C31 C30 120.5(9) . . ? C36 C32 C31 120.7(9) . . ? C36 C32 C28 120.2(9) . . ? C31 C32 C28 119.1(9) . . ? C34 C33 C31 120.7(10) . . ? C33 C34 C35 121.0(10) . . ? C34 C35 C36 117.7(9) . . ? C34 C35 C37 122.3(9) . . ? C36 C35 C37 120.0(9) . . ? C32 C36 C35 121.0(9) . . ? C38 C37 C39 120.8(9) . . ? C38 C37 C35 119.0(9) . . ? C39 C37 C35 120.2(9) . . ? C37 C38 C40 116.9(10) . . ? C46 C39 C37 120.9(9) . . ? N6 C40 C38 120.7(9) . . ? N6 C40 C41 111.5(9) . . ? C38 C40 C41 127.8(10) . . ? N7 C41 C42 122.8(10) . . ? N7 C41 C40 114.7(10) . . ? C42 C41 C40 122.5(11) . . ? C41 C42 C43 116.8(12) . . ? C44 C43 C42 119.5(12) . . ? C43 C44 C45 120.4(11) . . ? N7 C45 C44 122.5(12) . . ? N6 C46 C39 116.3(10) . . ? N6 C46 C47 114.3(9) . . ? C39 C46 C47 129.3(9) . . ? C48 C47 N5 121.2(10) . . ? C48 C47 C46 124.3(10) . . ? N5 C47 C46 114.4(9) . . ? C47 C48 C49 119.5(10) . . ? C50 C49 C48 119.1(11) . . ? C49 C50 C51 119.0(11) . . ? N5 C51 C50 122.9(10) . . ? C57 C52 C53 121.0(9) . . ? C57 C52 C26 120.1(10) . . ? C53 C52 C26 118.6(9) . . ? C52 C53 C54 120.6(10) . . ? C55 C54 C53 117.1(10) . . ? C55 C54 C58 121.0(9) . . ? C53 C54 C58 121.9(10) . . ? C56 C55 C54 122.8(10) . . ? C55 C56 C57 118.3(10) . . ? C55 C56 C62 119.9(10) . . ? C57 C56 C62 121.6(10) . . ? C52 C57 C56 120.1(10) . . ? C54 C58 C61 108.7(10) . . ? C54 C58 C60 108.7(9) . . ? C61 C58 C60 110.2(11) . . ? C54 C58 C59 112.6(9) . . ? C61 C58 C59 109.2(10) . . ? C60 C58 C59 107.5(11) . . ? C65 C62 C63 109.6(15) . . ? C65 C62 C56 113.6(11) . . ? C63 C62 C56 110.3(11) . . ? C65 C62 C64 111.2(18) . . ? C63 C62 C64 103.5(14) . . ? C56 C62 C64 108.2(11) . . ? O1 C66 N8 124(2) . . ? O2 C69 N9 125.3(10) . . ? N10 C72 O3 127(3) . . ? O4 C75 N11 132.0(17) . . ? O5 C78 N12 128.5(14) . . ? N13 C81 O6 128.0(18) . . ? N14 C84 O7 105(3) . . ? O8 C87 N15 127.5(14) . . ? O9 C90 N16 124(2) . . ? C1 N1 C5 118.1(9) . . ? C1 N1 Pt1 128.4(7) . . ? C5 N1 Pt1 113.4(6) . . ? C12 N2 C6 123.1(8) . . ? C12 N2 Pt1 119.0(7) . . ? C6 N2 Pt1 117.8(6) . . ? C7 N3 C11 119.6(9) . . ? C7 N3 Pt1 127.3(7) . . ? C11 N3 Pt1 113.1(7) . . ? C25 N4 C28 118.6(8) . . ? C51 N5 C47 118.3(9) . . ? C51 N5 Pt2 128.8(7) . . ? C47 N5 Pt2 112.9(7) . . ? C40 N6 C46 124.2(9) . . ? C40 N6 Pt2 119.3(7) . . ? C46 N6 Pt2 116.3(7) . . ? C41 N7 C45 118.0(10) . . ? C41 N7 Pt2 113.9(7) . . ? C45 N7 Pt2 128.1(9) . . ? C66 N8 C68 121(2) . . ? C66 N8 C67 122(2) . . ? C68 N8 C67 117(2) . . ? C69 N9 C71 121.6(9) . . ? C69 N9 C70 121.2(10) . . ? C71 N9 C70 117.1(10) . . ? C72 N10 C74 121(2) . . ? C72 N10 C73 120.8(19) . . ? C74 N10 C73 118.0(18) . . ? C75 N11 C77 128.8(16) . . ? C75 N11 C76 118.6(15) . . ? C77 N11 C76 112.5(15) . . ? C78 N12 C80 121.2(12) . . ? C78 N12 C79 122.8(15) . . ? C80 N12 C79 116.0(14) . . ? C81 N13 C83 117.3(17) . . ? C81 N13 C82 125.0(15) . . ? C83 N13 C82 117.5(16) . . ? C86 N14 C84 121(3) . . ? C86 N14 C85 117(3) . . ? C84 N14 C85 122(3) . . ? C87 N15 C89 120.3(13) . . ? C87 N15 C88 122.4(13) . . ? C89 N15 C88 117.2(13) . . ? C90 N16 C92 120.3(16) . . ? C90 N16 C91 123.2(15) . . ? C92 N16 C91 116.5(12) . . ? N2 Pt1 N3 80.7(4) . . ? N2 Pt1 N1 81.6(4) . . ? N3 Pt1 N1 162.3(3) . . ? N2 Pt1 Cl1 179.3(2) . . ? N3 Pt1 Cl1 99.0(3) . . ? N1 Pt1 Cl1 98.7(3) . . ? N6 Pt2 N7 80.6(4) . . ? N6 Pt2 N5 81.9(4) . . ? N7 Pt2 N5 162.4(3) . . ? N6 Pt2 Cl2 178.7(2) . . ? N7 Pt2 Cl2 99.6(3) . . ? N5 Pt2 Cl2 98.0(3) . . ? F3 Sb1 F4 91.6(7) . . ? F3 Sb1 F2 88.8(6) . . ? F4 Sb1 F2 90.1(5) . . ? F3 Sb1 F1 91.8(7) . . ? F4 Sb1 F1 176.5(6) . . ? F2 Sb1 F1 90.4(5) . . ? F3 Sb1 F5 93.7(7) . . ? F4 Sb1 F5 90.5(5) . . ? F2 Sb1 F5 177.4(5) . . ? F1 Sb1 F5 88.9(4) . . ? F3 Sb1 F6 179.5(5) . . ? F4 Sb1 F6 88.2(6) . . ? F2 Sb1 F6 90.7(5) . . ? F1 Sb1 F6 88.4(5) . . ? F5 Sb1 F6 86.7(6) . . ? F10 Sb2 F11 85.1(7) . . ? F10 Sb2 F9 96.1(6) . . ? F11 Sb2 F9 178.1(5) . . ? F10 Sb2 F12 92.4(5) . . ? F11 Sb2 F12 90.2(5) . . ? F9 Sb2 F12 91.2(5) . . ? F10 Sb2 F8 85.1(5) . . ? F11 Sb2 F8 89.6(5) . . ? F9 Sb2 F8 89.0(4) . . ? F12 Sb2 F8 177.5(5) . . ? F10 Sb2 F7 173.2(7) . . ? F11 Sb2 F7 89.9(5) . . ? F9 Sb2 F7 88.8(5) . . ? F12 Sb2 F7 92.3(6) . . ? F8 Sb2 F7 90.2(6) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.341(13) . ? C1 C2 1.385(16) . ? C2 C3 1.355(15) . ? C3 C4 1.396(14) . ? C4 C5 1.343(14) . ? C5 N1 1.382(12) . ? C5 C6 1.499(14) . ? C6 N2 1.341(13) . ? C6 C13 1.383(13) . ? C7 N3 1.338(13) . ? C7 C8 1.373(17) . ? C8 C9 1.367(18) . ? C9 C10 1.380(16) . ? C10 C11 1.394(15) . ? C11 N3 1.371(13) . ? C11 C12 1.481(14) . ? C12 N2 1.338(12) . ? C12 C15 1.394(13) . ? C13 C14 1.443(14) . ? C14 C15 1.383(14) . ? C14 C16 1.474(13) . ? C16 C17 1.401(13) . ? C16 C21 1.400(13) . ? C17 C18 1.389(13) . ? C18 C19 1.389(13) . ? C18 C25 1.478(13) . ? C19 C20 1.367(14) . ? C19 C22 1.508(14) . ? C20 C21 1.377(14) . ? C22 C23 1.479(17) . ? C23 C24 1.508(14) . ? C24 C26 1.385(14) . ? C24 C25 1.409(13) . ? C25 N4 1.339(12) . ? C26 C27 1.408(14) . ? C26 C52 1.520(13) . ? C27 C28 1.401(14) . ? C27 C29 1.482(14) . ? C28 N4 1.346(13) . ? C28 C32 1.495(13) . ? C29 C30 1.526(16) . ? C30 C31 1.515(15) . ? C31 C32 1.377(14) . ? C31 C33 1.417(15) . ? C32 C36 1.374(14) . ? C33 C34 1.363(16) . ? C34 C35 1.401(15) . ? C35 C36 1.417(13) . ? C35 C37 1.466(14) . ? C37 C38 1.388(14) . ? C37 C39 1.400(15) . ? C38 C40 1.418(15) . ? C39 C46 1.398(15) . ? C40 N6 1.331(14) . ? C40 C41 1.489(14) . ? C41 N7 1.351(15) . ? C41 C42 1.398(16) . ? C42 C43 1.442(15) . ? C43 C44 1.336(18) . ? C44 C45 1.380(18) . ? C45 N7 1.357(13) . ? C46 N6 1.376(13) . ? C46 C47 1.450(16) . ? C47 C48 1.364(15) . ? C47 N5 1.380(13) . ? C48 C49 1.384(16) . ? C49 C50 1.372(16) . ? C50 C51 1.377(16) . ? C51 N5 1.320(15) . ? C52 C57 1.370(15) . ? C52 C53 1.372(15) . ? C53 C54 1.405(14) . ? C54 C55 1.386(15) . ? C54 C58 1.532(16) . ? C55 C56 1.381(15) . ? C56 C57 1.392(14) . ? C56 C62 1.565(16) . ? C58 C61 1.533(16) . ? C58 C60 1.536(18) . ? C58 C59 1.537(16) . ? C62 C65 1.41(2) . ? C62 C63 1.508(18) . ? C62 C64 1.57(2) . ? C66 O1 1.21(2) . ? C66 N8 1.34(3) . ? C67 N8 1.46(2) . ? C68 N8 1.44(3) . ? C69 O2 1.222(13) . ? C69 N9 1.331(14) . ? C70 N9 1.465(15) . ? C71 N9 1.448(14) . ? C72 N10 1.26(3) . ? C72 O3 1.29(3) . ? C73 N10 1.44(2) . ? C74 N10 1.42(2) . ? C75 O4 1.215(17) . ? C75 N11 1.255(18) . ? C76 N11 1.48(2) . ? C77 N11 1.405(19) . ? C78 O5 1.176(15) . ? C78 N12 1.329(16) . ? C79 N12 1.44(2) . ? C80 N12 1.43(2) . ? C81 N13 1.215(18) . ? C81 O6 1.244(17) . ? C82 N13 1.467(19) . ? C83 N13 1.45(2) . ? C84 N14 1.38(3) . ? C84 O7 1.40(3) . ? C85 N14 1.38(3) . ? C86 N14 1.38(3) . ? C87 O8 1.199(15) . ? C87 N15 1.334(16) . ? C88 N15 1.46(2) . ? C89 N15 1.457(19) . ? C90 O9 1.28(2) . ? C90 N16 1.30(2) . ? C91 N16 1.447(18) . ? C92 N16 1.425(19) . ? Cl1 Pt1 2.294(5) . ? Cl2 Pt2 2.297(6) . ? F1 Sb1 1.852(9) . ? F2 Sb1 1.850(9) . ? F3 Sb1 1.801(10) . ? F4 Sb1 1.828(9) . ? F5 Sb1 1.857(9) . ? F6 Sb1 1.872(10) . ? F7 Sb2 1.881(12) . ? F8 Sb2 1.871(10) . ? F9 Sb2 1.862(9) . ? F10 Sb2 1.702(14) . ? F11 Sb2 1.855(9) . ? F12 Sb2 1.869(10) . ? N1 Pt1 2.028(9) . ? N2 Pt1 1.933(8) . ? N3 Pt1 2.028(9) . ? N5 Pt2 2.023(10) . ? N6 Pt2 1.926(10) . ? N7 Pt2 2.004(10) . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -1.4(14) . . . . ? C1 C2 C3 C4 0.3(14) . . . . ? C2 C3 C4 C5 0.1(14) . . . . ? C3 C4 C5 N1 0.6(13) . . . . ? C3 C4 C5 C6 179.7(8) . . . . ? C4 C5 C6 N2 -178.8(8) . . . . ? N1 C5 C6 N2 0.4(11) . . . . ? C4 C5 C6 C13 2.0(14) . . . . ? N1 C5 C6 C13 -178.8(8) . . . . ? N3 C7 C8 C9 -0.4(16) . . . . ? C7 C8 C9 C10 -0.1(17) . . . . ? C8 C9 C10 C11 -0.5(15) . . . . ? C9 C10 C11 N3 1.4(14) . . . . ? C9 C10 C11 C12 179.3(9) . . . . ? N3 C11 C12 N2 -0.9(11) . . . . ? C10 C11 C12 N2 -178.9(8) . . . . ? N3 C11 C12 C15 177.1(8) . . . . ? C10 C11 C12 C15 -0.9(15) . . . . ? N2 C6 C13 C14 -1.7(13) . . . . ? C5 C6 C13 C14 177.4(8) . . . . ? C6 C13 C14 C15 3.0(12) . . . . ? C6 C13 C14 C16 -176.2(8) . . . . ? C13 C14 C15 C12 -2.6(13) . . . . ? C16 C14 C15 C12 176.6(8) . . . . ? N2 C12 C15 C14 0.8(13) . . . . ? C11 C12 C15 C14 -177.1(8) . . . . ? C15 C14 C16 C17 -139.8(9) . . . . ? C13 C14 C16 C17 39.4(12) . . . . ? C15 C14 C16 C21 39.7(13) . . . . ? C13 C14 C16 C21 -141.1(9) . . . . ? C21 C16 C17 C18 -0.1(14) . . . . ? C14 C16 C17 C18 179.4(9) . . . . ? C16 C17 C18 C19 0.8(15) . . . . ? C16 C17 C18 C25 -178.6(9) . . . . ? C17 C18 C19 C20 -0.4(16) . . . . ? C25 C18 C19 C20 179.0(10) . . . . ? C17 C18 C19 C22 -178.8(10) . . . . ? C25 C18 C19 C22 0.6(15) . . . . ? C18 C19 C20 C21 -0.8(17) . . . . ? C22 C19 C20 C21 177.6(11) . . . . ? C19 C20 C21 C16 1.6(16) . . . . ? C17 C16 C21 C20 -1.1(15) . . . . ? C14 C16 C21 C20 179.4(9) . . . . ? C20 C19 C22 C23 144.9(11) . . . . ? C18 C19 C22 C23 -36.7(15) . . . . ? C19 C22 C23 C24 51.8(14) . . . . ? C22 C23 C24 C26 144.6(11) . . . . ? C22 C23 C24 C25 -33.5(15) . . . . ? C26 C24 C25 N4 0.7(16) . . . . ? C23 C24 C25 N4 178.8(10) . . . . ? C26 C24 C25 C18 179.4(10) . . . . ? C23 C24 C25 C18 -2.5(15) . . . . ? C19 C18 C25 N4 -161.4(10) . . . . ? C17 C18 C25 N4 18.0(14) . . . . ? C19 C18 C25 C24 19.9(15) . . . . ? C17 C18 C25 C24 -160.7(10) . . . . ? C25 C24 C26 C27 -0.9(16) . . . . ? C23 C24 C26 C27 -179.0(11) . . . . ? C25 C24 C26 C52 -178.1(10) . . . . ? C23 C24 C26 C52 3.8(17) . . . . ? C24 C26 C27 C28 1.0(16) . . . . ? C52 C26 C27 C28 178.2(10) . . . . ? C24 C26 C27 C29 177.5(11) . . . . ? C52 C26 C27 C29 -5.4(17) . . . . ? C26 C27 C28 N4 -0.9(16) . . . . ? C29 C27 C28 N4 -177.5(10) . . . . ? C26 C27 C28 C32 178.7(9) . . . . ? C29 C27 C28 C32 2.2(15) . . . . ? C28 C27 C29 C30 -35.6(15) . . . . ? C26 C27 C29 C30 148.0(11) . . . . ? C27 C29 C30 C31 50.0(13) . . . . ? C29 C30 C31 C32 -35.2(15) . . . . ? C29 C30 C31 C33 148.1(11) . . . . ? C33 C31 C32 C36 1.2(16) . . . . ? C30 C31 C32 C36 -175.6(10) . . . . ? C33 C31 C32 C28 179.2(10) . . . . ? C30 C31 C32 C28 2.4(15) . . . . ? N4 C28 C32 C36 13.5(14) . . . . ? C27 C28 C32 C36 -166.2(10) . . . . ? N4 C28 C32 C31 -164.5(10) . . . . ? C27 C28 C32 C31 15.8(15) . . . . ? C32 C31 C33 C34 -2.5(17) . . . . ? C30 C31 C33 C34 174.3(11) . . . . ? C31 C33 C34 C35 2.0(18) . . . . ? C33 C34 C35 C36 -0.3(16) . . . . ? C33 C34 C35 C37 -178.7(10) . . . . ? C31 C32 C36 C35 0.5(15) . . . . ? C28 C32 C36 C35 -177.4(9) . . . . ? C34 C35 C36 C32 -1.0(15) . . . . ? C37 C35 C36 C32 177.4(9) . . . . ? C34 C35 C37 C38 42.1(14) . . . . ? C36 C35 C37 C38 -136.4(10) . . . . ? C34 C35 C37 C39 -139.7(10) . . . . ? C36 C35 C37 C39 41.9(13) . . . . ? C39 C37 C38 C40 -3.5(13) . . . . ? C35 C37 C38 C40 174.8(8) . . . . ? C38 C37 C39 C46 3.8(13) . . . . ? C35 C37 C39 C46 -174.4(8) . . . . ? C37 C38 C40 N6 2.3(13) . . . . ? C37 C38 C40 C41 -177.7(9) . . . . ? N6 C40 C41 N7 -3.8(11) . . . . ? C38 C40 C41 N7 176.2(9) . . . . ? N6 C40 C41 C42 175.9(8) . . . . ? C38 C40 C41 C42 -4.2(15) . . . . ? N7 C41 C42 C43 -0.6(14) . . . . ? C40 C41 C42 C43 179.8(8) . . . . ? C41 C42 C43 C44 -1.2(14) . . . . ? C42 C43 C44 C45 1.6(15) . . . . ? C43 C44 C45 N7 -0.1(16) . . . . ? C37 C39 C46 N6 -2.7(13) . . . . ? C37 C39 C46 C47 178.7(9) . . . . ? N6 C46 C47 C48 -178.2(8) . . . . ? C39 C46 C47 C48 0.3(16) . . . . ? N6 C46 C47 N5 3.6(11) . . . . ? C39 C46 C47 N5 -177.8(9) . . . . ? N5 C47 C48 C49 -0.3(14) . . . . ? C46 C47 C48 C49 -178.3(9) . . . . ? C47 C48 C49 C50 -0.1(15) . . . . ? C48 C49 C50 C51 -0.5(15) . . . . ? C49 C50 C51 N5 1.7(16) . . . . ? C24 C26 C52 C57 -100.8(12) . . . . ? C27 C26 C52 C57 82.0(14) . . . . ? C24 C26 C52 C53 73.2(14) . . . . ? C27 C26 C52 C53 -104.0(12) . . . . ? C57 C52 C53 C54 -0.9(16) . . . . ? C26 C52 C53 C54 -174.8(9) . . . . ? C52 C53 C54 C55 0.1(15) . . . . ? C52 C53 C54 C58 178.5(10) . . . . ? C53 C54 C55 C56 -0.6(16) . . . . ? C58 C54 C55 C56 -179.1(10) . . . . ? C54 C55 C56 C57 1.9(16) . . . . ? C54 C55 C56 C62 176.9(10) . . . . ? C53 C52 C57 C56 2.2(16) . . . . ? C26 C52 C57 C56 176.0(9) . . . . ? C55 C56 C57 C52 -2.6(16) . . . . ? C62 C56 C57 C52 -177.5(10) . . . . ? C55 C54 C58 C61 50.2(14) . . . . ? C53 C54 C58 C61 -128.1(11) . . . . ? C55 C54 C58 C60 -69.7(13) . . . . ? C53 C54 C58 C60 111.9(12) . . . . ? C55 C54 C58 C59 171.3(10) . . . . ? C53 C54 C58 C59 -7.0(15) . . . . ? C55 C56 C62 C65 176.9(18) . . . . ? C57 C56 C62 C65 -8(2) . . . . ? C55 C56 C62 C63 53.4(15) . . . . ? C57 C56 C62 C63 -131.8(12) . . . . ? C55 C56 C62 C64 -59.1(17) . . . . ? C57 C56 C62 C64 115.7(15) . . . . ? C2 C1 N1 C5 2.0(13) . . . . ? C2 C1 N1 Pt1 179.6(7) . . . . ? C4 C5 N1 C1 -1.6(12) . . . . ? C6 C5 N1 C1 179.2(8) . . . . ? C4 C5 N1 Pt1 -179.6(7) . . . . ? C6 C5 N1 Pt1 1.2(9) . . . . ? C15 C12 N2 C6 0.5(13) . . . . ? C11 C12 N2 C6 178.7(8) . . . . ? C15 C12 N2 Pt1 -176.7(6) . . . . ? C11 C12 N2 Pt1 1.5(10) . . . . ? C13 C6 N2 C12 0.0(13) . . . . ? C5 C6 N2 C12 -179.2(7) . . . . ? C13 C6 N2 Pt1 177.3(7) . . . . ? C5 C6 N2 Pt1 -2.0(10) . . . . ? C8 C7 N3 C11 1.3(14) . . . . ? C8 C7 N3 Pt1 -178.6(8) . . . . ? C10 C11 N3 C7 -1.8(13) . . . . ? C12 C11 N3 C7 -179.9(8) . . . . ? C10 C11 N3 Pt1 178.1(7) . . . . ? C12 C11 N3 Pt1 0.0(9) . . . . ? C24 C25 N4 C28 -0.6(15) . . . . ? C18 C25 N4 C28 -179.3(9) . . . . ? C27 C28 N4 C25 0.7(15) . . . . ? C32 C28 N4 C25 -179.0(9) . . . . ? C50 C51 N5 C47 -2.1(14) . . . . ? C50 C51 N5 Pt2 178.9(7) . . . . ? C48 C47 N5 C51 1.4(13) . . . . ? C46 C47 N5 C51 179.6(8) . . . . ? C48 C47 N5 Pt2 -179.4(7) . . . . ? C46 C47 N5 Pt2 -1.2(10) . . . . ? C38 C40 N6 C46 -1.4(13) . . . . ? C41 C40 N6 C46 178.6(8) . . . . ? C38 C40 N6 Pt2 -176.5(7) . . . . ? C41 C40 N6 Pt2 3.5(10) . . . . ? C39 C46 N6 C40 1.6(13) . . . . ? C47 C46 N6 C40 -179.7(8) . . . . ? C39 C46 N6 Pt2 176.8(6) . . . . ? C47 C46 N6 Pt2 -4.4(10) . . . . ? C42 C41 N7 C45 2.0(14) . . . . ? C40 C41 N7 C45 -178.4(8) . . . . ? C42 C41 N7 Pt2 -177.2(7) . . . . ? C40 C41 N7 Pt2 2.4(10) . . . . ? C44 C45 N7 C41 -1.6(14) . . . . ? C44 C45 N7 Pt2 177.4(7) . . . . ? O1 C66 N8 C68 3(3) . . . . ? O1 C66 N8 C67 -174.9(19) . . . . ? O2 C69 N9 C71 1.3(17) . . . . ? O2 C69 N9 C70 -179.1(11) . . . . ? O3 C72 N10 C74 174(3) . . . . ? O3 C72 N10 C73 -10(5) . . . . ? O4 C75 N11 C77 176.7(16) . . . . ? O4 C75 N11 C76 1(3) . . . . ? O5 C78 N12 C80 -3(3) . . . . ? O5 C78 N12 C79 178(2) . . . . ? O6 C81 N13 C83 -1(2) . . . . ? O6 C81 N13 C82 174.9(14) . . . . ? O7 C84 N14 C86 -2(3) . . . . ? O7 C84 N14 C85 179(2) . . . . ? O8 C87 N15 C89 -3(2) . . . . ? O8 C87 N15 C88 179.5(14) . . . . ? O9 C90 N16 C92 169(2) . . . . ? O9 C90 N16 C91 -8(3) . . . . ? C12 N2 Pt1 N3 -1.2(6) . . . . ? C6 N2 Pt1 N3 -178.6(7) . . . . ? C12 N2 Pt1 N1 179.4(7) . . . . ? C6 N2 Pt1 N1 2.1(6) . . . . ? C7 N3 Pt1 N2 -179.5(8) . . . . ? C11 N3 Pt1 N2 0.6(6) . . . . ? C7 N3 Pt1 N1 -177.5(8) . . . . ? C11 N3 Pt1 N1 2.7(13) . . . . ? C7 N3 Pt1 Cl1 1.2(8) . . . . ? C11 N3 Pt1 Cl1 -178.7(6) . . . . ? C1 N1 Pt1 N2 -179.5(8) . . . . ? C5 N1 Pt1 N2 -1.7(6) . . . . ? C1 N1 Pt1 N3 178.5(8) . . . . ? C5 N1 Pt1 N3 -3.8(13) . . . . ? C1 N1 Pt1 Cl1 -0.2(8) . . . . ? C5 N1 Pt1 Cl1 177.6(5) . . . . ? C40 N6 Pt2 N7 -1.8(7) . . . . ? C46 N6 Pt2 N7 -177.3(7) . . . . ? C40 N6 Pt2 N5 178.4(7) . . . . ? C46 N6 Pt2 N5 3.0(6) . . . . ? C41 N7 Pt2 N6 -0.5(6) . . . . ? C45 N7 Pt2 N6 -179.6(8) . . . . ? C41 N7 Pt2 N5 0.2(14) . . . . ? C45 N7 Pt2 N5 -178.9(9) . . . . ? C41 N7 Pt2 Cl2 178.2(6) . . . . ? C45 N7 Pt2 Cl2 -0.9(8) . . . . ? C51 N5 Pt2 N6 178.2(9) . . . . ? C47 N5 Pt2 N6 -0.9(6) . . . . ? C51 N5 Pt2 N7 177.5(9) . . . . ? C47 N5 Pt2 N7 -1.6(13) . . . . ? C51 N5 Pt2 Cl2 -0.5(8) . . . . ? C47 N5 Pt2 Cl2 -179.6(6) . . . . ?
1100754.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100754.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100754 loop_ _publ_author_name 'James D. Crowley' 'Ian M. Steele' 'B. Bosnich' _publ_section_title ; Supramolecular Recognition Forces: An Examination of Weak Metal-Metal Interactions in Host-Guest Formation ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 2989 _journal_page_last 2991 _journal_paper_doi 10.1021/ic0481531 _journal_volume 44 _journal_year 2005 _chemical_absolute_configuration ad _chemical_formula_sum 'C18 H11 Au N2' _chemical_formula_weight 452.25 _chemical_name_systematic ; ? ; _space_group_IT_number 18 _symmetry_space_group_name_Hall 'P 2 2ab' _symmetry_space_group_name_H-M 'P 21 21 2' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 15.917(3) _cell_length_b 17.412(3) _cell_length_c 4.9587(10) _cell_measurement_temperature 100(2) _cell_volume 1374.3(4) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0872 _diffrn_reflns_av_sigmaI/netI 0.0438 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_number 34278 _diffrn_reflns_theta_full 30.50 _diffrn_reflns_theta_max 30.50 _diffrn_reflns_theta_min 3.74 _exptl_absorpt_coefficient_mu 10.697 _exptl_absorpt_correction_T_max 0.807 _exptl_absorpt_correction_T_min 0.220 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; absorption corrections were made based on correspondance of equivalent intensities usingprogram SADABS (G. Sheldrick, Bruker Analytical X-ray Systems, Madison, WI) ; _exptl_crystal_density_diffrn 2.186 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 848 _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _refine_diff_density_max 3.334 _refine_diff_density_min -4.249 _refine_diff_density_rms 0.243 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.227(16) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 190 _refine_ls_number_reflns 4179 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.043 _refine_ls_R_factor_all 0.0358 _refine_ls_R_factor_gt 0.0331 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0433P)^2^+5.4722P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0780 _refine_ls_wR_factor_ref 0.0787 _reflns_number_gt 3966 _reflns_number_total 4179 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic0481531si20041231_115410_2.cif _cod_data_source_block Au(2,6-diphpy)CN _cod_database_code 1100754 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.243867(11) 0.688572(11) 0.70790(4) 0.00547(6) Uani 1 1 d . . . C1 C 0.3276(4) 0.6051(4) 0.7499(14) 0.0125(13) Uani 1 1 d . . . C2 C 0.2895(4) 0.7623(4) 1.0009(13) 0.0108(12) Uani 1 1 d . . . C3 C 0.3560(4) 0.7541(4) 1.1760(14) 0.0111(12) Uani 1 1 d . . . H3 H 0.3893 0.7088 1.1691 0.013 Uiso 1 1 calc R . . C4 C 0.3756(4) 0.8117(4) 1.3650(13) 0.0137(11) Uani 1 1 d . . . H4 H 0.4218 0.8053 1.4840 0.016 Uiso 1 1 calc R . . C5 C 0.3267(4) 0.8783(4) 1.3770(15) 0.0136(12) Uani 1 1 d . . . H5 H 0.3400 0.9173 1.5042 0.016 Uiso 1 1 calc R . . C6 C 0.2580(4) 0.8881(3) 1.2018(12) 0.0112(10) Uani 1 1 d . . . H6 H 0.2244 0.9332 1.2088 0.013 Uiso 1 1 calc R . . C7 C 0.2404(4) 0.8295(3) 1.0169(11) 0.0082(10) Uani 1 1 d . . . C8 C 0.1683(4) 0.8358(3) 0.8274(14) 0.0110(12) Uani 1 1 d . . . C9 C 0.1103(4) 0.8955(3) 0.7983(16) 0.0135(11) Uani 1 1 d . . . H9 H 0.1135 0.9399 0.9088 0.016 Uiso 1 1 calc R . . C10 C 0.0482(4) 0.8884(4) 0.6052(16) 0.0171(13) Uani 1 1 d . . . H10 H 0.0087 0.9288 0.5836 0.021 Uiso 1 1 calc R . . C11 C 0.0420(4) 0.8238(4) 0.4419(15) 0.0137(13) Uani 1 1 d . . . H11 H -0.0010 0.8200 0.3098 0.016 Uiso 1 1 calc R . . C12 C 0.1003(4) 0.7647(4) 0.4755(13) 0.0082(11) Uani 1 1 d . . . C13 C 0.1052(3) 0.6904(4) 0.3297(12) 0.0097(10) Uani 1 1 d . . . C14 C 0.0484(4) 0.6702(4) 0.1283(14) 0.0123(12) Uani 1 1 d . . . H14 H 0.0051 0.7047 0.0770 0.015 Uiso 1 1 calc R . . C15 C 0.0555(5) 0.5986(4) 0.0015(14) 0.0156(13) Uani 1 1 d . . . H15 H 0.0164 0.5841 -0.1341 0.019 Uiso 1 1 calc R . . C16 C 0.1194(5) 0.5488(4) 0.0738(16) 0.0178(14) Uani 1 1 d . . . H16 H 0.1235 0.4999 -0.0100 0.021 Uiso 1 1 calc R . . C17 C 0.1782(4) 0.5702(3) 0.2699(14) 0.0121(12) Uani 1 1 d . . . H17 H 0.2231 0.5364 0.3130 0.015 Uiso 1 1 calc R . . C18 C 0.1715(4) 0.6409(3) 0.4032(13) 0.0086(11) Uani 1 1 d . . . N1 N 0.1593(3) 0.7736(3) 0.6687(11) 0.0078(10) Uani 1 1 d . . . N2 N 0.3755(4) 0.5573(4) 0.7736(15) 0.0227(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.00152(8) 0.00637(9) 0.00852(10) 0.00241(7) 0.00160(6) -0.00001(7) C1 0.009(2) 0.011(3) 0.018(4) 0.005(2) 0.002(2) -0.002(2) C2 0.004(2) 0.012(3) 0.016(3) 0.007(2) 0.003(2) -0.001(2) C3 0.006(2) 0.015(3) 0.013(3) 0.005(2) 0.004(2) 0.002(2) C4 0.011(2) 0.019(3) 0.010(3) 0.004(3) 0.000(2) -0.006(3) C5 0.014(3) 0.014(3) 0.013(3) -0.003(2) 0.001(2) -0.009(2) C6 0.013(2) 0.006(2) 0.015(2) -0.0014(19) 0.006(3) -0.0009(19) C7 0.009(3) 0.006(2) 0.009(3) 0.0016(17) 0.001(2) 0.000(2) C8 0.010(2) 0.007(2) 0.015(3) 0.002(2) 0.003(2) -0.0007(19) C9 0.013(3) 0.008(2) 0.020(3) 0.001(3) -0.002(3) 0.002(2) C10 0.015(3) 0.013(3) 0.024(4) 0.002(3) -0.002(3) 0.006(2) C11 0.005(2) 0.015(3) 0.020(3) 0.005(3) -0.004(2) 0.003(2) C12 0.003(2) 0.011(3) 0.011(3) 0.002(2) 0.001(2) -0.002(2) C13 0.008(2) 0.010(2) 0.012(3) 0.005(2) 0.0028(19) -0.003(2) C14 0.010(3) 0.015(3) 0.011(3) 0.000(2) -0.003(2) -0.001(2) C15 0.013(3) 0.021(3) 0.013(4) -0.005(3) 0.000(2) -0.002(3) C16 0.016(3) 0.017(3) 0.021(4) -0.007(3) 0.005(3) -0.001(3) C17 0.010(2) 0.009(2) 0.017(3) 0.000(2) 0.003(2) 0.000(2) C18 0.007(2) 0.011(3) 0.008(3) 0.002(2) 0.005(2) -0.002(2) N1 0.009(2) 0.0026(19) 0.012(3) 0.0018(18) -0.001(2) -0.0001(16) N2 0.017(3) 0.016(3) 0.034(4) 0.010(3) 0.002(3) 0.003(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Au1 N1 179.4(3) . . ? C1 Au1 C2 98.3(3) . . ? N1 Au1 C2 81.1(2) . . ? C1 Au1 C18 99.0(3) . . ? N1 Au1 C18 81.5(2) . . ? C2 Au1 C18 162.7(2) . . ? N2 C1 Au1 179.9(8) . . ? C3 C2 C7 118.5(6) . . ? C3 C2 Au1 130.3(5) . . ? C7 C2 Au1 111.1(4) . . ? C2 C3 C4 121.0(6) . . ? C5 C4 C3 119.8(6) . . ? C4 C5 C6 120.4(6) . . ? C7 C6 C5 118.1(5) . . ? C6 C7 C2 122.1(6) . . ? C6 C7 C8 121.0(5) . . ? C2 C7 C8 117.0(5) . . ? N1 C8 C9 117.8(6) . . ? N1 C8 C7 113.1(5) . . ? C9 C8 C7 129.0(6) . . ? C10 C9 C8 118.6(6) . . ? C9 C10 C11 121.8(6) . . ? C10 C11 C12 118.7(6) . . ? N1 C12 C11 117.5(6) . . ? N1 C12 C13 114.2(5) . . ? C11 C12 C13 128.3(6) . . ? C14 C13 C18 121.1(6) . . ? C14 C13 C12 122.4(5) . . ? C18 C13 C12 116.5(5) . . ? C13 C14 C15 119.7(6) . . ? C16 C15 C14 120.0(6) . . ? C15 C16 C17 120.3(6) . . ? C16 C17 C18 120.7(6) . . ? C17 C18 C13 118.1(6) . . ? C17 C18 Au1 130.8(5) . . ? C13 C18 Au1 111.0(4) . . ? C8 N1 C12 125.5(5) . . ? C8 N1 Au1 117.7(4) . . ? C12 N1 Au1 116.7(4) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 C1 1.982(6) . ? Au1 N1 2.010(5) . ? Au1 C2 2.070(7) . ? Au1 C18 2.073(7) . ? C1 N2 1.136(9) . ? C2 C3 1.377(9) . ? C2 C7 1.409(8) . ? C3 C4 1.408(10) . ? C4 C5 1.399(10) . ? C5 C6 1.407(9) . ? C6 C7 1.400(7) . ? C7 C8 1.487(9) . ? C8 N1 1.346(8) . ? C8 C9 1.398(8) . ? C9 C10 1.381(10) . ? C10 C11 1.389(10) . ? C11 C12 1.396(8) . ? C12 N1 1.351(8) . ? C12 C13 1.484(9) . ? C13 C14 1.392(8) . ? C13 C18 1.412(8) . ? C14 C15 1.401(9) . ? C15 C16 1.384(10) . ? C16 C17 1.399(10) . ? C17 C18 1.401(8) . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Au1 C2 C3 -1.9(6) . . . . ? N1 Au1 C2 C3 178.0(6) . . . . ? C18 Au1 C2 C3 177.2(7) . . . . ? C1 Au1 C2 C7 179.9(4) . . . . ? N1 Au1 C2 C7 -0.3(4) . . . . ? C18 Au1 C2 C7 -1.1(11) . . . . ? C7 C2 C3 C4 -0.8(9) . . . . ? Au1 C2 C3 C4 -178.9(5) . . . . ? C2 C3 C4 C5 0.3(9) . . . . ? C3 C4 C5 C6 0.2(10) . . . . ? C4 C5 C6 C7 -0.1(9) . . . . ? C5 C6 C7 C2 -0.5(9) . . . . ? C5 C6 C7 C8 179.5(6) . . . . ? C3 C2 C7 C6 0.9(9) . . . . ? Au1 C2 C7 C6 179.4(5) . . . . ? C3 C2 C7 C8 -179.1(6) . . . . ? Au1 C2 C7 C8 -0.6(7) . . . . ? C6 C7 C8 N1 -178.4(5) . . . . ? C2 C7 C8 N1 1.6(8) . . . . ? C6 C7 C8 C9 0.4(10) . . . . ? C2 C7 C8 C9 -179.6(7) . . . . ? N1 C8 C9 C10 -1.5(10) . . . . ? C7 C8 C9 C10 179.8(6) . . . . ? C8 C9 C10 C11 0.3(11) . . . . ? C9 C10 C11 C12 0.2(11) . . . . ? C10 C11 C12 N1 0.6(9) . . . . ? C10 C11 C12 C13 178.8(6) . . . . ? N1 C12 C13 C14 178.5(6) . . . . ? C11 C12 C13 C14 0.2(10) . . . . ? N1 C12 C13 C18 -2.3(8) . . . . ? C11 C12 C13 C18 179.5(6) . . . . ? C18 C13 C14 C15 2.0(9) . . . . ? C12 C13 C14 C15 -178.8(6) . . . . ? C13 C14 C15 C16 -1.0(10) . . . . ? C14 C15 C16 C17 -1.2(11) . . . . ? C15 C16 C17 C18 2.4(11) . . . . ? C16 C17 C18 C13 -1.4(9) . . . . ? C16 C17 C18 Au1 177.7(5) . . . . ? C14 C13 C18 C17 -0.7(9) . . . . ? C12 C13 C18 C17 180.0(5) . . . . ? C14 C13 C18 Au1 179.9(5) . . . . ? C12 C13 C18 Au1 0.7(6) . . . . ? C1 Au1 C18 C17 1.2(6) . . . . ? N1 Au1 C18 C17 -178.6(6) . . . . ? C2 Au1 C18 C17 -177.8(7) . . . . ? C1 Au1 C18 C13 -179.6(4) . . . . ? N1 Au1 C18 C13 0.6(4) . . . . ? C2 Au1 C18 C13 1.4(11) . . . . ? C9 C8 N1 C12 2.4(9) . . . . ? C7 C8 N1 C12 -178.6(6) . . . . ? C9 C8 N1 Au1 179.2(5) . . . . ? C7 C8 N1 Au1 -1.9(7) . . . . ? C11 C12 N1 C8 -2.0(9) . . . . ? C13 C12 N1 C8 179.6(5) . . . . ? C11 C12 N1 Au1 -178.7(4) . . . . ? C13 C12 N1 Au1 2.8(7) . . . . ? C2 Au1 N1 C8 1.2(5) . . . . ? C18 Au1 N1 C8 -179.0(5) . . . . ? C2 Au1 N1 C12 178.3(5) . . . . ? C18 Au1 N1 C12 -2.0(5) . . . . ?
1100755.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $ #$Revision: 176435 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100755.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100755 loop_ _publ_author_name 'Panagiotis Angaridis' 'Jeff W. Kampf' 'Vincent L. Pecoraro' _publ_contact_author_address ; Chemistry Department University of Michigan 930 N.University Ann Arbor, MI 48109, USA ; _publ_contact_author_email vlpec@umich.edu _publ_contact_author_fax '(734) 936 7628' _publ_contact_author_name 'Vincent. L. Pecoraro' _publ_contact_author_phone '(734) 763 1519' _publ_section_title ; Multinuclear Fe(III) Complexes with Polydentate Ligands of the Family of Dicarboxyimidazoles: Nuclearity- and Topology-Controlled Syntheses and Magneto-Structural Correlations ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3626 _journal_page_last 3635 _journal_paper_doi 10.1021/ic0481879 _journal_volume 44 _journal_year 2005 _chemical_formula_moiety '2(C39 H53 N4 O6 Fe), 2.5(C2 H3 N)' _chemical_formula_sum 'C41.5 H56.75 Fe N5.25 O6' _chemical_formula_weight 781.02 _chemical_name_systematic ; ? ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 109.456(4) _cell_angle_beta 111.060(4) _cell_angle_gamma 90.560(4) _cell_formula_units_Z 4 _cell_length_a 15.1085(11) _cell_length_b 17.2305(13) _cell_length_c 18.5398(14) _cell_measurement_reflns_used 5529 _cell_measurement_temperature 113(2) _cell_measurement_theta_max 23.31 _cell_measurement_theta_min 2.86 _cell_volume 4200.6(6) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _diffrn_ambient_temperature 113(2) _diffrn_measured_fraction_theta_full 0.956 _diffrn_measured_fraction_theta_max 0.956 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1247 _diffrn_reflns_av_sigmaI/netI 0.0954 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 37984 _diffrn_reflns_theta_full 23.66 _diffrn_reflns_theta_max 23.66 _diffrn_reflns_theta_min 2.86 _exptl_absorpt_coefficient_mu 0.410 _exptl_absorpt_correction_T_max 0.9525 _exptl_absorpt_correction_T_min 0.8533 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Blessing, R. Acta Cryst. (1995) A51 33-38 Sheldrick, G. TWINABS (Version 1.05), Bruker Nonius scaling and corrections for twinned crystals University of Gottingen, Germany 2003. ; _exptl_crystal_colour green _exptl_crystal_density_diffrn 1.235 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 1666 _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.12 _refine_diff_density_max 0.963 _refine_diff_density_min -0.942 _refine_diff_density_rms 0.094 _refine_ls_extinction_coef 0.0022(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 0.981 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 1028 _refine_ls_number_reflns 26563 _refine_ls_number_restraints 87 _refine_ls_restrained_S_all 0.992 _refine_ls_R_factor_all 0.1202 _refine_ls_R_factor_gt 0.0751 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1378P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1898 _refine_ls_wR_factor_ref 0.2148 _reflns_number_gt 17077 _reflns_number_total 26563 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic0481879si20041222_050013_2.cif _cod_data_source_block compound1 _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_cell_volume 4200.6(5) _cod_original_formula_sum 'C41.50 H56.75 Fe N5.25 O6' _cod_database_code 1100755 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.35618(3) 0.34894(3) -0.00036(3) 0.01788(13) Uani 1 1 d . . . Fe2 Fe 0.85982(3) 0.15413(3) 0.00497(3) 0.01790(13) Uani 1 1 d . . . N1 N 0.34828(17) 0.23743(15) -0.09691(15) 0.0187(7) Uani 1 1 d . . . N2 N 0.48737(17) 0.38000(15) -0.00595(14) 0.0185(7) Uani 1 1 d . . . N3 N 0.44191(16) 0.30576(15) 0.09904(15) 0.0183(7) Uani 1 1 d . . . N4 N 0.53955(17) 0.31498(16) 0.22321(15) 0.0227(8) Uani 1 1 d . . . N5 N 0.85344(16) 0.19754(15) -0.09045(15) 0.0186(7) Uani 1 1 d . . . N6 N 0.98854(16) 0.11705(15) -0.00456(14) 0.0176(7) Uani 1 1 d . . . N7 N 0.94552(16) 0.26738(15) 0.10493(15) 0.0184(7) Uani 1 1 d . . . N8 N 1.04549(17) 0.34832(16) 0.23154(15) 0.0227(8) Uani 1 1 d . . . N9 N 0.6911(2) 0.1757(2) 0.3857(2) 0.0535(11) Uani 1 1 d . . . C1 C 0.2732(2) 0.20571(19) -0.16498(18) 0.0224(9) Uani 1 1 d . . . H1A H 0.2750 0.1532 -0.2028 0.027 Uiso 1 1 calc R . . C2 C 0.1868(2) 0.24263(19) -0.18900(18) 0.0194(9) Uani 1 1 d . . . C3 C 0.1802(2) 0.32431(19) -0.14499(18) 0.0191(9) Uani 1 1 d . . . C4 C 0.0914(2) 0.35614(19) -0.17188(18) 0.0194(9) Uani 1 1 d . . . C5 C 0.0194(2) 0.3058(2) -0.24302(19) 0.0238(9) Uani 1 1 d . . . H5A H -0.0391 0.3269 -0.2615 0.029 Uiso 1 1 calc R . . C6 C 0.0260(2) 0.2242(2) -0.29144(19) 0.0246(10) Uani 1 1 d . . . C7 C 0.1109(2) 0.1946(2) -0.26215(18) 0.0213(9) Uani 1 1 d . . . H7A H 0.1181 0.1402 -0.2925 0.026 Uiso 1 1 calc R . . C8 C 0.0801(2) 0.4435(2) -0.1201(2) 0.0242(10) Uani 1 1 d . . . C9 C 0.1537(2) 0.5104(2) -0.1132(2) 0.0270(10) Uani 1 1 d . . . H9A H 0.1434 0.5100 -0.1686 0.041 Uiso 1 1 calc R . . H9B H 0.2186 0.4988 -0.0874 0.041 Uiso 1 1 calc R . . H9C H 0.1461 0.5652 -0.0791 0.041 Uiso 1 1 calc R . . C10 C 0.0951(2) 0.4465(2) -0.03241(19) 0.0246(10) Uani 1 1 d . . . H10A H 0.0900 0.5025 0.0012 0.037 Uiso 1 1 calc R . . H10B H 0.1588 0.4327 -0.0066 0.037 Uiso 1 1 calc R . . H10C H 0.0460 0.4061 -0.0361 0.037 Uiso 1 1 calc R . . C11 C -0.0192(2) 0.4656(2) -0.1586(2) 0.0319(11) Uani 1 1 d . . . H11A H -0.0245 0.5204 -0.1228 0.048 Uiso 1 1 calc R . . H11B H -0.0682 0.4237 -0.1643 0.048 Uiso 1 1 calc R . . H11C H -0.0288 0.4668 -0.2133 0.048 Uiso 1 1 calc R . . C12 C -0.0568(2) 0.1766(2) -0.3741(2) 0.0341(11) Uani 1 1 d . . . C13 C -0.0423(3) 0.0861(2) -0.4110(2) 0.0508(15) Uani 1 1 d . . . H13A H -0.0990 0.0561 -0.4609 0.076 Uiso 1 1 calc R . . H13B H -0.0325 0.0593 -0.3702 0.076 Uiso 1 1 calc R . . H13C H 0.0141 0.0850 -0.4256 0.076 Uiso 1 1 calc R . . C14 C -0.0621(3) 0.2182(3) -0.4359(2) 0.0664(16) Uani 1 1 d . . . H14A H -0.1128 0.1863 -0.4896 0.100 Uiso 1 1 calc R . . H14B H -0.0005 0.2201 -0.4422 0.100 Uiso 1 1 calc R . . H14C H -0.0762 0.2750 -0.4157 0.100 Uiso 1 1 calc R . . C15 C -0.1521(2) 0.1748(2) -0.3628(2) 0.0446(13) Uani 1 1 d . . . H15A H -0.1661 0.2317 -0.3436 0.067 Uiso 1 1 calc R . . H15B H -0.1477 0.1494 -0.3218 0.067 Uiso 1 1 calc R . . H15C H -0.2034 0.1421 -0.4158 0.067 Uiso 1 1 calc R . . C16 C 0.4314(2) 0.1935(2) -0.0855(2) 0.0245(10) Uani 1 1 d . . . H16A H 0.4141 0.1383 -0.1305 0.029 Uiso 1 1 calc R . . H16B H 0.4503 0.1847 -0.0322 0.029 Uiso 1 1 calc R . . C17 C 0.5175(2) 0.24316(19) -0.0859(2) 0.0239(10) Uani 1 1 d . . . H17A H 0.5760 0.2432 -0.0392 0.029 Uiso 1 1 calc R . . H17B H 0.5270 0.2136 -0.1378 0.029 Uiso 1 1 calc R . . C18 C 0.5075(2) 0.33214(19) -0.07911(18) 0.0195(9) Uani 1 1 d . . . H18A H 0.5675 0.3594 -0.0759 0.023 Uiso 1 1 calc R . . H18B H 0.4549 0.3326 -0.1297 0.023 Uiso 1 1 calc R . . C19 C 0.5537(2) 0.43702(18) 0.05390(17) 0.0181(9) Uani 1 1 d . . . H19A H 0.6123 0.4444 0.0472 0.022 Uiso 1 1 calc R . . C20 C 0.5479(2) 0.49062(18) 0.12983(18) 0.0190(9) Uani 1 1 d . . . C21 C 0.4603(2) 0.50018(18) 0.14065(18) 0.0190(9) Uani 1 1 d . . . C22 C 0.4597(2) 0.55819(19) 0.21573(19) 0.0208(9) Uani 1 1 d . . . C23 C 0.5491(2) 0.5978(2) 0.2770(2) 0.0265(10) Uani 1 1 d . . . H23A H 0.5495 0.6354 0.3280 0.032 Uiso 1 1 calc R . . C24 C 0.6374(2) 0.58779(19) 0.27093(19) 0.0206(9) Uani 1 1 d . . . C25 C 0.6350(2) 0.53499(18) 0.19508(18) 0.0213(9) Uani 1 1 d . . . H25A H 0.6933 0.5284 0.1867 0.026 Uiso 1 1 calc R . . C26 C 0.3654(2) 0.57535(19) 0.22710(19) 0.0225(9) Uani 1 1 d . . . C27 C 0.3067(2) 0.4958(2) 0.2158(2) 0.0316(10) Uani 1 1 d . . . H27A H 0.3470 0.4684 0.2517 0.047 Uiso 1 1 calc R . . H27B H 0.2844 0.4580 0.1579 0.047 Uiso 1 1 calc R . . H27C H 0.2514 0.5102 0.2307 0.047 Uiso 1 1 calc R . . C28 C 0.3053(2) 0.6116(2) 0.1626(2) 0.0312(11) Uani 1 1 d . . . H28A H 0.2428 0.6189 0.1667 0.047 Uiso 1 1 calc R . . H28B H 0.2959 0.5734 0.1069 0.047 Uiso 1 1 calc R . . H28C H 0.3390 0.6656 0.1731 0.047 Uiso 1 1 calc R . . C29 C 0.3821(2) 0.6385(2) 0.3133(2) 0.0380(12) Uani 1 1 d . . . H29A H 0.4243 0.6188 0.3557 0.057 Uiso 1 1 calc R . . H29B H 0.3206 0.6448 0.3196 0.057 Uiso 1 1 calc R . . H29C H 0.4123 0.6924 0.3198 0.057 Uiso 1 1 calc R . . C30 C 0.7304(2) 0.6334(2) 0.34466(19) 0.0248(10) Uani 1 1 d . . . C31 C 0.8190(2) 0.6143(2) 0.3244(2) 0.0311(11) Uani 1 1 d . . . H31A H 0.8148 0.6304 0.2773 0.047 Uiso 1 1 calc R . . H31B H 0.8225 0.5547 0.3100 0.047 Uiso 1 1 calc R . . H31C H 0.8766 0.6458 0.3727 0.047 Uiso 1 1 calc R . . C32 C 0.7377(3) 0.6071(2) 0.4172(2) 0.0393(12) Uani 1 1 d . . . H32A H 0.7972 0.6360 0.4646 0.059 Uiso 1 1 calc R . . H32B H 0.7378 0.5469 0.4010 0.059 Uiso 1 1 calc R . . H32C H 0.6827 0.6215 0.4327 0.059 Uiso 1 1 calc R . . C33 C 0.7301(2) 0.7268(2) 0.3677(2) 0.0309(11) Uani 1 1 d . . . H33A H 0.6740 0.7417 0.3812 0.046 Uiso 1 1 calc R . . H33B H 0.7274 0.7426 0.3209 0.046 Uiso 1 1 calc R . . H33C H 0.7886 0.7564 0.4160 0.046 Uiso 1 1 calc R . . C34 C 0.2824(2) 0.2883(2) 0.0993(2) 0.0242(10) Uani 1 1 d . . . C35 C 0.3894(2) 0.29941(18) 0.14301(19) 0.0177(9) Uani 1 1 d . . . C36 C 0.5326(2) 0.31507(19) 0.15030(19) 0.0199(9) Uani 1 1 d . . . H36D H 0.5861 0.3211 0.1361 0.024 Uiso 1 1 calc R . . C37 C 0.4473(2) 0.30460(19) 0.22116(19) 0.0203(9) Uani 1 1 d . . . C38 C 0.6308(2) 0.3259(2) 0.2925(2) 0.0361(11) Uani 1 1 d . . . H38A H 0.6840 0.3359 0.2767 0.054 Uiso 1 1 calc R . . H38B H 0.6360 0.2756 0.3064 0.054 Uiso 1 1 calc R . . H38C H 0.6335 0.3736 0.3408 0.054 Uiso 1 1 calc R . . C39 C 0.4262(2) 0.3027(2) 0.2916(2) 0.0312(10) Uani 1 1 d . . . C40 C 0.7799(2) 0.18127(19) -0.15773(19) 0.0194(9) Uani 1 1 d . . . H40A H 0.7834 0.2069 -0.1949 0.023 Uiso 1 1 calc R . . C41 C 0.6911(2) 0.12720(19) -0.18276(19) 0.0188(9) Uani 1 1 d . . . C42 C 0.6827(2) 0.07581(19) -0.13997(18) 0.0166(9) Uani 1 1 d . . . C43 C 0.5932(2) 0.02567(18) -0.16644(18) 0.0174(9) Uani 1 1 d . . . C44 C 0.5220(2) 0.02659(19) -0.23708(18) 0.0188(9) Uani 1 1 d . . . H44A H 0.4630 -0.0083 -0.2562 0.023 Uiso 1 1 calc R . . C45 C 0.5282(2) 0.07427(19) -0.28357(18) 0.0181(9) Uani 1 1 d . . . C46 C 0.6143(2) 0.1255(2) -0.25381(19) 0.0204(9) Uani 1 1 d . . . H46A H 0.6215 0.1604 -0.2823 0.024 Uiso 1 1 calc R . . C47 C 0.5797(2) -0.02505(19) -0.11601(18) 0.0167(9) Uani 1 1 d . . . C48 C 0.6537(2) -0.08788(19) -0.1098(2) 0.0248(10) Uani 1 1 d . . . H48A H 0.6416 -0.1222 -0.0805 0.037 Uiso 1 1 calc R . . H48B H 0.7188 -0.0571 -0.0795 0.037 Uiso 1 1 calc R . . H48C H 0.6468 -0.1237 -0.1657 0.037 Uiso 1 1 calc R . . C49 C 0.5946(2) 0.0333(2) -0.02904(19) 0.0245(10) Uani 1 1 d . . . H49A H 0.5458 0.0705 -0.0322 0.037 Uiso 1 1 calc R . . H49B H 0.6584 0.0665 -0.0028 0.037 Uiso 1 1 calc R . . H49C H 0.5892 0.0007 0.0039 0.037 Uiso 1 1 calc R . . C50 C 0.4799(2) -0.0751(2) -0.15655(19) 0.0241(10) Uani 1 1 d . . . H50A H 0.4740 -0.1083 -0.1242 0.036 Uiso 1 1 calc R . . H50B H 0.4693 -0.1121 -0.2130 0.036 Uiso 1 1 calc R . . H50C H 0.4320 -0.0371 -0.1586 0.036 Uiso 1 1 calc R . . C51 C 0.4464(2) 0.0668(2) -0.36417(19) 0.0243(10) Uani 1 1 d . . . C52 C 0.4628(2) 0.1340(2) -0.3962(2) 0.0294(11) Uani 1 1 d . . . H52A H 0.4702 0.1890 -0.3541 0.044 Uiso 1 1 calc R . . H52B H 0.4077 0.1283 -0.4469 0.044 Uiso 1 1 calc R . . H52C H 0.5209 0.1282 -0.4082 0.044 Uiso 1 1 calc R . . C53 C 0.4377(3) -0.0189(2) -0.4301(2) 0.0348(11) Uani 1 1 d . . . H53A H 0.3800 -0.0273 -0.4798 0.052 Uiso 1 1 calc R . . H53B H 0.4333 -0.0625 -0.4081 0.052 Uiso 1 1 calc R . . H53C H 0.4943 -0.0213 -0.4445 0.052 Uiso 1 1 calc R . . C54 C 0.3514(2) 0.0755(2) -0.3507(2) 0.0358(11) Uani 1 1 d . . . H54A H 0.3584 0.1284 -0.3059 0.054 Uiso 1 1 calc R . . H54B H 0.3353 0.0293 -0.3357 0.054 Uiso 1 1 calc R . . H54C H 0.3000 0.0744 -0.4018 0.054 Uiso 1 1 calc R . . C55 C 0.9398(2) 0.2480(2) -0.07906(19) 0.0224(9) Uani 1 1 d . . . H55A H 0.9643 0.2921 -0.0233 0.027 Uiso 1 1 calc R . . H55B H 0.9232 0.2752 -0.1206 0.027 Uiso 1 1 calc R . . C56 C 1.0188(2) 0.1935(2) -0.0885(2) 0.0271(10) Uani 1 1 d . . . H56A H 1.0200 0.1828 -0.1440 0.033 Uiso 1 1 calc R . . H56B H 1.0816 0.2254 -0.0469 0.033 Uiso 1 1 calc R . . C57 C 1.0068(2) 0.10990(19) -0.07845(18) 0.0207(9) Uani 1 1 d . . . H57A H 0.9528 0.0724 -0.1279 0.025 Uiso 1 1 calc R . . H57B H 1.0656 0.0842 -0.0758 0.025 Uiso 1 1 calc R . . C58 C 1.0549(2) 0.10315(18) 0.05538(18) 0.0178(9) Uani 1 1 d . . . H58A H 1.1131 0.0914 0.0482 0.021 Uiso 1 1 calc R . . C59 C 1.0502(2) 0.10356(19) 0.13167(19) 0.0181(9) Uani 1 1 d . . . C60 C 0.9631(2) 0.10075(19) 0.14273(18) 0.0190(9) Uani 1 1 d . . . C61 C 0.9637(2) 0.0964(2) 0.21804(18) 0.0210(9) Uani 1 1 d . . . C62 C 1.0507(2) 0.0993(2) 0.27750(19) 0.0229(9) Uani 1 1 d . . . H62A H 1.0512 0.0976 0.3284 0.027 Uiso 1 1 calc R . . C63 C 1.1396(2) 0.10453(19) 0.26964(19) 0.0207(9) Uani 1 1 d . . . C64 C 1.1377(2) 0.10399(19) 0.19586(18) 0.0195(9) Uani 1 1 d . . . H64A H 1.1957 0.1039 0.1868 0.023 Uiso 1 1 calc R . . C65 C 0.8691(2) 0.0855(2) 0.2316(2) 0.0256(10) Uani 1 1 d . . . C66 C 0.8861(2) 0.0828(2) 0.3162(2) 0.0418(11) Uani 1 1 d . . . H66A H 0.9228 0.1356 0.3590 0.063 Uiso 1 1 calc R . . H66B H 0.9222 0.0372 0.3238 0.063 Uiso 1 1 calc R . . H66C H 0.8244 0.0736 0.3204 0.063 Uiso 1 1 calc R . . C67 C 0.8131(2) 0.1589(2) 0.2233(2) 0.0284(10) Uani 1 1 d . . . H67A H 0.7560 0.1534 0.2356 0.043 Uiso 1 1 calc R . . H67B H 0.7937 0.1582 0.1666 0.043 Uiso 1 1 calc R . . H67C H 0.8542 0.2115 0.2623 0.043 Uiso 1 1 calc R . . C68 C 0.8067(2) 0.0040(2) 0.1655(2) 0.0301(10) Uani 1 1 d . . . H68A H 0.8402 -0.0431 0.1720 0.045 Uiso 1 1 calc R . . H68B H 0.7942 0.0051 0.1102 0.045 Uiso 1 1 calc R . . H68C H 0.7457 -0.0020 0.1720 0.045 Uiso 1 1 calc R . . C69 C 1.2328(2) 0.1124(2) 0.34328(19) 0.0236(10) Uani 1 1 d . . . C70 C 1.3203(2) 0.1071(2) 0.3201(2) 0.0291(11) Uani 1 1 d . . . H70A H 1.3280 0.1532 0.3019 0.044 Uiso 1 1 calc R . . H70B H 1.3115 0.0541 0.2750 0.044 Uiso 1 1 calc R . . H70C H 1.3777 0.1108 0.3684 0.044 Uiso 1 1 calc R . . C71 C 1.2471(2) 0.1959(2) 0.4119(2) 0.0417(13) Uani 1 1 d . . . H71A H 1.3071 0.2020 0.4588 0.063 Uiso 1 1 calc R . . H71B H 1.1934 0.1987 0.4300 0.063 Uiso 1 1 calc R . . H71C H 1.2500 0.2408 0.3910 0.063 Uiso 1 1 calc R . . C72 C 1.2251(3) 0.0407(2) 0.3740(2) 0.0507(13) Uani 1 1 d . . . H72A H 1.2066 -0.0125 0.3273 0.076 Uiso 1 1 calc R . . H72B H 1.1765 0.0482 0.3984 0.076 Uiso 1 1 calc R . . H72C H 1.2872 0.0407 0.4159 0.076 Uiso 1 1 calc R . . C73 C 0.7876(2) 0.28351(19) 0.1060(2) 0.0221(9) Uani 1 1 d . . . C74 C 0.8933(2) 0.30593(19) 0.15063(19) 0.0182(9) Uani 1 1 d . . . C75 C 1.0369(2) 0.2962(2) 0.1563(2) 0.0265(10) Uani 1 1 d . . . H75A H 1.0899 0.2814 0.1413 0.032 Uiso 1 1 calc R . . C76 C 0.9532(2) 0.3554(2) 0.2281(2) 0.0247(10) Uani 1 1 d . . . C77 C 1.1372(2) 0.3884(2) 0.3002(2) 0.0377(12) Uani 1 1 d . . . H77A H 1.1412 0.3741 0.3481 0.057 Uiso 1 1 calc R . . H77B H 1.1417 0.4489 0.3152 0.057 Uiso 1 1 calc R . . H77C H 1.1899 0.3690 0.2833 0.057 Uiso 1 1 calc R . . C78 C 0.9325(2) 0.4058(2) 0.3011(2) 0.0345(11) Uani 1 1 d . . . C79 C 0.6205(3) 0.2498(3) 0.4939(2) 0.0542(14) Uani 1 1 d . . . H79A H 0.5571 0.2626 0.4658 0.081 Uiso 1 1 calc R . . H79B H 0.6629 0.3015 0.5337 0.081 Uiso 1 1 calc R . . H79C H 0.6145 0.2133 0.5232 0.081 Uiso 1 1 calc R . . C80 C 0.6603(3) 0.2085(2) 0.4335(2) 0.0355(11) Uani 1 1 d . . . O1 O 0.25470(13) 0.37327(12) -0.08048(12) 0.0187(6) Uani 1 1 d . . . O2 O 0.37858(14) 0.45842(13) 0.07961(12) 0.0213(6) Uani 1 1 d . . . O3 O 0.25546(14) 0.29811(13) 0.03071(13) 0.0225(6) Uani 1 1 d . . . O4 O 0.22969(14) 0.26991(14) 0.13153(14) 0.0286(7) Uani 1 1 d . . . O5 O 0.33391(15) 0.28925(14) 0.27838(14) 0.0341(7) Uani 1 1 d . . . H5B H 0.3003 0.2825 0.2289 0.041 Uiso 1 1 calc R . . O6 O 0.48752(18) 0.31283(18) 0.35869(15) 0.0530(9) Uani 1 1 d . . . O7 O 0.75739(14) 0.07178(12) -0.07689(12) 0.0198(6) Uani 1 1 d . . . O8 O 0.88108(14) 0.10091(12) 0.08323(12) 0.0192(6) Uani 1 1 d . . . O9 O 0.75918(14) 0.22582(13) 0.03679(13) 0.0224(6) Uani 1 1 d . . . O10 O 0.73494(14) 0.32347(13) 0.14012(14) 0.0286(7) Uani 1 1 d . . . O11 O 0.84080(15) 0.40650(14) 0.28813(14) 0.0370(8) Uani 1 1 d . . . H11D H 0.8074 0.3780 0.2384 0.055 Uiso 1 1 calc R . . O12 O 0.99534(18) 0.4427(2) 0.36780(16) 0.0635(11) Uani 1 1 d . . . C96 C 0.22811(14) 0.5805(6) 0.45860(19) 0.080(3) Uani 0.50 1 d PDU A 1 H96A H 0.2836 0.5564 0.4847 0.121 Uiso 0.50 1 calc PR A 1 H96B H 0.2501 0.6342 0.4586 0.121 Uiso 0.50 1 calc PR A 1 H96C H 0.1925 0.5428 0.4014 0.121 Uiso 0.50 1 calc PR A 1 C97 C 0.1643(4) 0.5930(9) 0.5060(5) 0.039(4) Uani 0.50 1 d PDU A 1 N97 N 0.0984(2) 0.6073(7) 0.5238(3) 0.030(3) Uani 0.50 1 d PDU A 1 C98 C 0.1302(2) 0.6028(4) 0.52149(17) 0.058(3) Uani 0.50 1 d PDU B 2 H98A H 0.1702 0.5749 0.5570 0.087 Uiso 0.50 1 calc PR B 2 H98B H 0.0636 0.5753 0.4964 0.087 Uiso 0.50 1 calc PR B 2 H98C H 0.1336 0.6612 0.5548 0.087 Uiso 0.50 1 calc PR B 2 C99 C 0.1616(4) 0.5987(5) 0.4625(3) 0.044(2) Uani 0.50 1 d PDU B 2 N98 N 0.1734(4) 0.6063(4) 0.3978(2) 0.079(3) Uani 0.50 1 d PDU B 2 N95 N 0.46050(11) 0.4955(6) 0.4981(4) 0.130(6) Uani 0.50 1 d PDU . 1 C95 C 0.46050(11) 0.4955(6) 0.4981(4) 0.130(6) Uani 0.50 1 d PU . 2 C94 C 0.35754(15) 0.5023(8) 0.4774(5) 0.148(6) Uani 0.50 1 d PDU . 2 H94A H 0.3312 0.4702 0.5018 0.222 Uiso 0.50 1 calc PR . 2 H94B H 0.3233 0.4803 0.4171 0.222 Uiso 0.50 1 calc PR . 2 H94C H 0.3498 0.5608 0.4997 0.222 Uiso 0.50 1 calc PR . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0131(2) 0.0165(2) 0.0274(2) 0.00839(19) 0.01101(18) 0.00820(19) Fe2 0.0124(2) 0.0198(2) 0.0263(2) 0.01126(19) 0.00996(18) 0.00693(19) N1 0.0183(12) 0.0157(13) 0.0291(13) 0.0109(11) 0.0140(10) 0.0099(11) N2 0.0188(13) 0.0165(13) 0.0227(13) 0.0081(11) 0.0096(11) 0.0121(11) N3 0.0141(12) 0.0171(14) 0.0279(13) 0.0082(11) 0.0126(10) 0.0069(11) N4 0.0156(13) 0.0252(15) 0.0290(14) 0.0135(12) 0.0070(11) 0.0055(12) N5 0.0152(12) 0.0180(14) 0.0297(13) 0.0111(11) 0.0144(10) 0.0072(11) N6 0.0131(13) 0.0197(13) 0.0265(13) 0.0112(11) 0.0120(11) 0.0103(11) N7 0.0134(13) 0.0163(14) 0.0273(13) 0.0080(11) 0.0097(11) 0.0061(11) N8 0.0182(13) 0.0171(14) 0.0313(14) 0.0065(12) 0.0099(11) 0.0065(12) N9 0.0529(19) 0.066(2) 0.0594(18) 0.0317(17) 0.0329(15) 0.0151(18) C1 0.0258(17) 0.0187(17) 0.0262(16) 0.0074(14) 0.0148(13) 0.0041(14) C2 0.0192(15) 0.0220(17) 0.0234(15) 0.0096(13) 0.0140(13) 0.0077(14) C3 0.0202(16) 0.0191(17) 0.0248(15) 0.0120(13) 0.0124(13) 0.0056(14) C4 0.0164(15) 0.0236(17) 0.0256(15) 0.0126(13) 0.0128(13) 0.0082(14) C5 0.0177(16) 0.0289(18) 0.0333(17) 0.0177(14) 0.0131(13) 0.0108(14) C6 0.0224(17) 0.0246(18) 0.0298(16) 0.0123(14) 0.0112(14) -0.0016(15) C7 0.0259(16) 0.0167(17) 0.0270(16) 0.0073(13) 0.0171(13) 0.0072(14) C8 0.0199(16) 0.0202(17) 0.0374(18) 0.0132(14) 0.0137(14) 0.0082(14) C9 0.0234(16) 0.0248(18) 0.0392(18) 0.0128(15) 0.0177(14) 0.0138(15) C10 0.0169(16) 0.0201(18) 0.0347(18) 0.0038(15) 0.0130(14) 0.0055(14) C11 0.0216(17) 0.032(2) 0.047(2) 0.0173(16) 0.0155(15) 0.0144(16) C12 0.0278(19) 0.026(2) 0.035(2) 0.0051(16) 0.0031(16) -0.0028(16) C13 0.027(2) 0.046(3) 0.051(2) -0.007(2) 0.0067(18) -0.0012(19) C14 0.066(3) 0.071(3) 0.041(2) 0.025(2) -0.007(2) -0.025(3) C15 0.025(2) 0.034(2) 0.061(2) 0.0120(19) 0.0064(18) 0.0052(17) C16 0.0220(16) 0.0245(18) 0.0259(17) 0.0080(14) 0.0088(14) 0.0140(15) C17 0.0125(15) 0.0194(18) 0.0341(18) 0.0027(15) 0.0091(14) 0.0065(14) C18 0.0180(15) 0.0213(17) 0.0216(15) 0.0065(13) 0.0113(13) 0.0071(14) C19 0.0187(15) 0.0238(17) 0.0204(15) 0.0129(13) 0.0123(12) 0.0129(14) C20 0.0229(16) 0.0104(16) 0.0266(16) 0.0077(13) 0.0117(13) 0.0052(13) C21 0.0227(16) 0.0126(16) 0.0295(16) 0.0098(13) 0.0166(13) 0.0108(13) C22 0.0177(15) 0.0210(17) 0.0319(16) 0.0127(14) 0.0158(13) 0.0057(14) C23 0.0282(17) 0.0194(18) 0.0351(18) 0.0067(15) 0.0183(14) 0.0116(15) C24 0.0227(16) 0.0122(16) 0.0307(16) 0.0080(13) 0.0141(13) 0.0074(14) C25 0.0218(16) 0.0184(17) 0.0344(17) 0.0140(14) 0.0184(13) 0.0111(14) C26 0.0208(15) 0.0159(17) 0.0342(17) 0.0037(14) 0.0192(13) 0.0072(14) C27 0.0339(17) 0.032(2) 0.0426(18) 0.0128(16) 0.0300(15) 0.0130(16) C28 0.0207(17) 0.0243(19) 0.054(2) 0.0149(16) 0.0192(15) 0.0114(15) C29 0.0292(18) 0.040(2) 0.049(2) 0.0074(18) 0.0273(16) 0.0061(17) C30 0.0240(17) 0.0181(17) 0.0316(17) 0.0075(14) 0.0110(14) 0.0039(14) C31 0.0191(17) 0.026(2) 0.0341(19) -0.0015(16) 0.0060(15) 0.0025(15) C32 0.041(2) 0.041(2) 0.0310(19) 0.0143(17) 0.0074(17) -0.0021(18) C33 0.0233(17) 0.0222(19) 0.0343(19) -0.0017(16) 0.0076(15) 0.0035(15) C34 0.0207(16) 0.0192(17) 0.0377(18) 0.0101(14) 0.0166(14) 0.0119(14) C35 0.0143(15) 0.0104(15) 0.0337(17) 0.0110(13) 0.0122(13) 0.0055(13) C36 0.0150(15) 0.0206(17) 0.0285(16) 0.0126(13) 0.0099(13) 0.0049(14) C37 0.0172(14) 0.0186(17) 0.0384(17) 0.0132(13) 0.0228(13) 0.0083(13) C38 0.0207(18) 0.055(2) 0.0404(19) 0.0298(17) 0.0087(15) 0.0073(17) C39 0.0326(18) 0.0255(19) 0.0480(19) 0.0169(15) 0.0261(15) 0.0149(15) C40 0.0220(16) 0.0179(16) 0.0280(16) 0.0147(13) 0.0144(13) 0.0092(14) C41 0.0175(16) 0.0165(17) 0.0297(16) 0.0104(13) 0.0152(13) 0.0056(13) C42 0.0067(14) 0.0166(17) 0.0253(16) 0.0060(13) 0.0061(13) 0.0054(13) C43 0.0189(16) 0.0143(16) 0.0227(15) 0.0066(13) 0.0118(13) 0.0089(13) C44 0.0178(16) 0.0122(16) 0.0233(16) 0.0028(13) 0.0078(13) 0.0041(13) C45 0.0158(15) 0.0175(17) 0.0239(16) 0.0083(13) 0.0103(13) 0.0084(13) C46 0.0187(16) 0.0214(16) 0.0289(16) 0.0171(13) 0.0103(13) 0.0141(14) C47 0.0128(15) 0.0170(16) 0.0245(16) 0.0105(13) 0.0093(13) 0.0047(13) C48 0.0324(18) 0.0136(17) 0.0372(17) 0.0125(14) 0.0198(14) 0.0101(15) C49 0.0281(17) 0.0180(17) 0.0380(18) 0.0113(14) 0.0234(14) 0.0089(15) C50 0.0231(17) 0.0233(18) 0.0312(17) 0.0121(14) 0.0144(14) 0.0056(15) C51 0.0217(17) 0.0250(18) 0.0297(17) 0.0135(14) 0.0105(14) 0.0075(15) C52 0.0264(18) 0.0286(19) 0.0280(18) 0.0130(15) 0.0019(15) 0.0050(16) C53 0.038(2) 0.027(2) 0.0324(19) 0.0112(16) 0.0052(16) 0.0052(17) C54 0.0266(19) 0.050(2) 0.0330(18) 0.0216(17) 0.0077(15) 0.0124(17) C55 0.0164(15) 0.0302(18) 0.0314(16) 0.0176(14) 0.0152(13) 0.0024(14) C56 0.0150(16) 0.034(2) 0.0397(18) 0.0188(15) 0.0133(14) 0.0071(15) C57 0.0147(15) 0.0261(18) 0.0243(16) 0.0108(14) 0.0090(13) 0.0112(14) C58 0.0127(15) 0.0164(17) 0.0240(16) 0.0064(13) 0.0074(13) 0.0058(13) C59 0.0165(15) 0.0162(16) 0.0290(16) 0.0095(13) 0.0156(13) 0.0076(13) C60 0.0137(16) 0.0176(17) 0.0203(16) 0.0041(14) 0.0029(13) 0.0083(14) C61 0.0265(17) 0.0218(17) 0.0216(16) 0.0101(13) 0.0148(13) 0.0085(15) C62 0.0262(17) 0.0276(19) 0.0239(16) 0.0129(14) 0.0163(13) 0.0130(15) C63 0.0212(17) 0.0183(17) 0.0224(16) 0.0046(14) 0.0105(13) 0.0083(14) C64 0.0137(15) 0.0206(17) 0.0267(17) 0.0113(14) 0.0077(13) 0.0117(14) C65 0.0244(16) 0.0338(19) 0.0379(17) 0.0234(14) 0.0234(14) 0.0196(15) C66 0.0384(19) 0.067(2) 0.0503(19) 0.0379(18) 0.0352(15) 0.0269(19) C67 0.0226(16) 0.036(2) 0.0426(18) 0.0205(15) 0.0241(14) 0.0171(15) C68 0.0206(17) 0.037(2) 0.0501(19) 0.0248(16) 0.0250(14) 0.0073(16) C69 0.0230(17) 0.0281(18) 0.0234(16) 0.0128(14) 0.0097(14) 0.0100(15) C70 0.0181(17) 0.034(2) 0.0282(18) 0.0112(15) 0.0010(14) 0.0077(16) C71 0.0278(19) 0.053(2) 0.037(2) 0.0105(19) 0.0084(17) 0.0200(18) C72 0.032(2) 0.068(2) 0.071(2) 0.0527(19) 0.0149(18) 0.012(2) C73 0.0178(16) 0.0189(17) 0.0392(18) 0.0182(14) 0.0144(14) 0.0104(14) C74 0.0182(15) 0.0181(16) 0.0315(16) 0.0142(13) 0.0194(13) 0.0100(13) C75 0.0248(17) 0.0232(19) 0.0394(18) 0.0124(15) 0.0200(14) 0.0103(15) C76 0.0267(18) 0.0142(18) 0.0311(18) 0.0022(15) 0.0142(15) 0.0063(15) C77 0.0199(18) 0.040(2) 0.039(2) -0.0014(18) 0.0091(16) 0.0031(17) C78 0.0326(19) 0.025(2) 0.043(2) 0.0025(17) 0.0194(16) 0.0036(17) C79 0.083(3) 0.049(2) 0.041(2) 0.0194(19) 0.033(2) 0.023(2) C80 0.041(2) 0.034(2) 0.0336(19) 0.0172(16) 0.0124(17) 0.0029(18) O1 0.0137(10) 0.0149(11) 0.0270(11) 0.0069(9) 0.0077(9) 0.0066(9) O2 0.0140(10) 0.0227(12) 0.0285(11) 0.0077(9) 0.0108(9) 0.0083(9) O3 0.0135(10) 0.0253(12) 0.0325(11) 0.0137(10) 0.0099(9) 0.0056(9) O4 0.0158(10) 0.0338(13) 0.0492(12) 0.0216(10) 0.0208(9) 0.0099(10) O5 0.0300(12) 0.0487(14) 0.0408(12) 0.0264(11) 0.0231(10) 0.0148(11) O6 0.0382(15) 0.093(2) 0.0349(13) 0.0318(13) 0.0139(11) 0.0141(15) O7 0.0167(11) 0.0172(11) 0.0299(11) 0.0146(9) 0.0084(9) 0.0072(9) O8 0.0126(10) 0.0219(12) 0.0264(11) 0.0121(9) 0.0080(9) 0.0064(9) O9 0.0196(11) 0.0251(12) 0.0298(11) 0.0134(10) 0.0140(9) 0.0118(10) O10 0.0206(11) 0.0260(13) 0.0481(13) 0.0136(10) 0.0228(10) 0.0149(10) O11 0.0303(12) 0.0321(14) 0.0500(14) 0.0019(12) 0.0289(11) 0.0091(11) O12 0.0387(15) 0.077(2) 0.0485(16) -0.0153(16) 0.0225(13) 0.0008(15) C96 0.076(5) 0.043(5) 0.084(5) 0.005(4) 0.005(4) -0.021(4) C97 0.048(5) 0.031(5) 0.034(5) 0.019(4) 0.003(4) -0.003(4) N97 0.023(5) 0.039(5) 0.031(5) 0.006(4) 0.020(4) 0.001(4) C98 0.021(4) 0.073(7) 0.086(6) 0.020(5) 0.035(4) 0.018(4) C99 0.043(3) 0.029(4) 0.056(4) -0.010(3) 0.038(3) -0.003(3) N98 0.066(5) 0.028(4) 0.098(6) -0.022(4) 0.023(5) -0.007(4) N95 0.100(9) 0.055(6) 0.164(9) -0.024(6) 0.033(9) -0.016(8) C95 0.100(9) 0.055(6) 0.164(9) -0.024(6) 0.033(9) -0.016(8) C94 0.213(12) 0.121(10) 0.106(8) 0.018(8) 0.082(8) -0.055(10) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Fe1 O2 92.88(9) . . ? O1 Fe1 O3 88.61(9) . . ? O2 Fe1 O3 96.79(9) . . ? O1 Fe1 N2 110.55(10) . . ? O2 Fe1 N2 86.47(9) . . ? O3 Fe1 N2 160.44(10) . . ? O1 Fe1 N1 86.27(9) . . ? O2 Fe1 N1 169.19(11) . . ? O3 Fe1 N1 93.96(9) . . ? N2 Fe1 N1 83.75(10) . . ? O1 Fe1 N3 163.95(10) . . ? O2 Fe1 N3 89.44(9) . . ? O3 Fe1 N3 75.34(9) . . ? N2 Fe1 N3 85.43(10) . . ? N1 Fe1 N3 94.35(9) . . ? O7 Fe2 O8 93.26(9) . . ? O7 Fe2 O9 88.48(8) . . ? O8 Fe2 O9 96.86(9) . . ? O7 Fe2 N6 108.59(9) . . ? O8 Fe2 N6 86.63(10) . . ? O9 Fe2 N6 162.41(8) . . ? O7 Fe2 N5 85.84(9) . . ? O8 Fe2 N5 168.85(10) . . ? O9 Fe2 N5 94.23(10) . . ? N6 Fe2 N5 83.13(10) . . ? O7 Fe2 N7 163.97(10) . . ? O8 Fe2 N7 89.24(9) . . ? O9 Fe2 N7 75.50(8) . . ? N6 Fe2 N7 87.36(9) . . ? N5 Fe2 N7 94.69(10) . . ? C1 N1 C16 118.6(3) . . ? C1 N1 Fe1 123.4(2) . . ? C16 N1 Fe1 118.05(17) . . ? C19 N2 C18 118.0(3) . . ? C19 N2 Fe1 122.7(2) . . ? C18 N2 Fe1 119.24(17) . . ? C36 N3 C35 105.1(3) . . ? C36 N3 Fe1 138.9(2) . . ? C35 N3 Fe1 108.97(19) . . ? C36 N4 C37 107.9(2) . . ? C36 N4 C38 123.9(3) . . ? C37 N4 C38 128.2(3) . . ? C40 N5 C55 118.4(3) . . ? C40 N5 Fe2 123.9(2) . . ? C55 N5 Fe2 117.63(18) . . ? C58 N6 C57 118.3(3) . . ? C58 N6 Fe2 121.6(2) . . ? C57 N6 Fe2 120.09(19) . . ? C75 N7 C74 104.4(2) . . ? C75 N7 Fe2 139.2(2) . . ? C74 N7 Fe2 109.95(18) . . ? C75 N8 C76 106.1(2) . . ? C75 N8 C77 124.3(3) . . ? C76 N8 C77 129.6(3) . . ? N1 C1 C2 126.2(3) . . ? C3 C2 C7 120.6(3) . . ? C3 C2 C1 122.4(2) . . ? C7 C2 C1 116.9(3) . . ? O1 C3 C2 121.3(3) . . ? O1 C3 C4 119.6(3) . . ? C2 C3 C4 119.1(2) . . ? C5 C4 C3 117.4(3) . . ? C5 C4 C8 122.8(3) . . ? C3 C4 C8 119.8(2) . . ? C4 C5 C6 124.6(3) . . ? C7 C6 C5 116.4(3) . . ? C7 C6 C12 123.9(3) . . ? C5 C6 C12 119.6(3) . . ? C6 C7 C2 121.7(3) . . ? C11 C8 C9 107.3(3) . . ? C11 C8 C4 111.9(2) . . ? C9 C8 C4 111.0(3) . . ? C11 C8 C10 108.3(3) . . ? C9 C8 C10 109.0(2) . . ? C4 C8 C10 109.3(3) . . ? C14 C12 C15 109.8(3) . . ? C14 C12 C6 109.3(3) . . ? C15 C12 C6 110.9(3) . . ? C14 C12 C13 107.8(3) . . ? C15 C12 C13 107.4(3) . . ? C6 C12 C13 111.6(3) . . ? N1 C16 C17 111.4(3) . . ? C18 C17 C16 115.4(3) . . ? N2 C18 C17 112.4(3) . . ? N2 C19 C20 126.5(3) . . ? C21 C20 C25 120.1(3) . . ? C21 C20 C19 122.8(2) . . ? C25 C20 C19 117.1(3) . . ? O2 C21 C20 120.2(3) . . ? O2 C21 C22 120.1(3) . . ? C20 C21 C22 119.6(2) . . ? C23 C22 C21 116.0(3) . . ? C23 C22 C26 122.9(3) . . ? C21 C22 C26 121.1(2) . . ? C24 C23 C22 126.6(3) . . ? C25 C24 C23 115.8(3) . . ? C25 C24 C30 123.4(3) . . ? C23 C24 C30 120.8(3) . . ? C24 C25 C20 121.7(3) . . ? C22 C26 C29 112.0(2) . . ? C22 C26 C27 111.8(3) . . ? C29 C26 C27 107.4(3) . . ? C22 C26 C28 109.0(3) . . ? C29 C26 C28 107.8(3) . . ? C27 C26 C28 108.8(2) . . ? C33 C30 C32 110.9(3) . . ? C33 C30 C31 106.9(3) . . ? C32 C30 C31 108.7(3) . . ? C33 C30 C24 109.1(3) . . ? C32 C30 C24 109.1(3) . . ? C31 C30 C24 112.2(3) . . ? O4 C34 O3 126.6(3) . . ? O4 C34 C35 119.6(3) . . ? O3 C34 C35 113.9(3) . . ? N3 C35 C37 111.1(3) . . ? N3 C35 C34 116.4(3) . . ? C37 C35 C34 132.5(3) . . ? N4 C36 N3 111.9(3) . . ? C35 C37 N4 104.1(3) . . ? C35 C37 C39 132.2(3) . . ? N4 C37 C39 123.7(3) . . ? O6 C39 O5 120.6(4) . . ? O6 C39 C37 123.3(3) . . ? O5 C39 C37 116.1(3) . . ? N5 C40 C41 126.2(3) . . ? C46 C41 C42 120.4(3) . . ? C46 C41 C40 117.5(3) . . ? C42 C41 C40 122.1(3) . . ? O7 C42 C41 120.8(3) . . ? O7 C42 C43 119.8(3) . . ? C41 C42 C43 119.4(3) . . ? C44 C43 C42 116.6(3) . . ? C44 C43 C47 123.1(3) . . ? C42 C43 C47 120.3(3) . . ? C43 C44 C45 125.9(3) . . ? C46 C45 C44 116.0(3) . . ? C46 C45 C51 122.3(3) . . ? C44 C45 C51 121.6(3) . . ? C45 C46 C41 121.5(3) . . ? C50 C47 C49 109.0(3) . . ? C50 C47 C43 111.2(2) . . ? C49 C47 C43 109.6(3) . . ? C50 C47 C48 107.6(3) . . ? C49 C47 C48 109.0(2) . . ? C43 C47 C48 110.3(3) . . ? C52 C51 C45 112.0(3) . . ? C52 C51 C53 108.7(3) . . ? C45 C51 C53 108.9(3) . . ? C52 C51 C54 107.6(3) . . ? C45 C51 C54 110.1(3) . . ? C53 C51 C54 109.5(3) . . ? N5 C55 C56 110.9(3) . . ? C57 C56 C55 115.0(3) . . ? N6 C57 C56 113.3(3) . . ? N6 C58 C59 127.2(3) . . ? C60 C59 C64 120.4(3) . . ? C60 C59 C58 122.3(3) . . ? C64 C59 C58 117.3(3) . . ? O8 C60 C59 120.7(3) . . ? O8 C60 C61 120.4(3) . . ? C59 C60 C61 118.9(3) . . ? C62 C61 C60 117.3(3) . . ? C62 C61 C65 121.0(3) . . ? C60 C61 C65 121.6(3) . . ? C61 C62 C63 125.4(3) . . ? C64 C63 C62 116.8(3) . . ? C64 C63 C69 123.1(3) . . ? C62 C63 C69 120.0(3) . . ? C63 C64 C59 121.1(3) . . ? C66 C65 C68 108.5(3) . . ? C66 C65 C67 107.3(3) . . ? C68 C65 C67 108.9(3) . . ? C66 C65 C61 113.0(3) . . ? C68 C65 C61 109.0(3) . . ? C67 C65 C61 110.2(3) . . ? C71 C69 C70 108.5(3) . . ? C71 C69 C63 108.9(3) . . ? C70 C69 C63 112.4(3) . . ? C71 C69 C72 110.3(3) . . ? C70 C69 C72 107.8(3) . . ? C63 C69 C72 109.0(3) . . ? O9 C73 O10 125.9(3) . . ? O9 C73 C74 115.8(3) . . ? O10 C73 C74 118.3(3) . . ? C76 C74 N7 110.2(3) . . ? C76 C74 C73 135.1(3) . . ? N7 C74 C73 114.6(2) . . ? N7 C75 N8 112.6(3) . . ? C74 C76 N8 106.6(3) . . ? C74 C76 C78 130.8(3) . . ? N8 C76 C78 122.4(3) . . ? O12 C78 O11 122.4(3) . . ? O12 C78 C76 122.3(3) . . ? O11 C78 C76 115.3(3) . . ? N9 C80 C79 179.6(5) . . ? C3 O1 Fe1 131.0(2) . . ? C21 O2 Fe1 128.25(19) . . ? C34 O3 Fe1 119.10(19) . . ? C42 O7 Fe2 130.7(2) . . ? C60 O8 Fe2 128.6(2) . . ? C73 O9 Fe2 117.99(19) . . ? N97 C97 C96 160.9(11) . . ? N98 C99 C98 164.2(7) . . ? N95 N95 C94 161.0(15) 2_666 . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O1 1.877(2) . ? Fe1 O2 1.907(2) . ? Fe1 O3 2.087(2) . ? Fe1 N2 2.095(3) . ? Fe1 N1 2.112(2) . ? Fe1 N3 2.201(3) . ? Fe2 O7 1.8831(18) . ? Fe2 O8 1.899(2) . ? Fe2 O9 2.093(2) . ? Fe2 N6 2.102(3) . ? Fe2 N5 2.112(3) . ? Fe2 N7 2.176(2) . ? N1 C1 1.295(3) . ? N1 C16 1.459(4) . ? N2 C19 1.287(3) . ? N2 C18 1.473(4) . ? N3 C36 1.329(4) . ? N3 C35 1.352(4) . ? N4 C36 1.318(4) . ? N4 C37 1.389(4) . ? N4 C38 1.466(4) . ? N5 C40 1.279(3) . ? N5 C55 1.470(4) . ? N6 C58 1.296(4) . ? N6 C57 1.458(4) . ? N7 C75 1.336(4) . ? N7 C74 1.377(4) . ? N8 C75 1.342(4) . ? N8 C76 1.382(4) . ? N8 C77 1.464(4) . ? N9 C80 1.136(5) . ? C1 C2 1.447(4) . ? C2 C3 1.397(4) . ? C2 C7 1.398(4) . ? C3 O1 1.323(3) . ? C3 C4 1.438(4) . ? C4 C5 1.364(4) . ? C4 C8 1.541(4) . ? C5 C6 1.421(4) . ? C6 C7 1.377(4) . ? C6 C12 1.533(4) . ? C8 C11 1.526(4) . ? C8 C9 1.535(5) . ? C8 C10 1.541(5) . ? C12 C14 1.521(6) . ? C12 C15 1.528(5) . ? C12 C13 1.535(5) . ? C16 C17 1.553(5) . ? C17 C18 1.510(5) . ? C19 C20 1.437(4) . ? C20 C21 1.410(5) . ? C20 C25 1.414(4) . ? C21 O2 1.327(3) . ? C21 C22 1.421(4) . ? C22 C23 1.394(4) . ? C22 C26 1.531(5) . ? C23 C24 1.386(5) . ? C24 C25 1.384(4) . ? C24 C30 1.531(4) . ? C26 C29 1.532(4) . ? C26 C27 1.536(5) . ? C26 C28 1.541(5) . ? C30 C33 1.522(5) . ? C30 C32 1.526(5) . ? C30 C31 1.527(5) . ? C34 O4 1.247(4) . ? C34 O3 1.258(4) . ? C34 C35 1.503(4) . ? C35 C37 1.369(4) . ? C37 C39 1.461(5) . ? C39 O6 1.209(4) . ? C39 O5 1.329(4) . ? C40 C41 1.457(4) . ? C41 C46 1.399(4) . ? C41 C42 1.403(5) . ? C42 O7 1.324(3) . ? C42 C43 1.425(4) . ? C43 C44 1.369(4) . ? C43 C47 1.536(5) . ? C44 C45 1.398(5) . ? C45 C46 1.383(4) . ? C45 C51 1.523(4) . ? C47 C50 1.520(4) . ? C47 C49 1.522(4) . ? C47 C48 1.565(4) . ? C51 C52 1.521(5) . ? C51 C53 1.540(4) . ? C51 C54 1.544(5) . ? C55 C56 1.549(5) . ? C56 C57 1.530(5) . ? C58 C59 1.439(5) . ? C59 C60 1.405(5) . ? C59 C64 1.424(4) . ? C60 O8 1.331(3) . ? C60 C61 1.420(5) . ? C61 C62 1.366(4) . ? C61 C65 1.558(5) . ? C62 C63 1.407(5) . ? C63 C64 1.355(5) . ? C63 C69 1.535(4) . ? C65 C66 1.512(5) . ? C65 C68 1.537(4) . ? C65 C67 1.548(5) . ? C69 C71 1.520(5) . ? C69 C70 1.526(5) . ? C69 C72 1.543(5) . ? C73 O9 1.251(3) . ? C73 O10 1.260(4) . ? C73 C74 1.487(4) . ? C74 C76 1.358(4) . ? C76 C78 1.486(5) . ? C78 O12 1.206(4) . ? C78 O11 1.320(4) . ? C79 C80 1.442(6) . ? C96 C97 1.496(7) . ? C97 N97 1.160(6) . ? C98 C99 1.322(5) . ? C99 N98 1.322(6) . ? N95 N95 1.176(6) 2_666 ? N95 C94 1.478(4) . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H5B O4 0.84 1.67 2.511(3) 177.8 . O11 H11D O10 0.84 1.68 2.514(3) 176.4 .
1100756.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $ #$Revision: 176435 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100756.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100756 loop_ _publ_author_name 'Panagiotis Angaridis' 'Jeff W. Kampf' 'Vincent L. Pecoraro' _publ_contact_author_address ; Chemistry Department University of Michigan 930 N.University Ann Arbor, MI 48109, USA ; _publ_contact_author_email vlpec@umich.edu _publ_contact_author_fax '(734) 936 7628' _publ_contact_author_name 'Vincent. L. Pecoraro' _publ_contact_author_phone '(734) 763 1519' _publ_section_title ; Multinuclear Fe(III) Complexes with Polydentate Ligands of the Family of Dicarboxyimidazoles: Nuclearity- and Topology-Controlled Syntheses and Magneto-Structural Correlations ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3626 _journal_page_last 3635 _journal_paper_doi 10.1021/ic0481879 _journal_volume 44 _journal_year 2005 _chemical_formula_moiety 'C72 H100 Fe2 N6 O8, 2.5(C2 H3 N), 1.5(C H2 Cl)' _chemical_formula_sum 'C78.5 H110.5 Cl3 Fe2 N8.5 O8' _chemical_formula_weight 1519.30 _chemical_name_systematic ; ? ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 68.170(4) _cell_angle_beta 76.554(4) _cell_angle_gamma 74.682(4) _cell_formula_units_Z 2 _cell_length_a 11.162(3) _cell_length_b 19.736(4) _cell_length_c 21.367(5) _cell_measurement_reflns_used 8169 _cell_measurement_temperature 123(2) _cell_measurement_theta_max 23.21 _cell_measurement_theta_min 2.92 _cell_volume 4166.6(17) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _diffrn_ambient_temperature 123(2) _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0354 _diffrn_reflns_av_sigmaI/netI 0.0321 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 83901 _diffrn_reflns_theta_full 28.40 _diffrn_reflns_theta_max 28.40 _diffrn_reflns_theta_min 1.77 _exptl_absorpt_coefficient_mu 0.500 _exptl_absorpt_correction_T_max 0.9425 _exptl_absorpt_correction_T_min 0.8101 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour purple _exptl_crystal_density_diffrn 1.211 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 1616 _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.12 _refine_diff_density_max 1.108 _refine_diff_density_min -1.105 _refine_diff_density_rms 0.085 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 956 _refine_ls_number_reflns 20708 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.080 _refine_ls_R_factor_all 0.0787 _refine_ls_R_factor_gt 0.0591 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1010P)^2^+4.1268P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1742 _refine_ls_wR_factor_ref 0.1851 _reflns_number_gt 15988 _reflns_number_total 20708 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic0481879si20041222_050013_3.cif _cod_data_source_block compound2 _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_cell_volume 4166.7(16) _cod_original_formula_sum 'C78.50 H110.50 Cl3 Fe2 N8.50 O8' _cod_database_code 1100756 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.45505(3) 0.115381(19) 0.301902(17) 0.02212(9) Uani 1 1 d . . . Fe2 Fe 0.51761(3) 0.321161(18) 0.421739(17) 0.01957(9) Uani 1 1 d . . . O1 O 0.44702(17) 0.08726(10) 0.22535(9) 0.0246(4) Uani 1 1 d . . . O2 O 0.52764(17) 0.20040(9) 0.24282(9) 0.0236(3) Uani 1 1 d . . . O3 O 0.37812(16) 0.32074(10) 0.49259(9) 0.0229(3) Uani 1 1 d . . . O4 O 0.51020(17) 0.42602(9) 0.39168(9) 0.0245(4) Uani 1 1 d . . . O5 O 0.45695(18) 0.13621(10) 0.39082(9) 0.0261(4) Uani 1 1 d . . . O6 O 0.52352(17) 0.21045(10) 0.42699(9) 0.0244(4) Uani 1 1 d . . . O7 O 0.27424(18) 0.16561(11) 0.30837(10) 0.0310(4) Uani 1 1 d . . . O8 O 0.0976(2) 0.25005(17) 0.30508(18) 0.0653(9) Uani 1 1 d . . . N1 N 0.4143(2) 0.00949(12) 0.36279(11) 0.0261(4) Uani 1 1 d . . . N2 N 0.6456(2) 0.06031(12) 0.31321(11) 0.0250(4) Uani 1 1 d . . . N3 N 0.63256(19) 0.27327(11) 0.49869(11) 0.0218(4) Uani 1 1 d . . . N4 N 0.6887(2) 0.31710(12) 0.35290(11) 0.0242(4) Uani 1 1 d . . . N5 N 0.2330(2) 0.35618(14) 0.30160(12) 0.0322(5) Uani 1 1 d . . . N6 N 0.3956(2) 0.33336(12) 0.35280(11) 0.0239(4) Uani 1 1 d . . . C1 C 0.3568(3) -0.02679(14) 0.34404(13) 0.0260(5) Uani 1 1 d . . . H1A H 0.3294 -0.0690 0.3784 0.031 Uiso 1 1 calc R . . C2 C 0.3297(2) -0.00996(14) 0.27618(12) 0.0235(5) Uani 1 1 d . . . C3 C 0.3824(2) 0.04385(13) 0.21865(12) 0.0217(5) Uani 1 1 d . . . C4 C 0.3670(2) 0.04821(13) 0.15223(12) 0.0219(5) Uani 1 1 d . . . C5 C 0.3023(2) -0.00053(13) 0.14835(12) 0.0226(5) Uani 1 1 d . . . H5A H 0.2935 0.0020 0.1043 0.027 Uiso 1 1 calc R . . C6 C 0.2483(2) -0.05407(13) 0.20546(13) 0.0231(5) Uani 1 1 d . . . C7 C 0.2628(2) -0.05726(14) 0.26858(13) 0.0242(5) Uani 1 1 d . . . H7A H 0.2270 -0.0921 0.3081 0.029 Uiso 1 1 calc R . . C8 C 0.4209(3) 0.10563(14) 0.08764(13) 0.0274(5) Uani 1 1 d . . . C9 C 0.3927(3) 0.10149(16) 0.02242(14) 0.0342(6) Uani 1 1 d . . . H9A H 0.4268 0.0512 0.0201 0.051 Uiso 1 1 calc R . . H9B H 0.4316 0.1375 -0.0174 0.051 Uiso 1 1 calc R . . H9C H 0.3016 0.1131 0.0229 0.051 Uiso 1 1 calc R . . C10 C 0.3614(4) 0.18397(16) 0.09094(16) 0.0428(8) Uani 1 1 d . . . H10A H 0.2706 0.1932 0.0914 0.064 Uiso 1 1 calc R . . H10B H 0.3982 0.2209 0.0510 0.064 Uiso 1 1 calc R . . H10C H 0.3776 0.1879 0.1325 0.064 Uiso 1 1 calc R . . C11 C 0.5645(3) 0.09233(19) 0.08169(15) 0.0391(7) Uani 1 1 d . . . H11A H 0.5864 0.0936 0.1230 0.059 Uiso 1 1 calc R . . H11B H 0.5966 0.1313 0.0419 0.059 Uiso 1 1 calc R . . H11C H 0.6019 0.0436 0.0763 0.059 Uiso 1 1 calc R . . C12 C 0.1849(2) -0.10784(14) 0.19414(13) 0.0251(5) Uani 1 1 d . . . C13 C 0.0872(3) -0.06482(17) 0.14584(16) 0.0363(6) Uani 1 1 d . . . H13A H 0.0464 -0.0999 0.1400 0.054 Uiso 1 1 calc R . . H13B H 0.1290 -0.0370 0.1014 0.054 Uiso 1 1 calc R . . H13C H 0.0239 -0.0300 0.1652 0.054 Uiso 1 1 calc R . . C14 C 0.2864(3) -0.16128(17) 0.16290(17) 0.0360(6) Uani 1 1 d . . . H14A H 0.3469 -0.1901 0.1945 0.054 Uiso 1 1 calc R . . H14B H 0.3300 -0.1324 0.1197 0.054 Uiso 1 1 calc R . . H14C H 0.2466 -0.1953 0.1546 0.054 Uiso 1 1 calc R . . C15 C 0.1180(3) -0.15406(16) 0.26097(14) 0.0304(6) Uani 1 1 d . . . H15A H 0.0558 -0.1208 0.2826 0.046 Uiso 1 1 calc R . . H15B H 0.1796 -0.1848 0.2915 0.046 Uiso 1 1 calc R . . H15C H 0.0756 -0.1862 0.2518 0.046 Uiso 1 1 calc R . . C16 C 0.4648(3) -0.02931(15) 0.42756(13) 0.0303(6) Uani 1 1 d . . . H16A H 0.4237 -0.0721 0.4552 0.036 Uiso 1 1 calc R . . H16B H 0.4483 0.0050 0.4540 0.036 Uiso 1 1 calc R . . C17 C 0.6063(3) -0.05646(15) 0.41126(14) 0.0318(6) Uani 1 1 d . . . H17A H 0.6207 -0.0862 0.3807 0.038 Uiso 1 1 calc R . . H17B H 0.6382 -0.0899 0.4541 0.038 Uiso 1 1 calc R . . C18 C 0.6828(3) 0.00530(15) 0.37750(14) 0.0306(6) Uani 1 1 d . . . H18A H 0.6754 0.0317 0.4100 0.037 Uiso 1 1 calc R . . H18B H 0.7724 -0.0180 0.3687 0.037 Uiso 1 1 calc R . . C19 C 0.7315(2) 0.07448(14) 0.26129(13) 0.0263(5) Uani 1 1 d . . . H19A H 0.8112 0.0421 0.2651 0.032 Uiso 1 1 calc R . . C20 C 0.7188(2) 0.13526(14) 0.19709(13) 0.0244(5) Uani 1 1 d . . . C21 C 0.8145(2) 0.13235(15) 0.14134(13) 0.0272(5) Uani 1 1 d . A . H21A H 0.8796 0.0894 0.1460 0.033 Uiso 1 1 calc R . . C22 C 0.8159(2) 0.19042(16) 0.08017(14) 0.0282(5) Uani 1 1 d . . . C23 C 0.7230(3) 0.25483(15) 0.07803(13) 0.0276(5) Uani 1 1 d . A . H23A H 0.7250 0.2960 0.0369 0.033 Uiso 1 1 calc R . . C24 C 0.6282(2) 0.26266(14) 0.13175(13) 0.0240(5) Uani 1 1 d . . . C25 C 0.6207(2) 0.19873(14) 0.19206(12) 0.0231(5) Uani 1 1 d . A . C26 C 0.9149(3) 0.18696(18) 0.01749(14) 0.0344(6) Uani 0.629(7) 1 d P A 1 C27 C 0.8514(5) 0.2074(4) -0.0436(2) 0.0395(13) Uani 0.629(7) 1 d P A 1 H27A H 0.9150 0.2100 -0.0842 0.059 Uiso 0.629(7) 1 calc PR A 1 H27B H 0.7947 0.2559 -0.0498 0.059 Uiso 0.629(7) 1 calc PR A 1 H27C H 0.8032 0.1696 -0.0366 0.059 Uiso 0.629(7) 1 calc PR A 1 C28 C 1.0004(5) 0.2447(4) 0.0025(3) 0.0445(14) Uani 0.629(7) 1 d P A 1 H28A H 1.0663 0.2413 -0.0362 0.067 Uiso 0.629(7) 1 calc PR A 1 H28B H 1.0391 0.2337 0.0428 0.067 Uiso 0.629(7) 1 calc PR A 1 H28C H 0.9491 0.2951 -0.0085 0.067 Uiso 0.629(7) 1 calc PR A 1 C29 C 1.0020(5) 0.1114(3) 0.0273(3) 0.0470(15) Uani 0.629(7) 1 d P A 1 H29A H 0.9530 0.0738 0.0351 0.070 Uiso 0.629(7) 1 calc PR A 1 H29B H 1.0444 0.0983 0.0668 0.070 Uiso 0.629(7) 1 calc PR A 1 H29C H 1.0648 0.1135 -0.0136 0.070 Uiso 0.629(7) 1 calc PR A 1 C26A C 0.9149(3) 0.18696(18) 0.01749(14) 0.0344(6) Uani 0.371(7) 1 d P A 2 C27A C 1.0412(7) 0.1813(7) 0.0334(5) 0.053(3) Uani 0.371(7) 1 d P A 2 H27D H 1.1039 0.1829 -0.0075 0.080 Uiso 0.371(7) 1 calc PR A 2 H27E H 1.0633 0.1342 0.0698 0.080 Uiso 0.371(7) 1 calc PR A 2 H27F H 1.0394 0.2230 0.0482 0.080 Uiso 0.371(7) 1 calc PR A 2 C28A C 0.8854(10) 0.2501(7) -0.0475(5) 0.056(3) Uani 0.371(7) 1 d P A 2 H28D H 0.8886 0.2973 -0.0432 0.084 Uiso 0.371(7) 1 calc PR A 2 H28E H 0.8012 0.2521 -0.0553 0.084 Uiso 0.371(7) 1 calc PR A 2 H28F H 0.9474 0.2417 -0.0861 0.084 Uiso 0.371(7) 1 calc PR A 2 C29A C 0.9120(9) 0.1140(6) 0.0051(5) 0.057(3) Uani 0.371(7) 1 d P A 2 H29D H 0.9762 0.1079 -0.0335 0.085 Uiso 0.371(7) 1 calc PR A 2 H29E H 0.8290 0.1173 -0.0050 0.085 Uiso 0.371(7) 1 calc PR A 2 H29F H 0.9291 0.0711 0.0461 0.085 Uiso 0.371(7) 1 calc PR A 2 C30 C 0.5387(3) 0.33725(14) 0.12819(13) 0.0267(5) Uani 1 1 d . A . C31 C 0.4002(3) 0.33262(16) 0.13677(16) 0.0330(6) Uani 1 1 d . . . H31A H 0.3870 0.3199 0.0990 0.050 Uiso 1 1 calc R A . H31B H 0.3467 0.3808 0.1367 0.050 Uiso 1 1 calc R . . H31C H 0.3785 0.2942 0.1801 0.050 Uiso 1 1 calc R . . C32 C 0.5673(3) 0.39879(16) 0.06033(15) 0.0363(6) Uani 1 1 d . . . H32A H 0.6532 0.4059 0.0550 0.054 Uiso 1 1 calc R A . H32B H 0.5080 0.4454 0.0601 0.054 Uiso 1 1 calc R . . H32C H 0.5590 0.3844 0.0226 0.054 Uiso 1 1 calc R . . C33 C 0.5583(3) 0.36182(15) 0.18496(14) 0.0319(6) Uani 1 1 d . . . H33A H 0.5417 0.3237 0.2293 0.048 Uiso 1 1 calc R A . H33B H 0.5006 0.4090 0.1844 0.048 Uiso 1 1 calc R . . H33C H 0.6452 0.3684 0.1773 0.048 Uiso 1 1 calc R . . C34 C 0.5909(2) 0.24530(13) 0.56247(13) 0.0225(5) Uani 1 1 d . . . H34A H 0.6523 0.2230 0.5922 0.027 Uiso 1 1 calc R . . C35 C 0.4615(2) 0.24374(13) 0.59428(12) 0.0215(4) Uani 1 1 d . . . C36 C 0.3595(2) 0.27989(13) 0.55722(12) 0.0206(4) Uani 1 1 d . . . C37 C 0.2348(2) 0.27236(13) 0.59120(12) 0.0215(5) Uani 1 1 d . . . C38 C 0.2200(2) 0.23182(14) 0.66026(12) 0.0235(5) Uani 1 1 d . . . H38A H 0.1374 0.2265 0.6830 0.028 Uiso 1 1 calc R . . C39 C 0.3196(2) 0.19802(14) 0.69895(12) 0.0235(5) Uani 1 1 d . . . C40 C 0.4394(2) 0.20443(13) 0.66489(12) 0.0227(5) Uani 1 1 d . . . H40A H 0.5086 0.1819 0.6894 0.027 Uiso 1 1 calc R . . C41 C 0.1227(2) 0.30789(15) 0.55153(13) 0.0251(5) Uani 1 1 d . . . C42 C -0.0006(2) 0.28979(16) 0.59593(14) 0.0292(5) Uani 1 1 d . . . H42A H 0.0047 0.2358 0.6129 0.044 Uiso 1 1 calc R . . H42B H -0.0695 0.3140 0.5688 0.044 Uiso 1 1 calc R . . H42C H -0.0165 0.3080 0.6346 0.044 Uiso 1 1 calc R . . C43 C 0.1077(3) 0.39316(16) 0.52449(16) 0.0355(6) Uani 1 1 d . . . H43A H 0.0417 0.4150 0.4954 0.053 Uiso 1 1 calc R . . H43B H 0.1872 0.4067 0.4979 0.053 Uiso 1 1 calc R . . H43C H 0.0845 0.4121 0.5630 0.053 Uiso 1 1 calc R . . C44 C 0.1423(3) 0.27800(19) 0.49202(15) 0.0342(6) Uani 1 1 d . . . H44A H 0.1535 0.2236 0.5098 0.051 Uiso 1 1 calc R . . H44B H 0.2171 0.2924 0.4601 0.051 Uiso 1 1 calc R . . H44C H 0.0686 0.2990 0.4684 0.051 Uiso 1 1 calc R . . C45 C 0.2915(2) 0.15372(14) 0.77525(12) 0.0245(5) Uani 1 1 d . . . C46 C 0.1796(3) 0.19806(17) 0.81065(14) 0.0328(6) Uani 1 1 d . . . H46A H 0.1041 0.2059 0.7909 0.049 Uiso 1 1 calc R . . H46B H 0.1981 0.2463 0.8041 0.049 Uiso 1 1 calc R . . H46C H 0.1655 0.1701 0.8595 0.049 Uiso 1 1 calc R . . C47 C 0.4046(3) 0.13709(17) 0.81177(14) 0.0313(6) Uani 1 1 d . . . H47A H 0.3825 0.1106 0.8604 0.047 Uiso 1 1 calc R . . H47B H 0.4274 0.1839 0.8060 0.047 Uiso 1 1 calc R . . H47C H 0.4759 0.1061 0.7922 0.047 Uiso 1 1 calc R . . C48 C 0.2604(3) 0.07955(16) 0.78213(14) 0.0331(6) Uani 1 1 d . . . H48A H 0.3341 0.0499 0.7626 0.050 Uiso 1 1 calc R . . H48B H 0.1901 0.0895 0.7577 0.050 Uiso 1 1 calc R . . H48C H 0.2374 0.0520 0.8304 0.050 Uiso 1 1 calc R . . C49 C 0.7692(2) 0.26632(16) 0.47804(14) 0.0279(5) Uani 1 1 d . . . H49A H 0.8109 0.2452 0.5192 0.033 Uiso 1 1 calc R . . H49B H 0.7890 0.3163 0.4523 0.033 Uiso 1 1 calc R . . C50 C 0.8205(3) 0.21635(17) 0.43365(15) 0.0382(7) Uani 1 1 d . . . H50A H 0.9134 0.2061 0.4281 0.046 Uiso 1 1 calc R . . H50B H 0.7932 0.1682 0.4584 0.046 Uiso 1 1 calc R . . C51 C 0.7814(3) 0.24686(15) 0.36303(15) 0.0308(6) Uani 1 1 d . . . H51A H 0.8567 0.2552 0.3281 0.037 Uiso 1 1 calc R . . H51B H 0.7452 0.2095 0.3567 0.037 Uiso 1 1 calc R . . C52 C 0.7138(2) 0.37333(15) 0.30083(13) 0.0267(5) Uani 1 1 d . . . H52A H 0.7891 0.3651 0.2707 0.032 Uiso 1 1 calc R . . C53 C 0.6392(3) 0.44786(14) 0.28340(13) 0.0265(5) Uani 1 1 d . . . C54 C 0.5423(2) 0.47217(14) 0.33041(12) 0.0237(5) Uani 1 1 d . . . C55 C 0.4817(3) 0.54888(14) 0.31103(13) 0.0264(5) Uani 1 1 d . . . C56 C 0.5139(3) 0.59370(15) 0.24453(14) 0.0336(6) Uani 1 1 d . . . H56A H 0.4716 0.6443 0.2312 0.040 Uiso 1 1 calc R . . C57 C 0.6043(3) 0.56945(16) 0.19591(15) 0.0393(7) Uani 1 1 d . . . C58 C 0.6695(3) 0.49689(16) 0.21731(14) 0.0360(6) Uani 1 1 d . . . H58A H 0.7363 0.4797 0.1867 0.043 Uiso 1 1 calc R . . C59 C 0.3845(3) 0.58054(14) 0.36222(14) 0.0306(6) Uani 1 1 d . . . C60 C 0.2710(3) 0.54205(17) 0.38620(19) 0.0440(8) Uani 1 1 d . . . H60A H 0.2130 0.5601 0.4213 0.066 Uiso 1 1 calc R . . H60B H 0.2999 0.4881 0.4052 0.066 Uiso 1 1 calc R . . H60C H 0.2279 0.5534 0.3474 0.066 Uiso 1 1 calc R . . C61 C 0.3357(3) 0.66447(15) 0.33123(15) 0.0346(6) Uani 1 1 d . . . H61A H 0.4068 0.6901 0.3125 0.052 Uiso 1 1 calc R . . H61B H 0.2809 0.6834 0.3667 0.052 Uiso 1 1 calc R . . H61C H 0.2881 0.6736 0.2947 0.052 Uiso 1 1 calc R . . C62 C 0.4467(4) 0.56883(18) 0.42367(16) 0.0427(8) Uani 1 1 d . . . H62A H 0.5141 0.5972 0.4085 0.064 Uiso 1 1 calc R . . H62B H 0.4817 0.5158 0.4438 0.064 Uiso 1 1 calc R . . H62C H 0.3837 0.5860 0.4578 0.064 Uiso 1 1 calc R . . C63 C 0.6273(5) 0.62315(19) 0.12231(17) 0.0582(11) Uani 1 1 d . . . C64 C 0.6707(9) 0.6866(3) 0.1198(3) 0.122(3) Uani 1 1 d . . . H64A H 0.7473 0.6698 0.1408 0.184 Uiso 1 1 calc R . . H64B H 0.6056 0.7154 0.1447 0.184 Uiso 1 1 calc R . . H64C H 0.6888 0.7179 0.0722 0.184 Uiso 1 1 calc R . . C65 C 0.4916(6) 0.6619(5) 0.0962(3) 0.129(3) Uani 1 1 d . . . H65A H 0.4386 0.6888 0.1264 0.193 Uiso 1 1 calc R . . H65B H 0.4506 0.6234 0.0967 0.193 Uiso 1 1 calc R . . H65C H 0.5039 0.6969 0.0496 0.193 Uiso 1 1 calc R . . C66 C 0.6831(7) 0.5845(2) 0.07271(19) 0.090(2) Uani 1 1 d . . . H66A H 0.7054 0.6208 0.0280 0.135 Uiso 1 1 calc R . . H66B H 0.6226 0.5584 0.0694 0.135 Uiso 1 1 calc R . . H66C H 0.7589 0.5484 0.0874 0.135 Uiso 1 1 calc R . . C67 C 0.3769(2) 0.26716(14) 0.35290(12) 0.0238(5) Uani 1 1 d . . . C68 C 0.2752(2) 0.28002(15) 0.32104(13) 0.0272(5) Uani 1 1 d . . . C69 C 0.3078(3) 0.38564(15) 0.32100(14) 0.0288(5) Uani 1 1 d . . . H69A H 0.2987 0.4373 0.3129 0.035 Uiso 1 1 calc R . . C70 C 0.4581(2) 0.19934(14) 0.39197(12) 0.0230(5) Uani 1 1 d . . . C71 C 0.2091(3) 0.22883(18) 0.31040(15) 0.0340(6) Uani 1 1 d . . . C72 C 0.1258(3) 0.4013(2) 0.2658(2) 0.0516(9) Uani 1 1 d . . . H72A H 0.1240 0.4542 0.2555 0.077 Uiso 1 1 calc R . . H72B H 0.0475 0.3885 0.2947 0.077 Uiso 1 1 calc R . . H72C H 0.1345 0.3913 0.2231 0.077 Uiso 1 1 calc R . . Cl2 Cl 0.8329(2) 0.47300(11) 0.39215(11) 0.1200(6) Uani 1 1 d . . . Cl1 Cl 0.9325(2) 0.59055(10) 0.28157(14) 0.1404(8) Uani 1 1 d . . . N8 N 0.9407(4) 0.08013(19) 0.3631(2) 0.0594(8) Uani 1 1 d . . . C77 C 0.9915(3) 0.0998(2) 0.3104(2) 0.0451(8) Uani 1 1 d . . . N7 N 0.9603(4) 0.1102(2) 0.57528(18) 0.0641(9) Uani 1 1 d . . . C76 C 1.0548(4) 0.1311(2) 0.2398(2) 0.0542(9) Uani 1 1 d . . . H76A H 0.9967 0.1733 0.2139 0.081 Uiso 1 1 calc R . . H76B H 1.0804 0.0927 0.2180 0.081 Uiso 1 1 calc R . . H76C H 1.1291 0.1479 0.2410 0.081 Uiso 1 1 calc R . . C75 C 1.0316(4) 0.0901(2) 0.5353(2) 0.0513(9) Uani 1 1 d . . . C74 C 1.1247(4) 0.0641(3) 0.4834(2) 0.0628(11) Uani 1 1 d . . . H74A H 1.1880 0.0956 0.4644 0.094 Uiso 1 1 calc R . . H74B H 1.0823 0.0671 0.4469 0.094 Uiso 1 1 calc R . . H74C H 1.1657 0.0125 0.5045 0.094 Uiso 1 1 calc R . . C73 C 0.7938(5) 0.5672(3) 0.3324(3) 0.0936(18) Uani 1 1 d . . . H73A H 0.7339 0.5689 0.3039 0.112 Uiso 1 1 calc R . . H73B H 0.7545 0.6026 0.3576 0.112 Uiso 1 1 calc R . . Cl4 Cl 0.9217(6) 0.3328(4) 0.1339(3) 0.182(2) Uani 0.50 1 d P . . Cl3 Cl 1.0600(6) 0.4386(3) 0.0867(3) 0.186(3) Uani 0.50 1 d P . . C78 C 1.0548(11) 0.3452(6) 0.1194(7) 0.117(6) Uani 0.50 1 d P . . H78A H 1.1056 0.3205 0.0864 0.141 Uiso 0.50 1 calc PR . . H78B H 1.0921 0.3222 0.1621 0.141 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.03160(19) 0.02079(18) 0.01797(17) -0.00767(13) -0.00201(13) -0.01139(14) Fe2 0.02380(17) 0.01737(17) 0.01888(17) -0.00743(13) -0.00088(12) -0.00618(12) O1 0.0366(9) 0.0226(8) 0.0193(8) -0.0073(7) -0.0032(7) -0.0136(7) O2 0.0307(9) 0.0214(8) 0.0208(8) -0.0084(7) 0.0009(7) -0.0106(7) O3 0.0241(8) 0.0234(8) 0.0198(8) -0.0057(7) -0.0015(6) -0.0060(6) O4 0.0322(9) 0.0196(8) 0.0208(8) -0.0070(7) 0.0012(7) -0.0078(7) O5 0.0393(10) 0.0212(8) 0.0211(8) -0.0082(7) -0.0020(7) -0.0116(7) O6 0.0329(9) 0.0203(8) 0.0233(9) -0.0083(7) -0.0054(7) -0.0082(7) O7 0.0309(9) 0.0379(11) 0.0324(10) -0.0169(8) -0.0018(8) -0.0152(8) O8 0.0317(12) 0.081(2) 0.115(3) -0.071(2) -0.0153(14) -0.0011(12) N1 0.0381(12) 0.0259(11) 0.0176(10) -0.0066(8) -0.0043(8) -0.0127(9) N2 0.0370(11) 0.0213(10) 0.0211(10) -0.0073(8) -0.0079(8) -0.0095(8) N3 0.0228(9) 0.0208(10) 0.0253(10) -0.0109(8) -0.0013(8) -0.0072(7) N4 0.0269(10) 0.0225(10) 0.0256(10) -0.0118(8) -0.0002(8) -0.0063(8) N5 0.0302(11) 0.0379(13) 0.0323(12) -0.0184(10) -0.0084(9) 0.0005(9) N6 0.0296(10) 0.0228(10) 0.0205(10) -0.0086(8) -0.0016(8) -0.0070(8) C1 0.0379(13) 0.0230(12) 0.0196(11) -0.0065(9) -0.0017(10) -0.0128(10) C2 0.0317(12) 0.0212(11) 0.0199(11) -0.0074(9) -0.0028(9) -0.0091(9) C3 0.0275(11) 0.0193(11) 0.0211(11) -0.0085(9) -0.0035(9) -0.0064(9) C4 0.0296(12) 0.0179(11) 0.0194(11) -0.0060(9) -0.0025(9) -0.0081(9) C5 0.0289(12) 0.0211(11) 0.0204(11) -0.0083(9) -0.0047(9) -0.0059(9) C6 0.0267(11) 0.0205(11) 0.0250(12) -0.0084(9) -0.0040(9) -0.0076(9) C7 0.0302(12) 0.0219(11) 0.0220(12) -0.0064(9) -0.0023(9) -0.0106(9) C8 0.0444(15) 0.0250(12) 0.0174(11) -0.0058(9) -0.0045(10) -0.0160(11) C9 0.0552(17) 0.0313(14) 0.0200(12) -0.0059(10) -0.0054(12) -0.0192(13) C10 0.081(2) 0.0218(13) 0.0275(14) -0.0049(11) -0.0115(15) -0.0156(14) C11 0.0469(17) 0.0523(18) 0.0227(13) -0.0089(12) 0.0013(12) -0.0283(14) C12 0.0304(12) 0.0243(12) 0.0260(12) -0.0100(10) -0.0048(10) -0.0111(10) C13 0.0387(15) 0.0391(16) 0.0346(15) -0.0059(12) -0.0127(12) -0.0162(12) C14 0.0380(15) 0.0340(15) 0.0453(17) -0.0224(13) 0.0005(12) -0.0149(12) C15 0.0374(14) 0.0299(13) 0.0287(13) -0.0076(11) -0.0049(11) -0.0180(11) C16 0.0514(16) 0.0267(13) 0.0177(11) -0.0039(10) -0.0070(11) -0.0191(12) C17 0.0509(16) 0.0246(13) 0.0232(12) -0.0048(10) -0.0123(11) -0.0115(11) C18 0.0403(14) 0.0290(13) 0.0249(13) -0.0061(11) -0.0111(11) -0.0094(11) C19 0.0314(12) 0.0237(12) 0.0281(13) -0.0115(10) -0.0079(10) -0.0049(10) C20 0.0301(12) 0.0240(12) 0.0230(12) -0.0100(10) -0.0035(9) -0.0091(9) C21 0.0282(12) 0.0299(13) 0.0267(13) -0.0130(10) -0.0048(10) -0.0048(10) C22 0.0293(12) 0.0346(14) 0.0250(12) -0.0147(11) -0.0002(10) -0.0093(10) C23 0.0338(13) 0.0293(13) 0.0213(12) -0.0086(10) -0.0010(10) -0.0112(10) C24 0.0328(12) 0.0223(12) 0.0207(11) -0.0085(9) -0.0038(9) -0.0097(9) C25 0.0296(12) 0.0239(12) 0.0212(11) -0.0106(9) -0.0031(9) -0.0100(9) C26 0.0325(14) 0.0452(17) 0.0249(13) -0.0151(12) 0.0011(11) -0.0062(12) C27 0.038(3) 0.061(4) 0.024(2) -0.023(2) 0.0021(19) -0.010(2) C28 0.036(3) 0.061(4) 0.041(3) -0.024(3) 0.008(2) -0.020(2) C29 0.046(3) 0.044(3) 0.038(3) -0.016(2) 0.012(2) 0.001(2) C26A 0.0325(14) 0.0452(17) 0.0249(13) -0.0151(12) 0.0011(11) -0.0062(12) C27A 0.026(4) 0.087(9) 0.041(5) -0.024(5) 0.006(3) -0.007(4) C28A 0.046(5) 0.077(8) 0.034(5) -0.014(5) 0.009(4) -0.012(5) C29A 0.037(5) 0.092(8) 0.047(6) -0.046(6) 0.003(4) 0.002(5) C30 0.0376(14) 0.0217(12) 0.0224(12) -0.0081(10) -0.0008(10) -0.0106(10) C31 0.0367(14) 0.0256(13) 0.0376(15) -0.0134(11) -0.0035(11) -0.0051(11) C32 0.0513(17) 0.0263(14) 0.0276(14) -0.0057(11) -0.0022(12) -0.0096(12) C33 0.0471(16) 0.0251(13) 0.0278(13) -0.0132(11) 0.0001(11) -0.0128(11) C34 0.0259(11) 0.0195(11) 0.0253(12) -0.0087(9) -0.0057(9) -0.0060(9) C35 0.0252(11) 0.0195(11) 0.0224(11) -0.0091(9) -0.0014(9) -0.0075(9) C36 0.0270(11) 0.0184(11) 0.0191(11) -0.0085(9) -0.0010(9) -0.0074(9) C37 0.0243(11) 0.0196(11) 0.0220(11) -0.0095(9) -0.0014(9) -0.0046(9) C38 0.0249(11) 0.0247(12) 0.0220(12) -0.0093(9) 0.0005(9) -0.0077(9) C39 0.0296(12) 0.0212(11) 0.0210(11) -0.0076(9) -0.0017(9) -0.0082(9) C40 0.0255(11) 0.0214(11) 0.0228(12) -0.0074(9) -0.0041(9) -0.0064(9) C41 0.0230(11) 0.0290(13) 0.0221(12) -0.0071(10) -0.0023(9) -0.0063(9) C42 0.0250(12) 0.0347(14) 0.0262(13) -0.0081(11) -0.0028(10) -0.0066(10) C43 0.0299(13) 0.0286(14) 0.0393(16) -0.0015(12) -0.0067(11) -0.0043(11) C44 0.0287(13) 0.0521(18) 0.0291(14) -0.0193(13) -0.0033(10) -0.0124(12) C45 0.0288(12) 0.0270(12) 0.0190(11) -0.0077(9) -0.0025(9) -0.0082(10) C46 0.0337(14) 0.0419(16) 0.0238(13) -0.0144(12) 0.0002(10) -0.0075(12) C47 0.0317(13) 0.0389(15) 0.0235(13) -0.0090(11) -0.0058(10) -0.0076(11) C48 0.0418(15) 0.0296(14) 0.0267(13) -0.0040(11) -0.0036(11) -0.0145(11) C49 0.0216(11) 0.0336(14) 0.0292(13) -0.0112(11) -0.0002(9) -0.0084(10) C50 0.0357(15) 0.0353(15) 0.0327(15) -0.0105(12) 0.0012(12) 0.0041(12) C51 0.0288(13) 0.0280(13) 0.0353(14) -0.0151(11) 0.0004(11) -0.0025(10) C52 0.0301(12) 0.0277(13) 0.0266(12) -0.0153(10) 0.0034(10) -0.0102(10) C53 0.0368(13) 0.0226(12) 0.0227(12) -0.0088(10) 0.0012(10) -0.0131(10) C54 0.0330(12) 0.0215(11) 0.0205(11) -0.0078(9) -0.0015(9) -0.0126(9) C55 0.0382(14) 0.0212(12) 0.0224(12) -0.0080(10) -0.0026(10) -0.0106(10) C56 0.0566(18) 0.0201(12) 0.0243(13) -0.0060(10) -0.0044(12) -0.0113(11) C57 0.070(2) 0.0245(13) 0.0231(13) -0.0071(11) 0.0035(13) -0.0180(13) C58 0.0538(18) 0.0304(14) 0.0258(13) -0.0135(11) 0.0107(12) -0.0200(13) C59 0.0426(15) 0.0190(12) 0.0269(13) -0.0073(10) -0.0020(11) -0.0040(10) C60 0.0458(17) 0.0260(14) 0.054(2) -0.0153(14) 0.0110(14) -0.0093(12) C61 0.0460(16) 0.0209(13) 0.0349(15) -0.0080(11) -0.0048(12) -0.0061(11) C62 0.069(2) 0.0312(15) 0.0287(15) -0.0165(12) -0.0125(14) 0.0032(14) C63 0.112(3) 0.0317(17) 0.0253(15) -0.0069(13) 0.0129(18) -0.0288(19) C64 0.253(9) 0.075(4) 0.046(3) -0.005(2) 0.018(4) -0.101(5) C65 0.101(5) 0.155(7) 0.057(3) 0.030(4) -0.006(3) -0.003(4) C66 0.186(6) 0.045(2) 0.0252(18) -0.0094(16) -0.004(3) -0.012(3) C67 0.0287(12) 0.0267(12) 0.0194(11) -0.0119(9) 0.0023(9) -0.0101(9) C68 0.0265(12) 0.0336(14) 0.0253(12) -0.0159(11) 0.0001(9) -0.0065(10) C69 0.0328(13) 0.0266(13) 0.0273(13) -0.0121(10) -0.0051(10) -0.0011(10) C70 0.0290(12) 0.0252(12) 0.0180(11) -0.0105(9) 0.0029(9) -0.0116(9) C71 0.0298(13) 0.0459(17) 0.0370(15) -0.0263(13) 0.0001(11) -0.0111(12) C72 0.0445(18) 0.054(2) 0.062(2) -0.0273(18) -0.0289(17) 0.0111(15) Cl2 0.1623(18) 0.1005(12) 0.1245(14) -0.0328(11) -0.0535(13) -0.0491(12) Cl1 0.1355(17) 0.0772(11) 0.191(2) -0.0349(13) -0.0186(16) -0.0107(11) N8 0.069(2) 0.0455(18) 0.070(2) -0.0222(17) -0.0155(19) -0.0121(16) C77 0.0432(17) 0.0450(19) 0.057(2) -0.0294(17) -0.0143(16) -0.0008(14) N7 0.080(2) 0.055(2) 0.0431(18) -0.0114(15) -0.0039(17) -0.0018(17) C76 0.050(2) 0.061(2) 0.062(2) -0.031(2) -0.0142(17) -0.0065(17) C75 0.056(2) 0.047(2) 0.0433(19) -0.0048(16) -0.0161(17) -0.0060(16) C74 0.063(2) 0.070(3) 0.057(2) -0.023(2) -0.025(2) 0.003(2) C73 0.087(4) 0.105(4) 0.124(5) -0.056(4) -0.030(3) -0.037(3) Cl4 0.190(6) 0.185(5) 0.151(4) -0.092(4) 0.005(4) 0.020(4) Cl3 0.189(5) 0.189(5) 0.171(5) -0.083(4) -0.094(4) 0.069(4) C78 0.126(10) 0.114(9) 0.161(12) -0.112(10) -0.110(10) 0.072(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Fe1 O1 92.13(7) . . ? O2 Fe1 O7 98.79(8) . . ? O1 Fe1 O7 92.81(8) . . ? O2 Fe1 O5 93.54(7) . . ? O1 Fe1 O5 174.31(7) . . ? O7 Fe1 O5 86.65(8) . . ? O2 Fe1 N1 167.89(8) . . ? O1 Fe1 N1 85.28(8) . . ? O7 Fe1 N1 93.16(9) . . ? O5 Fe1 N1 89.09(8) . . ? O2 Fe1 N2 84.63(8) . . ? O1 Fe1 N2 96.52(8) . . ? O7 Fe1 N2 169.95(8) . . ? O5 Fe1 N2 83.70(8) . . ? N1 Fe1 N2 83.92(9) . . ? O3 Fe2 O4 95.39(7) . . ? O3 Fe2 N3 87.08(8) . . ? O4 Fe2 N3 106.30(8) . . ? O3 Fe2 N4 172.34(8) . . ? O4 Fe2 N4 85.80(8) . . ? N3 Fe2 N4 85.33(8) . . ? O3 Fe2 O6 93.73(7) . . ? O4 Fe2 O6 164.47(7) . . ? N3 Fe2 O6 86.67(7) . . ? N4 Fe2 O6 86.82(7) . . ? O3 Fe2 N6 90.19(8) . . ? O4 Fe2 N6 92.14(8) . . ? N3 Fe2 N6 161.53(8) . . ? N4 Fe2 N6 97.33(8) . . ? O6 Fe2 N6 75.28(7) . . ? C3 O1 Fe1 132.50(16) . . ? C25 O2 Fe1 124.35(15) . . ? C36 O3 Fe2 133.55(16) . . ? C54 O4 Fe2 129.99(16) . . ? C70 O5 Fe1 123.57(16) . . ? C70 O6 Fe2 119.64(16) . . ? C71 O7 Fe1 137.80(18) . . ? C1 N1 C16 116.9(2) . . ? C1 N1 Fe1 123.91(18) . . ? C16 N1 Fe1 118.91(16) . . ? C19 N2 C18 118.0(2) . . ? C19 N2 Fe1 118.91(18) . . ? C18 N2 Fe1 123.09(17) . . ? C34 N3 C49 118.0(2) . . ? C34 N3 Fe2 123.76(17) . . ? C49 N3 Fe2 118.10(16) . . ? C52 N4 C51 117.8(2) . . ? C52 N4 Fe2 122.64(18) . . ? C51 N4 Fe2 119.56(17) . . ? C69 N5 C68 108.3(2) . . ? C69 N5 C72 123.0(3) . . ? C68 N5 C72 128.6(3) . . ? C69 N6 C67 106.0(2) . . ? C69 N6 Fe2 137.31(18) . . ? C67 N6 Fe2 114.28(17) . . ? N1 C1 C2 126.9(2) . . ? C7 C2 C3 121.1(2) . . ? C7 C2 C1 116.4(2) . . ? C3 C2 C1 122.0(2) . . ? O1 C3 C2 121.3(2) . . ? O1 C3 C4 120.7(2) . . ? C2 C3 C4 118.0(2) . . ? C5 C4 C3 118.0(2) . . ? C5 C4 C8 121.2(2) . . ? C3 C4 C8 120.8(2) . . ? C4 C5 C6 124.5(2) . . ? C7 C6 C5 116.9(2) . . ? C7 C6 C12 123.6(2) . . ? C5 C6 C12 119.4(2) . . ? C6 C7 C2 121.5(2) . . ? C9 C8 C10 107.9(2) . . ? C9 C8 C4 112.3(2) . . ? C10 C8 C4 108.9(2) . . ? C9 C8 C11 107.0(2) . . ? C10 C8 C11 110.1(2) . . ? C4 C8 C11 110.5(2) . . ? C15 C12 C6 111.5(2) . . ? C15 C12 C13 107.9(2) . . ? C6 C12 C13 110.6(2) . . ? C15 C12 C14 108.4(2) . . ? C6 C12 C14 108.8(2) . . ? C13 C12 C14 109.5(2) . . ? N1 C16 C17 108.2(2) . . ? C16 C17 C18 114.9(2) . . ? N2 C18 C17 115.1(2) . . ? N2 C19 C20 126.5(2) . . ? C21 C20 C25 120.6(2) . . ? C21 C20 C19 117.6(2) . . ? C25 C20 C19 121.5(2) . . ? C22 C21 C20 121.7(2) . . ? C21 C22 C23 116.6(2) . . ? C21 C22 C26 122.7(2) . . ? C23 C22 C26 120.7(2) . . ? C24 C23 C22 124.8(2) . . ? C23 C24 C25 117.4(2) . . ? C23 C24 C30 121.7(2) . . ? C25 C24 C30 120.9(2) . . ? O2 C25 C20 121.0(2) . . ? O2 C25 C24 120.6(2) . . ? C20 C25 C24 118.3(2) . . ? C27 C26 C29 109.4(4) . . ? C27 C26 C22 109.9(3) . . ? C29 C26 C22 113.5(3) . . ? C27 C26 C28 108.5(4) . . ? C29 C26 C28 106.6(4) . . ? C22 C26 C28 108.9(3) . . ? C24 C30 C32 112.1(2) . . ? C24 C30 C31 112.7(2) . . ? C32 C30 C31 107.4(2) . . ? C24 C30 C33 107.9(2) . . ? C32 C30 C33 106.9(2) . . ? C31 C30 C33 109.7(2) . . ? N3 C34 C35 127.8(2) . . ? C40 C35 C36 120.2(2) . . ? C40 C35 C34 117.5(2) . . ? C36 C35 C34 122.3(2) . . ? O3 C36 C35 120.8(2) . . ? O3 C36 C37 120.0(2) . . ? C35 C36 C37 119.2(2) . . ? C38 C37 C36 117.6(2) . . ? C38 C37 C41 122.0(2) . . ? C36 C37 C41 120.4(2) . . ? C37 C38 C39 124.3(2) . . ? C40 C39 C38 117.2(2) . . ? C40 C39 C45 123.3(2) . . ? C38 C39 C45 119.4(2) . . ? C39 C40 C35 121.5(2) . . ? C42 C41 C37 112.2(2) . . ? C42 C41 C43 107.3(2) . . ? C37 C41 C43 110.1(2) . . ? C42 C41 C44 107.0(2) . . ? C37 C41 C44 110.0(2) . . ? C43 C41 C44 110.3(2) . . ? C47 C45 C39 111.5(2) . . ? C47 C45 C48 108.8(2) . . ? C39 C45 C48 108.5(2) . . ? C47 C45 C46 107.6(2) . . ? C39 C45 C46 110.6(2) . . ? C48 C45 C46 109.8(2) . . ? N3 C49 C50 111.5(2) . . ? C51 C50 C49 116.2(2) . . ? N4 C51 C50 112.2(2) . . ? N4 C52 C53 126.7(2) . . ? C58 C53 C54 120.6(2) . . ? C58 C53 C52 117.0(2) . . ? C54 C53 C52 122.3(2) . . ? O4 C54 C53 121.1(2) . . ? O4 C54 C55 120.4(2) . . ? C53 C54 C55 118.5(2) . . ? C56 C55 C54 117.7(2) . . ? C56 C55 C59 121.2(2) . . ? C54 C55 C59 121.0(2) . . ? C55 C56 C57 124.4(3) . . ? C58 C57 C56 116.9(3) . . ? C58 C57 C63 123.1(3) . . ? C56 C57 C63 119.9(3) . . ? C57 C58 C53 121.5(3) . . ? C61 C59 C55 112.1(2) . . ? C61 C59 C60 107.8(2) . . ? C55 C59 C60 110.5(2) . . ? C61 C59 C62 107.3(2) . . ? C55 C59 C62 109.1(2) . . ? C60 C59 C62 110.0(3) . . ? C64 C63 C66 121.4(4) . . ? C64 C63 C57 111.8(3) . . ? C66 C63 C57 112.9(3) . . ? C64 C63 C65 101.5(5) . . ? C66 C63 C65 98.6(5) . . ? C57 C63 C65 108.1(4) . . ? N6 C67 C68 109.9(2) . . ? N6 C67 C70 115.5(2) . . ? C68 C67 C70 134.2(2) . . ? C67 C68 N5 104.7(2) . . ? C67 C68 C71 132.6(3) . . ? N5 C68 C71 122.6(2) . . ? N6 C69 N5 111.1(2) . . ? O5 C70 O6 124.3(2) . . ? O5 C70 C67 121.0(2) . . ? O6 C70 C67 114.7(2) . . ? O8 C71 O7 124.9(3) . . ? O8 C71 C68 118.1(3) . . ? O7 C71 C68 117.0(2) . . ? N8 C77 C76 176.3(4) . . ? N7 C75 C74 179.7(5) . . ? Cl1 C73 Cl2 107.5(3) . . ? Cl4 C78 Cl3 111.6(6) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O2 1.9321(17) . ? Fe1 O1 1.9393(18) . ? Fe1 O7 1.998(2) . ? Fe1 O5 2.0937(18) . ? Fe1 N1 2.115(2) . ? Fe1 N2 2.141(2) . ? Fe2 O3 1.9020(17) . ? Fe2 O4 1.9099(18) . ? Fe2 N3 2.104(2) . ? Fe2 N4 2.126(2) . ? Fe2 O6 2.1298(18) . ? Fe2 N6 2.140(2) . ? O1 C3 1.319(3) . ? O2 C25 1.320(3) . ? O3 C36 1.314(3) . ? O4 C54 1.319(3) . ? O5 C70 1.259(3) . ? O6 C70 1.265(3) . ? O7 C71 1.278(4) . ? O8 C71 1.222(4) . ? N1 C1 1.289(3) . ? N1 C16 1.471(3) . ? N2 C19 1.282(3) . ? N2 C18 1.468(3) . ? N3 C34 1.288(3) . ? N3 C49 1.470(3) . ? N4 C52 1.284(3) . ? N4 C51 1.470(3) . ? N5 C69 1.344(4) . ? N5 C68 1.381(4) . ? N5 C72 1.472(4) . ? N6 C69 1.319(3) . ? N6 C67 1.376(3) . ? C1 C2 1.448(3) . ? C2 C7 1.411(3) . ? C2 C3 1.417(3) . ? C3 C4 1.437(3) . ? C4 C5 1.381(3) . ? C4 C8 1.537(3) . ? C5 C6 1.416(3) . ? C6 C7 1.372(3) . ? C6 C12 1.534(3) . ? C8 C9 1.533(4) . ? C8 C10 1.534(4) . ? C8 C11 1.537(4) . ? C12 C15 1.525(4) . ? C12 C13 1.536(4) . ? C12 C14 1.543(4) . ? C16 C17 1.530(4) . ? C17 C18 1.531(4) . ? C19 C20 1.455(4) . ? C20 C21 1.411(4) . ? C20 C25 1.418(4) . ? C21 C22 1.381(4) . ? C22 C23 1.406(4) . ? C22 C26 1.536(4) . ? C23 C24 1.394(4) . ? C24 C25 1.434(3) . ? C24 C30 1.532(4) . ? C26 C27 1.502(6) . ? C26 C29 1.519(6) . ? C26 C28 1.573(6) . ? C30 C32 1.536(4) . ? C30 C31 1.537(4) . ? C30 C33 1.540(4) . ? C34 C35 1.449(3) . ? C35 C40 1.413(3) . ? C35 C36 1.415(3) . ? C36 C37 1.430(3) . ? C37 C38 1.387(3) . ? C37 C41 1.537(3) . ? C38 C39 1.411(4) . ? C39 C40 1.379(3) . ? C39 C45 1.539(3) . ? C41 C42 1.525(3) . ? C41 C43 1.538(4) . ? C41 C44 1.541(4) . ? C45 C47 1.536(4) . ? C45 C48 1.539(4) . ? C45 C46 1.540(4) . ? C49 C50 1.531(4) . ? C50 C51 1.524(4) . ? C52 C53 1.444(4) . ? C53 C58 1.407(4) . ? C53 C54 1.410(4) . ? C54 C55 1.430(4) . ? C55 C56 1.388(4) . ? C55 C59 1.537(4) . ? C56 C57 1.398(4) . ? C57 C58 1.381(4) . ? C57 C63 1.542(4) . ? C59 C61 1.534(4) . ? C59 C60 1.537(4) . ? C59 C62 1.540(4) . ? C63 C64 1.437(6) . ? C63 C66 1.462(5) . ? C63 C65 1.630(7) . ? C67 C68 1.377(4) . ? C67 C70 1.480(4) . ? C68 C71 1.503(4) . ? Cl2 C73 1.827(7) . ? Cl1 C73 1.736(6) . ? N8 C77 1.111(5) . ? C77 C76 1.482(6) . ? N7 C75 1.136(5) . ? C75 C74 1.475(6) . ? Cl4 C78 1.512(13) . ? Cl3 C78 1.724(13) . ?
1100757.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100757.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100757 loop_ _publ_author_name 'Panagiotis Angaridis' 'Jeff W. Kampf' 'Vincent L. Pecoraro' _publ_contact_author_address ; Chemistry Department University of Michigan 930 N.University Ann Arbor, MI 48109, USA ; _publ_contact_author_email vlpec@umich.edu _publ_contact_author_fax '(734) 936 7628' _publ_contact_author_name 'Vincent. L. Pecoraro' _publ_contact_author_phone '(734) 763 1519' _publ_section_title ; Multinuclear Fe(III) Complexes with Polydentate Ligands of the Family of Dicarboxyimidazoles: Nuclearity- and Topology-Controlled Syntheses and Magneto-Structural Correlations ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3626 _journal_page_last 3635 _journal_paper_doi 10.1021/ic0481879 _journal_volume 44 _journal_year 2005 _chemical_formula_moiety '2(C71 H98 Fe2 N6 O8)' _chemical_formula_sum 'C71 H98 Fe2 N6 O8' _chemical_formula_weight 1275.25 _chemical_name_systematic ; ? ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 80.730(11) _cell_angle_beta 88.282(11) _cell_angle_gamma 85.548(11) _cell_formula_units_Z 4 _cell_length_a 12.641(2) _cell_length_b 17.362(3) _cell_length_c 33.972(6) _cell_measurement_reflns_used 5790 _cell_measurement_temperature 113(2) _cell_measurement_theta_max 26.07 _cell_measurement_theta_min 2.88 _cell_volume 7335(2) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _diffrn_ambient_temperature 113(2) _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0466 _diffrn_reflns_av_sigmaI/netI 0.0659 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_number 66017 _diffrn_reflns_theta_full 26.42 _diffrn_reflns_theta_max 26.42 _diffrn_reflns_theta_min 2.81 _exptl_absorpt_coefficient_mu 0.449 _exptl_absorpt_correction_T_max 0.9155 _exptl_absorpt_correction_T_min 0.8269 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Blessing, R. Acta Cryst. (1995) A51 33-38 Sheldrick, G. SADABS (Version 2.10) Bruker/Siemens area detector absorption and other corrections, University of Gottingen, Germany 2003. ; _exptl_crystal_colour purple _exptl_crystal_density_diffrn 1.155 _exptl_crystal_density_method 'not measured' _exptl_crystal_description wedge _exptl_crystal_F_000 2728 _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.20 _refine_diff_density_max 0.638 _refine_diff_density_min -0.617 _refine_diff_density_rms 0.064 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 1676 _refine_ls_number_reflns 29894 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.018 _refine_ls_R_factor_all 0.0973 _refine_ls_R_factor_gt 0.0571 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0657P)^2^+6.8096P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1344 _refine_ls_wR_factor_ref 0.1539 _reflns_number_gt 20140 _reflns_number_total 29894 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic0481879si20041222_050013_4.cif _cod_data_source_block compound3 _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_database_code 1100757 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.96071(3) 0.31914(3) 0.560944(13) 0.02949(11) Uani 1 1 d . . . Fe2 Fe 0.73750(3) 0.09098(3) 0.704392(13) 0.02720(11) Uani 1 1 d . . . Fe3 Fe 0.04603(3) 0.39207(3) 0.919619(13) 0.02823(11) Uani 1 1 d . . . Fe4 Fe 0.31840(3) 0.12765(2) 0.839087(13) 0.02537(11) Uani 1 1 d . . . N1 N 1.06433(19) 0.39425(15) 0.52674(7) 0.0288(6) Uani 1 1 d . . . N2 N 1.0268(2) 0.23533(15) 0.52624(8) 0.0311(6) Uani 1 1 d . . . N3 N 0.8970(2) 0.23459(15) 0.60641(8) 0.0306(6) Uani 1 1 d . . . N4 N 0.81970(19) 0.15633(15) 0.65631(7) 0.0285(6) Uani 1 1 d . . . N5 N 0.6985(3) 0.02509(17) 0.75989(8) 0.0424(7) Uani 1 1 d . . . N6 N 0.70918(19) 0.18759(15) 0.73513(7) 0.0289(6) Uani 1 1 d . . . N7 N -0.0710(2) 0.47887(15) 0.93245(8) 0.0295(6) Uani 1 1 d . . . N8 N 0.0002(2) 0.32950(16) 0.97562(8) 0.0394(7) Uani 1 1 d . . . N9 N 0.12448(19) 0.29389(14) 0.89840(7) 0.0270(5) Uani 1 1 d . . . N10 N 0.21921(19) 0.20621(14) 0.86758(7) 0.0257(5) Uani 1 1 d . . . N11 N 0.3630(2) 0.04947(15) 0.79925(8) 0.0310(6) Uani 1 1 d . . . N12 N 0.3290(2) 0.21276(15) 0.78698(7) 0.0301(6) Uani 1 1 d . . . O1 O 0.91594(18) 0.40447(14) 0.58686(7) 0.0432(6) Uani 1 1 d . . . O2 O 0.83737(16) 0.32406(12) 0.52947(6) 0.0288(5) Uani 1 1 d . . . O3 O 1.09503(18) 0.28302(15) 0.59889(7) 0.0424(6) Uani 1 1 d . . . O4 O 1.14553(18) 0.21013(17) 0.65688(7) 0.0519(7) Uani 1 1 d . . . H4A H 1.1169 0.1805 0.6755 0.078 Uiso 0.50 1 calc PR A 1 O5 O 1.05970(18) 0.12185(17) 0.71217(7) 0.0531(7) Uani 1 1 d . . . H5B H 1.0897 0.1513 0.6939 0.080 Uiso 0.50 1 calc PR B 2 O6 O 0.75021(18) -0.00651(12) 0.68565(6) 0.0347(5) Uani 1 1 d . . . O7 O 0.60272(15) 0.12150(11) 0.68076(6) 0.0256(4) Uani 1 1 d . . . O8 O 0.89764(17) 0.07984(14) 0.72555(6) 0.0377(5) Uani 1 1 d . . . O9 O 0.07020(16) 0.45891(12) 0.87090(6) 0.0324(5) Uani 1 1 d . . . O10 O 0.16935(17) 0.41238(13) 0.94576(7) 0.0372(5) Uani 1 1 d . . . O11 O -0.08321(16) 0.33942(13) 0.89616(7) 0.0351(5) Uani 1 1 d . . . O12 O -0.11959(17) 0.24701(14) 0.86057(7) 0.0410(6) Uani 1 1 d . . . H12S H -0.0850 0.2132 0.8492 0.062 Uiso 0.50 1 calc PR C 1 O13 O -0.01484(17) 0.14645(14) 0.82696(7) 0.0408(6) Uani 1 1 d . . . H13W H -0.0513 0.1798 0.8380 0.061 Uiso 0.50 1 calc PR D 2 O14 O 0.31114(16) 0.04000(12) 0.87976(6) 0.0310(5) Uani 1 1 d . . . O15 O 0.44556(15) 0.16186(12) 0.85531(6) 0.0275(5) Uani 1 1 d . . . O16 O 0.15675(17) 0.10885(12) 0.82025(6) 0.0332(5) Uani 1 1 d . . . C1 C 0.9616(3) 0.46558(19) 0.59434(10) 0.0343(7) Uani 1 1 d . . . C2 C 0.9249(3) 0.5059(2) 0.62597(11) 0.0458(9) Uani 1 1 d . . . C3 C 0.9755(3) 0.57016(19) 0.63151(10) 0.0379(8) Uani 1 1 d . . . H3A H 0.9506 0.5969 0.6527 0.046 Uiso 1 1 calc R . . C4 C 1.0613(2) 0.59937(18) 0.60832(10) 0.0309(7) Uani 1 1 d . . . C5 C 1.0947(2) 0.56087(18) 0.57763(9) 0.0306(7) Uani 1 1 d . . . H5A H 1.1514 0.5799 0.5608 0.037 Uiso 1 1 calc R . . C6 C 1.0480(2) 0.49418(17) 0.57028(9) 0.0280(7) Uani 1 1 d . . . C7 C 1.0896(2) 0.45817(18) 0.53696(9) 0.0303(7) Uani 1 1 d . . . H7A H 1.1419 0.4851 0.5207 0.036 Uiso 1 1 calc R . . C8 C 1.1218(3) 0.3679(2) 0.49257(10) 0.0365(8) Uani 1 1 d . . . H8A H 1.1635 0.4105 0.4787 0.044 Uiso 1 1 calc R . . H8B H 1.0703 0.3555 0.4735 0.044 Uiso 1 1 calc R . . C9 C 1.1956(3) 0.2961(2) 0.50597(13) 0.0490(10) Uani 1 1 d . . . H9A H 1.2414 0.3079 0.5271 0.059 Uiso 1 1 calc R . . H9B H 1.2424 0.2863 0.4831 0.059 Uiso 1 1 calc R . . C10 C 1.1423(3) 0.2211(2) 0.52189(11) 0.0414(8) Uani 1 1 d . . . H10A H 1.1579 0.1829 0.5034 0.050 Uiso 1 1 calc R . . H10B H 1.1722 0.1981 0.5481 0.050 Uiso 1 1 calc R . . C11 C 0.9675(3) 0.19236(19) 0.51035(10) 0.0343(7) Uani 1 1 d . . . H11A H 1.0028 0.1502 0.4994 0.041 Uiso 1 1 calc R . . C12 C 0.8540(3) 0.20084(18) 0.50729(9) 0.0316(7) Uani 1 1 d . . . C13 C 0.8069(3) 0.1442(2) 0.48986(10) 0.0408(8) Uani 1 1 d . . . H13A H 0.8496 0.0998 0.4840 0.049 Uiso 1 1 calc R . . C14 C 0.7017(3) 0.1511(2) 0.48105(10) 0.0411(8) Uani 1 1 d . . . C15 C 0.6418(3) 0.2155(2) 0.49110(10) 0.0404(8) Uani 1 1 d . . . H15A H 0.5679 0.2196 0.4859 0.048 Uiso 1 1 calc R . . C16 C 0.6816(2) 0.27451(19) 0.50826(9) 0.0324(7) Uani 1 1 d . . . C17 C 0.7925(2) 0.26753(18) 0.51597(9) 0.0288(7) Uani 1 1 d . . . C18 C 0.8083(2) 0.20165(18) 0.62046(9) 0.0280(7) Uani 1 1 d . . . H18A H 0.7435 0.2095 0.6064 0.034 Uiso 1 1 calc R . . C19 C 0.9236(2) 0.16081(19) 0.66557(9) 0.0322(7) Uani 1 1 d . . . C20 C 0.9706(2) 0.2084(2) 0.63515(9) 0.0346(7) Uani 1 1 d . . . C21 C 1.0776(3) 0.2357(2) 0.63010(10) 0.0401(8) Uani 1 1 d . . . C22 C 0.9625(3) 0.1182(2) 0.70319(10) 0.0383(8) Uani 1 1 d . . . C23 C 0.6840(3) -0.06244(19) 0.69233(10) 0.0352(8) Uani 1 1 d . . . C24 C 0.6779(3) -0.1152(2) 0.66483(11) 0.0409(8) Uani 1 1 d . . . C25 C 0.6011(3) -0.1678(2) 0.67205(13) 0.0537(11) Uani 1 1 d . . . H25A H 0.5934 -0.2009 0.6528 0.064 Uiso 1 1 calc R . . C26 C 0.5331(3) -0.1765(2) 0.70565(14) 0.0551(11) Uani 1 1 d . E . C27 C 0.5482(3) -0.1299(2) 0.73362(12) 0.0470(9) Uani 1 1 d . . . H27A H 0.5073 -0.1367 0.7577 0.056 Uiso 1 1 calc R . . C28 C 0.6219(3) -0.07270(18) 0.72806(10) 0.0347(7) Uani 1 1 d . . . C29 C 0.6436(3) -0.03430(19) 0.76096(10) 0.0399(8) Uani 1 1 d . . . H29A H 0.6142 -0.0550 0.7862 0.048 Uiso 1 1 calc R . . C30 C 0.7424(4) 0.0432(3) 0.79806(12) 0.0618(12) Uani 1 1 d . . . H30A H 0.7097 0.0100 0.8209 0.074 Uiso 1 1 calc R . . H30B H 0.8197 0.0288 0.7984 0.074 Uiso 1 1 calc R . . C31 C 0.7247(4) 0.1236(3) 0.80338(12) 0.0666(13) Uani 1 1 d . . . H31A H 0.7565 0.1283 0.8291 0.080 Uiso 1 1 calc R . . H31B H 0.6471 0.1345 0.8065 0.080 Uiso 1 1 calc R . . C32 C 0.7634(3) 0.1878(2) 0.77285(9) 0.0357(8) Uani 1 1 d . . . H32A H 0.7480 0.2389 0.7820 0.043 Uiso 1 1 calc R . . H32B H 0.8411 0.1794 0.7689 0.043 Uiso 1 1 calc R . . C33 C 0.6407(2) 0.24544(18) 0.72383(9) 0.0287(7) Uani 1 1 d . . . H33A H 0.6395 0.2883 0.7381 0.034 Uiso 1 1 calc R . . C34 C 0.5661(2) 0.25254(17) 0.69223(9) 0.0248(6) Uani 1 1 d . . . C35 C 0.5031(2) 0.32379(17) 0.68424(9) 0.0288(7) Uani 1 1 d . . . H35A H 0.5176 0.3657 0.6976 0.035 Uiso 1 1 calc R . . C36 C 0.4214(2) 0.33458(17) 0.65773(9) 0.0279(7) Uani 1 1 d . . . C37 C 0.4035(2) 0.27059(18) 0.63882(9) 0.0278(7) Uani 1 1 d . . . H37A H 0.3464 0.2766 0.6208 0.033 Uiso 1 1 calc R . . C38 C 0.4630(2) 0.19935(17) 0.64456(9) 0.0253(6) Uani 1 1 d . . . C39 C 0.5464(2) 0.18951(17) 0.67252(8) 0.0243(6) Uani 1 1 d . . . C40 C 0.8295(4) 0.4777(3) 0.65207(14) 0.0854(19) Uani 1 1 d D . . C41 C 0.8044(5) 0.5288(3) 0.68466(18) 0.113(3) Uani 1 1 d D . . H41A H 0.7819 0.5823 0.6722 0.170 Uiso 1 1 calc R . . H41B H 0.8680 0.5296 0.7004 0.170 Uiso 1 1 calc R . . H41C H 0.7473 0.5072 0.7022 0.170 Uiso 1 1 calc R . . C42 C 0.8551(6) 0.3932(3) 0.67302(17) 0.140(4) Uani 1 1 d D . . H42A H 0.7940 0.3755 0.6895 0.210 Uiso 1 1 calc R . . H42B H 0.9169 0.3913 0.6900 0.210 Uiso 1 1 calc R . . H42C H 0.8706 0.3590 0.6529 0.210 Uiso 1 1 calc R . . C43 C 0.7321(4) 0.4833(4) 0.6261(2) 0.141(4) Uani 1 1 d D . . H43A H 0.7123 0.5384 0.6157 0.211 Uiso 1 1 calc R . . H43B H 0.6731 0.4605 0.6421 0.211 Uiso 1 1 calc R . . H43C H 0.7484 0.4546 0.6038 0.211 Uiso 1 1 calc R . . C44 C 1.1083(3) 0.67451(19) 0.61542(10) 0.0378(8) Uani 1 1 d . . . C45 C 1.1107(5) 0.6806(3) 0.65902(13) 0.096(2) Uani 1 1 d . . . H45A H 1.1456 0.7275 0.6624 0.144 Uiso 1 1 calc R . . H45B H 1.1501 0.6341 0.6733 0.144 Uiso 1 1 calc R . . H45C H 1.0380 0.6841 0.6698 0.144 Uiso 1 1 calc R . . C46 C 1.0400(3) 0.7424(2) 0.59305(15) 0.0656(13) Uani 1 1 d . . . H46A H 0.9664 0.7397 0.6028 0.098 Uiso 1 1 calc R . . H46B H 1.0432 0.7395 0.5645 0.098 Uiso 1 1 calc R . . H46C H 1.0663 0.7919 0.5975 0.098 Uiso 1 1 calc R . . C47 C 1.2221(3) 0.6799(2) 0.59833(12) 0.0497(10) Uani 1 1 d . . . H47A H 1.2507 0.7276 0.6043 0.075 Uiso 1 1 calc R . . H47B H 1.2214 0.6814 0.5694 0.075 Uiso 1 1 calc R . . H47C H 1.2668 0.6341 0.6105 0.075 Uiso 1 1 calc R . . C48 C 0.6557(3) 0.0883(3) 0.46016(11) 0.0544(11) Uani 1 1 d . . . C49 C 0.5443(4) 0.1129(3) 0.4471(2) 0.102(2) Uani 1 1 d . . . H49A H 0.5180 0.0732 0.4331 0.153 Uiso 1 1 calc R . . H49B H 0.5432 0.1631 0.4291 0.153 Uiso 1 1 calc R . . H49C H 0.4988 0.1185 0.4705 0.153 Uiso 1 1 calc R . . C50 C 0.6587(4) 0.0113(3) 0.48860(15) 0.0772(15) Uani 1 1 d . . . H50A H 0.6146 0.0175 0.5123 0.116 Uiso 1 1 calc R . . H50B H 0.7321 -0.0045 0.4966 0.116 Uiso 1 1 calc R . . H50C H 0.6315 -0.0290 0.4753 0.116 Uiso 1 1 calc R . . C51 C 0.7273(4) 0.0751(3) 0.42378(14) 0.0837(17) Uani 1 1 d . . . H51A H 0.7024 0.0322 0.4118 0.126 Uiso 1 1 calc R . . H51B H 0.8006 0.0617 0.4324 0.126 Uiso 1 1 calc R . . H51C H 0.7243 0.1231 0.4040 0.126 Uiso 1 1 calc R . . C52 C 0.6113(2) 0.3445(2) 0.51837(10) 0.0385(8) Uani 1 1 d . . . C53 C 0.6477(3) 0.4204(2) 0.49359(12) 0.0507(10) Uani 1 1 d . . . H53A H 0.7208 0.4274 0.5004 0.076 Uiso 1 1 calc R . . H53B H 0.6011 0.4651 0.4995 0.076 Uiso 1 1 calc R . . H53C H 0.6444 0.4171 0.4651 0.076 Uiso 1 1 calc R . . C54 C 0.4943(3) 0.3388(3) 0.50851(13) 0.0546(11) Uani 1 1 d . . . H54A H 0.4882 0.3381 0.4799 0.082 Uiso 1 1 calc R . . H54B H 0.4514 0.3840 0.5158 0.082 Uiso 1 1 calc R . . H54C H 0.4689 0.2906 0.5236 0.082 Uiso 1 1 calc R . . C55 C 0.6168(3) 0.3499(2) 0.56278(10) 0.0417(8) Uani 1 1 d . . . H55A H 0.5863 0.3043 0.5785 0.063 Uiso 1 1 calc R . . H55B H 0.5765 0.3978 0.5681 0.063 Uiso 1 1 calc R . . H55C H 0.6910 0.3511 0.5701 0.063 Uiso 1 1 calc R . . C56 C 0.7569(3) -0.1145(2) 0.62964(11) 0.0463(9) Uani 1 1 d . . . C57 C 0.8695(3) -0.1271(2) 0.64577(11) 0.0489(9) Uani 1 1 d . . . H57A H 0.8819 -0.0858 0.6612 0.073 Uiso 1 1 calc R . . H57B H 0.9207 -0.1256 0.6235 0.073 Uiso 1 1 calc R . . H57C H 0.8782 -0.1782 0.6630 0.073 Uiso 1 1 calc R . . C58 C 0.7411(4) -0.1801(3) 0.60541(14) 0.0659(13) Uani 1 1 d . . . H58A H 0.7496 -0.2309 0.6228 0.099 Uiso 1 1 calc R . . H58B H 0.7939 -0.1784 0.5836 0.099 Uiso 1 1 calc R . . H58C H 0.6696 -0.1728 0.5943 0.099 Uiso 1 1 calc R . . C59 C 0.7448(4) -0.0370(3) 0.60096(12) 0.0659(13) Uani 1 1 d . . . H59A H 0.6711 -0.0273 0.5922 0.099 Uiso 1 1 calc R . . H59B H 0.7920 -0.0397 0.5777 0.099 Uiso 1 1 calc R . . H59C H 0.7634 0.0056 0.6146 0.099 Uiso 1 1 calc R . . C60 C 0.4474(4) -0.2352(3) 0.71054(17) 0.0789(15) Uani 1 1 d D . . C61A C 0.4488(12) -0.2859(10) 0.6779(5) 0.113(5) Uani 0.50 1 d PD E 1 H61A H 0.3886 -0.3188 0.6819 0.169 Uiso 0.50 1 calc PR E 1 H61B H 0.5152 -0.3192 0.6790 0.169 Uiso 0.50 1 calc PR E 1 H61C H 0.4435 -0.2523 0.6518 0.169 Uiso 0.50 1 calc PR E 1 C62A C 0.3365(6) -0.1918(7) 0.7121(4) 0.081(3) Uani 0.50 1 d PD E 1 H62A H 0.2826 -0.2300 0.7174 0.121 Uiso 0.50 1 calc PR E 1 H62B H 0.3225 -0.1581 0.6865 0.121 Uiso 0.50 1 calc PR E 1 H62C H 0.3339 -0.1597 0.7334 0.121 Uiso 0.50 1 calc PR E 1 C63A C 0.4590(9) -0.2825(8) 0.7526(4) 0.129(8) Uani 0.50 1 d PD E 1 H63A H 0.4456 -0.2475 0.7724 0.193 Uiso 0.50 1 calc PR E 1 H63B H 0.5312 -0.3076 0.7556 0.193 Uiso 0.50 1 calc PR E 1 H63C H 0.4078 -0.3227 0.7567 0.193 Uiso 0.50 1 calc PR E 1 C61B C 0.3936(15) -0.2478(13) 0.7503(4) 0.146(9) Uani 0.50 1 d PD E 2 H61D H 0.3541 -0.1992 0.7549 0.220 Uiso 0.50 1 calc PR E 2 H61E H 0.4468 -0.2635 0.7710 0.220 Uiso 0.50 1 calc PR E 2 H61F H 0.3445 -0.2891 0.7512 0.220 Uiso 0.50 1 calc PR E 2 C62B C 0.4986(10) -0.3175(5) 0.7066(5) 0.098(4) Uani 0.50 1 d PD E 2 H62D H 0.5515 -0.3336 0.7274 0.147 Uiso 0.50 1 calc PR E 2 H62E H 0.5331 -0.3160 0.6803 0.147 Uiso 0.50 1 calc PR E 2 H62F H 0.4436 -0.3549 0.7095 0.147 Uiso 0.50 1 calc PR E 2 C63B C 0.3711(11) -0.2124(11) 0.6757(4) 0.138(7) Uani 0.50 1 d PD E 2 H63A H 0.3154 -0.2492 0.6782 0.207 Uiso 0.50 1 calc PR E 2 H63B H 0.4103 -0.2140 0.6505 0.207 Uiso 0.50 1 calc PR E 2 H63C H 0.3388 -0.1593 0.6761 0.207 Uiso 0.50 1 calc PR E 2 C64 C 0.3502(3) 0.41060(18) 0.64901(10) 0.0331(7) Uani 1 1 d . . . C65 C 0.3518(3) 0.4415(2) 0.60406(11) 0.0590(12) Uani 1 1 d . . . H65A H 0.4247 0.4509 0.5951 0.088 Uiso 1 1 calc R . . H65B H 0.3070 0.4906 0.5987 0.088 Uiso 1 1 calc R . . H65C H 0.3246 0.4028 0.5897 0.088 Uiso 1 1 calc R . . C66 C 0.3880(3) 0.4740(2) 0.67078(13) 0.0509(10) Uani 1 1 d . . . H66A H 0.3877 0.4553 0.6996 0.076 Uiso 1 1 calc R . . H66B H 0.3403 0.5215 0.6650 0.076 Uiso 1 1 calc R . . H66C H 0.4602 0.4857 0.6617 0.076 Uiso 1 1 calc R . . C67 C 0.2362(3) 0.3958(2) 0.66226(11) 0.0407(8) Uani 1 1 d . . . H67A H 0.2111 0.3553 0.6486 0.061 Uiso 1 1 calc R . . H67B H 0.1908 0.4443 0.6555 0.061 Uiso 1 1 calc R . . H67C H 0.2335 0.3784 0.6912 0.061 Uiso 1 1 calc R . . C68 C 0.4442(2) 0.13421(18) 0.62056(9) 0.0287(7) Uani 1 1 d . . . C69 C 0.4194(3) 0.05753(19) 0.64764(10) 0.0360(8) Uani 1 1 d . . . H69A H 0.4747 0.0432 0.6677 0.054 Uiso 1 1 calc R . . H69B H 0.4174 0.0158 0.6315 0.054 Uiso 1 1 calc R . . H69C H 0.3504 0.0648 0.6610 0.054 Uiso 1 1 calc R . . C70 C 0.3516(3) 0.1568(2) 0.59208(10) 0.0393(8) Uani 1 1 d . . . H70A H 0.2866 0.1675 0.6074 0.059 Uiso 1 1 calc R . . H70B H 0.3420 0.1136 0.5774 0.059 Uiso 1 1 calc R . . H70C H 0.3666 0.2037 0.5732 0.059 Uiso 1 1 calc R . . C71 C 0.5442(2) 0.1194(2) 0.59502(9) 0.0335(7) Uani 1 1 d . . . H71A H 0.5577 0.1673 0.5766 0.050 Uiso 1 1 calc R . . H71B H 0.5333 0.0774 0.5797 0.050 Uiso 1 1 calc R . . H71C H 0.6051 0.1039 0.6124 0.050 Uiso 1 1 calc R . . C72 C 0.0163(2) 0.51734(17) 0.84929(9) 0.0287(7) Uani 1 1 d . . . C73 C 0.0421(2) 0.53942(18) 0.80791(9) 0.0319(7) Uani 1 1 d . . . C74 C -0.0159(3) 0.60256(19) 0.78705(10) 0.0367(8) Uani 1 1 d . . . H74A H 0.0013 0.6173 0.7596 0.044 Uiso 1 1 calc R . . C75 C -0.0987(3) 0.64667(19) 0.80352(11) 0.0409(8) Uani 1 1 d . . . C76 C -0.1229(3) 0.62363(19) 0.84325(10) 0.0376(8) Uani 1 1 d . . . H76A H -0.1788 0.6518 0.8554 0.045 Uiso 1 1 calc R . . C77 C -0.0673(2) 0.55957(17) 0.86638(9) 0.0294(7) Uani 1 1 d . . . C78 C -0.1037(2) 0.53776(18) 0.90724(9) 0.0298(7) Uani 1 1 d . . . H78A H -0.1586 0.5715 0.9163 0.036 Uiso 1 1 calc R . . C79 C -0.1296(3) 0.46490(19) 0.97097(10) 0.0355(8) Uani 1 1 d . . . H79A H -0.1832 0.5090 0.9727 0.043 Uiso 1 1 calc R . . H79B H -0.0799 0.4615 0.9932 0.043 Uiso 1 1 calc R . . C80 C -0.1844(3) 0.3886(2) 0.97422(10) 0.0400(8) Uani 1 1 d . . . H80A H -0.2404 0.3881 0.9953 0.048 Uiso 1 1 calc R . . H80B H -0.2196 0.3877 0.9487 0.048 Uiso 1 1 calc R . . C81 C -0.1112(3) 0.3144(2) 0.98376(11) 0.0454(9) Uani 1 1 d . . . H81A H -0.1203 0.2920 1.0122 0.054 Uiso 1 1 calc R . . H81B H -0.1313 0.2754 0.9676 0.054 Uiso 1 1 calc R . . C82 C 0.0684(3) 0.3013(2) 1.00268(11) 0.0516(10) Uani 1 1 d . . . H82A H 0.0417 0.2694 1.0257 0.062 Uiso 1 1 calc R . . C83 C 0.1801(3) 0.3125(3) 1.00209(11) 0.0549(11) Uani 1 1 d . . . C84 C 0.2419(4) 0.2679(3) 1.03296(13) 0.0850(18) Uani 1 1 d . . . H84A H 0.2090 0.2314 1.0525 0.102 Uiso 1 1 calc R . . C85 C 0.3488(5) 0.2765(4) 1.03520(15) 0.093(2) Uani 1 1 d . F . C86 C 0.3923(4) 0.3316(4) 1.00668(16) 0.0865(19) Uani 1 1 d . . . H86A H 0.4660 0.3376 1.0083 0.104 Uiso 1 1 calc R . . C87 C 0.3382(3) 0.3789(3) 0.97597(12) 0.0595(12) Uani 1 1 d . . . C88 C 0.2265(3) 0.3683(2) 0.97370(11) 0.0478(10) Uani 1 1 d . . . C89 C 0.2213(2) 0.26083(17) 0.89106(9) 0.0273(7) Uani 1 1 d . . . H89A H 0.2847 0.2749 0.9015 0.033 Uiso 1 1 calc R . . C90 C 0.1141(2) 0.20416(17) 0.85948(9) 0.0261(6) Uani 1 1 d . . . C91 C 0.0567(2) 0.25738(17) 0.87840(9) 0.0264(6) Uani 1 1 d . . . C92 C -0.0562(2) 0.28255(19) 0.87829(10) 0.0327(7) Uani 1 1 d . . . C93 C 0.0843(2) 0.14973(18) 0.83416(9) 0.0304(7) Uani 1 1 d . . . C94 C 0.2789(3) -0.02956(19) 0.87788(10) 0.0340(7) Uani 1 1 d . . . C95 C 0.2267(3) -0.0717(2) 0.91101(10) 0.0425(9) Uani 1 1 d D . . C96 C 0.1947(4) -0.1444(3) 0.90693(12) 0.0665(13) Uani 1 1 d U . . H96A H 0.1638 -0.1748 0.9295 0.080 Uiso 1 1 calc R . . C97 C 0.2049(4) -0.1754(3) 0.87215(14) 0.094(2) Uani 1 1 d DU G . C98 C 0.2616(4) -0.1363(2) 0.84115(13) 0.0726(14) Uani 1 1 d U . . H98A H 0.2774 -0.1599 0.8181 0.087 Uiso 1 1 calc R . . C99 C 0.2969(3) -0.0625(2) 0.84277(10) 0.0412(8) Uani 1 1 d D . . C100 C 0.3417(3) -0.0219(2) 0.80662(10) 0.0385(8) Uani 1 1 d . . . H10C H 0.3571 -0.0519 0.7858 0.046 Uiso 1 1 calc R . . C101 C 0.3965(3) 0.0802(2) 0.75836(10) 0.0360(8) Uani 1 1 d . . . H10D H 0.4200 0.0363 0.7441 0.043 Uiso 1 1 calc R . . H10E H 0.4572 0.1127 0.7591 0.043 Uiso 1 1 calc R . . C102 C 0.3053(3) 0.1293(2) 0.73620(10) 0.0382(8) Uani 1 1 d . . . H10F H 0.2437 0.0970 0.7377 0.046 Uiso 1 1 calc R . . H10L H 0.3265 0.1419 0.7077 0.046 Uiso 1 1 calc R . . C103 C 0.2699(3) 0.2053(2) 0.75114(10) 0.0370(8) Uani 1 1 d . . . H10G H 0.2822 0.2501 0.7299 0.044 Uiso 1 1 calc R . . H10H H 0.1930 0.2065 0.7576 0.044 Uiso 1 1 calc R . . C104 C 0.3888(2) 0.27010(18) 0.78448(9) 0.0296(7) Uani 1 1 d . . . H10I H 0.3832 0.3075 0.7608 0.036 Uiso 1 1 calc R . . C105 C 0.4630(2) 0.28435(18) 0.81324(9) 0.0283(7) Uani 1 1 d . . . C106 C 0.5162(2) 0.35321(18) 0.80455(9) 0.0293(7) Uani 1 1 d . . . H10J H 0.4965 0.3900 0.7816 0.035 Uiso 1 1 calc R . . C107 C 0.5952(2) 0.36933(18) 0.82782(10) 0.0320(7) Uani 1 1 d . . . C108 C 0.6202(2) 0.31404(18) 0.86182(9) 0.0313(7) Uani 1 1 d . . . H10K H 0.6760 0.3240 0.8780 0.038 Uiso 1 1 calc R . . C109 C 0.5692(2) 0.24594(18) 0.87335(9) 0.0279(7) Uani 1 1 d . . . C110 C 0.4903(2) 0.22927(17) 0.84759(9) 0.0260(6) Uani 1 1 d . . . C111 C 0.1310(3) 0.4939(2) 0.78784(10) 0.0416(8) Uani 1 1 d . . . C112 C 0.1457(3) 0.5281(2) 0.74370(11) 0.0557(11) Uani 1 1 d . . . H11B H 0.0799 0.5255 0.7295 0.084 Uiso 1 1 calc R . . H11C H 0.2037 0.4979 0.7320 0.084 Uiso 1 1 calc R . . H11D H 0.1628 0.5827 0.7413 0.084 Uiso 1 1 calc R . . C113 C 0.2368(3) 0.4982(3) 0.80809(13) 0.0667(13) Uani 1 1 d . . . H11E H 0.2537 0.5529 0.8055 0.100 Uiso 1 1 calc R . . H11F H 0.2932 0.4684 0.7953 0.100 Uiso 1 1 calc R . . H11G H 0.2311 0.4759 0.8364 0.100 Uiso 1 1 calc R . . C114 C 0.1045(4) 0.4085(2) 0.79055(12) 0.0590(12) Uani 1 1 d . . . H11H H 0.0989 0.3846 0.8186 0.088 Uiso 1 1 calc R . . H11I H 0.1609 0.3796 0.7773 0.088 Uiso 1 1 calc R . . H11J H 0.0369 0.4066 0.7775 0.088 Uiso 1 1 calc R . . C115 C -0.1573(3) 0.7165(2) 0.77711(12) 0.0555(11) Uani 1 1 d . . . C116 C -0.2007(3) 0.6903(3) 0.74040(12) 0.0603(11) Uani 1 1 d . . . H11K H -0.2400 0.7347 0.7243 0.090 Uiso 1 1 calc R . . H11L H -0.2483 0.6485 0.7488 0.090 Uiso 1 1 calc R . . H11M H -0.1418 0.6707 0.7245 0.090 Uiso 1 1 calc R . . C117 C -0.2513(5) 0.7506(3) 0.79990(15) 0.106(2) Uani 1 1 d . . . H11N H -0.2954 0.7878 0.7813 0.159 Uiso 1 1 calc R . . H11O H -0.2248 0.7776 0.8204 0.159 Uiso 1 1 calc R . . H11P H -0.2937 0.7082 0.8126 0.159 Uiso 1 1 calc R . . C118 C -0.0806(4) 0.7797(2) 0.76327(14) 0.0759(15) Uani 1 1 d . . . H11Q H -0.0192 0.7570 0.7497 0.114 Uiso 1 1 calc R . . H11R H -0.0568 0.8004 0.7864 0.114 Uiso 1 1 calc R . . H11S H -0.1167 0.8221 0.7448 0.114 Uiso 1 1 calc R . . C119 C 0.4182(5) 0.2303(5) 1.06903(17) 0.137(3) Uani 1 1 d D . . C120 C 0.5390(6) 0.2363(6) 1.0571(3) 0.065(3) Uani 0.50 1 d PDU F 1 H12A H 0.5823 0.1984 1.0756 0.098 Uiso 0.50 1 calc PR F 1 H12B H 0.5590 0.2892 1.0582 0.098 Uiso 0.50 1 calc PR F 1 H12C H 0.5509 0.2248 1.0299 0.098 Uiso 0.50 1 calc PR F 1 C121 C 0.4086(12) 0.1435(6) 1.0657(4) 0.123(5) Uani 0.50 1 d PDU F 1 H12D H 0.4125 0.1369 1.0376 0.184 Uiso 0.50 1 calc PR F 1 H12E H 0.3406 0.1270 1.0774 0.184 Uiso 0.50 1 calc PR F 1 H12F H 0.4668 0.1113 1.0801 0.184 Uiso 0.50 1 calc PR F 1 C122 C 0.3895(15) 0.2477(12) 1.1089(3) 0.147(7) Uani 0.50 1 d PDU F 1 H12G H 0.4367 0.2158 1.1285 0.220 Uiso 0.50 1 calc PR F 1 H12H H 0.3159 0.2355 1.1153 0.220 Uiso 0.50 1 calc PR F 1 H12I H 0.3966 0.3032 1.1095 0.220 Uiso 0.50 1 calc PR F 1 C12A C 0.3510(8) 0.1762(7) 1.0989(3) 0.101(4) Uani 0.50 1 d PDU F 2 H12J H 0.3263 0.1349 1.0857 0.151 Uiso 0.50 1 calc PR F 2 H12K H 0.2897 0.2070 1.1082 0.151 Uiso 0.50 1 calc PR F 2 H12L H 0.3945 0.1525 1.1217 0.151 Uiso 0.50 1 calc PR F 2 C12B C 0.4370(8) 0.2896(6) 1.0989(3) 0.078(3) Uani 0.50 1 d PDU F 2 H12M H 0.4734 0.2613 1.1226 0.116 Uiso 0.50 1 calc PR F 2 H12N H 0.3685 0.3133 1.1069 0.116 Uiso 0.50 1 calc PR F 2 H12O H 0.4807 0.3307 1.0856 0.116 Uiso 0.50 1 calc PR F 2 C12C C 0.5069(12) 0.1795(10) 1.0565(4) 0.126(5) Uani 0.50 1 d PDU F 2 H12P H 0.5436 0.1511 1.0801 0.189 Uiso 0.50 1 calc PR F 2 H12Q H 0.5567 0.2115 1.0397 0.189 Uiso 0.50 1 calc PR F 2 H12R H 0.4798 0.1421 1.0413 0.189 Uiso 0.50 1 calc PR F 2 C123 C 0.3918(3) 0.4392(3) 0.94553(14) 0.0589(12) Uani 1 1 d . . . C124 C 0.5119(3) 0.4396(3) 0.95313(16) 0.0858(18) Uani 1 1 d . . . H12A H 0.5477 0.3890 0.9496 0.129 Uiso 1 1 calc R . . H12B H 0.5220 0.4489 0.9804 0.129 Uiso 1 1 calc R . . H12C H 0.5420 0.4813 0.9342 0.129 Uiso 1 1 calc R . . C125 C 0.3421(3) 0.5209(3) 0.94880(18) 0.0826(17) Uani 1 1 d . . . H12D H 0.3773 0.5597 0.9297 0.124 Uiso 1 1 calc R . . H12E H 0.3507 0.5316 0.9759 0.124 Uiso 1 1 calc R . . H12F H 0.2664 0.5238 0.9428 0.124 Uiso 1 1 calc R . . C126 C 0.3813(3) 0.4220(2) 0.90349(12) 0.0498(10) Uani 1 1 d . . . H12G H 0.4171 0.3706 0.9014 0.075 Uiso 1 1 calc R . . H12H H 0.4139 0.4623 0.8845 0.075 Uiso 1 1 calc R . . H12I H 0.3060 0.4219 0.8974 0.075 Uiso 1 1 calc R . . C127 C 0.2020(3) -0.0371(2) 0.94902(11) 0.0456(9) Uani 1 1 d . . . C128 C 0.1407(4) -0.0913(3) 0.98040(12) 0.0665(13) Uani 1 1 d . . . H12J H 0.0732 -0.1011 0.9694 0.100 Uiso 1 1 calc R . . H12K H 0.1270 -0.0664 1.0041 0.100 Uiso 1 1 calc R . . H12L H 0.1830 -0.1411 0.9877 0.100 Uiso 1 1 calc R . . C129 C 0.1329(4) 0.0404(3) 0.93978(14) 0.0714(14) Uani 1 1 d . . . H12M H 0.1728 0.0790 0.9223 0.107 Uiso 1 1 calc R . . H12N H 0.1136 0.0600 0.9647 0.107 Uiso 1 1 calc R . . H12O H 0.0684 0.0315 0.9264 0.107 Uiso 1 1 calc R . . C130 C 0.3059(3) -0.0218(2) 0.96783(11) 0.0542(10) Uani 1 1 d . . . H13B H 0.3472 -0.0716 0.9762 0.081 Uiso 1 1 calc R . . H13C H 0.2895 0.0042 0.9911 0.081 Uiso 1 1 calc R . . H13D H 0.3472 0.0119 0.9482 0.081 Uiso 1 1 calc R . . C131 C 0.1619(7) -0.2542(3) 0.86990(16) 0.214(6) Uani 1 1 d DU . . C132 C 0.1588(5) -0.2741(3) 0.82966(15) 0.080(2) Uani 0.879(9) 1 d PD G 1 H13E H 0.2311 -0.2871 0.8204 0.120 Uiso 0.879(9) 1 calc PR G 1 H13F H 0.1267 -0.2293 0.8115 0.120 Uiso 0.879(9) 1 calc PR G 1 H13G H 0.1164 -0.3192 0.8302 0.120 Uiso 0.879(9) 1 calc PR G 1 C133 C 0.0359(8) -0.2408(6) 0.8787(3) 0.242(9) Uani 0.879(9) 1 d PD G 1 H13H H -0.0015 -0.2802 0.8681 0.364 Uiso 0.879(9) 1 calc PR G 1 H13I H 0.0100 -0.1884 0.8658 0.364 Uiso 0.879(9) 1 calc PR G 1 H13J H 0.0228 -0.2456 0.9075 0.364 Uiso 0.879(9) 1 calc PR G 1 C134 C 0.1825(7) -0.3158(3) 0.90325(18) 0.107(3) Uani 0.879(9) 1 d PD G 1 H13K H 0.1488 -0.3626 0.8989 0.160 Uiso 0.879(9) 1 calc PR G 1 H13L H 0.1534 -0.2987 0.9277 0.160 Uiso 0.879(9) 1 calc PR G 1 H13M H 0.2592 -0.3280 0.9058 0.160 Uiso 0.879(9) 1 calc PR G 1 C135 C 0.6570(3) 0.44317(19) 0.81718(11) 0.0409(8) Uani 1 1 d . . . C136 C 0.7673(3) 0.4210(2) 0.80233(14) 0.0607(12) Uani 1 1 d . . . H13N H 0.8036 0.3825 0.8228 0.091 Uiso 1 1 calc R . . H13O H 0.8074 0.4677 0.7967 0.091 Uiso 1 1 calc R . . H13P H 0.7624 0.3983 0.7779 0.091 Uiso 1 1 calc R . . C137 C 0.6013(3) 0.5021(2) 0.78471(16) 0.0702(14) Uani 1 1 d . . . H13Q H 0.6407 0.5492 0.7792 0.105 Uiso 1 1 calc R . . H13R H 0.5290 0.5160 0.7937 0.105 Uiso 1 1 calc R . . H13S H 0.5985 0.4788 0.7604 0.105 Uiso 1 1 calc R . . C138 C 0.6653(4) 0.4827(3) 0.85374(15) 0.0756(14) Uani 1 1 d . . . H13T H 0.7081 0.4482 0.8739 0.113 Uiso 1 1 calc R . . H13U H 0.5941 0.4933 0.8648 0.113 Uiso 1 1 calc R . . H13V H 0.6990 0.5320 0.8461 0.113 Uiso 1 1 calc R . . C139 C 0.5929(2) 0.19064(19) 0.91292(9) 0.0321(7) Uani 1 1 d . . . C140 C 0.6370(3) 0.1092(2) 0.90574(10) 0.0397(8) Uani 1 1 d . . . H14A H 0.5867 0.0874 0.8899 0.060 Uiso 1 1 calc R . . H14B H 0.6472 0.0749 0.9314 0.060 Uiso 1 1 calc R . . H14C H 0.7051 0.1133 0.8913 0.060 Uiso 1 1 calc R . . C141 C 0.6749(3) 0.2224(2) 0.93720(10) 0.0429(9) Uani 1 1 d . . . H14D H 0.7419 0.2265 0.9220 0.064 Uiso 1 1 calc R . . H14E H 0.6867 0.1867 0.9624 0.064 Uiso 1 1 calc R . . H14F H 0.6487 0.2742 0.9428 0.064 Uiso 1 1 calc R . . C142 C 0.4907(2) 0.1825(2) 0.93854(9) 0.0337(7) Uani 1 1 d . . . H14G H 0.4617 0.2343 0.9431 0.051 Uiso 1 1 calc R . . H14H H 0.5068 0.1495 0.9642 0.051 Uiso 1 1 calc R . . H14I H 0.4385 0.1584 0.9246 0.051 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0289(2) 0.0339(3) 0.0282(2) -0.01005(19) 0.00291(18) -0.00966(19) Fe2 0.0301(2) 0.0273(2) 0.0235(2) -0.00306(18) -0.00289(18) 0.00095(18) Fe3 0.0273(2) 0.0296(2) 0.0279(2) -0.00707(19) -0.00037(18) 0.00300(18) Fe4 0.0251(2) 0.0245(2) 0.0268(2) -0.00526(18) -0.00137(17) -0.00103(17) N1 0.0251(13) 0.0342(15) 0.0283(14) -0.0092(11) 0.0025(11) -0.0035(11) N2 0.0302(14) 0.0323(15) 0.0306(14) -0.0056(12) -0.0054(11) 0.0019(11) N3 0.0278(14) 0.0360(15) 0.0295(14) -0.0065(12) -0.0041(11) -0.0081(11) N4 0.0248(13) 0.0350(15) 0.0263(14) -0.0063(11) -0.0029(10) -0.0024(11) N5 0.068(2) 0.0342(16) 0.0243(15) -0.0026(12) -0.0052(14) -0.0033(15) N6 0.0277(14) 0.0335(15) 0.0271(14) -0.0086(11) -0.0025(11) -0.0037(11) N7 0.0296(14) 0.0282(14) 0.0314(14) -0.0088(12) 0.0036(11) -0.0004(11) N8 0.0477(18) 0.0357(16) 0.0326(16) -0.0038(13) 0.0053(13) 0.0060(13) N9 0.0267(13) 0.0267(13) 0.0275(14) -0.0053(11) -0.0030(10) 0.0013(11) N10 0.0253(13) 0.0234(13) 0.0286(14) -0.0043(10) -0.0022(10) -0.0025(10) N11 0.0288(14) 0.0314(15) 0.0334(15) -0.0071(12) -0.0022(11) -0.0013(11) N12 0.0287(14) 0.0336(15) 0.0276(14) -0.0040(11) -0.0035(11) -0.0003(12) O1 0.0432(14) 0.0460(14) 0.0484(15) -0.0270(12) 0.0214(11) -0.0221(11) O2 0.0296(11) 0.0287(11) 0.0295(11) -0.0072(9) 0.0012(9) -0.0056(9) O3 0.0351(13) 0.0617(16) 0.0319(13) -0.0053(12) -0.0030(10) -0.0164(12) O4 0.0320(13) 0.087(2) 0.0355(14) -0.0004(13) -0.0058(11) -0.0140(13) O5 0.0315(13) 0.088(2) 0.0360(14) 0.0033(13) -0.0091(11) -0.0049(13) O6 0.0420(13) 0.0279(12) 0.0337(12) -0.0066(10) -0.0036(10) 0.0051(10) O7 0.0269(11) 0.0239(11) 0.0266(11) -0.0052(9) -0.0015(9) -0.0027(8) O8 0.0321(12) 0.0498(15) 0.0285(12) 0.0008(11) -0.0042(10) 0.0015(11) O9 0.0316(12) 0.0339(12) 0.0301(12) -0.0044(10) 0.0033(9) 0.0054(10) O10 0.0323(12) 0.0441(14) 0.0384(13) -0.0197(11) -0.0055(10) 0.0059(10) O11 0.0270(11) 0.0397(13) 0.0396(13) -0.0119(11) 0.0004(10) 0.0036(10) O12 0.0246(12) 0.0465(14) 0.0562(15) -0.0205(12) -0.0042(11) -0.0017(10) O13 0.0270(12) 0.0456(14) 0.0544(15) -0.0204(12) -0.0096(11) -0.0023(10) O14 0.0347(12) 0.0268(12) 0.0312(12) -0.0024(9) -0.0027(9) -0.0048(9) O15 0.0256(11) 0.0273(11) 0.0290(11) -0.0023(9) -0.0016(9) -0.0019(9) O16 0.0315(12) 0.0324(12) 0.0377(13) -0.0119(10) -0.0050(10) -0.0006(10) C1 0.0334(18) 0.0333(18) 0.0392(19) -0.0119(15) 0.0063(14) -0.0110(14) C2 0.047(2) 0.044(2) 0.054(2) -0.0246(18) 0.0208(18) -0.0197(17) C3 0.0410(19) 0.0355(19) 0.040(2) -0.0157(15) 0.0080(15) -0.0060(15) C4 0.0306(17) 0.0266(17) 0.0353(18) -0.0032(14) -0.0007(14) -0.0040(13) C5 0.0280(16) 0.0311(17) 0.0320(17) -0.0027(14) 0.0033(13) -0.0043(13) C6 0.0276(16) 0.0275(16) 0.0291(16) -0.0051(13) 0.0003(13) -0.0027(13) C7 0.0276(16) 0.0332(18) 0.0295(17) -0.0033(14) 0.0011(13) -0.0035(13) C8 0.0344(18) 0.045(2) 0.0337(18) -0.0154(15) 0.0107(14) -0.0099(15) C9 0.0301(19) 0.053(2) 0.067(3) -0.023(2) 0.0096(18) -0.0018(17) C10 0.0291(18) 0.048(2) 0.047(2) -0.0135(17) -0.0042(15) 0.0077(15) C11 0.0405(19) 0.0310(18) 0.0329(18) -0.0113(14) -0.0010(14) 0.0006(14) C12 0.0362(18) 0.0304(17) 0.0298(17) -0.0079(14) -0.0032(14) -0.0046(14) C13 0.051(2) 0.039(2) 0.0364(19) -0.0146(16) 0.0009(16) -0.0097(16) C14 0.049(2) 0.047(2) 0.0309(18) -0.0093(16) -0.0016(16) -0.0193(17) C15 0.0327(18) 0.055(2) 0.0326(18) 0.0011(16) -0.0046(14) -0.0163(16) C16 0.0319(17) 0.0409(19) 0.0237(16) -0.0006(14) 0.0013(13) -0.0080(14) C17 0.0338(17) 0.0314(17) 0.0216(15) -0.0033(13) 0.0003(13) -0.0073(14) C18 0.0268(16) 0.0307(17) 0.0274(16) -0.0056(13) -0.0054(13) -0.0044(13) C19 0.0272(16) 0.0415(19) 0.0283(17) -0.0066(14) -0.0038(13) -0.0007(14) C20 0.0271(16) 0.048(2) 0.0295(17) -0.0066(15) -0.0036(13) -0.0065(15) C21 0.0326(18) 0.059(2) 0.0302(18) -0.0083(17) -0.0045(15) -0.0084(16) C22 0.0316(18) 0.053(2) 0.0289(18) -0.0062(16) -0.0038(14) 0.0031(16) C23 0.0348(18) 0.0314(18) 0.0379(19) -0.0052(14) -0.0128(15) 0.0111(14) C24 0.039(2) 0.0352(19) 0.049(2) -0.0135(16) -0.0142(16) 0.0118(16) C25 0.046(2) 0.048(2) 0.072(3) -0.028(2) -0.020(2) 0.0103(19) C26 0.042(2) 0.045(2) 0.082(3) -0.016(2) -0.014(2) -0.0047(18) C27 0.0351(19) 0.044(2) 0.060(2) -0.0071(19) -0.0063(17) 0.0046(16) C28 0.0340(18) 0.0280(17) 0.0409(19) -0.0037(14) -0.0082(15) 0.0059(14) C29 0.053(2) 0.0309(19) 0.0328(19) 0.0015(15) 0.0008(16) 0.0020(16) C30 0.073(3) 0.069(3) 0.040(2) -0.001(2) -0.006(2) 0.000(2) C31 0.108(4) 0.060(3) 0.036(2) -0.005(2) -0.018(2) -0.030(3) C32 0.0360(18) 0.042(2) 0.0316(18) -0.0118(15) -0.0092(14) -0.0046(15) C33 0.0278(16) 0.0305(17) 0.0305(17) -0.0108(13) 0.0035(13) -0.0077(13) C34 0.0218(14) 0.0264(16) 0.0265(16) -0.0042(12) 0.0013(12) -0.0044(12) C35 0.0306(16) 0.0248(16) 0.0318(17) -0.0065(13) 0.0064(13) -0.0051(13) C36 0.0271(16) 0.0262(16) 0.0286(16) -0.0003(13) 0.0062(13) -0.0006(13) C37 0.0237(15) 0.0364(18) 0.0226(15) -0.0031(13) -0.0007(12) -0.0005(13) C38 0.0229(15) 0.0295(16) 0.0237(15) -0.0052(12) 0.0045(12) -0.0031(12) C39 0.0235(15) 0.0253(16) 0.0239(15) -0.0032(12) 0.0036(12) -0.0033(12) C40 0.086(3) 0.093(4) 0.102(4) -0.074(3) 0.069(3) -0.062(3) C41 0.122(5) 0.119(5) 0.129(5) -0.096(4) 0.102(4) -0.083(4) C42 0.248(9) 0.087(4) 0.109(5) -0.064(4) 0.133(6) -0.111(5) C43 0.064(3) 0.197(7) 0.213(8) -0.171(7) 0.081(4) -0.075(4) C44 0.045(2) 0.0301(18) 0.0396(19) -0.0078(15) 0.0031(16) -0.0094(15) C45 0.151(5) 0.110(4) 0.045(3) -0.031(3) 0.021(3) -0.093(4) C46 0.061(3) 0.031(2) 0.102(4) -0.003(2) 0.009(3) -0.0020(19) C47 0.045(2) 0.042(2) 0.066(3) -0.0150(19) 0.0002(19) -0.0119(17) C48 0.060(3) 0.070(3) 0.038(2) -0.011(2) -0.0049(18) -0.030(2) C49 0.085(4) 0.085(4) 0.148(6) -0.035(4) -0.062(4) -0.019(3) C50 0.101(4) 0.060(3) 0.079(3) -0.020(3) -0.012(3) -0.036(3) C51 0.107(4) 0.095(4) 0.065(3) -0.039(3) 0.007(3) -0.052(3) C52 0.0265(17) 0.045(2) 0.041(2) 0.0017(16) 0.0026(14) -0.0013(15) C53 0.040(2) 0.047(2) 0.057(2) 0.0111(19) 0.0093(18) 0.0063(17) C54 0.0286(19) 0.068(3) 0.063(3) 0.002(2) -0.0003(18) -0.0010(18) C55 0.0365(19) 0.041(2) 0.047(2) -0.0065(16) 0.0115(16) -0.0029(15) C56 0.055(2) 0.043(2) 0.042(2) -0.0186(17) -0.0123(18) 0.0159(18) C57 0.052(2) 0.049(2) 0.046(2) -0.0171(18) 0.0001(18) 0.0127(18) C58 0.068(3) 0.067(3) 0.069(3) -0.039(2) -0.019(2) 0.020(2) C59 0.095(4) 0.060(3) 0.039(2) -0.010(2) -0.008(2) 0.027(2) C60 0.065(3) 0.068(3) 0.111(4) -0.025(3) -0.014(3) -0.024(3) C61A 0.088(10) 0.105(11) 0.168(16) -0.078(12) 0.004(10) -0.042(9) C62A 0.041(5) 0.119(9) 0.096(9) -0.050(7) -0.009(5) -0.017(5) C63A 0.048(7) 0.060(8) 0.28(2) -0.005(10) -0.011(10) -0.036(6) C61B 0.146(15) 0.22(2) 0.098(11) -0.055(12) 0.046(10) -0.146(16) C62B 0.121(12) 0.064(8) 0.116(11) -0.016(7) 0.007(9) -0.043(7) C63B 0.096(10) 0.188(17) 0.133(13) 0.015(12) -0.055(10) -0.087(11) C64 0.0348(18) 0.0299(17) 0.0325(18) -0.0029(14) 0.0069(14) 0.0043(14) C65 0.071(3) 0.051(2) 0.042(2) 0.0123(18) 0.018(2) 0.030(2) C66 0.042(2) 0.0278(19) 0.081(3) -0.0054(19) 0.001(2) 0.0042(16) C67 0.0329(18) 0.038(2) 0.049(2) -0.0067(16) 0.0055(16) 0.0064(15) C68 0.0272(16) 0.0314(17) 0.0289(16) -0.0091(13) -0.0038(13) -0.0010(13) C69 0.0398(19) 0.0333(18) 0.0381(19) -0.0118(15) 0.0013(15) -0.0102(15) C70 0.0331(18) 0.049(2) 0.040(2) -0.0178(16) -0.0092(15) -0.0013(15) C71 0.0328(17) 0.0400(19) 0.0300(17) -0.0132(14) 0.0036(14) -0.0025(14) C72 0.0299(16) 0.0237(16) 0.0333(17) -0.0056(13) 0.0007(13) -0.0060(13) C73 0.0334(17) 0.0297(17) 0.0331(18) -0.0068(14) 0.0052(14) -0.0046(14) C74 0.045(2) 0.0307(18) 0.0334(18) -0.0021(14) 0.0060(15) -0.0059(15) C75 0.049(2) 0.0300(18) 0.041(2) -0.0009(15) 0.0064(16) 0.0041(15) C76 0.0378(19) 0.0302(18) 0.042(2) -0.0031(15) 0.0056(15) 0.0050(14) C77 0.0302(16) 0.0250(16) 0.0335(17) -0.0064(13) 0.0043(13) -0.0023(13) C78 0.0265(16) 0.0278(17) 0.0367(18) -0.0116(14) 0.0034(13) 0.0010(13) C79 0.0404(19) 0.0367(19) 0.0293(17) -0.0091(14) 0.0077(14) 0.0018(15) C80 0.0392(19) 0.043(2) 0.0354(19) -0.0014(15) 0.0113(15) -0.0012(16) C81 0.052(2) 0.041(2) 0.039(2) 0.0007(16) 0.0122(17) -0.0016(17) C82 0.064(3) 0.054(2) 0.031(2) -0.0015(17) 0.0037(18) 0.017(2) C83 0.058(3) 0.070(3) 0.032(2) -0.0132(19) -0.0052(18) 0.032(2) C84 0.089(4) 0.116(4) 0.038(2) -0.008(3) -0.007(2) 0.056(3) C85 0.079(4) 0.146(5) 0.047(3) -0.023(3) -0.026(3) 0.061(4) C86 0.057(3) 0.147(5) 0.062(3) -0.058(4) -0.024(3) 0.044(3) C87 0.047(2) 0.090(3) 0.047(2) -0.043(2) -0.0180(19) 0.031(2) C88 0.043(2) 0.066(3) 0.038(2) -0.0296(19) -0.0093(17) 0.0210(19) C89 0.0230(15) 0.0283(16) 0.0316(17) -0.0077(13) -0.0036(12) -0.0006(12) C90 0.0231(15) 0.0256(16) 0.0291(16) -0.0021(13) -0.0034(12) -0.0020(12) C91 0.0244(15) 0.0275(16) 0.0274(16) -0.0041(13) -0.0024(12) -0.0024(12) C92 0.0267(16) 0.0349(18) 0.0361(18) -0.0051(15) 0.0009(14) -0.0027(14) C93 0.0286(17) 0.0298(17) 0.0341(18) -0.0080(14) -0.0038(13) -0.0031(13) C94 0.0348(18) 0.0300(18) 0.0361(19) 0.0008(14) -0.0114(14) -0.0042(14) C95 0.044(2) 0.045(2) 0.037(2) 0.0044(16) -0.0105(16) -0.0125(17) C96 0.097(3) 0.065(3) 0.039(2) 0.0095(19) -0.012(2) -0.049(3) C97 0.178(6) 0.062(3) 0.050(3) -0.006(2) -0.005(3) -0.076(4) C98 0.132(4) 0.049(3) 0.043(2) -0.011(2) -0.003(3) -0.040(3) C99 0.057(2) 0.0295(18) 0.039(2) -0.0040(15) -0.0094(17) -0.0124(16) C100 0.045(2) 0.038(2) 0.0351(19) -0.0122(15) -0.0050(15) -0.0007(16) C101 0.0360(18) 0.0405(19) 0.0334(18) -0.0118(15) 0.0069(14) -0.0049(15) C102 0.044(2) 0.044(2) 0.0283(18) -0.0076(15) 0.0009(15) -0.0079(16) C103 0.0357(18) 0.046(2) 0.0288(17) -0.0032(15) -0.0077(14) -0.0033(15) C104 0.0278(16) 0.0325(17) 0.0256(16) 0.0017(13) 0.0026(13) 0.0015(13) C105 0.0255(15) 0.0317(17) 0.0269(16) -0.0038(13) 0.0015(12) 0.0003(13) C106 0.0268(16) 0.0280(17) 0.0313(17) -0.0006(13) 0.0035(13) -0.0007(13) C107 0.0242(16) 0.0295(17) 0.0413(19) -0.0046(14) 0.0055(14) -0.0007(13) C108 0.0230(15) 0.0364(18) 0.0351(18) -0.0073(14) 0.0010(13) -0.0030(13) C109 0.0211(15) 0.0329(17) 0.0287(16) -0.0032(13) 0.0035(12) -0.0011(13) C110 0.0227(15) 0.0292(16) 0.0264(16) -0.0055(13) 0.0037(12) -0.0025(12) C111 0.046(2) 0.045(2) 0.0323(19) -0.0070(16) 0.0114(16) 0.0064(16) C112 0.068(3) 0.054(2) 0.040(2) -0.0018(18) 0.019(2) 0.010(2) C113 0.042(2) 0.103(4) 0.050(3) -0.008(2) 0.0148(19) 0.010(2) C114 0.091(3) 0.038(2) 0.044(2) -0.0096(18) 0.012(2) 0.016(2) C115 0.074(3) 0.039(2) 0.044(2) 0.0079(17) 0.009(2) 0.019(2) C116 0.063(3) 0.057(3) 0.053(3) 0.009(2) -0.005(2) 0.007(2) C117 0.146(5) 0.087(4) 0.058(3) 0.019(3) 0.019(3) 0.083(4) C118 0.128(5) 0.032(2) 0.063(3) 0.005(2) -0.017(3) -0.003(3) C119 0.111(5) 0.219(9) 0.062(4) -0.015(5) -0.034(4) 0.093(6) C120 0.075(6) 0.074(6) 0.043(4) -0.019(4) -0.025(4) 0.043(5) C121 0.109(8) 0.139(8) 0.097(7) 0.051(7) -0.021(6) 0.004(7) C122 0.155(10) 0.173(10) 0.106(9) -0.014(8) -0.013(8) 0.013(8) C12A 0.101(7) 0.122(8) 0.064(6) 0.012(6) -0.039(5) 0.044(6) C12B 0.065(6) 0.133(8) 0.029(4) -0.002(5) -0.008(4) 0.006(5) C12C 0.111(8) 0.149(9) 0.101(8) -0.002(7) -0.010(7) 0.058(7) C123 0.032(2) 0.082(3) 0.074(3) -0.049(3) -0.0079(19) 0.006(2) C124 0.031(2) 0.139(5) 0.108(4) -0.087(4) -0.017(2) 0.014(3) C125 0.038(2) 0.087(4) 0.142(5) -0.079(4) -0.005(3) 0.001(2) C126 0.035(2) 0.059(3) 0.061(3) -0.025(2) -0.0028(18) -0.0042(18) C127 0.050(2) 0.045(2) 0.036(2) 0.0125(16) 0.0008(17) -0.0046(17) C128 0.079(3) 0.069(3) 0.044(2) 0.017(2) 0.004(2) -0.014(2) C129 0.072(3) 0.071(3) 0.058(3) 0.017(2) 0.024(2) 0.013(2) C130 0.078(3) 0.051(2) 0.034(2) -0.0024(18) -0.0081(19) -0.016(2) C131 0.475(18) 0.140(6) 0.056(4) -0.009(4) 0.009(7) -0.232(10) C132 0.130(5) 0.047(3) 0.074(4) -0.028(3) 0.001(3) -0.045(3) C133 0.386(19) 0.273(14) 0.125(8) -0.091(9) 0.090(10) -0.295(15) C134 0.209(9) 0.025(3) 0.088(5) -0.002(3) -0.032(5) -0.024(4) C135 0.0338(18) 0.0300(18) 0.057(2) 0.0027(16) -0.0006(16) -0.0089(14) C136 0.038(2) 0.051(2) 0.088(3) 0.006(2) 0.013(2) -0.0159(18) C137 0.049(2) 0.041(2) 0.113(4) 0.021(2) -0.019(2) -0.0182(19) C138 0.090(4) 0.059(3) 0.085(4) -0.019(3) 0.007(3) -0.043(3) C139 0.0259(16) 0.0395(19) 0.0298(17) -0.0015(14) -0.0031(13) -0.0037(14) C140 0.0354(19) 0.041(2) 0.038(2) 0.0026(16) -0.0033(15) 0.0061(15) C141 0.0347(19) 0.053(2) 0.039(2) 0.0019(17) -0.0107(15) -0.0101(16) C142 0.0315(17) 0.0426(19) 0.0271(17) -0.0043(14) -0.0013(13) -0.0049(14) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Fe1 O2 96.10(10) . . ? O1 Fe1 N1 86.78(10) . . ? O2 Fe1 N1 105.37(9) . . ? O1 Fe1 N2 170.99(10) . . ? O2 Fe1 N2 86.05(9) . . ? N1 Fe1 N2 84.21(10) . . ? O1 Fe1 N3 93.91(10) . . ? O2 Fe1 N3 91.71(9) . . ? N1 Fe1 N3 162.74(10) . . ? N2 Fe1 N3 94.78(10) . . ? O1 Fe1 O3 94.10(11) . . ? O2 Fe1 O3 165.81(9) . . ? N1 Fe1 O3 85.00(9) . . ? N2 Fe1 O3 85.40(10) . . ? N3 Fe1 O3 77.75(9) . . ? O6 Fe2 O7 93.75(9) . . ? O6 Fe2 N5 85.28(10) . . ? O7 Fe2 N5 103.32(11) . . ? O6 Fe2 N6 168.89(10) . . ? O7 Fe2 N6 86.43(9) . . ? N5 Fe2 N6 83.88(11) . . ? O6 Fe2 N4 97.62(10) . . ? O7 Fe2 N4 92.72(9) . . ? N5 Fe2 N4 163.51(11) . . ? N6 Fe2 N4 93.46(10) . . ? O6 Fe2 O8 93.99(10) . . ? O7 Fe2 O8 168.37(9) . . ? N5 Fe2 O8 85.97(11) . . ? N6 Fe2 O8 87.64(9) . . ? N4 Fe2 O8 77.65(9) . . ? O9 Fe3 O10 96.90(10) . . ? O9 Fe3 N7 86.63(9) . . ? O10 Fe3 N7 104.76(10) . . ? O9 Fe3 N9 92.41(9) . . ? O10 Fe3 N9 92.37(9) . . ? N7 Fe3 N9 162.85(10) . . ? O9 Fe3 N8 171.50(10) . . ? O10 Fe3 N8 85.98(11) . . ? N7 Fe3 N8 84.90(10) . . ? N9 Fe3 N8 95.46(10) . . ? O9 Fe3 O11 93.37(9) . . ? O10 Fe3 O11 165.87(9) . . ? N7 Fe3 O11 85.47(9) . . ? N9 Fe3 O11 77.49(9) . . ? N8 Fe3 O11 85.24(10) . . ? O15 Fe4 O14 96.80(9) . . ? O15 Fe4 N11 106.06(9) . . ? O14 Fe4 N11 87.93(10) . . ? O15 Fe4 N10 94.62(9) . . ? O14 Fe4 N10 96.81(9) . . ? N11 Fe4 N10 158.12(10) . . ? O15 Fe4 N12 87.34(9) . . ? O14 Fe4 N12 170.76(10) . . ? N11 Fe4 N12 82.98(10) . . ? N10 Fe4 N12 91.07(10) . . ? O15 Fe4 O16 169.86(8) . . ? O14 Fe4 O16 89.38(9) . . ? N11 Fe4 O16 82.11(9) . . ? N10 Fe4 O16 76.62(9) . . ? N12 Fe4 O16 87.74(9) . . ? C7 N1 C8 117.3(3) . . ? C7 N1 Fe1 123.1(2) . . ? C8 N1 Fe1 119.0(2) . . ? C11 N2 C10 117.9(3) . . ? C11 N2 Fe1 121.2(2) . . ? C10 N2 Fe1 120.8(2) . . ? C18 N3 C20 104.6(3) . . ? C18 N3 Fe1 144.3(2) . . ? C20 N3 Fe1 110.53(19) . . ? C18 N4 C19 104.3(2) . . ? C18 N4 Fe2 144.4(2) . . ? C19 N4 Fe2 110.99(19) . . ? C29 N5 C30 119.8(3) . . ? C29 N5 Fe2 119.5(2) . . ? C30 N5 Fe2 120.5(2) . . ? C33 N6 C32 117.0(3) . . ? C33 N6 Fe2 123.2(2) . . ? C32 N6 Fe2 119.7(2) . . ? C78 N7 C79 117.2(3) . . ? C78 N7 Fe3 124.1(2) . . ? C79 N7 Fe3 118.1(2) . . ? C82 N8 C81 118.1(3) . . ? C82 N8 Fe3 122.1(3) . . ? C81 N8 Fe3 119.8(2) . . ? C89 N9 C91 104.8(2) . . ? C89 N9 Fe3 142.6(2) . . ? C91 N9 Fe3 111.16(19) . . ? C89 N10 C90 104.7(2) . . ? C89 N10 Fe4 142.5(2) . . ? C90 N10 Fe4 112.80(19) . . ? C100 N11 C101 117.5(3) . . ? C100 N11 Fe4 121.5(2) . . ? C101 N11 Fe4 119.5(2) . . ? C104 N12 C103 117.4(3) . . ? C104 N12 Fe4 122.7(2) . . ? C103 N12 Fe4 119.9(2) . . ? C1 O1 Fe1 133.9(2) . . ? C17 O2 Fe1 129.73(19) . . ? C21 O3 Fe1 115.8(2) . . ? C23 O6 Fe2 127.4(2) . . ? C39 O7 Fe2 133.36(18) . . ? C22 O8 Fe2 115.2(2) . . ? C72 O9 Fe3 135.43(19) . . ? C88 O10 Fe3 130.8(3) . . ? C92 O11 Fe3 115.35(19) . . ? C94 O14 Fe4 129.3(2) . . ? C110 O15 Fe4 133.22(19) . . ? C93 O16 Fe4 114.30(19) . . ? O1 C1 C6 120.3(3) . . ? O1 C1 C2 121.4(3) . . ? C6 C1 C2 118.3(3) . . ? C3 C2 C1 118.0(3) . . ? C3 C2 C40 122.3(3) . . ? C1 C2 C40 119.7(3) . . ? C2 C3 C4 124.9(3) . . ? C5 C4 C3 116.6(3) . . ? C5 C4 C44 122.4(3) . . ? C3 C4 C44 120.8(3) . . ? C4 C5 C6 122.0(3) . . ? C5 C6 C1 120.2(3) . . ? C5 C6 C7 117.3(3) . . ? C1 C6 C7 122.5(3) . . ? N1 C7 C6 127.7(3) . . ? N1 C8 C9 110.9(3) . . ? C8 C9 C10 116.0(3) . . ? N2 C10 C9 112.1(3) . . ? N2 C11 C12 127.4(3) . . ? C13 C12 C17 120.1(3) . . ? C13 C12 C11 116.6(3) . . ? C17 C12 C11 122.7(3) . . ? C14 C13 C12 121.9(3) . . ? C13 C14 C15 117.2(3) . . ? C13 C14 C48 119.3(3) . . ? C15 C14 C48 123.5(3) . . ? C14 C15 C16 124.8(3) . . ? C15 C16 C17 117.0(3) . . ? C15 C16 C52 122.4(3) . . ? C17 C16 C52 120.6(3) . . ? O2 C17 C12 120.7(3) . . ? O2 C17 C16 120.4(3) . . ? C12 C17 C16 118.8(3) . . ? N3 C18 N4 113.6(3) . . ? C20 C19 N4 108.7(3) . . ? C20 C19 C22 132.7(3) . . ? N4 C19 C22 118.6(3) . . ? N3 C20 C19 108.7(3) . . ? N3 C20 C21 119.4(3) . . ? C19 C20 C21 131.8(3) . . ? O3 C21 O4 125.1(3) . . ? O3 C21 C20 116.3(3) . . ? O4 C21 C20 118.7(3) . . ? O8 C22 O5 123.5(3) . . ? O8 C22 C19 117.3(3) . . ? O5 C22 C19 119.2(3) . . ? O6 C23 C24 120.4(3) . . ? O6 C23 C28 120.3(3) . . ? C24 C23 C28 119.3(3) . . ? C25 C24 C23 117.1(3) . . ? C25 C24 C56 122.4(3) . . ? C23 C24 C56 120.5(3) . . ? C24 C25 C26 125.2(4) . . ? C27 C26 C25 116.2(4) . . ? C27 C26 C60 122.3(4) . . ? C25 C26 C60 121.5(4) . . ? C26 C27 C28 122.4(4) . . ? C27 C28 C23 119.3(3) . . ? C27 C28 C29 118.7(3) . . ? C23 C28 C29 121.4(3) . . ? N5 C29 C28 126.7(3) . . ? C31 C30 N5 114.4(3) . . ? C30 C31 C32 120.8(4) . . ? N6 C32 C31 108.6(3) . . ? N6 C33 C34 127.5(3) . . ? C35 C34 C39 120.0(3) . . ? C35 C34 C33 116.8(3) . . ? C39 C34 C33 122.9(3) . . ? C36 C35 C34 122.1(3) . . ? C35 C36 C37 116.4(3) . . ? C35 C36 C64 123.4(3) . . ? C37 C36 C64 120.2(3) . . ? C38 C37 C36 124.9(3) . . ? C37 C38 C39 117.5(3) . . ? C37 C38 C68 122.0(3) . . ? C39 C38 C68 120.4(3) . . ? O7 C39 C34 120.5(3) . . ? O7 C39 C38 120.4(3) . . ? C34 C39 C38 119.0(3) . . ? C43 C40 C42 111.0(5) . . ? C43 C40 C41 108.1(4) . . ? C42 C40 C41 107.6(4) . . ? C43 C40 C2 109.3(4) . . ? C42 C40 C2 109.9(4) . . ? C41 C40 C2 111.0(3) . . ? C45 C44 C46 110.6(4) . . ? C45 C44 C4 112.0(3) . . ? C46 C44 C4 106.9(3) . . ? C45 C44 C47 108.1(4) . . ? C46 C44 C47 107.5(3) . . ? C4 C44 C47 111.6(3) . . ? C49 C48 C50 110.3(4) . . ? C49 C48 C51 110.1(4) . . ? C50 C48 C51 107.2(4) . . ? C49 C48 C14 111.1(4) . . ? C50 C48 C14 109.2(3) . . ? C51 C48 C14 108.9(3) . . ? C16 C52 C55 110.8(3) . . ? C16 C52 C53 109.7(3) . . ? C55 C52 C53 109.3(3) . . ? C16 C52 C54 111.6(3) . . ? C55 C52 C54 107.9(3) . . ? C53 C52 C54 107.4(3) . . ? C57 C56 C59 109.7(4) . . ? C57 C56 C24 108.9(3) . . ? C59 C56 C24 111.2(3) . . ? C57 C56 C58 107.8(3) . . ? C59 C56 C58 107.2(3) . . ? C24 C56 C58 111.9(3) . . ? C61B C60 C61A 128.3(9) . . ? C61B C60 C26 115.5(6) . . ? C61A C60 C26 114.3(6) . . ? C61B C60 C63B 113.9(11) . . ? C61A C60 C63B 60.7(9) . . ? C26 C60 C63B 108.0(6) . . ? C61B C60 C63A 37.9(10) . . ? C61A C60 C63A 113.5(10) . . ? C26 C60 C63A 106.5(6) . . ? C63B C60 C63A 143.6(7) . . ? C61B C60 C62A 65.6(10) . . ? C61A C60 C62A 108.5(8) . . ? C26 C60 C62A 110.0(5) . . ? C63B C60 C62A 53.8(8) . . ? C63A C60 C62A 103.3(8) . . ? C61B C60 C62B 103.2(12) . . ? C61A C60 C62B 46.3(7) . . ? C26 C60 C62B 109.5(6) . . ? C63B C60 C62B 106.2(10) . . ? C63A C60 C62B 72.0(8) . . ? C62A C60 C62B 139.8(7) . . ? C67 C64 C36 110.1(3) . . ? C67 C64 C66 108.6(3) . . ? C36 C64 C66 111.4(3) . . ? C67 C64 C65 108.6(3) . . ? C36 C64 C65 109.9(3) . . ? C66 C64 C65 108.2(3) . . ? C70 C68 C38 112.1(3) . . ? C70 C68 C69 107.1(3) . . ? C38 C68 C69 112.2(2) . . ? C70 C68 C71 107.3(3) . . ? C38 C68 C71 108.8(2) . . ? C69 C68 C71 109.3(3) . . ? O9 C72 C77 120.6(3) . . ? O9 C72 C73 120.5(3) . . ? C77 C72 C73 118.9(3) . . ? C74 C73 C72 117.7(3) . . ? C74 C73 C111 121.6(3) . . ? C72 C73 C111 120.7(3) . . ? C73 C74 C75 124.6(3) . . ? C76 C75 C74 116.6(3) . . ? C76 C75 C115 123.6(3) . . ? C74 C75 C115 119.8(3) . . ? C75 C76 C77 121.9(3) . . ? C72 C77 C76 120.3(3) . . ? C72 C77 C78 122.6(3) . . ? C76 C77 C78 117.1(3) . . ? N7 C78 C77 127.9(3) . . ? N7 C79 C80 109.5(3) . . ? C81 C80 C79 114.9(3) . . ? N8 C81 C80 112.0(3) . . ? N8 C82 C83 127.5(4) . . ? C88 C83 C84 120.3(4) . . ? C88 C83 C82 122.2(3) . . ? C84 C83 C82 117.4(4) . . ? C85 C84 C83 121.1(5) . . ? C84 C85 C86 117.2(4) . . ? C84 C85 C119 122.6(6) . . ? C86 C85 C119 120.1(6) . . ? C87 C86 C85 125.9(5) . . ? C86 C87 C88 116.2(5) . . ? C86 C87 C123 122.9(4) . . ? C88 C87 C123 120.9(4) . . ? O10 C88 C83 121.1(3) . . ? O10 C88 C87 119.6(4) . . ? C83 C88 C87 119.2(4) . . ? N10 C89 N9 113.1(3) . . ? C91 C90 N10 108.7(3) . . ? C91 C90 C93 132.7(3) . . ? N10 C90 C93 118.6(3) . . ? N9 C91 C90 108.7(3) . . ? N9 C91 C92 119.2(3) . . ? C90 C91 C92 131.9(3) . . ? O11 C92 O12 124.7(3) . . ? O11 C92 C91 116.2(3) . . ? O12 C92 C91 119.1(3) . . ? O16 C93 O13 123.4(3) . . ? O16 C93 C90 117.7(3) . . ? O13 C93 C90 119.0(3) . . ? O14 C94 C99 119.9(3) . . ? O14 C94 C95 120.4(3) . . ? C99 C94 C95 119.7(3) . . ? C96 C95 C94 117.3(3) . . ? C96 C95 C127 121.1(3) . . ? C94 C95 C127 121.5(3) . . ? C97 C96 C95 123.9(4) . . ? C98 C97 C96 117.9(4) . . ? C98 C97 C131 121.8(4) . . ? C96 C97 C131 120.1(4) . . ? C97 C98 C99 121.4(4) . . ? C98 C99 C94 119.2(3) . . ? C98 C99 C100 116.8(3) . . ? C94 C99 C100 123.8(3) . . ? N11 C100 C99 127.5(3) . . ? N11 C101 C102 110.3(3) . . ? C101 C102 C103 116.0(3) . . ? N12 C103 C102 110.6(3) . . ? N12 C104 C105 127.8(3) . . ? C106 C105 C110 119.6(3) . . ? C106 C105 C104 117.4(3) . . ? C110 C105 C104 122.8(3) . . ? C107 C106 C105 122.4(3) . . ? C106 C107 C108 116.8(3) . . ? C106 C107 C135 122.3(3) . . ? C108 C107 C135 120.8(3) . . ? C109 C108 C107 124.5(3) . . ? C108 C109 C110 117.2(3) . . ? C108 C109 C139 122.5(3) . . ? C110 C109 C139 120.2(3) . . ? O15 C110 C105 120.8(3) . . ? O15 C110 C109 119.8(3) . . ? C105 C110 C109 119.3(3) . . ? C73 C111 C112 111.9(3) . . ? C73 C111 C114 109.6(3) . . ? C112 C111 C114 108.2(3) . . ? C73 C111 C113 109.9(3) . . ? C112 C111 C113 106.9(3) . . ? C114 C111 C113 110.3(3) . . ? C116 C115 C117 107.7(4) . . ? C116 C115 C118 108.5(3) . . ? C117 C115 C118 109.8(4) . . ? C116 C115 C75 110.2(3) . . ? C117 C115 C75 110.8(3) . . ? C118 C115 C75 109.7(4) . . ? C122 C119 C12C 129.3(10) . . ? C122 C119 C85 114.7(8) . . ? C12C C119 C85 115.9(7) . . ? C122 C119 C121 112.4(11) . . ? C12C C119 C121 57.0(8) . . ? C85 C119 C121 104.7(7) . . ? C122 C119 C12A 57.9(9) . . ? C12C C119 C12A 105.7(10) . . ? C85 C119 C12A 110.9(6) . . ? C121 C119 C12A 57.5(8) . . ? C122 C119 C120 114.9(10) . . ? C12C C119 C120 42.1(8) . . ? C85 C119 C120 109.6(6) . . ? C121 C119 C120 99.0(7) . . ? C12A C119 C120 137.1(6) . . ? C122 C119 C12B 37.6(8) . . ? C12C C119 C12B 120.4(10) . . ? C85 C119 C12B 106.5(6) . . ? C121 C119 C12B 144.5(8) . . ? C12A C119 C12B 95.3(7) . . ? C120 C119 C12B 86.0(6) . . ? C126 C123 C125 110.3(4) . . ? C126 C123 C87 111.0(3) . . ? C125 C123 C87 109.3(4) . . ? C126 C123 C124 107.1(3) . . ? C125 C123 C124 106.9(4) . . ? C87 C123 C124 112.2(4) . . ? C95 C127 C128 112.8(3) . . ? C95 C127 C130 109.8(3) . . ? C128 C127 C130 107.8(3) . . ? C95 C127 C129 110.5(3) . . ? C128 C127 C129 106.8(3) . . ? C130 C127 C129 109.1(4) . . ? C134 C131 C132 119.3(5) . . ? C134 C131 C97 117.0(4) . . ? C132 C131 C97 115.0(4) . . ? C134 C131 C133 96.1(6) . . ? C132 C131 C133 99.4(6) . . ? C97 C131 C133 104.4(4) . . ? C136 C135 C138 109.2(4) . . ? C136 C135 C137 108.6(3) . . ? C138 C135 C137 108.0(4) . . ? C136 C135 C107 109.7(3) . . ? C138 C135 C107 110.2(3) . . ? C137 C135 C107 111.1(3) . . ? C141 C139 C140 107.3(3) . . ? C141 C139 C142 107.6(3) . . ? C140 C139 C142 108.9(3) . . ? C141 C139 C109 111.5(3) . . ? C140 C139 C109 111.7(3) . . ? C142 C139 C109 109.7(2) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O1 1.884(2) . ? Fe1 O2 1.906(2) . ? Fe1 N1 2.110(3) . ? Fe1 N2 2.123(3) . ? Fe1 N3 2.137(3) . ? Fe1 O3 2.155(2) . ? Fe2 O6 1.896(2) . ? Fe2 O7 1.906(2) . ? Fe2 N5 2.108(3) . ? Fe2 N6 2.117(3) . ? Fe2 N4 2.126(3) . ? Fe2 O8 2.153(2) . ? Fe3 O9 1.894(2) . ? Fe3 O10 1.901(2) . ? Fe3 N7 2.116(3) . ? Fe3 N9 2.121(2) . ? Fe3 N8 2.121(3) . ? Fe3 O11 2.164(2) . ? Fe4 O15 1.883(2) . ? Fe4 O14 1.890(2) . ? Fe4 N11 2.102(3) . ? Fe4 N10 2.111(2) . ? Fe4 N12 2.123(3) . ? Fe4 O16 2.223(2) . ? N1 C7 1.281(4) . ? N1 C8 1.468(4) . ? N2 C11 1.284(4) . ? N2 C10 1.469(4) . ? N3 C18 1.339(4) . ? N3 C20 1.367(4) . ? N4 C18 1.344(4) . ? N4 C19 1.371(4) . ? N5 C29 1.282(4) . ? N5 C30 1.513(5) . ? N6 C33 1.291(4) . ? N6 C32 1.472(4) . ? N7 C78 1.274(4) . ? N7 C79 1.479(4) . ? N8 C82 1.290(5) . ? N8 C81 1.463(5) . ? N9 C89 1.345(4) . ? N9 C91 1.363(4) . ? N10 C89 1.336(4) . ? N10 C90 1.370(4) . ? N11 C100 1.273(4) . ? N11 C101 1.468(4) . ? N12 C104 1.286(4) . ? N12 C103 1.475(4) . ? O1 C1 1.309(4) . ? O2 C17 1.320(4) . ? O3 C21 1.257(4) . ? O4 C21 1.272(4) . ? O5 C22 1.284(4) . ? O6 C23 1.318(4) . ? O7 C39 1.325(3) . ? O8 C22 1.255(4) . ? O9 C72 1.309(4) . ? O10 C88 1.315(4) . ? O11 C92 1.260(4) . ? O12 C92 1.269(4) . ? O13 C93 1.292(4) . ? O14 C94 1.316(4) . ? O15 C110 1.324(3) . ? O16 C93 1.244(4) . ? C1 C6 1.417(4) . ? C1 C2 1.422(5) . ? C2 C3 1.369(5) . ? C2 C40 1.539(5) . ? C3 C4 1.400(4) . ? C4 C5 1.366(4) . ? C4 C44 1.530(4) . ? C5 C6 1.400(4) . ? C6 C7 1.446(4) . ? C8 C9 1.514(5) . ? C9 C10 1.526(5) . ? C11 C12 1.436(4) . ? C12 C13 1.404(4) . ? C12 C17 1.410(4) . ? C13 C14 1.364(5) . ? C14 C15 1.383(5) . ? C14 C48 1.551(5) . ? C15 C16 1.391(5) . ? C16 C17 1.427(4) . ? C16 C52 1.528(5) . ? C19 C20 1.367(4) . ? C19 C22 1.449(4) . ? C20 C21 1.465(4) . ? C23 C24 1.418(5) . ? C23 C28 1.420(5) . ? C24 C25 1.373(5) . ? C24 C56 1.534(5) . ? C25 C26 1.404(6) . ? C26 C27 1.370(5) . ? C26 C60 1.532(6) . ? C27 C28 1.401(5) . ? C28 C29 1.434(5) . ? C30 C31 1.436(6) . ? C31 C32 1.497(5) . ? C33 C34 1.434(4) . ? C34 C35 1.411(4) . ? C34 C39 1.413(4) . ? C35 C36 1.373(4) . ? C36 C37 1.405(4) . ? C36 C64 1.531(4) . ? C37 C38 1.386(4) . ? C38 C39 1.422(4) . ? C38 C68 1.533(4) . ? C40 C43 1.524(7) . ? C40 C42 1.538(7) . ? C40 C41 1.539(5) . ? C44 C45 1.503(5) . ? C44 C46 1.518(5) . ? C44 C47 1.540(5) . ? C48 C49 1.498(6) . ? C48 C50 1.517(6) . ? C48 C51 1.547(6) . ? C52 C55 1.531(5) . ? C52 C53 1.539(5) . ? C52 C54 1.541(5) . ? C56 C57 1.528(5) . ? C56 C59 1.528(5) . ? C56 C58 1.537(5) . ? C60 C61B 1.485(8) . ? C60 C61A 1.521(8) . ? C60 C63B 1.532(8) . ? C60 C63A 1.534(9) . ? C60 C62A 1.543(7) . ? C60 C62B 1.546(8) . ? C64 C67 1.525(4) . ? C64 C66 1.534(5) . ? C64 C65 1.535(5) . ? C68 C70 1.528(4) . ? C68 C69 1.539(4) . ? C68 C71 1.540(4) . ? C72 C77 1.404(4) . ? C72 C73 1.431(4) . ? C73 C74 1.378(5) . ? C73 C111 1.531(4) . ? C74 C75 1.405(5) . ? C75 C76 1.377(5) . ? C75 C115 1.541(5) . ? C76 C77 1.407(4) . ? C77 C78 1.450(4) . ? C79 C80 1.529(5) . ? C80 C81 1.522(5) . ? C82 C83 1.440(6) . ? C83 C88 1.402(6) . ? C83 C84 1.415(5) . ? C84 C85 1.377(8) . ? C85 C86 1.381(8) . ? C85 C119 1.545(7) . ? C86 C87 1.381(6) . ? C87 C88 1.444(6) . ? C87 C123 1.531(7) . ? C90 C91 1.361(4) . ? C90 C93 1.453(4) . ? C91 C92 1.460(4) . ? C94 C99 1.409(5) . ? C94 C95 1.416(5) . ? C95 C96 1.384(5) . ? C95 C127 1.524(5) . ? C96 C97 1.373(6) . ? C97 C98 1.372(6) . ? C97 C131 1.525(7) . ? C98 C99 1.398(5) . ? C99 C100 1.438(5) . ? C101 C102 1.521(5) . ? C102 C103 1.520(5) . ? C104 C105 1.437(4) . ? C105 C106 1.403(4) . ? C105 C110 1.417(4) . ? C106 C107 1.364(4) . ? C107 C108 1.405(4) . ? C107 C135 1.541(4) . ? C108 C109 1.386(4) . ? C109 C110 1.422(4) . ? C109 C139 1.543(4) . ? C111 C112 1.533(5) . ? C111 C114 1.533(5) . ? C111 C113 1.534(5) . ? C115 C116 1.525(6) . ? C115 C117 1.530(6) . ? C115 C118 1.529(6) . ? C119 C122 1.462(9) . ? C119 C12C 1.469(8) . ? C119 C121 1.545(9) . ? C119 C12A 1.548(9) . ? C119 C120 1.575(8) . ? C119 C12B 1.592(8) . ? C123 C126 1.517(5) . ? C123 C125 1.526(6) . ? C123 C124 1.548(5) . ? C127 C128 1.537(5) . ? C127 C130 1.537(5) . ? C127 C129 1.540(5) . ? C131 C134 1.442(6) . ? C131 C132 1.466(6) . ? C131 C133 1.618(9) . ? C135 C136 1.511(5) . ? C135 C138 1.523(6) . ? C135 C137 1.526(5) . ? C139 C141 1.531(4) . ? C139 C140 1.533(5) . ? C139 C142 1.539(4) . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H4A O5 0.84 1.66 2.502(4) 179.8 . O5 H5B O4 0.84 1.66 2.502(4) 178.2 . O12 H12S O13 0.84 1.67 2.510(3) 179.3 . O13 H13W O12 0.84 1.67 2.510(3) 177.9 .
1100758.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $ #$Revision: 176435 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100758.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100758 loop_ _publ_author_name 'Panagiotis Angaridis' 'Jeff W. Kampf' 'Vincent L. Pecoraro' _publ_contact_author_address ; Chemistry Department University of Michigan 930 N.University Ann Arbor, MI 48109, USA ; _publ_contact_author_email vlpec@umich.edu _publ_contact_author_fax '(734) 936 7628' _publ_contact_author_name 'Vincent. L. Pecoraro' _publ_contact_author_phone '(734) 763 1519' _publ_section_title ; Multinuclear Fe(III) Complexes with Polydentate Ligands of the Family of Dicarboxyimidazoles: Nuclearity- and Topology-Controlled Syntheses and Magneto-Structural Correlations ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3626 _journal_page_last 3635 _journal_paper_doi 10.1021/ic0481879 _journal_volume 44 _journal_year 2005 _chemical_formula_moiety 'C104 H145 N8 O10 Fe3, 2.5(C2H3N)' _chemical_formula_sum 'C109 H152.5 Fe3 N10.5 O10' _chemical_formula_weight 1937.46 _chemical_name_systematic ; ? ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 104.552(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 26.567(5) _cell_length_b 15.983(3) _cell_length_c 26.753(5) _cell_measurement_reflns_used 8333 _cell_measurement_temperature 113(2) _cell_measurement_theta_max 23.35 _cell_measurement_theta_min 2.81 _cell_volume 10995(4) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _diffrn_ambient_temperature 113(2) _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0498 _diffrn_reflns_av_sigmaI/netI 0.0426 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_number 130850 _diffrn_reflns_theta_full 28.45 _diffrn_reflns_theta_max 28.45 _diffrn_reflns_theta_min 2.80 _exptl_absorpt_coefficient_mu 0.449 _exptl_absorpt_correction_T_max 0.9316 _exptl_absorpt_correction_T_min 0.7806 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Blessing, R. Acta Cryst. (1995) A51 33-38 Sheldrick, G. SADABS (Version 2.10) Bruker/Siemens area detector absorption and other corrections, University of Gottingen, Germany 2003. ; _exptl_crystal_colour purple _exptl_crystal_density_diffrn 1.170 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 4152 _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.16 _refine_diff_density_max 0.765 _refine_diff_density_min -0.464 _refine_diff_density_rms 0.064 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 1246 _refine_ls_number_reflns 27591 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.023 _refine_ls_R_factor_all 0.0715 _refine_ls_R_factor_gt 0.0439 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0595P)^2^+7.3751P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1126 _refine_ls_wR_factor_ref 0.1267 _reflns_number_gt 20240 _reflns_number_total 27591 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic0481879si20041222_050013_1.cif _cod_data_source_block compound4 _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_cell_volume 10996(3) _cod_original_formula_sum 'C109 H152.50 Fe3 N10.50 O10' _cod_database_code 1100758 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.253826(8) -0.104428(13) 0.381267(8) 0.02017(5) Uani 1 1 d . . . Fe2 Fe 0.295893(8) 0.192627(13) 0.251927(7) 0.01848(4) Uani 1 1 d . . . Fe3 Fe 0.257387(8) 0.239892(13) 0.477492(7) 0.01822(4) Uani 1 1 d . . . N1 N 0.25692(5) -0.19799(8) 0.32457(5) 0.0227(3) Uani 1 1 d . . . N2 N 0.33460(5) -0.13217(8) 0.40569(5) 0.0235(3) Uani 1 1 d . . . N3 N 0.31611(5) 0.13673(8) 0.18770(4) 0.0196(3) Uani 1 1 d . . . N4 N 0.37715(5) 0.18399(8) 0.28873(4) 0.0222(3) Uani 1 1 d . . . N5 N 0.17497(5) 0.23585(8) 0.45817(4) 0.0222(3) Uani 1 1 d . . . N6 N 0.25231(5) 0.22283(8) 0.55395(4) 0.0196(3) Uani 1 1 d . . . N7 N 0.27555(5) 0.19736(7) 0.32337(4) 0.0204(3) Uani 1 1 d . . . N8 N 0.26106(5) 0.21375(8) 0.40130(4) 0.0204(3) Uani 1 1 d . . . O1 O 0.18087(4) -0.10281(7) 0.35272(4) 0.0260(2) Uani 1 1 d . . . O2 O 0.24700(4) -0.17240(6) 0.43788(4) 0.0227(2) Uani 1 1 d . . . O3 O 0.22847(4) 0.20703(7) 0.20744(4) 0.0226(2) Uani 1 1 d . . . O4 O 0.30875(4) 0.30941(6) 0.24965(4) 0.0223(2) Uani 1 1 d . . . O5 O 0.25020(4) 0.35702(6) 0.46706(4) 0.0213(2) Uani 1 1 d . . . O6 O 0.33053(4) 0.24325(7) 0.50281(4) 0.0234(2) Uani 1 1 d . . . O7 O 0.26907(4) -0.02574(6) 0.32503(4) 0.0248(2) Uani 1 1 d . . . O8 O 0.28706(4) 0.06512(6) 0.26939(4) 0.0225(2) Uani 1 1 d . . . O9 O 0.25900(4) -0.00520(6) 0.42880(4) 0.0259(2) Uani 1 1 d . . . O10 O 0.25470(4) 0.10820(6) 0.47449(4) 0.0238(2) Uani 1 1 d . . . C1 C 0.21708(6) -0.22326(9) 0.29005(6) 0.0247(3) Uani 1 1 d . . . H1A H 0.2237 -0.2634 0.2663 0.030 Uiso 1 1 calc R . . C2 C 0.16365(6) -0.19839(9) 0.28280(6) 0.0244(3) Uani 1 1 d . . . C3 C 0.14743(6) -0.13844(10) 0.31430(6) 0.0241(3) Uani 1 1 d . . . C4 C 0.09369(6) -0.11702(10) 0.30293(6) 0.0265(3) Uani 1 1 d . . . C5 C 0.06089(6) -0.15314(11) 0.25999(6) 0.0296(4) Uani 1 1 d . . . H5A H 0.0252 -0.1377 0.2520 0.036 Uiso 1 1 calc R . . C6 C 0.07641(6) -0.21093(10) 0.22731(6) 0.0282(4) Uani 1 1 d . . . C7 C 0.12796(6) -0.23308(10) 0.24001(6) 0.0271(4) Uani 1 1 d . . . H7A H 0.1398 -0.2730 0.2193 0.033 Uiso 1 1 calc R . . C8 C 0.07420(6) -0.05530(11) 0.33754(6) 0.0320(4) Uani 1 1 d . . . C9 C 0.10044(8) 0.02988(12) 0.33767(8) 0.0448(5) Uani 1 1 d . . . H9A H 0.0877 0.0684 0.3602 0.067 Uiso 1 1 calc R . . H9B H 0.0922 0.0524 0.3025 0.067 Uiso 1 1 calc R . . H9C H 0.1382 0.0234 0.3504 0.067 Uiso 1 1 calc R . . C10 C 0.08565(8) -0.09024(14) 0.39271(7) 0.0455(5) Uani 1 1 d . . . H10A H 0.1233 -0.0969 0.4063 0.068 Uiso 1 1 calc R . . H10B H 0.0686 -0.1447 0.3923 0.068 Uiso 1 1 calc R . . H10C H 0.0724 -0.0514 0.4147 0.068 Uiso 1 1 calc R . . C11 C 0.01515(7) -0.04097(13) 0.31957(7) 0.0419(5) Uani 1 1 d . . . H11A H 0.0043 -0.0029 0.3436 0.063 Uiso 1 1 calc R . . H11B H -0.0030 -0.0946 0.3187 0.063 Uiso 1 1 calc R . . H11C H 0.0065 -0.0163 0.2849 0.063 Uiso 1 1 calc R . . C12 C 0.03718(6) -0.24426(11) 0.17927(6) 0.0326(4) Uani 1 1 d . . . C13 C 0.05970(8) -0.31332(13) 0.15202(7) 0.0451(5) Uani 1 1 d . . . H13A H 0.0716 -0.3596 0.1761 0.068 Uiso 1 1 calc R . . H13B H 0.0891 -0.2912 0.1401 0.068 Uiso 1 1 calc R . . H13C H 0.0328 -0.3335 0.1223 0.068 Uiso 1 1 calc R . . C14 C 0.02153(8) -0.17239(13) 0.14084(7) 0.0451(5) Uani 1 1 d . . . H14A H -0.0046 -0.1921 0.1104 0.068 Uiso 1 1 calc R . . H14B H 0.0522 -0.1524 0.1303 0.068 Uiso 1 1 calc R . . H14C H 0.0070 -0.1266 0.1571 0.068 Uiso 1 1 calc R . . C15 C -0.01100(7) -0.27777(14) 0.19363(7) 0.0457(5) Uani 1 1 d . . . H15A H -0.0360 -0.2979 0.1625 0.068 Uiso 1 1 calc R . . H15B H -0.0269 -0.2330 0.2094 0.068 Uiso 1 1 calc R . . H15C H -0.0011 -0.3240 0.2182 0.068 Uiso 1 1 calc R . . C16 C 0.30743(6) -0.22965(10) 0.32003(6) 0.0279(4) Uani 1 1 d . . . H16A H 0.3022 -0.2641 0.2884 0.033 Uiso 1 1 calc R . . H16B H 0.3225 -0.2660 0.3500 0.033 Uiso 1 1 calc R . . C17 C 0.34536(6) -0.15935(10) 0.31773(6) 0.0278(4) Uani 1 1 d . . . H17A H 0.3274 -0.1169 0.2925 0.033 Uiso 1 1 calc R . . H17B H 0.3745 -0.1823 0.3050 0.033 Uiso 1 1 calc R . . C18 C 0.36758(6) -0.11639(10) 0.37016(6) 0.0274(4) Uani 1 1 d . . . H18A H 0.4031 -0.1377 0.3856 0.033 Uiso 1 1 calc R . . H18B H 0.3700 -0.0554 0.3649 0.033 Uiso 1 1 calc R . . C19 C 0.35651(6) -0.16886(10) 0.44831(6) 0.0258(3) Uani 1 1 d . . . H19A H 0.3927 -0.1795 0.4542 0.031 Uiso 1 1 calc R . . C20 C 0.33233(6) -0.19570(10) 0.48821(5) 0.0244(3) Uani 1 1 d . . . C21 C 0.36562(6) -0.22604(10) 0.53431(6) 0.0288(4) Uani 1 1 d . . . H21A H 0.4019 -0.2298 0.5370 0.035 Uiso 1 1 calc R . . C22 C 0.34681(7) -0.25018(10) 0.57528(6) 0.0308(4) Uani 1 1 d . . . C23 C 0.29308(7) -0.24271(10) 0.56949(6) 0.0302(4) Uani 1 1 d . . . H23A H 0.2797 -0.2584 0.5979 0.036 Uiso 1 1 calc R . . C24 C 0.25826(6) -0.21414(10) 0.52547(6) 0.0254(3) Uani 1 1 d . . . C25 C 0.27836(6) -0.19255(9) 0.48229(5) 0.0228(3) Uani 1 1 d . . . C26 C 0.38176(7) -0.28198(13) 0.62611(6) 0.0405(5) Uani 1 1 d . . . C27 C 0.36566(10) -0.37132(14) 0.63664(8) 0.0578(6) Uani 1 1 d . . . H27A H 0.3692 -0.4082 0.6085 0.087 Uiso 1 1 calc R . . H27B H 0.3294 -0.3712 0.6389 0.087 Uiso 1 1 calc R . . H27C H 0.3881 -0.3915 0.6693 0.087 Uiso 1 1 calc R . . C28 C 0.37565(9) -0.22527(15) 0.67049(7) 0.0542(6) Uani 1 1 d . . . H28A H 0.3980 -0.2457 0.7031 0.081 Uiso 1 1 calc R . . H28B H 0.3393 -0.2259 0.6725 0.081 Uiso 1 1 calc R . . H28C H 0.3857 -0.1680 0.6642 0.081 Uiso 1 1 calc R . . C29 C 0.43879(8) -0.28303(17) 0.62447(8) 0.0594(7) Uani 1 1 d . . . H29A H 0.4429 -0.3192 0.5962 0.089 Uiso 1 1 calc R . . H29B H 0.4601 -0.3044 0.6573 0.089 Uiso 1 1 calc R . . H29C H 0.4499 -0.2261 0.6188 0.089 Uiso 1 1 calc R . . C30 C 0.20061(6) -0.20157(11) 0.52257(6) 0.0321(4) Uani 1 1 d . . . C31 C 0.18674(7) -0.23131(15) 0.57204(7) 0.0475(5) Uani 1 1 d . . . H31A H 0.1966 -0.2902 0.5783 0.071 Uiso 1 1 calc R . . H31B H 0.1492 -0.2254 0.5680 0.071 Uiso 1 1 calc R . . H31C H 0.2055 -0.1974 0.6013 0.071 Uiso 1 1 calc R . . C32 C 0.16689(7) -0.25180(12) 0.47740(7) 0.0376(4) Uani 1 1 d . . . H32A H 0.1717 -0.2299 0.4447 0.056 Uiso 1 1 calc R . . H32B H 0.1302 -0.2468 0.4778 0.056 Uiso 1 1 calc R . . H32C H 0.1772 -0.3108 0.4809 0.056 Uiso 1 1 calc R . . C33 C 0.18854(7) -0.10743(12) 0.51589(7) 0.0373(4) Uani 1 1 d . . . H33A H 0.2088 -0.0770 0.5461 0.056 Uiso 1 1 calc R . . H33B H 0.1514 -0.0982 0.5126 0.056 Uiso 1 1 calc R . . H33C H 0.1977 -0.0871 0.4848 0.056 Uiso 1 1 calc R . . C34 C 0.28205(6) 0.10567(9) 0.14947(5) 0.0210(3) Uani 1 1 d . . . H34A H 0.2952 0.0741 0.1254 0.025 Uiso 1 1 calc R . . C35 C 0.22640(6) 0.11291(9) 0.13864(5) 0.0210(3) Uani 1 1 d . . . C36 C 0.20128(6) 0.16351(9) 0.16849(5) 0.0209(3) Uani 1 1 d . . . C37 C 0.14589(6) 0.16819(10) 0.15455(6) 0.0249(3) Uani 1 1 d . . . C38 C 0.11962(6) 0.12173(10) 0.11282(6) 0.0270(4) Uani 1 1 d . . . H38A H 0.0827 0.1243 0.1037 0.032 Uiso 1 1 calc R . . C39 C 0.14354(6) 0.07058(10) 0.08260(5) 0.0255(3) Uani 1 1 d . . . C40 C 0.19684(6) 0.06807(9) 0.09600(5) 0.0231(3) Uani 1 1 d . . . H40A H 0.2143 0.0352 0.0760 0.028 Uiso 1 1 calc R . . C41 C 0.11729(6) 0.22425(12) 0.18512(6) 0.0329(4) Uani 1 1 d . . . C42 C 0.13095(7) 0.31558(11) 0.17810(7) 0.0389(4) Uani 1 1 d . . . H42A H 0.1151 0.3513 0.1997 0.058 Uiso 1 1 calc R . . H42B H 0.1177 0.3315 0.1418 0.058 Uiso 1 1 calc R . . H42C H 0.1688 0.3225 0.1883 0.058 Uiso 1 1 calc R . . C43 C 0.05822(7) 0.21542(14) 0.16593(8) 0.0485(5) Uani 1 1 d . . . H43A H 0.0483 0.1572 0.1698 0.073 Uiso 1 1 calc R . . H43B H 0.0472 0.2315 0.1295 0.073 Uiso 1 1 calc R . . H43C H 0.0413 0.2519 0.1863 0.073 Uiso 1 1 calc R . . C44 C 0.13224(8) 0.20077(15) 0.24242(7) 0.0491(5) Uani 1 1 d . . . H44A H 0.1694 0.2110 0.2568 0.074 Uiso 1 1 calc R . . H44B H 0.1247 0.1414 0.2462 0.074 Uiso 1 1 calc R . . H44C H 0.1121 0.2348 0.2610 0.074 Uiso 1 1 calc R . . C45 C 0.10958(6) 0.02008(11) 0.03825(6) 0.0310(4) Uani 1 1 d . . . C46 C 0.07886(7) -0.04489(13) 0.06095(7) 0.0451(5) Uani 1 1 d . . . H46A H 0.0564 -0.0771 0.0329 0.068 Uiso 1 1 calc R . . H46B H 0.0574 -0.0162 0.0806 0.068 Uiso 1 1 calc R . . H46C H 0.1031 -0.0828 0.0839 0.068 Uiso 1 1 calc R . . C47 C 0.14227(7) -0.02630(11) 0.00798(6) 0.0345(4) Uani 1 1 d . . . H47A H 0.1632 0.0140 -0.0058 0.052 Uiso 1 1 calc R . . H47B H 0.1194 -0.0569 -0.0206 0.052 Uiso 1 1 calc R . . H47C H 0.1654 -0.0658 0.0308 0.052 Uiso 1 1 calc R . . C48 C 0.07174(7) 0.07836(14) 0.00162(7) 0.0423(5) Uani 1 1 d . . . H48A H 0.0913 0.1224 -0.0107 0.063 Uiso 1 1 calc R . . H48B H 0.0480 0.1037 0.0200 0.063 Uiso 1 1 calc R . . H48C H 0.0517 0.0462 -0.0279 0.063 Uiso 1 1 calc R . . C49 C 0.37065(6) 0.11653(10) 0.19140(5) 0.0246(3) Uani 1 1 d . . . H49A H 0.3911 0.1689 0.1948 0.030 Uiso 1 1 calc R . . H49B H 0.3735 0.0880 0.1594 0.030 Uiso 1 1 calc R . . C50 C 0.39301(6) 0.06012(10) 0.23769(6) 0.0274(4) Uani 1 1 d . . . H50A H 0.4260 0.0359 0.2336 0.033 Uiso 1 1 calc R . . H50B H 0.3685 0.0132 0.2371 0.033 Uiso 1 1 calc R . . C51 C 0.40357(6) 0.10256(10) 0.29081(6) 0.0266(4) Uani 1 1 d . . . H51A H 0.3916 0.0653 0.3151 0.032 Uiso 1 1 calc R . . H51B H 0.4415 0.1108 0.3042 0.032 Uiso 1 1 calc R . . C52 C 0.40437(6) 0.24580(10) 0.31174(5) 0.0234(3) Uani 1 1 d . . . H52A H 0.4386 0.2330 0.3312 0.028 Uiso 1 1 calc R . . C53 C 0.38875(6) 0.33253(10) 0.31132(5) 0.0231(3) Uani 1 1 d . . . C54 C 0.42481(6) 0.38930(10) 0.34056(6) 0.0269(4) Uani 1 1 d . . . H54A H 0.4566 0.3687 0.3617 0.032 Uiso 1 1 calc R . . C55 C 0.41517(6) 0.47397(10) 0.33940(6) 0.0290(4) Uani 1 1 d . . . C56 C 0.36777(6) 0.50104(10) 0.30762(6) 0.0282(3) Uani 1 1 d . . . H56A H 0.3606 0.5593 0.3065 0.034 Uiso 1 1 calc R . . C57 C 0.33058(6) 0.44851(10) 0.27769(5) 0.0247(3) Uani 1 1 d . . . C58 C 0.34165(6) 0.36155(9) 0.27904(5) 0.0218(3) Uani 1 1 d . . . C59 C 0.45562(7) 0.53591(11) 0.37059(7) 0.0359(4) Uani 1 1 d . . . C60 C 0.43250(10) 0.61893(15) 0.37729(11) 0.0722(8) Uani 1 1 d . . . H60A H 0.4590 0.6545 0.3994 0.108 Uiso 1 1 calc R . . H60B H 0.4035 0.6112 0.3934 0.108 Uiso 1 1 calc R . . H60C H 0.4197 0.6456 0.3435 0.108 Uiso 1 1 calc R . . C61 C 0.47765(10) 0.50131(16) 0.42591(8) 0.0639(7) Uani 1 1 d . . . H61A H 0.5021 0.5419 0.4463 0.096 Uiso 1 1 calc R . . H61B H 0.4958 0.4484 0.4241 0.096 Uiso 1 1 calc R . . H61C H 0.4490 0.4918 0.4423 0.096 Uiso 1 1 calc R . . C62 C 0.50045(9) 0.54385(16) 0.34556(9) 0.0637(6) Uani 1 1 d . . . H62A H 0.4876 0.5652 0.3103 0.095 Uiso 1 1 calc R . . H62B H 0.5164 0.4888 0.3445 0.095 Uiso 1 1 calc R . . H62C H 0.5264 0.5826 0.3656 0.095 Uiso 1 1 calc R . . C63 C 0.27858(7) 0.48133(10) 0.24482(6) 0.0297(4) Uani 1 1 d . . . C64 C 0.27429(8) 0.57641(11) 0.24833(7) 0.0414(5) Uani 1 1 d . . . H64A H 0.2765 0.5925 0.2842 0.062 Uiso 1 1 calc R . . H64B H 0.2409 0.5949 0.2262 0.062 Uiso 1 1 calc R . . H64C H 0.3027 0.6028 0.2368 0.062 Uiso 1 1 calc R . . C65 C 0.27219(8) 0.45950(11) 0.18758(6) 0.0382(4) Uani 1 1 d . . . H65A H 0.3016 0.4821 0.1760 0.057 Uiso 1 1 calc R . . H65B H 0.2398 0.4839 0.1669 0.057 Uiso 1 1 calc R . . H65C H 0.2711 0.3986 0.1833 0.057 Uiso 1 1 calc R . . C66 C 0.23408(7) 0.44361(11) 0.26421(7) 0.0345(4) Uani 1 1 d . . . H66A H 0.2351 0.3825 0.2617 0.052 Uiso 1 1 calc R . . H66B H 0.2008 0.4644 0.2431 0.052 Uiso 1 1 calc R . . H66C H 0.2379 0.4598 0.3003 0.052 Uiso 1 1 calc R . . C67 C 0.14714(6) 0.29232(10) 0.43014(6) 0.0253(3) Uani 1 1 d . . . H67A H 0.1110 0.2810 0.4186 0.030 Uiso 1 1 calc R . . C68 C 0.16451(6) 0.37115(10) 0.41409(5) 0.0245(3) Uani 1 1 d . . . C69 C 0.21536(6) 0.40173(9) 0.43431(5) 0.0219(3) Uani 1 1 d . . . C70 C 0.22810(6) 0.48379(10) 0.42053(5) 0.0244(3) Uani 1 1 d . . . C71 C 0.18900(6) 0.52951(10) 0.38807(6) 0.0283(4) Uani 1 1 d . . . H71A H 0.1974 0.5839 0.3783 0.034 Uiso 1 1 calc R . . C77 C 0.28815(7) 0.60666(11) 0.42032(8) 0.0391(4) Uani 1 1 d . . . H77A H 0.2831 0.6025 0.3828 0.059 Uiso 1 1 calc R . . H77B H 0.3231 0.6283 0.4360 0.059 Uiso 1 1 calc R . . H77C H 0.2621 0.6446 0.4280 0.059 Uiso 1 1 calc R . . C72 C 0.13813(6) 0.50126(10) 0.36865(6) 0.0295(4) Uani 1 1 d . . . C73 C 0.12682(6) 0.42206(11) 0.38191(6) 0.0288(4) Uani 1 1 d . . . H73A H 0.0926 0.4010 0.3690 0.035 Uiso 1 1 calc R . . C74 C 0.28220(6) 0.51989(10) 0.44243(6) 0.0270(3) Uani 1 1 d . . . C75 C 0.32373(6) 0.46286(11) 0.42965(7) 0.0343(4) Uani 1 1 d . . . H75A H 0.3217 0.4072 0.4444 0.051 Uiso 1 1 calc R . . H75B H 0.3583 0.4867 0.4443 0.051 Uiso 1 1 calc R . . H75C H 0.3178 0.4582 0.3921 0.051 Uiso 1 1 calc R . . C76 C 0.29237(7) 0.52857(12) 0.50158(6) 0.0355(4) Uani 1 1 d . . . H76A H 0.2660 0.5653 0.5098 0.053 Uiso 1 1 calc R . . H76B H 0.3270 0.5526 0.5156 0.053 Uiso 1 1 calc R . . H76C H 0.2906 0.4733 0.5169 0.053 Uiso 1 1 calc R . . C78 C 0.09831(7) 0.55849(11) 0.33310(6) 0.0338(4) Uani 1 1 d . . . C79 C 0.11098(8) 0.56095(13) 0.28048(7) 0.0436(5) Uani 1 1 d . . . H79A H 0.1081 0.5045 0.2658 0.065 Uiso 1 1 calc R . . H79B H 0.1465 0.5818 0.2846 0.065 Uiso 1 1 calc R . . H79C H 0.0865 0.5982 0.2573 0.065 Uiso 1 1 calc R . . C80 C 0.09986(8) 0.64694(12) 0.35539(7) 0.0432(5) Uani 1 1 d . . . H80A H 0.0740 0.6819 0.3321 0.065 Uiso 1 1 calc R . . H80B H 0.1346 0.6709 0.3591 0.065 Uiso 1 1 calc R . . H80C H 0.0921 0.6446 0.3893 0.065 Uiso 1 1 calc R . . C81 C 0.04298(7) 0.52514(13) 0.32530(7) 0.0429(5) Uani 1 1 d . . . H81A H 0.0185 0.5637 0.3032 0.064 Uiso 1 1 calc R . . H81B H 0.0346 0.5203 0.3588 0.064 Uiso 1 1 calc R . . H81C H 0.0403 0.4700 0.3089 0.064 Uiso 1 1 calc R . . C82 C 0.14779(6) 0.16472(10) 0.47447(6) 0.0268(4) Uani 1 1 d . . . H82A H 0.1512 0.1150 0.4535 0.032 Uiso 1 1 calc R . . H82B H 0.1103 0.1780 0.4681 0.032 Uiso 1 1 calc R . . C83 C 0.16981(6) 0.14444(10) 0.53185(6) 0.0278(4) Uani 1 1 d . . . H83A H 0.1406 0.1291 0.5469 0.033 Uiso 1 1 calc R . . H83B H 0.1927 0.0949 0.5347 0.033 Uiso 1 1 calc R . . C84 C 0.20052(6) 0.21516(10) 0.56389(5) 0.0235(3) Uani 1 1 d . . . H84A H 0.1814 0.2685 0.5551 0.028 Uiso 1 1 calc R . . H84B H 0.2043 0.2039 0.6010 0.028 Uiso 1 1 calc R . . C85 C 0.29180(6) 0.21023(9) 0.59195(5) 0.0201(3) Uani 1 1 d . . . H85A H 0.2849 0.2047 0.6249 0.024 Uiso 1 1 calc R . . C86 C 0.34569(6) 0.20346(9) 0.59062(5) 0.0204(3) Uani 1 1 d . . . C87 C 0.38085(6) 0.17674(10) 0.63604(5) 0.0234(3) Uani 1 1 d . . . H87A H 0.3692 0.1710 0.6667 0.028 Uiso 1 1 calc R . . C88 C 0.43171(6) 0.15868(10) 0.63740(5) 0.0246(3) Uani 1 1 d . . . C89 C 0.44731(6) 0.16881(10) 0.59152(5) 0.0240(3) Uani 1 1 d . . . H89A H 0.4823 0.1560 0.5919 0.029 Uiso 1 1 calc R . . C90 C 0.41481(6) 0.19633(10) 0.54557(5) 0.0231(3) Uani 1 1 d . . . C91 C 0.36269(6) 0.21522(9) 0.54493(5) 0.0206(3) Uani 1 1 d . . . C92 C 0.46945(6) 0.12850(12) 0.68720(6) 0.0342(4) Uani 1 1 d . . . C93 C 0.47777(8) 0.19949(16) 0.72666(7) 0.0540(6) Uani 1 1 d . . . H93A H 0.5010 0.1805 0.7592 0.081 Uiso 1 1 calc R . . H93B H 0.4443 0.2160 0.7327 0.081 Uiso 1 1 calc R . . H93C H 0.4934 0.2475 0.7134 0.081 Uiso 1 1 calc R . . C94 C 0.44686(8) 0.05276(15) 0.70889(8) 0.0540(6) Uani 1 1 d . . . H94A H 0.4426 0.0064 0.6842 0.081 Uiso 1 1 calc R . . H94B H 0.4130 0.0675 0.7147 0.081 Uiso 1 1 calc R . . H94C H 0.4706 0.0358 0.7416 0.081 Uiso 1 1 calc R . . C95 C 0.52204(7) 0.10483(15) 0.67911(7) 0.0490(5) Uani 1 1 d . . . H95A H 0.5455 0.0892 0.7123 0.074 Uiso 1 1 calc R . . H95B H 0.5366 0.1526 0.6646 0.074 Uiso 1 1 calc R . . H95C H 0.5180 0.0574 0.6552 0.074 Uiso 1 1 calc R . . C96 C 0.43442(6) 0.20300(12) 0.49626(6) 0.0312(4) Uani 1 1 d . . . C97 C 0.40303(7) 0.14335(14) 0.45494(6) 0.0434(5) Uani 1 1 d . . . H97A H 0.3663 0.1599 0.4461 0.065 Uiso 1 1 calc R . . H97B H 0.4063 0.0860 0.4684 0.065 Uiso 1 1 calc R . . H97C H 0.4164 0.1461 0.4240 0.065 Uiso 1 1 calc R . . C98 C 0.49172(6) 0.17880(14) 0.50582(6) 0.0413(5) Uani 1 1 d . . . H98A H 0.5027 0.1842 0.4736 0.062 Uiso 1 1 calc R . . H98B H 0.4964 0.1208 0.5179 0.062 Uiso 1 1 calc R . . H98C H 0.5128 0.2159 0.5320 0.062 Uiso 1 1 calc R . . C99 C 0.42909(7) 0.29262(14) 0.47608(7) 0.0449(5) Uani 1 1 d . . . H99A H 0.4491 0.3302 0.5027 0.067 Uiso 1 1 calc R . . H99B H 0.3924 0.3090 0.4674 0.067 Uiso 1 1 calc R . . H99C H 0.4424 0.2962 0.4451 0.067 Uiso 1 1 calc R . . C100 C 0.27024(5) 0.11969(9) 0.34323(5) 0.0185(3) Uani 1 1 d . . . C101 C 0.26145(5) 0.12986(9) 0.39130(5) 0.0187(3) Uani 1 1 d . . . C102 C 0.26971(6) 0.25133(9) 0.35955(5) 0.0205(3) Uani 1 1 d . . . H10D H 0.2715 0.3103 0.3560 0.025 Uiso 1 1 calc R . . C103 C 0.27557(5) 0.04755(9) 0.31151(5) 0.0196(3) Uani 1 1 d . . . C104 C 0.25775(6) 0.07261(9) 0.43317(5) 0.0209(3) Uani 1 1 d . . . N200 N 0.45078(11) -0.05645(17) 0.58035(13) 0.1067(9) Uani 1 1 d . . . C200 C 0.40759(11) -0.03774(15) 0.56993(11) 0.0682(7) Uani 1 1 d . . . C201 C 0.35315(10) -0.01489(14) 0.55909(9) 0.0625(7) Uani 1 1 d . . . H20A H 0.3331 -0.0621 0.5673 0.094 Uiso 1 1 calc R . . H20B H 0.3405 -0.0007 0.5224 0.094 Uiso 1 1 calc R . . H20C H 0.3491 0.0335 0.5802 0.094 Uiso 1 1 calc R . . N201 N 0.24457(9) -0.14720(17) 0.18254(8) 0.0777(7) Uani 1 1 d . . . C202 C 0.21592(9) -0.10151(15) 0.19256(7) 0.0490(5) Uani 1 1 d . . . C203 C 0.17891(8) -0.04485(12) 0.20585(7) 0.0425(5) Uani 1 1 d . . . H20D H 0.1455 -0.0735 0.2018 0.064 Uiso 1 1 calc R . . H20E H 0.1742 0.0040 0.1830 0.064 Uiso 1 1 calc R . . H20F H 0.1919 -0.0266 0.2418 0.064 Uiso 1 1 calc R . . N202 N 0.0664(3) 0.5113(4) 0.0695(3) 0.155(2) Uani 0.50 1 d P . . C205 C 0.0171(4) 0.3721(8) -0.0003(4) 0.251(6) Uani 0.50 1 d P . . H20G H -0.0162 0.3942 -0.0206 0.376 Uiso 0.50 1 calc PR . . H20H H 0.0108 0.3225 0.0188 0.376 Uiso 0.50 1 calc PR . . H20I H 0.0389 0.3567 -0.0235 0.376 Uiso 0.50 1 calc PR . . C204 C 0.0418(3) 0.4313(7) 0.0335(5) 0.194(4) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.02484(10) 0.01434(10) 0.02114(9) 0.00030(8) 0.00544(7) 0.00002(8) Fe2 0.02440(9) 0.01513(9) 0.01625(8) -0.00045(7) 0.00576(7) 0.00053(8) Fe3 0.02287(9) 0.01619(10) 0.01533(8) -0.00068(7) 0.00429(7) 0.00090(8) N1 0.0260(6) 0.0143(6) 0.0279(6) 0.0007(5) 0.0072(5) -0.0001(5) N2 0.0262(6) 0.0209(6) 0.0245(5) -0.0018(5) 0.0083(5) -0.0035(5) N3 0.0234(5) 0.0180(6) 0.0184(5) 0.0014(4) 0.0072(4) 0.0017(5) N4 0.0271(6) 0.0192(6) 0.0203(5) 0.0008(5) 0.0057(5) 0.0000(5) N5 0.0264(6) 0.0190(6) 0.0204(5) -0.0026(5) 0.0040(5) -0.0019(5) N6 0.0236(6) 0.0169(6) 0.0194(5) -0.0022(4) 0.0075(4) 0.0001(5) N7 0.0272(6) 0.0157(6) 0.0178(5) 0.0002(4) 0.0046(4) -0.0003(5) N8 0.0255(6) 0.0172(6) 0.0182(5) 0.0000(5) 0.0049(4) 0.0009(5) O1 0.0252(5) 0.0243(5) 0.0265(5) -0.0024(4) 0.0027(4) 0.0032(4) O2 0.0254(5) 0.0189(5) 0.0229(4) 0.0034(4) 0.0044(4) 0.0001(4) O3 0.0257(5) 0.0232(5) 0.0186(4) -0.0025(4) 0.0051(4) 0.0024(4) O4 0.0286(5) 0.0166(5) 0.0209(4) -0.0003(4) 0.0045(4) -0.0009(4) O5 0.0244(5) 0.0170(5) 0.0215(4) -0.0004(4) 0.0036(4) 0.0006(4) O6 0.0222(5) 0.0303(6) 0.0173(4) 0.0044(4) 0.0043(4) 0.0023(4) O7 0.0394(6) 0.0151(5) 0.0210(4) -0.0003(4) 0.0098(4) -0.0017(4) O8 0.0320(5) 0.0169(5) 0.0199(4) -0.0023(4) 0.0092(4) -0.0011(4) O9 0.0403(6) 0.0148(5) 0.0233(5) -0.0004(4) 0.0095(4) 0.0000(4) O10 0.0345(5) 0.0194(5) 0.0188(4) 0.0012(4) 0.0093(4) 0.0022(4) C1 0.0324(7) 0.0158(7) 0.0265(6) -0.0004(6) 0.0084(6) -0.0010(6) C2 0.0269(7) 0.0189(7) 0.0272(7) 0.0036(6) 0.0061(6) -0.0022(6) C3 0.0261(7) 0.0203(7) 0.0262(6) 0.0053(6) 0.0073(6) -0.0002(6) C4 0.0282(7) 0.0245(8) 0.0264(7) 0.0052(6) 0.0061(6) 0.0008(6) C5 0.0247(7) 0.0317(9) 0.0315(7) 0.0076(7) 0.0051(6) 0.0007(7) C6 0.0305(8) 0.0258(8) 0.0274(7) 0.0040(6) 0.0057(6) -0.0049(6) C7 0.0309(8) 0.0222(8) 0.0279(7) 0.0009(6) 0.0070(6) -0.0039(6) C8 0.0285(8) 0.0352(9) 0.0317(7) 0.0012(7) 0.0065(6) 0.0075(7) C9 0.0423(10) 0.0325(10) 0.0589(11) -0.0060(9) 0.0114(9) 0.0097(8) C10 0.0459(10) 0.0617(13) 0.0310(8) 0.0047(8) 0.0135(7) 0.0190(9) C11 0.0311(8) 0.0531(12) 0.0404(9) -0.0030(9) 0.0068(7) 0.0128(8) C12 0.0302(8) 0.0359(9) 0.0284(7) 0.0044(7) 0.0013(6) -0.0060(7) C13 0.0454(10) 0.0496(12) 0.0332(9) -0.0096(8) -0.0035(8) -0.0029(9) C14 0.0473(11) 0.0481(12) 0.0343(9) 0.0069(8) -0.0003(8) -0.0025(9) C15 0.0396(9) 0.0575(12) 0.0371(9) -0.0002(9) 0.0044(8) -0.0194(9) C16 0.0267(7) 0.0211(7) 0.0362(7) -0.0048(6) 0.0085(6) 0.0013(6) C17 0.0287(7) 0.0276(8) 0.0290(7) -0.0047(6) 0.0108(6) -0.0013(6) C18 0.0269(7) 0.0287(8) 0.0275(7) -0.0008(6) 0.0084(6) -0.0050(6) C19 0.0248(7) 0.0234(8) 0.0287(7) -0.0031(6) 0.0059(6) 0.0007(6) C20 0.0289(7) 0.0194(7) 0.0237(6) 0.0005(6) 0.0043(6) 0.0020(6) C21 0.0295(8) 0.0276(8) 0.0274(7) 0.0007(6) 0.0037(6) 0.0054(7) C22 0.0389(9) 0.0266(8) 0.0243(7) 0.0035(6) 0.0031(6) 0.0060(7) C23 0.0416(8) 0.0256(8) 0.0243(7) 0.0041(6) 0.0099(6) 0.0003(7) C24 0.0300(7) 0.0199(7) 0.0264(7) 0.0013(6) 0.0075(6) -0.0007(6) C25 0.0302(7) 0.0133(7) 0.0239(6) 0.0004(5) 0.0052(6) 0.0005(6) C26 0.0460(10) 0.0479(11) 0.0244(7) 0.0079(7) 0.0032(7) 0.0138(9) C27 0.0805(15) 0.0500(12) 0.0386(10) 0.0189(9) 0.0067(10) 0.0183(11) C28 0.0611(13) 0.0672(14) 0.0278(8) -0.0018(9) -0.0010(9) 0.0141(11) C29 0.0466(11) 0.0927(17) 0.0335(9) 0.0164(11) -0.0005(8) 0.0234(12) C30 0.0300(8) 0.0381(9) 0.0300(7) 0.0052(7) 0.0107(6) -0.0018(7) C31 0.0406(9) 0.0714(14) 0.0343(8) 0.0111(9) 0.0166(7) -0.0019(10) C32 0.0330(8) 0.0440(10) 0.0356(8) 0.0076(8) 0.0079(7) -0.0091(8) C33 0.0352(8) 0.0415(10) 0.0365(8) -0.0018(8) 0.0116(7) 0.0089(8) C34 0.0270(7) 0.0181(7) 0.0194(6) 0.0000(5) 0.0088(5) 0.0003(6) C35 0.0255(7) 0.0189(7) 0.0193(6) 0.0017(5) 0.0069(5) 0.0001(6) C36 0.0253(7) 0.0197(7) 0.0188(6) 0.0020(5) 0.0076(5) 0.0000(6) C37 0.0261(7) 0.0244(8) 0.0264(6) 0.0012(6) 0.0106(5) -0.0006(6) C38 0.0212(7) 0.0300(8) 0.0305(7) 0.0023(6) 0.0077(6) -0.0023(6) C39 0.0295(7) 0.0240(8) 0.0230(6) 0.0009(6) 0.0064(6) -0.0051(6) C40 0.0291(7) 0.0210(7) 0.0204(6) -0.0005(6) 0.0087(5) -0.0012(6) C41 0.0275(7) 0.0388(9) 0.0352(7) -0.0062(7) 0.0131(6) 0.0025(7) C42 0.0339(8) 0.0342(9) 0.0488(9) -0.0114(8) 0.0105(7) 0.0072(7) C43 0.0301(8) 0.0589(13) 0.0611(11) -0.0194(10) 0.0199(8) 0.0003(9) C44 0.0477(9) 0.0708(14) 0.0376(8) -0.0008(9) 0.0270(7) 0.0088(10) C45 0.0296(8) 0.0340(9) 0.0281(7) -0.0047(7) 0.0051(6) -0.0082(7) C46 0.0447(10) 0.0462(11) 0.0462(9) -0.0095(8) 0.0145(8) -0.0235(9) C47 0.0411(9) 0.0335(9) 0.0268(7) -0.0086(7) 0.0045(7) -0.0067(7) C48 0.0335(9) 0.0575(12) 0.0315(8) -0.0046(8) 0.0000(7) -0.0008(9) C49 0.0234(7) 0.0267(8) 0.0249(6) -0.0030(6) 0.0085(5) 0.0014(6) C50 0.0271(7) 0.0234(8) 0.0304(7) -0.0016(6) 0.0047(6) 0.0065(6) C51 0.0284(7) 0.0202(7) 0.0280(7) 0.0019(6) 0.0010(6) 0.0035(6) C52 0.0257(7) 0.0242(8) 0.0202(6) 0.0012(6) 0.0056(5) 0.0001(6) C53 0.0287(7) 0.0209(7) 0.0211(6) -0.0014(5) 0.0091(5) -0.0034(6) C54 0.0269(7) 0.0296(8) 0.0255(6) -0.0042(6) 0.0087(6) -0.0045(6) C55 0.0343(8) 0.0251(8) 0.0313(7) -0.0072(6) 0.0151(6) -0.0082(6) C56 0.0374(8) 0.0183(7) 0.0331(7) -0.0047(6) 0.0168(6) -0.0041(6) C57 0.0331(7) 0.0200(7) 0.0241(6) -0.0012(6) 0.0127(6) -0.0014(6) C58 0.0304(7) 0.0178(7) 0.0201(6) -0.0008(5) 0.0117(5) -0.0034(6) C59 0.0358(8) 0.0313(9) 0.0427(8) -0.0151(7) 0.0139(7) -0.0126(7) C60 0.0530(13) 0.0556(13) 0.1016(18) -0.0462(13) 0.0075(12) -0.0104(11) C61 0.0709(14) 0.0669(15) 0.0486(11) -0.0144(11) 0.0050(11) -0.0272(12) C62 0.0569(12) 0.0717(15) 0.0693(13) -0.0298(11) 0.0289(10) -0.0314(11) C63 0.0400(8) 0.0176(7) 0.0312(7) -0.0023(6) 0.0086(6) 0.0032(7) C64 0.0526(11) 0.0216(8) 0.0465(10) -0.0018(8) 0.0057(8) 0.0076(8) C65 0.0551(11) 0.0289(9) 0.0279(7) 0.0023(7) 0.0053(7) 0.0114(8) C66 0.0336(8) 0.0299(9) 0.0390(8) -0.0047(7) 0.0073(7) 0.0056(7) C67 0.0244(7) 0.0255(8) 0.0237(6) -0.0033(6) 0.0017(6) -0.0021(6) C68 0.0288(7) 0.0197(7) 0.0229(6) -0.0008(6) 0.0026(6) 0.0007(6) C69 0.0277(7) 0.0185(7) 0.0193(6) -0.0020(5) 0.0056(5) 0.0021(6) C70 0.0318(7) 0.0193(7) 0.0233(6) -0.0018(6) 0.0092(5) 0.0004(6) C71 0.0400(8) 0.0190(7) 0.0275(7) 0.0020(6) 0.0118(6) 0.0031(6) C77 0.0411(9) 0.0229(8) 0.0547(10) 0.0030(8) 0.0145(8) -0.0042(7) C72 0.0358(8) 0.0266(8) 0.0237(7) 0.0021(6) 0.0033(6) 0.0061(7) C73 0.0289(8) 0.0287(8) 0.0252(7) -0.0006(6) -0.0002(6) 0.0026(7) C74 0.0320(7) 0.0184(7) 0.0324(7) -0.0009(6) 0.0112(6) -0.0019(6) C75 0.0344(8) 0.0263(8) 0.0474(9) 0.0005(7) 0.0201(7) -0.0017(7) C76 0.0384(9) 0.0323(9) 0.0349(8) -0.0090(7) 0.0073(7) -0.0093(7) C78 0.0393(9) 0.0273(8) 0.0308(8) 0.0043(7) 0.0012(7) 0.0082(7) C79 0.0547(11) 0.0415(11) 0.0310(8) 0.0100(8) 0.0041(8) 0.0113(9) C80 0.0510(11) 0.0315(9) 0.0421(9) 0.0057(8) 0.0023(8) 0.0126(8) C81 0.0411(10) 0.0385(10) 0.0423(9) 0.0080(8) -0.0022(8) 0.0099(8) C82 0.0267(7) 0.0228(8) 0.0298(7) 0.0002(6) 0.0051(6) -0.0056(6) C83 0.0306(7) 0.0260(8) 0.0273(7) 0.0018(6) 0.0082(6) -0.0054(6) C84 0.0243(7) 0.0243(8) 0.0231(6) 0.0000(6) 0.0083(5) 0.0011(6) C85 0.0278(7) 0.0165(7) 0.0176(5) -0.0009(5) 0.0086(5) 0.0013(6) C86 0.0247(7) 0.0185(7) 0.0184(6) -0.0021(5) 0.0063(5) -0.0004(6) C87 0.0289(7) 0.0253(8) 0.0172(6) 0.0001(5) 0.0076(5) 0.0023(6) C88 0.0276(7) 0.0258(8) 0.0197(6) 0.0026(6) 0.0047(5) 0.0036(6) C89 0.0232(7) 0.0270(8) 0.0224(6) -0.0008(6) 0.0065(5) 0.0033(6) C90 0.0260(7) 0.0251(8) 0.0188(6) -0.0018(6) 0.0068(5) 0.0001(6) C91 0.0256(7) 0.0183(7) 0.0177(6) -0.0003(5) 0.0050(5) -0.0001(6) C92 0.0296(8) 0.0508(11) 0.0218(7) 0.0105(7) 0.0054(6) 0.0113(8) C93 0.0444(11) 0.0875(17) 0.0232(8) -0.0044(10) -0.0044(8) 0.0153(11) C94 0.0481(11) 0.0707(14) 0.0456(9) 0.0332(10) 0.0162(8) 0.0191(10) C95 0.0354(9) 0.0798(15) 0.0329(8) 0.0227(9) 0.0104(7) 0.0245(10) C96 0.0262(7) 0.0491(10) 0.0201(6) 0.0021(7) 0.0090(5) 0.0005(7) C97 0.0346(9) 0.0716(14) 0.0263(7) -0.0117(8) 0.0117(6) -0.0015(9) C98 0.0290(8) 0.0715(14) 0.0256(7) 0.0018(8) 0.0109(6) 0.0060(9) C99 0.0366(9) 0.0631(13) 0.0376(8) 0.0197(9) 0.0138(7) -0.0009(9) C100 0.0211(6) 0.0159(7) 0.0176(6) 0.0005(5) 0.0034(5) 0.0004(5) C101 0.0222(6) 0.0152(6) 0.0174(6) -0.0004(5) 0.0025(5) 0.0007(5) C102 0.0278(7) 0.0157(7) 0.0172(6) -0.0002(5) 0.0043(5) 0.0006(5) C103 0.0209(6) 0.0177(7) 0.0189(6) -0.0008(5) 0.0024(5) 0.0004(5) C104 0.0234(7) 0.0192(7) 0.0193(6) 0.0002(5) 0.0039(5) -0.0009(6) N200 0.0858(16) 0.0756(16) 0.167(2) -0.0574(16) 0.0483(16) -0.0152(14) C200 0.0821(16) 0.0405(12) 0.0889(16) -0.0255(12) 0.0343(13) -0.0127(12) C201 0.0886(17) 0.0318(11) 0.0585(13) -0.0098(10) 0.0022(12) 0.0036(11) N201 0.0863(14) 0.0987(18) 0.0529(10) -0.0109(11) 0.0264(10) 0.0089(14) C202 0.0598(12) 0.0579(13) 0.0284(8) 0.0016(9) 0.0097(8) -0.0106(11) C203 0.0552(11) 0.0353(10) 0.0342(8) 0.0051(8) 0.0060(8) -0.0119(9) N202 0.199(4) 0.113(5) 0.213(5) -0.061(4) 0.164(4) -0.021(4) C205 0.171(8) 0.340(12) 0.203(9) -0.170(8) -0.025(7) 0.132(9) C204 0.083(3) 0.223(8) 0.304(11) 0.150(8) 0.102(5) 0.108(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Fe1 O2 92.07(5) . . ? O1 Fe1 O9 98.29(5) . . ? O2 Fe1 O9 87.26(5) . . ? O1 Fe1 O7 93.76(5) . . ? O2 Fe1 O7 173.56(4) . . ? O9 Fe1 O7 89.19(4) . . ? O1 Fe1 N2 167.60(5) . . ? O2 Fe1 N2 85.83(5) . . ? O9 Fe1 N2 93.82(5) . . ? O7 Fe1 N2 89.05(5) . . ? O1 Fe1 N1 86.65(5) . . ? O2 Fe1 N1 101.09(5) . . ? O9 Fe1 N1 170.19(5) . . ? O7 Fe1 N1 82.00(5) . . ? N2 Fe1 N1 81.78(5) . . ? O3 Fe2 O4 90.56(4) . . ? O3 Fe2 N7 98.46(5) . . ? O4 Fe2 N7 94.74(5) . . ? O3 Fe2 O8 96.64(4) . . ? O4 Fe2 O8 169.39(4) . . ? N7 Fe2 O8 76.54(4) . . ? O3 Fe2 N3 86.23(4) . . ? O4 Fe2 N3 107.66(5) . . ? N7 Fe2 N3 157.12(5) . . ? O8 Fe2 N3 80.68(4) . . ? O3 Fe2 N4 168.41(5) . . ? O4 Fe2 N4 84.81(5) . . ? N7 Fe2 N4 92.52(5) . . ? O8 Fe2 N4 89.50(4) . . ? N3 Fe2 N4 85.07(5) . . ? O6 Fe3 O5 94.65(4) . . ? O6 Fe3 N6 88.08(4) . . ? O5 Fe3 N6 104.05(5) . . ? O6 Fe3 N8 93.38(5) . . ? O5 Fe3 N8 94.64(5) . . ? N6 Fe3 N8 161.08(5) . . ? O6 Fe3 O10 93.67(4) . . ? O5 Fe3 O10 168.51(4) . . ? N6 Fe3 O10 84.12(4) . . ? N8 Fe3 O10 76.96(4) . . ? O6 Fe3 N5 173.36(4) . . ? O5 Fe3 N5 86.25(5) . . ? N6 Fe3 N5 85.32(5) . . ? N8 Fe3 N5 93.10(5) . . ? O10 Fe3 N5 86.40(4) . . ? C1 N1 C16 115.99(13) . . ? C1 N1 Fe1 123.85(11) . . ? C16 N1 Fe1 119.80(9) . . ? C19 N2 C18 116.27(13) . . ? C19 N2 Fe1 124.41(11) . . ? C18 N2 Fe1 119.05(9) . . ? C34 N3 C49 117.17(12) . . ? C34 N3 Fe2 122.48(10) . . ? C49 N3 Fe2 119.06(8) . . ? C52 N4 C51 117.07(12) . . ? C52 N4 Fe2 123.47(10) . . ? C51 N4 Fe2 119.37(9) . . ? C67 N5 C82 117.62(13) . . ? C67 N5 Fe3 121.96(11) . . ? C82 N5 Fe3 120.35(9) . . ? C85 N6 C84 117.43(12) . . ? C85 N6 Fe3 123.58(10) . . ? C84 N6 Fe3 118.60(8) . . ? C102 N7 C100 105.19(12) . . ? C102 N7 Fe2 141.42(10) . . ? C100 N7 Fe2 113.10(9) . . ? C102 N8 C101 105.41(12) . . ? C102 N8 Fe3 141.08(10) . . ? C101 N8 Fe3 112.83(9) . . ? C3 O1 Fe1 137.23(10) . . ? C25 O2 Fe1 134.00(10) . . ? C36 O3 Fe2 132.80(10) . . ? C58 O4 Fe2 134.46(9) . . ? C69 O5 Fe3 131.54(9) . . ? C91 O6 Fe3 133.45(10) . . ? C103 O7 Fe1 147.42(10) . . ? C103 O8 Fe2 118.23(9) . . ? C104 O9 Fe1 147.39(9) . . ? C104 O10 Fe3 118.30(9) . . ? N1 C1 C2 128.13(14) . . ? C7 C2 C3 120.62(14) . . ? C7 C2 C1 116.21(14) . . ? C3 C2 C1 123.03(13) . . ? O1 C3 C2 121.01(13) . . ? O1 C3 C4 120.63(14) . . ? C2 C3 C4 118.36(13) . . ? C5 C4 C3 117.78(15) . . ? C5 C4 C8 122.27(14) . . ? C3 C4 C8 119.95(13) . . ? C4 C5 C6 124.77(15) . . ? C7 C6 C5 116.55(14) . . ? C7 C6 C12 122.97(15) . . ? C5 C6 C12 120.46(14) . . ? C6 C7 C2 121.84(15) . . ? C9 C8 C4 110.61(15) . . ? C9 C8 C10 109.97(15) . . ? C4 C8 C10 109.39(14) . . ? C9 C8 C11 107.26(15) . . ? C4 C8 C11 112.38(14) . . ? C10 C8 C11 107.15(15) . . ? C15 C12 C13 108.74(16) . . ? C15 C12 C14 109.27(15) . . ? C13 C12 C14 107.19(15) . . ? C15 C12 C6 110.38(14) . . ? C13 C12 C6 112.75(14) . . ? C14 C12 C6 108.41(14) . . ? N1 C16 C17 112.18(13) . . ? C16 C17 C18 113.50(13) . . ? N2 C18 C17 111.03(12) . . ? N2 C19 C20 127.31(14) . . ? C25 C20 C21 120.61(14) . . ? C25 C20 C19 122.56(13) . . ? C21 C20 C19 116.83(14) . . ? C22 C21 C20 121.46(15) . . ? C21 C22 C23 116.99(14) . . ? C21 C22 C26 122.93(16) . . ? C23 C22 C26 120.07(15) . . ? C24 C23 C22 124.64(15) . . ? C23 C24 C25 117.54(15) . . ? C23 C24 C30 122.39(14) . . ? C25 C24 C30 120.00(13) . . ? O2 C25 C20 120.71(14) . . ? O2 C25 C24 120.70(14) . . ? C20 C25 C24 118.57(13) . . ? C29 C26 C22 111.33(16) . . ? C29 C26 C28 109.10(17) . . ? C22 C26 C28 109.47(16) . . ? C29 C26 C27 108.60(18) . . ? C22 C26 C27 109.72(16) . . ? C28 C26 C27 108.57(17) . . ? C24 C30 C31 111.72(13) . . ? C24 C30 C32 110.49(14) . . ? C31 C30 C32 107.29(15) . . ? C24 C30 C33 108.15(14) . . ? C31 C30 C33 108.34(16) . . ? C32 C30 C33 110.85(14) . . ? N3 C34 C35 127.81(13) . . ? C40 C35 C36 120.11(13) . . ? C40 C35 C34 117.29(13) . . ? C36 C35 C34 122.59(12) . . ? O3 C36 C35 120.57(13) . . ? O3 C36 C37 120.46(13) . . ? C35 C36 C37 118.94(13) . . ? C38 C37 C36 117.61(14) . . ? C38 C37 C41 121.92(14) . . ? C36 C37 C41 120.47(13) . . ? C37 C38 C39 124.68(14) . . ? C40 C39 C38 116.88(13) . . ? C40 C39 C45 123.84(14) . . ? C38 C39 C45 119.27(14) . . ? C39 C40 C35 121.75(14) . . ? C42 C41 C43 107.60(15) . . ? C42 C41 C44 110.35(15) . . ? C43 C41 C44 107.43(15) . . ? C42 C41 C37 109.11(14) . . ? C43 C41 C37 111.73(14) . . ? C44 C41 C37 110.58(14) . . ? C47 C45 C39 111.48(13) . . ? C47 C45 C48 109.09(14) . . ? C39 C45 C48 109.89(15) . . ? C47 C45 C46 108.19(15) . . ? C39 C45 C46 108.56(13) . . ? C48 C45 C46 109.59(15) . . ? N3 C49 C50 111.24(12) . . ? C49 C50 C51 115.68(13) . . ? N4 C51 C50 112.38(12) . . ? N4 C52 C53 127.35(14) . . ? C54 C53 C58 120.31(14) . . ? C54 C53 C52 117.40(13) . . ? C58 C53 C52 121.98(13) . . ? C55 C54 C53 121.68(14) . . ? C54 C55 C56 116.86(14) . . ? C54 C55 C59 121.22(14) . . ? C56 C55 C59 121.89(15) . . ? C57 C56 C55 124.42(15) . . ? C56 C57 C58 117.70(14) . . ? C56 C57 C63 122.20(14) . . ? C58 C57 C63 120.09(13) . . ? O4 C58 C53 120.81(13) . . ? O4 C58 C57 120.18(13) . . ? C53 C58 C57 119.00(13) . . ? C60 C59 C62 111.88(19) . . ? C60 C59 C55 112.58(16) . . ? C62 C59 C55 109.49(15) . . ? C60 C59 C61 105.70(18) . . ? C62 C59 C61 107.61(17) . . ? C55 C59 C61 109.39(15) . . ? C64 C63 C66 107.18(15) . . ? C64 C63 C57 112.06(14) . . ? C66 C63 C57 109.45(13) . . ? C64 C63 C65 107.18(14) . . ? C66 C63 C65 110.31(14) . . ? C57 C63 C65 110.60(14) . . ? N5 C67 C68 127.42(14) . . ? C73 C68 C69 120.06(14) . . ? C73 C68 C67 117.12(14) . . ? C69 C68 C67 122.37(13) . . ? O5 C69 C68 120.90(13) . . ? O5 C69 C70 119.94(13) . . ? C68 C69 C70 119.11(13) . . ? C71 C70 C69 117.28(14) . . ? C71 C70 C74 121.91(14) . . ? C69 C70 C74 120.77(13) . . ? C70 C71 C72 124.55(15) . . ? C73 C72 C71 117.25(14) . . ? C73 C72 C78 123.37(15) . . ? C71 C72 C78 119.36(15) . . ? C72 C73 C68 121.72(15) . . ? C70 C74 C77 111.94(13) . . ? C70 C74 C75 110.55(13) . . ? C77 C74 C75 107.58(14) . . ? C70 C74 C76 109.50(13) . . ? C77 C74 C76 107.83(14) . . ? C75 C74 C76 109.36(13) . . ? C81 C78 C79 108.08(15) . . ? C81 C78 C80 107.83(16) . . ? C79 C78 C80 110.16(16) . . ? C81 C78 C72 111.50(15) . . ? C79 C78 C72 108.01(15) . . ? C80 C78 C72 111.23(14) . . ? N5 C82 C83 111.58(12) . . ? C84 C83 C82 114.94(13) . . ? N6 C84 C83 110.65(12) . . ? N6 C85 C86 127.70(13) . . ? C87 C86 C91 120.06(13) . . ? C87 C86 C85 116.77(13) . . ? C91 C86 C85 122.92(12) . . ? C88 C87 C86 121.63(13) . . ? C87 C88 C89 117.29(13) . . ? C87 C88 C92 120.95(13) . . ? C89 C88 C92 121.77(14) . . ? C90 C89 C88 124.01(14) . . ? C89 C90 C91 117.99(13) . . ? C89 C90 C96 120.87(13) . . ? C91 C90 C96 121.10(12) . . ? O6 C91 C90 120.59(13) . . ? O6 C91 C86 120.43(13) . . ? C90 C91 C86 118.98(12) . . ? C95 C92 C93 107.80(16) . . ? C95 C92 C94 108.71(17) . . ? C93 C92 C94 109.17(16) . . ? C95 C92 C88 112.35(13) . . ? C93 C92 C88 108.48(15) . . ? C94 C92 C88 110.26(14) . . ? C99 C96 C98 107.28(15) . . ? C99 C96 C97 110.03(14) . . ? C98 C96 C97 107.51(15) . . ? C99 C96 C90 110.33(15) . . ? C98 C96 C90 112.12(12) . . ? C97 C96 C90 109.52(14) . . ? N7 C100 C101 108.30(12) . . ? N7 C100 C103 117.09(12) . . ? C101 C100 C103 134.60(13) . . ? N8 C101 C100 108.08(12) . . ? N8 C101 C104 117.16(12) . . ? C100 C101 C104 134.45(13) . . ? N7 C102 N8 113.02(13) . . ? O7 C103 O8 123.01(13) . . ? O7 C103 C100 122.08(13) . . ? O8 C103 C100 114.91(13) . . ? O9 C104 O10 122.59(13) . . ? O9 C104 C101 122.67(13) . . ? O10 C104 C101 114.71(13) . . ? N200 C200 C201 177.5(3) . . ? N201 C202 C203 178.7(3) . . ? C205 C204 N202 172.7(9) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O1 1.8965(11) . ? Fe1 O2 1.9093(10) . ? Fe1 O9 2.0158(11) . ? Fe1 O7 2.0775(11) . ? Fe1 N2 2.1271(13) . ? Fe1 N1 2.1463(13) . ? Fe2 O3 1.8992(10) . ? Fe2 O4 1.9012(11) . ? Fe2 N7 2.1142(12) . ? Fe2 O8 2.1171(11) . ? Fe2 N3 2.1220(12) . ? Fe2 N4 2.1402(13) . ? Fe3 O6 1.8910(10) . ? Fe3 O5 1.8952(11) . ? Fe3 N6 2.1013(12) . ? Fe3 N8 2.1070(12) . ? Fe3 O10 2.1070(11) . ? Fe3 N5 2.1206(13) . ? N1 C1 1.2827(19) . ? N1 C16 1.468(2) . ? N2 C19 1.2840(19) . ? N2 C18 1.467(2) . ? N3 C34 1.2830(17) . ? N3 C49 1.4635(19) . ? N4 C52 1.2863(19) . ? N4 C51 1.473(2) . ? N5 C67 1.2826(19) . ? N5 C82 1.470(2) . ? N6 C85 1.2802(17) . ? N6 C84 1.4706(19) . ? N7 C102 1.3344(18) . ? N7 C100 1.3715(18) . ? N8 C102 1.3378(18) . ? N8 C101 1.3678(19) . ? O1 C3 1.3081(17) . ? O2 C25 1.3084(17) . ? O3 C36 1.3088(17) . ? O4 C58 1.3159(17) . ? O5 C69 1.3146(17) . ? O6 C91 1.3102(16) . ? O7 C103 1.2507(18) . ? O8 C103 1.2705(17) . ? O9 C104 1.2504(18) . ? O10 C104 1.2636(17) . ? C1 C2 1.440(2) . ? C2 C7 1.404(2) . ? C2 C3 1.413(2) . ? C3 C4 1.425(2) . ? C4 C5 1.382(2) . ? C4 C8 1.530(2) . ? C5 C6 1.403(2) . ? C6 C7 1.372(2) . ? C6 C12 1.532(2) . ? C8 C9 1.529(3) . ? C8 C10 1.535(2) . ? C8 C11 1.538(2) . ? C12 C15 1.523(3) . ? C12 C13 1.525(3) . ? C12 C14 1.528(3) . ? C16 C17 1.521(2) . ? C17 C18 1.540(2) . ? C19 C20 1.442(2) . ? C20 C25 1.403(2) . ? C20 C21 1.411(2) . ? C21 C22 1.369(2) . ? C22 C23 1.402(2) . ? C22 C26 1.528(2) . ? C23 C24 1.380(2) . ? C24 C25 1.431(2) . ? C24 C30 1.527(2) . ? C26 C29 1.527(3) . ? C26 C28 1.535(3) . ? C26 C27 1.537(3) . ? C30 C31 1.536(2) . ? C30 C32 1.537(2) . ? C30 C33 1.539(3) . ? C34 C35 1.438(2) . ? C35 C40 1.4076(19) . ? C35 C36 1.416(2) . ? C36 C37 1.426(2) . ? C37 C38 1.376(2) . ? C37 C41 1.537(2) . ? C38 C39 1.408(2) . ? C39 C40 1.371(2) . ? C39 C45 1.528(2) . ? C41 C42 1.527(3) . ? C41 C43 1.530(2) . ? C41 C44 1.531(2) . ? C45 C47 1.521(2) . ? C45 C48 1.531(2) . ? C45 C46 1.537(3) . ? C49 C50 1.526(2) . ? C50 C51 1.535(2) . ? C52 C53 1.446(2) . ? C53 C54 1.406(2) . ? C53 C58 1.408(2) . ? C54 C55 1.376(2) . ? C55 C56 1.399(2) . ? C55 C59 1.543(2) . ? C56 C57 1.388(2) . ? C57 C58 1.419(2) . ? C57 C63 1.532(2) . ? C59 C60 1.492(3) . ? C59 C62 1.511(3) . ? C59 C61 1.550(3) . ? C63 C64 1.529(2) . ? C63 C66 1.529(3) . ? C63 C65 1.538(2) . ? C67 C68 1.444(2) . ? C68 C73 1.405(2) . ? C68 C69 1.410(2) . ? C69 C70 1.426(2) . ? C70 C71 1.384(2) . ? C70 C74 1.523(2) . ? C71 C72 1.396(2) . ? C77 C74 1.531(2) . ? C72 C73 1.368(2) . ? C72 C78 1.534(2) . ? C74 C75 1.535(2) . ? C74 C76 1.543(2) . ? C78 C81 1.528(3) . ? C78 C79 1.528(3) . ? C78 C80 1.531(3) . ? C82 C83 1.534(2) . ? C83 C84 1.525(2) . ? C85 C86 1.445(2) . ? C86 C87 1.4005(19) . ? C86 C91 1.418(2) . ? C87 C88 1.373(2) . ? C88 C89 1.400(2) . ? C88 C92 1.530(2) . ? C89 C90 1.3845(19) . ? C90 C91 1.413(2) . ? C90 C96 1.539(2) . ? C92 C95 1.515(2) . ? C92 C93 1.528(3) . ? C92 C94 1.529(3) . ? C96 C99 1.525(3) . ? C96 C98 1.529(2) . ? C96 C97 1.537(2) . ? C100 C101 1.3733(19) . ? C100 C103 1.459(2) . ? C101 C104 1.469(2) . ? N200 C200 1.150(4) . ? C200 C201 1.449(4) . ? N201 C202 1.134(3) . ? C202 C203 1.445(3) . ? N202 C204 1.636(13) . ? C205 C204 1.359(15) . ?
1100759.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100759.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100759 loop_ _publ_author_name 'Ji-Min Zheng' 'Stuart R. Batten' 'Miao Du' _publ_contact_author ; Miao Du College of Chemistry and Life Science, Tianjin Normal University, Tianjin 300074,China ; _publ_contact_author_email dumiao@public.tpt.tj.cn _publ_section_title ; A Unique Cyanide-Bridged Three-Dimensional (3-D) Copper(II)-Copper(I) Mixed-Valence Polymer Containing 1-D Water Tapes with Cyclic Pentamer Units ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3371 _journal_page_last 3373 _journal_paper_doi 10.1021/ic0483491 _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C4 H10 Cu3 N4 O5' _chemical_formula_weight 384.78 _chemical_name_systematic ; ? ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 111.979(4) _cell_angle_beta 96.879(5) _cell_angle_gamma 106.678(5) _cell_formula_units_Z 2 _cell_length_a 6.720(2) _cell_length_b 9.494(3) _cell_length_c 10.682(3) _cell_measurement_reflns_used 988 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 26.33 _cell_measurement_theta_min 3.82 _cell_volume 585.3(3) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0201 _diffrn_reflns_av_sigmaI/netI 0.0369 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 3023 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_min 2.48 _exptl_absorpt_coefficient_mu 5.411 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_correction_T_min 0.540125 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour Green _exptl_crystal_density_diffrn 2.183 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Block _exptl_crystal_F_000 378 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _refine_diff_density_max 0.926 _refine_diff_density_min -0.652 _refine_diff_density_rms 0.141 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 145 _refine_ls_number_reflns 2041 _refine_ls_number_restraints 9 _refine_ls_restrained_S_all 1.070 _refine_ls_R_factor_all 0.0461 _refine_ls_R_factor_gt 0.0387 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0613P)^2^+1.4445P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1041 _refine_ls_wR_factor_ref 0.1094 _reflns_number_gt 1764 _reflns_number_total 2041 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic0483491si20050210_055704.cif _cod_data_source_block 1 _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. '_exptl_absorpt_correction_type' value 'MULTI-SCAN' changed to 'multi-scan' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_database_code 1100759 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.16819(10) 0.39624(7) 0.29210(6) 0.0222(2) Uani 1 1 d . . . Cu2 Cu 0.01050(10) 0.14908(8) -0.23073(6) 0.0248(2) Uani 1 1 d . . . Cu3 Cu -0.35954(10) 0.03642(7) -0.39001(6) 0.0226(2) Uani 1 1 d . . . N1 N 0.1442(9) 0.7226(7) 0.3098(5) 0.0332(12) Uani 0.50 1 d P . . N2 N 0.2755(9) 0.1163(7) 0.3314(5) 0.0339(12) Uani 0.50 1 d P . . N3 N 0.0559(9) 0.2325(7) -0.0314(6) 0.0349(12) Uani 0.50 1 d P . . N4 N 0.2235(7) 0.0886(6) -0.3278(5) 0.0204(10) Uani 0.50 1 d P . . C1' C 0.1442(9) 0.7226(7) 0.3098(5) 0.0332(12) Uani 0.50 1 d P . . C2' C 0.2755(9) 0.1163(7) 0.3314(5) 0.0339(12) Uani 0.50 1 d P . . C3' C 0.0559(9) 0.2325(7) -0.0314(6) 0.0349(12) Uani 0.50 1 d P . . C4' C 0.2235(7) 0.0886(6) -0.3278(5) 0.0204(10) Uani 0.50 1 d P . . C1 C 0.1189(8) 0.5948(5) 0.2972(5) 0.0210(10) Uani 0.50 1 d P . . C2 C 0.2477(8) 0.2178(5) 0.3092(5) 0.0198(9) Uani 0.50 1 d P . . C3 C 0.0919(8) 0.2891(6) 0.0878(5) 0.0229(10) Uani 0.50 1 d P . . C4 C 0.3521(9) 0.0568(6) -0.3800(6) 0.0322(12) Uani 0.50 1 d P . . N1' N 0.1189(8) 0.5948(5) 0.2972(5) 0.0210(10) Uani 0.50 1 d P . . N2' N 0.2477(8) 0.2178(5) 0.3092(5) 0.0198(9) Uani 0.50 1 d P . . N3' N 0.0919(8) 0.2891(6) 0.0878(5) 0.0229(10) Uani 0.50 1 d P . . N4' N 0.3521(9) 0.0568(6) -0.3800(6) 0.0322(12) Uani 0.50 1 d P . . O1 O 0.2451(8) 0.5033(6) 0.4958(4) 0.0451(11) Uani 1 1 d . . . H1A H 0.3726 0.5690 0.5403 0.068 Uiso 1 1 d R . . H1B H 0.1513 0.4845 0.5401 0.068 Uiso 1 1 d R . . O2 O -0.1906(7) 0.2482(5) 0.2959(5) 0.0438(11) Uani 1 1 d . . . H2A H -0.2070 0.1911 0.3417 0.066 Uiso 1 1 d R . . H2B H -0.2996 0.2538 0.2515 0.066 Uiso 1 1 d R . . O3 O 0.5561(7) 0.5464(5) 0.2965(5) 0.0458(11) Uani 1 1 d D . . H3A H 0.6744 0.5898 0.3590 0.069 Uiso 1 1 d RD . . H3B H 0.5560 0.5299 0.2123 0.069 Uiso 1 1 d RD . . O4 O 0.4894(13) 0.1444(11) 0.0628(9) 0.111(3) Uani 1 1 d D . . H4A H 0.5212 0.0590 0.0211 0.166 Uiso 1 1 d RD . . H4B H 0.3488 0.1343 0.0313 0.166 Uiso 1 1 d RD . . O5 O 0.6362(13) 0.4152(11) 0.0289(8) 0.113(3) Uani 1 1 d D . . H5B H 0.6142 0.3252 0.0360 0.169 Uiso 1 1 d RD . . H5A H 0.5412 0.4606 0.0444 0.169 Uiso 1 1 d RD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0381(4) 0.0166(3) 0.0174(3) 0.0094(3) 0.0064(3) 0.0150(3) Cu2 0.0295(4) 0.0294(4) 0.0188(3) 0.0093(3) 0.0092(3) 0.0154(3) Cu3 0.0252(4) 0.0213(4) 0.0292(4) 0.0151(3) 0.0083(3) 0.0132(3) N1 0.040(3) 0.041(3) 0.029(3) 0.018(2) 0.016(2) 0.022(3) N2 0.036(3) 0.036(3) 0.029(3) 0.012(2) 0.011(2) 0.013(3) N3 0.033(3) 0.034(3) 0.044(3) 0.020(3) 0.012(2) 0.016(2) N4 0.021(2) 0.026(2) 0.024(2) 0.013(2) 0.015(2) 0.016(2) C1' 0.040(3) 0.041(3) 0.029(3) 0.018(2) 0.016(2) 0.022(3) C2' 0.036(3) 0.036(3) 0.029(3) 0.012(2) 0.011(2) 0.013(3) C3' 0.033(3) 0.034(3) 0.044(3) 0.020(3) 0.012(2) 0.016(2) C4' 0.021(2) 0.026(2) 0.024(2) 0.013(2) 0.015(2) 0.016(2) C1 0.033(3) 0.009(2) 0.026(2) 0.0109(19) 0.005(2) 0.0106(19) C2 0.033(3) 0.013(2) 0.026(2) 0.0154(19) 0.009(2) 0.016(2) C3 0.040(3) 0.020(2) 0.010(2) 0.0066(18) 0.007(2) 0.014(2) C4 0.037(3) 0.024(3) 0.042(3) 0.017(2) 0.012(3) 0.013(2) N1' 0.033(3) 0.009(2) 0.026(2) 0.0109(19) 0.005(2) 0.0106(19) N2' 0.033(3) 0.013(2) 0.026(2) 0.0154(19) 0.009(2) 0.016(2) N3' 0.040(3) 0.020(2) 0.010(2) 0.0066(18) 0.007(2) 0.014(2) N4' 0.037(3) 0.024(3) 0.042(3) 0.017(2) 0.012(3) 0.013(2) O1 0.070(3) 0.047(3) 0.019(2) 0.0075(19) 0.006(2) 0.034(2) O2 0.046(3) 0.040(2) 0.059(3) 0.029(2) 0.023(2) 0.020(2) O3 0.046(3) 0.044(3) 0.053(3) 0.027(2) 0.007(2) 0.017(2) O4 0.097(5) 0.150(8) 0.110(6) 0.062(6) 0.038(5) 0.067(6) O5 0.096(5) 0.128(7) 0.111(6) 0.050(6) 0.036(5) 0.033(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 C3 179.8(2) . . ? O1 Cu1 C2 86.93(18) . . ? C3 Cu1 C2 93.05(19) . . ? O1 Cu1 C1 86.91(18) . . ? C3 Cu1 C1 93.09(19) . . ? C2 Cu1 C1 172.55(18) . . ? O1 Cu1 O2 89.03(19) . . ? C3 Cu1 O2 91.13(18) . . ? C2 Cu1 O2 86.24(17) . . ? C1 Cu1 O2 97.85(17) . . ? N3 Cu2 N4 123.2(2) . . ? N3 Cu2 C1' 110.6(2) . 2_565 ? N4 Cu2 C1' 113.60(18) . 2_565 ? N3 Cu2 N1 110.6(2) . 2_565 ? N4 Cu2 N1 113.60(18) . 2_565 ? C1' Cu2 N1 0.00(18) 2_565 2_565 ? N3 Cu2 C2' 106.9(2) . 2 ? N4 Cu2 C2' 98.89(19) . 2 ? C1' Cu2 C2' 99.7(2) 2_565 2 ? N1 Cu2 C2' 99.7(2) 2_565 2 ? N3 Cu2 N2 106.9(2) . 2 ? N4 Cu2 N2 98.89(19) . 2 ? C1' Cu2 N2 99.7(2) 2_565 2 ? N1 Cu2 N2 99.7(2) 2_565 2 ? C2' Cu2 N2 0.0(3) 2 2 ? N3 Cu2 Cu3 121.36(16) . . ? N4 Cu2 Cu3 113.32(14) . . ? C1' Cu2 Cu3 52.86(15) 2_565 . ? N1 Cu2 Cu3 52.86(15) 2_565 . ? C2' Cu2 Cu3 46.92(14) 2 . ? N2 Cu2 Cu3 46.92(14) 2 . ? C2' Cu3 N2 0.0(5) 2 2 ? C2' Cu3 N4' 120.2(2) 2 1_455 ? N2 Cu3 N4' 120.2(2) 2 1_455 ? C2' Cu3 C4 120.2(2) 2 1_455 ? N2 Cu3 C4 120.2(2) 2 1_455 ? N4' Cu3 C4 0.0(6) 1_455 1_455 ? C2' Cu3 N1 118.5(2) 2 2_565 ? N2 Cu3 N1 118.5(2) 2 2_565 ? N4' Cu3 N1 104.4(2) 1_455 2_565 ? C4 Cu3 N1 104.4(2) 1_455 2_565 ? C2' Cu3 C1' 118.5(2) 2 2_565 ? N2 Cu3 C1' 118.5(2) 2 2_565 ? N4' Cu3 C1' 104.4(2) 1_455 2_565 ? C4 Cu3 C1' 104.4(2) 1_455 2_565 ? N1 Cu3 C1' 0.0(2) 2_565 2_565 ? C2' Cu3 N4' 103.14(19) 2 2_554 ? N2 Cu3 N4' 103.14(19) 2 2_554 ? N4' Cu3 N4' 107.47(17) 1_455 2_554 ? C4 Cu3 N4' 107.47(17) 1_455 2_554 ? N1 Cu3 N4' 100.97(18) 2_565 2_554 ? C1' Cu3 N4' 100.97(18) 2_565 2_554 ? C2' Cu3 C4 103.14(19) 2 2_554 ? N2 Cu3 C4 103.14(19) 2 2_554 ? N4' Cu3 C4 107.47(17) 1_455 2_554 ? C4 Cu3 C4 107.47(17) 1_455 2_554 ? N1 Cu3 C4 100.97(18) 2_565 2_554 ? C1' Cu3 C4 100.97(18) 2_565 2_554 ? N4' Cu3 C4 0.0(4) 2_554 2_554 ? C2' Cu3 Cu2 64.25(16) 2 . ? N2 Cu3 Cu2 64.25(16) 2 . ? N4' Cu3 Cu2 138.24(16) 1_455 . ? C4 Cu3 Cu2 138.24(16) 1_455 . ? N1 Cu3 Cu2 54.30(15) 2_565 . ? C1' Cu3 Cu2 54.30(15) 2_565 . ? N4' Cu3 Cu2 111.57(14) 2_554 . ? C4 Cu3 Cu2 111.57(14) 2_554 . ? C2' Cu3 Cu3 126.87(16) 2 2_454 ? N2 Cu3 Cu3 126.87(16) 2 2_454 ? N4' Cu3 Cu3 58.76(16) 1_455 2_454 ? C4 Cu3 Cu3 58.76(16) 1_455 2_454 ? N1 Cu3 Cu3 111.51(15) 2_565 2_454 ? C1' Cu3 Cu3 111.51(15) 2_565 2_454 ? N4' Cu3 Cu3 48.71(14) 2_554 2_454 ? C4 Cu3 Cu3 48.71(14) 2_554 2_454 ? Cu2 Cu3 Cu3 156.49(4) . 2_454 ? C1 N1 Cu3 146.6(5) . 2_565 ? C1 N1 Cu2 140.0(5) . 2_565 ? Cu3 N1 Cu2 72.84(18) 2_565 2_565 ? C2 N2 Cu3 172.0(5) . 2 ? C2 N2 Cu2 118.9(4) . 2 ? Cu3 N2 Cu2 68.84(17) 2 2 ? C3 N3 Cu2 176.3(5) . . ? C4 N4 Cu2 177.7(5) . . ? N1 C1 Cu1 163.1(5) . . ? N2 C2 Cu1 170.5(4) . . ? N3 C3 Cu1 176.6(5) . . ? N4 C4 Cu3 156.6(5) . 1_655 ? N4 C4 Cu3 130.8(4) . 2_554 ? Cu3 C4 Cu3 72.53(17) 1_655 2_554 ? Cu1 O1 H1A 119.9 . . ? Cu1 O1 H1B 120.1 . . ? H1A O1 H1B 120.0 . . ? Cu1 O2 H2A 120.1 . . ? Cu1 O2 H2B 119.9 . . ? H2A O2 H2B 120.0 . . ? H3A O3 H3B 120.3 . . ? H4A O4 H4B 115.6 . . ? H5B O5 H5A 118.1 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.952(4) . ? Cu1 C3 1.958(4) . ? Cu1 C2 1.980(4) . ? Cu1 C1 1.988(4) . ? Cu1 O2 2.431(4) . ? Cu2 N3 1.923(6) . ? Cu2 N4 1.958(4) . ? Cu2 C1' 2.137(5) 2_565 ? Cu2 N1 2.137(5) 2_565 ? Cu2 C2' 2.428(6) 2 ? Cu2 N2 2.428(6) 2 ? Cu2 Cu3 2.5139(12) . ? Cu3 C2' 1.969(6) 2 ? Cu3 N2 1.969(6) 2 ? Cu3 N4' 2.014(5) 1_455 ? Cu3 C4 2.014(5) 1_455 ? Cu3 N1 2.097(6) 2_565 ? Cu3 C1' 2.097(6) 2_565 ? Cu3 N4' 2.292(5) 2_554 ? Cu3 C4 2.292(5) 2_554 ? Cu3 Cu3 2.5564(14) 2_454 ? N1 C1 1.128(7) . ? N1 Cu3 2.097(6) 2_565 ? N1 Cu2 2.137(5) 2_565 ? N2 C2 1.133(7) . ? N2 Cu3 1.969(6) 2 ? N2 Cu2 2.428(6) 2 ? N3 C3 1.143(7) . ? N4 C4 1.135(7) . ? C4 Cu3 2.014(5) 1_655 ? C4 Cu3 2.292(5) 2_554 ? O1 H1A 0.8500 . ? O1 H1B 0.8500 . ? O2 H2A 0.8499 . ? O2 H2B 0.8499 . ? O3 H3A 0.8521 . ? O3 H3B 0.8531 . ? O4 H4A 0.8683 . ? O4 H4B 0.9293 . ? O5 H5B 0.8585 . ? O5 H5A 0.8661 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Cu2 Cu3 C2' -84.1(2) . . . 2 ? N4 Cu2 Cu3 C2' 80.1(2) . . . 2 ? C1' Cu2 Cu3 C2' -177.2(2) 2_565 . . 2 ? N1 Cu2 Cu3 C2' -177.2(2) 2_565 . . 2 ? N2 Cu2 Cu3 C2' 0.0 2 . . 2 ? N3 Cu2 Cu3 N2 -84.1(2) . . . 2 ? N4 Cu2 Cu3 N2 80.1(2) . . . 2 ? C1' Cu2 Cu3 N2 -177.2(2) 2_565 . . 2 ? N1 Cu2 Cu3 N2 -177.2(2) 2_565 . . 2 ? C2' Cu2 Cu3 N2 0.0 2 . . 2 ? N3 Cu2 Cu3 N4' 23.3(3) . . . 1_455 ? N4 Cu2 Cu3 N4' -172.6(3) . . . 1_455 ? C1' Cu2 Cu3 N4' -69.9(3) 2_565 . . 1_455 ? N1 Cu2 Cu3 N4' -69.9(3) 2_565 . . 1_455 ? C2' Cu2 Cu3 N4' 107.4(3) 2 . . 1_455 ? N2 Cu2 Cu3 N4' 107.4(3) 2 . . 1_455 ? N3 Cu2 Cu3 C4 23.3(3) . . . 1_455 ? N4 Cu2 Cu3 C4 -172.6(3) . . . 1_455 ? C1' Cu2 Cu3 C4 -69.9(3) 2_565 . . 1_455 ? N1 Cu2 Cu3 C4 -69.9(3) 2_565 . . 1_455 ? C2' Cu2 Cu3 C4 107.4(3) 2 . . 1_455 ? N2 Cu2 Cu3 C4 107.4(3) 2 . . 1_455 ? N3 Cu2 Cu3 N1 93.2(2) . . . 2_565 ? N4 Cu2 Cu3 N1 -102.7(2) . . . 2_565 ? C1' Cu2 Cu3 N1 0.0 2_565 . . 2_565 ? C2' Cu2 Cu3 N1 177.2(2) 2 . . 2_565 ? N2 Cu2 Cu3 N1 177.2(2) 2 . . 2_565 ? N3 Cu2 Cu3 C1' 93.2(2) . . . 2_565 ? N4 Cu2 Cu3 C1' -102.7(2) . . . 2_565 ? N1 Cu2 Cu3 C1' 0.0 2_565 . . 2_565 ? C2' Cu2 Cu3 C1' 177.2(2) 2 . . 2_565 ? N2 Cu2 Cu3 C1' 177.2(2) 2 . . 2_565 ? N3 Cu2 Cu3 N4' -178.7(2) . . . 2_554 ? N4 Cu2 Cu3 N4' -14.6(2) . . . 2_554 ? C1' Cu2 Cu3 N4' 88.2(2) 2_565 . . 2_554 ? N1 Cu2 Cu3 N4' 88.2(2) 2_565 . . 2_554 ? C2' Cu2 Cu3 N4' -94.6(2) 2 . . 2_554 ? N2 Cu2 Cu3 N4' -94.6(2) 2 . . 2_554 ? N3 Cu2 Cu3 C4 -178.7(2) . . . 2_554 ? N4 Cu2 Cu3 C4 -14.6(2) . . . 2_554 ? C1' Cu2 Cu3 C4 88.2(2) 2_565 . . 2_554 ? N1 Cu2 Cu3 C4 88.2(2) 2_565 . . 2_554 ? C2' Cu2 Cu3 C4 -94.6(2) 2 . . 2_554 ? N2 Cu2 Cu3 C4 -94.6(2) 2 . . 2_554 ? N3 Cu2 Cu3 Cu3 151.8(2) . . . 2_454 ? N4 Cu2 Cu3 Cu3 -44.07(19) . . . 2_454 ? C1' Cu2 Cu3 Cu3 58.66(19) 2_565 . . 2_454 ? N1 Cu2 Cu3 Cu3 58.66(19) 2_565 . . 2_454 ? C2' Cu2 Cu3 Cu3 -124.12(19) 2 . . 2_454 ? N2 Cu2 Cu3 Cu3 -124.12(19) 2 . . 2_454 ?
1100760.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100760.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100760 loop_ _publ_author_name 'Sergey M. Dibrov' 'Bin Deng' 'Donald E. Ellis' 'James A. Ibers' _publ_contact_author_name 'James A. Ibers' _publ_section_title ; Synthesis and Structural Characterization of Some Selenoruthenates and Telluroruthenates ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3441 _journal_page_last 3448 _journal_paper_doi 10.1021/ic0483646 _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C46 H40 P2 Ru2 Se4' _chemical_formula_weight 1172.70 _chemical_name_systematic ; ? ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 93.561(3) _cell_angle_beta 93.604(3) _cell_angle_gamma 109.951(2) _cell_formula_units_Z 1 _cell_length_a 9.5419(14) _cell_length_b 11.8807(17) _cell_length_c 11.9229(18) _cell_measurement_reflns_used 3844 _cell_measurement_temperature 153(2) _cell_measurement_theta_max 26.40 _cell_measurement_theta_min 1.72 _cell_volume 1263.0(3) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 153(2) _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Bruker 1000-CCD' _diffrn_measurement_method 'omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0517 _diffrn_reflns_av_sigmaI/netI 0.0702 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 13958 _diffrn_reflns_theta_full 26.40 _diffrn_reflns_theta_max 26.40 _diffrn_reflns_theta_min 1.72 _exptl_absorpt_coefficient_mu 3.570 _exptl_absorpt_correction_T_max 0.93407 _exptl_absorpt_correction_T_min 0.74289 _exptl_absorpt_correction_type numerical _exptl_crystal_colour green _exptl_crystal_density_diffrn 1.542 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 570 _exptl_crystal_size_max 0.082 _exptl_crystal_size_mid 0.048 _exptl_crystal_size_min 0.020 _refine_diff_density_max 1.214 _refine_diff_density_min -0.888 _refine_diff_density_rms 0.206 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 244 _refine_ls_number_reflns 5146 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.020 _refine_ls_R_factor_all 0.0686 _refine_ls_R_factor_gt 0.0443 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0680P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1192 _refine_ls_wR_factor_ref 0.1295 _reflns_number_gt 3436 _reflns_number_total 5146 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic0483646si20041124_025321_2.cif _cod_data_source_block Ru2Se4 _cod_database_code 1100760 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.07912(5) 0.15215(4) 0.13978(4) 0.02444(15) Uani 1 1 d . . . Se1 Se 0.19293(7) 0.16348(5) -0.03697(5) 0.02568(17) Uani 1 1 d . . . Se2 Se 0.00785(7) -0.05847(5) 0.16843(5) 0.02640(17) Uani 1 1 d . . . P1 P 0.30542(18) 0.18522(14) 0.23675(13) 0.0244(4) Uani 1 1 d . . . C1 C 0.4616(7) 0.3160(6) 0.2026(5) 0.0292(14) Uani 1 1 d . . . C2 C 0.4353(9) 0.4143(6) 0.1650(6) 0.050(2) Uani 1 1 d . . . H2 H 0.3373 0.4134 0.1562 0.060 Uiso 1 1 calc R . . C3 C 0.5504(9) 0.5148(6) 0.1400(6) 0.051(2) Uani 1 1 d . . . H3 H 0.5301 0.5807 0.1149 0.061 Uiso 1 1 calc R . . C4 C 0.6930(10) 0.5163(7) 0.1523(8) 0.064(3) Uani 1 1 d . . . H4 H 0.7703 0.5816 0.1314 0.077 Uiso 1 1 calc R . . C5 C 0.7243(11) 0.4232(8) 0.1950(14) 0.123(6) Uani 1 1 d . . . H5 H 0.8231 0.4272 0.2082 0.148 Uiso 1 1 calc R . . C6 C 0.6083(10) 0.3222(8) 0.2188(12) 0.095(4) Uani 1 1 d . . . H6 H 0.6298 0.2577 0.2462 0.114 Uiso 1 1 calc R . . C7 C 0.3898(6) 0.0680(5) 0.2364(5) 0.0260(13) Uani 1 1 d . . . C8 C 0.3781(7) -0.0035(6) 0.1371(5) 0.0304(14) Uani 1 1 d . . . H8 H 0.3248 0.0075 0.0732 0.036 Uiso 1 1 calc R . . C9 C 0.4444(7) -0.0916(6) 0.1311(6) 0.0351(16) Uani 1 1 d . . . H9 H 0.4377 -0.1374 0.0634 0.042 Uiso 1 1 calc R . . C10 C 0.5195(8) -0.1097(6) 0.2261(6) 0.0383(17) Uani 1 1 d . . . H10 H 0.5614 -0.1698 0.2236 0.046 Uiso 1 1 calc R . . C11 C 0.5333(8) -0.0388(7) 0.3260(6) 0.0419(18) Uani 1 1 d . . . H11 H 0.5871 -0.0501 0.3894 0.050 Uiso 1 1 calc R . . C12 C 0.4676(7) 0.0487(6) 0.3318(5) 0.0340(15) Uani 1 1 d . . . H12 H 0.4753 0.0945 0.3995 0.041 Uiso 1 1 calc R . . C13 C 0.2927(7) 0.2159(6) 0.3881(5) 0.0288(14) Uani 1 1 d . . . C14 C 0.2014(8) 0.1257(6) 0.4439(5) 0.0362(17) Uani 1 1 d . . . H14 H 0.1527 0.0506 0.4051 0.043 Uiso 1 1 calc R . . C15 C 0.1796(7) 0.1431(7) 0.5564(6) 0.0391(17) Uani 1 1 d . . . H15 H 0.1209 0.0794 0.5935 0.047 Uiso 1 1 calc R . . C16 C 0.2442(9) 0.2532(7) 0.6116(6) 0.0470(19) Uani 1 1 d . . . H16 H 0.2308 0.2658 0.6874 0.056 Uiso 1 1 calc R . . C17 C 0.3285(12) 0.3452(8) 0.5566(7) 0.077(3) Uani 1 1 d . . . H17 H 0.3686 0.4218 0.5941 0.093 Uiso 1 1 calc R . . C18 C 0.3562(9) 0.3276(7) 0.4454(6) 0.053(2) Uani 1 1 d . . . H18 H 0.4175 0.3912 0.4097 0.064 Uiso 1 1 calc R . . C19 C 0.0423(8) 0.3064(6) 0.2335(6) 0.0384(17) Uani 1 1 d . . . H19 H 0.1166 0.3594 0.2847 0.046 Uiso 1 1 calc R . . C20 C -0.0678(9) 0.2001(7) 0.2580(6) 0.046(2) Uani 1 1 d . . . H20 H -0.0794 0.1702 0.3284 0.055 Uiso 1 1 calc R . . C21 C -0.1574(8) 0.1467(6) 0.1577(7) 0.0418(18) Uani 1 1 d . . . H21 H -0.2396 0.0757 0.1508 0.050 Uiso 1 1 calc R . . C22 C -0.1031(8) 0.2178(6) 0.0695(6) 0.0355(16) Uani 1 1 d . . . H22 H -0.1405 0.2020 -0.0059 0.043 Uiso 1 1 calc R . . C23 C 0.0205(8) 0.3187(6) 0.1178(6) 0.0386(17) Uani 1 1 d . . . H23 H 0.0773 0.3821 0.0794 0.046 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0261(3) 0.0261(3) 0.0213(3) 0.0001(2) 0.0009(2) 0.0100(2) Se1 0.0264(3) 0.0271(3) 0.0223(3) 0.0036(2) 0.0025(2) 0.0073(3) Se2 0.0294(3) 0.0280(3) 0.0204(3) 0.0041(2) 0.0008(2) 0.0081(3) P1 0.0267(8) 0.0240(8) 0.0214(8) 0.0013(6) 0.0027(6) 0.0072(7) C1 0.029(3) 0.028(3) 0.028(3) -0.001(3) 0.007(3) 0.007(3) C2 0.052(5) 0.032(4) 0.051(5) 0.011(3) -0.018(4) -0.003(4) C3 0.065(6) 0.029(4) 0.038(4) 0.007(3) -0.009(4) -0.007(4) C4 0.064(6) 0.032(4) 0.086(7) 0.001(4) 0.047(5) -0.002(4) C5 0.054(6) 0.036(5) 0.295(19) 0.047(8) 0.089(9) 0.017(5) C6 0.054(6) 0.042(5) 0.205(14) 0.041(7) 0.052(7) 0.024(5) C7 0.019(3) 0.028(3) 0.031(3) 0.007(3) 0.008(3) 0.007(3) C8 0.031(4) 0.035(4) 0.025(3) 0.003(3) 0.000(3) 0.012(3) C9 0.034(4) 0.040(4) 0.034(4) -0.005(3) 0.006(3) 0.017(3) C10 0.038(4) 0.040(4) 0.046(4) 0.008(3) 0.013(3) 0.023(3) C11 0.043(4) 0.058(5) 0.032(4) 0.010(3) -0.003(3) 0.027(4) C12 0.031(4) 0.047(4) 0.027(4) 0.003(3) 0.002(3) 0.018(3) C13 0.028(3) 0.035(4) 0.023(3) 0.002(3) 0.000(3) 0.011(3) C14 0.044(4) 0.034(4) 0.019(3) 0.003(3) 0.005(3) -0.002(3) C15 0.029(4) 0.051(5) 0.035(4) 0.009(3) 0.005(3) 0.009(3) C16 0.070(6) 0.043(5) 0.027(4) -0.001(3) 0.011(4) 0.018(4) C17 0.133(9) 0.040(5) 0.035(5) -0.011(4) 0.003(5) 0.003(5) C18 0.073(6) 0.036(4) 0.031(4) -0.002(3) 0.011(4) -0.006(4) C19 0.045(4) 0.040(4) 0.035(4) -0.013(3) -0.004(3) 0.024(4) C20 0.066(5) 0.062(5) 0.032(4) 0.014(4) 0.022(4) 0.047(5) C21 0.032(4) 0.033(4) 0.067(5) 0.001(4) 0.016(4) 0.019(3) C22 0.042(4) 0.044(4) 0.027(4) -0.012(3) -0.007(3) 0.028(3) C23 0.044(4) 0.038(4) 0.046(4) 0.012(3) 0.004(3) 0.029(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C19 Ru1 C20 36.6(3) . . ? C19 Ru1 C23 36.5(2) . . ? C20 Ru1 C23 60.7(3) . . ? C19 Ru1 C21 60.8(3) . . ? C20 Ru1 C21 36.5(3) . . ? C23 Ru1 C21 60.2(3) . . ? C19 Ru1 C22 61.3(2) . . ? C20 Ru1 C22 61.0(2) . . ? C23 Ru1 C22 36.6(2) . . ? C21 Ru1 C22 36.1(3) . . ? C19 Ru1 P1 93.78(18) . . ? C20 Ru1 P1 108.0(2) . . ? C23 Ru1 P1 114.98(19) . . ? C21 Ru1 P1 144.0(2) . . ? C22 Ru1 P1 151.52(18) . . ? C19 Ru1 Se2 132.8(2) . . ? C20 Ru1 Se2 98.1(2) . . ? C23 Ru1 Se2 150.98(19) . . ? C21 Ru1 Se2 90.85(18) . . ? C22 Ru1 Se2 117.22(18) . . ? P1 Ru1 Se2 89.45(5) . . ? C19 Ru1 Se1 124.4(2) . . ? C20 Ru1 Se1 152.37(19) . . ? C23 Ru1 Se1 93.06(19) . . ? C21 Ru1 Se1 124.6(2) . . ? C22 Ru1 Se1 93.03(18) . . ? P1 Ru1 Se1 90.36(5) . . ? Se2 Ru1 Se1 102.67(3) . . ? Se2 Se1 Ru1 103.40(3) 2 . ? Se1 Se2 Ru1 107.83(3) 2 . ? C7 P1 C1 101.9(3) . . ? C7 P1 C13 102.1(3) . . ? C1 P1 C13 103.8(3) . . ? C7 P1 Ru1 120.9(2) . . ? C1 P1 Ru1 116.3(2) . . ? C13 P1 Ru1 109.6(2) . . ? C2 C1 C6 117.6(7) . . ? C2 C1 P1 120.3(5) . . ? C6 C1 P1 122.1(6) . . ? C1 C2 C3 121.7(8) . . ? C4 C3 C2 119.3(8) . . ? C3 C4 C5 120.6(8) . . ? C4 C5 C6 119.6(9) . . ? C1 C6 C5 120.9(9) . . ? C8 C7 C12 118.5(6) . . ? C8 C7 P1 119.1(5) . . ? C12 C7 P1 122.5(5) . . ? C7 C8 C9 121.5(6) . . ? C10 C9 C8 119.1(6) . . ? C9 C10 C11 120.4(6) . . ? C12 C11 C10 120.5(6) . . ? C11 C12 C7 120.1(6) . . ? C14 C13 C18 117.8(6) . . ? C14 C13 P1 118.2(5) . . ? C18 C13 P1 123.6(5) . . ? C13 C14 C15 121.9(6) . . ? C16 C15 C14 119.3(7) . . ? C15 C16 C17 119.8(7) . . ? C16 C17 C18 121.3(7) . . ? C13 C18 C17 119.8(7) . . ? C20 C19 C23 107.9(6) . . ? C20 C19 Ru1 71.7(4) . . ? C23 C19 Ru1 72.9(4) . . ? C19 C20 C21 108.0(6) . . ? C19 C20 Ru1 71.6(4) . . ? C21 C20 Ru1 73.0(4) . . ? C22 C21 C20 109.0(6) . . ? C22 C21 Ru1 72.4(4) . . ? C20 C21 Ru1 70.6(4) . . ? C21 C22 C23 106.7(6) . . ? C21 C22 Ru1 71.6(4) . . ? C23 C22 Ru1 71.2(4) . . ? C19 C23 C22 108.4(6) . . ? C19 C23 Ru1 70.6(4) . . ? C22 C23 Ru1 72.2(4) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C19 2.228(6) . ? Ru1 C20 2.229(7) . ? Ru1 C23 2.258(6) . ? Ru1 C21 2.260(7) . ? Ru1 C22 2.271(6) . ? Ru1 P1 2.2813(17) . ? Ru1 Se2 2.4114(8) . ? Ru1 Se1 2.4211(8) . ? Se1 Se2 2.3307(9) 2 ? Se2 Se1 2.3307(9) 2 ? P1 C7 1.831(6) . ? P1 C1 1.837(6) . ? P1 C13 1.838(6) . ? C1 C2 1.371(9) . ? C1 C6 1.377(11) . ? C2 C3 1.383(10) . ? C3 C4 1.353(11) . ? C4 C5 1.360(13) . ? C5 C6 1.386(12) . ? C7 C8 1.389(9) . ? C7 C12 1.392(8) . ? C8 C9 1.396(9) . ? C9 C10 1.370(9) . ? C10 C11 1.387(10) . ? C11 C12 1.386(9) . ? C13 C14 1.369(9) . ? C13 C18 1.372(9) . ? C14 C15 1.384(9) . ? C15 C16 1.348(10) . ? C16 C17 1.353(11) . ? C17 C18 1.385(11) . ? C19 C20 1.401(10) . ? C19 C23 1.406(9) . ? C20 C21 1.405(11) . ? C21 C22 1.402(10) . ? C22 C23 1.423(9) . ?
1100761.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100761.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100761 loop_ _publ_author_name 'Sergey M. Dibrov' 'Bin Deng' 'Donald E. Ellis' 'James A. Ibers' _publ_contact_author_name 'James A. Ibers' _publ_section_title ; Synthesis and Structural Characterization of Some Selenoruthenates and Telluroruthenates ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3441 _journal_page_last 3448 _journal_paper_doi 10.1021/ic0483646 _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C20 H20 Ru4 Se6' _chemical_formula_weight 1138.40 _chemical_name_systematic ; ? ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 110.628(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 12.401(3) _cell_length_b 13.607(3) _cell_length_c 14.801(3) _cell_measurement_reflns_used 5839 _cell_measurement_temperature 153(2) _cell_measurement_theta_max 28.94 _cell_measurement_theta_min 2.31 _cell_volume 2337.4(9) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 153(2) _diffrn_measured_fraction_theta_full 0.930 _diffrn_measured_fraction_theta_max 0.930 _diffrn_measurement_device_type 'Bruker 1000-CCD' _diffrn_measurement_method 'omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0530 _diffrn_reflns_av_sigmaI/netI 0.0419 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 13716 _diffrn_reflns_theta_full 28.94 _diffrn_reflns_theta_max 28.94 _diffrn_reflns_theta_min 2.31 _exptl_absorpt_coefficient_mu 11.886 _exptl_absorpt_correction_T_max 0.68343 _exptl_absorpt_correction_T_min 0.13242 _exptl_absorpt_correction_type numerical _exptl_crystal_colour brown _exptl_crystal_density_diffrn 3.235 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 2080 _exptl_crystal_size_max 0.176 _exptl_crystal_size_mid 0.056 _exptl_crystal_size_min 0.038 _refine_diff_density_max 1.325 _refine_diff_density_min -0.904 _refine_diff_density_rms 0.259 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.116 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 136 _refine_ls_number_reflns 2878 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.116 _refine_ls_R_factor_all 0.0540 _refine_ls_R_factor_gt 0.0347 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0380P)^2^+13.1919P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0772 _refine_ls_wR_factor_ref 0.0860 _reflns_number_gt 2237 _reflns_number_total 2878 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic0483646si20041124_025321_3.cif _cod_data_source_block Ru4Se6 _cod_original_cell_volume 2337.5(8) _cod_database_code 1100761 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.99668(4) 0.21122(4) 0.61636(3) 0.01353(12) Uani 1 1 d . . . Ru2 Ru 1.17818(4) 0.08056(4) 0.71171(3) 0.01555(13) Uani 1 1 d . . . Se1 Se 0.87219(5) 0.22395(4) 0.71571(4) 0.01384(14) Uani 1 1 d . . . Se2 Se 0.98380(5) 0.03600(5) 0.60385(4) 0.01773(15) Uani 1 1 d . . . Se3 Se 1.14903(6) -0.03018(5) 0.83160(5) 0.02213(16) Uani 1 1 d . . . C1 C 0.9802(6) 0.3646(5) 0.5611(4) 0.0204(14) Uani 1 1 d . . . H1 H 0.9819 0.4199 0.6007 0.024 Uiso 1 1 calc R . . C2 C 0.8808(6) 0.3124(5) 0.5046(4) 0.0229(14) Uani 1 1 d . . . H2 H 0.8039 0.3258 0.5004 0.027 Uiso 1 1 calc R . . C3 C 0.9158(6) 0.2366(5) 0.4554(4) 0.0197(13) Uani 1 1 d . . . H3 H 0.8662 0.1909 0.4118 0.024 Uiso 1 1 calc R . . C4 C 1.0377(6) 0.2405(5) 0.4823(4) 0.0232(14) Uani 1 1 d . . . H4 H 1.0840 0.1979 0.4604 0.028 Uiso 1 1 calc R . . C5 C 1.0774(6) 0.3198(5) 0.5480(4) 0.0241(15) Uani 1 1 d . . . H5 H 1.1553 0.3395 0.5782 0.029 Uiso 1 1 calc R . . C6 C 1.3370(6) 0.1563(5) 0.7117(6) 0.0291(16) Uani 1 1 d . . . H6 H 1.3521 0.2234 0.7297 0.035 Uiso 1 1 calc R . . C7 C 1.2820(6) 0.1214(6) 0.6175(5) 0.0339(18) Uani 1 1 d . . . H7 H 1.2540 0.1604 0.5607 0.041 Uiso 1 1 calc R . . C8 C 1.2756(6) 0.0181(6) 0.6218(5) 0.0314(17) Uani 1 1 d . . . H8 H 1.2427 -0.0245 0.5683 0.038 Uiso 1 1 calc R . . C9 C 1.3263(6) -0.0108(5) 0.7187(5) 0.0265(15) Uani 1 1 d . . . H9 H 1.3329 -0.0762 0.7424 0.032 Uiso 1 1 calc R . . C10 C 1.3660(6) 0.0757(5) 0.7752(5) 0.0250(15) Uani 1 1 d . . . H10 H 1.4049 0.0782 0.8431 0.030 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0135(2) 0.0182(3) 0.0098(2) 0.00076(17) 0.00507(18) -0.00099(18) Ru2 0.0158(3) 0.0189(3) 0.0146(2) 0.00028(19) 0.00853(19) 0.0019(2) Se1 0.0133(3) 0.0176(3) 0.0112(3) 0.0007(2) 0.0051(2) 0.0009(2) Se2 0.0200(3) 0.0203(3) 0.0159(3) -0.0044(2) 0.0100(2) -0.0038(2) Se3 0.0263(4) 0.0221(3) 0.0236(3) 0.0073(3) 0.0157(3) 0.0089(3) C1 0.030(4) 0.016(3) 0.018(3) 0.003(2) 0.011(3) -0.001(3) C2 0.021(3) 0.028(4) 0.018(3) 0.014(3) 0.005(3) 0.004(3) C3 0.028(4) 0.022(3) 0.008(3) 0.002(2) 0.006(2) -0.008(3) C4 0.028(4) 0.031(4) 0.015(3) 0.009(3) 0.013(3) 0.003(3) C5 0.025(4) 0.031(4) 0.018(3) -0.001(3) 0.010(3) -0.013(3) C6 0.022(4) 0.029(4) 0.048(4) 0.007(3) 0.026(3) 0.007(3) C7 0.027(4) 0.056(5) 0.029(4) 0.019(4) 0.022(3) 0.010(4) C8 0.022(4) 0.048(5) 0.027(4) -0.011(3) 0.012(3) 0.006(3) C9 0.021(3) 0.032(4) 0.032(4) 0.002(3) 0.016(3) 0.010(3) C10 0.016(3) 0.038(4) 0.023(3) -0.007(3) 0.010(3) 0.006(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 Ru1 C1 37.4(2) . . ? C5 Ru1 C2 61.9(3) . . ? C1 Ru1 C2 36.9(2) . . ? C5 Ru1 C4 37.0(2) . . ? C1 Ru1 C4 61.9(2) . . ? C2 Ru1 C4 61.7(2) . . ? C5 Ru1 C3 61.4(2) . . ? C1 Ru1 C3 61.3(2) . . ? C2 Ru1 C3 36.7(2) . . ? C4 Ru1 C3 36.7(2) . . ? C5 Ru1 Se2 131.08(18) . . ? C1 Ru1 Se2 155.71(16) . . ? C2 Ru1 Se2 123.18(18) . . ? C4 Ru1 Se2 97.92(18) . . ? C3 Ru1 Se2 94.47(16) . . ? C5 Ru1 Se1 99.83(17) . 2_756 ? C1 Ru1 Se1 104.42(17) . 2_756 ? C2 Ru1 Se1 136.81(18) . 2_756 ? C4 Ru1 Se1 127.33(18) . 2_756 ? C3 Ru1 Se1 161.26(16) . 2_756 ? Se2 Ru1 Se1 98.70(3) . 2_756 ? C5 Ru1 Se1 134.23(19) . . ? C1 Ru1 Se1 99.01(17) . . ? C2 Ru1 Se1 91.33(18) . . ? C4 Ru1 Se1 152.86(18) . . ? C3 Ru1 Se1 118.37(17) . . ? Se2 Ru1 Se1 94.40(3) . . ? Se1 Ru1 Se1 73.95(3) 2_756 . ? C5 Ru1 Ru2 103.83(19) . . ? C1 Ru1 Ru2 136.72(17) . . ? C2 Ru1 Ru2 161.15(18) . . ? C4 Ru1 Ru2 99.44(18) . . ? C3 Ru1 Ru2 127.00(17) . . ? Se2 Ru1 Ru2 55.33(2) . . ? Se1 Ru1 Ru2 53.88(2) 2_756 . ? Se1 Ru1 Ru2 107.46(3) . . ? C10 Ru2 C9 38.1(3) . . ? C10 Ru2 C6 37.2(3) . . ? C9 Ru2 C6 62.3(3) . . ? C10 Ru2 C8 62.0(3) . . ? C9 Ru2 C8 36.8(3) . . ? C6 Ru2 C8 61.1(3) . . ? C10 Ru2 C7 61.5(3) . . ? C9 Ru2 C7 61.4(3) . . ? C6 Ru2 C7 36.3(3) . . ? C8 Ru2 C7 36.2(3) . . ? C10 Ru2 Se1 103.73(18) . 2_756 ? C9 Ru2 Se1 141.47(19) . 2_756 ? C6 Ru2 Se1 89.60(19) . 2_756 ? C8 Ru2 Se1 147.5(2) . 2_756 ? C7 Ru2 Se1 111.5(2) . 2_756 ? C10 Ru2 Se3 94.41(19) . . ? C9 Ru2 Se3 87.25(19) . . ? C6 Ru2 Se3 129.94(19) . . ? C8 Ru2 Se3 116.3(2) . . ? C7 Ru2 Se3 148.6(2) . . ? Se1 Ru2 Se3 92.72(3) 2_756 . ? C10 Ru2 Se2 157.98(17) . . ? C9 Ru2 Se2 120.4(2) . . ? C6 Ru2 Se2 141.5(2) . . ? C8 Ru2 Se2 97.52(19) . . ? C7 Ru2 Se2 107.5(2) . . ? Se1 Ru2 Se2 98.07(3) 2_756 . ? Se3 Ru2 Se2 87.56(3) . . ? C10 Ru2 Ru1 140.8(2) . . ? C9 Ru2 Ru1 152.65(18) . . ? C6 Ru2 Ru1 104.95(18) . . ? C8 Ru2 Ru1 116.1(2) . . ? C7 Ru2 Ru1 93.64(19) . . ? Se1 Ru2 Ru1 55.10(2) 2_756 . ? Se3 Ru2 Ru1 117.00(3) . . ? Se2 Ru2 Ru1 53.35(2) . . ? Ru2 Se1 Ru1 71.01(2) 2_756 2_756 ? Ru2 Se1 Ru1 121.28(3) 2_756 . ? Ru1 Se1 Ru1 105.46(3) 2_756 . ? Se3 Se2 Ru1 112.76(3) 2_756 . ? Se3 Se2 Ru2 119.87(3) 2_756 . ? Ru1 Se2 Ru2 71.32(2) . . ? Se2 Se3 Ru2 111.19(3) 2_756 . ? C2 C1 C5 108.0(6) . . ? C2 C1 Ru1 72.2(4) . . ? C5 C1 Ru1 71.0(4) . . ? C2 C1 H1 126.0 . . ? C5 C1 H1 126.0 . . ? Ru1 C1 H1 122.4 . . ? C1 C2 C3 107.9(6) . . ? C1 C2 Ru1 70.9(3) . . ? C3 C2 Ru1 72.5(3) . . ? C1 C2 H2 126.0 . . ? C3 C2 H2 126.0 . . ? Ru1 C2 H2 122.3 . . ? C2 C3 C4 108.5(6) . . ? C2 C3 Ru1 70.9(3) . . ? C4 C3 Ru1 71.2(3) . . ? C2 C3 H3 125.8 . . ? C4 C3 H3 125.8 . . ? Ru1 C3 H3 123.8 . . ? C5 C4 C3 107.3(6) . . ? C5 C4 Ru1 70.2(3) . . ? C3 C4 Ru1 72.1(3) . . ? C5 C4 H4 126.3 . . ? C3 C4 H4 126.3 . . ? Ru1 C4 H4 123.0 . . ? C4 C5 C1 108.3(6) . . ? C4 C5 Ru1 72.7(4) . . ? C1 C5 Ru1 71.6(4) . . ? C4 C5 H5 125.9 . . ? C1 C5 H5 125.9 . . ? Ru1 C5 H5 121.5 . . ? C7 C6 C10 108.6(7) . . ? C7 C6 Ru2 73.9(4) . . ? C10 C6 Ru2 69.9(4) . . ? C7 C6 H6 125.7 . . ? C10 C6 H6 125.7 . . ? Ru2 C6 H6 122.2 . . ? C6 C7 C8 108.0(6) . . ? C6 C7 Ru2 69.8(4) . . ? C8 C7 Ru2 71.1(4) . . ? C6 C7 H7 126.0 . . ? C8 C7 H7 126.0 . . ? Ru2 C7 H7 124.6 . . ? C9 C8 C7 108.3(7) . . ? C9 C8 Ru2 69.1(4) . . ? C7 C8 Ru2 72.6(4) . . ? C9 C8 H8 125.9 . . ? C7 C8 H8 125.9 . . ? Ru2 C8 H8 124.0 . . ? C8 C9 C10 107.8(7) . . ? C8 C9 Ru2 74.2(4) . . ? C10 C9 Ru2 70.7(4) . . ? C8 C9 H9 126.1 . . ? C10 C9 H9 126.1 . . ? Ru2 C9 H9 120.8 . . ? C6 C10 C9 107.4(6) . . ? C6 C10 Ru2 72.9(4) . . ? C9 C10 Ru2 71.2(4) . . ? C6 C10 H10 126.3 . . ? C9 C10 H10 126.3 . . ? Ru2 C10 H10 121.4 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C5 2.218(6) . ? Ru1 C1 2.225(6) . ? Ru1 C2 2.241(6) . ? Ru1 C4 2.250(6) . ? Ru1 C3 2.262(6) . ? Ru1 Se2 2.3924(9) . ? Ru1 Se1 2.4503(8) 2_756 ? Ru1 Se1 2.4851(8) . ? Ru1 Ru2 2.8250(8) . ? Ru2 C10 2.184(7) . ? Ru2 C9 2.190(7) . ? Ru2 C6 2.223(7) . ? Ru2 C8 2.256(7) . ? Ru2 C7 2.275(7) . ? Ru2 Se1 2.4133(8) 2_756 ? Ru2 Se3 2.4500(9) . ? Ru2 Se2 2.4526(9) . ? Se1 Ru2 2.4133(8) 2_756 ? Se1 Ru1 2.4503(8) 2_756 ? Se2 Se3 2.3550(9) 2_756 ? Se3 Se2 2.3550(9) 2_756 ? C1 C2 1.413(9) . ? C1 C5 1.423(10) . ? C1 H1 0.9500 . ? C2 C3 1.417(9) . ? C2 H2 0.9500 . ? C3 C4 1.422(9) . ? C3 H3 0.9500 . ? C4 C5 1.420(9) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.403(11) . ? C6 C10 1.406(10) . ? C6 H6 0.9500 . ? C7 C8 1.409(11) . ? C7 H7 0.9500 . ? C8 C9 1.404(10) . ? C8 H8 0.9500 . ? C9 C10 1.427(10) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ?
1100762.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100762.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100762 loop_ _publ_author_name 'Sergey M. Dibrov' 'Bin Deng' 'Donald E. Ellis' 'James A. Ibers' _publ_contact_author_name 'James A. Ibers' _publ_section_title ; Synthesis and Structural Characterization of Some Selenoruthenates and Telluroruthenates ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3441 _journal_page_last 3448 _journal_paper_doi 10.1021/ic0483646 _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C46 H40 P2 Ru2 Te6' _chemical_formula_weight 1622.46 _chemical_name_systematic ; ? ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 119.5060(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 25.211(2) _cell_length_b 13.8374(12) _cell_length_c 17.1079(15) _cell_measurement_reflns_used 8699 _cell_measurement_temperature 153(2) _cell_measurement_theta_max 28.98 _cell_measurement_theta_min 1.74 _cell_volume 5194.1(8) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 153(2) _diffrn_measured_fraction_theta_full 0.935 _diffrn_measured_fraction_theta_max 0.935 _diffrn_measurement_device_type 'Bruker 1000-CCD' _diffrn_measurement_method 'omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0636 _diffrn_reflns_av_sigmaI/netI 0.0612 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 31234 _diffrn_reflns_theta_full 28.98 _diffrn_reflns_theta_max 28.98 _diffrn_reflns_theta_min 1.74 _exptl_absorpt_coefficient_mu 3.975 _exptl_absorpt_correction_T_max 0.89389 _exptl_absorpt_correction_T_min 0.58003 _exptl_absorpt_correction_type numerical _exptl_crystal_colour ?brown _exptl_crystal_density_diffrn 2.075 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 2984 _exptl_crystal_size_max 0.202 _exptl_crystal_size_mid 0.062 _exptl_crystal_size_min 0.028 _refine_diff_density_max 1.677 _refine_diff_density_min -1.118 _refine_diff_density_rms 0.227 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.975 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 253 _refine_ls_number_reflns 6440 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.975 _refine_ls_R_factor_all 0.0697 _refine_ls_R_factor_gt 0.0426 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0563P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0932 _refine_ls_wR_factor_ref 0.1022 _reflns_number_gt 4585 _reflns_number_total 6440 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic0483646si20041124_025321_4.cif _cod_data_source_block Ru2Te6 _cod_original_cell_volume 5194.2(8) _cod_database_code 1100762 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.12148(2) 0.08085(4) 0.23728(3) 0.01829(12) Uani 1 1 d . . . Te1 Te 0.066017(18) 0.16129(3) 0.31407(2) 0.01973(10) Uani 1 1 d . . . Te2 Te 0.059003(18) 0.02801(3) 0.43160(3) 0.02311(11) Uani 1 1 d . . . Te3 Te -0.035325(18) 0.12948(3) 0.42606(3) 0.02055(11) Uani 1 1 d . . . P1 P 0.17293(7) 0.21934(12) 0.24438(11) 0.0218(3) Uani 1 1 d . . . C1 C 0.1533(3) 0.3373(5) 0.2726(4) 0.0265(14) Uani 1 1 d . . . C2 C 0.1977(3) 0.4013(5) 0.3303(4) 0.0287(15) Uani 1 1 d . . . H2 H 0.2393 0.3828 0.3590 0.034 Uiso 1 1 calc R . . C3 C 0.1818(4) 0.4926(5) 0.3465(5) 0.0413(19) Uani 1 1 d . . . H3 H 0.2124 0.5358 0.3868 0.050 Uiso 1 1 calc R . . C4 C 0.1217(4) 0.5196(5) 0.3039(5) 0.044(2) Uani 1 1 d . . . H4 H 0.1106 0.5821 0.3138 0.053 Uiso 1 1 calc R . . C5 C 0.0765(4) 0.4550(5) 0.2454(5) 0.0391(18) Uani 1 1 d . . . H5 H 0.0347 0.4734 0.2168 0.047 Uiso 1 1 calc R . . C6 C 0.0929(3) 0.3650(5) 0.2299(4) 0.0303(15) Uani 1 1 d . . . H6 H 0.0624 0.3218 0.1894 0.036 Uiso 1 1 calc R . . C7 C 0.2542(3) 0.2099(5) 0.3269(4) 0.0244(14) Uani 1 1 d . . . C8 C 0.2702(3) 0.1876(5) 0.4160(4) 0.0323(16) Uani 1 1 d . . . H8 H 0.2392 0.1809 0.4319 0.039 Uiso 1 1 calc R . . C9 C 0.3308(3) 0.1754(5) 0.4810(5) 0.0358(17) Uani 1 1 d . . . H9 H 0.3414 0.1621 0.5415 0.043 Uiso 1 1 calc R . . C10 C 0.3755(3) 0.1826(5) 0.4574(5) 0.0391(18) Uani 1 1 d . . . H10 H 0.4170 0.1735 0.5017 0.047 Uiso 1 1 calc R . . C11 C 0.3611(3) 0.2028(6) 0.3708(5) 0.0411(19) Uani 1 1 d . . . H11 H 0.3923 0.2076 0.3551 0.049 Uiso 1 1 calc R . . C12 C 0.3002(3) 0.2163(5) 0.3057(4) 0.0275(14) Uani 1 1 d . . . H12 H 0.2903 0.2301 0.2456 0.033 Uiso 1 1 calc R . . C13 C 0.1737(3) 0.2507(5) 0.1399(4) 0.0243(14) Uani 1 1 d . . . C14 C 0.1714(3) 0.3440(5) 0.1107(5) 0.0326(16) Uani 1 1 d . . . H14 H 0.1687 0.3957 0.1451 0.039 Uiso 1 1 calc R . . C15 C 0.1730(4) 0.3649(5) 0.0316(5) 0.0401(18) Uani 1 1 d . . . H15 H 0.1707 0.4297 0.0118 0.048 Uiso 1 1 calc R . . C16 C 0.1780(3) 0.2890(5) -0.0169(4) 0.0368(18) Uani 1 1 d . . . H16 H 0.1785 0.3020 -0.0711 0.044 Uiso 1 1 calc R . . C17 C 0.1823(3) 0.1947(5) 0.0120(5) 0.0318(16) Uani 1 1 d . . . H17 H 0.1877 0.1434 -0.0203 0.038 Uiso 1 1 calc R . . C18 C 0.1785(3) 0.1756(5) 0.0897(4) 0.0311(15) Uani 1 1 d . . . H18 H 0.1793 0.1106 0.1082 0.037 Uiso 1 1 calc R . . C19 C 0.1814(3) -0.0230(5) 0.3409(4) 0.0327(16) Uani 1 1 d . . . H19 H 0.2026 -0.0068 0.4029 0.039 Uiso 1 1 calc R . . C20 C 0.2023(3) -0.0104(5) 0.2793(5) 0.0353(17) Uani 1 1 d . . . H20 H 0.2407 0.0162 0.2930 0.042 Uiso 1 1 calc R . . C21 C 0.1578(3) -0.0431(5) 0.1945(4) 0.0282(15) Uani 1 1 d . . . H21 H 0.1611 -0.0435 0.1415 0.034 Uiso 1 1 calc R . . C22 C 0.1072(3) -0.0753(5) 0.2016(5) 0.0296(15) Uani 1 1 d . . . H22 H 0.0699 -0.0997 0.1542 0.036 Uiso 1 1 calc R . . C23 C 0.1225(3) -0.0644(4) 0.2930(5) 0.0291(15) Uani 1 1 d . . . H23 H 0.0975 -0.0820 0.3177 0.035 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0186(2) 0.0234(3) 0.0158(2) -0.00161(19) 0.0107(2) -0.0023(2) Te1 0.0205(2) 0.0267(2) 0.01503(19) -0.00210(16) 0.01107(16) -0.00215(16) Te2 0.0206(2) 0.0338(3) 0.0178(2) 0.00352(17) 0.01165(17) 0.00399(17) Te3 0.0221(2) 0.0273(2) 0.0156(2) 0.00090(16) 0.01193(17) 0.00256(17) P1 0.0243(8) 0.0256(9) 0.0208(8) -0.0042(7) 0.0151(7) -0.0073(7) C1 0.034(4) 0.031(4) 0.030(4) -0.006(3) 0.027(3) -0.008(3) C2 0.043(4) 0.025(4) 0.026(3) -0.008(3) 0.023(3) -0.005(3) C3 0.055(5) 0.035(4) 0.042(5) -0.015(4) 0.031(4) -0.014(4) C4 0.072(6) 0.028(4) 0.046(5) -0.008(3) 0.040(5) -0.005(4) C5 0.045(5) 0.032(4) 0.050(5) 0.002(4) 0.032(4) 0.006(3) C6 0.046(4) 0.027(4) 0.028(4) -0.004(3) 0.025(3) -0.004(3) C7 0.017(3) 0.031(4) 0.028(3) -0.006(3) 0.013(3) -0.007(3) C8 0.038(4) 0.039(4) 0.026(4) -0.011(3) 0.020(3) -0.014(3) C9 0.030(4) 0.051(5) 0.024(4) -0.011(3) 0.012(3) -0.014(3) C10 0.032(4) 0.039(4) 0.037(4) -0.008(3) 0.010(3) -0.009(3) C11 0.025(4) 0.056(5) 0.051(5) 0.005(4) 0.026(4) 0.001(3) C12 0.029(4) 0.032(4) 0.028(3) -0.005(3) 0.019(3) -0.002(3) C13 0.018(3) 0.034(4) 0.023(3) -0.007(3) 0.011(3) -0.004(3) C14 0.046(4) 0.033(4) 0.029(4) -0.012(3) 0.027(3) -0.013(3) C15 0.060(5) 0.035(4) 0.040(4) 0.000(3) 0.036(4) -0.013(4) C16 0.053(5) 0.046(5) 0.021(3) -0.002(3) 0.026(3) -0.013(4) C17 0.040(4) 0.035(4) 0.035(4) -0.006(3) 0.030(3) -0.006(3) C18 0.039(4) 0.030(4) 0.032(4) 0.003(3) 0.023(3) -0.002(3) C19 0.044(4) 0.026(4) 0.020(3) 0.007(3) 0.010(3) 0.000(3) C20 0.026(4) 0.032(4) 0.040(4) 0.007(3) 0.010(3) 0.009(3) C21 0.039(4) 0.027(4) 0.030(4) 0.001(3) 0.026(3) 0.011(3) C22 0.029(4) 0.027(4) 0.033(4) -0.005(3) 0.016(3) 0.000(3) C23 0.043(4) 0.015(3) 0.047(4) 0.008(3) 0.036(4) 0.003(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C20 Ru1 C19 37.2(3) . . ? C20 Ru1 C23 61.7(3) . . ? C19 Ru1 C23 37.3(2) . . ? C20 Ru1 C22 62.0(3) . . ? C19 Ru1 C22 62.7(3) . . ? C23 Ru1 C22 37.3(2) . . ? C20 Ru1 C21 36.9(3) . . ? C19 Ru1 C21 62.2(3) . . ? C23 Ru1 C21 61.6(2) . . ? C22 Ru1 C21 37.0(2) . . ? C20 Ru1 P1 93.1(2) . . ? C19 Ru1 P1 111.01(19) . . ? C23 Ru1 P1 148.32(19) . . ? C22 Ru1 P1 147.17(17) . . ? C21 Ru1 P1 110.38(18) . . ? C20 Ru1 Te1 136.53(19) . . ? C19 Ru1 Te1 101.49(19) . . ? C23 Ru1 Te1 93.83(17) . . ? C22 Ru1 Te1 120.04(17) . . ? C21 Ru1 Te1 155.09(17) . . ? P1 Ru1 Te1 92.68(4) . . ? C20 Ru1 Te3 129.72(19) . 2 ? C19 Ru1 Te3 153.74(18) . 2 ? C23 Ru1 Te3 120.92(19) . 2 ? C22 Ru1 Te3 91.10(18) . 2 ? C21 Ru1 Te3 96.03(17) . 2 ? P1 Ru1 Te3 89.54(5) . 2 ? Te1 Ru1 Te3 93.37(2) . 2 ? Ru1 Te1 Te2 108.77(2) . . ? Ru1 Te1 Te1 108.43(2) . 2 ? Te2 Te1 Te1 94.961(17) . 2 ? Te3 Te2 Te1 89.904(17) . . ? Ru1 Te3 Te2 98.872(19) 2 . ? C7 P1 C1 101.8(3) . . ? C7 P1 C13 102.8(3) . . ? C1 P1 C13 100.3(3) . . ? C7 P1 Ru1 111.8(2) . . ? C1 P1 Ru1 122.6(2) . . ? C13 P1 Ru1 114.9(2) . . ? C6 C1 C2 119.5(6) . . ? C6 C1 P1 118.5(5) . . ? C2 C1 P1 121.8(5) . . ? C1 C2 C3 120.8(7) . . ? C1 C2 H2 119.6 . . ? C3 C2 H2 119.6 . . ? C4 C3 C2 119.3(7) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C3 C4 C5 120.3(7) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C6 C5 C4 119.7(7) . . ? C6 C5 H5 120.2 . . ? C4 C5 H5 120.2 . . ? C5 C6 C1 120.4(7) . . ? C5 C6 H6 119.8 . . ? C1 C6 H6 119.8 . . ? C12 C7 C8 118.1(6) . . ? C12 C7 P1 124.0(5) . . ? C8 C7 P1 117.8(5) . . ? C9 C8 C7 120.7(6) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? C10 C9 C8 119.5(7) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? C11 C10 C9 120.9(7) . . ? C11 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? C10 C11 C12 119.5(7) . . ? C10 C11 H11 120.2 . . ? C12 C11 H11 120.2 . . ? C7 C12 C11 121.2(6) . . ? C7 C12 H12 119.4 . . ? C11 C12 H12 119.4 . . ? C14 C13 C18 118.6(6) . . ? C14 C13 P1 123.5(5) . . ? C18 C13 P1 117.9(5) . . ? C13 C14 C15 121.8(6) . . ? C13 C14 H14 119.1 . . ? C15 C14 H14 119.1 . . ? C16 C15 C14 118.4(7) . . ? C16 C15 H15 120.8 . . ? C14 C15 H15 120.8 . . ? C15 C16 C17 121.2(6) . . ? C15 C16 H16 119.4 . . ? C17 C16 H16 119.4 . . ? C16 C17 C18 119.2(6) . . ? C16 C17 H17 120.4 . . ? C18 C17 H17 120.4 . . ? C13 C18 C17 120.7(6) . . ? C13 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? C20 C19 C23 106.9(6) . . ? C20 C19 Ru1 71.2(4) . . ? C23 C19 Ru1 72.0(4) . . ? C20 C19 H19 126.6 . . ? C23 C19 H19 126.6 . . ? Ru1 C19 H19 122.1 . . ? C19 C20 C21 109.4(6) . . ? C19 C20 Ru1 71.7(4) . . ? C21 C20 Ru1 72.9(4) . . ? C19 C20 H20 125.3 . . ? C21 C20 H20 125.3 . . ? Ru1 C20 H20 121.8 . . ? C20 C21 C22 108.0(6) . . ? C20 C21 Ru1 70.2(4) . . ? C22 C21 Ru1 71.3(4) . . ? C20 C21 H21 126.0 . . ? C22 C21 H21 126.0 . . ? Ru1 C21 H21 124.1 . . ? C21 C22 C23 107.0(6) . . ? C21 C22 Ru1 71.7(4) . . ? C23 C22 Ru1 71.1(4) . . ? C21 C22 H22 126.5 . . ? C23 C22 H22 126.5 . . ? Ru1 C22 H22 122.5 . . ? C19 C23 C22 108.7(6) . . ? C19 C23 Ru1 70.7(4) . . ? C22 C23 Ru1 71.6(4) . . ? C19 C23 H23 125.6 . . ? C22 C23 H23 125.6 . . ? Ru1 C23 H23 123.6 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C20 2.195(7) . ? Ru1 C19 2.202(6) . ? Ru1 C23 2.218(6) . ? Ru1 C22 2.226(7) . ? Ru1 C21 2.231(6) . ? Ru1 P1 2.2836(16) . ? Ru1 Te1 2.5940(6) . ? Ru1 Te3 2.6458(6) 2 ? Te1 Te2 2.7975(6) . ? Te1 Te1 2.9493(8) 2 ? Te2 Te3 2.7228(6) . ? Te3 Ru1 2.6458(6) 2 ? P1 C7 1.833(6) . ? P1 C1 1.838(7) . ? P1 C13 1.849(6) . ? C1 C6 1.380(9) . ? C1 C2 1.387(9) . ? C2 C3 1.393(10) . ? C2 H2 0.9500 . ? C3 C4 1.370(11) . ? C3 H3 0.9500 . ? C4 C5 1.406(11) . ? C4 H4 0.9500 . ? C5 C6 1.380(9) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.379(8) . ? C7 C8 1.405(9) . ? C8 C9 1.388(10) . ? C8 H8 0.9500 . ? C9 C10 1.376(10) . ? C9 H9 0.9500 . ? C10 C11 1.369(10) . ? C10 H10 0.9500 . ? C11 C12 1.395(9) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.376(9) . ? C13 C18 1.391(9) . ? C14 C15 1.405(9) . ? C14 H14 0.9500 . ? C15 C16 1.381(10) . ? C15 H15 0.9500 . ? C16 C17 1.382(10) . ? C16 H16 0.9500 . ? C17 C18 1.402(9) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.402(10) . ? C19 C23 1.415(10) . ? C19 H19 0.9500 . ? C20 C21 1.403(9) . ? C20 H20 0.9500 . ? C21 C22 1.413(9) . ? C21 H21 0.9500 . ? C22 C23 1.421(9) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ?
1100763.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100763.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100763 loop_ _publ_author_name 'Sergey M. Dibrov' 'Bin Deng' 'Donald E. Ellis' 'James A. Ibers' _publ_contact_author_name 'James A. Ibers' _publ_section_title ; Synthesis and Structural Characterization of Some Selenoruthenates and Telluroruthenates ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3441 _journal_page_last 3448 _journal_paper_doi 10.1021/ic0483646 _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C47 H42 Cl2 P2 Ru2 Te6' _chemical_formula_weight 1707.39 _chemical_name_systematic ; ? ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 81.536(3) _cell_angle_beta 83.552(3) _cell_angle_gamma 74.870(3) _cell_formula_units_Z 2 _cell_length_a 9.3753(16) _cell_length_b 14.520(2) _cell_length_c 19.117(3) _cell_measurement_reflns_used 8584 _cell_measurement_temperature 153(2) _cell_measurement_theta_max 27.18 _cell_measurement_theta_min 1.46 _cell_volume 2477.4(7) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 153(2) _diffrn_measured_fraction_theta_full 0.697 _diffrn_measured_fraction_theta_max 0.697 _diffrn_measurement_device_type 'Bruker 1000-CCD' _diffrn_measurement_method 'omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0468 _diffrn_reflns_av_sigmaI/netI 0.0663 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 18061 _diffrn_reflns_theta_full 27.18 _diffrn_reflns_theta_max 27.18 _diffrn_reflns_theta_min 1.46 _exptl_absorpt_coefficient_mu 4.277 _exptl_absorpt_correction_T_max 0.84811 _exptl_absorpt_correction_T_min 0.43897 _exptl_absorpt_correction_type numerical _exptl_crystal_colour brown _exptl_crystal_density_diffrn 2.289 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 1576 _exptl_crystal_size_max 0.234 _exptl_crystal_size_mid 0.088 _exptl_crystal_size_min 0.042 _refine_diff_density_max 2.919 _refine_diff_density_min -1.305 _refine_diff_density_rms 0.302 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 532 _refine_ls_number_reflns 7678 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.063 _refine_ls_R_factor_all 0.0719 _refine_ls_R_factor_gt 0.0496 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0874P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1279 _refine_ls_wR_factor_ref 0.1459 _reflns_number_gt 5759 _reflns_number_total 7678 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic0483646si20041124_025321_1.cif _cod_data_source_block ru2te6d _cod_original_cell_volume 2477.5(7) _cod_database_code 1100763 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.89326(9) -0.00222(6) 0.31200(4) 0.0186(2) Uani 1 1 d . . . Ru2 Ru 0.34319(9) 0.35904(6) 0.40279(4) 0.0174(2) Uani 1 1 d . . . Te1 Te 0.63701(8) -0.04597(5) 0.31303(4) 0.0273(2) Uani 1 1 d . . . Te2 Te 0.45957(8) 0.05776(5) 0.41113(4) 0.0266(2) Uani 1 1 d . . . Te3 Te 0.44287(7) 0.22602(5) 0.32250(3) 0.01862(19) Uani 1 1 d . . . Te4 Te 0.78026(7) 0.17891(5) 0.30956(3) 0.01941(19) Uani 1 1 d . . . Te5 Te 0.77982(8) 0.21642(5) 0.44514(4) 0.0263(2) Uani 1 1 d . . . Te6 Te 0.60181(7) 0.39456(5) 0.41569(4) 0.02069(19) Uani 1 1 d . . . P1 P 0.9224(3) 0.01808(19) 0.19042(14) 0.0205(6) Uani 1 1 d . . . P2 P 0.3038(3) 0.47307(19) 0.30627(14) 0.0192(6) Uani 1 1 d . . . C1 C 1.1286(12) -0.0535(8) 0.3328(6) 0.029(3) Uani 1 1 d . . . H1 H 1.2039 -0.0370 0.2996 0.035 Uiso 1 1 calc R . . C2 C 1.0713(11) -0.1368(8) 0.3350(6) 0.029(3) Uani 1 1 d . . . H2 H 1.1020 -0.1858 0.3047 0.035 Uiso 1 1 calc R . . C3 C 0.9614(12) -0.1305(8) 0.3910(6) 0.032(3) Uani 1 1 d . . . H3 H 0.9036 -0.1759 0.4050 0.038 Uiso 1 1 calc R . . C4 C 0.9479(13) -0.0483(8) 0.4237(6) 0.032(3) Uani 1 1 d . . . H4 H 0.8801 -0.0278 0.4625 0.039 Uiso 1 1 calc R . . C5 C 1.0557(13) -0.0010(8) 0.3874(6) 0.032(3) Uani 1 1 d . . . H5 H 1.0745 0.0562 0.3986 0.039 Uiso 1 1 calc R . . C6 C 1.0408(11) -0.0861(8) 0.1496(5) 0.022(2) Uani 1 1 d . . . C7 C 1.1527(13) -0.0782(8) 0.0978(6) 0.029(3) Uani 1 1 d . . . H7 H 1.1728 -0.0172 0.0828 0.035 Uiso 1 1 calc R . . C8 C 1.2359(14) -0.1575(9) 0.0673(6) 0.038(3) Uani 1 1 d . . . H8 H 1.3150 -0.1512 0.0327 0.046 Uiso 1 1 calc R . . C9 C 1.2048(13) -0.2457(9) 0.0868(6) 0.036(3) Uani 1 1 d . . . H9 H 1.2602 -0.3000 0.0648 0.043 Uiso 1 1 calc R . . C10 C 1.0910(14) -0.2549(8) 0.1393(6) 0.036(3) Uani 1 1 d . . . H10 H 1.0681 -0.3154 0.1523 0.043 Uiso 1 1 calc R . . C11 C 1.0124(12) -0.1774(8) 0.1722(6) 0.029(3) Uani 1 1 d . . . H11 H 0.9395 -0.1848 0.2099 0.035 Uiso 1 1 calc R . . C12 C 0.7553(11) 0.0450(7) 0.1425(5) 0.019(2) Uani 1 1 d . . . C13 C 0.6557(11) 0.1354(8) 0.1406(6) 0.026(3) Uani 1 1 d . . . H13 H 0.6833 0.1855 0.1585 0.031 Uiso 1 1 calc R . . C14 C 0.5186(12) 0.1551(8) 0.1137(6) 0.027(3) Uani 1 1 d . . . H14 H 0.4531 0.2172 0.1143 0.032 Uiso 1 1 calc R . . C15 C 0.4783(13) 0.0856(8) 0.0866(6) 0.032(3) Uani 1 1 d . . . H15 H 0.3841 0.0992 0.0682 0.038 Uiso 1 1 calc R . . C16 C 0.5715(13) -0.0037(9) 0.0854(7) 0.041(3) Uani 1 1 d . . . H16 H 0.5413 -0.0516 0.0661 0.049 Uiso 1 1 calc R . . C17 C 0.7131(12) -0.0263(8) 0.1127(6) 0.027(3) Uani 1 1 d . . . H17 H 0.7781 -0.0883 0.1110 0.033 Uiso 1 1 calc R . . C18 C 1.0059(11) 0.1169(7) 0.1510(5) 0.018(2) Uani 1 1 d . . . C19 C 1.0892(11) 0.1539(8) 0.1910(6) 0.024(3) Uani 1 1 d . . . H19 H 1.1073 0.1253 0.2382 0.029 Uiso 1 1 calc R . . C20 C 1.1444(13) 0.2306(8) 0.1630(6) 0.031(3) Uani 1 1 d . . . H20 H 1.2053 0.2523 0.1902 0.037 Uiso 1 1 calc R . . C21 C 1.1137(12) 0.2779(8) 0.0956(6) 0.032(3) Uani 1 1 d . . . H21 H 1.1465 0.3341 0.0778 0.038 Uiso 1 1 calc R . . C22 C 1.0341(13) 0.2406(8) 0.0552(6) 0.035(3) Uani 1 1 d . . . H22 H 1.0159 0.2700 0.0082 0.042 Uiso 1 1 calc R . . C23 C 0.9811(12) 0.1626(7) 0.0813(5) 0.025(3) Uani 1 1 d . . . H23 H 0.9268 0.1385 0.0523 0.030 Uiso 1 1 calc R . . C24 C 0.1707(12) 0.4389(8) 0.4765(6) 0.031(3) Uani 1 1 d . . . H24 H 0.1386 0.5071 0.4713 0.038 Uiso 1 1 calc R . . C25 C 0.2860(12) 0.3812(8) 0.5160(6) 0.031(3) Uani 1 1 d . . . H25 H 0.3468 0.4045 0.5421 0.037 Uiso 1 1 calc R . . C26 C 0.2983(12) 0.2840(8) 0.5113(5) 0.025(3) Uani 1 1 d . . . H26 H 0.3667 0.2305 0.5337 0.029 Uiso 1 1 calc R . . C27 C 0.1895(12) 0.2811(8) 0.4670(6) 0.030(3) Uani 1 1 d . . . H27 H 0.1726 0.2244 0.4540 0.036 Uiso 1 1 calc R . . C28 C 0.1110(11) 0.3743(8) 0.4454(6) 0.029(3) Uani 1 1 d . . . H28 H 0.0317 0.3921 0.4153 0.035 Uiso 1 1 calc R . . C29 C 0.3842(11) 0.4451(7) 0.2169(5) 0.019(2) Uani 1 1 d . . . C30 C 0.5399(12) 0.4086(7) 0.2090(5) 0.022(2) Uani 1 1 d . . . H30 H 0.5948 0.3951 0.2498 0.026 Uiso 1 1 calc R . . C31 C 0.6132(13) 0.3924(8) 0.1447(6) 0.029(3) Uani 1 1 d . . . H31 H 0.7178 0.3687 0.1403 0.035 Uiso 1 1 calc R . . C32 C 0.5315(14) 0.4114(8) 0.0853(6) 0.034(3) Uani 1 1 d . . . H32 H 0.5813 0.4006 0.0401 0.041 Uiso 1 1 calc R . . C33 C 0.3825(13) 0.4450(8) 0.0913(6) 0.032(3) Uani 1 1 d . . . H33 H 0.3285 0.4570 0.0503 0.038 Uiso 1 1 calc R . . C34 C 0.3082(13) 0.4620(7) 0.1568(6) 0.027(3) Uani 1 1 d . . . H34 H 0.2034 0.4856 0.1604 0.033 Uiso 1 1 calc R . . C35 C 0.1041(11) 0.5153(7) 0.2940(5) 0.022(2) Uani 1 1 d . . . C36 C 0.0290(11) 0.4529(8) 0.2762(5) 0.020(2) Uani 1 1 d . . . H36 H 0.0834 0.3913 0.2648 0.024 Uiso 1 1 calc R . . C37 C -0.1221(13) 0.4778(9) 0.2747(6) 0.035(3) Uani 1 1 d . . . H37 H -0.1712 0.4345 0.2611 0.042 Uiso 1 1 calc R . . C38 C -0.2037(12) 0.5671(10) 0.2934(6) 0.035(3) Uani 1 1 d . . . H38 H -0.3089 0.5835 0.2950 0.042 Uiso 1 1 calc R . . C39 C -0.1296(12) 0.6324(8) 0.3096(6) 0.029(3) Uani 1 1 d . . . H39 H -0.1841 0.6943 0.3204 0.035 Uiso 1 1 calc R . . C40 C 0.0215(11) 0.6070(8) 0.3100(5) 0.026(3) Uani 1 1 d . . . H40 H 0.0713 0.6515 0.3212 0.031 Uiso 1 1 calc R . . C41 C 0.3597(10) 0.5865(7) 0.3061(5) 0.021(2) Uani 1 1 d . . . C42 C 0.3713(11) 0.6154(7) 0.3707(5) 0.020(2) Uani 1 1 d . . . H42 H 0.3543 0.5765 0.4137 0.024 Uiso 1 1 calc R . . C43 C 0.4086(11) 0.7033(7) 0.3718(6) 0.027(3) Uani 1 1 d . . . H43 H 0.4158 0.7248 0.4156 0.033 Uiso 1 1 calc R . . C44 C 0.4341(11) 0.7568(7) 0.3090(6) 0.026(3) Uani 1 1 d . . . H44 H 0.4621 0.8150 0.3097 0.031 Uiso 1 1 calc R . . C45 C 0.4208(11) 0.7298(8) 0.2454(6) 0.026(3) Uani 1 1 d . . . H45 H 0.4354 0.7698 0.2026 0.031 Uiso 1 1 calc R . . C46 C 0.3858(11) 0.6435(7) 0.2436(6) 0.022(2) Uani 1 1 d . . . H46 H 0.3795 0.6232 0.1993 0.027 Uiso 1 1 calc R . . C47 C -0.2661(15) 0.6224(11) 0.1187(7) 0.055(4) Uani 1 1 d . . . H47A H -0.3253 0.5828 0.1496 0.066 Uiso 1 1 calc R . . H47B H -0.2294 0.6593 0.1492 0.066 Uiso 1 1 calc R . . Cl1 Cl -0.1124(4) 0.5456(3) 0.07567(18) 0.0527(9) Uani 1 1 d . . . Cl2 Cl -0.3785(4) 0.7017(3) 0.05884(19) 0.0640(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0174(5) 0.0174(5) 0.0221(5) -0.0031(4) -0.0032(3) -0.0055(4) Ru2 0.0149(5) 0.0184(5) 0.0195(5) -0.0023(3) -0.0001(3) -0.0056(4) Te1 0.0241(4) 0.0223(4) 0.0402(5) -0.0069(3) -0.0025(3) -0.0124(3) Te2 0.0235(4) 0.0235(4) 0.0331(4) 0.0022(3) -0.0001(3) -0.0105(3) Te3 0.0176(4) 0.0180(4) 0.0220(4) -0.0027(3) -0.0024(3) -0.0070(3) Te4 0.0169(4) 0.0177(4) 0.0251(4) -0.0049(3) -0.0001(3) -0.0063(3) Te5 0.0227(4) 0.0263(4) 0.0305(4) -0.0086(3) -0.0083(3) -0.0014(3) Te6 0.0166(4) 0.0210(4) 0.0271(4) -0.0062(3) -0.0023(3) -0.0073(3) P1 0.0208(15) 0.0201(15) 0.0230(15) -0.0049(12) -0.0044(11) -0.0074(13) P2 0.0156(15) 0.0207(15) 0.0228(15) -0.0043(11) -0.0021(11) -0.0064(12) C1 0.018(6) 0.025(6) 0.042(7) 0.006(5) -0.001(5) -0.008(5) C2 0.016(6) 0.030(7) 0.039(7) -0.013(5) -0.010(5) 0.006(5) C3 0.029(7) 0.032(7) 0.032(7) 0.012(5) -0.007(5) -0.009(6) C4 0.036(7) 0.038(7) 0.013(6) 0.006(5) -0.001(5) 0.003(6) C5 0.034(7) 0.026(6) 0.036(7) -0.010(5) -0.019(6) 0.003(6) C6 0.010(5) 0.033(6) 0.024(6) -0.004(5) 0.001(4) -0.005(5) C7 0.041(8) 0.024(6) 0.024(6) -0.002(5) -0.009(5) -0.008(6) C8 0.034(7) 0.042(8) 0.037(7) -0.008(6) 0.005(6) -0.007(6) C9 0.032(7) 0.035(7) 0.034(7) -0.011(6) -0.002(6) 0.008(6) C10 0.045(8) 0.024(6) 0.038(7) -0.003(5) -0.025(6) 0.003(6) C11 0.031(7) 0.034(7) 0.020(6) -0.006(5) -0.004(5) -0.003(6) C12 0.015(6) 0.022(6) 0.021(6) -0.001(4) -0.010(4) -0.006(5) C13 0.018(6) 0.024(6) 0.034(7) -0.004(5) -0.002(5) -0.002(5) C14 0.018(6) 0.020(6) 0.038(7) 0.000(5) -0.002(5) 0.002(5) C15 0.027(7) 0.030(7) 0.038(7) 0.003(5) -0.013(5) -0.005(6) C16 0.029(7) 0.047(8) 0.055(9) -0.006(7) -0.016(6) -0.020(7) C17 0.025(7) 0.019(6) 0.036(7) -0.008(5) -0.008(5) 0.003(5) C18 0.014(6) 0.019(5) 0.023(6) -0.014(4) 0.002(4) -0.004(5) C19 0.014(6) 0.033(7) 0.022(6) -0.013(5) 0.004(4) 0.000(5) C20 0.033(7) 0.032(7) 0.036(7) -0.008(5) 0.000(5) -0.021(6) C21 0.028(7) 0.031(7) 0.038(7) -0.001(6) 0.002(5) -0.014(6) C22 0.039(8) 0.031(7) 0.029(7) 0.004(5) -0.004(5) -0.003(6) C23 0.035(7) 0.022(6) 0.026(6) -0.006(5) -0.007(5) -0.018(5) C24 0.023(7) 0.024(6) 0.042(7) 0.001(5) 0.008(5) -0.004(5) C25 0.026(7) 0.048(8) 0.021(6) -0.016(5) 0.011(5) -0.016(6) C26 0.023(6) 0.027(6) 0.017(6) 0.006(5) 0.009(5) -0.003(5) C27 0.031(7) 0.036(7) 0.034(7) -0.018(5) 0.018(5) -0.027(6) C28 0.008(6) 0.041(7) 0.035(7) 0.002(6) 0.000(5) -0.005(5) C29 0.017(6) 0.017(5) 0.024(6) -0.001(4) -0.001(4) -0.009(5) C30 0.028(7) 0.018(6) 0.019(6) 0.003(4) -0.006(5) -0.005(5) C31 0.027(7) 0.030(7) 0.027(7) 0.001(5) 0.002(5) -0.005(6) C32 0.047(8) 0.029(7) 0.030(7) -0.007(5) 0.015(6) -0.021(6) C33 0.036(8) 0.040(7) 0.020(6) -0.005(5) 0.007(5) -0.016(6) C34 0.030(7) 0.024(6) 0.028(7) -0.010(5) 0.001(5) -0.007(5) C35 0.017(6) 0.024(6) 0.022(6) 0.000(5) -0.004(4) 0.000(5) C36 0.015(6) 0.025(6) 0.020(6) -0.001(5) -0.005(4) -0.004(5) C37 0.031(7) 0.045(8) 0.033(7) -0.004(6) -0.003(5) -0.018(6) C38 0.012(6) 0.067(9) 0.023(6) 0.005(6) -0.002(5) -0.011(6) C39 0.024(7) 0.030(6) 0.031(7) -0.003(5) -0.001(5) -0.005(6) C40 0.017(6) 0.026(6) 0.033(7) -0.002(5) 0.010(5) -0.004(5) C41 0.003(5) 0.023(6) 0.034(7) -0.005(5) -0.005(4) 0.002(5) C42 0.017(6) 0.019(6) 0.025(6) -0.007(4) 0.004(4) -0.008(5) C43 0.017(6) 0.020(6) 0.048(8) -0.012(5) -0.011(5) -0.002(5) C44 0.014(6) 0.018(6) 0.050(8) -0.006(5) 0.000(5) -0.010(5) C45 0.019(6) 0.024(6) 0.034(7) 0.001(5) -0.002(5) -0.005(5) C46 0.016(6) 0.017(6) 0.032(6) 0.000(5) 0.001(5) -0.003(5) C47 0.044(9) 0.074(11) 0.048(9) -0.021(8) 0.008(7) -0.014(8) Cl1 0.043(2) 0.051(2) 0.052(2) 0.0044(17) 0.0020(16) 0.0007(17) Cl2 0.049(2) 0.076(3) 0.048(2) -0.0033(19) -0.0022(17) 0.015(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ru1 C4 62.2(4) . . ? C1 Ru1 C5 36.8(4) . . ? C4 Ru1 C5 37.6(4) . . ? C1 Ru1 C3 61.5(4) . . ? C4 Ru1 C3 36.7(4) . . ? C5 Ru1 C3 61.5(4) . . ? C1 Ru1 C2 37.9(4) . . ? C4 Ru1 C2 62.2(4) . . ? C5 Ru1 C2 62.3(4) . . ? C3 Ru1 C2 36.5(4) . . ? C1 Ru1 P1 98.2(3) . . ? C4 Ru1 P1 159.9(3) . . ? C5 Ru1 P1 127.7(3) . . ? C3 Ru1 P1 131.7(3) . . ? C2 Ru1 P1 100.0(3) . . ? C1 Ru1 Te4 116.3(3) . . ? C4 Ru1 Te4 103.1(3) . . ? C5 Ru1 Te4 92.2(3) . . ? C3 Ru1 Te4 138.8(3) . . ? C2 Ru1 Te4 153.3(3) . . ? P1 Ru1 Te4 89.28(7) . . ? C1 Ru1 Te1 147.0(3) . . ? C4 Ru1 Te1 101.9(3) . . ? C5 Ru1 Te1 139.2(3) . . ? C3 Ru1 Te1 88.2(3) . . ? C2 Ru1 Te1 109.5(3) . . ? P1 Ru1 Te1 92.60(8) . . ? Te4 Ru1 Te1 94.90(4) . . ? C28 Ru2 C27 36.6(4) . . ? C28 Ru2 C25 61.7(4) . . ? C27 Ru2 C25 61.1(4) . . ? C28 Ru2 C24 37.8(4) . . ? C27 Ru2 C24 62.0(4) . . ? C25 Ru2 C24 36.8(4) . . ? C28 Ru2 C26 61.6(4) . . ? C27 Ru2 C26 36.8(4) . . ? C25 Ru2 C26 36.5(4) . . ? C24 Ru2 C26 61.8(4) . . ? C28 Ru2 P2 98.5(3) . . ? C27 Ru2 P2 130.2(3) . . ? C25 Ru2 P2 127.2(3) . . ? C24 Ru2 P2 96.7(3) . . ? C26 Ru2 P2 157.8(3) . . ? C28 Ru2 Te3 114.9(3) . . ? C27 Ru2 Te3 93.1(3) . . ? C25 Ru2 Te3 141.7(3) . . ? C24 Ru2 Te3 152.5(3) . . ? C26 Ru2 Te3 105.9(3) . . ? P2 Ru2 Te3 90.98(7) . . ? C28 Ru2 Te6 146.7(3) . . ? C27 Ru2 Te6 137.6(3) . . ? C25 Ru2 Te6 87.3(3) . . ? C24 Ru2 Te6 109.6(3) . . ? C26 Ru2 Te6 101.1(3) . . ? P2 Ru2 Te6 90.86(7) . . ? Te3 Ru2 Te6 96.62(3) . . ? Ru1 Te1 Te2 103.95(3) . . ? Te1 Te2 Te3 91.71(3) . . ? Ru2 Te3 Te2 104.95(3) . . ? Ru2 Te3 Te4 109.06(3) . . ? Te2 Te3 Te4 88.50(3) . . ? Ru1 Te4 Te5 105.40(3) . . ? Ru1 Te4 Te3 111.48(3) . . ? Te5 Te4 Te3 90.44(3) . . ? Te6 Te5 Te4 91.34(3) . . ? Ru2 Te6 Te5 102.79(3) . . ? C12 P1 C18 101.4(5) . . ? C12 P1 C6 102.0(5) . . ? C18 P1 C6 103.1(4) . . ? C12 P1 Ru1 117.4(3) . . ? C18 P1 Ru1 115.3(3) . . ? C6 P1 Ru1 115.4(3) . . ? C35 P2 C29 102.6(5) . . ? C35 P2 C41 102.9(5) . . ? C29 P2 C41 98.7(5) . . ? C35 P2 Ru2 110.1(3) . . ? C29 P2 Ru2 121.1(3) . . ? C41 P2 Ru2 119.0(3) . . ? C5 C1 C2 108.9(10) . . ? C5 C1 Ru1 72.3(6) . . ? C2 C1 Ru1 72.5(6) . . ? C5 C1 H1 125.5 . . ? C2 C1 H1 125.5 . . ? Ru1 C1 H1 121.3 . . ? C3 C2 C1 105.6(10) . . ? C3 C2 Ru1 71.0(6) . . ? C1 C2 Ru1 69.6(6) . . ? C3 C2 H2 127.2 . . ? C1 C2 H2 127.2 . . ? Ru1 C2 H2 123.9 . . ? C2 C3 C4 110.8(10) . . ? C2 C3 Ru1 72.5(6) . . ? C4 C3 Ru1 71.5(6) . . ? C2 C3 H3 124.6 . . ? C4 C3 H3 124.6 . . ? Ru1 C3 H3 123.0 . . ? C3 C4 C5 106.7(10) . . ? C3 C4 Ru1 71.7(6) . . ? C5 C4 Ru1 71.2(6) . . ? C3 C4 H4 126.7 . . ? C5 C4 H4 126.7 . . ? Ru1 C4 H4 122.1 . . ? C1 C5 C4 108.0(10) . . ? C1 C5 Ru1 70.9(6) . . ? C4 C5 Ru1 71.2(6) . . ? C1 C5 H5 126.0 . . ? C4 C5 H5 126.0 . . ? Ru1 C5 H5 123.5 . . ? C7 C6 C11 119.2(10) . . ? C7 C6 P1 122.8(8) . . ? C11 C6 P1 118.0(8) . . ? C6 C7 C8 121.0(11) . . ? C6 C7 H7 119.5 . . ? C8 C7 H7 119.5 . . ? C9 C8 C7 120.2(11) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C8 C9 C10 119.5(11) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? C11 C10 C9 120.6(12) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C10 C11 C6 119.4(11) . . ? C10 C11 H11 120.3 . . ? C6 C11 H11 120.3 . . ? C13 C12 C17 117.0(9) . . ? C13 C12 P1 120.6(8) . . ? C17 C12 P1 122.0(8) . . ? C14 C13 C12 122.7(10) . . ? C14 C13 H13 118.7 . . ? C12 C13 H13 118.7 . . ? C15 C14 C13 119.7(10) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C14 C15 C16 120.7(11) . . ? C14 C15 H15 119.6 . . ? C16 C15 H15 119.6 . . ? C15 C16 C17 121.0(11) . . ? C15 C16 H16 119.5 . . ? C17 C16 H16 119.5 . . ? C12 C17 C16 118.9(10) . . ? C12 C17 H17 120.5 . . ? C16 C17 H17 120.5 . . ? C19 C18 C23 117.3(9) . . ? C19 C18 P1 120.6(8) . . ? C23 C18 P1 121.9(7) . . ? C20 C19 C18 120.7(10) . . ? C20 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? C19 C20 C21 121.5(11) . . ? C19 C20 H20 119.3 . . ? C21 C20 H20 119.3 . . ? C22 C21 C20 118.0(10) . . ? C22 C21 H21 121.0 . . ? C20 C21 H21 121.0 . . ? C23 C22 C21 121.4(11) . . ? C23 C22 H22 119.3 . . ? C21 C22 H22 119.3 . . ? C22 C23 C18 120.9(10) . . ? C22 C23 H23 119.5 . . ? C18 C23 H23 119.5 . . ? C25 C24 C28 106.2(10) . . ? C25 C24 Ru2 71.6(6) . . ? C28 C24 Ru2 70.4(6) . . ? C25 C24 H24 126.9 . . ? C28 C24 H24 126.9 . . ? Ru2 C24 H24 122.9 . . ? C26 C25 C24 109.9(11) . . ? C26 C25 Ru2 72.8(6) . . ? C24 C25 Ru2 71.6(6) . . ? C26 C25 H25 125.0 . . ? C24 C25 H25 125.0 . . ? Ru2 C25 H25 122.2 . . ? C25 C26 C27 106.7(10) . . ? C25 C26 Ru2 70.7(6) . . ? C27 C26 Ru2 70.4(6) . . ? C25 C26 H26 126.6 . . ? C27 C26 H26 126.6 . . ? Ru2 C26 H26 123.9 . . ? C28 C27 C26 109.1(10) . . ? C28 C27 Ru2 71.2(6) . . ? C26 C27 Ru2 72.8(6) . . ? C28 C27 H27 125.4 . . ? C26 C27 H27 125.4 . . ? Ru2 C27 H27 122.2 . . ? C27 C28 C24 108.0(10) . . ? C27 C28 Ru2 72.2(6) . . ? C24 C28 Ru2 71.8(6) . . ? C27 C28 H28 126.0 . . ? C24 C28 H28 126.0 . . ? Ru2 C28 H28 121.8 . . ? C34 C29 C30 117.4(9) . . ? C34 C29 P2 126.0(8) . . ? C30 C29 P2 116.4(7) . . ? C31 C30 C29 121.8(10) . . ? C31 C30 H30 119.1 . . ? C29 C30 H30 119.1 . . ? C30 C31 C32 118.6(11) . . ? C30 C31 H31 120.7 . . ? C32 C31 H31 120.7 . . ? C33 C32 C31 121.0(11) . . ? C33 C32 H32 119.5 . . ? C31 C32 H32 119.5 . . ? C32 C33 C34 120.3(11) . . ? C32 C33 H33 119.9 . . ? C34 C33 H33 119.9 . . ? C29 C34 C33 120.9(11) . . ? C29 C34 H34 119.6 . . ? C33 C34 H34 119.6 . . ? C36 C35 C40 118.4(10) . . ? C36 C35 P2 119.7(8) . . ? C40 C35 P2 121.4(8) . . ? C37 C36 C35 121.5(10) . . ? C37 C36 H36 119.2 . . ? C35 C36 H36 119.2 . . ? C36 C37 C38 119.7(11) . . ? C36 C37 H37 120.1 . . ? C38 C37 H37 120.1 . . ? C37 C38 C39 119.6(11) . . ? C37 C38 H38 120.2 . . ? C39 C38 H38 120.2 . . ? C40 C39 C38 120.0(11) . . ? C40 C39 H39 120.0 . . ? C38 C39 H39 120.0 . . ? C39 C40 C35 120.7(11) . . ? C39 C40 H40 119.7 . . ? C35 C40 H40 119.7 . . ? C42 C41 C46 119.9(10) . . ? C42 C41 P2 118.4(8) . . ? C46 C41 P2 121.7(8) . . ? C41 C42 C43 119.3(10) . . ? C41 C42 H42 120.4 . . ? C43 C42 H42 120.4 . . ? C44 C43 C42 118.8(10) . . ? C44 C43 H43 120.6 . . ? C42 C43 H43 120.6 . . ? C45 C44 C43 122.3(10) . . ? C45 C44 H44 118.9 . . ? C43 C44 H44 118.9 . . ? C44 C45 C46 119.4(10) . . ? C44 C45 H45 120.3 . . ? C46 C45 H45 120.3 . . ? C45 C46 C41 120.3(10) . . ? C45 C46 H46 119.9 . . ? C41 C46 H46 119.9 . . ? Cl2 C47 Cl1 112.1(7) . . ? Cl2 C47 H47A 109.2 . . ? Cl1 C47 H47A 109.2 . . ? Cl2 C47 H47B 109.2 . . ? Cl1 C47 H47B 109.2 . . ? H47A C47 H47B 107.9 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C1 2.199(11) . ? Ru1 C4 2.217(10) . ? Ru1 C5 2.217(11) . ? Ru1 C3 2.219(10) . ? Ru1 C2 2.238(10) . ? Ru1 P1 2.294(3) . ? Ru1 Te4 2.5616(11) . ? Ru1 Te1 2.6378(11) . ? Ru2 C28 2.203(10) . ? Ru2 C27 2.216(10) . ? Ru2 C25 2.220(10) . ? Ru2 C24 2.221(11) . ? Ru2 C26 2.246(9) . ? Ru2 P2 2.284(3) . ? Ru2 Te3 2.5628(11) . ? Ru2 Te6 2.6514(11) . ? Te1 Te2 2.7159(11) . ? Te2 Te3 2.7397(10) . ? Te3 Te4 3.0461(11) . ? Te4 Te5 2.7254(11) . ? Te5 Te6 2.7058(10) . ? P1 C12 1.828(10) . ? P1 C18 1.837(10) . ? P1 C6 1.845(11) . ? P2 C35 1.843(10) . ? P2 C29 1.846(10) . ? P2 C41 1.854(11) . ? C1 C5 1.392(16) . ? C1 C2 1.440(15) . ? C1 H1 0.9500 . ? C2 C3 1.396(15) . ? C2 H2 0.9500 . ? C3 C4 1.398(16) . ? C3 H3 0.9500 . ? C4 C5 1.428(16) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.376(14) . ? C6 C11 1.415(15) . ? C7 C8 1.378(16) . ? C7 H7 0.9500 . ? C8 C9 1.377(17) . ? C8 H8 0.9500 . ? C9 C10 1.400(17) . ? C9 H9 0.9500 . ? C10 C11 1.370(15) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C13 1.397(14) . ? C12 C17 1.411(14) . ? C13 C14 1.383(14) . ? C13 H13 0.9500 . ? C14 C15 1.351(15) . ? C14 H14 0.9500 . ? C15 C16 1.364(16) . ? C15 H15 0.9500 . ? C16 C17 1.421(15) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C19 1.400(14) . ? C18 C23 1.413(14) . ? C19 C20 1.364(15) . ? C19 H19 0.9500 . ? C20 C21 1.392(15) . ? C20 H20 0.9500 . ? C21 C22 1.382(16) . ? C21 H21 0.9500 . ? C22 C23 1.360(15) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C25 1.402(16) . ? C24 C28 1.435(16) . ? C24 H24 0.9500 . ? C25 C26 1.400(15) . ? C25 H25 0.9500 . ? C26 C27 1.410(15) . ? C26 H26 0.9500 . ? C27 C28 1.388(15) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C34 1.377(14) . ? C29 C30 1.416(14) . ? C30 C31 1.361(14) . ? C30 H30 0.9500 . ? C31 C32 1.393(16) . ? C31 H31 0.9500 . ? C32 C33 1.351(16) . ? C32 H32 0.9500 . ? C33 C34 1.387(14) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 C36 1.381(14) . ? C35 C40 1.413(14) . ? C36 C37 1.370(15) . ? C36 H36 0.9500 . ? C37 C38 1.397(17) . ? C37 H37 0.9500 . ? C38 C39 1.398(16) . ? C38 H38 0.9500 . ? C39 C40 1.367(14) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 C42 1.384(14) . ? C41 C46 1.387(14) . ? C42 C43 1.413(14) . ? C42 H42 0.9500 . ? C43 C44 1.364(15) . ? C43 H43 0.9500 . ? C44 C45 1.359(15) . ? C44 H44 0.9500 . ? C45 C46 1.381(14) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 Cl2 1.730(14) . ? C47 Cl1 1.779(13) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ?
1100764.cif	#------------------------------------------------------------------------------ #$Date: 2016-01-28 14:09:35 +0200 (Thu, 28 Jan 2016) $ #$Revision: 175230 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100764.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100764 loop_ _publ_author_name 'Mian Ji' 'Boumahdi Benkmil' 'Heinrich Vahrenkamp' _publ_section_title ; Zinc-Thiolate Complexes of the Bis(pyrazolyl)(thioimidazolyl)hydroborate Tripods for the Modeling of Thiolate Alkylating Enzymes ; _journal_issue 10 _journal_name_full 'Inorganic Chemistry' _journal_page_first 3518 _journal_page_last 3523 _journal_paper_doi 10.1021/ic0484147 _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C60 H92 B4 N24 S8 Zn4' _chemical_formula_weight 1710.94 _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 103.45(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 1 _cell_length_a 10.100(19) _cell_length_b 13.80(3) _cell_length_c 14.71(3) _cell_measurement_temperature 245(2) _cell_volume 1994(7) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 245(2) _diffrn_measured_fraction_theta_full 0.863 _diffrn_measured_fraction_theta_max 0.863 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1274 _diffrn_reflns_av_sigmaI/netI 0.2134 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 11699 _diffrn_reflns_theta_full 28.76 _diffrn_reflns_theta_max 28.76 _diffrn_reflns_theta_min 2.05 _exptl_absorpt_coefficient_mu 1.451 _exptl_crystal_density_diffrn 1.425 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 888 _refine_diff_density_max 1.311 _refine_diff_density_min -1.377 _refine_diff_density_rms 0.144 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.604 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 318 _refine_ls_number_reflns 4469 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.604 _refine_ls_R_factor_all 0.1094 _refine_ls_R_factor_gt 0.0474 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0662 _refine_ls_wR_factor_ref 0.0863 _reflns_number_gt 1725 _reflns_number_total 4469 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic0484147si20041111_081517_1.cif _cod_data_source_block benkam _cod_database_code 1100764 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn -0.09057(4) 0.19330(4) -0.06129(3) 0.03562(16) Uani 1 1 d . . . S1 S 0.14169(10) 0.20919(9) -0.05907(7) 0.0409(3) Uani 1 1 d . . . S2 S -0.24002(12) 0.13757(10) -0.18643(8) 0.0564(4) Uani 1 1 d . . . N1 N -0.0850(3) 0.1366(3) 0.0660(2) 0.0363(9) Uani 1 1 d . . . N2 N -0.0369(3) 0.1939(3) 0.1420(2) 0.0319(8) Uani 1 1 d . . . N3 N -0.1266(3) 0.3310(3) -0.0255(2) 0.0376(9) Uani 1 1 d . . . N4 N -0.0694(3) 0.3598(3) 0.0641(2) 0.0357(9) Uani 1 1 d . . . N5 N 0.1739(3) 0.2863(2) 0.1199(2) 0.0287(8) Uani 1 1 d . . . N6 N 0.3663(3) 0.2633(2) 0.0750(2) 0.0296(8) Uani 1 1 d . . . C1 C -0.0531(5) 0.1469(4) 0.2185(3) 0.0444(13) Uani 1 1 d . . . C2 C -0.1116(5) 0.0590(4) 0.1929(4) 0.0514(15) Uani 1 1 d . . . C3 C -0.1299(5) 0.0559(4) 0.0974(4) 0.0442(13) Uani 1 1 d . . . C4 C -0.1121(5) 0.4503(4) 0.0772(4) 0.0466(13) Uani 1 1 d . . . C5 C -0.1988(5) 0.4818(4) -0.0045(4) 0.0564(16) Uani 1 1 d . . . C6 C -0.2043(4) 0.4057(4) -0.0658(4) 0.0483(14) Uani 1 1 d . . . C7 C 0.2827(4) 0.3160(3) 0.1910(3) 0.0366(11) Uani 1 1 d . . . C8 C 0.3984(4) 0.3024(3) 0.1645(3) 0.0358(11) Uani 1 1 d . . . C9 C 0.2266(4) 0.2536(3) 0.0489(3) 0.0285(10) Uani 1 1 d . . . C10 C 0.4691(4) 0.2390(3) 0.0187(3) 0.0343(11) Uani 1 1 d . . . C11 C 0.4619(5) 0.1320(4) -0.0054(5) 0.0564(16) Uani 1 1 d . . . C12 C 0.6117(5) 0.2606(5) 0.0805(4) 0.0521(16) Uani 1 1 d . . . C13 C 0.4466(5) 0.3050(5) -0.0659(4) 0.0503(15) Uani 1 1 d . . . C14 C -0.2574(8) 0.0082(5) -0.1629(6) 0.072(2) Uani 1 1 d . . . C15 C -0.3639(15) -0.0352(8) -0.2388(7) 0.131(6) Uani 1 1 d . . . B1 B 0.0252(4) 0.2956(4) 0.1367(3) 0.0335(12) Uani 1 1 d . . . H1 H 0.047(3) 0.333(2) 0.207(2) 0.034(10) Uiso 1 1 d . . . H1A H -0.034(4) 0.176(3) 0.278(3) 0.061(15) Uiso 1 1 d . . . H2A H -0.135(4) 0.011(3) 0.228(3) 0.044(14) Uiso 1 1 d . . . H3A H -0.172(4) 0.006(3) 0.058(3) 0.056(15) Uiso 1 1 d . . . H4A H -0.089(4) 0.476(3) 0.137(3) 0.049(15) Uiso 1 1 d . . . H5A H -0.244(4) 0.542(3) -0.007(3) 0.063(16) Uiso 1 1 d . . . H6A H -0.260(4) 0.392(3) -0.131(3) 0.048(13) Uiso 1 1 d . . . H7A H 0.267(3) 0.337(2) 0.251(2) 0.021(10) Uiso 1 1 d . . . H8A H 0.488(3) 0.313(2) 0.195(2) 0.031(11) Uiso 1 1 d . . . H11A H 0.483(4) 0.094(3) 0.057(3) 0.067(17) Uiso 1 1 d . . . H11B H 0.535(4) 0.112(3) -0.042(3) 0.066(15) Uiso 1 1 d . . . H11C H 0.382(4) 0.109(4) -0.047(3) 0.070(17) Uiso 1 1 d . . . H12A H 0.624(4) 0.221(3) 0.133(3) 0.072(19) Uiso 1 1 d . . . H12B H 0.626(4) 0.337(3) 0.093(3) 0.058(16) Uiso 1 1 d . . . H12C H 0.669(4) 0.241(3) 0.044(3) 0.042(14) Uiso 1 1 d . . . H13A H 0.367(4) 0.294(3) -0.101(3) 0.050(14) Uiso 1 1 d . . . H13B H 0.517(4) 0.282(3) -0.103(3) 0.072(16) Uiso 1 1 d . . . H13C H 0.459(5) 0.371(4) -0.051(4) 0.11(3) Uiso 1 1 d . . . H14A H -0.187(6) -0.003(5) -0.182(5) 0.12(3) Uiso 1 1 d . . . H14B H -0.298(6) 0.015(4) -0.114(4) 0.12(3) Uiso 1 1 d . . . H15A H -0.375(6) -0.080(4) -0.224(4) 0.05(2) Uiso 1 1 d . . . H15B H -0.361(6) -0.012(5) -0.294(4) 0.13(3) Uiso 1 1 d . . . H15C H -0.466(8) -0.034(8) -0.225(6) 0.22(5) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0247(2) 0.0438(4) 0.0359(3) 0.0010(3) 0.0019(2) -0.0025(2) S1 0.0232(5) 0.0603(10) 0.0380(6) -0.0151(6) 0.0048(5) -0.0030(6) S2 0.0483(7) 0.0561(10) 0.0510(8) 0.0066(7) -0.0165(6) -0.0123(7) N1 0.0301(19) 0.037(3) 0.041(2) 0.0018(19) 0.0059(17) -0.0053(18) N2 0.0268(17) 0.036(2) 0.033(2) 0.0014(19) 0.0076(15) 0.0019(17) N3 0.0288(19) 0.040(3) 0.044(2) 0.0046(19) 0.0084(16) 0.0034(17) N4 0.0292(19) 0.030(3) 0.049(2) -0.0019(19) 0.0114(17) -0.0026(17) N5 0.0218(16) 0.034(2) 0.0306(19) -0.0023(17) 0.0061(14) -0.0005(16) N6 0.0221(17) 0.034(2) 0.0315(19) 0.0007(17) 0.0037(15) 0.0005(16) C1 0.045(3) 0.053(4) 0.036(3) 0.003(3) 0.011(2) -0.004(3) C2 0.058(3) 0.044(4) 0.050(4) 0.018(3) 0.008(3) -0.009(3) C3 0.046(3) 0.033(4) 0.050(3) 0.003(3) 0.003(2) -0.007(3) C4 0.037(3) 0.038(4) 0.067(4) -0.009(3) 0.017(3) -0.001(2) C5 0.045(3) 0.035(4) 0.092(5) 0.007(3) 0.022(3) 0.011(3) C6 0.032(3) 0.055(4) 0.061(4) 0.018(3) 0.015(3) 0.009(2) C7 0.032(2) 0.046(3) 0.029(2) -0.009(2) 0.0031(19) -0.003(2) C8 0.023(2) 0.044(3) 0.037(3) -0.002(2) 0.0002(19) -0.001(2) C9 0.022(2) 0.024(3) 0.039(3) 0.001(2) 0.0051(18) 0.0000(18) C10 0.024(2) 0.041(3) 0.039(3) -0.002(2) 0.0093(19) -0.002(2) C11 0.039(3) 0.055(4) 0.079(5) -0.011(4) 0.021(3) 0.006(3) C12 0.021(2) 0.079(5) 0.057(4) -0.001(4) 0.011(2) -0.002(3) C13 0.034(3) 0.074(5) 0.044(3) 0.008(3) 0.011(2) -0.002(3) C14 0.077(5) 0.057(5) 0.075(5) -0.006(4) 0.004(5) -0.003(4) C15 0.217(14) 0.066(7) 0.079(6) 0.009(6) -0.026(7) -0.077(8) B1 0.027(2) 0.038(4) 0.036(3) -0.007(3) 0.008(2) 0.004(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Zn1 N3 95.17(18) . . ? N1 Zn1 S2 120.01(16) . . ? N3 Zn1 S2 114.21(12) . . ? N1 Zn1 S1 102.20(10) . . ? N3 Zn1 S1 98.49(11) . . ? S2 Zn1 S1 121.75(10) . . ? C9 S1 Zn1 109.01(16) . . ? C14 S2 Zn1 104.9(2) . . ? C3 N1 N2 106.7(4) . . ? C3 N1 Zn1 135.3(3) . . ? N2 N1 Zn1 117.6(3) . . ? C1 N2 N1 108.5(4) . . ? C1 N2 B1 127.6(4) . . ? N1 N2 B1 123.8(4) . . ? C6 N3 N4 105.9(4) . . ? C6 N3 Zn1 136.4(4) . . ? N4 N3 Zn1 117.5(3) . . ? C4 N4 N3 109.2(4) . . ? C4 N4 B1 127.0(4) . . ? N3 N4 B1 123.8(4) . . ? C9 N5 C7 107.1(3) . . ? C9 N5 B1 134.8(3) . . ? C7 N5 B1 118.1(3) . . ? C9 N6 C8 107.4(3) . . ? C9 N6 C10 128.0(3) . . ? C8 N6 C10 124.6(3) . . ? N2 C1 C2 109.1(5) . . ? C1 C2 C3 104.9(5) . . ? N1 C3 C2 110.7(5) . . ? N4 C4 C5 109.0(5) . . ? C6 C5 C4 104.5(5) . . ? N3 C6 C5 111.4(5) . . ? C8 C7 N5 109.5(4) . . ? C7 C8 N6 107.8(4) . . ? N5 C9 N6 108.2(3) . . ? N5 C9 S1 128.7(3) . . ? N6 C9 S1 123.1(3) . . ? N6 C10 C11 110.1(4) . . ? N6 C10 C13 109.0(4) . . ? C11 C10 C13 113.8(5) . . ? N6 C10 C12 107.5(4) . . ? C11 C10 C12 108.3(4) . . ? C13 C10 C12 107.9(4) . . ? C15 C14 S2 109.6(6) . . ? N4 B1 N2 111.3(3) . . ? N4 B1 N5 113.4(4) . . ? N2 B1 N5 110.2(4) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N1 2.018(5) . ? Zn1 N3 2.028(5) . ? Zn1 S2 2.228(3) . ? Zn1 S1 2.349(5) . ? S1 C9 1.732(5) . ? S2 C14 1.835(8) . ? N1 C3 1.326(6) . ? N1 N2 1.363(5) . ? N2 C1 1.342(6) . ? N2 B1 1.547(6) . ? N3 C6 1.346(6) . ? N3 N4 1.369(5) . ? N4 C4 1.349(6) . ? N4 B1 1.538(6) . ? N5 C9 1.355(5) . ? N5 C7 1.391(5) . ? N5 B1 1.583(6) . ? N6 C9 1.380(5) . ? N6 C8 1.389(5) . ? N6 C10 1.508(5) . ? C1 C2 1.364(7) . ? C2 C3 1.374(7) . ? C4 C5 1.381(7) . ? C5 C6 1.377(7) . ? C7 C8 1.328(6) . ? C10 C11 1.516(7) . ? C10 C13 1.517(7) . ? C10 C12 1.543(6) . ? C14 C15 1.484(10) . ?
1100765.cif	#------------------------------------------------------------------------------ #$Date: 2016-01-28 14:09:35 +0200 (Thu, 28 Jan 2016) $ #$Revision: 175230 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100765.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100765 loop_ _publ_author_name 'Mian Ji' 'Boumahdi Benkmil' 'Heinrich Vahrenkamp' _publ_section_title ; Zinc-Thiolate Complexes of the Bis(pyrazolyl)(thioimidazolyl)hydroborate Tripods for the Modeling of Thiolate Alkylating Enzymes ; _journal_issue 10 _journal_name_full 'Inorganic Chemistry' _journal_page_first 3518 _journal_page_last 3523 _journal_paper_doi 10.1021/ic0484147 _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C20 H25 B N6 S2 Zn' _chemical_formula_weight 489.76 _space_group_IT_number 19 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P 21 21 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 9.392(4) _cell_length_b 12.838(5) _cell_length_c 19.134(8) _cell_measurement_temperature 230(2) _cell_volume 2307.1(16) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 230(2) _diffrn_measured_fraction_theta_full 0.950 _diffrn_measured_fraction_theta_max 0.950 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0538 _diffrn_reflns_av_sigmaI/netI 0.0411 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 19702 _diffrn_reflns_theta_full 28.81 _diffrn_reflns_theta_max 28.81 _diffrn_reflns_theta_min 1.91 _exptl_absorpt_coefficient_mu 1.265 _exptl_absorpt_correction_type none _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.410 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needles _exptl_crystal_F_000 1016 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.32 _refine_diff_density_max 0.531 _refine_diff_density_min -0.368 _refine_diff_density_rms 0.057 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.020(10) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 275 _refine_ls_number_reflns 5559 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.067 _refine_ls_R_factor_all 0.0451 _refine_ls_R_factor_gt 0.0333 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0315P)^2^+0.3873P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0719 _refine_ls_wR_factor_ref 0.0777 _reflns_number_gt 4629 _reflns_number_total 5559 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic0484147si20041111_081517_2.cif _cod_data_source_block jiwm _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_cell_volume 2307.2(17) _cod_database_code 1100765 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.26979(3) 0.32479(2) 0.254186(14) 0.03516(8) Uani 1 1 d . . . S1 S 0.35353(7) 0.34010(5) 0.36836(3) 0.03847(15) Uani 1 1 d . . . S2 S 0.05406(8) 0.25187(8) 0.25761(4) 0.0681(3) Uani 1 1 d . . . N1 N 0.6091(2) 0.40409(15) 0.31099(11) 0.0323(5) Uani 1 1 d . . . N2 N 0.6072(2) 0.39801(17) 0.42598(11) 0.0393(5) Uani 1 1 d . . . N6 N 0.4246(2) 0.25525(15) 0.19850(11) 0.0339(5) Uani 1 1 d . . . C7 C 0.5270(3) 0.38351(18) 0.36713(13) 0.0327(5) Uani 1 1 d . . . N5 N 0.5541(2) 0.30161(15) 0.19835(10) 0.0324(5) Uani 1 1 d . . . C10 C 0.2539(4) 0.5484(2) 0.18988(13) 0.0473(7) Uani 1 1 d . . . H10A H 0.1544 0.5554 0.1877 0.057 Uiso 1 1 calc R . . N4 N 0.3217(2) 0.46558(17) 0.21455(11) 0.0383(5) Uani 1 1 d . . . N3 N 0.4634(2) 0.48606(15) 0.20945(11) 0.0352(5) Uani 1 1 d . . . C11 C 0.6461(3) 0.2409(2) 0.16415(14) 0.0437(6) Uani 1 1 d . . . H11A H 0.7429 0.2561 0.1569 0.052 Uiso 1 1 calc R . . C9 C 0.3498(4) 0.6224(2) 0.16795(15) 0.0539(8) Uani 1 1 d . . . H9A H 0.3292 0.6878 0.1483 0.065 Uiso 1 1 calc R . . C13 C 0.4381(3) 0.1666(2) 0.16378(13) 0.0443(6) Uani 1 1 d . . . H13A H 0.3639 0.1191 0.1554 0.053 Uiso 1 1 calc R . . C14 C 0.0309(3) 0.2038(3) 0.17126(14) 0.0459(7) Uani 1 1 d . . . C6 C 0.7432(3) 0.4285(2) 0.33536(15) 0.0421(6) Uani 1 1 d . . . H6A H 0.8223 0.4448 0.3074 0.050 Uiso 1 1 calc R . . C5 C 0.7426(3) 0.4252(2) 0.40525(15) 0.0465(7) Uani 1 1 d . . . H5A H 0.8203 0.4390 0.4348 0.056 Uiso 1 1 calc R . . C8 C 0.4812(4) 0.5812(2) 0.18067(14) 0.0459(7) Uani 1 1 d . . . H8A H 0.5689 0.6135 0.1711 0.055 Uiso 1 1 calc R . . C12 C 0.5781(3) 0.1540(2) 0.14152(14) 0.0500(7) Uani 1 1 d . . . H12A H 0.6170 0.0979 0.1164 0.060 Uiso 1 1 calc R . . C17 C -0.0267(4) 0.1296(3) 0.03624(16) 0.0529(8) Uani 1 1 d . . . C19 C -0.0307(3) 0.1087(2) 0.16052(16) 0.0465(7) Uani 1 1 d . . . H19A H -0.0539 0.0670 0.1992 0.056 Uiso 1 1 calc R . . C4 C 0.5622(3) 0.3854(3) 0.50118(14) 0.0501(7) Uani 1 1 d . . . B1 B 0.5817(3) 0.4097(2) 0.22964(15) 0.0335(6) Uani 1 1 d . . . C18 C -0.0593(3) 0.0729(2) 0.09423(17) 0.0497(7) Uani 1 1 d . . . H18A H -0.1026 0.0074 0.0888 0.060 Uiso 1 1 calc R . . C2 C 0.6849(4) 0.4210(3) 0.54827(17) 0.0715(11) Uani 1 1 d . . . H2A H 0.7051 0.4939 0.5395 0.107 Uiso 1 1 calc R . . H2B H 0.7690 0.3798 0.5383 0.107 Uiso 1 1 calc R . . H2C H 0.6582 0.4119 0.5969 0.107 Uiso 1 1 calc R . . C20 C -0.0591(5) 0.0908(3) -0.03617(18) 0.0821(12) Uani 1 1 d . . . H20A H -0.1047 0.0232 -0.0333 0.123 Uiso 1 1 calc R . . H20B H 0.0287 0.0848 -0.0625 0.123 Uiso 1 1 calc R . . H20C H -0.1223 0.1395 -0.0594 0.123 Uiso 1 1 calc R . . C16 C 0.0386(5) 0.2237(3) 0.04672(16) 0.0742(12) Uani 1 1 d . . . H16A H 0.0648 0.2639 0.0077 0.089 Uiso 1 1 calc R . . C1 C 0.4352(4) 0.4551(3) 0.51536(17) 0.0719(10) Uani 1 1 d . . . H1A H 0.3562 0.4340 0.4859 0.108 Uiso 1 1 calc R . . H1B H 0.4603 0.5268 0.5052 0.108 Uiso 1 1 calc R . . H1C H 0.4078 0.4490 0.5641 0.108 Uiso 1 1 calc R . . C15 C 0.0673(4) 0.2615(3) 0.11307(16) 0.0701(11) Uani 1 1 d . . . H15A H 0.1116 0.3266 0.1185 0.084 Uiso 1 1 calc R . . C3 C 0.5327(5) 0.2711(3) 0.51534(18) 0.0730(11) Uani 1 1 d . . . H3A H 0.4554 0.2476 0.4856 0.110 Uiso 1 1 calc R . . H3D H 0.5062 0.2621 0.5640 0.110 Uiso 1 1 calc R . . H3B H 0.6175 0.2306 0.5055 0.110 Uiso 1 1 calc R . . H1 H 0.678(3) 0.436(2) 0.2060(14) 0.040(8) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.03323(13) 0.04149(15) 0.03077(14) 0.00052(14) 0.00092(12) -0.00308(11) S1 0.0376(3) 0.0497(4) 0.0282(3) 0.0009(3) 0.0011(2) -0.0051(3) S2 0.0451(4) 0.1224(8) 0.0369(4) -0.0072(5) 0.0048(4) -0.0328(4) N1 0.0330(11) 0.0304(10) 0.0334(11) -0.0045(9) -0.0011(9) 0.0005(9) N2 0.0417(12) 0.0428(12) 0.0335(11) -0.0043(10) -0.0065(10) 0.0042(10) N6 0.0424(12) 0.0272(10) 0.0323(11) -0.0026(9) 0.0022(9) -0.0022(9) C7 0.0408(13) 0.0268(12) 0.0306(12) -0.0034(10) -0.0023(11) 0.0039(10) N5 0.0364(11) 0.0302(11) 0.0306(10) -0.0030(8) 0.0047(9) 0.0032(9) C10 0.0643(19) 0.0504(16) 0.0273(12) -0.0017(11) -0.0038(13) 0.0218(16) N4 0.0481(13) 0.0368(11) 0.0299(11) 0.0020(9) 0.0045(9) 0.0077(10) N3 0.0500(13) 0.0264(11) 0.0290(11) -0.0004(8) 0.0011(10) -0.0032(9) C11 0.0458(15) 0.0456(16) 0.0397(14) -0.0014(13) 0.0063(12) 0.0137(13) C9 0.096(3) 0.0311(14) 0.0347(15) 0.0023(12) -0.0095(16) 0.0103(17) C13 0.0680(18) 0.0304(13) 0.0346(13) -0.0023(12) -0.0012(13) -0.0039(14) C14 0.0335(13) 0.072(2) 0.0318(14) 0.0028(13) -0.0013(11) -0.0058(13) C6 0.0345(14) 0.0425(14) 0.0492(15) -0.0029(12) -0.0012(12) -0.0011(12) C5 0.0379(15) 0.0526(16) 0.0491(16) -0.0076(13) -0.0106(13) 0.0015(13) C8 0.075(2) 0.0303(14) 0.0330(15) -0.0009(11) -0.0029(14) -0.0122(14) C12 0.073(2) 0.0371(15) 0.0394(15) -0.0069(12) 0.0091(15) 0.0141(14) C17 0.0562(18) 0.0599(19) 0.0426(16) 0.0031(15) -0.0079(15) -0.0088(16) C19 0.0430(15) 0.0521(17) 0.0446(16) 0.0090(14) 0.0099(13) -0.0008(14) C4 0.0551(18) 0.066(2) 0.0291(14) -0.0027(13) -0.0085(13) 0.0065(16) B1 0.0342(14) 0.0330(14) 0.0334(15) -0.0029(11) 0.0050(11) -0.0040(11) C18 0.0474(16) 0.0452(16) 0.0566(19) -0.0050(14) 0.0093(15) -0.0035(13) C2 0.074(2) 0.101(3) 0.0395(17) -0.0082(18) -0.0193(16) 0.001(2) C20 0.105(3) 0.092(3) 0.049(2) -0.0099(19) -0.011(2) -0.026(2) C16 0.112(3) 0.075(2) 0.0360(17) 0.0156(16) -0.0145(19) -0.036(2) C1 0.076(2) 0.104(3) 0.0358(17) -0.0167(18) 0.0000(17) 0.024(2) C15 0.096(3) 0.071(2) 0.0435(18) 0.0109(16) -0.0169(18) -0.042(2) C3 0.098(3) 0.077(2) 0.0444(19) 0.0176(18) -0.0114(19) -0.007(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 Zn1 N4 91.37(8) . . ? N6 Zn1 S2 119.03(7) . . ? N4 Zn1 S2 127.24(7) . . ? N6 Zn1 S1 106.86(7) . . ? N4 Zn1 S1 101.25(7) . . ? S2 Zn1 S1 108.31(3) . . ? C7 S1 Zn1 109.50(9) . . ? C14 S2 Zn1 103.25(9) . . ? C7 N1 C6 107.3(2) . . ? C7 N1 B1 134.5(2) . . ? C6 N1 B1 118.2(2) . . ? C7 N2 C5 107.8(2) . . ? C7 N2 C4 128.1(2) . . ? C5 N2 C4 124.1(2) . . ? C13 N6 N5 106.9(2) . . ? C13 N6 Zn1 135.76(19) . . ? N5 N6 Zn1 117.08(14) . . ? N1 C7 N2 108.3(2) . . ? N1 C7 S1 127.98(19) . . ? N2 C7 S1 123.64(19) . . ? C11 N5 N6 109.0(2) . . ? C11 N5 B1 127.6(2) . . ? N6 N5 B1 123.28(19) . . ? N4 C10 C9 110.4(3) . . ? C10 N4 N3 106.8(2) . . ? C10 N4 Zn1 137.3(2) . . ? N3 N4 Zn1 115.85(16) . . ? C8 N3 N4 109.0(2) . . ? C8 N3 B1 126.3(2) . . ? N4 N3 B1 124.6(2) . . ? N5 C11 C12 109.4(3) . . ? C8 C9 C10 105.6(2) . . ? N6 C13 C12 110.1(3) . . ? C19 C14 C15 117.6(3) . . ? C19 C14 S2 120.1(2) . . ? C15 C14 S2 122.2(2) . . ? C5 C6 N1 109.1(3) . . ? C6 C5 N2 107.4(2) . . ? N3 C8 C9 108.2(3) . . ? C11 C12 C13 104.6(2) . . ? C18 C17 C16 116.9(3) . . ? C18 C17 C20 121.9(3) . . ? C16 C17 C20 121.2(3) . . ? C14 C19 C18 121.3(3) . . ? N2 C4 C1 109.1(2) . . ? N2 C4 C3 109.0(2) . . ? C1 C4 C3 113.3(3) . . ? N2 C4 C2 108.5(3) . . ? C1 C4 C2 108.1(3) . . ? C3 C4 C2 108.7(3) . . ? N3 B1 N5 111.0(2) . . ? N3 B1 N1 113.4(2) . . ? N5 B1 N1 111.8(2) . . ? C17 C18 C19 121.9(3) . . ? C17 C16 C15 122.0(3) . . ? C14 C15 C16 120.3(3) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N6 2.011(2) . ? Zn1 N4 2.020(2) . ? Zn1 S2 2.2330(11) . ? Zn1 S1 2.3302(11) . ? S1 C7 1.722(3) . ? S2 C14 1.777(3) . ? N1 C7 1.348(3) . ? N1 C6 1.379(3) . ? N1 B1 1.580(4) . ? N2 C7 1.367(3) . ? N2 C5 1.377(4) . ? N2 C4 1.509(4) . ? N6 C13 1.324(3) . ? N6 N5 1.354(3) . ? N5 C11 1.334(3) . ? N5 B1 1.534(3) . ? C10 N4 1.326(3) . ? C10 C9 1.376(4) . ? N4 N3 1.360(3) . ? N3 C8 1.350(3) . ? N3 B1 1.531(4) . ? C11 C12 1.356(4) . ? C9 C8 1.364(5) . ? C13 C12 1.392(4) . ? C14 C19 1.366(4) . ? C14 C15 1.380(4) . ? C6 C5 1.338(4) . ? C17 C18 1.362(4) . ? C17 C16 1.370(5) . ? C17 C20 1.503(4) . ? C19 C18 1.376(4) . ? C4 C1 1.516(5) . ? C4 C3 1.517(5) . ? C4 C2 1.533(4) . ? C16 C15 1.385(4) . ?
1100766.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $ #$Revision: 176428 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100766.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100766 loop_ _publ_author_name 'Mian Ji' 'Boumahdi Benkmil' 'Heinrich Vahrenkamp' _publ_section_title ; Zinc-Thiolate Complexes of the Bis(pyrazolyl)(thioimidazolyl)hydroborate Tripods for the Modeling of Thiolate Alkylating Enzymes ; _journal_issue 10 _journal_name_full 'Inorganic Chemistry' _journal_page_first 3518 _journal_page_last 3523 _journal_paper_doi 10.1021/ic0484147 _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C19 H22 B Cl N6 S2 Zn' _chemical_formula_weight 510.18 _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 103.741(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 10.1030(17) _cell_length_b 23.398(4) _cell_length_c 10.1354(17) _cell_measurement_temperature 499(2) _cell_volume 2327.3(7) _diffrn_ambient_temperature 499(2) _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0341 _diffrn_reflns_av_sigmaI/netI 0.0588 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 15557 _diffrn_reflns_theta_max 30.04 _diffrn_reflns_theta_min 1.74 _exptl_absorpt_coefficient_mu 1.368 _exptl_absorpt_correction_type none _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.456 _exptl_crystal_density_method 'not measured' _exptl_crystal_description isometric _exptl_crystal_F_000 1048 _exptl_crystal_size_max 0.050 _exptl_crystal_size_mid 0.090 _exptl_crystal_size_min 0.200 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 275 _refine_ls_number_reflns 6438 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.002 _refine_ls_R_factor_all 0.0833 _refine_ls_R_factor_gt 0.0406 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0351P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0767 _refine_ls_wR_factor_ref 0.0903 _reflns_number_gt 3822 _reflns_number_total 6438 _reflns_threshold_expression >2sigma(I) _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_sg_symbol_H-M P2(1)/n _cod_database_code 1100766 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.17123(3) 1.120770(12) -0.53143(3) 0.03073(9) Uani 1 1 d . . . S1 S 0.19916(7) 1.13170(3) -0.75033(6) 0.0468(2) Uani 1 1 d . . . S2 S -0.05022(7) 1.10643(3) -0.54293(7) 0.0484(2) Uani 1 1 d . . . N1 N 0.47533(19) 1.14409(8) -0.63141(18) 0.0284(4) Uani 1 1 d . . . N2 N 0.42335(19) 1.13798(8) -0.85473(18) 0.0284(4) Uani 1 1 d . . . N3 N 0.45055(19) 1.08682(8) -0.42149(18) 0.0297(4) Uani 1 1 d . . . N4 N 0.3201(2) 1.06731(8) -0.43777(19) 0.0331(5) Uani 1 1 d . . . N5 N 0.4059(2) 1.19310(8) -0.42785(18) 0.0302(4) Uani 1 1 d . . . N6 N 0.2692(2) 1.19051(8) -0.43779(19) 0.0332(5) Uani 1 1 d . . . B1 B 0.4884(3) 1.14464(13) -0.4745(3) 0.0308(6) Uani 1 1 d . . . C1 C 0.2500(3) 1.18415(15) -1.0366(3) 0.0699(10) Uani 1 1 d . . . H1A H 0.1851 1.1829 -0.9811 0.105 Uiso 1 1 calc R . . H1B H 0.2029 1.1821 -1.1306 0.105 Uiso 1 1 calc R . . H1C H 0.3005 1.2193 -1.0201 0.105 Uiso 1 1 calc R . . C2 C 0.2752(3) 1.07621(14) -1.0260(3) 0.0685(10) Uani 1 1 d . . . H2A H 0.3408 1.0460 -1.0027 0.103 Uiso 1 1 calc R . . H2B H 0.2288 1.0730 -1.1201 0.103 Uiso 1 1 calc R . . H2C H 0.2103 1.0734 -0.9708 0.103 Uiso 1 1 calc R . . C3 C 0.4501(3) 1.13678(13) -1.0905(3) 0.0555(8) Uani 1 1 d . . . H3A H 0.5122 1.1052 -1.0697 0.083 Uiso 1 1 calc R . . H3B H 0.5001 1.1720 -1.0733 0.083 Uiso 1 1 calc R . . H3C H 0.4024 1.1351 -1.1844 0.083 Uiso 1 1 calc R . . C4 C 0.3477(3) 1.13375(12) -1.0014(2) 0.0400(6) Uani 1 1 d . . . C5 C 0.5633(2) 1.14318(10) -0.8117(2) 0.0344(6) Uani 1 1 d . . . H5A H 0.6247 1.1438 -0.8670 0.041 Uiso 1 1 calc R . . C6 C 0.5940(2) 1.14712(11) -0.6770(2) 0.0351(6) Uani 1 1 d . . . H6A H 0.6814 1.1513 -0.6221 0.042 Uiso 1 1 calc R . . C7 C 0.3701(2) 1.13819(10) -0.7428(2) 0.0283(5) Uani 1 1 d . . . C8 C 0.5368(3) 1.04798(11) -0.3505(2) 0.0386(6) Uani 1 1 d . . . H8A H 0.6312 1.0512 -0.3264 0.046 Uiso 1 1 calc R . . C9 C 0.4637(3) 1.00305(12) -0.3196(3) 0.0455(7) Uani 1 1 d . . . H9A H 0.4972 0.9703 -0.2711 0.055 Uiso 1 1 calc R . . C10 C 0.3292(3) 1.01665(11) -0.3759(2) 0.0414(6) Uani 1 1 d . . . H10A H 0.2553 0.9937 -0.3713 0.050 Uiso 1 1 calc R . . C11 C 0.4554(3) 1.24148(11) -0.3634(2) 0.0415(6) Uani 1 1 d . . . H11A H 0.5461 1.2530 -0.3438 0.050 Uiso 1 1 calc R . . C12 C 0.3505(3) 1.27088(12) -0.3315(3) 0.0487(7) Uani 1 1 d . . . H12A H 0.3550 1.3058 -0.2869 0.058 Uiso 1 1 calc R . . C13 C 0.2362(3) 1.23764(11) -0.3795(3) 0.0433(7) Uani 1 1 d . . . H13A H 0.1488 1.2469 -0.3722 0.052 Uiso 1 1 calc R . . C14 C -0.0672(2) 1.09960(12) -0.3723(3) 0.0392(6) Uani 1 1 d . . . C15 C -0.0977(3) 1.14662(12) -0.3014(3) 0.0472(7) Uani 1 1 d . . . H15A H -0.1012 1.1828 -0.3401 0.057 Uiso 1 1 calc R . . C16 C -0.1233(3) 1.14029(12) -0.1727(3) 0.0497(7) Uani 1 1 d . . . H16A H -0.1425 1.1721 -0.1253 0.060 Uiso 1 1 calc R . . C17 C -0.1198(2) 1.08707(12) -0.1172(3) 0.0405(6) Uani 1 1 d . . . C18 C -0.0890(3) 1.03978(12) -0.1850(3) 0.0425(7) Uani 1 1 d . . . H18A H -0.0856 1.0037 -0.1458 0.051 Uiso 1 1 calc R . . C19 C -0.0630(2) 1.04645(12) -0.3121(3) 0.0418(6) Uani 1 1 d . . . H19A H -0.0423 1.0145 -0.3580 0.050 Uiso 1 1 calc R . . Cl1 Cl -0.15460(8) 1.07846(4) 0.04249(7) 0.0588(2) Uani 1 1 d . . . H1 H 0.592(2) 1.1525(8) -0.4259(19) 0.020(5) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.02255(15) 0.03699(17) 0.03302(16) 0.00153(13) 0.00731(11) 0.00078(12) S1 0.0213(3) 0.0892(6) 0.0291(3) 0.0038(3) 0.0042(3) 0.0000(3) S2 0.0232(3) 0.0766(6) 0.0449(4) 0.0100(4) 0.0071(3) -0.0019(3) N1 0.0217(10) 0.0345(11) 0.0295(10) -0.0005(9) 0.0071(8) -0.0010(8) N2 0.0270(11) 0.0333(11) 0.0262(10) -0.0008(8) 0.0090(8) -0.0015(8) N3 0.0270(11) 0.0354(12) 0.0251(10) 0.0000(9) 0.0028(8) 0.0043(9) N4 0.0305(11) 0.0325(12) 0.0348(11) 0.0019(9) 0.0051(9) 0.0005(9) N5 0.0323(11) 0.0301(11) 0.0282(10) -0.0020(9) 0.0069(9) -0.0024(9) N6 0.0303(11) 0.0326(12) 0.0374(11) -0.0017(9) 0.0095(9) 0.0036(9) B1 0.0237(14) 0.0404(17) 0.0275(14) 0.0007(12) 0.0042(11) -0.0019(12) C1 0.066(2) 0.103(3) 0.0384(17) 0.0201(18) 0.0079(15) 0.026(2) C2 0.069(2) 0.092(3) 0.0454(18) -0.0236(18) 0.0159(16) -0.034(2) C3 0.057(2) 0.082(2) 0.0310(14) -0.0028(15) 0.0176(14) -0.0045(16) C4 0.0404(16) 0.0549(18) 0.0239(12) 0.0013(12) 0.0060(11) -0.0035(12) C5 0.0306(14) 0.0408(15) 0.0360(14) -0.0016(12) 0.0160(11) -0.0049(11) C6 0.0208(12) 0.0451(15) 0.0410(14) -0.0011(12) 0.0105(11) -0.0037(11) C7 0.0239(12) 0.0316(13) 0.0291(12) 0.0018(10) 0.0060(10) 0.0014(10) C8 0.0353(15) 0.0473(17) 0.0295(13) -0.0019(12) 0.0002(11) 0.0142(12) C9 0.0595(19) 0.0335(16) 0.0409(15) 0.0042(12) 0.0065(14) 0.0141(14) C10 0.0538(18) 0.0298(15) 0.0415(15) 0.0017(12) 0.0134(13) -0.0020(12) C11 0.0490(17) 0.0371(16) 0.0389(15) -0.0037(12) 0.0113(12) -0.0108(13) C12 0.064(2) 0.0317(16) 0.0518(17) -0.0100(13) 0.0173(15) -0.0015(14) C13 0.0492(17) 0.0350(16) 0.0493(16) 0.0007(13) 0.0187(13) 0.0089(13) C14 0.0181(12) 0.0504(17) 0.0476(15) 0.0029(13) 0.0047(11) -0.0011(11) C15 0.0410(17) 0.0429(17) 0.0578(18) 0.0067(14) 0.0115(14) -0.0026(13) C16 0.0448(17) 0.0450(18) 0.0593(19) -0.0090(15) 0.0124(14) 0.0026(13) C17 0.0270(14) 0.0505(18) 0.0448(15) -0.0026(13) 0.0102(11) -0.0005(12) C18 0.0356(15) 0.0425(17) 0.0503(17) 0.0040(13) 0.0122(13) 0.0028(12) C19 0.0337(15) 0.0444(17) 0.0485(16) -0.0059(13) 0.0121(12) 0.0028(12) Cl1 0.0604(5) 0.0711(5) 0.0499(4) -0.0002(4) 0.0230(4) 0.0074(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
1100767.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $ #$Revision: 176428 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100767.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100767 loop_ _publ_author_name 'Mian Ji' 'Boumahdi Benkmil' 'Heinrich Vahrenkamp' _publ_section_title ; Zinc-Thiolate Complexes of the Bis(pyrazolyl)(thioimidazolyl)hydroborate Tripods for the Modeling of Thiolate Alkylating Enzymes ; _journal_issue 10 _journal_name_full 'Inorganic Chemistry' _journal_page_first 3518 _journal_page_last 3523 _journal_paper_doi 10.1021/ic0484147 _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C19 H22 B Cl N6 S2 Zn' _chemical_formula_weight 510.18 _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 103.741(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 10.1030(17) _cell_length_b 23.398(4) _cell_length_c 10.1354(17) _cell_measurement_temperature 499(2) _cell_volume 2327.3(7) _diffrn_ambient_temperature 499(2) _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0341 _diffrn_reflns_av_sigmaI/netI 0.0588 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 15557 _diffrn_reflns_theta_max 30.04 _diffrn_reflns_theta_min 1.74 _exptl_absorpt_coefficient_mu 1.368 _exptl_absorpt_correction_type none _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.456 _exptl_crystal_density_method 'not measured' _exptl_crystal_description isometric _exptl_crystal_F_000 1048 _exptl_crystal_size_max 0.050 _exptl_crystal_size_mid 0.090 _exptl_crystal_size_min 0.200 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 275 _refine_ls_number_reflns 6438 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.002 _refine_ls_R_factor_all 0.0833 _refine_ls_R_factor_gt 0.0406 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0351P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0767 _refine_ls_wR_factor_ref 0.0903 _reflns_number_gt 3822 _reflns_number_total 6438 _reflns_threshold_expression >2sigma(I) _cod_duplicate_entry 1100766 _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_sg_symbol_H-M P2(1)/n _cod_database_code 1100767 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.17123(3) 1.120770(12) -0.53143(3) 0.03073(9) Uani 1 1 d . . . S1 S 0.19916(7) 1.13170(3) -0.75033(6) 0.0468(2) Uani 1 1 d . . . S2 S -0.05022(7) 1.10643(3) -0.54293(7) 0.0484(2) Uani 1 1 d . . . N1 N 0.47533(19) 1.14409(8) -0.63141(18) 0.0284(4) Uani 1 1 d . . . N2 N 0.42335(19) 1.13798(8) -0.85473(18) 0.0284(4) Uani 1 1 d . . . N3 N 0.45055(19) 1.08682(8) -0.42149(18) 0.0297(4) Uani 1 1 d . . . N4 N 0.3201(2) 1.06731(8) -0.43777(19) 0.0331(5) Uani 1 1 d . . . N5 N 0.4059(2) 1.19310(8) -0.42785(18) 0.0302(4) Uani 1 1 d . . . N6 N 0.2692(2) 1.19051(8) -0.43779(19) 0.0332(5) Uani 1 1 d . . . B1 B 0.4884(3) 1.14464(13) -0.4745(3) 0.0308(6) Uani 1 1 d . . . C1 C 0.2500(3) 1.18415(15) -1.0366(3) 0.0699(10) Uani 1 1 d . . . H1A H 0.1851 1.1829 -0.9811 0.105 Uiso 1 1 calc R . . H1B H 0.2029 1.1821 -1.1306 0.105 Uiso 1 1 calc R . . H1C H 0.3005 1.2193 -1.0201 0.105 Uiso 1 1 calc R . . C2 C 0.2752(3) 1.07621(14) -1.0260(3) 0.0685(10) Uani 1 1 d . . . H2A H 0.3408 1.0460 -1.0027 0.103 Uiso 1 1 calc R . . H2B H 0.2288 1.0730 -1.1201 0.103 Uiso 1 1 calc R . . H2C H 0.2103 1.0734 -0.9708 0.103 Uiso 1 1 calc R . . C3 C 0.4501(3) 1.13678(13) -1.0905(3) 0.0555(8) Uani 1 1 d . . . H3A H 0.5122 1.1052 -1.0697 0.083 Uiso 1 1 calc R . . H3B H 0.5001 1.1720 -1.0733 0.083 Uiso 1 1 calc R . . H3C H 0.4024 1.1351 -1.1844 0.083 Uiso 1 1 calc R . . C4 C 0.3477(3) 1.13375(12) -1.0014(2) 0.0400(6) Uani 1 1 d . . . C5 C 0.5633(2) 1.14318(10) -0.8117(2) 0.0344(6) Uani 1 1 d . . . H5A H 0.6247 1.1438 -0.8670 0.041 Uiso 1 1 calc R . . C6 C 0.5940(2) 1.14712(11) -0.6770(2) 0.0351(6) Uani 1 1 d . . . H6A H 0.6814 1.1513 -0.6221 0.042 Uiso 1 1 calc R . . C7 C 0.3701(2) 1.13819(10) -0.7428(2) 0.0283(5) Uani 1 1 d . . . C8 C 0.5368(3) 1.04798(11) -0.3505(2) 0.0386(6) Uani 1 1 d . . . H8A H 0.6312 1.0512 -0.3264 0.046 Uiso 1 1 calc R . . C9 C 0.4637(3) 1.00305(12) -0.3196(3) 0.0455(7) Uani 1 1 d . . . H9A H 0.4972 0.9703 -0.2711 0.055 Uiso 1 1 calc R . . C10 C 0.3292(3) 1.01665(11) -0.3759(2) 0.0414(6) Uani 1 1 d . . . H10A H 0.2553 0.9937 -0.3713 0.050 Uiso 1 1 calc R . . C11 C 0.4554(3) 1.24148(11) -0.3634(2) 0.0415(6) Uani 1 1 d . . . H11A H 0.5461 1.2530 -0.3438 0.050 Uiso 1 1 calc R . . C12 C 0.3505(3) 1.27088(12) -0.3315(3) 0.0487(7) Uani 1 1 d . . . H12A H 0.3550 1.3058 -0.2869 0.058 Uiso 1 1 calc R . . C13 C 0.2362(3) 1.23764(11) -0.3795(3) 0.0433(7) Uani 1 1 d . . . H13A H 0.1488 1.2469 -0.3722 0.052 Uiso 1 1 calc R . . C14 C -0.0672(2) 1.09960(12) -0.3723(3) 0.0392(6) Uani 1 1 d . . . C15 C -0.0977(3) 1.14662(12) -0.3014(3) 0.0472(7) Uani 1 1 d . . . H15A H -0.1012 1.1828 -0.3401 0.057 Uiso 1 1 calc R . . C16 C -0.1233(3) 1.14029(12) -0.1727(3) 0.0497(7) Uani 1 1 d . . . H16A H -0.1425 1.1721 -0.1253 0.060 Uiso 1 1 calc R . . C17 C -0.1198(2) 1.08707(12) -0.1172(3) 0.0405(6) Uani 1 1 d . . . C18 C -0.0890(3) 1.03978(12) -0.1850(3) 0.0425(7) Uani 1 1 d . . . H18A H -0.0856 1.0037 -0.1458 0.051 Uiso 1 1 calc R . . C19 C -0.0630(2) 1.04645(12) -0.3121(3) 0.0418(6) Uani 1 1 d . . . H19A H -0.0423 1.0145 -0.3580 0.050 Uiso 1 1 calc R . . Cl1 Cl -0.15460(8) 1.07846(4) 0.04249(7) 0.0588(2) Uani 1 1 d . . . H1 H 0.592(2) 1.1525(8) -0.4259(19) 0.020(5) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.02255(15) 0.03699(17) 0.03302(16) 0.00153(13) 0.00731(11) 0.00078(12) S1 0.0213(3) 0.0892(6) 0.0291(3) 0.0038(3) 0.0042(3) 0.0000(3) S2 0.0232(3) 0.0766(6) 0.0449(4) 0.0100(4) 0.0071(3) -0.0019(3) N1 0.0217(10) 0.0345(11) 0.0295(10) -0.0005(9) 0.0071(8) -0.0010(8) N2 0.0270(11) 0.0333(11) 0.0262(10) -0.0008(8) 0.0090(8) -0.0015(8) N3 0.0270(11) 0.0354(12) 0.0251(10) 0.0000(9) 0.0028(8) 0.0043(9) N4 0.0305(11) 0.0325(12) 0.0348(11) 0.0019(9) 0.0051(9) 0.0005(9) N5 0.0323(11) 0.0301(11) 0.0282(10) -0.0020(9) 0.0069(9) -0.0024(9) N6 0.0303(11) 0.0326(12) 0.0374(11) -0.0017(9) 0.0095(9) 0.0036(9) B1 0.0237(14) 0.0404(17) 0.0275(14) 0.0007(12) 0.0042(11) -0.0019(12) C1 0.066(2) 0.103(3) 0.0384(17) 0.0201(18) 0.0079(15) 0.026(2) C2 0.069(2) 0.092(3) 0.0454(18) -0.0236(18) 0.0159(16) -0.034(2) C3 0.057(2) 0.082(2) 0.0310(14) -0.0028(15) 0.0176(14) -0.0045(16) C4 0.0404(16) 0.0549(18) 0.0239(12) 0.0013(12) 0.0060(11) -0.0035(12) C5 0.0306(14) 0.0408(15) 0.0360(14) -0.0016(12) 0.0160(11) -0.0049(11) C6 0.0208(12) 0.0451(15) 0.0410(14) -0.0011(12) 0.0105(11) -0.0037(11) C7 0.0239(12) 0.0316(13) 0.0291(12) 0.0018(10) 0.0060(10) 0.0014(10) C8 0.0353(15) 0.0473(17) 0.0295(13) -0.0019(12) 0.0002(11) 0.0142(12) C9 0.0595(19) 0.0335(16) 0.0409(15) 0.0042(12) 0.0065(14) 0.0141(14) C10 0.0538(18) 0.0298(15) 0.0415(15) 0.0017(12) 0.0134(13) -0.0020(12) C11 0.0490(17) 0.0371(16) 0.0389(15) -0.0037(12) 0.0113(12) -0.0108(13) C12 0.064(2) 0.0317(16) 0.0518(17) -0.0100(13) 0.0173(15) -0.0015(14) C13 0.0492(17) 0.0350(16) 0.0493(16) 0.0007(13) 0.0187(13) 0.0089(13) C14 0.0181(12) 0.0504(17) 0.0476(15) 0.0029(13) 0.0047(11) -0.0011(11) C15 0.0410(17) 0.0429(17) 0.0578(18) 0.0067(14) 0.0115(14) -0.0026(13) C16 0.0448(17) 0.0450(18) 0.0593(19) -0.0090(15) 0.0124(14) 0.0026(13) C17 0.0270(14) 0.0505(18) 0.0448(15) -0.0026(13) 0.0102(11) -0.0005(12) C18 0.0356(15) 0.0425(17) 0.0503(17) 0.0040(13) 0.0122(13) 0.0028(12) C19 0.0337(15) 0.0444(17) 0.0485(16) -0.0059(13) 0.0121(12) 0.0028(12) Cl1 0.0604(5) 0.0711(5) 0.0499(4) -0.0002(4) 0.0230(4) 0.0074(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
1100768.cif	#------------------------------------------------------------------------------ #$Date: 2016-01-28 14:09:35 +0200 (Thu, 28 Jan 2016) $ #$Revision: 175230 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100768.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100768 loop_ _publ_author_name 'Mian Ji' 'Boumahdi Benkmil' 'Heinrich Vahrenkamp' _publ_section_title ; Zinc-Thiolate Complexes of the Bis(pyrazolyl)(thioimidazolyl)hydroborate Tripods for the Modeling of Thiolate Alkylating Enzymes ; _journal_issue 10 _journal_name_full 'Inorganic Chemistry' _journal_page_first 3518 _journal_page_last 3523 _journal_paper_doi 10.1021/ic0484147 _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C19 H23 B N6 S2 Zn' _chemical_formula_weight 475.73 _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 98.926(4) _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 21.345(4) _cell_length_b 8.6672(16) _cell_length_c 24.500(5) _cell_measurement_temperature 245(2) _cell_volume 4477.6(15) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 245(2) _diffrn_measured_fraction_theta_full 0.921 _diffrn_measured_fraction_theta_max 0.921 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0611 _diffrn_reflns_av_sigmaI/netI 0.1037 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 14568 _diffrn_reflns_theta_full 30.03 _diffrn_reflns_theta_max 30.03 _diffrn_reflns_theta_min 1.68 _exptl_absorpt_coefficient_mu 1.301 _exptl_absorpt_correction_type none _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.411 _exptl_crystal_density_method 'not measured' _exptl_crystal_description isometric _exptl_crystal_F_000 1968 _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _refine_diff_density_max 0.439 _refine_diff_density_min -0.430 _refine_diff_density_rms 0.076 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.907 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 266 _refine_ls_number_reflns 6034 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.907 _refine_ls_R_factor_all 0.1475 _refine_ls_R_factor_gt 0.0473 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0426P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0903 _refine_ls_wR_factor_ref 0.1180 _reflns_number_gt 2306 _reflns_number_total 6034 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic0484147si20041111_081517_5.cif _cod_data_source_block mianam _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_cell_volume 4477.8(15) _cod_database_code 1100768 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.183124(19) 0.17024(5) 0.605383(17) 0.04990(16) Uani 1 1 d . . . S1 S 0.07853(4) 0.13618(12) 0.56502(4) 0.0581(3) Uani 1 1 d . . . S2 S 0.25780(5) 0.04949(12) 0.56735(4) 0.0616(3) Uani 1 1 d . . . N1 N 0.04953(14) 0.3443(3) 0.64499(12) 0.0526(8) Uani 1 1 d . . . N4 N 0.17868(15) 0.1330(4) 0.68607(13) 0.0586(9) Uani 1 1 d . . . N5 N 0.15911(15) 0.4680(4) 0.65310(12) 0.0540(8) Uani 1 1 d . . . N6 N 0.19036(14) 0.4003(4) 0.61501(12) 0.0519(8) Uani 1 1 d . . . N2 N -0.02863(15) 0.2806(3) 0.57959(13) 0.0529(8) Uani 1 1 d . . . C4 C -0.0522(2) 0.3808(5) 0.61431(18) 0.0702(12) Uani 1 1 d . . . H4A H -0.0943 0.4160 0.6108 0.084 Uiso 1 1 calc R . . C6 C 0.03401(17) 0.2589(4) 0.59861(15) 0.0466(9) Uani 1 1 d . . . C5 C -0.0054(2) 0.4193(5) 0.65358(18) 0.0680(12) Uani 1 1 d . . . H5A H -0.0088 0.4872 0.6829 0.082 Uiso 1 1 calc R . . C12 C 0.22159(18) 0.5123(5) 0.59311(16) 0.0592(11) Uani 1 1 d . . . H12A H 0.2474 0.4974 0.5658 0.071 Uiso 1 1 calc R . . C13 C 0.32482(17) 0.1546(4) 0.59861(16) 0.0531(10) Uani 1 1 d . . . C10 C 0.1708(2) 0.6199(5) 0.65338(18) 0.0693(13) Uani 1 1 d . . . H10A H 0.1542 0.6928 0.6757 0.083 Uiso 1 1 calc R . . B1 B 0.1131(2) 0.3789(6) 0.6840(2) 0.0591(13) Uani 1 1 d . . . C9 C 0.1973(2) 0.0213(5) 0.72247(19) 0.0718(13) Uani 1 1 d . . . H9A H 0.2220 -0.0641 0.7156 0.086 Uiso 1 1 calc R . . C7 C 0.1419(2) 0.1818(6) 0.76326(17) 0.0774(14) Uani 1 1 d . . . H7A H 0.1205 0.2304 0.7893 0.093 Uiso 1 1 calc R . . C3 C -0.06371(18) 0.2205(5) 0.52723(18) 0.0625(11) Uani 1 1 d . . . H3A H -0.0435 0.1225 0.5188 0.075 Uiso 1 1 calc R . . C1 C -0.0586(2) 0.3321(5) 0.48070(18) 0.0837(14) Uani 1 1 d . . . H1A H -0.0142 0.3503 0.4784 0.126 Uiso 1 1 calc R . . H1B H -0.0787 0.4288 0.4877 0.126 Uiso 1 1 calc R . . H1C H -0.0794 0.2887 0.4461 0.126 Uiso 1 1 calc R . . C8 C 0.1753(2) 0.0482(6) 0.7713(2) 0.0884(16) Uani 1 1 d . . . H8A H 0.1819 -0.0127 0.8035 0.106 Uiso 1 1 calc R . . N3 N 0.14452(15) 0.2330(4) 0.71189(13) 0.0592(9) Uani 1 1 d . . . C16 C 0.43694(19) 0.3114(5) 0.64506(18) 0.0639(11) Uani 1 1 d . . . C19 C 0.34471(18) 0.1588(4) 0.65509(16) 0.0582(10) Uani 1 1 d . . . H19A H 0.3205 0.1080 0.6786 0.070 Uiso 1 1 calc R . . C14 C 0.3629(2) 0.2293(5) 0.56566(17) 0.0646(12) Uani 1 1 d . . . H14A H 0.3514 0.2273 0.5270 0.078 Uiso 1 1 calc R . . C11 C 0.2106(2) 0.6529(5) 0.61617(19) 0.0730(13) Uani 1 1 d . . . H11A H 0.2269 0.7498 0.6082 0.088 Uiso 1 1 calc R . . C18 C 0.3993(2) 0.2360(5) 0.67786(17) 0.0636(11) Uani 1 1 d . . . H18A H 0.4112 0.2373 0.7165 0.076 Uiso 1 1 calc R . . C15 C 0.4173(2) 0.3064(5) 0.58868(18) 0.0695(12) Uani 1 1 d . . . H15A H 0.4417 0.3570 0.5653 0.083 Uiso 1 1 calc R . . C2 C -0.13178(18) 0.1858(5) 0.5332(2) 0.0903(16) Uani 1 1 d . . . H2A H -0.1326 0.1133 0.5632 0.135 Uiso 1 1 calc R . . H2B H -0.1535 0.1412 0.4991 0.135 Uiso 1 1 calc R . . H2C H -0.1529 0.2805 0.5411 0.135 Uiso 1 1 calc R . . C17 C 0.4968(2) 0.3951(6) 0.66990(19) 0.0969(16) Uani 1 1 d . . . H17A H 0.5029 0.3850 0.7098 0.145 Uiso 1 1 calc R . . H17B H 0.4932 0.5035 0.6600 0.145 Uiso 1 1 calc R . . H17C H 0.5329 0.3506 0.6558 0.145 Uiso 1 1 calc R . . H1 H 0.1003(13) 0.459(4) 0.7158(12) 0.052(9) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0511(3) 0.0462(3) 0.0528(3) -0.0004(2) 0.0094(2) 0.0009(2) S1 0.0462(6) 0.0668(7) 0.0626(7) -0.0218(5) 0.0122(5) 0.0000(5) S2 0.0619(7) 0.0543(7) 0.0701(7) -0.0103(6) 0.0147(6) 0.0048(5) N1 0.056(2) 0.052(2) 0.053(2) -0.0088(16) 0.0156(17) 0.0060(16) N4 0.067(2) 0.054(2) 0.053(2) 0.0110(18) 0.0052(18) 0.0000(17) N5 0.062(2) 0.042(2) 0.057(2) -0.0065(16) 0.0064(17) -0.0034(16) N6 0.056(2) 0.0485(19) 0.051(2) -0.0068(16) 0.0098(17) -0.0069(16) N2 0.050(2) 0.0477(19) 0.061(2) -0.0071(17) 0.0091(17) 0.0052(15) C4 0.064(3) 0.065(3) 0.083(3) -0.009(3) 0.017(3) 0.018(2) C6 0.051(2) 0.042(2) 0.049(2) 0.0005(18) 0.0141(19) -0.0038(18) C5 0.077(3) 0.062(3) 0.069(3) -0.017(2) 0.025(3) 0.014(2) C12 0.055(3) 0.055(3) 0.065(3) 0.011(2) 0.003(2) -0.010(2) C13 0.054(2) 0.047(2) 0.060(3) 0.003(2) 0.015(2) 0.0142(19) C10 0.077(3) 0.045(3) 0.081(3) -0.013(2) -0.004(3) -0.005(2) B1 0.071(3) 0.059(3) 0.048(3) -0.016(3) 0.013(3) -0.001(3) C9 0.080(3) 0.064(3) 0.068(3) 0.014(3) -0.001(3) -0.011(2) C7 0.080(3) 0.114(4) 0.040(3) 0.001(3) 0.015(2) -0.017(3) C3 0.052(3) 0.054(3) 0.079(3) -0.013(2) 0.003(2) 0.006(2) C1 0.085(3) 0.088(4) 0.072(3) 0.002(3) -0.009(3) 0.006(3) C8 0.096(4) 0.099(4) 0.064(3) 0.033(3) -0.004(3) -0.028(3) N3 0.068(2) 0.070(2) 0.039(2) 0.0025(18) 0.0068(17) -0.0057(19) C16 0.061(3) 0.066(3) 0.067(3) 0.009(2) 0.017(2) -0.002(2) C19 0.059(3) 0.061(3) 0.059(3) 0.006(2) 0.022(2) 0.001(2) C14 0.067(3) 0.073(3) 0.056(3) 0.015(2) 0.013(2) 0.001(2) C11 0.076(3) 0.054(3) 0.081(3) 0.012(3) -0.010(3) -0.012(2) C18 0.064(3) 0.072(3) 0.057(3) 0.001(2) 0.017(2) 0.002(2) C15 0.066(3) 0.077(3) 0.068(3) 0.021(2) 0.020(2) 0.001(2) C2 0.050(3) 0.083(3) 0.136(4) -0.015(3) 0.007(3) 0.000(2) C17 0.083(4) 0.112(4) 0.094(4) 0.005(3) 0.009(3) -0.034(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 Zn1 N4 93.33(13) . . ? N6 Zn1 S2 117.89(10) . . ? N4 Zn1 S2 118.66(10) . . ? N6 Zn1 S1 103.17(9) . . ? N4 Zn1 S1 102.06(10) . . ? S2 Zn1 S1 117.79(4) . . ? C6 S1 Zn1 106.53(13) . . ? C13 S2 Zn1 99.21(12) . . ? C6 N1 C5 106.4(3) . . ? C6 N1 B1 134.0(3) . . ? C5 N1 B1 119.5(3) . . ? C9 N4 N3 106.2(4) . . ? C9 N4 Zn1 135.7(3) . . ? N3 N4 Zn1 117.8(2) . . ? C10 N5 N6 108.4(3) . . ? C10 N5 B1 128.6(4) . . ? N6 N5 B1 122.7(3) . . ? C12 N6 N5 106.9(3) . . ? C12 N6 Zn1 135.0(3) . . ? N5 N6 Zn1 118.1(2) . . ? C6 N2 C4 108.2(3) . . ? C6 N2 C3 126.1(3) . . ? C4 N2 C3 125.4(3) . . ? C5 C4 N2 107.7(4) . . ? N1 C6 N2 108.2(3) . . ? N1 C6 S1 131.2(3) . . ? N2 C6 S1 120.6(3) . . ? C4 C5 N1 109.5(4) . . ? N6 C12 C11 110.5(4) . . ? C19 C13 C14 116.9(4) . . ? C19 C13 S2 123.3(3) . . ? C14 C13 S2 119.7(3) . . ? N5 C10 C11 109.7(4) . . ? N5 B1 N3 111.3(4) . . ? N5 B1 N1 110.8(3) . . ? N3 B1 N1 113.0(3) . . ? N4 C9 C8 110.7(4) . . ? N3 C7 C8 108.7(4) . . ? N2 C3 C1 110.1(3) . . ? N2 C3 C2 110.6(4) . . ? C1 C3 C2 112.6(4) . . ? C7 C8 C9 105.1(4) . . ? C7 N3 N4 109.3(4) . . ? C7 N3 B1 127.4(4) . . ? N4 N3 B1 123.3(3) . . ? C15 C16 C18 117.0(4) . . ? C15 C16 C17 121.5(4) . . ? C18 C16 C17 121.5(4) . . ? C13 C19 C18 121.6(4) . . ? C15 C14 C13 121.2(4) . . ? C10 C11 C12 104.5(4) . . ? C16 C18 C19 121.5(4) . . ? C16 C15 C14 121.9(4) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N6 2.011(3) . ? Zn1 N4 2.020(3) . ? Zn1 S2 2.2283(11) . ? Zn1 S1 2.3162(11) . ? S1 C6 1.719(4) . ? S2 C13 1.767(4) . ? N1 C6 1.353(4) . ? N1 C5 1.385(4) . ? N1 B1 1.563(5) . ? N4 C9 1.334(5) . ? N4 N3 1.351(4) . ? N5 C10 1.341(4) . ? N5 N6 1.361(4) . ? N5 B1 1.538(6) . ? N6 C12 1.336(4) . ? N2 C6 1.359(4) . ? N2 C4 1.365(4) . ? N2 C3 1.476(5) . ? C4 C5 1.318(5) . ? C12 C11 1.378(5) . ? C13 C19 1.383(5) . ? C13 C14 1.391(5) . ? C10 C11 1.370(5) . ? B1 N3 1.541(6) . ? C9 C8 1.372(6) . ? C7 N3 1.344(5) . ? C7 C8 1.358(6) . ? C3 C1 1.512(5) . ? C3 C2 1.513(5) . ? C16 C15 1.380(5) . ? C16 C18 1.384(5) . ? C16 C17 1.514(5) . ? C19 C18 1.384(5) . ? C14 C15 1.383(5) . ?
1100769.cif	#------------------------------------------------------------------------------ #$Date: 2016-01-28 14:09:35 +0200 (Thu, 28 Jan 2016) $ #$Revision: 175230 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100769.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100769 loop_ _publ_author_name 'Mian Ji' 'Boumahdi Benkmil' 'Heinrich Vahrenkamp' _publ_section_title ; Zinc-Thiolate Complexes of the Bis(pyrazolyl)(thioimidazolyl)hydroborate Tripods for the Modeling of Thiolate Alkylating Enzymes ; _journal_issue 10 _journal_name_full 'Inorganic Chemistry' _journal_page_first 3518 _journal_page_last 3523 _journal_paper_doi 10.1021/ic0484147 _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C18 H20 B Cl N6 S2 Zn' _chemical_formula_weight 496.15 _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 100.111(4) _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 20.688(4) _cell_length_b 8.5506(17) _cell_length_c 25.364(5) _cell_measurement_temperature 245(2) _cell_volume 4417.1(15) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 245(2) _diffrn_measured_fraction_theta_full 0.897 _diffrn_measured_fraction_theta_max 0.897 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0252 _diffrn_reflns_av_sigmaI/netI 0.0491 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_number 11586 _diffrn_reflns_theta_full 30.03 _diffrn_reflns_theta_max 30.03 _diffrn_reflns_theta_min 1.63 _exptl_absorpt_coefficient_mu 1.439 _exptl_absorpt_correction_type none _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.492 _exptl_crystal_density_method 'not measured' _exptl_crystal_description isometric _exptl_crystal_F_000 2032 _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.30 _refine_diff_density_max 0.371 _refine_diff_density_min -0.594 _refine_diff_density_rms 0.065 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.892 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 266 _refine_ls_number_reflns 5801 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.892 _refine_ls_R_factor_all 0.0631 _refine_ls_R_factor_gt 0.0351 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0356P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0700 _refine_ls_wR_factor_ref 0.0774 _reflns_number_gt 3669 _reflns_number_total 5801 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic0484147si20041111_081517_6.cif _cod_data_source_block jiz1m _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_cell_volume 4417.2(15) _cod_database_code 1100769 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn -0.312081(11) 0.82127(3) 0.605150(10) 0.03669(8) Uani 1 1 d . . . S1 S -0.41926(3) 0.85446(7) 0.56216(2) 0.04478(15) Uani 1 1 d . . . S2 S -0.23248(3) 0.93409(7) 0.56894(3) 0.04773(16) Uani 1 1 d . . . N1 N -0.45327(8) 0.66344(19) 0.64285(7) 0.0387(4) Uani 1 1 d . . . N2 N -0.53312(8) 0.7313(2) 0.57848(8) 0.0408(4) Uani 1 1 d . . . N3 N -0.35284(9) 0.7692(2) 0.70787(7) 0.0434(4) Uani 1 1 d . . . N4 N -0.31599(9) 0.8669(2) 0.68287(7) 0.0422(4) Uani 1 1 d . . . N5 N -0.34168(8) 0.5263(2) 0.65271(7) 0.0410(4) Uani 1 1 d . . . N6 N -0.30641(8) 0.5883(2) 0.61752(7) 0.0411(4) Uani 1 1 d . . . Cl1 Cl 0.02182(3) 0.57644(9) 0.67846(3) 0.0730(2) Uani 1 1 d . . . B1 B -0.38759(13) 0.6230(3) 0.68154(11) 0.0432(6) Uani 1 1 d . . . HB1 H -0.4020(9) 0.545(2) 0.7115(7) 0.033(5) Uiso 1 1 d . . . C1 C -0.63845(11) 0.8274(3) 0.52846(13) 0.0692(8) Uani 1 1 d . . . H1A H -0.6394 0.9068 0.5556 0.104 Uiso 1 1 calc R . . H1B H -0.6611 0.7345 0.5376 0.104 Uiso 1 1 calc R . . H1C H -0.6601 0.8668 0.4940 0.104 Uiso 1 1 calc R . . C2 C -0.56231(14) 0.6653(3) 0.48335(11) 0.0693(8) Uani 1 1 d . . . H2A H -0.5163 0.6441 0.4829 0.104 Uiso 1 1 calc R . . H2B H -0.5831 0.7040 0.4485 0.104 Uiso 1 1 calc R . . H2C H -0.5839 0.5697 0.4914 0.104 Uiso 1 1 calc R . . C3 C -0.56793(11) 0.7868(3) 0.52564(10) 0.0482(6) Uani 1 1 d . . . H3A H -0.5459 0.8832 0.5164 0.058 Uiso 1 1 calc R . . C4 C -0.55999(12) 0.6414(3) 0.61370(11) 0.0531(6) Uani 1 1 d . . . H4A H -0.6045 0.6138 0.6108 0.064 Uiso 1 1 calc R . . C5 C -0.51131(12) 0.6000(3) 0.65292(10) 0.0514(6) Uani 1 1 d . . . H5A H -0.5158 0.5377 0.6826 0.062 Uiso 1 1 calc R . . C6 C -0.46792(10) 0.7446(2) 0.59636(9) 0.0352(5) Uani 1 1 d . . . C7 C -0.35341(12) 0.8245(3) 0.75772(9) 0.0563(7) Uani 1 1 d . . . H7A H -0.3754 0.7786 0.7832 0.068 Uiso 1 1 calc R . . C8 C -0.31664(13) 0.9585(3) 0.76485(10) 0.0603(7) Uani 1 1 d . . . H8A H -0.3084 1.0220 0.7955 0.072 Uiso 1 1 calc R . . C9 C -0.29454(11) 0.9798(3) 0.71770(10) 0.0505(6) Uani 1 1 d . . . H9A H -0.2677 1.0633 0.7108 0.061 Uiso 1 1 calc R . . C10 C -0.33272(12) 0.3699(3) 0.65387(10) 0.0534(6) Uani 1 1 d . . . H10A H -0.3519 0.2990 0.6749 0.064 Uiso 1 1 calc R . . C11 C -0.29131(13) 0.3314(3) 0.61952(11) 0.0580(7) Uani 1 1 d . . . H11A H -0.2761 0.2312 0.6125 0.070 Uiso 1 1 calc R . . C12 C -0.27671(11) 0.4707(3) 0.59741(10) 0.0495(6) Uani 1 1 d . . . H12A H -0.2495 0.4813 0.5716 0.059 Uiso 1 1 calc R . . C13 C -0.16298(10) 0.8272(2) 0.60128(9) 0.0386(5) Uani 1 1 d . . . C14 C -0.12153(11) 0.7594(3) 0.57040(10) 0.0484(6) Uani 1 1 d . . . H14A H -0.1322 0.7649 0.5329 0.058 Uiso 1 1 calc R . . C15 C -0.06459(12) 0.6834(3) 0.59401(10) 0.0538(6) Uani 1 1 d . . . H15A H -0.0364 0.6394 0.5727 0.065 Uiso 1 1 calc R . . C16 C -0.04973(11) 0.6731(3) 0.64848(10) 0.0464(6) Uani 1 1 d . . . C17 C -0.08980(11) 0.7388(3) 0.68031(10) 0.0481(6) Uani 1 1 d . . . H17A H -0.0790 0.7313 0.7178 0.058 Uiso 1 1 calc R . . C18 C -0.14619(10) 0.8162(3) 0.65648(9) 0.0452(5) Uani 1 1 d . . . H18A H -0.1735 0.8620 0.6781 0.054 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.03079(14) 0.03922(14) 0.03981(15) 0.00173(11) 0.00550(11) 0.00045(11) S1 0.0292(3) 0.0619(4) 0.0430(3) 0.0169(3) 0.0056(3) -0.0002(3) S2 0.0371(3) 0.0486(3) 0.0580(4) 0.0157(3) 0.0098(3) 0.0007(3) N1 0.0343(10) 0.0410(10) 0.0414(11) 0.0068(8) 0.0085(9) -0.0013(8) N2 0.0305(9) 0.0403(10) 0.0499(12) 0.0059(9) 0.0024(9) -0.0034(8) N3 0.0406(11) 0.0554(11) 0.0335(10) 0.0002(9) 0.0039(9) 0.0076(9) N4 0.0434(11) 0.0425(10) 0.0392(11) -0.0034(9) 0.0033(9) 0.0004(8) N5 0.0398(10) 0.0380(10) 0.0430(11) 0.0058(8) 0.0015(9) 0.0036(8) N6 0.0375(10) 0.0417(10) 0.0440(11) 0.0017(8) 0.0069(9) 0.0068(8) Cl1 0.0514(4) 0.0855(5) 0.0771(5) -0.0089(4) -0.0026(4) 0.0269(4) B1 0.0413(15) 0.0487(15) 0.0387(15) 0.0116(12) 0.0042(13) 0.0019(12) C1 0.0337(13) 0.0652(17) 0.104(2) 0.0187(16) -0.0018(15) 0.0043(12) C2 0.0612(18) 0.0773(19) 0.0603(18) -0.0026(15) -0.0146(15) 0.0015(15) C3 0.0321(12) 0.0467(13) 0.0610(16) 0.0145(12) -0.0047(11) -0.0010(10) C4 0.0366(13) 0.0519(14) 0.0709(18) 0.0116(13) 0.0101(13) -0.0114(11) C5 0.0441(14) 0.0530(14) 0.0591(16) 0.0168(12) 0.0142(13) -0.0068(11) C6 0.0306(11) 0.0350(11) 0.0393(12) 0.0014(9) 0.0046(10) 0.0001(9) C7 0.0534(15) 0.0819(19) 0.0327(13) -0.0004(13) 0.0053(12) 0.0174(14) C8 0.0608(17) 0.0714(18) 0.0429(15) -0.0178(13) -0.0067(13) 0.0197(14) C9 0.0445(14) 0.0488(13) 0.0520(16) -0.0097(12) -0.0087(12) 0.0090(11) C10 0.0540(15) 0.0380(13) 0.0616(17) 0.0103(11) -0.0079(14) 0.0003(11) C11 0.0603(16) 0.0408(14) 0.0658(17) -0.0068(12) -0.0081(14) 0.0141(12) C12 0.0420(13) 0.0535(14) 0.0509(15) -0.0108(12) 0.0022(12) 0.0109(11) C13 0.0312(11) 0.0378(11) 0.0472(13) 0.0029(10) 0.0079(10) -0.0070(9) C14 0.0475(14) 0.0549(14) 0.0415(14) -0.0056(11) 0.0047(12) 0.0030(12) C15 0.0470(14) 0.0597(15) 0.0565(16) -0.0112(13) 0.0135(13) 0.0087(12) C16 0.0351(12) 0.0456(13) 0.0572(16) -0.0040(11) 0.0047(12) 0.0040(10) C17 0.0417(13) 0.0581(14) 0.0446(14) 0.0060(11) 0.0082(12) 0.0020(11) C18 0.0363(12) 0.0539(13) 0.0497(14) 0.0035(12) 0.0194(11) 0.0038(11) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 Zn1 N4 92.85(7) . . ? N6 Zn1 S2 117.54(5) . . ? N4 Zn1 S2 118.31(6) . . ? N6 Zn1 S1 102.68(5) . . ? N4 Zn1 S1 103.70(5) . . ? S2 Zn1 S1 117.87(3) . . ? C6 S1 Zn1 107.05(7) . . ? C13 S2 Zn1 100.53(7) . . ? C6 N1 C5 107.04(18) . . ? C6 N1 B1 133.93(18) . . ? C5 N1 B1 118.89(18) . . ? C6 N2 C4 108.92(19) . . ? C6 N2 C3 125.05(18) . . ? C4 N2 C3 125.52(18) . . ? C7 N3 N4 108.6(2) . . ? C7 N3 B1 127.7(2) . . ? N4 N3 B1 123.72(18) . . ? C9 N4 N3 106.54(19) . . ? C9 N4 Zn1 136.05(17) . . ? N3 N4 Zn1 117.21(13) . . ? C10 N5 N6 108.32(19) . . ? C10 N5 B1 128.1(2) . . ? N6 N5 B1 123.45(17) . . ? C12 N6 N5 107.19(18) . . ? C12 N6 Zn1 135.01(17) . . ? N5 N6 Zn1 117.75(13) . . ? N3 B1 N5 111.32(19) . . ? N3 B1 N1 112.36(19) . . ? N5 B1 N1 111.13(19) . . ? N2 C3 C2 109.59(19) . . ? N2 C3 C1 110.5(2) . . ? C2 C3 C1 112.7(2) . . ? C5 C4 N2 107.2(2) . . ? C4 C5 N1 109.0(2) . . ? N2 C6 N1 107.86(17) . . ? N2 C6 S1 121.02(16) . . ? N1 C6 S1 131.09(16) . . ? N3 C7 C8 108.7(2) . . ? C9 C8 C7 105.1(2) . . ? N4 C9 C8 111.1(2) . . ? N5 C10 C11 108.9(2) . . ? C10 C11 C12 105.0(2) . . ? N6 C12 C11 110.5(2) . . ? C18 C13 C14 118.2(2) . . ? C18 C13 S2 122.71(17) . . ? C14 C13 S2 119.00(18) . . ? C15 C14 C13 121.0(2) . . ? C16 C15 C14 119.4(2) . . ? C15 C16 C17 121.1(2) . . ? C15 C16 Cl1 119.62(18) . . ? C17 C16 Cl1 119.30(19) . . ? C16 C17 C18 119.2(2) . . ? C17 C18 C13 121.1(2) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N6 2.0165(18) . ? Zn1 N4 2.0249(19) . ? Zn1 S2 2.2398(7) . ? Zn1 S1 2.3101(7) . ? S1 C6 1.719(2) . ? S2 C13 1.778(2) . ? N1 C6 1.356(3) . ? N1 C5 1.382(3) . ? N1 B1 1.569(3) . ? N2 C6 1.350(3) . ? N2 C4 1.369(3) . ? N2 C3 1.484(3) . ? N3 C7 1.352(3) . ? N3 N4 1.360(2) . ? N3 B1 1.535(3) . ? N4 C9 1.332(3) . ? N5 C10 1.349(3) . ? N5 N6 1.356(2) . ? N5 B1 1.538(3) . ? N6 C12 1.326(3) . ? Cl1 C16 1.749(2) . ? C1 C3 1.513(3) . ? C2 C3 1.513(3) . ? C4 C5 1.333(3) . ? C7 C8 1.370(4) . ? C8 C9 1.365(3) . ? C10 C11 1.365(4) . ? C11 C12 1.373(3) . ? C13 C18 1.385(3) . ? C13 C14 1.386(3) . ? C14 C15 1.386(3) . ? C15 C16 1.364(3) . ? C16 C17 1.375(3) . ? C17 C18 1.384(3) . ?
1100770.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100770.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100770 loop_ _publ_author_name 'Deng-Ke Cao' 'Yi-Zhi Li' 'You Song' 'Li-Min Zheng' _publ_section_title ; Three-, Two-, and One-Dimensional Metal Phosphonates Based on [Hydroxy(4-pyridyl)methyl]phosphonate: M{(4-C5H4N)CH(OH)PO3}(H2O) (M = Ni, Cd) and Gd{(4-C5H4N)CH(OH)P(OH)O2}3.6H2O ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3599 _journal_page_last 3604 _journal_paper_doi 10.1021/ic0484248 _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C6 H8 N Ni O5 P' _chemical_formula_weight 263.81 _chemical_name_systematic ; ? ; _space_group_IT_number 61 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_space_group_name_H-M 'P b c a' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 8.7980(13) _cell_length_b 10.1982(15) _cell_length_c 17.945(3) _cell_measurement_reflns_used 327 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 16.818 _cell_measurement_theta_min 3.24 _cell_volume 1610.1(4) _computing_cell_refinement SMART _computing_data_collection 'SMART (Bruker, 2000)' _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _computing_structure_refinement SHELXTL _computing_structure_solution 'SHELXTL (Bruker, 2000)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker Smart Aepex CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1062 _diffrn_reflns_av_sigmaI/netI 0.1220 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 7358 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_min 2.27 _exptl_absorpt_coefficient_mu 2.602 _exptl_absorpt_correction_T_max 0.949 _exptl_absorpt_correction_T_min 0.911 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS(Bruker, 2000)' _exptl_crystal_colour green _exptl_crystal_density_diffrn 2.177 _exptl_crystal_density_method 'not measured' _exptl_crystal_description blocky _exptl_crystal_F_000 1072 _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _refine_diff_density_max 1.017 _refine_diff_density_min -1.250 _refine_diff_density_rms 0.123 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.919 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 133 _refine_ls_number_reflns 1415 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.919 _refine_ls_R_factor_all 0.1099 _refine_ls_R_factor_gt 0.0541 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0165P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0834 _refine_ls_wR_factor_ref 0.0958 _reflns_number_gt 816 _reflns_number_total 1415 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic0484248si20050317_103348_1.cif _cod_data_source_block Ni{(4-C5H4N)CH(OH)PO3}(H2O) _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_database_code 1100770 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.34085(11) 0.34372(9) 0.81005(5) 0.0190(3) Uani 1 1 d . . . P1 P 0.5409(2) 0.1536(2) 0.71157(10) 0.0185(5) Uani 1 1 d . . . O1 O 0.5196(5) 0.2198(4) 0.7871(2) 0.0169(13) Uani 1 1 d . . . O2 O 0.5260(6) 0.0058(5) 0.7138(3) 0.0255(14) Uani 1 1 d . . . O3 O 0.6885(5) 0.1920(4) 0.6739(2) 0.0159(13) Uani 1 1 d . . . O4 O 0.3032(6) 0.3217(5) 0.6889(3) 0.0307(15) Uani 1 1 d . . . H4 H 0.215(9) 0.309(7) 0.666(4) 0.043 Uiso 1 1 d . . . N1 N 0.3848(6) 0.1601(7) 0.4236(3) 0.0168(14) Uani 1 1 d . . . C1 C 0.3306(10) 0.0672(8) 0.4697(4) 0.035(2) Uani 1 1 d . . . H1A H 0.2951 -0.0101 0.4483 0.042 Uiso 1 1 calc R . . C2 C 0.3237(10) 0.0775(9) 0.5449(4) 0.039(2) Uani 1 1 d . . . H2A H 0.2830 0.0102 0.5736 0.046 Uiso 1 1 calc R . . C3 C 0.3788(9) 0.1908(9) 0.5781(4) 0.030(2) Uani 1 1 d . . . C4 C 0.4366(10) 0.2875(8) 0.5325(5) 0.038(2) Uani 1 1 d . . . H4A H 0.4744 0.3650 0.5526 0.046 Uiso 1 1 calc R . . C5 C 0.4374(10) 0.2674(8) 0.4568(5) 0.034(2) Uani 1 1 d . . . H5A H 0.4775 0.3332 0.4268 0.041 Uiso 1 1 calc R . . C6 C 0.3740(9) 0.2061(8) 0.6602(4) 0.032(2) Uani 1 1 d . . . H6A H 0.3001 0.1385 0.6742 0.038 Uiso 1 1 calc R . . O1W O 0.1602(7) 0.4649(5) 0.8289(3) 0.0284(14) Uani 1 1 d G . . H1WA H 0.0963 0.4605 0.7900 0.040 Uiso 1 1 d G . . H1WB H 0.2050 0.5421 0.8394 0.040 Uiso 1 1 d G . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0242(6) 0.0167(5) 0.0161(5) -0.0002(5) -0.0003(5) 0.0012(5) P1 0.0209(12) 0.0192(11) 0.0154(10) 0.0000(10) -0.0016(9) 0.0021(11) O1 0.015(3) 0.022(3) 0.014(3) -0.002(2) 0.003(2) 0.001(2) O2 0.026(3) 0.012(3) 0.038(3) -0.007(2) 0.016(3) -0.004(2) O3 0.024(3) 0.004(3) 0.020(3) -0.002(2) 0.005(2) -0.002(2) O4 0.035(4) 0.027(3) 0.030(3) -0.004(3) -0.011(3) 0.006(3) N1 0.016(4) 0.013(3) 0.021(3) 0.000(3) -0.002(3) -0.002(3) C1 0.045(6) 0.033(6) 0.027(5) -0.002(4) -0.011(5) -0.014(5) C2 0.036(6) 0.056(7) 0.024(5) 0.008(5) -0.009(5) -0.014(5) C3 0.027(6) 0.036(6) 0.026(5) -0.001(4) 0.004(4) 0.023(4) C4 0.057(7) 0.023(5) 0.034(5) -0.016(4) -0.014(5) 0.002(5) C5 0.039(6) 0.024(5) 0.039(6) 0.009(4) -0.008(5) -0.005(5) C6 0.036(6) 0.029(5) 0.030(5) -0.004(4) -0.011(4) 0.007(4) O1W 0.031(4) 0.022(3) 0.032(4) -0.005(3) -0.011(3) -0.001(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1W Ni1 O1 177.83(18) . . ? O1W Ni1 O3 85.72(19) . 6_557 ? O1 Ni1 O3 93.66(18) . 6_557 ? O1W Ni1 O2 89.5(2) . 3_656 ? O1 Ni1 O2 90.96(19) . 3_656 ? O3 Ni1 O2 173.24(19) 6_557 3_656 ? O1W Ni1 N1 89.6(2) . 7_566 ? O1 Ni1 N1 92.4(2) . 7_566 ? O3 Ni1 N1 88.3(2) 6_557 7_566 ? O2 Ni1 N1 96.5(2) 3_656 7_566 ? O1W Ni1 O4 96.20(19) . . ? O1 Ni1 O4 81.70(19) . . ? O3 Ni1 O4 87.94(18) 6_557 . ? O2 Ni1 O4 87.84(19) 3_656 . ? N1 Ni1 O4 172.8(2) 7_566 . ? O2 P1 O3 110.1(3) . . ? O2 P1 O1 114.0(3) . . ? O3 P1 O1 112.8(3) . . ? O2 P1 C6 103.8(3) . . ? O3 P1 C6 113.0(3) . . ? O1 P1 C6 102.8(3) . . ? P1 O1 Ni1 122.9(3) . . ? P1 O2 Ni1 137.8(3) . 3_646 ? P1 O3 Ni1 133.4(3) . 6_657 ? C6 O4 Ni1 111.9(4) . . ? C6 O4 H4 95(5) . . ? Ni1 O4 H4 127(5) . . ? C5 N1 C1 115.3(6) . . ? C5 N1 Ni1 121.4(5) . 7_565 ? C1 N1 Ni1 121.6(5) . 7_565 ? N1 C1 C2 125.0(8) . . ? N1 C1 H1A 117.5 . . ? C2 C1 H1A 117.5 . . ? C1 C2 C3 118.5(8) . . ? C1 C2 H2A 120.8 . . ? C3 C2 H2A 120.8 . . ? C4 C3 C2 118.0(7) . . ? C4 C3 C6 121.7(8) . . ? C2 C3 C6 120.3(8) . . ? C5 C4 C3 118.8(8) . . ? C5 C4 H4A 120.6 . . ? C3 C4 H4A 120.6 . . ? N1 C5 C4 124.4(8) . . ? N1 C5 H5A 117.8 . . ? C4 C5 H5A 117.8 . . ? O4 C6 C3 117.2(6) . . ? O4 C6 P1 114.4(5) . . ? C3 C6 P1 116.8(6) . . ? O4 C6 H6A 101.5 . . ? C3 C6 H6A 101.5 . . ? P1 C6 H6A 101.5 . . ? Ni1 O1W H1WA 109.2 . . ? Ni1 O1W H1WB 102.9 . . ? H1WA O1W H1WB 118.8 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O1W 2.041(5) . ? Ni1 O1 2.059(5) . ? Ni1 O3 2.067(4) 6_557 ? Ni1 O2 2.071(5) 3_656 ? Ni1 N1 2.075(5) 7_566 ? Ni1 O4 2.210(5) . ? P1 O2 1.513(5) . ? P1 O3 1.516(5) . ? P1 O1 1.526(4) . ? P1 C6 1.815(8) . ? O2 Ni1 2.071(5) 3_646 ? O3 Ni1 2.067(4) 6_657 ? O4 C6 1.430(9) . ? O4 H4 0.89(7) . ? N1 C5 1.329(9) . ? N1 C1 1.346(9) . ? N1 Ni1 2.075(5) 7_565 ? C1 C2 1.355(9) . ? C1 H1A 0.9300 . ? C2 C3 1.388(10) . ? C2 H2A 0.9300 . ? C3 C4 1.379(11) . ? C3 C6 1.482(10) . ? C4 C5 1.374(10) . ? C4 H4A 0.9300 . ? C5 H5A 0.9300 . ? C6 H6A 0.9800 . ? O1W H1WA 0.8978 . ? O1W H1WB 0.8998 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1WB O3 0.90 1.81 2.671(6) 159.8 3_656 O1W H1WA O2 0.90 1.80 2.669(7) 162.2 8_665 O4 H4 O1 0.89(7) 2.12(8) 2.737(7) 126(6) 6_557 loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 P1 O1 Ni1 -114.6(3) . . . . ? O3 P1 O1 Ni1 118.9(3) . . . . ? C6 P1 O1 Ni1 -3.0(4) . . . . ? O3 Ni1 O1 P1 78.8(3) 6_557 . . . ? O2 Ni1 O1 P1 -96.2(3) 3_656 . . . ? N1 Ni1 O1 P1 167.2(3) 7_566 . . . ? O4 Ni1 O1 P1 -8.6(3) . . . . ? O3 P1 O2 Ni1 8.0(5) . . . 3_646 ? O1 P1 O2 Ni1 -119.9(4) . . . 3_646 ? C6 P1 O2 Ni1 129.2(5) . . . 3_646 ? O2 P1 O3 Ni1 -145.4(3) . . . 6_657 ? O1 P1 O3 Ni1 -16.8(5) . . . 6_657 ? C6 P1 O3 Ni1 99.2(4) . . . 6_657 ? O1W Ni1 O4 C6 -158.5(5) . . . . ? O1 Ni1 O4 C6 21.0(5) . . . . ? O3 Ni1 O4 C6 -73.0(5) 6_557 . . . ? O2 Ni1 O4 C6 112.3(5) 3_656 . . . ? C5 N1 C1 C2 1.5(13) . . . . ? Ni1 N1 C1 C2 -164.1(7) 7_565 . . . ? N1 C1 C2 C3 -1.3(14) . . . . ? C1 C2 C3 C4 0.5(13) . . . . ? C1 C2 C3 C6 -179.8(8) . . . . ? C2 C3 C4 C5 -0.2(13) . . . . ? C6 C3 C4 C5 -179.8(7) . . . . ? C1 N1 C5 C4 -1.1(12) . . . . ? Ni1 N1 C5 C4 164.5(7) 7_565 . . . ? C3 C4 C5 N1 0.5(14) . . . . ? Ni1 O4 C6 C3 -170.3(6) . . . . ? Ni1 O4 C6 P1 -28.2(7) . . . . ? C4 C3 C6 O4 53.0(11) . . . . ? C2 C3 C6 O4 -126.7(8) . . . . ? C4 C3 C6 P1 -88.3(9) . . . . ? C2 C3 C6 P1 92.1(9) . . . . ? O2 P1 C6 O4 139.8(6) . . . . ? O3 P1 C6 O4 -101.0(6) . . . . ? O1 P1 C6 O4 20.8(7) . . . . ? O2 P1 C6 C3 -77.8(7) . . . . ? O3 P1 C6 C3 41.4(7) . . . . ? O1 P1 C6 C3 163.2(6) . . . . ?
1100771.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100771.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100771 loop_ _publ_author_name 'Deng-Ke Cao' 'Yi-Zhi Li' 'You Song' 'Li-Min Zheng' _publ_section_title ; Three-, Two-, and One-Dimensional Metal Phosphonates Based on [Hydroxy(4-pyridyl)methyl]phosphonate: M{(4-C5H4N)CH(OH)PO3}(H2O) (M = Ni, Cd) and Gd{(4-C5H4N)CH(OH)P(OH)O2}3.6H2O ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3599 _journal_page_last 3604 _journal_paper_doi 10.1021/ic0484248 _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C6 H8 Cd N O5 P' _chemical_formula_weight 317.50 _chemical_name_systematic ; ? ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 121.576(4) _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 23.344(6) _cell_length_b 5.2745(14) _cell_length_c 16.571(4) _cell_measurement_reflns_used 1042 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 26.942 _cell_measurement_theta_min 2.516 _cell_volume 1738.3(8) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 4K _diffrn_measured_fraction_theta_full 0.936 _diffrn_measured_fraction_theta_max 0.936 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0614 _diffrn_reflns_av_sigmaI/netI 0.0886 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 4535 _diffrn_reflns_theta_full 28.04 _diffrn_reflns_theta_max 28.04 _diffrn_reflns_theta_min 2.05 _exptl_absorpt_coefficient_mu 2.690 _exptl_absorpt_correction_T_max 0.9631 _exptl_absorpt_correction_T_min 0.6871 _exptl_absorpt_correction_type empirical _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 2.426 _exptl_crystal_density_method 'not measured' _exptl_crystal_description column _exptl_crystal_F_000 1232 _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _refine_diff_density_max 1.079 _refine_diff_density_min -2.046 _refine_diff_density_rms 0.211 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.218 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 133 _refine_ls_number_reflns 1963 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.218 _refine_ls_R_factor_all 0.0953 _refine_ls_R_factor_gt 0.0715 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0336P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1120 _refine_ls_wR_factor_ref 0.1192 _reflns_number_gt 1624 _reflns_number_total 1963 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic0484248si20050317_103348_2.cif _cod_data_source_block Cd{(4-C5H4N)CH(OH)PO3}(H2O) _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_database_code 1100771 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.08218(3) 0.64814(11) 0.02397(4) 0.01878(19) Uani 1 1 d . . . P1 P 0.44767(10) 0.6142(4) 0.36485(14) 0.0181(5) Uani 1 1 d . . . O1 O 0.4148(3) 0.3601(11) 0.3553(4) 0.0247(13) Uani 1 1 d . . . O1W O 0.0851(3) 0.3550(12) -0.0788(4) 0.0278(14) Uani 1 1 d G . . H1WA H 0.0660 0.4197 -0.1384 0.039 Uiso 1 1 d G . . H1WB H 0.0681 0.2022 -0.0743 0.039 Uiso 1 1 d G . . O2 O 0.5227(3) 0.5936(11) 0.4040(4) 0.0279(15) Uani 1 1 d . . . O3 O 0.4343(4) 0.8041(12) 0.4208(4) 0.047(2) Uani 1 1 d . . . N1 N 0.1951(3) 0.7045(14) 0.0899(5) 0.0247(17) Uani 1 1 d . . . C1 C 0.2319(4) 0.5321(18) 0.0774(6) 0.031(2) Uani 1 1 d . . . H1A H 0.2100 0.4010 0.0344 0.037 Uiso 1 1 calc R . . C2 C 0.3014(4) 0.5421(18) 0.1260(6) 0.026(2) Uani 1 1 d . . . H2A H 0.3254 0.4185 0.1157 0.031 Uiso 1 1 calc R . . C3 C 0.3353(4) 0.7357(16) 0.1898(5) 0.0185(18) Uani 1 1 d . . . C4 C 0.2972(4) 0.9148(17) 0.2002(6) 0.027(2) Uani 1 1 d . . . H4A H 0.3179 1.0515 0.2408 0.033 Uiso 1 1 calc R . . C5 C 0.2278(4) 0.8927(16) 0.1504(6) 0.025(2) Uani 1 1 d . . . H5A H 0.2029 1.0145 0.1597 0.030 Uiso 1 1 calc R . . C6 C 0.4113(4) 0.7425(16) 0.2448(5) 0.0188(18) Uani 1 1 d . . . H6A H 0.4270 0.6392 0.2110 0.023 Uiso 1 1 calc R . . O4 O 0.4353(3) 0.9989(13) 0.2512(5) 0.0383(17) Uani 1 1 d D . . H4 H 0.399(3) 1.069(18) 0.247(7) 0.054 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0147(3) 0.0202(3) 0.0203(3) 0.0030(3) 0.0083(2) -0.0002(3) P1 0.0207(11) 0.0131(12) 0.0159(10) -0.0009(8) 0.0065(9) 0.0010(9) O1 0.020(3) 0.028(4) 0.022(3) 0.000(3) 0.009(2) 0.000(3) O1W 0.035(3) 0.025(4) 0.026(3) 0.004(3) 0.018(3) -0.007(3) O2 0.018(3) 0.024(4) 0.027(3) 0.004(3) 0.002(3) -0.002(2) O3 0.089(6) 0.024(4) 0.031(4) 0.006(3) 0.033(4) 0.016(4) N1 0.013(3) 0.031(5) 0.026(4) -0.003(3) 0.007(3) 0.000(3) C1 0.018(5) 0.036(6) 0.026(5) -0.013(4) 0.003(4) -0.013(4) C2 0.016(4) 0.036(5) 0.029(5) -0.008(4) 0.014(4) -0.001(4) C3 0.015(4) 0.026(5) 0.014(4) 0.008(3) 0.007(3) 0.002(3) C4 0.028(5) 0.021(5) 0.030(5) -0.006(4) 0.013(4) -0.003(4) C5 0.025(5) 0.027(5) 0.029(5) -0.005(4) 0.018(4) 0.004(4) C6 0.011(4) 0.028(5) 0.013(4) 0.002(3) 0.002(3) -0.002(3) O4 0.031(4) 0.041(5) 0.046(4) 0.010(4) 0.023(3) 0.000(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Cd1 O2 137.4(2) 4_545 8_465 ? O3 Cd1 O1 88.3(2) 4_545 4 ? O2 Cd1 O1 101.9(2) 8_465 4 ? O3 Cd1 N1 108.9(3) 4_545 . ? O2 Cd1 N1 112.1(2) 8_465 . ? O1 Cd1 N1 91.1(2) 4 . ? O3 Cd1 O1W 80.3(2) 4_545 . ? O2 Cd1 O1W 89.8(2) 8_465 . ? O1 Cd1 O1W 167.6(2) 4 . ? N1 Cd1 O1W 88.1(2) . . ? O3 P1 O1 113.4(4) . . ? O3 P1 O2 110.5(4) . . ? O1 P1 O2 113.0(3) . . ? O3 P1 C6 107.2(4) . . ? O1 P1 C6 107.0(3) . . ? O2 P1 C6 105.3(3) . . ? P1 O1 Cd1 124.5(3) . 4_545 ? P1 O2 Cd1 112.5(3) . 8_566 ? P1 O3 Cd1 164.3(4) . 4 ? C5 N1 C1 117.5(7) . . ? C5 N1 Cd1 121.3(5) . . ? C1 N1 Cd1 120.7(6) . . ? N1 C1 C2 122.4(8) . . ? C3 C2 C1 120.0(8) . . ? C4 C3 C2 117.2(7) . . ? C4 C3 C6 122.9(8) . . ? C2 C3 C6 119.9(8) . . ? C3 C4 C5 120.1(8) . . ? N1 C5 C4 122.8(8) . . ? O4 C6 C3 110.7(7) . . ? O4 C6 P1 108.9(5) . . ? C3 C6 P1 112.0(5) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O3 2.155(6) 4_545 ? Cd1 O2 2.202(6) 8_465 ? Cd1 O1 2.261(6) 4 ? Cd1 N1 2.283(6) . ? Cd1 O1W 2.327(6) . ? P1 O3 1.505(7) . ? P1 O1 1.511(6) . ? P1 O2 1.520(6) . ? P1 C6 1.835(8) . ? O1 Cd1 2.261(6) 4_545 ? O2 Cd1 2.202(6) 8_566 ? O3 Cd1 2.155(6) 4 ? N1 C5 1.331(10) . ? N1 C1 1.340(11) . ? C1 C2 1.384(11) . ? C2 C3 1.383(11) . ? C3 C4 1.369(11) . ? C3 C6 1.512(10) . ? C4 C5 1.386(11) . ? C6 O4 1.446(10) . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1WA O4 0.91 1.90 2.750(9) 153.8 7_565 O1W H1WB O2 0.92 1.81 2.714(8) 166.3 8_455 O4 H4 O1 0.902(10) 2.23(9) 2.774(9) 118(7) 1_565 loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 P1 O1 Cd1 -46.4(5) . . . 4_545 ? O2 P1 O1 Cd1 80.2(4) . . . 4_545 ? C6 P1 O1 Cd1 -164.3(4) . . . 4_545 ? O3 P1 O2 Cd1 -1.2(4) . . . 8_566 ? O1 P1 O2 Cd1 -129.4(3) . . . 8_566 ? C6 P1 O2 Cd1 114.2(4) . . . 8_566 ? O1 P1 O3 Cd1 -150.2(17) . . . 4 ? O2 P1 O3 Cd1 81.9(18) . . . 4 ? C6 P1 O3 Cd1 -32.4(19) . . . 4 ? O3 Cd1 N1 C5 -111.7(7) 4_545 . . . ? O2 Cd1 N1 C5 80.2(7) 8_465 . . . ? O1 Cd1 N1 C5 -23.1(7) 4 . . . ? O1W Cd1 N1 C5 169.3(7) . . . . ? O3 Cd1 N1 C1 60.5(7) 4_545 . . . ? O2 Cd1 N1 C1 -107.6(7) 8_465 . . . ? O1 Cd1 N1 C1 149.1(7) 4 . . . ? O1W Cd1 N1 C1 -18.5(7) . . . . ? C5 N1 C1 C2 1.2(13) . . . . ? Cd1 N1 C1 C2 -171.3(7) . . . . ? N1 C1 C2 C3 -0.4(14) . . . . ? C1 C2 C3 C4 -1.4(13) . . . . ? C1 C2 C3 C6 178.4(8) . . . . ? C2 C3 C4 C5 2.3(13) . . . . ? C6 C3 C4 C5 -177.5(8) . . . . ? C1 N1 C5 C4 -0.4(13) . . . . ? Cd1 N1 C5 C4 172.1(6) . . . . ? C3 C4 C5 N1 -1.4(13) . . . . ? C4 C3 C6 O4 -40.8(10) . . . . ? C2 C3 C6 O4 139.4(8) . . . . ? C4 C3 C6 P1 80.9(9) . . . . ? C2 C3 C6 P1 -98.9(8) . . . . ? O3 P1 C6 O4 51.2(6) . . . . ? O1 P1 C6 O4 173.1(5) . . . . ? O2 P1 C6 O4 -66.4(6) . . . . ? O3 P1 C6 C3 -71.5(7) . . . . ? O1 P1 C6 C3 50.4(7) . . . . ? O2 P1 C6 C3 170.8(6) . . . . ?
1100772.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100772.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100772 loop_ _publ_author_name 'Deng-Ke Cao' 'Yi-Zhi Li' 'You Song' 'Li-Min Zheng' _publ_section_title ; Three-, Two-, and One-Dimensional Metal Phosphonates Based on [Hydroxy(4-pyridyl)methyl]phosphonate: M{(4-C5H4N)CH(OH)PO3}(H2O) (M = Ni, Cd) and Gd{(4-C5H4N)CH(OH)P(OH)O2}3.6H2O ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3599 _journal_page_last 3604 _journal_paper_doi 10.1021/ic0484248 _journal_volume 44 _journal_year 2005 _chemical_formula_moiety 'C18 H21 Gd N3 O12 P3, 6(H2 O)' _chemical_formula_sum 'C18 H33 Gd N3 O18 P3' _chemical_formula_weight 829.63 _chemical_name_systematic ; ? ; _space_group_IT_number 148 _symmetry_cell_setting rhombohedral _symmetry_space_group_name_Hall '-R 3' _symmetry_space_group_name_H-M 'R -3 :H' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_formula_units_Z 6 _cell_length_a 22.2714(16) _cell_length_b 22.2714(16) _cell_length_c 9.8838(11) _cell_measurement_reflns_used 647 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 18.078 _cell_measurement_theta_min 3.166 _cell_volume 4245.7(6) _computing_cell_refinement SMART _computing_data_collection 'SMART (Bruker, 2000)' _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _computing_structure_refinement SHELXTL _computing_structure_solution 'SHELXTL (Bruker, 2000)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker Smart Aepex CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0225 _diffrn_reflns_av_sigmaI/netI 0.0410 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 7268 _diffrn_reflns_theta_full 25.99 _diffrn_reflns_theta_max 25.99 _diffrn_reflns_theta_min 1.83 _exptl_absorpt_coefficient_mu 2.600 _exptl_absorpt_correction_T_max 0.56 _exptl_absorpt_correction_T_min 0.46 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS(Bruker, 2000)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.947 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 2490 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _refine_diff_density_max 0.927 _refine_diff_density_min -0.756 _refine_diff_density_rms 0.189 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 131 _refine_ls_number_reflns 1856 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.995 _refine_ls_R_factor_all 0.0627 _refine_ls_R_factor_gt 0.0516 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1200P)^2^+1.9900P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1502 _refine_ls_wR_factor_ref 0.1532 _reflns_number_gt 1419 _reflns_number_total 1856 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic0484248si20050317_103348_3.cif _cod_data_source_block Gd{(4-C5H4N)CH(OH)P(OH)O2}3.6H2O _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Rhombohedral' changed to 'rhombohedral' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_sg_symbol_H-M 'R -3' _cod_database_code 1100772 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.0000 0.0000 0.0000 0.0224(3) Uani 1 6 d S . . Gd2 Gd 0.0000 0.0000 0.5000 0.0220(3) Uani 1 6 d S . . P1 P -0.02670(9) 0.10377(9) 0.25873(17) 0.0269(4) Uani 1 1 d . . . C1 C 0.1141(4) 0.3598(4) 0.2008(8) 0.0379(16) Uani 1 1 d . . . H1B H 0.1174 0.4009 0.2313 0.045 Uiso 1 1 calc R . . C2 C 0.0839(4) 0.2989(4) 0.2844(7) 0.0365(16) Uani 1 1 d . . . H2A H 0.0669 0.2998 0.3699 0.044 Uiso 1 1 calc R . . C3 C 0.0804(4) 0.2393(3) 0.2367(7) 0.0355(17) Uani 1 1 d . . . C4 C 0.1082(3) 0.2422(4) 0.1072(7) 0.0323(15) Uani 1 1 d . . . H4D H 0.1112 0.2049 0.0730 0.039 Uiso 1 1 calc R . . C5 C 0.1306(4) 0.3020(4) 0.0327(7) 0.0326(15) Uani 1 1 d . . . H5A H 0.1411 0.3007 -0.0580 0.039 Uiso 1 1 calc R . . C6 C 0.0518(4) 0.1755(3) 0.3254(7) 0.0327(15) Uani 1 1 d . . . H6A H 0.0868 0.1612 0.3323 0.039 Uiso 1 1 calc R . . N1 N 0.1378(3) 0.3561(3) 0.0763(6) 0.0385(15) Uani 1 1 d . . . O1 O -0.0500(2) 0.0496(3) 0.3733(4) 0.0300(10) Uani 1 1 d . . . O2 O -0.0091(2) 0.0798(2) 0.1283(4) 0.0244(9) Uani 1 1 d . . . O3 O -0.0781(3) 0.1289(2) 0.2415(4) 0.0314(10) Uani 1 1 d . . . H3B H -0.0852 0.1418 0.3177 0.038 Uiso 1 1 d R . . O4 O 0.0407(3) 0.1944(3) 0.4568(5) 0.0372(12) Uani 1 1 d . . . H4A H 0.0783 0.2280 0.4869 0.045 Uiso 1 1 d R . . O1W O 0.8886(2) 0.3104(3) 0.1050(4) 0.0317(10) Uani 1 1 d . . . H5E H 0.8517 0.2893 0.0582 0.038 Uiso 1 1 d R . . H5C H 0.8745 0.3201 0.1773 0.038 Uiso 1 1 d R . . O2W O 0.9751(3) 0.2566(3) 0.0360(5) 0.0372(12) Uani 1 1 d . . . H6E H 0.9496 0.2731 0.0593 0.045 Uiso 1 1 d R . . H6B H 1.0156 0.2816 0.0685 0.045 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.0207(3) 0.0207(3) 0.0260(4) 0.000 0.000 0.01034(15) Gd2 0.0238(3) 0.0238(3) 0.0185(4) 0.000 0.000 0.01188(15) P1 0.0336(9) 0.0297(9) 0.0144(7) 0.0006(6) -0.0006(7) 0.0135(7) C1 0.043(4) 0.025(3) 0.042(4) 0.008(3) 0.011(3) 0.014(3) C2 0.041(4) 0.043(4) 0.028(4) -0.002(3) 0.002(3) 0.023(3) C3 0.050(4) 0.008(3) 0.037(4) -0.005(3) -0.005(3) 0.005(3) C4 0.027(3) 0.031(3) 0.029(4) -0.003(3) -0.004(3) 0.007(3) C5 0.036(4) 0.050(4) 0.022(3) 0.000(3) -0.003(3) 0.029(3) C6 0.032(4) 0.024(3) 0.032(4) -0.004(3) 0.001(3) 0.007(3) N1 0.036(3) 0.021(3) 0.032(3) 0.012(2) 0.005(3) -0.006(2) O1 0.030(2) 0.048(3) 0.014(2) -0.0050(19) -0.0107(17) 0.021(2) O2 0.0138(19) 0.022(2) 0.029(2) -0.0019(18) -0.0005(16) 0.0029(17) O3 0.048(3) 0.043(3) 0.014(2) 0.0072(19) 0.005(2) 0.031(2) O4 0.038(3) 0.032(3) 0.029(3) 0.003(2) -0.001(2) 0.008(2) O1W 0.033(2) 0.044(3) 0.019(2) -0.006(2) -0.0065(19) 0.021(2) O2W 0.038(3) 0.055(3) 0.025(3) -0.001(2) -0.003(2) 0.029(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Gd1 O2 88.08(15) 10 3 ? O2 Gd1 O2 91.92(15) 10 12 ? O2 Gd1 O2 180.0(3) 3 12 ? O2 Gd1 O2 180.0(2) 10 . ? O2 Gd1 O2 91.92(15) 3 . ? O2 Gd1 O2 88.08(15) 12 . ? O2 Gd1 O2 91.92(15) 10 11 ? O2 Gd1 O2 88.08(15) 3 11 ? O2 Gd1 O2 91.92(15) 12 11 ? O2 Gd1 O2 88.08(15) . 11 ? O2 Gd1 O2 88.08(15) 10 2 ? O2 Gd1 O2 91.92(15) 3 2 ? O2 Gd1 O2 88.08(15) 12 2 ? O2 Gd1 O2 91.92(15) . 2 ? O2 Gd1 O2 180.0(4) 11 2 ? O1 Gd2 O1 180.00(19) 11_556 2 ? O1 Gd2 O1 86.98(15) 11_556 3 ? O1 Gd2 O1 93.02(15) 2 3 ? O1 Gd2 O1 93.02(15) 11_556 12_556 ? O1 Gd2 O1 86.98(15) 2 12_556 ? O1 Gd2 O1 180.00(19) 3 12_556 ? O1 Gd2 O1 93.02(15) 11_556 10_556 ? O1 Gd2 O1 86.98(15) 2 10_556 ? O1 Gd2 O1 86.98(15) 3 10_556 ? O1 Gd2 O1 93.02(15) 12_556 10_556 ? O1 Gd2 O1 86.98(15) 11_556 . ? O1 Gd2 O1 93.02(15) 2 . ? O1 Gd2 O1 93.02(15) 3 . ? O1 Gd2 O1 86.98(15) 12_556 . ? O1 Gd2 O1 180.00(17) 10_556 . ? O3 P1 O2 114.2(3) . . ? O3 P1 O1 110.5(3) . . ? O2 P1 O1 113.1(3) . . ? O3 P1 C6 107.0(3) . . ? O2 P1 C6 108.3(3) . . ? O1 P1 C6 102.8(3) . . ? N1 C1 C2 118.4(6) . . ? N1 C1 H1B 120.8 . . ? C2 C1 H1B 120.8 . . ? C3 C2 C1 119.3(7) . . ? C3 C2 H2A 120.4 . . ? C1 C2 H2A 120.4 . . ? C2 C3 C4 117.1(6) . . ? C2 C3 C6 120.2(7) . . ? C4 C3 C6 122.6(6) . . ? C5 C4 C3 117.9(7) . . ? C5 C4 H4D 121.0 . . ? C3 C4 H4D 121.0 . . ? N1 C5 C4 125.1(7) . . ? N1 C5 H5A 117.5 . . ? C4 C5 H5A 117.5 . . ? O4 C6 C3 107.7(5) . . ? O4 C6 P1 111.1(5) . . ? C3 C6 P1 112.8(5) . . ? O4 C6 H6A 108.4 . . ? C3 C6 H6A 108.4 . . ? P1 C6 H6A 108.4 . . ? C5 N1 C1 121.4(6) . . ? P1 O1 Gd2 136.3(3) . . ? P1 O2 Gd1 152.5(3) . . ? P1 O3 H3B 109.2 . . ? C6 O4 H4A 109.8 . . ? H5E O1W H5C 102.7 . . ? H6E O2W H6B 109.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O2 2.273(4) 10 ? Gd1 O2 2.273(4) 3 ? Gd1 O2 2.273(4) 12 ? Gd1 O2 2.273(4) . ? Gd1 O2 2.273(4) 11 ? Gd1 O2 2.273(4) 2 ? Gd2 O1 2.293(4) 11_556 ? Gd2 O1 2.293(4) 2 ? Gd2 O1 2.293(4) 3 ? Gd2 O1 2.293(4) 12_556 ? Gd2 O1 2.293(4) 10_556 ? Gd2 O1 2.293(4) . ? P1 O3 1.513(5) . ? P1 O2 1.520(5) . ? P1 O1 1.543(5) . ? P1 C6 1.803(7) . ? C1 N1 1.358(10) . ? C1 C2 1.436(10) . ? C1 H1B 0.9300 . ? C2 C3 1.374(10) . ? C2 H2A 0.9300 . ? C3 C4 1.409(10) . ? C3 C6 1.513(9) . ? C4 C5 1.378(10) . ? C4 H4D 0.9300 . ? C5 N1 1.212(9) . ? C5 H5A 0.9300 . ? C6 O4 1.425(8) . ? C6 H6A 0.9800 . ? O3 H3B 0.8498 . ? O4 H4A 0.8498 . ? O1W H5E 0.8500 . ? O1W H5C 0.8503 . ? O2W H6E 0.8501 . ? O2W H6B 0.8498 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3B N1 0.85 1.87 2.621(7) 146.6 6_455 O4 H4A N1 0.85 2.54 3.376(8) 169.2 16 O1W H5E O3 0.85 2.20 2.878(7) 136.2 13 O1W H5C O2W 0.85 2.37 2.882(6) 119.1 6_665 O2W H6E O1W 0.85 1.97 2.816(7) 177.4 . O2W H6B N1 0.85 2.38 3.189(8) 159.7 1_655
1100773.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100773.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100773 loop_ _publ_author_name 'Nicola Y. Edwards' 'Rebecca A. Eikey' 'Megan I. Loring' 'Mahdi M. Abu-Omar' _publ_section_title ; High-Valent Imido Complexes of Manganese and Chromium Corroles ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3700 _journal_page_last 3708 _journal_paper_doi 10.1021/ic0484506 _journal_volume 44 _journal_year 2005 _chemical_formula_moiety 'C46 H19 Cr F15 N5, C7 H8 ' _chemical_formula_sum 'C53 H27 Cr F15 N5' _chemical_formula_weight 1070.80 _chemical_name_systematic ; ? ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 99.792(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 14.9131(12) _cell_length_b 12.6146(10) _cell_length_c 24.0113(19) _cell_measurement_reflns_used 4792 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 27.41 _cell_measurement_theta_min 2.21 _cell_volume 4451.3(6) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.968 _diffrn_measured_fraction_theta_max 0.968 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0481 _diffrn_reflns_av_sigmaI/netI 0.0705 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 28739 _diffrn_reflns_theta_full 28.30 _diffrn_reflns_theta_max 28.30 _diffrn_reflns_theta_min 1.83 _exptl_absorpt_coefficient_mu 0.366 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.815 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Sadabs (Bruker)' _exptl_crystal_colour black _exptl_crystal_density_diffrn 1.598 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 2156 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _refine_diff_density_max 0.389 _refine_diff_density_min -0.467 _refine_diff_density_rms 0.072 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 671 _refine_ls_number_reflns 10704 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.022 _refine_ls_R_factor_all 0.0997 _refine_ls_R_factor_gt 0.0437 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0368P)^2^+3.6526P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0910 _refine_ls_wR_factor_ref 0.1160 _reflns_number_gt 6523 _reflns_number_total 10704 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic0484506si20041104_031204.cif _cod_data_source_block abu402sm _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_database_code 1100773 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr1 Cr 0.49631(3) 0.30256(3) 0.635739(17) 0.01638(10) Uani 1 1 d . . . F1 F 0.74871(13) 0.02480(14) 0.71195(8) 0.0465(5) Uani 1 1 d . . . F2 F 0.89073(13) -0.05692(16) 0.78446(10) 0.0649(7) Uani 1 1 d . . . F3 F 0.93506(12) 0.02287(17) 0.88961(10) 0.0717(8) Uani 1 1 d . . . F4 F 0.83044(17) 0.17599(17) 0.92556(9) 0.0774(8) Uani 1 1 d . . . F5 F 0.68893(14) 0.25756(14) 0.85367(7) 0.0496(5) Uani 1 1 d . . . F6 F 0.64989(11) 0.71469(12) 0.65103(7) 0.0300(4) Uani 1 1 d . . . F7 F 0.78124(12) 0.85191(12) 0.63496(7) 0.0382(4) Uani 1 1 d . . . F8 F 0.91438(11) 0.79127(14) 0.57763(8) 0.0431(5) Uani 1 1 d . . . F9 F 0.91241(10) 0.59284(14) 0.53315(7) 0.0362(4) Uani 1 1 d . . . F10 F 0.78065(10) 0.45559(12) 0.54731(7) 0.0298(4) Uani 1 1 d . . . F11 F 0.19632(11) 0.24237(14) 0.75563(7) 0.0389(4) Uani 1 1 d . . . F12 F 0.05471(12) 0.12302(17) 0.77424(8) 0.0548(5) Uani 1 1 d . . . F13 F 0.01750(12) -0.06281(16) 0.71753(9) 0.0552(6) Uani 1 1 d . . . F14 F 0.12255(12) -0.12819(14) 0.64332(8) 0.0477(5) Uani 1 1 d . . . F15 F 0.26600(11) -0.01049(13) 0.62569(8) 0.0378(4) Uani 1 1 d . . . N1 N 0.48189(14) 0.21018(16) 0.69900(8) 0.0181(4) Uani 1 1 d . . . N2 N 0.61843(14) 0.34404(16) 0.67045(8) 0.0181(4) Uani 1 1 d . . . N3 N 0.48709(14) 0.44340(16) 0.60253(9) 0.0186(4) Uani 1 1 d . . . N4 N 0.36810(14) 0.33237(16) 0.63046(9) 0.0197(5) Uani 1 1 d . . . N5 N 0.50539(13) 0.22535(15) 0.58226(9) 0.0177(4) Uani 1 1 d . . . C1 C 0.40255(17) 0.15912(19) 0.70770(10) 0.0187(5) Uani 1 1 d . . . C2 C 0.42680(18) 0.0806(2) 0.75088(11) 0.0219(6) Uani 1 1 d . . . H2 H 0.3859 0.0339 0.7650 0.026 Uiso 1 1 calc R . . C3 C 0.51806(18) 0.0846(2) 0.76809(11) 0.0224(6) Uani 1 1 d . . . H3 H 0.5526 0.0417 0.7965 0.027 Uiso 1 1 calc R . . C4 C 0.55289(17) 0.16505(19) 0.73584(10) 0.0183(5) Uani 1 1 d . . . C5 C 0.64314(17) 0.19804(19) 0.73945(10) 0.0189(5) Uani 1 1 d . . . C6 C 0.67443(16) 0.28104(19) 0.70924(10) 0.0184(5) Uani 1 1 d . . . C7 C 0.76593(17) 0.3180(2) 0.71340(11) 0.0221(6) Uani 1 1 d . . . H7 H 0.8179 0.2894 0.7370 0.026 Uiso 1 1 calc R . . C8 C 0.76536(17) 0.4017(2) 0.67752(11) 0.0209(5) Uani 1 1 d . . . H8 H 0.8170 0.4415 0.6716 0.025 Uiso 1 1 calc R . . C9 C 0.67399(17) 0.41941(19) 0.65035(10) 0.0188(5) Uani 1 1 d . . . C10 C 0.64190(17) 0.50142(19) 0.61254(11) 0.0195(5) Uani 1 1 d . . . C11 C 0.54991(18) 0.51527(19) 0.59059(11) 0.0205(5) Uani 1 1 d . . . C12 C 0.50162(18) 0.5982(2) 0.55759(11) 0.0247(6) Uani 1 1 d . . . H12 H 0.5280 0.6584 0.5430 0.030 Uiso 1 1 calc R . . C13 C 0.41058(19) 0.5753(2) 0.55070(11) 0.0264(6) Uani 1 1 d . . . H13 H 0.3625 0.6167 0.5306 0.032 Uiso 1 1 calc R . . C14 C 0.40157(17) 0.47815(19) 0.57919(11) 0.0206(5) Uani 1 1 d . . . C15 C 0.33271(17) 0.41151(19) 0.59361(11) 0.0201(5) Uani 1 1 d . . . C16 C 0.23702(18) 0.3993(2) 0.58173(11) 0.0237(6) Uani 1 1 d . . . H16 H 0.1954 0.4431 0.5576 0.028 Uiso 1 1 calc R . . C17 C 0.21526(17) 0.3125(2) 0.61140(11) 0.0228(6) Uani 1 1 d . . . H17 H 0.1558 0.2853 0.6113 0.027 Uiso 1 1 calc R . . C18 C 0.29779(17) 0.27046(19) 0.64229(11) 0.0190(5) Uani 1 1 d . . . C19 C 0.31529(17) 0.18534(19) 0.67955(10) 0.0197(5) Uani 1 1 d . . . C20 C 0.71501(17) 0.1441(2) 0.78062(11) 0.0208(5) Uani 1 1 d . . . C21 C 0.76767(19) 0.0631(2) 0.76465(12) 0.0291(6) Uani 1 1 d . . . C22 C 0.8412(2) 0.0216(2) 0.80074(16) 0.0397(8) Uani 1 1 d . . . C23 C 0.8631(2) 0.0618(3) 0.85388(16) 0.0437(9) Uani 1 1 d . . . C24 C 0.8112(2) 0.1396(3) 0.87266(13) 0.0426(9) Uani 1 1 d . . . C25 C 0.7376(2) 0.1800(2) 0.83556(12) 0.0313(7) Uani 1 1 d . . . C26 C 0.71042(17) 0.5800(2) 0.60014(11) 0.0218(6) Uani 1 1 d . . . C27 C 0.71289(18) 0.6832(2) 0.62083(11) 0.0242(6) Uani 1 1 d . . . C28 C 0.78051(19) 0.7538(2) 0.61345(12) 0.0278(6) Uani 1 1 d . . . C29 C 0.84801(19) 0.7233(2) 0.58453(13) 0.0319(7) Uani 1 1 d . . . C30 C 0.84703(18) 0.6229(2) 0.56209(12) 0.0281(6) Uani 1 1 d . . . C31 C 0.77893(18) 0.5532(2) 0.56984(11) 0.0240(6) Uani 1 1 d . . . C32 C 0.23635(17) 0.1202(2) 0.69027(11) 0.0212(5) Uani 1 1 d . . . C33 C 0.17990(18) 0.1511(2) 0.72756(11) 0.0269(6) Uani 1 1 d . . . C34 C 0.10644(19) 0.0906(3) 0.73690(13) 0.0347(7) Uani 1 1 d . . . C35 C 0.08741(19) -0.0029(2) 0.70814(14) 0.0356(7) Uani 1 1 d . . . C36 C 0.14114(19) -0.0359(2) 0.67056(13) 0.0323(7) Uani 1 1 d . . . C37 C 0.21472(18) 0.0249(2) 0.66254(12) 0.0276(6) Uani 1 1 d . . . C38 C 0.50842(16) 0.17675(18) 0.53170(10) 0.0168(5) Uani 1 1 d . . . C39 C 0.59275(17) 0.16888(18) 0.51211(11) 0.0186(5) Uani 1 1 d . . . C40 C 0.59155(18) 0.12975(19) 0.45817(11) 0.0218(6) Uani 1 1 d . . . H40 H 0.6471 0.1257 0.4439 0.026 Uiso 1 1 calc R . . C41 C 0.51120(18) 0.09593(19) 0.42390(11) 0.0219(6) Uani 1 1 d . . . C42 C 0.43041(18) 0.09981(19) 0.44576(11) 0.0212(6) Uani 1 1 d . . . H42 H 0.3762 0.0738 0.4234 0.025 Uiso 1 1 calc R . . C43 C 0.42615(17) 0.14005(19) 0.49868(10) 0.0185(5) Uani 1 1 d . . . C44 C 0.33818(17) 0.1476(2) 0.52061(11) 0.0250(6) Uani 1 1 d . . . H44A H 0.3215 0.2224 0.5234 0.038 Uiso 1 1 calc R . . H44B H 0.3451 0.1148 0.5581 0.038 Uiso 1 1 calc R . . H44C H 0.2904 0.1108 0.4947 0.038 Uiso 1 1 calc R . . C45 C 0.5111(2) 0.0566(2) 0.36498(12) 0.0303(6) Uani 1 1 d . . . H45A H 0.5296 -0.0180 0.3663 0.045 Uiso 1 1 calc R . . H45B H 0.5539 0.0986 0.3473 0.045 Uiso 1 1 calc R . . H45C H 0.4498 0.0635 0.3428 0.045 Uiso 1 1 calc R . . C46 C 0.67910(17) 0.2043(2) 0.54941(11) 0.0248(6) Uani 1 1 d . . . H46A H 0.7295 0.2015 0.5281 0.037 Uiso 1 1 calc R . . H46B H 0.6922 0.1573 0.5823 0.037 Uiso 1 1 calc R . . H46C H 0.6717 0.2771 0.5621 0.037 Uiso 1 1 calc R . . C1S C 0.0541(2) 0.7101(3) 0.96481(18) 0.0542(11) Uani 1 1 d . . . H1S H 0.0450 0.7291 1.0017 0.065 Uiso 1 1 calc R . . C2S C 0.0343(2) 0.7820(3) 0.9222(2) 0.0640(13) Uani 1 1 d . . . H2S H 0.0119 0.8502 0.9296 0.077 Uiso 1 1 calc R . . C3S C 0.0466(2) 0.7555(3) 0.8687(2) 0.0633(12) Uani 1 1 d . . . H3S H 0.0328 0.8055 0.8388 0.076 Uiso 1 1 calc R . . C4S C 0.0791(2) 0.6560(3) 0.85795(17) 0.0504(9) Uani 1 1 d . . . H4S H 0.0879 0.6375 0.8209 0.060 Uiso 1 1 calc R . . C5S C 0.0988(2) 0.5840(3) 0.90166(16) 0.0426(8) Uani 1 1 d . . . H5S H 0.1205 0.5155 0.8944 0.051 Uiso 1 1 calc R . . C6S C 0.0872(2) 0.6105(3) 0.95594(15) 0.0424(8) Uani 1 1 d . . . C7S C 0.1139(3) 0.5340(4) 1.00397(17) 0.0674(12) Uani 1 1 d . . . H7S1 H 0.1018 0.4613 0.9903 0.101 Uiso 1 1 calc R . . H7S2 H 0.0783 0.5488 1.0339 0.101 Uiso 1 1 calc R . . H7S3 H 0.1788 0.5419 1.0191 0.101 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr1 0.0193(2) 0.01553(19) 0.0143(2) 0.00079(16) 0.00290(15) 0.00118(16) F1 0.0673(13) 0.0401(10) 0.0356(11) -0.0007(8) 0.0189(9) 0.0201(9) F2 0.0485(12) 0.0572(13) 0.0976(18) 0.0350(12) 0.0370(12) 0.0326(10) F3 0.0292(10) 0.0699(14) 0.1014(18) 0.0532(13) -0.0303(11) -0.0116(10) F4 0.113(2) 0.0625(14) 0.0377(12) 0.0043(11) -0.0427(12) -0.0157(13) F5 0.0815(14) 0.0385(10) 0.0254(10) -0.0091(8) -0.0009(9) 0.0151(10) F6 0.0347(9) 0.0243(8) 0.0322(9) -0.0034(7) 0.0095(7) -0.0043(7) F7 0.0456(11) 0.0244(9) 0.0438(11) -0.0018(8) 0.0057(8) -0.0122(7) F8 0.0366(10) 0.0445(11) 0.0487(11) 0.0077(9) 0.0092(8) -0.0207(8) F9 0.0246(9) 0.0519(11) 0.0332(10) 0.0057(8) 0.0084(7) -0.0002(8) F10 0.0339(9) 0.0268(8) 0.0297(9) -0.0010(7) 0.0081(7) 0.0021(7) F11 0.0367(10) 0.0482(11) 0.0349(10) -0.0107(8) 0.0146(8) 0.0045(8) F12 0.0408(11) 0.0817(15) 0.0504(13) -0.0020(11) 0.0322(10) 0.0010(10) F13 0.0354(10) 0.0647(13) 0.0701(14) 0.0186(11) 0.0226(10) -0.0156(9) F14 0.0434(11) 0.0355(10) 0.0654(14) -0.0032(9) 0.0126(10) -0.0161(8) F15 0.0365(10) 0.0339(9) 0.0482(11) -0.0137(8) 0.0223(8) -0.0099(7) N1 0.0213(11) 0.0175(10) 0.0156(11) 0.0006(8) 0.0038(9) 0.0012(8) N2 0.0245(11) 0.0162(10) 0.0137(11) 0.0015(8) 0.0033(9) 0.0007(8) N3 0.0220(11) 0.0175(10) 0.0157(11) 0.0010(8) 0.0019(9) 0.0009(8) N4 0.0211(11) 0.0194(11) 0.0193(11) 0.0020(9) 0.0054(9) 0.0034(8) N5 0.0191(11) 0.0181(10) 0.0159(11) 0.0019(8) 0.0026(8) -0.0012(8) C1 0.0217(13) 0.0177(12) 0.0180(13) 0.0001(10) 0.0068(11) -0.0004(10) C2 0.0265(14) 0.0223(13) 0.0183(14) 0.0028(11) 0.0078(11) -0.0010(11) C3 0.0263(14) 0.0232(13) 0.0180(13) 0.0051(11) 0.0052(11) 0.0021(11) C4 0.0247(13) 0.0162(12) 0.0145(13) -0.0004(10) 0.0046(10) 0.0013(10) C5 0.0239(13) 0.0168(12) 0.0150(12) -0.0001(10) 0.0006(10) 0.0026(10) C6 0.0195(12) 0.0201(13) 0.0148(13) -0.0010(10) 0.0010(10) 0.0007(10) C7 0.0236(13) 0.0228(14) 0.0189(13) -0.0004(11) 0.0009(11) 0.0014(10) C8 0.0208(13) 0.0232(13) 0.0185(13) 0.0012(11) 0.0026(11) -0.0027(10) C9 0.0241(13) 0.0168(12) 0.0165(13) -0.0020(10) 0.0060(11) -0.0020(10) C10 0.0262(14) 0.0149(12) 0.0180(13) 0.0003(10) 0.0052(11) -0.0018(10) C11 0.0277(14) 0.0176(12) 0.0163(13) 0.0006(10) 0.0041(11) -0.0009(10) C12 0.0319(15) 0.0173(13) 0.0237(15) 0.0058(11) 0.0012(12) -0.0015(11) C13 0.0304(15) 0.0201(13) 0.0259(15) 0.0038(11) -0.0029(12) 0.0029(11) C14 0.0237(13) 0.0198(13) 0.0170(13) 0.0021(10) -0.0002(11) 0.0021(10) C15 0.0238(13) 0.0175(12) 0.0182(13) 0.0003(10) 0.0015(11) 0.0047(10) C16 0.0241(14) 0.0227(13) 0.0235(14) 0.0001(11) 0.0021(11) 0.0059(11) C17 0.0187(13) 0.0278(14) 0.0223(14) -0.0010(11) 0.0049(11) 0.0031(11) C18 0.0210(13) 0.0193(12) 0.0174(13) -0.0023(10) 0.0055(10) 0.0027(10) C19 0.0227(13) 0.0220(13) 0.0161(13) -0.0017(10) 0.0079(10) 0.0019(10) C20 0.0227(13) 0.0207(13) 0.0183(13) 0.0042(11) 0.0018(11) -0.0015(10) C21 0.0309(16) 0.0277(15) 0.0303(17) 0.0081(12) 0.0094(13) 0.0025(12) C22 0.0259(16) 0.0338(17) 0.063(2) 0.0221(16) 0.0168(16) 0.0067(13) C23 0.0218(16) 0.0408(19) 0.062(2) 0.0284(18) -0.0117(15) -0.0071(14) C24 0.051(2) 0.0385(18) 0.0297(18) 0.0090(14) -0.0179(15) -0.0162(16) C25 0.0417(17) 0.0233(15) 0.0261(16) 0.0023(12) -0.0021(13) -0.0007(12) C26 0.0244(14) 0.0208(13) 0.0189(14) 0.0046(11) -0.0001(11) -0.0035(10) C27 0.0277(14) 0.0244(14) 0.0210(14) 0.0040(11) 0.0049(11) -0.0016(11) C28 0.0359(16) 0.0201(14) 0.0254(15) 0.0028(12) -0.0007(13) -0.0059(12) C29 0.0294(16) 0.0341(16) 0.0307(17) 0.0085(13) 0.0007(13) -0.0120(12) C30 0.0230(14) 0.0389(16) 0.0227(15) 0.0067(13) 0.0048(12) 0.0011(12) C31 0.0287(15) 0.0235(14) 0.0185(14) 0.0022(11) -0.0001(11) -0.0026(11) C32 0.0216(13) 0.0247(13) 0.0179(13) 0.0055(11) 0.0052(11) 0.0042(10) C33 0.0271(15) 0.0319(15) 0.0218(15) 0.0031(12) 0.0041(12) 0.0068(12) C34 0.0249(15) 0.054(2) 0.0292(17) 0.0100(15) 0.0159(13) 0.0067(14) C35 0.0229(15) 0.0424(18) 0.0429(19) 0.0153(15) 0.0094(13) -0.0037(13) C36 0.0306(16) 0.0294(15) 0.0370(18) 0.0046(13) 0.0066(13) -0.0052(12) C37 0.0247(15) 0.0284(15) 0.0317(16) 0.0026(12) 0.0109(12) 0.0016(11) C38 0.0234(13) 0.0143(12) 0.0134(12) 0.0029(9) 0.0046(10) 0.0014(9) C39 0.0234(13) 0.0140(12) 0.0183(13) 0.0037(10) 0.0032(11) 0.0025(9) C40 0.0253(14) 0.0185(12) 0.0230(14) 0.0013(11) 0.0079(11) 0.0018(10) C41 0.0308(15) 0.0176(13) 0.0178(14) -0.0002(10) 0.0057(11) 0.0035(10) C42 0.0275(14) 0.0170(12) 0.0182(13) -0.0007(10) 0.0015(11) -0.0031(10) C43 0.0219(13) 0.0153(12) 0.0180(13) 0.0033(10) 0.0026(10) -0.0013(10) C44 0.0235(14) 0.0289(14) 0.0231(14) -0.0042(12) 0.0050(11) -0.0056(11) C45 0.0387(17) 0.0317(15) 0.0213(15) -0.0068(12) 0.0077(12) -0.0011(13) C46 0.0214(13) 0.0284(14) 0.0251(15) -0.0021(12) 0.0048(11) 0.0004(11) C1S 0.0233(16) 0.059(2) 0.079(3) -0.036(2) 0.0048(17) -0.0034(16) C2S 0.0250(18) 0.038(2) 0.127(4) -0.018(3) 0.007(2) -0.0007(15) C3S 0.0260(19) 0.053(2) 0.109(4) 0.025(3) 0.006(2) -0.0079(17) C4S 0.0310(18) 0.063(2) 0.057(2) -0.002(2) 0.0067(17) -0.0099(17) C5S 0.0225(16) 0.0394(18) 0.065(2) -0.0156(18) 0.0043(15) -0.0007(13) C6S 0.0212(15) 0.048(2) 0.055(2) -0.0110(17) -0.0039(15) -0.0006(14) C7S 0.042(2) 0.092(3) 0.063(3) 0.000(2) -0.005(2) 0.006(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Cr1 N4 106.12(10) . . ? N5 Cr1 N2 107.50(9) . . ? N4 Cr1 N2 145.24(9) . . ? N5 Cr1 N3 103.40(9) . . ? N4 Cr1 N3 78.16(9) . . ? N2 Cr1 N3 85.73(8) . . ? N5 Cr1 N1 106.85(9) . . ? N4 Cr1 N1 85.90(9) . . ? N2 Cr1 N1 92.65(8) . . ? N3 Cr1 N1 148.71(9) . . ? C4 N1 C1 106.9(2) . . ? C4 N1 Cr1 124.71(17) . . ? C1 N1 Cr1 126.89(16) . . ? C6 N2 C9 107.2(2) . . ? C6 N2 Cr1 123.12(16) . . ? C9 N2 Cr1 127.02(16) . . ? C11 N3 C14 108.9(2) . . ? C11 N3 Cr1 133.51(17) . . ? C14 N3 Cr1 117.07(16) . . ? C18 N4 C15 108.8(2) . . ? C18 N4 Cr1 131.06(17) . . ? C15 N4 Cr1 116.74(17) . . ? C38 N5 Cr1 169.59(18) . . ? N1 C1 C19 124.2(2) . . ? N1 C1 C2 108.1(2) . . ? C19 C1 C2 127.7(2) . . ? C3 C2 C1 108.1(2) . . ? C3 C2 H2 125.9 . . ? C1 C2 H2 125.9 . . ? C2 C3 C4 107.5(2) . . ? C2 C3 H3 126.2 . . ? C4 C3 H3 126.2 . . ? N1 C4 C5 122.8(2) . . ? N1 C4 C3 109.3(2) . . ? C5 C4 C3 127.9(2) . . ? C4 C5 C6 126.4(2) . . ? C4 C5 C20 118.8(2) . . ? C6 C5 C20 114.8(2) . . ? N2 C6 C5 124.1(2) . . ? N2 C6 C7 108.5(2) . . ? C5 C6 C7 127.4(2) . . ? C8 C7 C6 107.8(2) . . ? C8 C7 H7 126.1 . . ? C6 C7 H7 126.1 . . ? C7 C8 C9 108.3(2) . . ? C7 C8 H8 125.9 . . ? C9 C8 H8 125.9 . . ? N2 C9 C10 124.5(2) . . ? N2 C9 C8 108.2(2) . . ? C10 C9 C8 127.2(2) . . ? C11 C10 C9 122.8(2) . . ? C11 C10 C26 120.4(2) . . ? C9 C10 C26 116.7(2) . . ? N3 C11 C10 120.2(2) . . ? N3 C11 C12 107.6(2) . . ? C10 C11 C12 132.2(2) . . ? C13 C12 C11 107.9(2) . . ? C13 C12 H12 126.0 . . ? C11 C12 H12 126.0 . . ? C12 C13 C14 107.2(2) . . ? C12 C13 H13 126.4 . . ? C14 C13 H13 126.4 . . ? N3 C14 C15 111.9(2) . . ? N3 C14 C13 108.3(2) . . ? C15 C14 C13 139.7(2) . . ? N4 C15 C16 108.3(2) . . ? N4 C15 C14 111.9(2) . . ? C16 C15 C14 139.8(2) . . ? C17 C16 C15 107.5(2) . . ? C17 C16 H16 126.2 . . ? C15 C16 H16 126.2 . . ? C16 C17 C18 107.9(2) . . ? C16 C17 H17 126.1 . . ? C18 C17 H17 126.1 . . ? N4 C18 C19 120.3(2) . . ? N4 C18 C17 107.6(2) . . ? C19 C18 C17 132.1(2) . . ? C18 C19 C1 123.3(2) . . ? C18 C19 C32 117.9(2) . . ? C1 C19 C32 118.8(2) . . ? C25 C20 C21 116.7(2) . . ? C25 C20 C5 121.0(2) . . ? C21 C20 C5 122.1(2) . . ? F1 C21 C22 118.3(3) . . ? F1 C21 C20 119.4(2) . . ? C22 C21 C20 122.3(3) . . ? F2 C22 C23 119.7(3) . . ? F2 C22 C21 121.2(3) . . ? C23 C22 C21 119.1(3) . . ? F3 C23 C22 120.0(3) . . ? F3 C23 C24 119.0(3) . . ? C22 C23 C24 121.0(3) . . ? F4 C24 C23 121.1(3) . . ? F4 C24 C25 120.2(3) . . ? C23 C24 C25 118.7(3) . . ? F5 C25 C20 119.6(2) . . ? F5 C25 C24 118.3(3) . . ? C20 C25 C24 122.1(3) . . ? C27 C26 C31 115.8(2) . . ? C27 C26 C10 121.9(2) . . ? C31 C26 C10 122.2(2) . . ? F6 C27 C28 118.2(2) . . ? F6 C27 C26 119.4(2) . . ? C28 C27 C26 122.3(3) . . ? F7 C28 C29 119.7(2) . . ? F7 C28 C27 120.3(3) . . ? C29 C28 C27 119.9(3) . . ? F8 C29 C28 120.2(3) . . ? F8 C29 C30 120.0(3) . . ? C28 C29 C30 119.8(3) . . ? F9 C30 C29 120.1(3) . . ? F9 C30 C31 120.4(3) . . ? C29 C30 C31 119.5(3) . . ? F10 C31 C30 117.6(2) . . ? F10 C31 C26 119.8(2) . . ? C30 C31 C26 122.6(2) . . ? C33 C32 C37 116.0(2) . . ? C33 C32 C19 122.7(2) . . ? C37 C32 C19 121.4(2) . . ? F11 C33 C34 118.4(3) . . ? F11 C33 C32 119.3(2) . . ? C34 C33 C32 122.3(3) . . ? F12 C34 C35 120.3(3) . . ? F12 C34 C33 120.1(3) . . ? C35 C34 C33 119.6(3) . . ? F13 C35 C36 120.0(3) . . ? F13 C35 C34 120.1(3) . . ? C36 C35 C34 119.9(3) . . ? F14 C36 C35 119.3(3) . . ? F14 C36 C37 121.2(3) . . ? C35 C36 C37 119.4(3) . . ? F15 C37 C36 117.7(3) . . ? F15 C37 C32 119.6(2) . . ? C36 C37 C32 122.8(3) . . ? N5 C38 C39 119.4(2) . . ? N5 C38 C43 119.1(2) . . ? C39 C38 C43 121.5(2) . . ? C40 C39 C38 117.7(2) . . ? C40 C39 C46 122.4(2) . . ? C38 C39 C46 119.9(2) . . ? C39 C40 C41 122.2(2) . . ? C39 C40 H40 118.9 . . ? C41 C40 H40 118.9 . . ? C42 C41 C40 118.4(2) . . ? C42 C41 C45 120.3(2) . . ? C40 C41 C45 121.2(2) . . ? C43 C42 C41 122.5(2) . . ? C43 C42 H42 118.7 . . ? C41 C42 H42 118.7 . . ? C42 C43 C38 117.6(2) . . ? C42 C43 C44 121.8(2) . . ? C38 C43 C44 120.5(2) . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C41 C45 H45A 109.5 . . ? C41 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C41 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C39 C46 H46A 109.5 . . ? C39 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C39 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C2S C1S C6S 121.9(4) . . ? C2S C1S H1S 119.0 . . ? C6S C1S H1S 119.0 . . ? C1S C2S C3S 119.7(4) . . ? C1S C2S H2S 120.1 . . ? C3S C2S H2S 120.1 . . ? C2S C3S C4S 120.1(4) . . ? C2S C3S H3S 119.9 . . ? C4S C3S H3S 119.9 . . ? C5S C4S C3S 119.3(4) . . ? C5S C4S H4S 120.3 . . ? C3S C4S H4S 120.3 . . ? C4S C5S C6S 120.8(3) . . ? C4S C5S H5S 119.6 . . ? C6S C5S H5S 119.6 . . ? C1S C6S C5S 118.1(4) . . ? C1S C6S C7S 121.4(4) . . ? C5S C6S C7S 120.5(3) . . ? C6S C7S H7S1 109.5 . . ? C6S C7S H7S2 109.5 . . ? H7S1 C7S H7S2 109.5 . . ? C6S C7S H7S3 109.5 . . ? H7S1 C7S H7S3 109.5 . . ? H7S2 C7S H7S3 109.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 N5 1.635(2) . ? Cr1 N4 1.932(2) . ? Cr1 N2 1.941(2) . ? Cr1 N3 1.943(2) . ? Cr1 N1 1.955(2) . ? F1 C21 1.339(3) . ? F2 C22 1.333(4) . ? F3 C23 1.347(3) . ? F4 C24 1.335(4) . ? F5 C25 1.334(3) . ? F6 C27 1.341(3) . ? F7 C28 1.340(3) . ? F8 C29 1.341(3) . ? F9 C30 1.344(3) . ? F10 C31 1.347(3) . ? F11 C33 1.335(3) . ? F12 C34 1.342(3) . ? F13 C35 1.337(3) . ? F14 C36 1.341(3) . ? F15 C37 1.340(3) . ? N1 C4 1.382(3) . ? N1 C1 1.394(3) . ? N2 C6 1.390(3) . ? N2 C9 1.400(3) . ? N3 C11 1.369(3) . ? N3 C14 1.375(3) . ? N4 C18 1.375(3) . ? N4 C15 1.378(3) . ? N5 C38 1.368(3) . ? C1 C19 1.400(3) . ? C1 C2 1.435(3) . ? C2 C3 1.354(4) . ? C2 H2 0.9500 . ? C3 C4 1.427(3) . ? C3 H3 0.9500 . ? C4 C5 1.397(3) . ? C5 C6 1.398(3) . ? C5 C20 1.493(3) . ? C6 C7 1.430(3) . ? C7 C8 1.362(3) . ? C7 H7 0.9500 . ? C8 C9 1.425(3) . ? C8 H8 0.9500 . ? C9 C10 1.406(3) . ? C10 C11 1.394(4) . ? C10 C26 1.489(3) . ? C11 C12 1.430(3) . ? C12 C13 1.370(4) . ? C12 H12 0.9500 . ? C13 C14 1.421(4) . ? C13 H13 0.9500 . ? C14 C15 1.415(4) . ? C15 C16 1.415(4) . ? C16 C17 1.375(4) . ? C16 H16 0.9500 . ? C17 C18 1.427(3) . ? C17 H17 0.9500 . ? C18 C19 1.393(3) . ? C19 C32 1.494(3) . ? C20 C25 1.381(4) . ? C20 C21 1.382(4) . ? C21 C22 1.380(4) . ? C22 C23 1.360(5) . ? C23 C24 1.373(5) . ? C24 C25 1.387(4) . ? C26 C27 1.392(4) . ? C26 C31 1.393(4) . ? C27 C28 1.379(4) . ? C28 C29 1.372(4) . ? C29 C30 1.375(4) . ? C30 C31 1.379(4) . ? C32 C33 1.385(4) . ? C32 C37 1.386(4) . ? C33 C34 1.384(4) . ? C34 C35 1.373(4) . ? C35 C36 1.369(4) . ? C36 C37 1.379(4) . ? C38 C39 1.419(3) . ? C38 C43 1.420(3) . ? C39 C40 1.383(3) . ? C39 C46 1.506(3) . ? C40 C41 1.400(4) . ? C40 H40 0.9500 . ? C41 C42 1.394(4) . ? C41 C45 1.499(4) . ? C42 C43 1.380(3) . ? C42 H42 0.9500 . ? C43 C44 1.498(4) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C1S C2S 1.361(6) . ? C1S C6S 1.379(5) . ? C1S H1S 0.9500 . ? C2S C3S 1.371(6) . ? C2S H2S 0.9500 . ? C3S C4S 1.386(5) . ? C3S H3S 0.9500 . ? C4S C5S 1.381(5) . ? C4S H4S 0.9500 . ? C5S C6S 1.384(5) . ? C5S H5S 0.9500 . ? C6S C7S 1.505(5) . ? C7S H7S1 0.9800 . ? C7S H7S2 0.9800 . ? C7S H7S3 0.9800 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5 Cr1 N1 C4 85.3(2) . . . . ? N4 Cr1 N1 C4 -169.1(2) . . . . ? N2 Cr1 N1 C4 -23.9(2) . . . . ? N3 Cr1 N1 C4 -110.0(2) . . . . ? N5 Cr1 N1 C1 -79.0(2) . . . . ? N4 Cr1 N1 C1 26.6(2) . . . . ? N2 Cr1 N1 C1 171.8(2) . . . . ? N3 Cr1 N1 C1 85.7(3) . . . . ? N5 Cr1 N2 C6 -82.9(2) . . . . ? N4 Cr1 N2 C6 112.4(2) . . . . ? N3 Cr1 N2 C6 174.4(2) . . . . ? N1 Cr1 N2 C6 25.7(2) . . . . ? N5 Cr1 N2 C9 76.3(2) . . . . ? N4 Cr1 N2 C9 -88.5(2) . . . . ? N3 Cr1 N2 C9 -26.4(2) . . . . ? N1 Cr1 N2 C9 -175.1(2) . . . . ? N5 Cr1 N3 C11 -83.4(2) . . . . ? N4 Cr1 N3 C11 172.6(2) . . . . ? N2 Cr1 N3 C11 23.5(2) . . . . ? N1 Cr1 N3 C11 111.6(3) . . . . ? N5 Cr1 N3 C14 87.31(19) . . . . ? N4 Cr1 N3 C14 -16.68(18) . . . . ? N2 Cr1 N3 C14 -165.71(19) . . . . ? N1 Cr1 N3 C14 -77.6(2) . . . . ? N5 Cr1 N4 C18 74.8(2) . . . . ? N2 Cr1 N4 C18 -120.4(2) . . . . ? N3 Cr1 N4 C18 175.5(2) . . . . ? N1 Cr1 N4 C18 -31.6(2) . . . . ? N5 Cr1 N4 C15 -81.70(19) . . . . ? N2 Cr1 N4 C15 83.2(2) . . . . ? N3 Cr1 N4 C15 19.02(17) . . . . ? N1 Cr1 N4 C15 171.94(18) . . . . ? N4 Cr1 N5 C38 69.0(10) . . . . ? N2 Cr1 N5 C38 -102.1(10) . . . . ? N3 Cr1 N5 C38 -12.4(10) . . . . ? N1 Cr1 N5 C38 159.5(10) . . . . ? C4 N1 C1 C19 177.6(2) . . . . ? Cr1 N1 C1 C19 -15.8(3) . . . . ? C4 N1 C1 C2 -0.3(3) . . . . ? Cr1 N1 C1 C2 166.29(17) . . . . ? N1 C1 C2 C3 0.4(3) . . . . ? C19 C1 C2 C3 -177.4(3) . . . . ? C1 C2 C3 C4 -0.4(3) . . . . ? C1 N1 C4 C5 -179.0(2) . . . . ? Cr1 N1 C4 C5 14.1(3) . . . . ? C1 N1 C4 C3 0.1(3) . . . . ? Cr1 N1 C4 C3 -166.90(17) . . . . ? C2 C3 C4 N1 0.2(3) . . . . ? C2 C3 C4 C5 179.2(2) . . . . ? N1 C4 C5 C6 2.5(4) . . . . ? C3 C4 C5 C6 -176.4(3) . . . . ? N1 C4 C5 C20 -180.0(2) . . . . ? C3 C4 C5 C20 1.2(4) . . . . ? C9 N2 C6 C5 178.5(2) . . . . ? Cr1 N2 C6 C5 -18.8(3) . . . . ? C9 N2 C6 C7 0.2(3) . . . . ? Cr1 N2 C6 C7 162.91(17) . . . . ? C4 C5 C6 N2 0.2(4) . . . . ? C20 C5 C6 N2 -177.5(2) . . . . ? C4 C5 C6 C7 178.1(2) . . . . ? C20 C5 C6 C7 0.4(4) . . . . ? N2 C6 C7 C8 -0.3(3) . . . . ? C5 C6 C7 C8 -178.5(2) . . . . ? C6 C7 C8 C9 0.3(3) . . . . ? C6 N2 C9 C10 -176.4(2) . . . . ? Cr1 N2 C9 C10 21.7(3) . . . . ? C6 N2 C9 C8 0.0(3) . . . . ? Cr1 N2 C9 C8 -161.87(17) . . . . ? C7 C8 C9 N2 -0.1(3) . . . . ? C7 C8 C9 C10 176.1(2) . . . . ? N2 C9 C10 C11 -0.6(4) . . . . ? C8 C9 C10 C11 -176.3(2) . . . . ? N2 C9 C10 C26 174.5(2) . . . . ? C8 C9 C10 C26 -1.2(4) . . . . ? C14 N3 C11 C10 176.2(2) . . . . ? Cr1 N3 C11 C10 -12.5(4) . . . . ? C14 N3 C11 C12 -0.8(3) . . . . ? Cr1 N3 C11 C12 170.47(18) . . . . ? C9 C10 C11 N3 -4.5(4) . . . . ? C26 C10 C11 N3 -179.4(2) . . . . ? C9 C10 C11 C12 171.6(3) . . . . ? C26 C10 C11 C12 -3.3(4) . . . . ? N3 C11 C12 C13 0.6(3) . . . . ? C10 C11 C12 C13 -175.9(3) . . . . ? C11 C12 C13 C14 -0.1(3) . . . . ? C11 N3 C14 C15 -175.5(2) . . . . ? Cr1 N3 C14 C15 11.6(3) . . . . ? C11 N3 C14 C13 0.8(3) . . . . ? Cr1 N3 C14 C13 -172.17(17) . . . . ? C12 C13 C14 N3 -0.4(3) . . . . ? C12 C13 C14 C15 174.2(3) . . . . ? C18 N4 C15 C16 0.0(3) . . . . ? Cr1 N4 C15 C16 161.43(17) . . . . ? C18 N4 C15 C14 -179.6(2) . . . . ? Cr1 N4 C15 C14 -18.1(3) . . . . ? N3 C14 C15 N4 4.0(3) . . . . ? C13 C14 C15 N4 -170.5(3) . . . . ? N3 C14 C15 C16 -175.4(3) . . . . ? C13 C14 C15 C16 10.2(6) . . . . ? N4 C15 C16 C17 -0.2(3) . . . . ? C14 C15 C16 C17 179.2(3) . . . . ? C15 C16 C17 C18 0.3(3) . . . . ? C15 N4 C18 C19 -178.9(2) . . . . ? Cr1 N4 C18 C19 23.2(4) . . . . ? C15 N4 C18 C17 0.2(3) . . . . ? Cr1 N4 C18 C17 -157.65(18) . . . . ? C16 C17 C18 N4 -0.3(3) . . . . ? C16 C17 C18 C19 178.7(3) . . . . ? N4 C18 C19 C1 1.5(4) . . . . ? C17 C18 C19 C1 -177.4(3) . . . . ? N4 C18 C19 C32 -179.3(2) . . . . ? C17 C18 C19 C32 1.8(4) . . . . ? N1 C1 C19 C18 -4.4(4) . . . . ? C2 C1 C19 C18 173.1(2) . . . . ? N1 C1 C19 C32 176.4(2) . . . . ? C2 C1 C19 C32 -6.1(4) . . . . ? C4 C5 C20 C25 -88.9(3) . . . . ? C6 C5 C20 C25 88.9(3) . . . . ? C4 C5 C20 C21 97.3(3) . . . . ? C6 C5 C20 C21 -84.9(3) . . . . ? C25 C20 C21 F1 179.7(2) . . . . ? C5 C20 C21 F1 -6.2(4) . . . . ? C25 C20 C21 C22 -2.0(4) . . . . ? C5 C20 C21 C22 172.1(3) . . . . ? F1 C21 C22 F2 -2.1(4) . . . . ? C20 C21 C22 F2 179.6(3) . . . . ? F1 C21 C22 C23 178.0(3) . . . . ? C20 C21 C22 C23 -0.2(4) . . . . ? F2 C22 C23 F3 0.6(4) . . . . ? C21 C22 C23 F3 -179.5(3) . . . . ? F2 C22 C23 C24 -177.2(3) . . . . ? C21 C22 C23 C24 2.7(5) . . . . ? F3 C23 C24 F4 -0.6(5) . . . . ? C22 C23 C24 F4 177.2(3) . . . . ? F3 C23 C24 C25 179.5(3) . . . . ? C22 C23 C24 C25 -2.7(5) . . . . ? C21 C20 C25 F5 -179.5(3) . . . . ? C5 C20 C25 F5 6.3(4) . . . . ? C21 C20 C25 C24 2.0(4) . . . . ? C5 C20 C25 C24 -172.2(3) . . . . ? F4 C24 C25 F5 1.9(4) . . . . ? C23 C24 C25 F5 -178.2(3) . . . . ? F4 C24 C25 C20 -179.6(3) . . . . ? C23 C24 C25 C20 0.3(5) . . . . ? C11 C10 C26 C27 67.1(3) . . . . ? C9 C10 C26 C27 -108.1(3) . . . . ? C11 C10 C26 C31 -116.5(3) . . . . ? C9 C10 C26 C31 68.3(3) . . . . ? C31 C26 C27 F6 -179.2(2) . . . . ? C10 C26 C27 F6 -2.6(4) . . . . ? C31 C26 C27 C28 -2.0(4) . . . . ? C10 C26 C27 C28 174.6(2) . . . . ? F6 C27 C28 F7 -1.6(4) . . . . ? C26 C27 C28 F7 -178.8(2) . . . . ? F6 C27 C28 C29 177.7(2) . . . . ? C26 C27 C28 C29 0.5(4) . . . . ? F7 C28 C29 F8 -0.2(4) . . . . ? C27 C28 C29 F8 -179.4(2) . . . . ? F7 C28 C29 C30 -179.5(2) . . . . ? C27 C28 C29 C30 1.2(4) . . . . ? F8 C29 C30 F9 -0.1(4) . . . . ? C28 C29 C30 F9 179.3(2) . . . . ? F8 C29 C30 C31 179.4(2) . . . . ? C28 C29 C30 C31 -1.2(4) . . . . ? F9 C30 C31 F10 -0.3(4) . . . . ? C29 C30 C31 F10 -179.8(2) . . . . ? F9 C30 C31 C26 179.1(2) . . . . ? C29 C30 C31 C26 -0.5(4) . . . . ? C27 C26 C31 F10 -178.7(2) . . . . ? C10 C26 C31 F10 4.7(4) . . . . ? C27 C26 C31 C30 2.0(4) . . . . ? C10 C26 C31 C30 -174.6(2) . . . . ? C18 C19 C32 C33 -80.5(3) . . . . ? C1 C19 C32 C33 98.7(3) . . . . ? C18 C19 C32 C37 98.7(3) . . . . ? C1 C19 C32 C37 -82.1(3) . . . . ? C37 C32 C33 F11 -179.7(2) . . . . ? C19 C32 C33 F11 -0.5(4) . . . . ? C37 C32 C33 C34 0.3(4) . . . . ? C19 C32 C33 C34 179.5(3) . . . . ? F11 C33 C34 F12 -1.3(4) . . . . ? C32 C33 C34 F12 178.8(2) . . . . ? F11 C33 C34 C35 179.3(3) . . . . ? C32 C33 C34 C35 -0.7(4) . . . . ? F12 C34 C35 F13 -0.5(4) . . . . ? C33 C34 C35 F13 178.9(3) . . . . ? F12 C34 C35 C36 -179.3(3) . . . . ? C33 C34 C35 C36 0.1(4) . . . . ? F13 C35 C36 F14 0.3(4) . . . . ? C34 C35 C36 F14 179.1(3) . . . . ? F13 C35 C36 C37 -178.0(3) . . . . ? C34 C35 C36 C37 0.8(5) . . . . ? F14 C36 C37 F15 1.3(4) . . . . ? C35 C36 C37 F15 179.6(3) . . . . ? F14 C36 C37 C32 -179.5(3) . . . . ? C35 C36 C37 C32 -1.2(4) . . . . ? C33 C32 C37 F15 179.9(2) . . . . ? C19 C32 C37 F15 0.7(4) . . . . ? C33 C32 C37 C36 0.7(4) . . . . ? C19 C32 C37 C36 -178.5(3) . . . . ? Cr1 N5 C38 C39 95.8(10) . . . . ? Cr1 N5 C38 C43 -81.1(10) . . . . ? N5 C38 C39 C40 -173.1(2) . . . . ? C43 C38 C39 C40 3.7(3) . . . . ? N5 C38 C39 C46 5.9(3) . . . . ? C43 C38 C39 C46 -177.3(2) . . . . ? C38 C39 C40 C41 -1.7(4) . . . . ? C46 C39 C40 C41 179.3(2) . . . . ? C39 C40 C41 C42 -1.5(4) . . . . ? C39 C40 C41 C45 178.3(2) . . . . ? C40 C41 C42 C43 3.0(4) . . . . ? C45 C41 C42 C43 -176.8(2) . . . . ? C41 C42 C43 C38 -1.1(4) . . . . ? C41 C42 C43 C44 177.5(2) . . . . ? N5 C38 C43 C42 174.5(2) . . . . ? C39 C38 C43 C42 -2.3(3) . . . . ? N5 C38 C43 C44 -4.2(3) . . . . ? C39 C38 C43 C44 179.0(2) . . . . ? C6S C1S C2S C3S 0.4(5) . . . . ? C1S C2S C3S C4S 0.0(5) . . . . ? C2S C3S C4S C5S 0.1(5) . . . . ? C3S C4S C5S C6S -0.7(5) . . . . ? C2S C1S C6S C5S -0.9(5) . . . . ? C2S C1S C6S C7S 176.5(3) . . . . ? C4S C5S C6S C1S 1.0(5) . . . . ? C4S C5S C6S C7S -176.4(3) . . . . ?
1100774.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100774.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100774 loop_ _publ_author_name 'Qiong Ye' 'Yong-Hua Li' 'Yu-Mei Song' 'Xue-Feng Huang' 'Ren-Gen Xiong' 'Ziling Xue' _publ_section_title ; A Second-Order Nonlinear Optical Material Prepared through In Situ Hydrothermal Ligand Synthesis ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3618 _journal_page_last 3625 _journal_paper_doi 10.1021/ic0500098 _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C14 H10 N8 Zn' _chemical_formula_weight 355.67 _chemical_name_systematic ; ? ; _space_group_IT_number 122 _symmetry_cell_setting tetragonal _symmetry_space_group_name_Hall 'I -4 2bw' _symmetry_space_group_name_H-M 'I -4 2 d' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 16 _cell_length_a 14.2430(18) _cell_length_b 14.2430(18) _cell_length_c 28.419(5) _cell_measurement_temperature 293(2) _cell_volume 5765.2(14) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.973 _diffrn_measured_fraction_theta_max 0.973 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0464 _diffrn_reflns_av_sigmaI/netI 0.0297 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_number 15888 _diffrn_reflns_theta_full 28.32 _diffrn_reflns_theta_max 28.32 _diffrn_reflns_theta_min 2.48 _exptl_absorpt_coefficient_mu 1.716 _exptl_absorpt_correction_type none _exptl_crystal_density_diffrn 1.639 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2880 _refine_diff_density_max 0.410 _refine_diff_density_min -0.265 _refine_diff_density_rms 0.055 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.08(3) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 208 _refine_ls_number_reflns 3415 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.033 _refine_ls_R_factor_all 0.0450 _refine_ls_R_factor_gt 0.0317 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0515P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0894 _refine_ls_wR_factor_ref 0.0929 _reflns_number_gt 2513 _reflns_number_total 3415 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic0500098si20050104_032035_1.cif _cod_data_source_block 1 _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_cell_volume 5765.2(15) _cod_database_code 1100774 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x+1/2, y, -z+3/4' 'x+1/2, -y, -z+3/4' '-y+1/2, -x, z+3/4' 'y+1/2, x, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' '-x+1, y+1/2, -z+5/4' 'x+1, -y+1/2, -z+5/4' '-y+1, -x+1/2, z+5/4' 'y+1, x+1/2, z+5/4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn2 Zn 0.25038(2) 0.2500 0.1250 0.02622(14) Uani 1 2 d S . . Zn3 Zn 0.5000 0.5000 0.0000 0.02749(16) Uani 1 4 d S . . N4 N 0.41348(16) 0.43010(17) 0.04266(9) 0.0383(6) Uani 1 1 d . . . N3 N 0.32705(16) 0.33840(16) 0.08521(9) 0.0344(6) Uani 1 1 d . . . N2 N 0.17533(15) 0.16799(16) 0.08187(8) 0.0293(5) Uani 1 1 d . . . C3 C 0.40835(17) 0.34646(18) 0.06315(9) 0.0324(5) Uani 1 1 d . . . C2 C 0.48292(18) 0.27554(19) 0.06148(9) 0.0374(6) Uani 1 1 d . . . N7 N 0.17005(15) 0.09590(17) 0.01558(7) 0.0422(6) Uani 1 1 d . . . N8 N 0.22272(14) 0.14887(17) 0.04122(7) 0.0424(6) Uani 1 1 d . . . C8 C 0.09260(17) 0.12584(17) 0.07877(8) 0.0264(5) Uani 1 1 d . . . N9 N 0.08752(14) 0.08041(16) 0.03746(9) 0.0302(5) Uani 1 1 d . . . Zn1 Zn 0.0000 0.0000 0.0000 0.02384(15) Uani 1 4 d S . . N1 N 0.28084(15) 0.42141(16) 0.07848(9) 0.0441(6) Uani 1 1 d . . . C12 C -0.14382(19) 0.1220(2) 0.13573(11) 0.0466(7) Uani 1 1 d . . . H12A H -0.2065 0.1189 0.1267 0.056 Uiso 1 1 calc R . . C11 C 0.01854(16) 0.12574(16) 0.11459(8) 0.0280(5) Uani 1 1 d . . . N6 N 0.33212(16) 0.47536(16) 0.05323(8) 0.0446(6) Uani 1 1 d . . . C10 C -0.07514(18) 0.12560(18) 0.10198(8) 0.0375(6) Uani 1 1 d . . . H10A H -0.0917 0.1280 0.0704 0.045 Uiso 1 1 calc R . . C9 C 0.04235(18) 0.12592(18) 0.16223(8) 0.0369(6) Uani 1 1 d . . . H9A H 0.1050 0.1267 0.1714 0.044 Uiso 1 1 calc R . . C13 C -0.1211(2) 0.1228(3) 0.18290(13) 0.0459(7) Uani 1 1 d . . . H13A H -0.1681 0.1219 0.2056 0.055 Uiso 1 1 calc R . . C14 C -0.02845(19) 0.1249(2) 0.19582(9) 0.0445(7) Uani 1 1 d . . . H14A H -0.0127 0.1257 0.2276 0.053 Uiso 1 1 calc R . . C1 C 0.5773(2) 0.3015(2) 0.06255(11) 0.0520(8) Uani 1 1 d . . . H1B H 0.5929 0.3645 0.0661 0.062 Uiso 1 1 calc R . . C7 C 0.6460(2) 0.2377(3) 0.05863(12) 0.0665(10) Uani 1 1 d . . . H7B H 0.7083 0.2572 0.0596 0.080 Uiso 1 1 calc R . . C6 C 0.4631(2) 0.1830(2) 0.05641(17) 0.0875(14) Uani 1 1 d . . . H6B H 0.4010 0.1626 0.0558 0.105 Uiso 1 1 calc R . . C5 C 0.6265(3) 0.1463(4) 0.0533(2) 0.110(2) Uani 1 1 d . . . H5A H 0.6741 0.1020 0.0505 0.132 Uiso 1 1 calc R . . C4 C 0.5340(3) 0.1205(3) 0.0522(3) 0.187(4) Uani 1 1 d . . . H4A H 0.5193 0.0573 0.0484 0.224 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn2 0.0256(2) 0.0289(2) 0.0241(3) -0.00289(15) 0.000 0.000 Zn3 0.0261(2) 0.0261(2) 0.0302(4) 0.000 0.000 0.000 N4 0.0307(12) 0.0403(13) 0.0440(16) 0.0105(12) 0.0010(12) -0.0036(12) N3 0.0312(12) 0.0358(12) 0.0362(14) 0.0039(11) 0.0069(10) -0.0008(12) N2 0.0265(11) 0.0387(12) 0.0228(12) -0.0073(10) -0.0012(9) -0.0010(11) C3 0.0302(15) 0.0381(15) 0.0290(12) 0.0020(12) -0.0002(11) -0.0027(11) C2 0.0355(14) 0.0461(16) 0.0307(13) -0.0022(13) 0.0014(12) 0.0016(12) N7 0.0353(12) 0.0626(15) 0.0286(11) -0.0160(11) 0.0032(9) -0.0099(11) N8 0.0331(12) 0.0632(15) 0.0310(12) -0.0106(11) 0.0039(10) -0.0081(11) C8 0.0256(12) 0.0274(12) 0.0263(12) -0.0014(10) -0.0057(10) 0.0045(10) N9 0.0272(11) 0.0380(12) 0.0254(12) -0.0046(10) 0.0014(10) -0.0020(11) Zn1 0.0257(2) 0.0257(2) 0.0202(3) 0.000 0.000 0.000 N1 0.0329(12) 0.0406(13) 0.0588(16) 0.0064(12) 0.0086(11) 0.0012(11) C12 0.0315(14) 0.0614(19) 0.0469(18) 0.0005(15) 0.0020(12) 0.0028(14) C11 0.0333(13) 0.0264(12) 0.0242(12) -0.0027(10) 0.0015(10) -0.0008(10) N6 0.0331(13) 0.0424(13) 0.0582(16) 0.0114(12) 0.0056(11) 0.0017(11) C10 0.0365(14) 0.0473(16) 0.0285(13) -0.0041(12) -0.0036(11) 0.0067(12) C9 0.0350(14) 0.0444(16) 0.0312(14) 0.0000(12) -0.0017(11) -0.0044(11) C13 0.0393(15) 0.0600(17) 0.0385(16) 0.0078(14) 0.0125(12) 0.0086(13) C14 0.0517(17) 0.0595(18) 0.0225(12) 0.0013(13) 0.0027(12) 0.0037(14) C1 0.0335(15) 0.0580(18) 0.065(2) 0.0134(16) -0.0050(14) -0.0012(14) C7 0.0348(17) 0.091(3) 0.074(2) -0.005(2) -0.0061(16) 0.0074(18) C6 0.0437(19) 0.056(2) 0.162(4) -0.047(3) -0.007(2) 0.0031(16) C5 0.047(2) 0.092(4) 0.192(6) -0.077(4) -0.018(3) 0.028(2) C4 0.055(3) 0.069(3) 0.438(11) -0.129(5) -0.022(4) 0.014(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Zn2 N2 115.47(11) . 14_454 ? N2 Zn2 N3 108.08(12) . . ? N2 Zn2 N3 105.58(9) 14_454 . ? N2 Zn2 N3 105.58(9) . 14_454 ? N2 Zn2 N3 108.08(12) 14_454 14_454 ? N3 Zn2 N3 114.33(12) . 14_454 ? N4 Zn3 N4 111.68(8) 2_665 3_565 ? N4 Zn3 N4 111.68(8) 2_665 4_655 ? N4 Zn3 N4 105.15(15) 3_565 4_655 ? N4 Zn3 N4 105.15(15) 2_665 . ? N4 Zn3 N4 111.68(8) 3_565 . ? N4 Zn3 N4 111.68(8) 4_655 . ? C3 N4 N6 106.4(2) . . ? C3 N4 Zn3 138.42(18) . . ? N6 N4 Zn3 115.10(18) . . ? C3 N3 N1 106.3(2) . . ? C3 N3 Zn2 142.71(18) . . ? N1 N3 Zn2 110.99(17) . . ? C8 N2 N8 107.0(2) . . ? C8 N2 Zn2 141.21(18) . . ? N8 N2 Zn2 111.74(17) . . ? N3 C3 N4 109.5(2) . . ? N3 C3 C2 126.2(2) . . ? N4 C3 C2 124.3(2) . . ? C6 C2 C1 117.4(3) . . ? C6 C2 C3 121.5(3) . . ? C1 C2 C3 121.0(2) . . ? N8 N7 N9 110.0(2) . . ? N7 N8 N2 107.9(2) . . ? N2 C8 N9 108.9(2) . . ? N2 C8 C11 126.5(2) . . ? N9 C8 C11 124.6(2) . . ? C8 N9 N7 106.1(2) . . ? C8 N9 Zn1 140.83(18) . . ? N7 N9 Zn1 113.06(18) . . ? N9 Zn1 N9 106.46(6) . 4 ? N9 Zn1 N9 106.46(6) . 3 ? N9 Zn1 N9 115.67(14) 4 3 ? N9 Zn1 N9 115.67(14) . 2 ? N9 Zn1 N9 106.46(6) 4 2 ? N9 Zn1 N9 106.46(6) 3 2 ? N6 N1 N3 108.8(2) . . ? C13 C12 C10 120.8(3) . . ? C13 C12 H12A 119.6 . . ? C10 C12 H12A 119.6 . . ? C9 C11 C10 119.1(2) . . ? C9 C11 C8 119.9(2) . . ? C10 C11 C8 121.0(2) . . ? N1 N6 N4 109.0(2) . . ? C12 C10 C11 120.5(2) . . ? C12 C10 H10A 119.7 . . ? C11 C10 H10A 119.7 . . ? C14 C9 C11 119.4(2) . . ? C14 C9 H9A 120.3 . . ? C11 C9 H9A 120.3 . . ? C14 C13 C12 119.1(3) . . ? C14 C13 H13A 120.5 . . ? C12 C13 H13A 120.5 . . ? C13 C14 C9 121.0(3) . . ? C13 C14 H14A 119.5 . . ? C9 C14 H14A 119.5 . . ? C7 C1 C2 121.5(3) . . ? C7 C1 H1B 119.2 . . ? C2 C1 H1B 119.2 . . ? C5 C7 C1 121.1(3) . . ? C5 C7 H7B 119.4 . . ? C1 C7 H7B 119.4 . . ? C2 C6 C4 119.6(3) . . ? C2 C6 H6B 120.2 . . ? C4 C6 H6B 120.2 . . ? C7 C5 C4 117.6(3) . . ? C7 C5 H5A 121.2 . . ? C4 C5 H5A 121.2 . . ? C6 C4 C5 122.7(4) . . ? C6 C4 H4A 118.6 . . ? C5 C4 H4A 118.6 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn2 N2 2.002(3) . ? Zn2 N2 2.002(3) 14_454 ? Zn2 N3 2.014(3) . ? Zn2 N3 2.014(3) 14_454 ? Zn3 N4 1.995(3) 2_665 ? Zn3 N4 1.995(3) 3_565 ? Zn3 N4 1.995(3) 4_655 ? Zn3 N4 1.995(3) . ? N4 C3 1.328(4) . ? N4 N6 1.360(3) . ? N3 C3 1.322(3) . ? N3 N1 1.367(3) . ? N2 C8 1.325(3) . ? N2 N8 1.365(3) . ? C3 C2 1.466(3) . ? C2 C6 1.356(4) . ? C2 C1 1.394(4) . ? N7 N8 1.290(3) . ? N7 N9 1.348(3) . ? C8 N9 1.343(3) . ? C8 C11 1.466(3) . ? N9 Zn1 2.000(3) . ? Zn1 N9 2.000(3) 4 ? Zn1 N9 2.000(3) 3 ? Zn1 N9 2.000(3) 2 ? N1 N6 1.280(3) . ? C12 C13 1.379(5) . ? C12 C10 1.371(4) . ? C12 H12A 0.9300 . ? C11 C9 1.396(3) . ? C11 C10 1.382(3) . ? C10 H10A 0.9300 . ? C9 C14 1.389(3) . ? C9 H9A 0.9300 . ? C13 C14 1.370(4) . ? C13 H13A 0.9300 . ? C14 H14A 0.9300 . ? C1 C7 1.340(4) . ? C1 H1B 0.9300 . ? C7 C5 1.339(6) . ? C7 H7B 0.9300 . ? C6 C4 1.352(5) . ? C6 H6B 0.9300 . ? C5 C4 1.368(6) . ? C5 H5A 0.9300 . ? C4 H4A 0.9300 . ?
1100775.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100775.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100775 loop_ _publ_author_name 'Qiong Ye' 'Yong-Hua Li' 'Yu-Mei Song' 'Xue-Feng Huang' 'Ren-Gen Xiong' 'Ziling Xue' _publ_section_title ; A Second-Order Nonlinear Optical Material Prepared through In Situ Hydrothermal Ligand Synthesis ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3618 _journal_page_last 3625 _journal_paper_doi 10.1021/ic0500098 _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C12 H10 Cl0 N12 Zn' _chemical_formula_weight 387.69 _chemical_name_systematic ; ? ; _space_group_IT_number 122 _symmetry_cell_setting tetragonal _symmetry_space_group_name_Hall 'I -4 2bw' _symmetry_space_group_name_H-M 'I -4 2 d' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 10.4850(16) _cell_length_b 10.4850(16) _cell_length_c 13.088(3) _cell_measurement_temperature 293(2) _cell_volume 1438.8(5) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0543 _diffrn_reflns_av_sigmaI/netI 0.0459 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 4184 _diffrn_reflns_theta_full 28.18 _diffrn_reflns_theta_max 28.18 _diffrn_reflns_theta_min 2.49 _exptl_absorpt_coefficient_mu 1.735 _exptl_absorpt_correction_type none _exptl_crystal_density_diffrn 1.790 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _refine_diff_density_max 0.832 _refine_diff_density_min -0.587 _refine_diff_density_rms 0.107 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(5) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 67 _refine_ls_number_reflns 878 _refine_ls_number_restraints 45 _refine_ls_restrained_S_all 1.179 _refine_ls_R_factor_all 0.0502 _refine_ls_R_factor_gt 0.0449 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0709P)^2^+1.8741P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1179 _refine_ls_wR_factor_ref 0.1196 _reflns_number_gt 809 _reflns_number_total 878 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic0500098si20050104_032035_2.cif _cod_data_source_block 2 _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_cell_volume 1438.9(4) _cod_database_code 1100775 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x+1/2, y, -z+3/4' 'x+1/2, -y, -z+3/4' '-y+1/2, -x, z+3/4' 'y+1/2, x, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' '-x+1, y+1/2, -z+5/4' 'x+1, -y+1/2, -z+5/4' '-y+1, -x+1/2, z+5/4' 'y+1, x+1/2, z+5/4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.5000 0.5000 0.0000 0.01824(12) Uani 1 4 d S . . N1 N 0.4725(2) 0.3428(2) 0.08684(18) 0.0226(6) Uani 1 1 d . . . N2 N 0.3500(2) 0.3041(2) 0.1031(2) 0.0262(6) Uani 1 1 d . . . C1 C 0.5481(4) 0.2500 0.1250 0.0227(9) Uani 1 2 d S . . C2 C 0.6864(4) 0.2500 0.1250 0.0281(10) Uani 1 2 d SDU . . C3 C 0.7521(3) 0.1363(4) 0.1133(3) 0.0494(9) Uani 1 1 d DU . . H3A H 0.7001 0.0616 0.1051 0.059 Uiso 1 1 d R . . C4 C 0.8807(4) 0.1313(5) 0.1130(4) 0.0815(12) Uani 0.50 1 d PDU . . H4A H 0.9174 0.0489 0.1006 0.098 Uiso 0.50 1 d PR . . N3 N 0.8807(4) 0.1313(5) 0.1130(4) 0.0815(12) Uani 0.50 1 d PU . . C5 C 0.9437(6) 0.2417(9) 0.1317(13) 0.0781(17) Uani 0.50 1 d PDU . . N4 N 1.0692(5) 0.1792(7) 0.1233(6) 0.0514(17) Uani 0.50 1 d PU . . H4B H 1.0954 0.0987 0.1119 0.062 Uiso 0.50 1 d PR . . H4C H 1.1269 0.2414 0.1338 0.062 Uiso 0.50 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.01614(14) 0.01614(14) 0.0224(2) 0.000 0.000 0.000 N1 0.0222(15) 0.0200(10) 0.0255(10) 0.0051(9) 0.0014(8) -0.0009(8) N2 0.0189(11) 0.0288(12) 0.0309(13) 0.0074(10) 0.0017(10) 0.0051(10) C1 0.0177(15) 0.034(2) 0.0170(16) -0.0006(18) 0.000 0.000 C2 0.0186(17) 0.039(2) 0.0269(18) 0.0133(19) 0.000 0.000 C3 0.0372(15) 0.070(2) 0.0413(17) 0.0121(17) 0.0092(16) 0.0259(17) C4 0.0592(18) 0.132(3) 0.053(2) 0.012(2) 0.0123(18) 0.048(2) N3 0.0592(18) 0.132(3) 0.053(2) 0.012(2) 0.0123(18) 0.048(2) C5 0.038(2) 0.151(4) 0.045(3) -0.002(3) 0.012(4) 0.031(4) N4 0.013(2) 0.087(4) 0.054(3) -0.018(4) 0.000(3) 0.028(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Zn1 N1 108.40(7) 2_665 4_655 ? N1 Zn1 N1 108.40(7) 2_665 3_565 ? N1 Zn1 N1 111.64(14) 4_655 3_565 ? N1 Zn1 N1 111.64(14) 2_665 . ? N1 Zn1 N1 108.40(7) 4_655 . ? N1 Zn1 N1 108.40(7) 3_565 . ? C1 N1 N2 106.3(2) . . ? C1 N1 Zn1 135.29(19) . . ? N2 N1 Zn1 117.69(18) . . ? N2 N2 N1 109.64(15) 14_454 . ? N1 C1 N1 108.1(3) 14_454 . ? N1 C1 C2 125.95(16) 14_454 . ? N1 C1 C2 125.95(16) . . ? C3 C2 C3 120.4(4) 14_454 . ? C3 C2 C1 119.8(2) 14_454 . ? C3 C2 C1 119.8(2) . . ? C4 C3 C2 122.0(4) . . ? C4 C3 H3A 122.4 . . ? C2 C3 H3A 115.6 . . ? C3 C4 C5 117.0(5) . . ? C3 C4 C5 114.1(5) . 14_454 ? C5 C4 C5 8.4(13) . 14_454 ? C3 C4 H4A 115.8 . . ? C5 C4 H4A 127.2 . . ? C5 C4 H4A 129.5 14_454 . ? C5 C5 C4 118(5) 14_454 . ? C5 C5 N4 105(3) 14_454 . ? C4 C5 N4 92.4(6) . . ? C5 C5 C4 53(4) 14_454 14_454 ? C4 C5 C4 123.8(6) . 14_454 ? N4 C5 C4 142.9(7) . 14_454 ? C5 C5 N3 53(4) 14_454 14_454 ? C4 C5 N3 123.8(6) . 14_454 ? N4 C5 N3 142.9(7) . 14_454 ? C4 C5 N3 0.0(5) 14_454 14_454 ? C5 C5 N4 66(2) 14_454 14_454 ? C4 C5 N4 149.3(8) . 14_454 ? N4 C5 N4 58.6(6) . 14_454 ? C4 C5 N4 84.3(5) 14_454 14_454 ? N3 C5 N4 84.3(5) 14_454 14_454 ? C5 N4 N4 63.5(4) . 14_454 ? C5 N4 C5 8.8(11) . 14_454 ? N4 N4 C5 57.9(4) 14_454 14_454 ? C5 N4 H4B 134.6 . . ? N4 N4 H4B 160.4 14_454 . ? C5 N4 H4B 138.6 14_454 . ? C5 N4 H4C 105.4 . . ? N4 N4 H4C 43.2 14_454 . ? C5 N4 H4C 100.8 14_454 . ? H4B N4 H4C 120.0 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N1 2.023(2) 2_665 ? Zn1 N1 2.023(2) 4_655 ? Zn1 N1 2.023(2) 3_565 ? Zn1 N1 2.023(2) . ? N1 C1 1.351(3) . ? N1 N2 1.363(3) . ? N2 N2 1.271(5) 14_454 ? C1 N1 1.351(3) 14_454 ? C1 C2 1.450(6) . ? C2 C3 1.386(4) 14_454 ? C2 C3 1.386(4) . ? C3 C4 1.350(5) . ? C3 H3A 0.9600 . ? C4 C5 1.355(8) . ? C4 C5 1.488(11) 14_454 ? C4 H4A 0.9600 . ? C5 C5 0.25(3) 14_454 ? C5 N4 1.474(9) . ? C5 C4 1.488(11) 14_454 ? C5 N3 1.488(11) 14_454 ? C5 N4 1.557(9) 14_454 ? N4 N4 1.485(16) 14_454 ? N4 C5 1.557(9) 14_454 ? N4 H4B 0.9000 . ? N4 H4C 0.9000 . ?
1100776.cif	#------------------------------------------------------------------------------ #$Date: 2017-02-19 20:20:29 +0200 (Sun, 19 Feb 2017) $ #$Revision: 192294 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/10/07/1100776.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100776 loop_ _publ_author_name 'Robert J. Wright' 'Marcin Brynda' 'Philip P. Power' _publ_section_title ; A Monomeric Thallium(I) Amide in the Solid State: Synthesis and Structure of TlN(Me)Ar^Mes~2~^ (Ar^Mes~2~^= C~6~H~3~-2,6-Mes~2~) ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3368 _journal_page_last 3370 _journal_paper_doi 10.1021/ic0500255 _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C25.75 H30 N O0.25 Tl' _chemical_formula_weight 561.88 _chemical_name_common J*N(Me)Tl _chemical_name_systematic ? _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 110.8800(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 14.0469(8) _cell_length_b 23.9451(13) _cell_length_c 14.2106(8) _cell_measurement_reflns_used 13010 _cell_measurement_temperature 90(2) _cell_measurement_theta_max 31.354 _cell_measurement_theta_min 2.301 _cell_volume 4465.9(4) _computing_cell_refinement 'SAINT (7.06a) (Bruker, 2004)' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'SAINT (7.06a) (Bruker, 2004)' _computing_molecular_graphics 'SHELXTL 5.1, XP (Sheldrick, 1994)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 90(2) _diffrn_detector_area_resol_mean 8.3 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method '\w and \f' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0523 _diffrn_reflns_av_sigmaI/netI 0.0458 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 57024 _diffrn_reflns_theta_full 30.00 _diffrn_reflns_theta_max 30.00 _diffrn_reflns_theta_min 1.70 _diffrn_standards_number '50 frames remeasured' _exptl_absorpt_coefficient_mu 7.245 _exptl_absorpt_correction_T_max 0.3182 _exptl_absorpt_correction_T_min 0.1386 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS 2.10 (Sheldrick, 2003) ' _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.671 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 2196 _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.20 _refine_diff_density_max 1.663 _refine_diff_density_min -1.129 _refine_diff_density_rms 0.167 _refine_ls_extinction_coef 0.00001 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 528 _refine_ls_number_reflns 13010 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.034 _refine_ls_R_factor_all 0.0566 _refine_ls_R_factor_gt 0.0301 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0344P)^2^+0.7610P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0663 _refine_ls_wR_factor_ref 0.0728 _reflns_number_gt 9882 _reflns_number_total 13010 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic0500255si20050107_043931.cif _cod_data_source_block rjw47ff _cod_depositor_comments ; Marking atoms 'CNT1' and 'CNT2' as dummy atoms. Antanas Vaitkus, 2017-02-19 ; _cod_original_sg_symbol_H-M 'P 21/c' _cod_original_formula_sum 'C51.50 H60 N2 O0.50 Tl2' _cod_database_code 1100776 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tl1 Tl 0.141281(11) 0.722416(6) 0.517335(10) 0.01816(4) Uani 1 1 d . . . Tl2 Tl 0.680816(12) 0.793696(6) 0.103287(11) 0.01983(4) Uani 1 1 d . . . N1 N 0.0693(3) 0.78415(12) 0.3822(2) 0.0174(6) Uani 1 1 d . . . C1 C 0.0378(3) 0.77764(14) 0.2807(3) 0.0142(7) Uani 1 1 d . . . N2 N 0.6017(2) 0.72351(12) 0.1687(2) 0.0158(6) Uani 1 1 d . . . C2 C 0.0212(3) 0.82232(14) 0.2084(3) 0.0154(7) Uani 1 1 d . . . C3 C -0.0318(3) 0.81090(16) 0.1062(3) 0.0187(7) Uani 1 1 d . . . H3 H -0.0484 0.8411 0.0597 0.022 Uiso 1 1 calc R . . C4 C -0.0610(3) 0.75731(17) 0.0702(3) 0.0218(8) Uani 1 1 d . . . H4 H -0.0997 0.7511 0.0011 0.026 Uiso 1 1 calc R . . C5 C -0.0320(3) 0.71280(15) 0.1380(3) 0.0196(8) Uani 1 1 d . . . H5 H -0.0464 0.6756 0.1140 0.024 Uiso 1 1 calc R . . C6 C 0.0176(3) 0.72250(14) 0.2399(3) 0.0140(7) Uani 1 1 d . . . C7 C 0.0672(3) 0.87958(15) 0.2352(3) 0.0167(7) Uani 1 1 d . . . C8 C 0.1737(3) 0.88565(15) 0.2793(3) 0.0166(7) Uani 1 1 d . . . C9 C 0.2152(3) 0.93886(16) 0.3042(3) 0.0212(8) Uani 1 1 d . . . H9 H 0.2872 0.9427 0.3327 0.025 Uiso 1 1 calc R . . C10 C 0.1557(3) 0.98626(15) 0.2892(3) 0.0219(8) Uani 1 1 d . . . C11 C 0.0507(3) 0.97977(15) 0.2443(3) 0.0208(8) Uani 1 1 d . . . H11 H 0.0085 1.0120 0.2318 0.025 Uiso 1 1 calc R . . C12 C 0.0054(3) 0.92745(15) 0.2170(3) 0.0187(7) Uani 1 1 d . . . CNT1 . 0.07480(12) 0.62731(6) 0.37474(11) . . . . dum . . . C13 C 0.0474(3) 0.67339(14) 0.3091(3) 0.0149(7) Uani 1 1 d . . . C14 C 0.1436(3) 0.64827(15) 0.3319(3) 0.0189(7) Uani 1 1 d . . . C15 C 0.1698(3) 0.60303(15) 0.3990(3) 0.0204(8) Uani 1 1 d . . . H15 H 0.2351 0.5864 0.4152 0.024 Uiso 1 1 calc R . . C16 C 0.1029(3) 0.58200(15) 0.4422(3) 0.0207(8) Uani 1 1 d . . . C17 C 0.0072(3) 0.60587(15) 0.4157(3) 0.0199(8) Uani 1 1 d . . . H17 H -0.0400 0.5908 0.4429 0.024 Uiso 1 1 calc R . . C18 C -0.0221(3) 0.65128(14) 0.3506(3) 0.0159(7) Uani 1 1 d . . . C19 C 0.2442(3) 0.83613(15) 0.3019(3) 0.0188(8) Uani 1 1 d . . . H19A H 0.3143 0.8490 0.3168 0.028 Uiso 1 1 calc R . . H19B H 0.2244 0.8112 0.2435 0.028 Uiso 1 1 calc R . . H19C H 0.2398 0.8160 0.3603 0.028 Uiso 1 1 calc R . . C20 C 0.2022(4) 1.04350(17) 0.3190(3) 0.0315(10) Uani 1 1 d . . . H20A H 0.2741 1.0396 0.3617 0.047 Uiso 1 1 calc R . . H20B H 0.1657 1.0633 0.3561 0.047 Uiso 1 1 calc R . . H20C H 0.1970 1.0647 0.2583 0.047 Uiso 1 1 calc R . . C21 C -0.1090(3) 0.92339(16) 0.1730(3) 0.0246(9) Uani 1 1 d . . . H21A H -0.1389 0.9593 0.1807 0.037 Uiso 1 1 calc R . . H21B H -0.1321 0.8943 0.2084 0.037 Uiso 1 1 calc R . . H21C H -0.1304 0.9139 0.1014 0.037 Uiso 1 1 calc R . . C22 C 0.2188(3) 0.66950(18) 0.2862(3) 0.0292(9) Uani 1 1 d . . . H22A H 0.2433 0.7065 0.3136 0.044 Uiso 1 1 calc R . . H22B H 0.1853 0.6721 0.2129 0.044 Uiso 1 1 calc R . . H22C H 0.2765 0.6437 0.3024 0.044 Uiso 1 1 calc R . . C23 C 0.1347(4) 0.53435(17) 0.5171(3) 0.0308(10) Uani 1 1 d . . . H23A H 0.1261 0.5456 0.5800 0.046 Uiso 1 1 calc R . . H23B H 0.2063 0.5251 0.5307 0.046 Uiso 1 1 calc R . . H23C H 0.0921 0.5016 0.4892 0.046 Uiso 1 1 calc R . . C24 C -0.1259(3) 0.67812(15) 0.3241(3) 0.0198(8) Uani 1 1 d . . . H24A H -0.1667 0.6702 0.2535 0.030 Uiso 1 1 calc R . . H24B H -0.1179 0.7186 0.3340 0.030 Uiso 1 1 calc R . . H24C H -0.1603 0.6629 0.3675 0.030 Uiso 1 1 calc R . . C25 C 0.0618(3) 0.83868(15) 0.4236(3) 0.0206(8) Uani 1 1 d . . . H25A H 0.1187 0.8621 0.4229 0.031 Uiso 1 1 calc R . . H25B H 0.0644 0.8344 0.4931 0.031 Uiso 1 1 calc R . . H25C H -0.0027 0.8563 0.3829 0.031 Uiso 1 1 calc R . . C26 C 0.5620(3) 0.72409(14) 0.2430(3) 0.0130(6) Uani 1 1 d . . . C27 C 0.5530(3) 0.77759(14) 0.2861(3) 0.0132(7) Uani 1 1 d . . . C28 C 0.5197(3) 0.78234(14) 0.3663(3) 0.0167(7) Uani 1 1 d . . . H28 H 0.5162 0.8183 0.3932 0.020 Uiso 1 1 calc R . . C29 C 0.4913(3) 0.73601(15) 0.4087(3) 0.0188(7) Uani 1 1 d . . . H29 H 0.4710 0.7395 0.4655 0.023 Uiso 1 1 calc R . . C30 C 0.4936(3) 0.68412(15) 0.3651(3) 0.0163(7) Uani 1 1 d . . . H30 H 0.4726 0.6522 0.3924 0.020 Uiso 1 1 calc R . . C31 C 0.5249(3) 0.67674(14) 0.2840(3) 0.0147(7) Uani 1 1 d . . . CNT2 . 0.59595(12) 0.88314(6) 0.20822(11) . . . . dum . . . C32 C 0.5784(3) 0.83049(14) 0.2438(3) 0.0146(7) Uiso 1 1 d . . . C33 C 0.6695(3) 0.85890(14) 0.2921(3) 0.0157(7) Uiso 1 1 d . . . C34 C 0.6857(3) 0.91127(15) 0.2576(3) 0.0187(7) Uiso 1 1 d . . . H34 H 0.7475 0.9305 0.2922 0.022 Uiso 1 1 calc R . . C35 C 0.6133(3) 0.93613(15) 0.1735(3) 0.0189(8) Uani 1 1 d . . . C36 C 0.5243(3) 0.90675(15) 0.1243(3) 0.0181(7) Uani 1 1 d . . . H36 H 0.4753 0.9224 0.0655 0.022 Uiso 1 1 calc R . . C37 C 0.5045(3) 0.85534(14) 0.1580(3) 0.0165(7) Uani 1 1 d . . . C38 C 0.5097(3) 0.61936(14) 0.2382(3) 0.0150(7) Uani 1 1 d . . . C39 C 0.5718(3) 0.57493(15) 0.2871(3) 0.0177(7) Uani 1 1 d . . . C40 C 0.5558(3) 0.52199(15) 0.2427(3) 0.0227(8) Uani 1 1 d . . . H40 H 0.5997 0.4922 0.2757 0.027 Uiso 1 1 calc R . . C41 C 0.4775(3) 0.51170(15) 0.1519(3) 0.0243(9) Uani 1 1 d . . . C42 C 0.4136(3) 0.55602(16) 0.1059(3) 0.0203(8) Uani 1 1 d . . . H42 H 0.3584 0.5496 0.0446 0.024 Uiso 1 1 calc R . . C43 C 0.4285(3) 0.60948(15) 0.1472(3) 0.0169(7) Uani 1 1 d . . . C44 C 0.7505(3) 0.83398(17) 0.3847(3) 0.0245(8) Uani 1 1 d . . . H44A H 0.8170 0.8501 0.3926 0.037 Uiso 1 1 calc R . . H44B H 0.7528 0.7934 0.3766 0.037 Uiso 1 1 calc R . . H44C H 0.7338 0.8424 0.4445 0.037 Uiso 1 1 calc R . . C45 C 0.6305(3) 0.99380(15) 0.1383(3) 0.0250(9) Uani 1 1 d . . . H45A H 0.6209 0.9924 0.0666 0.037 Uiso 1 1 calc R . . H45B H 0.7000 1.0061 0.1770 0.037 Uiso 1 1 calc R . . H45C H 0.5817 1.0201 0.1487 0.037 Uiso 1 1 calc R . . C46 C 0.4026(3) 0.82737(15) 0.1070(3) 0.0191(8) Uani 1 1 d . . . H46A H 0.3592 0.8336 0.1468 0.029 Uiso 1 1 calc R . . H46B H 0.4128 0.7872 0.1017 0.029 Uiso 1 1 calc R . . H46C H 0.3698 0.8432 0.0395 0.029 Uiso 1 1 calc R . . C47 C 0.6588(3) 0.58387(17) 0.3862(3) 0.0267(9) Uani 1 1 d . . . H47A H 0.6876 0.6212 0.3871 0.040 Uiso 1 1 calc R . . H47B H 0.7117 0.5557 0.3938 0.040 Uiso 1 1 calc R . . H47C H 0.6334 0.5804 0.4419 0.040 Uiso 1 1 calc R . . C48 C 0.4655(4) 0.45471(17) 0.1042(3) 0.0313(10) Uani 1 1 d . . . H48A H 0.3929 0.4463 0.0709 0.047 Uiso 1 1 calc R . . H48B H 0.4968 0.4266 0.1563 0.047 Uiso 1 1 calc R . . H48C H 0.4991 0.4541 0.0545 0.047 Uiso 1 1 calc R . . C49 C 0.3589(3) 0.65634(16) 0.0927(3) 0.0233(8) Uani 1 1 d . . . H49A H 0.3381 0.6779 0.1408 0.035 Uiso 1 1 calc R . . H49B H 0.2984 0.6408 0.0406 0.035 Uiso 1 1 calc R . . H49C H 0.3950 0.6808 0.0613 0.035 Uiso 1 1 calc R . . C50 C 0.6231(3) 0.67041(15) 0.1279(3) 0.0187(8) Uani 1 1 d . . . H50A H 0.6537 0.6440 0.1832 0.028 Uiso 1 1 calc R . . H50B H 0.6704 0.6771 0.0924 0.028 Uiso 1 1 calc R . . H50C H 0.5594 0.6548 0.0809 0.028 Uiso 1 1 calc R . . C61 C 0.8674(8) 0.4841(6) -0.0419(11) 0.077(5) Uani 0.50 1 d P . . H61A H 0.8826 0.4624 -0.0933 0.115 Uiso 0.50 1 calc PR . . H61B H 0.8023 0.5036 -0.0728 0.115 Uiso 0.50 1 calc PR . . H61C H 0.8631 0.4590 0.0109 0.115 Uiso 0.50 1 calc PR . . O62 O 0.9529(6) 0.5273(3) 0.0049(6) 0.0463(18) Uani 0.50 1 d P . . C63 C 1.0481(10) 0.5037(5) 0.0466(8) 0.049(3) Uani 0.50 1 d P . . H63A H 1.0706 0.4909 -0.0084 0.059 Uiso 0.50 1 calc PR . . H63B H 1.0433 0.4705 0.0861 0.059 Uiso 0.50 1 calc PR . . C64 C 1.1319(5) 0.5448(3) 0.1176(5) 0.0121(13) Uani 0.50 1 d P . . H64A H 1.1259 0.5814 0.0850 0.018 Uiso 0.50 1 calc PR . . H64B H 1.1999 0.5294 0.1298 0.018 Uiso 0.50 1 calc PR . . H64C H 1.1215 0.5490 0.1819 0.018 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tl1 0.01788(7) 0.01880(7) 0.01529(7) 0.00021(5) 0.00284(5) 0.00111(5) Tl2 0.02150(8) 0.01785(7) 0.02547(8) 0.00078(5) 0.01491(6) -0.00248(5) N1 0.0222(17) 0.0162(15) 0.0139(15) -0.0008(11) 0.0065(13) -0.0002(12) C1 0.0114(17) 0.0168(17) 0.0149(17) -0.0016(13) 0.0054(14) -0.0010(13) N2 0.0189(16) 0.0150(14) 0.0161(15) -0.0002(12) 0.0093(13) 0.0008(12) C2 0.0136(18) 0.0164(17) 0.0179(17) 0.0021(13) 0.0078(15) 0.0010(13) C3 0.0131(18) 0.0250(19) 0.0172(18) 0.0051(15) 0.0043(15) -0.0027(14) C4 0.022(2) 0.028(2) 0.0131(17) -0.0001(15) 0.0030(16) -0.0049(16) C5 0.0167(19) 0.0218(19) 0.0209(19) -0.0040(15) 0.0073(16) -0.0078(14) C6 0.0124(17) 0.0149(16) 0.0150(16) -0.0003(13) 0.0053(14) -0.0022(13) C7 0.0183(19) 0.0186(18) 0.0139(17) 0.0013(13) 0.0065(15) -0.0014(14) C8 0.0156(18) 0.0206(18) 0.0136(17) 0.0015(13) 0.0054(15) -0.0016(14) C9 0.018(2) 0.026(2) 0.0181(18) 0.0000(15) 0.0042(16) -0.0049(15) C10 0.027(2) 0.0172(18) 0.0196(19) -0.0017(14) 0.0063(17) -0.0073(15) C11 0.025(2) 0.0146(17) 0.024(2) 0.0020(14) 0.0099(17) -0.0003(15) C12 0.019(2) 0.0197(18) 0.0178(18) 0.0023(14) 0.0071(16) -0.0002(15) C13 0.0177(18) 0.0124(16) 0.0130(16) -0.0022(13) 0.0035(14) 0.0003(13) C14 0.020(2) 0.0159(17) 0.0207(18) -0.0061(14) 0.0063(16) -0.0023(14) C15 0.020(2) 0.0169(18) 0.0223(19) -0.0018(14) 0.0046(16) 0.0048(15) C16 0.024(2) 0.0178(18) 0.0190(18) -0.0032(14) 0.0066(17) 0.0013(15) C17 0.026(2) 0.0132(17) 0.0207(19) -0.0022(14) 0.0085(17) -0.0031(15) C18 0.0160(18) 0.0129(16) 0.0176(17) -0.0054(13) 0.0046(15) -0.0042(13) C19 0.0122(18) 0.0241(19) 0.0194(18) -0.0041(15) 0.0046(15) -0.0019(14) C20 0.034(3) 0.019(2) 0.038(3) -0.0015(18) 0.009(2) -0.0048(18) C21 0.017(2) 0.0211(19) 0.037(2) 0.0043(17) 0.0116(18) 0.0011(15) C22 0.024(2) 0.029(2) 0.038(2) 0.0020(18) 0.016(2) 0.0023(17) C23 0.043(3) 0.020(2) 0.031(2) 0.0065(17) 0.014(2) 0.0087(18) C24 0.0170(19) 0.0202(19) 0.0231(19) -0.0006(15) 0.0083(16) -0.0023(15) C25 0.028(2) 0.0162(18) 0.0189(18) 0.0007(14) 0.0099(17) -0.0019(15) C26 0.0111(16) 0.0140(16) 0.0123(16) 0.0018(13) 0.0023(13) 0.0023(13) C27 0.0141(17) 0.0109(15) 0.0138(16) 0.0021(12) 0.0040(14) -0.0003(13) C28 0.0189(19) 0.0143(17) 0.0183(17) -0.0008(13) 0.0085(15) 0.0025(14) C29 0.022(2) 0.0207(18) 0.0170(18) 0.0023(14) 0.0106(16) 0.0018(15) C30 0.0153(18) 0.0194(17) 0.0147(17) 0.0060(14) 0.0059(15) -0.0012(14) C31 0.0127(17) 0.0149(17) 0.0144(16) 0.0022(13) 0.0021(14) 0.0010(13) C35 0.020(2) 0.0148(17) 0.026(2) 0.0009(14) 0.0142(17) -0.0002(14) C36 0.022(2) 0.0185(18) 0.0167(17) 0.0039(14) 0.0101(16) 0.0062(15) C37 0.0171(19) 0.0156(17) 0.0190(18) -0.0013(14) 0.0090(15) 0.0010(14) C38 0.0173(18) 0.0116(16) 0.0183(17) 0.0040(13) 0.0090(15) -0.0021(13) C39 0.021(2) 0.0160(17) 0.0178(18) 0.0060(14) 0.0094(16) 0.0017(14) C40 0.030(2) 0.0166(18) 0.027(2) 0.0047(15) 0.0162(18) -0.0003(16) C41 0.036(2) 0.0169(18) 0.030(2) -0.0070(16) 0.024(2) -0.0103(16) C42 0.021(2) 0.024(2) 0.0181(18) -0.0032(15) 0.0093(16) -0.0084(15) C43 0.0159(19) 0.0202(18) 0.0145(17) 0.0011(14) 0.0053(15) -0.0035(14) C44 0.016(2) 0.029(2) 0.025(2) 0.0042(16) 0.0039(17) -0.0003(16) C45 0.028(2) 0.0166(18) 0.035(2) 0.0056(16) 0.0169(19) 0.0008(16) C46 0.0174(19) 0.0210(18) 0.0175(18) 0.0013(14) 0.0046(15) 0.0002(14) C47 0.030(2) 0.023(2) 0.024(2) 0.0046(16) 0.0053(18) 0.0045(17) C48 0.048(3) 0.020(2) 0.037(2) -0.0080(17) 0.028(2) -0.0106(19) C49 0.016(2) 0.029(2) 0.0207(19) 0.0006(16) 0.0014(16) -0.0030(16) C50 0.0180(19) 0.0188(18) 0.0239(19) 0.0000(14) 0.0129(16) -0.0036(14) C61 0.026(6) 0.093(10) 0.099(10) 0.092(9) 0.009(6) 0.001(6) O62 0.048(5) 0.035(4) 0.057(5) 0.023(4) 0.021(4) 0.001(3) C63 0.076(10) 0.035(6) 0.038(6) 0.011(5) 0.022(6) 0.016(6) C64 0.020(4) 0.009(3) 0.010(3) 0.009(2) 0.009(3) 0.006(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tl Tl -2.8358 9.6688 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Tl1 CNT1 89.18(8) . . ? N2 Tl2 CNT2 89.24(7) . . ? C1 N1 C25 119.4(3) . . ? C1 N1 Tl1 132.7(2) . . ? C25 N1 Tl1 107.9(2) . . ? N1 C1 C6 118.6(3) . . ? N1 C1 C2 125.4(3) . . ? C6 C1 C2 116.0(3) . . ? C26 N2 C50 120.9(3) . . ? C26 N2 Tl2 132.4(2) . . ? C50 N2 Tl2 105.5(2) . . ? C3 C2 C1 118.9(3) . . ? C3 C2 C7 117.5(3) . . ? C1 C2 C7 123.3(3) . . ? C4 C3 C2 122.7(3) . . ? C4 C3 H3 118.7 . . ? C2 C3 H3 118.7 . . ? C3 C4 C5 118.5(3) . . ? C3 C4 H4 120.8 . . ? C5 C4 H4 120.8 . . ? C6 C5 C4 120.5(3) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C5 C6 C1 122.1(3) . . ? C5 C6 C13 118.3(3) . . ? C1 C6 C13 119.5(3) . . ? C12 C7 C8 119.1(3) . . ? C12 C7 C2 121.0(3) . . ? C8 C7 C2 119.9(3) . . ? C9 C8 C7 119.3(3) . . ? C9 C8 C19 118.8(3) . . ? C7 C8 C19 121.8(3) . . ? C10 C9 C8 122.5(4) . . ? C10 C9 H9 118.8 . . ? C8 C9 H9 118.8 . . ? C9 C10 C11 117.6(3) . . ? C9 C10 C20 121.6(4) . . ? C11 C10 C20 120.7(4) . . ? C10 C11 C12 122.1(4) . . ? C10 C11 H11 119.0 . . ? C12 C11 H11 119.0 . . ? C11 C12 C7 119.4(4) . . ? C11 C12 C21 119.1(3) . . ? C7 C12 C21 121.4(3) . . ? C14 C13 C18 119.6(3) . . ? C14 C13 C6 120.6(3) . . ? C18 C13 C6 119.8(3) . . ? C15 C14 C13 119.0(3) . . ? C15 C14 C22 119.8(4) . . ? C13 C14 C22 121.2(3) . . ? C16 C15 C14 121.7(4) . . ? C16 C15 H15 119.2 . . ? C14 C15 H15 119.2 . . ? C17 C16 C15 118.4(4) . . ? C17 C16 C23 121.1(4) . . ? C15 C16 C23 120.5(4) . . ? C16 C17 C18 122.1(4) . . ? C16 C17 H17 118.9 . . ? C18 C17 H17 118.9 . . ? C17 C18 C13 119.1(3) . . ? C17 C18 C24 121.9(3) . . ? C13 C18 C24 119.0(3) . . ? C8 C19 H19A 109.5 . . ? C8 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C8 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C10 C20 H20A 109.5 . . ? C10 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C10 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C12 C21 H21A 109.5 . . ? C12 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C12 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C14 C22 H22A 109.5 . . ? C14 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C14 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C16 C23 H23A 109.5 . . ? C16 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C16 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C18 C24 H24A 109.5 . . ? C18 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C18 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N1 C25 H25A 109.5 . . ? N1 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N1 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N2 C26 C27 117.4(3) . . ? N2 C26 C31 127.5(3) . . ? C27 C26 C31 115.0(3) . . ? C28 C27 C26 121.9(3) . . ? C28 C27 C32 117.4(3) . . ? C26 C27 C32 120.7(3) . . ? C27 C28 C29 121.8(3) . . ? C27 C28 H28 119.1 . . ? C29 C28 H28 119.1 . . ? C28 C29 C30 117.6(3) . . ? C28 C29 H29 121.2 . . ? C30 C29 H29 121.2 . . ? C31 C30 C29 123.3(3) . . ? C31 C30 H30 118.3 . . ? C29 C30 H30 118.3 . . ? C30 C31 C26 120.0(3) . . ? C30 C31 C38 116.1(3) . . ? C26 C31 C38 123.7(3) . . ? C33 C32 C37 118.7(3) . . ? C33 C32 C27 121.5(3) . . ? C37 C32 C27 119.5(3) . . ? C34 C33 C32 120.1(3) . . ? C34 C33 C44 119.4(3) . . ? C32 C33 C44 120.4(3) . . ? C33 C34 C35 121.6(4) . . ? C33 C34 H34 119.2 . . ? C35 C34 H34 119.2 . . ? C36 C35 C34 117.8(3) . . ? C36 C35 C45 121.1(4) . . ? C34 C35 C45 121.1(4) . . ? C37 C36 C35 122.2(4) . . ? C37 C36 H36 118.9 . . ? C35 C36 H36 118.9 . . ? C36 C37 C32 119.6(3) . . ? C36 C37 C46 120.1(3) . . ? C32 C37 C46 120.2(3) . . ? C39 C38 C43 119.2(3) . . ? C39 C38 C31 121.0(3) . . ? C43 C38 C31 119.7(3) . . ? C38 C39 C40 119.7(4) . . ? C38 C39 C47 120.6(3) . . ? C40 C39 C47 119.6(3) . . ? C41 C40 C39 121.8(4) . . ? C41 C40 H40 119.1 . . ? C39 C40 H40 119.1 . . ? C40 C41 C42 117.8(3) . . ? C40 C41 C48 120.3(4) . . ? C42 C41 C48 121.9(4) . . ? C43 C42 C41 121.8(4) . . ? C43 C42 H42 119.1 . . ? C41 C42 H42 119.1 . . ? C42 C43 C38 119.5(3) . . ? C42 C43 C49 119.7(3) . . ? C38 C43 C49 120.8(3) . . ? C33 C44 H44A 109.5 . . ? C33 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C33 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C35 C45 H45A 109.5 . . ? C35 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C35 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C37 C46 H46A 109.5 . . ? C37 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C37 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C39 C47 H47A 109.5 . . ? C39 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C39 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C41 C48 H48A 109.5 . . ? C41 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C41 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C43 C49 H49A 109.5 . . ? C43 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C43 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? N2 C50 H50A 109.5 . . ? N2 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? N2 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? O62 C61 H61A 109.5 . . ? O62 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? O62 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C63 O62 C61 113.5(9) . . ? O62 C63 C64 113.9(9) . . ? O62 C63 H63A 108.8 . . ? C64 C63 H63A 108.8 . . ? O62 C63 H63B 108.8 . . ? C64 C63 H63B 108.8 . . ? H63A C63 H63B 107.7 . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tl1 N1 2.348(3) . ? Tl1 CNT1 2.9692(14) . ? Tl2 N2 2.379(3) . ? Tl2 CNT2 3.0821(14) . ? N1 C1 1.359(4) . ? N1 C25 1.451(4) . ? C1 C6 1.429(5) . ? C1 C2 1.444(5) . ? N2 C26 1.359(4) . ? N2 C50 1.472(4) . ? C2 C3 1.402(5) . ? C2 C7 1.506(5) . ? C3 C4 1.388(5) . ? C3 H3 0.9500 . ? C4 C5 1.396(5) . ? C4 H4 0.9500 . ? C5 C6 1.385(5) . ? C5 H5 0.9500 . ? C6 C13 1.493(5) . ? C7 C12 1.405(5) . ? C7 C8 1.409(5) . ? C8 C9 1.393(5) . ? C8 C19 1.504(5) . ? C9 C10 1.380(5) . ? C9 H9 0.9500 . ? C10 C11 1.392(6) . ? C10 C20 1.512(5) . ? C11 C12 1.396(5) . ? C11 H11 0.9500 . ? C12 C21 1.505(5) . ? C13 C14 1.407(5) . ? C13 C18 1.411(5) . ? C14 C15 1.403(5) . ? C14 C22 1.511(5) . ? C15 C16 1.388(5) . ? C15 H15 0.9500 . ? C16 C17 1.384(5) . ? C16 C23 1.515(5) . ? C17 C18 1.391(5) . ? C17 H17 0.9500 . ? C18 C24 1.513(5) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.445(5) . ? C26 C31 1.454(5) . ? C27 C28 1.383(5) . ? C27 C32 1.498(5) . ? C28 C29 1.388(5) . ? C28 H28 0.9500 . ? C29 C30 1.394(5) . ? C29 H29 0.9500 . ? C30 C31 1.383(5) . ? C30 H30 0.9500 . ? C31 C38 1.503(5) . ? C32 C33 1.395(5) . ? C32 C37 1.420(5) . ? C33 C34 1.394(5) . ? C33 C44 1.521(5) . ? C34 C35 1.397(5) . ? C34 H34 0.9500 . ? C35 C36 1.387(5) . ? C35 C45 1.517(5) . ? C36 C37 1.384(5) . ? C36 H36 0.9500 . ? C37 C46 1.511(5) . ? C38 C39 1.394(5) . ? C38 C43 1.406(5) . ? C39 C40 1.398(5) . ? C39 C47 1.516(5) . ? C40 C41 1.387(6) . ? C40 H40 0.9500 . ? C41 C42 1.393(6) . ? C41 C48 1.506(5) . ? C42 C43 1.393(5) . ? C42 H42 0.9500 . ? C43 C49 1.508(5) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C61 O62 1.544(15) . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? O62 C63 1.376(13) . ? C63 C64 1.589(14) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ?
1100777.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100777.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100777 loop_ _publ_author_name 'Rolf W. Berg' 'Niels Thorup' _publ_contact_author_address ; Department of Chemistry Technical University of Denmark DTU-207 DK-2800 Lyngby Denmark ; _publ_contact_author_email rwb@kemi.dtu.dk _publ_contact_author_fax '+45 4588 3136' _publ_contact_author_name 'Rolf W. Berg' _publ_contact_author_phone '+45 4525 2412' _publ_section_title ; The Reaction between ZnO and Molten Na2S2O7 or K2S2O7 Forming Na2Zn(SO4)2 or K2Zn(SO4)2, Studied by Raman Spectroscopy and X-ray Diffraction ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3485 _journal_page_last 3493 _journal_paper_doi 10.1021/ic0500513 _journal_volume 44 _journal_year 2005 _chemical_formula_moiety 'Na2 O8 S2 Zn' _chemical_formula_sum 'Na2 O8 S2 Zn' _chemical_formula_weight 303.47 _space_group_IT_number 13 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yac' _symmetry_space_group_name_H-M 'P 1 2/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method 'manual editing of SHELXL-97 cif' _cell_angle_alpha 90.00 _cell_angle_beta 90.879(6) _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 8.648(3) _cell_length_b 10.323(3) _cell_length_c 15.103(5) _cell_measurement_reflns_used 923 _cell_measurement_temperature 295(2) _cell_measurement_theta_max 28.627 _cell_measurement_theta_min 3.342 _cell_volume 1348.1(8) _computing_cell_refinement 'SAINT ver 6.02a (Bruker AXS, 2000)' _computing_data_collection 'SMART ver 5.054 (Bruker AXS, 1998)' _computing_data_reduction 'SAINT ver 6.02a (Bruker AXS, 2000)' _computing_molecular_graphics 'SHELXTL ver 6.12 (Bruker AXS, 2001)' _computing_publication_material 'SHELXTL ver 6.12 (Bruker AXS, 2001)' _computing_structure_refinement 'SHELXTL ver 6.12 (Bruker AXS, 2001)' _computing_structure_solution 'SHELXTL ver 6.12 (Bruker AXS, 2001)' _diffrn_ambient_temperature 295(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Siemens/Bruker SMART 1K' _diffrn_measurement_method 'omega scan, frame data integration' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0702 _diffrn_reflns_av_sigmaI/netI 0.0559 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 13993 _diffrn_reflns_theta_full 26.36 _diffrn_reflns_theta_max 26.36 _diffrn_reflns_theta_min 1.97 _exptl_absorpt_coefficient_mu 4.401 _exptl_absorpt_correction_T_max 0.9573 _exptl_absorpt_correction_T_min 0.3519 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Sheldrick, 2000)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.991 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 1184 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.01 _refine_diff_density_max 0.581 _refine_diff_density_min -0.554 _refine_diff_density_rms 0.133 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 237 _refine_ls_number_reflns 2748 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.999 _refine_ls_R_factor_all 0.0758 _refine_ls_R_factor_gt 0.0369 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0399P)^2^+0.3988P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0810 _refine_ls_wR_factor_ref 0.0945 _reflns_number_gt 1741 _reflns_number_total 2748 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic0500513si20050113_124143_1.cif _cod_data_source_block naznc _cod_original_cell_volume 1348.1(7) _cod_database_code 1100777 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.58357(6) 0.61983(5) 0.12303(3) 0.01704(16) Uani 1 1 d . . . Zn2 Zn 1.07368(6) 0.87539(5) 0.12374(3) 0.01721(17) Uani 1 1 d . . . S1 S 0.92734(13) 0.60864(11) 0.15714(7) 0.0139(3) Uani 1 1 d . . . S2 S 0.92296(13) 1.12960(11) 0.09012(7) 0.0160(3) Uani 1 1 d . . . S3 S 0.43586(13) 0.88941(11) 0.15759(7) 0.0141(3) Uani 1 1 d . . . S4 S 0.43670(13) 0.37216(11) 0.09497(7) 0.0156(3) Uani 1 1 d . . . Na1 Na 0.2500 0.1589(3) 0.2500 0.0301(7) Uani 1 2 d S . . Na2 Na 0.8023(2) 0.39753(18) -0.01361(12) 0.0252(5) Uani 1 1 d . . . Na3 Na 1.2500 0.5798(3) 0.2500 0.0286(7) Uani 1 2 d S . . Na4 Na 0.3021(2) 0.10596(19) 0.01832(13) 0.0306(5) Uani 1 1 d . . . Na5 Na 0.7500 1.0048(3) 0.2500 0.0357(8) Uani 1 2 d S . . Na6 Na 0.7500 0.3458(3) 0.2500 0.0491(10) Uani 1 2 d S . . O1 O 0.7947(4) 0.6968(3) 0.1471(2) 0.0216(8) Uani 1 1 d . . . O2 O 0.5726(4) 0.5452(3) 0.2555(2) 0.0201(8) Uani 1 1 d . . . O3 O 0.9287(4) 0.5127(3) 0.0885(2) 0.0293(9) Uani 1 1 d . . . O4 O 1.0698(3) 0.6873(3) 0.1523(2) 0.0162(7) Uani 1 1 d . . . O5 O 0.8991(4) 0.9850(3) 0.0856(2) 0.0198(7) Uani 1 1 d . . . O6 O 0.8280(4) 1.1802(3) 0.1595(2) 0.0230(8) Uani 1 1 d . . . O7 O 1.0851(4) 1.1552(3) 0.1054(2) 0.0261(8) Uani 1 1 d . . . O8 O 1.1289(4) 0.8177(3) -0.0035(2) 0.0274(9) Uani 1 1 d . . . O9 O 0.4154(4) 0.7475(3) 0.1486(2) 0.0206(8) Uani 1 1 d . . . O10 O 1.2830(4) 0.9494(3) 0.1473(2) 0.0291(9) Uani 1 1 d . . . O11 O 0.5382(4) 0.9405(3) 0.0933(2) 0.0327(9) Uani 1 1 d . . . O12 O 1.0037(4) 0.9209(3) 0.2541(2) 0.0296(9) Uani 1 1 d . . . O13 O 0.6010(4) 0.6799(3) -0.0067(2) 0.0248(8) Uani 1 1 d . . . O14 O 0.5967(4) 0.4268(3) 0.0929(2) 0.0230(8) Uani 1 1 d . . . O15 O 0.3350(4) 0.4800(3) 0.1158(2) 0.0269(9) Uani 1 1 d . . . O16 O 0.4268(4) 0.2705(3) 0.1591(2) 0.0284(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0170(3) 0.0164(3) 0.0177(3) -0.0030(2) 0.0006(2) 0.0012(2) Zn2 0.0181(3) 0.0156(3) 0.0179(3) 0.0009(2) -0.0006(2) 0.0021(2) S1 0.0136(6) 0.0163(7) 0.0117(6) 0.0002(5) 0.0009(5) -0.0026(5) S2 0.0189(7) 0.0159(7) 0.0134(6) 0.0004(5) 0.0029(5) 0.0047(5) S3 0.0138(6) 0.0148(6) 0.0140(6) 0.0012(5) 0.0033(5) 0.0007(5) S4 0.0211(7) 0.0130(6) 0.0126(6) 0.0004(5) 0.0006(5) -0.0011(5) Na1 0.0393(18) 0.0290(17) 0.0223(16) 0.000 0.0126(14) 0.000 Na2 0.0317(12) 0.0243(12) 0.0196(10) -0.0032(8) 0.0000(9) 0.0086(9) Na3 0.0258(16) 0.0406(19) 0.0194(15) 0.000 -0.0008(13) 0.000 Na4 0.0348(12) 0.0275(12) 0.0299(11) -0.0057(9) 0.0168(10) -0.0067(9) Na5 0.0245(17) 0.0322(19) 0.051(2) 0.000 0.0145(15) 0.000 Na6 0.091(3) 0.0189(18) 0.0379(19) 0.000 0.0305(19) 0.000 O1 0.0161(18) 0.025(2) 0.0241(19) 0.0063(15) -0.0013(15) 0.0028(14) O2 0.026(2) 0.0184(19) 0.0159(17) -0.0048(13) 0.0057(15) -0.0014(14) O3 0.037(2) 0.029(2) 0.0213(19) -0.0110(15) 0.0019(17) -0.0044(17) O4 0.0128(17) 0.0137(18) 0.0221(17) 0.0027(14) 0.0038(14) -0.0018(13) O5 0.0235(18) 0.0153(18) 0.0206(18) 0.0009(14) 0.0011(15) 0.0035(14) O6 0.028(2) 0.025(2) 0.0170(17) -0.0036(15) 0.0071(15) 0.0076(15) O7 0.0203(19) 0.028(2) 0.030(2) 0.0000(16) 0.0040(16) -0.0011(15) O8 0.041(2) 0.027(2) 0.0143(18) 0.0022(15) 0.0019(17) 0.0164(16) O9 0.021(2) 0.0147(19) 0.0256(18) 0.0023(14) 0.0035(15) 0.0000(14) O10 0.024(2) 0.021(2) 0.043(2) -0.0004(16) -0.0070(17) 0.0043(15) O11 0.038(2) 0.026(2) 0.035(2) -0.0019(17) 0.0239(18) -0.0072(17) O12 0.040(2) 0.033(2) 0.0162(18) 0.0001(16) -0.0068(17) 0.0135(18) O13 0.038(2) 0.022(2) 0.0144(18) -0.0046(14) -0.0003(16) -0.0075(16) O14 0.0214(19) 0.0220(19) 0.0256(19) -0.0070(15) 0.0061(15) -0.0060(15) O15 0.029(2) 0.026(2) 0.025(2) -0.0054(15) -0.0033(16) 0.0099(16) O16 0.038(2) 0.023(2) 0.025(2) 0.0093(16) 0.0065(18) -0.0008(17) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O9 Zn1 O1 111.29(13) . . ? O9 Zn1 O14 136.52(13) . . ? O1 Zn1 O14 111.72(13) . . ? O9 Zn1 O13 92.80(13) . . ? O1 Zn1 O13 88.47(13) . . ? O14 Zn1 O13 94.39(13) . . ? O9 Zn1 O2 90.81(12) . . ? O1 Zn1 O2 91.51(12) . . ? O14 Zn1 O2 82.02(12) . . ? O13 Zn1 O2 176.14(12) . . ? O9 Zn1 Na3 50.81(10) . 1_455 ? O1 Zn1 Na3 134.11(9) . 1_455 ? O14 Zn1 Na3 93.18(10) . 1_455 ? O13 Zn1 Na3 128.79(10) . 1_455 ? O2 Zn1 Na3 53.19(9) . 1_455 ? O9 Zn1 Na2 155.43(10) . . ? O1 Zn1 Na2 82.74(10) . . ? O14 Zn1 Na2 39.52(9) . . ? O13 Zn1 Na2 66.71(10) . . ? O2 Zn1 Na2 109.45(9) . . ? Na3 Zn1 Na2 132.39(6) 1_455 . ? O9 Zn1 Na4 78.96(9) . 3_665 ? O1 Zn1 Na4 63.40(10) . 3_665 ? O14 Zn1 Na4 127.00(9) . 3_665 ? O13 Zn1 Na4 36.45(9) . 3_665 ? O2 Zn1 Na4 146.13(9) . 3_665 ? Na3 Zn1 Na4 129.48(6) 1_455 3_665 ? Na2 Zn1 Na4 90.54(5) . 3_665 ? O5 Zn2 O4 127.57(13) . . ? O5 Zn2 O10 121.57(14) . . ? O4 Zn2 O10 110.72(13) . . ? O5 Zn2 O8 94.60(13) . . ? O4 Zn2 O8 85.72(12) . . ? O10 Zn2 O8 93.11(14) . . ? O5 Zn2 O12 85.17(13) . . ? O4 Zn2 O12 90.54(13) . . ? O10 Zn2 O12 91.16(14) . . ? O8 Zn2 O12 175.11(14) . . ? O5 Zn2 Na2 124.85(10) . 3_765 ? O4 Zn2 Na2 46.68(9) . 3_765 ? O10 Zn2 Na2 96.38(10) . 3_765 ? O8 Zn2 Na2 40.68(9) . 3_765 ? O12 Zn2 Na2 136.34(10) . 3_765 ? O5 Zn2 Na4 84.92(10) . 1_665 ? O4 Zn2 Na4 140.84(9) . 1_665 ? O10 Zn2 Na4 45.69(11) . 1_665 ? O8 Zn2 Na4 68.49(10) . 1_665 ? O12 Zn2 Na4 116.32(11) . 1_665 ? Na2 Zn2 Na4 98.89(5) 3_765 1_665 ? O5 Zn2 Na5 49.70(9) . . ? O4 Zn2 Na5 103.17(10) . . ? O10 Zn2 Na5 117.80(10) . . ? O8 Zn2 Na5 140.85(10) . . ? O12 Zn2 Na5 37.34(9) . . ? Na2 Zn2 Na5 142.59(5) 3_765 . ? Na4 Zn2 Na5 115.51(6) 1_665 . ? O3 S1 O1 111.6(2) . . ? O3 S1 O2 109.9(2) . 2_655 ? O1 S1 O2 110.94(18) . 2_655 ? O3 S1 O4 109.10(19) . . ? O1 S1 O4 107.72(19) . . ? O2 S1 O4 107.46(19) 2_655 . ? O3 S1 Na3 103.98(16) . . ? O1 S1 Na3 142.85(15) . . ? O2 S1 Na3 64.33(13) 2_655 . ? O4 S1 Na3 48.25(13) . . ? O3 S1 Na2 58.97(14) . 3_765 ? O1 S1 Na2 121.13(13) . 3_765 ? O2 S1 Na2 127.25(14) 2_655 3_765 ? O4 S1 Na2 50.33(13) . 3_765 ? Na3 S1 Na2 69.28(5) . 3_765 ? O6 S2 O7 112.4(2) . . ? O6 S2 O8 109.98(19) . 3_775 ? O7 S2 O8 110.8(2) . 3_775 ? O6 S2 O5 108.25(18) . . ? O7 S2 O5 108.72(19) . . ? O8 S2 O5 106.50(19) 3_775 . ? O6 S2 Na5 45.93(14) . . ? O7 S2 Na5 115.25(15) . . ? O8 S2 Na5 133.60(15) 3_775 . ? O5 S2 Na5 64.02(13) . . ? O6 S2 Na2 82.14(14) . 1_565 ? O7 S2 Na2 102.66(15) . 1_565 ? O5 S2 Na2 139.21(14) . 1_565 ? Na5 S2 Na2 123.52(6) . 1_565 ? O11 S3 O12 108.8(2) . 2_655 ? O11 S3 O10 109.9(2) . 1_455 ? O12 S3 O10 108.1(2) 2_655 1_455 ? O11 S3 O9 112.20(19) . . ? O12 S3 O9 110.1(2) 2_655 . ? O10 S3 O9 107.56(19) 1_455 . ? O11 S3 Na5 68.58(16) . . ? O10 S3 Na5 129.41(15) 1_455 . ? O9 S3 Na5 119.89(14) . . ? O11 S3 Na4 61.68(16) . 1_565 ? O12 S3 Na4 123.57(15) 2_655 1_565 ? O10 S3 Na4 48.20(14) 1_455 1_565 ? O9 S3 Na4 125.20(14) . 1_565 ? Na5 S3 Na4 108.05(7) . 1_565 ? O16 S4 O15 111.8(2) . . ? O16 S4 O13 109.3(2) . 3_665 ? O15 S4 O13 110.4(2) . 3_665 ? O16 S4 O14 110.9(2) . . ? O15 S4 O14 106.2(2) . . ? O13 S4 O14 108.17(19) 3_665 . ? O16 S4 Na4 65.75(15) . . ? O15 S4 Na4 121.18(15) . . ? O14 S4 Na4 130.51(14) . . ? O16 S4 Na2 136.15(15) . 3_665 ? O13 S4 Na2 78.53(14) 3_665 3_665 ? O14 S4 Na2 106.77(15) . 3_665 ? Na4 S4 Na2 104.87(6) . 3_665 ? O16 Na1 O16 121.8(2) 2 . ? O16 Na1 O7 82.55(11) 2 2_645 ? O16 Na1 O7 98.28(12) . 2_645 ? O16 Na1 O7 98.28(12) 2 1_445 ? O16 Na1 O7 82.55(11) . 1_445 ? O7 Na1 O7 178.3(2) 2_645 1_445 ? O16 Na1 O10 88.96(11) 2 2_645 ? O16 Na1 O10 143.46(12) . 2_645 ? O7 Na1 O10 64.04(11) 2_645 2_645 ? O7 Na1 O10 114.45(13) 1_445 2_645 ? O16 Na1 O10 143.46(13) 2 1_445 ? O16 Na1 O10 88.96(11) . 1_445 ? O7 Na1 O10 114.45(13) 2_645 1_445 ? O7 Na1 O10 64.04(11) 1_445 1_445 ? O10 Na1 O10 72.33(16) 2_645 1_445 ? O16 Na1 Na4 54.23(9) 2 2 ? O16 Na1 Na4 137.16(10) . 2 ? O7 Na1 Na4 41.30(8) 2_645 2 ? O7 Na1 Na4 138.31(8) 1_445 2 ? O10 Na1 Na4 45.12(8) 2_645 2 ? O10 Na1 Na4 117.32(11) 1_445 2 ? O16 Na1 Na4 137.16(10) 2 . ? O16 Na1 Na4 54.23(9) . . ? O7 Na1 Na4 138.31(8) 2_645 . ? O7 Na1 Na4 41.30(8) 1_445 . ? O10 Na1 Na4 117.32(11) 2_645 . ? O10 Na1 Na4 45.12(8) 1_445 . ? Na4 Na1 Na4 162.42(11) 2 . ? O3 Na2 O15 114.42(15) . 3_665 ? O3 Na2 O8 108.25(15) . 3_765 ? O15 Na2 O8 136.82(15) 3_665 3_765 ? O3 Na2 O14 80.30(13) . . ? O15 Na2 O14 90.02(13) 3_665 . ? O8 Na2 O14 103.57(13) 3_765 . ? O3 Na2 O4 122.76(14) . 3_765 ? O15 Na2 O4 82.16(12) 3_665 3_765 ? O8 Na2 O4 69.29(11) 3_765 3_765 ? O14 Na2 O4 156.86(13) . 3_765 ? O3 Na2 O3 72.31(13) . 3_765 ? O15 Na2 O3 88.28(13) 3_665 3_765 ? O8 Na2 O3 98.71(13) 3_765 3_765 ? O14 Na2 O3 148.97(13) . 3_765 ? O4 Na2 O3 52.97(10) 3_765 3_765 ? O3 Na2 S1 97.09(11) . 3_765 ? O15 Na2 S1 86.10(10) 3_665 3_765 ? O8 Na2 S1 82.40(10) 3_765 3_765 ? O14 Na2 S1 173.96(11) . 3_765 ? O4 Na2 S1 26.63(7) 3_765 3_765 ? O3 Na2 S1 26.41(7) 3_765 3_765 ? O3 Na2 S2 88.31(11) . 1_545 ? O15 Na2 S2 157.08(12) 3_665 1_545 ? O8 Na2 S2 22.16(8) 3_765 1_545 ? O14 Na2 S2 91.09(10) . 1_545 ? O4 Na2 S2 87.96(9) 3_765 1_545 ? O3 Na2 S2 102.19(10) 3_765 1_545 ? S1 Na2 S2 94.28(6) 3_765 1_545 ? O3 Na2 S4 99.69(11) . 3_665 ? O15 Na2 S4 20.60(8) 3_665 3_665 ? O8 Na2 S4 150.87(12) 3_765 3_665 ? O14 Na2 S4 72.74(10) . 3_665 ? O4 Na2 S4 102.42(9) 3_765 3_665 ? O3 Na2 S4 97.44(9) 3_765 3_665 ? S1 Na2 S4 102.50(6) 3_765 3_665 ? S2 Na2 S4 160.27(7) 1_545 3_665 ? O3 Na2 Zn2 128.17(12) . 3_765 ? O15 Na2 Zn2 106.58(10) 3_665 3_765 ? O8 Na2 Zn2 35.76(8) 3_765 3_765 ? O14 Na2 Zn2 130.95(10) . 3_765 ? O4 Na2 Zn2 34.75(7) 3_765 3_765 ? O3 Na2 Zn2 78.86(8) 3_765 3_765 ? S1 Na2 Zn2 54.82(4) 3_765 3_765 ? S2 Na2 Zn2 56.81(4) 1_545 3_765 ? S4 Na2 Zn2 126.42(6) 3_665 3_765 ? O3 Na2 Na3 134.97(12) . 3_765 ? O15 Na2 Na3 41.07(9) 3_665 3_765 ? O8 Na2 Na3 101.62(11) 3_765 3_765 ? O14 Na2 Na3 124.43(11) . 3_765 ? O4 Na2 Na3 41.76(8) 3_765 3_765 ? O3 Na2 Na3 70.47(8) 3_765 3_765 ? S1 Na2 Na3 54.11(4) 3_765 3_765 ? S2 Na2 Na3 123.58(7) 1_545 3_765 ? S4 Na2 Na3 61.67(5) 3_665 3_765 ? Zn2 Na2 Na3 67.07(6) 3_765 3_765 ? O3 Na2 Zn1 61.52(10) . . ? O15 Na2 Zn1 76.53(9) 3_665 . ? O8 Na2 Zn1 132.67(10) 3_765 . ? O14 Na2 Zn1 32.34(8) . . ? O4 Na2 Zn1 157.32(10) 3_765 . ? O3 Na2 Zn1 117.98(9) 3_765 . ? S1 Na2 Zn1 141.77(7) 3_765 . ? S2 Na2 Zn1 114.72(6) 1_545 . ? S4 Na2 Zn1 55.96(4) 3_665 . ? Zn2 Na2 Zn1 163.14(7) 3_765 . ? Na3 Na2 Zn1 117.60(6) 3_765 . ? O15 Na3 O15 129.2(2) 2_655 1_655 ? O15 Na3 O4 83.29(11) 2_655 2_755 ? O15 Na3 O4 120.90(11) 1_655 2_755 ? O15 Na3 O4 120.90(11) 2_655 . ? O15 Na3 O4 83.29(11) 1_655 . ? O4 Na3 O4 124.94(19) 2_755 . ? O15 Na3 O9 68.19(11) 2_655 2_655 ? O15 Na3 O9 156.34(12) 1_655 2_655 ? O4 Na3 O9 72.69(11) 2_755 2_655 ? O4 Na3 O9 73.22(12) . 2_655 ? O15 Na3 O9 156.34(12) 2_655 1_655 ? O15 Na3 O9 68.19(11) 1_655 1_655 ? O4 Na3 O9 73.22(12) 2_755 1_655 ? O4 Na3 O9 72.69(11) . 1_655 ? O9 Na3 O9 101.28(16) 2_655 1_655 ? O15 Na3 O2 69.76(10) 2_655 2_655 ? O15 Na3 O2 103.71(11) 1_655 2_655 ? O4 Na3 O2 135.29(10) 2_755 2_655 ? O4 Na3 O2 53.61(9) . 2_655 ? O9 Na3 O2 64.49(9) 2_655 2_655 ? O9 Na3 O2 126.28(11) 1_655 2_655 ? O15 Na3 O2 103.71(11) 2_655 1_655 ? O15 Na3 O2 69.76(10) 1_655 1_655 ? O4 Na3 O2 53.61(9) 2_755 1_655 ? O4 Na3 O2 135.29(10) . 1_655 ? O9 Na3 O2 126.28(11) 2_655 1_655 ? O9 Na3 O2 64.49(9) 1_655 1_655 ? O2 Na3 O2 165.42(17) 2_655 1_655 ? O15 Na3 S1 86.82(9) 2_655 2_755 ? O15 Na3 S1 97.91(9) 1_655 2_755 ? O4 Na3 S1 27.34(7) 2_755 2_755 ? O4 Na3 S1 143.13(13) . 2_755 ? O9 Na3 S1 99.20(9) 2_655 2_755 ? O9 Na3 S1 73.68(8) 1_655 2_755 ? O2 Na3 S1 154.94(6) 2_655 2_755 ? O2 Na3 S1 28.16(6) 1_655 2_755 ? O15 Na3 S1 97.91(9) 2_655 . ? O15 Na3 S1 86.82(9) 1_655 . ? O4 Na3 S1 143.13(13) 2_755 . ? O4 Na3 S1 27.34(7) . . ? O9 Na3 S1 73.68(8) 2_655 . ? O9 Na3 S1 99.20(9) 1_655 . ? O2 Na3 S1 28.16(6) 2_655 . ? O2 Na3 S1 154.94(6) 1_655 . ? S1 Na3 S1 169.03(12) 2_755 . ? O15 Na3 Zn1 47.51(8) 2_655 2_655 ? O15 Na3 Zn1 140.94(10) 1_655 2_655 ? O4 Na3 Zn1 98.07(8) 2_755 2_655 ? O4 Na3 Zn1 75.57(8) . 2_655 ? O9 Na3 Zn1 34.68(6) 2_655 2_655 ? O9 Na3 Zn1 132.30(12) 1_655 2_655 ? O2 Na3 Zn1 37.68(6) 2_655 2_655 ? O2 Na3 Zn1 145.22(6) 1_655 2_655 ? S1 Na3 Zn1 118.68(4) 2_755 2_655 ? S1 Na3 Zn1 59.84(3) . 2_655 ? O15 Na3 Zn1 140.94(10) 2_655 1_655 ? O15 Na3 Zn1 47.51(8) 1_655 1_655 ? O4 Na3 Zn1 75.57(8) 2_755 1_655 ? O4 Na3 Zn1 98.07(8) . 1_655 ? O9 Na3 Zn1 132.30(12) 2_655 1_655 ? O9 Na3 Zn1 34.68(6) 1_655 1_655 ? O2 Na3 Zn1 145.22(6) 2_655 1_655 ? O2 Na3 Zn1 37.68(6) 1_655 1_655 ? S1 Na3 Zn1 59.84(3) 2_755 1_655 ? S1 Na3 Zn1 118.68(4) . 1_655 ? Zn1 Na3 Zn1 166.48(10) 2_655 1_655 ? O11 Na4 O7 164.96(17) 3_665 1_445 ? O11 Na4 O13 85.48(13) 3_665 3_665 ? O7 Na4 O13 97.19(13) 1_445 3_665 ? O11 Na4 O5 83.08(14) 3_665 3_665 ? O7 Na4 O5 83.08(13) 1_445 3_665 ? O13 Na4 O5 123.05(14) 3_665 3_665 ? O11 Na4 O10 119.19(15) 3_665 1_445 ? O7 Na4 O10 69.43(12) 1_445 1_445 ? O13 Na4 O10 132.62(14) 3_665 1_445 ? O5 Na4 O10 100.93(12) 3_665 1_445 ? O11 Na4 O11 74.21(14) 3_665 1_545 ? O7 Na4 O11 118.24(13) 1_445 1_545 ? O13 Na4 O11 109.42(13) 3_665 1_545 ? O5 Na4 O11 120.32(12) 3_665 1_545 ? O10 Na4 O11 51.30(10) 1_445 1_545 ? O11 Na4 O16 116.51(14) 3_665 . ? O7 Na4 O16 75.93(12) 1_445 . ? O13 Na4 O16 51.94(11) 3_665 . ? O5 Na4 O16 156.93(13) 3_665 . ? O10 Na4 O16 80.72(12) 1_445 . ? O11 Na4 O16 78.87(11) 1_545 . ? O11 Na4 S4 103.31(11) 3_665 . ? O7 Na4 S4 84.34(10) 1_445 . ? O13 Na4 S4 25.54(8) 3_665 . ? O5 Na4 S4 142.59(11) 3_665 . ? O10 Na4 S4 107.28(11) 1_445 . ? O11 Na4 S4 96.63(10) 1_545 . ? O16 Na4 S4 26.59(7) . . ? O11 Na4 S3 96.95(12) 3_665 1_545 ? O7 Na4 S3 93.76(11) 1_445 1_545 ? O13 Na4 S3 124.25(12) 3_665 1_545 ? O5 Na4 S3 112.46(10) 3_665 1_545 ? O10 Na4 S3 25.49(8) 1_445 1_545 ? O11 Na4 S3 25.82(6) 1_545 1_545 ? O16 Na4 S3 78.81(9) . 1_545 ? S4 Na4 S3 103.39(7) . 1_545 ? O11 Na4 Zn2 123.71(11) 3_665 1_445 ? O7 Na4 Zn2 55.50(9) 1_445 1_445 ? O13 Na4 Zn2 150.69(10) 3_665 1_445 ? O5 Na4 Zn2 68.81(8) 3_665 1_445 ? O10 Na4 Zn2 34.15(8) 1_445 1_445 ? O11 Na4 Zn2 79.57(8) 1_545 1_445 ? O16 Na4 Zn2 105.67(8) . 1_445 ? S4 Na4 Zn2 128.79(6) . 1_445 ? S3 Na4 Zn2 55.78(4) 1_545 1_445 ? O11 Na4 Na1 148.67(13) 3_665 . ? O7 Na4 Na1 46.37(9) 1_445 . ? O13 Na4 Na1 88.84(10) 3_665 . ? O5 Na4 Na1 124.96(10) 3_665 . ? O10 Na4 Na1 48.38(9) 1_445 . ? O11 Na4 Na1 78.77(9) 1_545 . ? O16 Na4 Na1 41.25(7) . . ? S4 Na4 Na1 64.20(6) . . ? S3 Na4 Na1 61.55(6) 1_545 . ? Zn2 Na4 Na1 65.01(5) 1_445 . ? O11 Na4 Zn1 63.67(10) 3_665 3_665 ? O7 Na4 Zn1 112.27(11) 1_445 3_665 ? O13 Na4 Zn1 31.12(8) 3_665 3_665 ? O5 Na4 Zn1 96.58(10) 3_665 3_665 ? O10 Na4 Zn1 162.47(11) 1_445 3_665 ? O11 Na4 Zn1 119.19(9) 1_545 3_665 ? O16 Na4 Zn1 82.84(8) . 3_665 ? S4 Na4 Zn1 56.65(4) . 3_665 ? S3 Na4 Zn1 143.28(7) 1_545 3_665 ? Zn2 Na4 Zn1 160.94(7) 1_445 3_665 ? Na1 Na4 Zn1 119.18(7) . 3_665 ? O12 Na5 O12 136.9(2) 2_655 . ? O12 Na5 O6 91.29(12) 2_655 2_655 ? O12 Na5 O6 122.53(13) . 2_655 ? O12 Na5 O6 122.53(13) 2_655 . ? O12 Na5 O6 91.29(12) . . ? O6 Na5 O6 80.52(17) 2_655 . ? O12 Na5 O5 63.84(10) 2_655 2_655 ? O12 Na5 O5 112.80(11) . 2_655 ? O6 Na5 O5 53.92(10) 2_655 2_655 ? O6 Na5 O5 134.42(14) . 2_655 ? O12 Na5 O5 112.80(11) 2_655 . ? O12 Na5 O5 63.84(10) . . ? O6 Na5 O5 134.42(14) 2_655 . ? O6 Na5 O5 53.92(10) . . ? O5 Na5 O5 171.66(17) 2_655 . ? O12 Na5 S2 73.53(8) 2_655 2_655 ? O12 Na5 S2 125.81(8) . 2_655 ? O6 Na5 S2 25.84(7) 2_655 2_655 ? O6 Na5 S2 105.86(12) . 2_655 ? O5 Na5 S2 28.72(7) 2_655 2_655 ? O5 Na5 S2 159.50(13) . 2_655 ? O12 Na5 S2 125.81(8) 2_655 . ? O12 Na5 S2 73.53(8) . . ? O6 Na5 S2 105.86(12) 2_655 . ? O6 Na5 S2 25.84(7) . . ? O5 Na5 S2 159.50(13) 2_655 . ? O5 Na5 S2 28.72(7) . . ? S2 Na5 S2 131.51(11) 2_655 . ? O12 Na5 S3 23.95(8) 2_655 . ? O12 Na5 S3 130.21(13) . . ? O6 Na5 S3 106.44(9) 2_655 . ? O6 Na5 S3 105.95(9) . . ? O5 Na5 S3 87.78(7) 2_655 . ? O5 Na5 S3 89.18(8) . . ? S2 Na5 S3 94.34(3) 2_655 . ? S2 Na5 S3 102.98(3) . . ? O12 Na5 S3 130.21(13) 2_655 2_655 ? O12 Na5 S3 23.95(8) . 2_655 ? O6 Na5 S3 105.95(9) 2_655 2_655 ? O6 Na5 S3 106.44(9) . 2_655 ? O5 Na5 S3 89.18(8) 2_655 2_655 ? O5 Na5 S3 87.78(7) . 2_655 ? S2 Na5 S3 102.98(3) 2_655 2_655 ? S2 Na5 S3 94.34(3) . 2_655 ? S3 Na5 S3 137.13(11) . 2_655 ? O12 Na5 Na6 111.54(11) 2_655 1_565 ? O12 Na5 Na6 111.54(11) . 1_565 ? O6 Na5 Na6 40.26(9) 2_655 1_565 ? O6 Na5 Na6 40.26(9) . 1_565 ? O5 Na5 Na6 94.17(9) 2_655 1_565 ? O5 Na5 Na6 94.17(9) . 1_565 ? S2 Na5 Na6 65.75(5) 2_655 1_565 ? S2 Na5 Na6 65.75(5) . 1_565 ? S3 Na5 Na6 111.43(5) . 1_565 ? S3 Na5 Na6 111.43(5) 2_655 1_565 ? O12 Na5 Zn2 33.05(8) 2_655 2_655 ? O12 Na5 Zn2 124.78(12) . 2_655 ? O6 Na5 Zn2 75.65(7) 2_655 2_655 ? O6 Na5 Zn2 143.56(10) . 2_655 ? O5 Na5 Zn2 32.08(7) 2_655 2_655 ? O5 Na5 Zn2 142.59(10) . 2_655 ? S2 Na5 Zn2 51.09(3) 2_655 2_655 ? S2 Na5 Zn2 158.08(3) . 2_655 ? S3 Na5 Zn2 56.72(3) . 2_655 ? S3 Na5 Zn2 106.39(6) 2_655 2_655 ? Na6 Na5 Zn2 111.39(4) 1_565 2_655 ? O6 Na6 O6 83.77(19) 2_645 1_545 ? O6 Na6 O2 142.82(11) 2_645 2_655 ? O6 Na6 O2 113.34(11) 1_545 2_655 ? O6 Na6 O2 113.34(11) 2_645 . ? O6 Na6 O2 142.82(11) 1_545 . ? O2 Na6 O2 73.52(16) 2_655 . ? O6 Na6 O14 81.90(11) 2_645 2_655 ? O6 Na6 O14 125.55(12) 1_545 2_655 ? O2 Na6 O14 61.15(10) 2_655 2_655 ? O2 Na6 O14 90.49(12) . 2_655 ? O6 Na6 O14 125.55(12) 2_645 . ? O6 Na6 O14 81.90(11) 1_545 . ? O2 Na6 O14 90.49(12) 2_655 . ? O2 Na6 O14 61.15(10) . . ? O14 Na6 O14 145.59(17) 2_655 . ? O6 Na6 Na5 41.89(10) 2_645 1_545 ? O6 Na6 Na5 41.89(10) 1_545 1_545 ? O2 Na6 Na5 143.24(8) 2_655 1_545 ? O2 Na6 Na5 143.24(8) . 1_545 ? O14 Na6 Na5 107.21(9) 2_655 1_545 ? O14 Na6 Na5 107.21(9) . 1_545 ? O6 Na6 Na2 58.31(9) 2_645 2_655 ? O6 Na6 Na2 136.17(12) 1_545 2_655 ? O2 Na6 Na2 90.11(8) 2_655 2_655 ? O2 Na6 Na2 77.70(8) . 2_655 ? O14 Na6 Na2 36.26(7) 2_655 2_655 ? O14 Na6 Na2 136.75(9) . 2_655 ? Na5 Na6 Na2 97.57(5) 1_545 2_655 ? O6 Na6 Na2 136.17(12) 2_645 . ? O6 Na6 Na2 58.31(9) 1_545 . ? O2 Na6 Na2 77.70(8) 2_655 . ? O2 Na6 Na2 90.11(8) . . ? O14 Na6 Na2 136.75(9) 2_655 . ? O14 Na6 Na2 36.26(7) . . ? Na5 Na6 Na2 97.57(5) 1_545 . ? Na2 Na6 Na2 164.86(10) 2_655 . ? S1 O1 Zn1 118.47(19) . . ? S1 O2 Zn1 132.50(19) 2_655 . ? S1 O2 Na6 113.16(18) 2_655 . ? Zn1 O2 Na6 102.85(11) . . ? S1 O2 Na3 87.51(14) 2_655 1_455 ? Zn1 O2 Na3 89.13(11) . 1_455 ? Na6 O2 Na3 133.89(14) . 1_455 ? S1 O3 Na2 149.5(2) . . ? S1 O3 Na2 94.62(17) . 3_765 ? Na2 O3 Na2 107.69(13) . 3_765 ? S1 O4 Zn2 124.30(18) . . ? S1 O4 Na3 104.41(16) . . ? Zn2 O4 Na3 124.85(16) . . ? S1 O4 Na2 103.04(16) . 3_765 ? Zn2 O4 Na2 98.57(12) . 3_765 ? Na3 O4 Na2 93.49(11) . 3_765 ? S2 O5 Zn2 116.88(19) . . ? S2 O5 Na4 119.48(18) . 3_665 ? Zn2 O5 Na4 119.38(14) . 3_665 ? S2 O5 Na5 87.26(15) . . ? Zn2 O5 Na5 98.22(12) . . ? Na4 O5 Na5 104.83(12) 3_665 . ? S2 O6 Na6 151.6(2) . 1_565 ? S2 O6 Na5 108.22(18) . . ? Na6 O6 Na5 97.85(13) 1_565 . ? S2 O7 Na4 130.6(2) . 1_665 ? S2 O7 Na1 131.20(19) . 1_665 ? Na4 O7 Na1 92.33(13) 1_665 1_665 ? S2 O8 Zn2 130.0(2) 3_775 . ? S2 O8 Na2 121.70(19) 3_775 3_765 ? Zn2 O8 Na2 103.56(14) . 3_765 ? S3 O9 Zn1 125.58(19) . . ? S3 O9 Na3 129.68(17) . 1_455 ? Zn1 O9 Na3 94.51(12) . 1_455 ? S3 O10 Zn2 132.3(2) 1_655 . ? S3 O10 Na4 106.32(18) 1_655 1_665 ? Zn2 O10 Na4 100.15(15) . 1_665 ? S3 O10 Na1 112.58(18) 1_655 1_665 ? Zn2 O10 Na1 107.98(14) . 1_665 ? Na4 O10 Na1 86.50(12) 1_665 1_665 ? S3 O11 Na4 145.9(2) . 3_665 ? S3 O11 Na4 92.50(17) . 1_565 ? Na4 O11 Na4 105.79(14) 3_665 1_565 ? S3 O12 Zn2 134.0(2) 2_655 . ? S3 O12 Na5 115.13(18) 2_655 . ? Zn2 O12 Na5 109.61(14) . . ? S4 O13 Zn1 137.1(2) 3_665 . ? S4 O13 Na4 110.36(18) 3_665 3_665 ? Zn1 O13 Na4 112.43(14) . 3_665 ? S4 O14 Zn1 107.96(18) . . ? S4 O14 Na2 130.70(19) . . ? Zn1 O14 Na2 108.14(14) . . ? S4 O14 Na6 107.05(16) . . ? Zn1 O14 Na6 97.37(13) . . ? Na2 O14 Na6 100.37(12) . . ? S4 O15 Na2 125.49(19) . 3_665 ? S4 O15 Na3 134.8(2) . 1_455 ? Na2 O15 Na3 99.71(13) 3_665 1_455 ? S4 O16 Na1 142.6(2) . . ? S4 O16 Na4 87.65(16) . . ? Na1 O16 Na4 84.52(12) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O9 2.005(3) . ? Zn1 O1 2.019(3) . ? Zn1 O14 2.047(3) . ? Zn1 O13 2.063(3) . ? Zn1 O2 2.147(3) . ? Zn1 Na3 3.5126(10) 1_455 ? Zn1 Na2 3.636(2) . ? Zn1 Na4 3.690(2) 3_665 ? Zn2 O5 1.966(3) . ? Zn2 O4 1.989(3) . ? Zn2 O10 1.992(3) . ? Zn2 O8 2.075(3) . ? Zn2 O12 2.121(3) . ? Zn2 Na2 3.451(2) 3_765 ? Zn2 Na4 3.492(2) 1_665 ? Zn2 Na5 3.6634(14) . ? S1 O3 1.434(3) . ? S1 O1 1.471(3) . ? S1 O2 1.473(3) 2_655 ? S1 O4 1.479(3) . ? S1 Na3 3.1179(14) . ? S1 Na2 3.213(2) 3_765 ? S2 O6 1.439(3) . ? S2 O7 1.442(3) . ? S2 O8 1.480(3) 3_775 ? S2 O5 1.509(3) . ? S2 Na5 3.1365(18) . ? S2 Na2 3.338(2) 1_565 ? S3 O11 1.425(3) . ? S3 O12 1.462(3) 2_655 ? S3 O10 1.466(3) 1_455 ? S3 O9 1.481(3) . ? S3 Na5 3.2605(18) . ? S3 Na4 3.269(2) 1_565 ? S4 O16 1.431(3) . ? S4 O15 1.456(3) . ? S4 O13 1.469(3) 3_665 ? S4 O14 1.495(3) . ? S4 Na4 3.195(2) . ? S4 Na2 3.370(2) 3_665 ? Na1 O16 2.369(3) 2 ? Na1 O16 2.369(3) . ? Na1 O7 2.591(4) 2_645 ? Na1 O7 2.591(4) 1_445 ? Na1 O10 2.679(4) 2_645 ? Na1 O10 2.679(4) 1_445 ? Na1 Na4 3.577(2) 2 ? Na1 Na4 3.577(2) . ? Na2 O3 2.222(4) . ? Na2 O15 2.309(4) 3_665 ? Na2 O8 2.314(4) 3_765 ? Na2 O14 2.435(4) . ? Na2 O4 2.539(3) 3_765 ? Na2 O3 2.762(4) 3_765 ? Na2 S1 3.213(2) 3_765 ? Na2 S2 3.338(2) 1_545 ? Na2 S4 3.370(2) 3_665 ? Na2 Zn2 3.451(2) 3_765 ? Na2 Na3 3.599(2) 3_765 ? Na3 O15 2.399(3) 2_655 ? Na3 O15 2.399(3) 1_655 ? Na3 O4 2.402(3) 2_755 ? Na3 O4 2.402(3) . ? Na3 O9 2.731(4) 2_655 ? Na3 O9 2.731(4) 1_655 ? Na3 O2 2.813(3) 2_655 ? Na3 O2 2.813(3) 1_655 ? Na3 S1 3.1179(14) 2_755 ? Na3 Zn1 3.5126(10) 2_655 ? Na3 Zn1 3.5127(10) 1_655 ? Na4 O11 2.247(4) 3_665 ? Na4 O7 2.363(4) 1_445 ? Na4 O13 2.371(4) 3_665 ? Na4 O5 2.507(4) 3_665 ? Na4 O10 2.539(4) 1_445 ? Na4 O11 2.881(4) 1_545 ? Na4 O16 2.915(4) . ? Na4 S3 3.269(2) 1_545 ? Na4 Zn2 3.492(2) 1_445 ? Na4 Zn1 3.690(2) 3_665 ? Na5 O12 2.359(4) 2_655 ? Na5 O12 2.359(4) . ? Na5 O6 2.373(4) 2_655 ? Na5 O6 2.373(4) . ? Na5 O5 2.823(3) 2_655 ? Na5 O5 2.823(3) . ? Na5 S2 3.1365(18) 2_655 ? Na5 S3 3.2605(17) 2_655 ? Na5 Na6 3.520(4) 1_565 ? Na5 Zn2 3.6634(14) 2_655 ? Na6 O6 2.297(4) 2_645 ? Na6 O6 2.297(4) 1_545 ? Na6 O2 2.569(4) 2_655 ? Na6 O2 2.569(4) . ? Na6 O14 2.826(4) 2_655 ? Na6 O14 2.826(4) . ? Na6 Na5 3.520(4) 1_545 ? Na6 Na2 4.049(2) 2_655 ? O2 S1 1.473(3) 2_655 ? O2 Na3 2.813(3) 1_455 ? O3 Na2 2.762(4) 3_765 ? O4 Na2 2.539(3) 3_765 ? O5 Na4 2.507(4) 3_665 ? O6 Na6 2.297(4) 1_565 ? O7 Na4 2.363(4) 1_665 ? O7 Na1 2.591(4) 1_665 ? O8 S2 1.480(3) 3_775 ? O8 Na2 2.314(4) 3_765 ? O9 Na3 2.731(4) 1_455 ? O10 S3 1.466(3) 1_655 ? O10 Na4 2.539(4) 1_665 ? O10 Na1 2.679(4) 1_665 ? O11 Na4 2.247(4) 3_665 ? O11 Na4 2.881(4) 1_565 ? O12 S3 1.462(3) 2_655 ? O13 S4 1.469(3) 3_665 ? O13 Na4 2.371(4) 3_665 ? O15 Na2 2.309(4) 3_665 ? O15 Na3 2.399(3) 1_455 ?
1100778.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100778.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100778 loop_ _publ_author_name 'Rolf W. Berg' 'Niels Thorup' _publ_contact_author_address ; Department of Chemistry Technical University of Denmark DTU-207 DK-2800 Lyngby Denmark ; _publ_contact_author_email rwb@kemi.dtu.dk _publ_contact_author_fax '+45 4588 3136' _publ_contact_author_name 'Rolf W. Berg' _publ_contact_author_phone '+45 4525 2412' _publ_section_title ; The Reaction between ZnO and Molten Na2S2O7 or K2S2O7 Forming Na2Zn(SO4)2 or K2Zn(SO4)2, Studied by Raman Spectroscopy and X-ray Diffraction ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3485 _journal_page_last 3493 _journal_paper_doi 10.1021/ic0500513 _journal_volume 44 _journal_year 2005 _chemical_formula_moiety 'K2 O8 S2 Zn' _chemical_formula_sum 'K2 O8 S2 Zn' _chemical_formula_weight 335.69 _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method 'manual editing of SHELXL-97 cif' _cell_angle_alpha 90.00 _cell_angle_beta 91.78(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 5.3582(11) _cell_length_b 8.7653(18) _cell_length_c 16.152(3) _cell_measurement_temperature 293(2) _cell_volume 758.2(3) _computing_cell_refinement 'SAINT ver 6.02a (Bruker AXS, 2000)' _computing_data_collection 'SMART ver 5.054 (Bruker AXS, 1998)' _computing_data_reduction 'SAINT ver 6.02a (Bruker AXS, 2000)' _computing_molecular_graphics 'SHELXTL ver 6.12 (Bruker AXS, 2001)' _computing_publication_material 'SHELXTL ver 6.12 (Bruker AXS, 2001)' _computing_structure_refinement 'SHELXTL ver 6.12 (Bruker AXS, 2001)' _computing_structure_solution 'SHELXTL ver 6.12 (Bruker AXS, 2001)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.905 _diffrn_measured_fraction_theta_max 0.905 _diffrn_measurement_device_type 'Siemens/Bruker SMART 1K' _diffrn_measurement_method 'omega scan, frame data integration' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0389 _diffrn_reflns_av_sigmaI/netI 0.0508 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 5068 _diffrn_reflns_theta_full 29.56 _diffrn_reflns_theta_max 29.56 _diffrn_reflns_theta_min 2.52 _exptl_absorpt_coefficient_mu 4.898 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Sheldrick, 2000)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.941 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 656 _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.01 _refine_diff_density_max 0.646 _refine_diff_density_min -0.799 _refine_diff_density_rms 0.158 _refine_ls_extinction_coef 0.0092(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 119 _refine_ls_number_reflns 1930 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.039 _refine_ls_R_factor_all 0.0526 _refine_ls_R_factor_gt 0.0351 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0342P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0694 _refine_ls_wR_factor_ref 0.0758 _reflns_number_gt 1538 _reflns_number_total 1930 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic0500513si20050113_124143_2.cif _cod_data_source_block ks _cod_database_code 1100778 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.24459(7) 0.52820(5) 0.63046(2) 0.01091(13) Uani 1 1 d . . . K1 K 0.26381(16) 0.17285(10) 0.47760(5) 0.01795(19) Uani 1 1 d . . . S1 S 0.26453(16) 0.88425(10) 0.67672(5) 0.01138(19) Uani 1 1 d . . . K2 K 0.73457(15) 1.14449(9) 0.72887(5) 0.01736(19) Uani 1 1 d . . . S2 S 0.75457(16) 0.39075(10) 0.57224(5) 0.01105(19) Uani 1 1 d . . . O5 O 0.3317(5) 0.6180(3) 0.51531(15) 0.0175(6) Uani 1 1 d . . . O6 O 0.5304(5) 0.3788(3) 0.62523(15) 0.0154(5) Uani 1 1 d . . . O7 O -0.1213(5) 0.5398(3) 0.58997(16) 0.0166(5) Uani 1 1 d . . . O8 O -0.0718(5) 0.2670(3) 0.59260(16) 0.0209(6) Uani 1 1 d . . . O1 O 0.3573(5) 0.9538(3) 0.75544(15) 0.0202(6) Uani 1 1 d . . . O2 O 0.3656(5) 0.9699(3) 0.60784(16) 0.0230(6) Uani 1 1 d . . . O3 O 0.3688(5) 0.7262(3) 0.67683(17) 0.0222(6) Uani 1 1 d . . . O4 O -0.0075(5) 0.8786(3) 0.67242(17) 0.0215(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0095(2) 0.0123(2) 0.0110(2) -0.00021(16) 0.00173(15) 0.00104(16) K1 0.0177(4) 0.0193(4) 0.0170(4) 0.0009(3) 0.0030(3) 0.0026(3) S1 0.0135(4) 0.0105(4) 0.0103(4) -0.0010(3) 0.0021(3) -0.0003(3) K2 0.0172(4) 0.0181(4) 0.0168(4) 0.0013(3) 0.0017(3) -0.0036(3) S2 0.0083(4) 0.0136(4) 0.0114(4) 0.0017(3) 0.0036(3) 0.0011(3) O5 0.0186(14) 0.0242(14) 0.0097(12) 0.0003(10) 0.0007(10) -0.0023(11) O6 0.0126(13) 0.0170(13) 0.0170(13) 0.0045(10) 0.0078(10) 0.0027(10) O7 0.0132(12) 0.0159(13) 0.0207(13) 0.0008(11) -0.0003(10) -0.0037(11) O8 0.0190(14) 0.0230(15) 0.0213(14) 0.0059(11) 0.0085(11) 0.0113(12) O1 0.0200(14) 0.0269(15) 0.0141(13) -0.0101(11) 0.0060(11) -0.0092(12) O2 0.0291(16) 0.0213(15) 0.0191(14) 0.0075(11) 0.0099(12) 0.0027(12) O3 0.0279(16) 0.0129(14) 0.0253(15) -0.0033(11) -0.0078(12) 0.0037(11) O4 0.0140(14) 0.0269(15) 0.0236(14) -0.0036(12) 0.0003(11) 0.0005(11) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Zn1 O6 109.59(11) . . ? O3 Zn1 O1 91.97(12) . 2_546 ? O6 Zn1 O1 93.16(10) . 2_546 ? O3 Zn1 O7 112.39(11) . . ? O6 Zn1 O7 137.57(11) . . ? O1 Zn1 O7 91.37(11) 2_546 . ? O3 Zn1 O5 85.70(11) . . ? O6 Zn1 O5 90.94(10) . . ? O1 Zn1 O5 175.78(11) 2_546 . ? O7 Zn1 O5 86.27(10) . . ? O3 Zn1 K2 75.81(8) . 2_546 ? O6 Zn1 K2 139.57(7) . 2_546 ? O1 Zn1 K2 46.46(8) 2_546 2_546 ? O7 Zn1 K2 59.82(7) . 2_546 ? O5 Zn1 K2 129.40(8) . 2_546 ? O3 Zn1 K2 44.88(8) . 2_646 ? O6 Zn1 K2 69.17(8) . 2_646 ? O1 Zn1 K2 75.58(9) 2_546 2_646 ? O7 Zn1 K2 151.76(8) . 2_646 ? O5 Zn1 K2 105.01(8) . 2_646 ? K2 Zn1 K2 94.20(3) 2_546 2_646 ? O3 Zn1 K1 154.01(8) . . ? O6 Zn1 K1 55.38(8) . . ? O1 Zn1 K1 108.81(9) 2_546 . ? O7 Zn1 K1 83.32(8) . . ? O5 Zn1 K1 74.41(8) . . ? K2 Zn1 K1 129.89(2) 2_546 . ? K2 Zn1 K1 124.42(2) 2_646 . ? O8 K1 O2 166.18(8) . 3_666 ? O8 K1 O4 108.72(9) . 3_566 ? O2 K1 O4 80.45(9) 3_666 3_566 ? O8 K1 O2 78.42(8) . 1_545 ? O2 K1 O2 87.77(8) 3_666 1_545 ? O4 K1 O2 129.14(9) 3_566 1_545 ? O8 K1 O5 107.06(9) . 3_666 ? O2 K1 O5 75.64(9) 3_666 3_666 ? O4 K1 O5 119.67(8) 3_566 3_666 ? O2 K1 O5 104.46(9) 1_545 3_666 ? O8 K1 O7 79.62(8) . 3_566 ? O2 K1 O7 113.57(8) 3_666 3_566 ? O4 K1 O7 71.92(8) 3_566 3_566 ? O2 K1 O7 153.80(8) 1_545 3_566 ? O5 K1 O7 68.82(8) 3_666 3_566 ? O8 K1 O6 67.88(8) . . ? O2 K1 O6 108.04(8) 3_666 . ? O4 K1 O6 155.91(8) 3_566 . ? O2 K1 O6 74.52(8) 1_545 . ? O5 K1 O6 45.65(7) 3_666 . ? O7 K1 O6 84.09(7) 3_566 . ? O8 K1 O3 146.75(8) . 3_666 ? O2 K1 O3 45.25(7) 3_666 3_666 ? O4 K1 O3 71.31(8) 3_566 3_666 ? O2 K1 O3 128.59(8) 1_545 3_666 ? O5 K1 O3 52.61(7) 3_666 3_666 ? O7 K1 O3 68.68(7) 3_566 3_666 ? O6 K1 O3 98.25(7) . 3_666 ? O8 K1 S2 92.22(7) . . ? O2 K1 S2 85.66(7) 3_666 . ? O4 K1 S2 143.03(7) 3_566 . ? O2 K1 S2 83.91(7) 1_545 . ? O5 K1 S2 23.41(5) 3_666 . ? O7 K1 S2 82.84(6) 3_566 . ? O6 K1 S2 24.93(4) . . ? O3 K1 S2 74.58(5) 3_666 . ? O8 K1 S1 170.38(7) . 3_666 ? O2 K1 S1 21.14(6) 3_666 3_666 ? O4 K1 S1 73.49(6) 3_566 3_666 ? O2 K1 S1 107.72(6) 1_545 3_666 ? O5 K1 S1 64.58(6) 3_666 3_666 ? O7 K1 S1 92.46(6) 3_566 3_666 ? O6 K1 S1 106.11(5) . 3_666 ? O3 K1 S1 24.22(5) 3_666 3_666 ? S2 K1 S1 81.28(3) . 3_666 ? O8 K1 S2 20.04(6) . 1_455 ? O2 K1 S2 173.79(6) 3_666 1_455 ? O4 K1 S2 95.34(6) 3_566 1_455 ? O2 K1 S2 98.44(6) 1_545 1_455 ? O5 K1 S2 102.83(6) 3_666 1_455 ? O7 K1 S2 60.53(5) 3_566 1_455 ? O6 K1 S2 74.08(5) . 1_455 ? O3 K1 S2 129.08(6) 3_666 1_455 ? S2 K1 S2 95.17(3) . 1_455 ? S1 K1 S2 152.97(3) 3_666 1_455 ? O8 K1 S1 89.60(7) . 3_566 ? O2 K1 S1 98.49(7) 3_666 3_566 ? O4 K1 S1 19.53(6) 3_566 3_566 ? O2 K1 S1 122.77(7) 1_545 3_566 ? O5 K1 S1 132.33(6) 3_666 3_566 ? O7 K1 S1 70.99(6) 3_566 3_566 ? O6 K1 S1 149.26(5) . 3_566 ? O3 K1 S1 89.39(5) 3_666 3_566 ? S2 K1 S1 152.99(3) . 3_566 ? S1 K1 S1 93.01(3) 3_666 3_566 ? S2 K1 S1 78.00(3) 1_455 3_566 ? O4 S1 O2 112.05(17) . . ? O4 S1 O1 111.29(16) . . ? O2 S1 O1 108.64(17) . . ? O4 S1 O3 109.98(17) . . ? O2 S1 O3 109.27(16) . . ? O1 S1 O3 105.37(17) . . ? O4 S1 K2 138.46(12) . . ? O2 S1 K2 64.20(13) . . ? O1 S1 K2 45.74(10) . . ? O3 S1 K2 109.85(12) . . ? O4 S1 K1 132.63(12) . 3_666 ? O1 S1 K1 115.01(11) . 3_666 ? O3 S1 K1 66.77(11) . 3_666 ? K2 S1 K1 75.12(3) . 3_666 ? O4 S1 K2 135.36(12) . 2_646 ? O2 S1 K2 108.93(12) . 2_646 ? O1 S1 K2 70.15(12) . 2_646 ? K2 S1 K2 76.26(3) . 2_646 ? K1 S1 K2 72.17(3) 3_666 2_646 ? O2 S1 K1 81.51(13) . 3_566 ? O1 S1 K1 148.43(12) . 3_566 ? O3 S1 K1 98.73(11) . 3_566 ? K2 S1 K1 140.74(3) . 3_566 ? K1 S1 K1 93.01(3) 3_666 3_566 ? K2 S1 K1 136.19(3) 2_646 3_566 ? O2 S1 K2 99.18(12) . 1_455 ? O1 S1 K2 78.09(12) . 1_455 ? O3 S1 K2 147.97(12) . 1_455 ? K2 S1 K2 95.40(3) . 1_455 ? K1 S1 K2 141.51(3) 3_666 1_455 ? K2 S1 K2 142.73(3) 2_646 1_455 ? K1 S1 K2 70.71(3) 3_566 1_455 ? O2 S1 K2 151.82(13) . 2_546 ? O1 S1 K2 96.07(11) . 2_546 ? O3 S1 K2 75.64(12) . 2_546 ? K2 S1 K2 141.81(3) . 2_546 ? K1 S1 K2 135.93(3) 3_666 2_546 ? K2 S1 K2 91.80(3) 2_646 2_546 ? K1 S1 K2 70.31(3) 3_566 2_546 ? K2 S1 K2 72.34(2) 1_455 2_546 ? O1 K2 O3 132.00(9) . 2_656 ? O1 K2 O8 134.11(9) . 1_665 ? O3 K2 O8 92.24(9) 2_656 1_665 ? O1 K2 O6 105.50(9) . 1_565 ? O3 K2 O6 115.19(9) 2_656 1_565 ? O8 K2 O6 51.75(7) 1_665 1_565 ? O1 K2 O4 85.25(8) . 1_655 ? O3 K2 O4 90.95(9) 2_656 1_655 ? O8 K2 O4 82.09(8) 1_665 1_655 ? O6 K2 O4 125.35(8) 1_565 1_655 ? O1 K2 O4 91.26(8) . 2_556 ? O3 K2 O4 80.58(8) 2_656 2_556 ? O8 K2 O4 110.38(8) 1_665 2_556 ? O6 K2 O4 69.60(8) 1_565 2_556 ? O4 K2 O4 165.03(5) 1_655 2_556 ? O1 K2 O2 47.80(7) . . ? O3 K2 O2 163.85(9) 2_656 . ? O8 K2 O2 86.35(8) 1_665 . ? O6 K2 O2 76.25(8) 1_565 . ? O4 K2 O2 72.91(8) 1_655 . ? O4 K2 O2 114.99(8) 2_556 . ? O1 K2 O7 59.88(8) . 2_556 ? O3 K2 O7 73.81(8) 2_656 2_556 ? O8 K2 O7 165.93(9) 1_665 2_556 ? O6 K2 O7 132.54(7) 1_565 2_556 ? O4 K2 O7 99.63(8) 1_655 2_556 ? O4 K2 O7 66.23(7) 2_556 2_556 ? O2 K2 O7 107.55(7) . 2_556 ? O1 K2 S2 124.80(7) . 1_565 ? O3 K2 S2 102.43(7) 2_656 1_565 ? O8 K2 S2 25.31(6) 1_665 1_565 ? O6 K2 S2 26.67(5) 1_565 1_565 ? O4 K2 S2 104.93(6) 1_655 1_565 ? O4 K2 S2 89.02(6) 2_556 1_565 ? O2 K2 S2 82.95(6) . 1_565 ? O7 K2 S2 155.24(6) 2_556 1_565 ? O1 K2 S1 23.44(5) . . ? O3 K2 S1 150.41(7) 2_656 . ? O8 K2 S1 111.01(7) 1_665 . ? O6 K2 S1 93.93(6) 1_565 . ? O4 K2 S1 75.11(6) 1_655 . ? O4 K2 S1 106.55(6) 2_556 . ? O2 K2 S1 24.79(5) . . ? O7 K2 S1 82.80(6) 2_556 . ? S2 K2 S1 106.32(4) 1_565 . ? O1 K2 Zn1 33.75(5) . 2_556 ? O3 K2 Zn1 106.51(7) 2_656 2_556 ? O8 K2 Zn1 157.60(7) 1_665 2_556 ? O6 K2 Zn1 107.73(5) 1_565 2_556 ? O4 K2 Zn1 109.13(6) 1_655 2_556 ? O4 K2 Zn1 62.33(6) 2_556 2_556 ? O2 K2 Zn1 78.96(5) . 2_556 ? O7 K2 Zn1 34.31(5) 2_556 2_556 ? S2 K2 Zn1 134.28(3) 1_565 2_556 ? S1 K2 Zn1 56.40(2) . 2_556 ? O1 K2 Zn1 106.89(7) . 2_656 ? O3 K2 Zn1 31.80(6) 2_656 2_656 ? O8 K2 Zn1 108.13(7) 1_665 2_656 ? O6 K2 Zn1 146.25(6) 1_565 2_656 ? O4 K2 Zn1 66.98(6) 1_655 2_656 ? O4 K2 Zn1 100.36(6) 2_556 2_656 ? O2 K2 Zn1 134.40(6) . 2_656 ? O7 K2 Zn1 60.67(5) 2_556 2_656 ? S2 K2 Zn1 127.28(3) 1_565 2_656 ? S1 K2 Zn1 119.73(3) . 2_656 ? Zn1 K2 Zn1 94.20(3) 2_556 2_656 ? O8 S2 O5 110.82(16) 1_655 3_666 ? O8 S2 O7 109.31(17) 1_655 1_655 ? O5 S2 O7 110.76(15) 3_666 1_655 ? O8 S2 O6 109.62(15) 1_655 . ? O5 S2 O6 108.09(15) 3_666 . ? O7 S2 O6 108.19(15) 1_655 . ? O8 S2 K2 51.87(10) 1_655 1_545 ? O5 S2 K2 132.66(12) 3_666 1_545 ? O7 S2 K2 116.56(11) 1_655 1_545 ? O6 S2 K2 58.41(10) . 1_545 ? O8 S2 K1 98.93(13) 1_655 . ? O5 S2 K1 49.83(11) 3_666 . ? O7 S2 K1 150.84(11) 1_655 . ? O6 S2 K1 67.25(11) . . ? K2 S2 K1 86.42(3) 1_545 . ? O5 S2 K1 77.89(11) 3_666 1_655 ? O7 S2 K1 101.62(10) 1_655 1_655 ? O6 S2 K1 144.46(11) . 1_655 ? K2 S2 K1 91.20(3) 1_545 1_655 ? K1 S2 K1 95.17(3) . 1_655 ? S2 O5 Zn1 139.69(17) 3_666 . ? S2 O5 K1 106.75(13) 3_666 3_666 ? Zn1 O5 K1 113.55(11) . 3_666 ? S2 O6 Zn1 126.92(15) . . ? S2 O6 K2 94.92(12) . 1_545 ? Zn1 O6 K2 136.18(11) . 1_545 ? S2 O6 K1 87.82(11) . . ? Zn1 O6 K1 94.22(9) . . ? K2 O6 K1 100.42(8) 1_545 . ? S2 O7 Zn1 115.78(16) 1_455 . ? S2 O7 K1 126.21(14) 1_455 3_566 ? Zn1 O7 K1 114.18(11) . 3_566 ? S2 O7 K2 109.69(12) 1_455 2_546 ? Zn1 O7 K2 85.87(9) . 2_546 ? K1 O7 K2 92.37(8) 3_566 2_546 ? S2 O8 K2 102.82(12) 1_455 1_445 ? S2 O8 K1 119.74(14) 1_455 . ? K2 O8 K1 135.27(11) 1_445 . ? S1 O1 Zn1 144.34(17) . 2_556 ? S1 O1 K2 110.82(13) . . ? Zn1 O1 K2 99.79(10) 2_556 . ? S1 O2 K1 116.02(15) . 3_666 ? S1 O2 K1 146.31(17) . 1_565 ? K1 O2 K1 92.23(8) 3_666 1_565 ? S1 O2 K2 91.01(13) . . ? K1 O2 K2 94.81(9) 3_666 . ? K1 O2 K2 105.25(9) 1_565 . ? S1 O3 Zn1 133.29(18) . . ? S1 O3 K2 122.68(15) . 2_646 ? Zn1 O3 K2 103.32(11) . 2_646 ? S1 O3 K1 89.01(12) . 3_666 ? Zn1 O3 K1 98.46(10) . 3_666 ? K2 O3 K1 91.13(8) 2_646 3_666 ? S1 O4 K1 120.81(15) . 3_566 ? S1 O4 K2 116.56(15) . 1_455 ? K1 O4 K2 100.28(9) 3_566 1_455 ? S1 O4 K2 115.81(15) . 2_546 ? K1 O4 K2 99.24(9) 3_566 2_546 ? K2 O4 K2 100.72(8) 1_455 2_546 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O3 1.997(3) . ? Zn1 O6 2.018(3) . ? Zn1 O1 2.045(2) 2_546 ? Zn1 O7 2.050(3) . ? Zn1 O5 2.086(3) . ? Zn1 K2 3.6270(13) 2_546 ? Zn1 K2 3.6871(14) 2_646 ? Zn1 K1 3.9779(11) . ? K1 O8 2.752(3) . ? K1 O2 2.754(3) 3_666 ? K1 O4 2.784(3) 3_566 ? K1 O2 2.796(3) 1_545 ? K1 O5 2.838(3) 3_666 ? K1 O7 2.840(3) 3_566 ? K1 O6 3.282(3) . ? K1 O3 3.345(3) 3_666 ? K1 S2 3.5565(15) . ? K1 S1 3.6390(15) 3_666 ? K1 S2 3.6999(14) 1_455 ? K1 S1 3.7468(17) 3_566 ? S1 O4 1.458(3) . ? S1 O2 1.460(3) . ? S1 O1 1.482(3) . ? S1 O3 1.493(3) . ? S1 K2 3.4820(13) . ? S1 K1 3.6390(15) 3_666 ? S1 K2 3.7001(14) 2_646 ? S1 K1 3.7468(17) 3_566 ? S1 K2 3.7584(14) 1_455 ? S1 K2 3.7613(14) 2_546 ? K2 O1 2.668(3) . ? K2 O3 2.674(3) 2_656 ? K2 O8 2.686(3) 1_665 ? K2 O6 2.847(3) 1_565 ? K2 O4 2.873(3) 1_655 ? K2 O4 2.890(3) 2_556 ? K2 O2 3.135(3) . ? K2 O7 3.144(3) 2_556 ? K2 S2 3.3299(13) 1_565 ? K2 Zn1 3.6270(13) 2_556 ? K2 Zn1 3.6871(14) 2_656 ? S2 O8 1.460(3) 1_655 ? S2 O5 1.476(3) 3_666 ? S2 O7 1.490(3) 1_655 ? S2 O6 1.500(2) . ? S2 K2 3.3298(13) 1_545 ? S2 K1 3.6999(14) 1_655 ? O5 S2 1.476(3) 3_666 ? O5 K1 2.838(3) 3_666 ? O6 K2 2.847(3) 1_545 ? O7 S2 1.490(3) 1_455 ? O7 K1 2.840(3) 3_566 ? O7 K2 3.144(3) 2_546 ? O8 S2 1.460(3) 1_455 ? O8 K2 2.686(3) 1_445 ? O1 Zn1 2.045(2) 2_556 ? O2 K1 2.754(3) 3_666 ? O2 K1 2.796(3) 1_565 ? O3 K2 2.674(3) 2_646 ? O3 K1 3.345(3) 3_666 ? O4 K1 2.784(3) 3_566 ? O4 K2 2.873(3) 1_455 ? O4 K2 2.890(3) 2_546 ?
1100779.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100779.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100779 loop_ _publ_author_name 'Deng-Ke Cao' 'Yi-Zhi Li' 'Li-Min Zheng' _publ_section_title ; [Zn7{(2-C5H4N)CH(OH)PO3}6(H2O)6]SO4.4H2O: A Zinc Phosphonate Cluster with a Drum-like Cage Structure ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 2984 _journal_page_last 2985 _journal_paper_doi 10.1021/ic0500659 _journal_volume 44 _journal_year 2005 _chemical_formula_moiety '2(C36 H48 N6 O30 P6 Zn7), O8 S2, 2.26(H2 O), 1.74(H2 O)' _chemical_formula_sum 'C72 H104 N12 O72 P12 S2 Zn14' _chemical_formula_weight 3640.61 _chemical_name_systematic ; ? ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 93.390(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 22.690(2) _cell_length_b 16.6746(17) _cell_length_c 18.1507(19) _cell_measurement_reflns_used 741 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 17.91 _cell_measurement_theta_min 2.75 _cell_volume 6855.2(12) _computing_cell_refinement SMART _computing_data_collection 'SMART (Bruker, 2000)' _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _computing_structure_refinement SHELXTL _computing_structure_solution 'SHELXTL (Bruker, 2000)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.986 _diffrn_measured_fraction_theta_max 0.986 _diffrn_measurement_device_type 'Bruker Smart Apex CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0471 _diffrn_reflns_av_sigmaI/netI 0.0649 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 17197 _diffrn_reflns_theta_full 26.00 _diffrn_reflns_theta_max 26.00 _diffrn_reflns_theta_min 1.86 _exptl_absorpt_coefficient_mu 2.669 _exptl_absorpt_correction_T_max 0.56 _exptl_absorpt_correction_T_min 0.45 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS,(Bruker, 2000)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.764 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 3656 _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.654 _refine_diff_density_min -0.899 _refine_diff_density_rms 0.115 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 449 _refine_ls_number_reflns 6652 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.104 _refine_ls_R_factor_all 0.0850 _refine_ls_R_factor_gt 0.0570 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0571P)^2^+13.0953P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1159 _refine_ls_wR_factor_ref 0.1231 _reflns_number_gt 5251 _reflns_number_total 6652 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic0500659si20050116_082103.cif _cod_data_source_block '[Zn7{(2-C5H4N)CH(OH)PO3}6(H2O)6]SO4.2H2O' _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_cell_volume 6855.1(12) _cod_original_sg_symbol_H-M 'C 1 2/c 1 ' _cod_database_code 1100779 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.2500 0.2500 0.0000 0.01719(17) Uani 1 2 d S . . Zn2 Zn 0.15712(3) 0.40588(4) 0.08583(3) 0.02577(15) Uani 1 1 d . . . Zn3 Zn 0.32509(3) 0.25599(4) 0.18654(3) 0.02740(16) Uani 1 1 d . . . Zn4 Zn 0.18576(3) 0.06783(4) 0.07763(3) 0.02859(16) Uani 1 1 d . . . P1 P 0.17746(6) 0.39808(7) -0.08404(7) 0.0230(3) Uani 1 1 d . . . P2 P 0.29622(6) 0.41154(7) 0.09289(6) 0.0222(3) Uani 1 1 d . . . P3 P 0.18794(6) 0.23523(8) 0.15718(6) 0.0238(3) Uani 1 1 d . . . O1 O 0.19087(14) 0.3495(2) -0.01425(17) 0.0212(7) Uani 1 1 d . . . O2 O 0.14917(17) 0.3480(2) -0.14727(19) 0.0339(9) Uani 1 1 d . . . O3 O 0.22852(17) 0.44927(18) -0.10373(18) 0.0266(8) Uani 1 1 d . . . O4 O 0.14517(15) 0.5162(2) 0.00357(16) 0.0219(7) Uani 1 1 d . . . H4A H 0.1536 0.5704 0.0102 0.026 Uiso 1 1 calc R . . O5 O 0.23772(16) 0.4438(2) 0.11213(19) 0.0279(8) Uani 1 1 d . . . O6 O 0.29603(15) 0.32013(19) 0.08511(16) 0.0205(7) Uani 1 1 d . . . O7 O 0.32379(17) 0.4539(2) 0.02984(19) 0.0283(8) Uani 1 1 d . . . O8 O 0.32304(17) 0.3900(2) 0.23096(19) 0.0291(8) Uani 1 1 d . . . H8A H 0.3437 0.3961 0.2711 0.035 Uiso 1 1 d R . . O9 O 0.20172(14) 0.19804(18) 0.08256(17) 0.0181(7) Uani 1 1 d . . . O10 O 0.15150(17) 0.31028(19) 0.15008(19) 0.0278(8) Uani 1 1 d . . . O11 O 0.24168(17) 0.2430(2) 0.21015(19) 0.0321(9) Uani 1 1 d . . . O12 O 0.17388(17) 0.0877(2) 0.2064(2) 0.0321(9) Uani 1 1 d . . . H12B H 0.1901 0.0514 0.1806 0.039 Uiso 1 1 d R . . O1W O 0.1281(2) 0.4768(3) 0.1743(2) 0.0428(10) Uani 1 1 d . . . H1WC H 0.1152 0.4439 0.2053 0.051 Uiso 1 1 d R . . H1WA H 0.1005 0.5092 0.1614 0.051 Uiso 1 1 d R . . O2W O 0.34662(17) 0.2155(2) 0.2974(2) 0.0351(9) Uani 1 1 d . . . H2WA H 0.3521 0.1651 0.2975 0.042 Uiso 1 1 d R . . H2WC H 0.3185 0.2269 0.3245 0.042 Uiso 1 1 d R . . O3W O 0.1679(2) -0.0513(2) 0.1021(2) 0.0389(9) Uani 1 1 d . . . H3WA H 0.2014 -0.0745 0.1309 0.047 Uiso 1 1 d R . . H3WB H 0.1625 -0.0942 0.0642 0.047 Uiso 1 1 d R . . N1 N 0.07404(19) 0.3980(3) 0.0316(2) 0.0297(10) Uani 1 1 d . . . N2 N 0.4055(2) 0.3131(3) 0.1729(2) 0.0324(10) Uani 1 1 d . . . N3 N 0.1007(2) 0.0999(3) 0.0899(3) 0.0419(13) Uani 1 1 d . . . S1 S 0.22509(13) 0.29333(17) 0.42292(17) 0.0356(6) Uani 0.50 1 d P . . O21 O 0.2820(4) 0.3140(6) 0.3945(5) 0.053(2) Uani 0.50 1 d P . . O22 O 0.2134(4) 0.3233(4) 0.4941(4) 0.039(2) Uani 0.50 1 d P . . O23 O 0.2158(4) 0.2062(5) 0.4208(4) 0.0366(18) Uani 0.50 1 d P . . O24 O 0.1744(4) 0.3292(4) 0.3740(5) 0.0394(19) Uani 0.50 1 d P . . C1 C 0.0681(2) 0.4314(3) -0.0367(3) 0.0265(11) Uani 1 1 d . . . C2 C 0.0148(3) 0.4286(4) -0.0790(3) 0.0465(16) Uani 1 1 d . . . H2 H 0.0109 0.4507 -0.1263 0.056 Uiso 1 1 d R . . C3 C -0.0322(3) 0.3831(5) -0.0506(3) 0.0516(18) Uani 1 1 d . . . H3 H -0.0665 0.3740 -0.0799 0.062 Uiso 1 1 calc R . . C4 C -0.0270(3) 0.3535(4) 0.0177(3) 0.0437(15) Uani 1 1 d . . . H4 H -0.0593 0.3286 0.0371 0.052 Uiso 1 1 calc R . . C5 C 0.0274(3) 0.3593(3) 0.0621(3) 0.0302(12) Uani 1 1 d . . . H5 H 0.0311 0.3378 0.1094 0.036 Uiso 1 1 calc R . . C6 C 0.1211(2) 0.4737(3) -0.0588(3) 0.0273(11) Uani 1 1 d . . . H6 H 0.1115 0.5103 -0.1000 0.033 Uiso 1 1 calc R . . C7 C 0.4020(3) 0.3949(3) 0.1707(3) 0.0333(13) Uani 1 1 d . . . C8 C 0.4507(3) 0.4395(4) 0.1592(3) 0.0444(16) Uani 1 1 d . . . H8 H 0.4476 0.4951 0.1580 0.053 Uiso 1 1 calc R . . C9 C 0.5056(3) 0.4033(4) 0.1490(4) 0.0493(17) Uani 1 1 d . . . H9 H 0.5390 0.4340 0.1418 0.059 Uiso 1 1 calc R . . C10 C 0.5082(3) 0.3185(4) 0.1500(3) 0.0382(14) Uani 1 1 d . . . H10 H 0.5433 0.2917 0.1428 0.046 Uiso 1 1 calc R . . C11 C 0.4561(2) 0.2761(3) 0.1623(3) 0.0324(12) Uani 1 1 d . . . H11 H 0.4571 0.2203 0.1630 0.039 Uiso 1 1 calc R . . C12 C 0.3431(2) 0.4300(3) 0.1749(3) 0.0302(12) Uani 1 1 d . . . H12 H 0.3456 0.4876 0.1858 0.036 Uiso 1 1 calc R . . C13 C 0.0920(2) 0.1450(3) 0.1512(3) 0.0301(12) Uani 1 1 d . . . C14 C 0.0331(3) 0.1770(4) 0.1618(4) 0.0525(18) Uani 1 1 d . . . H14 H 0.0257 0.2097 0.2017 0.063 Uiso 1 1 calc R . . C15 C -0.0116(3) 0.1562(4) 0.1089(3) 0.0482(17) Uani 1 1 d . . . H15 H -0.0498 0.1737 0.1155 0.058 Uiso 1 1 calc R . . C16 C -0.0017(3) 0.1121(4) 0.0490(4) 0.0529(17) Uani 1 1 d . . . H16 H -0.0327 0.1015 0.0146 0.063 Uiso 1 1 calc R . . C17 C 0.0546(3) 0.0819(4) 0.0373(4) 0.0441(15) Uani 1 1 d . . . H17 H 0.0613 0.0508 -0.0039 0.053 Uiso 1 1 calc R . . C18 C 0.1417(2) 0.1626(3) 0.1998(3) 0.0300(12) Uani 1 1 d . . . H18 H 0.1297 0.1813 0.2478 0.036 Uiso 1 1 calc R . . O4W O 0.0576(3) 0.5954(4) 0.2448(4) 0.036(2) Uani 0.565(9) 1 d P . . H4WA H 0.0703 0.5948 0.2898 0.043 Uiso 0.565(9) 1 d PR . . H4WC H 0.0212 0.5830 0.2417 0.043 Uiso 0.565(9) 1 d PR . . O5W O 0.0843(3) 0.3251(4) 0.2792(4) 0.017(2) Uani 0.435(9) 1 d P . . H5WD H 0.0821 0.3327 0.3253 0.021 Uiso 0.435(9) 1 d PR . . H5WB H 0.0510 0.3352 0.2571 0.021 Uiso 0.435(9) 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0281(4) 0.0118(3) 0.0123(3) -0.0002(3) 0.0066(3) -0.0044(3) Zn2 0.0322(3) 0.0253(3) 0.0195(3) 0.0016(2) -0.0009(2) -0.0064(2) Zn3 0.0349(4) 0.0264(3) 0.0211(3) -0.0003(2) 0.0026(2) -0.0064(3) Zn4 0.0415(4) 0.0234(3) 0.0217(3) -0.0015(2) 0.0091(2) -0.0027(3) P1 0.0375(8) 0.0150(6) 0.0169(6) -0.0037(4) 0.0045(5) -0.0076(5) P2 0.0345(7) 0.0150(6) 0.0170(6) 0.0024(5) 0.0000(5) -0.0039(5) P3 0.0369(7) 0.0229(6) 0.0125(5) -0.0008(5) 0.0097(5) -0.0025(5) O1 0.0247(17) 0.0272(18) 0.0125(14) -0.0012(13) 0.0062(12) -0.0092(14) O2 0.035(2) 0.042(2) 0.0232(18) 0.0024(16) -0.0114(16) -0.0034(18) O3 0.047(2) 0.0094(16) 0.0227(17) -0.0003(13) -0.0023(16) -0.0097(15) O4 0.0284(19) 0.0242(17) 0.0129(14) -0.0020(13) -0.0004(13) -0.0056(14) O5 0.037(2) 0.0167(17) 0.0296(19) 0.0048(14) -0.0004(16) -0.0030(15) O6 0.0275(18) 0.0193(16) 0.0146(15) 0.0025(13) 0.0014(13) -0.0010(14) O7 0.042(2) 0.0198(17) 0.0236(17) 0.0021(14) 0.0050(15) -0.0026(16) O8 0.040(2) 0.0177(17) 0.0286(18) 0.0021(14) -0.0048(16) -0.0013(15) O9 0.0208(16) 0.0122(16) 0.0209(16) -0.0033(12) -0.0018(13) -0.0044(12) O10 0.041(2) 0.0135(16) 0.0285(19) 0.0004(14) -0.0009(16) 0.0019(15) O11 0.038(2) 0.035(2) 0.0236(18) 0.0038(15) 0.0076(16) -0.0043(17) O12 0.041(2) 0.0145(17) 0.042(2) 0.0032(15) 0.0172(17) 0.0017(15) O1W 0.056(3) 0.045(3) 0.0278(19) -0.0084(18) 0.0120(18) -0.008(2) O2W 0.042(2) 0.029(2) 0.036(2) 0.0041(16) 0.0129(18) 0.0064(17) O3W 0.054(3) 0.028(2) 0.034(2) -0.0017(16) -0.0042(18) -0.0025(18) N1 0.019(2) 0.034(3) 0.036(2) 0.005(2) 0.0008(18) -0.0013(18) N2 0.031(2) 0.036(3) 0.030(2) 0.0019(19) 0.0001(19) -0.009(2) N3 0.020(2) 0.050(3) 0.056(3) 0.017(3) 0.006(2) -0.008(2) S1 0.0390(16) 0.0270(14) 0.0418(16) 0.0022(12) 0.0103(12) -0.0012(12) O21 0.039(5) 0.062(6) 0.057(6) -0.010(5) 0.003(4) 0.020(5) O22 0.065(6) 0.025(4) 0.030(4) -0.004(3) 0.028(4) 0.001(4) O23 0.039(5) 0.034(4) 0.039(4) -0.007(3) 0.017(4) -0.002(3) O24 0.052(5) 0.027(4) 0.041(4) -0.004(3) 0.013(4) -0.004(4) C1 0.040(3) 0.020(2) 0.018(2) 0.0046(18) -0.009(2) -0.008(2) C2 0.071(5) 0.048(4) 0.022(3) -0.008(3) 0.015(3) -0.020(3) C3 0.043(4) 0.077(5) 0.033(3) -0.008(3) -0.007(3) -0.024(3) C4 0.028(3) 0.069(4) 0.035(3) 0.000(3) 0.004(2) -0.012(3) C5 0.042(3) 0.021(3) 0.027(3) -0.003(2) -0.003(2) 0.006(2) C6 0.023(3) 0.016(2) 0.042(3) 0.006(2) -0.007(2) -0.001(2) C7 0.035(3) 0.034(3) 0.029(3) 0.004(2) -0.015(2) -0.018(2) C8 0.061(4) 0.050(4) 0.020(3) 0.007(2) -0.014(3) -0.014(3) C9 0.038(4) 0.061(4) 0.048(4) 0.017(3) -0.007(3) -0.023(3) C10 0.029(3) 0.061(4) 0.025(3) -0.001(3) 0.010(2) -0.009(3) C11 0.032(3) 0.030(3) 0.035(3) -0.008(2) -0.006(2) 0.010(2) C12 0.025(3) 0.019(2) 0.048(3) 0.010(2) 0.015(2) -0.002(2) C13 0.034(3) 0.032(3) 0.024(3) 0.001(2) -0.001(2) -0.012(2) C14 0.060(5) 0.050(4) 0.049(4) 0.001(3) 0.015(3) -0.029(3) C15 0.049(4) 0.058(4) 0.036(3) 0.008(3) -0.009(3) -0.026(3) C16 0.059(5) 0.053(4) 0.047(4) -0.001(3) 0.001(3) -0.010(3) C17 0.052(4) 0.036(3) 0.045(4) 0.004(3) 0.006(3) -0.013(3) C18 0.043(3) 0.006(2) 0.042(3) 0.001(2) 0.015(2) -0.001(2) O4W 0.037(4) 0.030(4) 0.039(4) -0.004(3) -0.008(3) 0.008(3) O5W 0.010(4) 0.021(4) 0.022(4) 0.001(3) 0.009(3) 0.000(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O9 Zn1 O9 180.0(2) . 7 ? O9 Zn1 O1 86.77(12) . 7 ? O9 Zn1 O1 93.23(12) 7 7 ? O9 Zn1 O1 93.23(12) . . ? O9 Zn1 O1 86.77(12) 7 . ? O1 Zn1 O1 180.0(2) 7 . ? O9 Zn1 O6 92.09(11) . 7 ? O9 Zn1 O6 87.91(11) 7 7 ? O1 Zn1 O6 86.55(12) 7 7 ? O1 Zn1 O6 93.45(12) . 7 ? O9 Zn1 O6 87.91(11) . . ? O9 Zn1 O6 92.09(11) 7 . ? O1 Zn1 O6 93.45(12) 7 . ? O1 Zn1 O6 86.55(12) . . ? O6 Zn1 O6 180.00(19) 7 . ? O5 Zn2 O10 101.94(14) . . ? O5 Zn2 N1 159.96(16) . . ? O10 Zn2 N1 98.02(17) . . ? O5 Zn2 O1W 87.85(16) . . ? O10 Zn2 O1W 88.25(16) . . ? N1 Zn2 O1W 94.60(18) . . ? O5 Zn2 O1 88.51(14) . . ? O10 Zn2 O1 100.25(13) . . ? N1 Zn2 O1 86.16(16) . . ? O1W Zn2 O1 171.30(15) . . ? O5 Zn2 O4 88.48(12) . . ? O10 Zn2 O4 169.50(14) . . ? N1 Zn2 O4 71.62(14) . . ? O1W Zn2 O4 90.86(14) . . ? O1 Zn2 O4 81.13(12) . . ? O2 Zn3 O11 106.78(16) 7 . ? O2 Zn3 N2 94.51(18) 7 . ? O11 Zn3 N2 158.63(18) . . ? O2 Zn3 O2W 90.36(15) 7 . ? O11 Zn3 O2W 85.99(15) . . ? N2 Zn3 O2W 95.85(16) . . ? O2 Zn3 O6 101.86(13) 7 . ? O11 Zn3 O6 89.51(14) . . ? N2 Zn3 O6 84.26(15) . . ? O2W Zn3 O6 167.74(14) . . ? O2 Zn3 O8 163.63(15) 7 . ? O11 Zn3 O8 89.52(15) . . ? N2 Zn3 O8 69.27(17) . . ? O2W Zn3 O8 89.17(13) . . ? O6 Zn3 O8 79.38(12) . . ? O7 Zn4 O3 104.81(15) 7 7 ? O7 Zn4 N3 96.11(19) 7 . ? O3 Zn4 N3 158.87(19) 7 . ? O7 Zn4 O3W 91.42(15) 7 . ? O3 Zn4 O3W 90.71(15) 7 . ? N3 Zn4 O3W 91.71(19) . . ? O7 Zn4 O9 103.18(13) 7 . ? O3 Zn4 O9 88.60(12) 7 . ? N3 Zn4 O9 83.72(17) . . ? O3W Zn4 O9 165.07(14) . . ? O7 Zn4 O12 167.02(15) 7 . ? O3 Zn4 O12 87.27(14) 7 . ? N3 Zn4 O12 72.16(18) . . ? O3W Zn4 O12 83.60(14) . . ? O9 Zn4 O12 81.48(12) . . ? O7 Zn4 H12B 160.9 7 . ? O3 Zn4 H12B 75.6 7 . ? N3 Zn4 H12B 85.6 . . ? O3W Zn4 H12B 69.5 . . ? O9 Zn4 H12B 96.0 . . ? O12 Zn4 H12B 18.8 . . ? O3 P1 O1 112.51(19) . . ? O3 P1 O2 115.3(2) . . ? O1 P1 O2 112.9(2) . . ? O3 P1 C6 102.9(2) . . ? O1 P1 C6 105.1(2) . . ? O2 P1 C6 106.8(2) . . ? O5 P2 O7 115.0(2) . . ? O5 P2 O6 112.5(2) . . ? O7 P2 O6 113.23(19) . . ? O5 P2 C12 103.6(2) . . ? O7 P2 C12 107.1(2) . . ? O6 P2 C12 104.2(2) . . ? O10 P3 O11 113.7(2) . . ? O10 P3 O9 113.57(19) . . ? O11 P3 O9 113.3(2) . . ? O10 P3 C18 105.4(2) . . ? O11 P3 C18 104.6(2) . . ? O9 P3 C18 105.1(2) . . ? P1 O1 Zn1 127.40(19) . . ? P1 O1 Zn2 113.23(19) . . ? Zn1 O1 Zn2 118.25(14) . . ? P1 O2 Zn3 129.0(2) . 7 ? P1 O3 Zn4 128.2(2) . 7 ? C6 O4 Zn2 98.0(3) . . ? C6 O4 H4A 131.0 . . ? Zn2 O4 H4A 131.0 . . ? P2 O5 Zn2 130.9(2) . . ? P2 O6 Zn1 127.18(18) . . ? P2 O6 Zn3 114.11(17) . . ? Zn1 O6 Zn3 116.42(14) . . ? P2 O7 Zn4 129.3(2) . 7 ? C12 O8 Zn3 101.5(3) . . ? C12 O8 H8A 113.7 . . ? Zn3 O8 H8A 112.6 . . ? P3 O9 Zn1 127.23(18) . . ? P3 O9 Zn4 113.06(17) . . ? Zn1 O9 Zn4 118.06(14) . . ? P3 O10 Zn2 131.8(2) . . ? P3 O11 Zn3 128.1(2) . . ? C18 O12 Zn4 97.1(3) . . ? C18 O12 H12B 142.3 . . ? Zn4 O12 H12B 45.1 . . ? Zn2 O1W H1WC 105.9 . . ? Zn2 O1W H1WA 113.6 . . ? H1WC O1W H1WA 108.4 . . ? Zn3 O2W H2WA 109.8 . . ? Zn3 O2W H2WC 109.6 . . ? H2WA O2W H2WC 109.4 . . ? Zn4 O3W H3WA 109.7 . . ? Zn4 O3W H3WB 123.8 . . ? H3WA O3W H3WB 98.3 . . ? C1 N1 C5 121.3(4) . . ? C1 N1 Zn2 116.4(3) . . ? C5 N1 Zn2 122.3(3) . . ? C11 N2 C7 120.7(5) . . ? C11 N2 Zn3 125.1(4) . . ? C7 N2 Zn3 114.1(4) . . ? C13 N3 C17 122.1(5) . . ? C13 N3 Zn4 114.8(4) . . ? C17 N3 Zn4 123.0(5) . . ? O22 S1 O21 117.0(5) . . ? O22 S1 O23 109.6(5) . . ? O21 S1 O23 110.7(5) . . ? O22 S1 O24 102.5(5) . . ? O21 S1 O24 110.6(5) . . ? O23 S1 O24 105.6(5) . . ? N1 C1 C2 121.7(5) . . ? N1 C1 C6 113.9(4) . . ? C2 C1 C6 124.3(5) . . ? C1 C2 C3 117.3(6) . . ? C1 C2 H2 121.6 . . ? C3 C2 H2 120.7 . . ? C4 C3 C2 120.4(6) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 121.5(6) . . ? C3 C4 H4 119.2 . . ? C5 C4 H4 119.2 . . ? N1 C5 C4 117.3(5) . . ? N1 C5 H5 121.3 . . ? C4 C5 H5 121.3 . . ? O4 C6 C1 107.8(4) . . ? O4 C6 P1 107.3(3) . . ? C1 C6 P1 109.0(3) . . ? O4 C6 H6 110.9 . . ? C1 C6 H6 110.9 . . ? P1 C6 H6 110.9 . . ? C8 C7 N2 120.2(6) . . ? C8 C7 C12 122.8(6) . . ? N2 C7 C12 116.8(5) . . ? C7 C8 C9 121.3(6) . . ? C7 C8 H8 119.3 . . ? C9 C8 H8 119.3 . . ? C8 C9 C10 117.6(6) . . ? C8 C9 H9 121.2 . . ? C10 C9 H9 121.2 . . ? C11 C10 C9 118.1(6) . . ? C11 C10 H10 121.0 . . ? C9 C10 H10 121.0 . . ? N2 C11 C10 122.0(5) . . ? N2 C11 H11 119.0 . . ? C10 C11 H11 119.0 . . ? O8 C12 C7 101.2(4) . . ? O8 C12 P2 109.6(4) . . ? C7 C12 P2 112.6(4) . . ? O8 C12 H12 111.0 . . ? C7 C12 H12 111.0 . . ? P2 C12 H12 111.0 . . ? N3 C13 C18 118.1(5) . . ? N3 C13 C14 119.0(5) . . ? C18 C13 C14 122.8(5) . . ? C15 C14 C13 116.7(7) . . ? C15 C14 H14 121.6 . . ? C13 C14 H14 121.6 . . ? C16 C15 C14 122.9(8) . . ? C16 C15 H15 118.5 . . ? C14 C15 H15 118.5 . . ? C15 C16 C17 121.2(7) . . ? C15 C16 H16 119.4 . . ? C17 C16 H16 119.4 . . ? C16 C17 N3 118.0(6) . . ? C16 C17 H17 121.0 . . ? N3 C17 H17 121.0 . . ? C13 C18 O12 104.6(4) . . ? C13 C18 P3 109.4(4) . . ? O12 C18 P3 108.1(3) . . ? C13 C18 H18 111.5 . . ? O12 C18 H18 111.5 . . ? P3 C18 H18 111.5 . . ? H4WA O4W H4WC 109.5 . . ? H5WD O5W H5WB 109.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O9 2.095(3) . ? Zn1 O9 2.095(3) 7 ? Zn1 O1 2.140(3) 7 ? Zn1 O1 2.140(3) . ? Zn1 O6 2.157(3) 7 ? Zn1 O6 2.157(3) . ? Zn2 O5 1.967(4) . ? Zn2 O10 1.984(3) . ? Zn2 N1 2.078(4) . ? Zn2 O1W 2.130(4) . ? Zn2 O1 2.221(3) . ? Zn2 O4 2.375(3) . ? Zn3 O2 1.977(4) 7 ? Zn3 O11 1.977(4) . ? Zn3 N2 2.086(5) . ? Zn3 O2W 2.150(4) . ? Zn3 O6 2.196(3) . ? Zn3 O8 2.376(3) . ? Zn4 O7 1.983(3) 7 ? Zn4 O3 1.995(4) 7 ? Zn4 N3 2.027(5) . ? Zn4 O3W 2.081(4) . ? Zn4 O9 2.202(3) . ? Zn4 O12 2.391(4) . ? Zn4 H12B 1.8862 . ? P1 O3 1.499(4) . ? P1 O1 1.519(3) . ? P1 O2 1.529(4) . ? P1 C6 1.872(5) . ? P2 O5 1.493(4) . ? P2 O7 1.511(4) . ? P2 O6 1.531(3) . ? P2 C12 1.804(6) . ? P3 O10 1.501(4) . ? P3 O11 1.513(4) . ? P3 O9 1.539(3) . ? P3 C18 1.806(5) . ? O2 Zn3 1.977(4) 7 ? O3 Zn4 1.995(4) 7 ? O4 C6 1.416(6) . ? O4 H4A 0.9300 . ? O7 Zn4 1.983(3) 7 ? O8 C12 1.321(6) . ? O8 H8A 0.8500 . ? O12 C18 1.448(6) . ? O12 H12B 0.8591 . ? O1W H1WC 0.8500 . ? O1W H1WA 0.8500 . ? O2W H2WA 0.8503 . ? O2W H2WC 0.8500 . ? O3W H3WA 0.9759 . ? O3W H3WB 0.9956 . ? N1 C1 1.359(6) . ? N1 C5 1.383(7) . ? N2 C11 1.327(7) . ? N2 C7 1.368(7) . ? N3 C13 1.368(8) . ? N3 C17 1.405(8) . ? S1 O22 1.426(8) . ? S1 O21 1.460(10) . ? S1 O23 1.468(8) . ? S1 O24 1.532(9) . ? C1 C2 1.395(9) . ? C1 C6 1.472(7) . ? C2 C3 1.429(9) . ? C2 H2 0.9327 . ? C3 C4 1.333(9) . ? C3 H3 0.9300 . ? C4 C5 1.436(8) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 H6 0.9800 . ? C7 C8 1.358(8) . ? C7 C12 1.464(8) . ? C8 C9 1.407(10) . ? C8 H8 0.9300 . ? C9 C10 1.415(9) . ? C9 H9 0.9300 . ? C10 C11 1.406(8) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 H12 0.9800 . ? C13 C18 1.421(8) . ? C13 C14 1.463(10) . ? C14 C15 1.397(9) . ? C14 H14 0.9300 . ? C15 C16 1.343(10) . ? C15 H15 0.9300 . ? C16 C17 1.401(10) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 H18 0.9800 . ? O4W H4WA 0.8500 . ? O4W H4WC 0.8500 . ? O5W H5WD 0.8501 . ? O5W H5WB 0.8501 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3W H3WA O21 0.98 1.96 2.516(11) 113.9 4_545 O4W H4WC O4W 0.85 1.83 2.632(15) 156.5 2 O4W H4WA O2 0.85 2.27 2.926(8) 133.6 6_566 O2W H2WA O4W 0.85 2.51 3.085(8) 125.3 4_545 O12 H12B O3 0.86 2.38 3.040(5) 133.9 7 O8 H8A O3W 0.85 2.49 3.179(5) 138.8 4 O4 H4A O22 0.93 2.26 3.101(8) 150.0 6_565 O1W H1WA O4W 0.85 2.34 2.889(8) 122.7 . O1W H1WC O5W 0.85 2.52 3.352(8) 168.2 . O12 H12B O3W 0.86 2.27 2.990(5) 141.9 . O2W H2WC O21 0.85 2.13 2.874(10) 146.0 .
1100780.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $ #$Revision: 176435 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100780.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100780 loop_ _publ_author_name 'Chizu Shimokawa' 'Shinobu Itoh' _publ_section_title ; The First \b-Diketiminate-Ag(I) Complexes. Macrocyclic Dinuclear and Tetranuclear Ag(I)-Complexes and Linear Coordination Polymer Ag(I)-Complex ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3010 _journal_page_last 3012 _journal_paper_doi 10.1021/ic0501014 _journal_volume 44 _journal_year 2005 _chemical_formula_moiety 'C56 H78 N4 ' _chemical_formula_sum 'C56 H78 N4' _chemical_formula_weight 807.26 _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _cell_angle_alpha 90 _cell_angle_beta 108.296(4) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 11.824(2) _cell_length_b 10.358(2) _cell_length_c 21.483(4) _cell_measurement_reflns_used 8394 _cell_measurement_temperature 153.1 _cell_measurement_theta_max 27.5 _cell_measurement_theta_min 4.1 _cell_volume 2498.1(8) _computing_cell_refinement CrystalClear _computing_data_collection CrystalClear _computing_data_reduction CrystalStructure _computing_molecular_graphics ORTEP3 _computing_publication_material 'CrystalStructure 3.6.0' _computing_structure_refinement CRYSTALS _computing_structure_solution SIR92 _diffrn_detector_area_resol_mean 7.31 _diffrn_measured_fraction_theta_full 0.9820 _diffrn_measured_fraction_theta_max 0.9820 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents 0.038 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 24350 _diffrn_reflns_theta_full 27.48 _diffrn_reflns_theta_max 27.48 _exptl_absorpt_coefficient_mu 0.062 _exptl_absorpt_correction_T_max 0.988 _exptl_absorpt_correction_T_min 0.986 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Higashi, T. (1999). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.073 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 884.00 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _refine_diff_density_max 0.50 _refine_diff_density_min -0.61 _refine_ls_extinction_coef 715.3(16) _refine_ls_extinction_method 'Larson (1970) Crystallographic Computing eq. 22' _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_hydrogen_treatment refall _refine_ls_number_parameters 311 _refine_ls_number_reflns 9427 _refine_ls_R_factor_gt 0.0530 _refine_ls_shift/su_max 0.0000 _refine_ls_structure_factor_coef F _refine_ls_weighting_details 'w = 1/[0.0005Fo^2^ + 2.0000\s(Fo^2^)]' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.0540 _reflns_number_gt 9427 _reflns_number_total 20636 _reflns_threshold_expression F^2^>2.0\s(F^2^) _cod_data_source_file ic0501014si20050122_011347_1.cif _cod_data_source_block '__(L2)2' _cod_original_formula_sum 'C56 H78 N4 ' _cod_database_code 1100780 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 +X,1/2-Y,1/2+Z loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N(1) N 0.25659(6) 0.06917(7) 0.46755(4) 0.0226(2) Uani 1.00 1 d . . . N(2) N 0.51849(7) 0.20091(8) 0.60265(5) 0.0281(2) Uani 1.00 1 d . . . C(1) C 0.46748(8) 0.02550(8) 0.52454(5) 0.0210(2) Uani 1.00 1 d . . . C(2) C 0.36118(8) 0.11037(9) 0.48852(5) 0.0216(2) Uani 1.00 1 d . . . C(3) C 0.55311(8) 0.10614(9) 0.57740(5) 0.0244(3) Uani 1.00 1 d . . . C(4) C 0.42606(9) -0.08908(9) 0.55791(6) 0.0287(3) Uani 1.00 1 d . . . C(5) C 0.16423(8) 0.16058(9) 0.43887(6) 0.0267(3) Uani 1.00 1 d . . . C(6) C 0.11685(9) 0.23168(11) 0.47990(6) 0.0345(3) Uani 1.00 1 d . . . C(7) C 0.02414(10) 0.31746(11) 0.45132(7) 0.0448(4) Uani 1.00 1 d . . . C(8) C -0.01953(10) 0.33102(11) 0.38478(7) 0.0447(4) Uani 1.00 1 d . . . C(9) C 0.02891(10) 0.26053(10) 0.34501(6) 0.0393(3) Uani 1.00 1 d . . . C(10) C 0.11953(8) 0.17373(9) 0.36990(6) 0.0274(3) Uani 1.00 1 d . . . C(11) C 0.16277(11) 0.2172(1) 0.55358(6) 0.0463(4) Uani 1.00 1 d . . . C(12) C 0.1606(3) 0.3448(2) 0.58792(11) 0.1329(10) Uani 1.00 1 d . . . C(13) C 0.0957(3) 0.1203(3) 0.57686(12) 0.1360(10) Uani 1.00 1 d . . . C(14) C 0.16953(9) 0.09064(10) 0.32624(5) 0.0323(3) Uani 1.00 1 d . . . C(15) C 0.12266(10) -0.04586(12) 0.32412(7) 0.0451(4) Uani 1.00 1 d . . . C(16) C 0.14477(12) 0.1459(2) 0.25733(7) 0.0594(4) Uani 1.00 1 d . . . C(17) C 0.60505(8) 0.26707(9) 0.65536(6) 0.0285(3) Uani 1.00 1 d . . . C(18) C 0.67696(9) 0.36341(10) 0.63906(6) 0.0333(3) Uani 1.00 1 d . . . C(19) C 0.76025(10) 0.42542(10) 0.69117(8) 0.0414(4) Uani 1.00 1 d . . . C(20) C 0.77223(10) 0.39705(12) 0.75577(7) 0.0479(4) Uani 1.00 1 d . . . C(21) C 0.69855(11) 0.30546(12) 0.77045(7) 0.0475(4) Uani 1.00 1 d . . . C(22) C 0.61383(9) 0.24071(11) 0.72021(7) 0.0387(3) Uani 1.00 1 d . . . C(23) C 0.66660(10) 0.39804(10) 0.56938(7) 0.0392(3) Uani 1.00 1 d . . . C(24) C 0.64205(13) 0.54217(11) 0.55638(9) 0.0615(5) Uani 1.00 1 d . . . C(25) C 0.77592(12) 0.3611(1) 0.55124(9) 0.0564(4) Uani 1.00 1 d . . . C(26) C 0.53068(12) 0.1406(1) 0.73636(7) 0.0525(4) Uani 1.00 1 d . . . C(27) C 0.5846(2) 0.0680(3) 0.7964(2) 0.202(2) Uani 1.00 1 d . . . C(28) C 0.4253(2) 0.1973(2) 0.7412(2) 0.184(2) Uani 1.00 1 d . . . H(1) H 0.3755 0.1989 0.4823 0.026 Uiso 1.00 1 c R . . H(2) H 0.6351 0.0837 0.5921 0.028 Uiso 1.00 1 c R . . H(3) H 0.4307 -0.0646 0.6013 0.037 Uiso 1.00 1 c R . . H(4) H 0.4758 -0.1618 0.5594 0.036 Uiso 1.00 1 c R . . H(5) H 0.3461 -0.1105 0.5340 0.035 Uiso 1.00 1 c R . . H(6) H -0.0113 0.3643 0.4784 0.052 Uiso 1.00 1 c R . . H(7) H -0.0813 0.3914 0.3661 0.051 Uiso 1.00 1 c R . . H(8) H -0.0021 0.2712 0.2988 0.043 Uiso 1.00 1 c R . . H(9) H 0.2429 0.1885 0.5645 0.056 Uiso 1.00 1 c R . . H(10) H 0.2346 0.3871 0.5940 0.154 Uiso 1.00 1 c R . . H(11) H 0.1497 0.3305 0.6293 0.154 Uiso 1.00 1 c R . . H(12) H 0.0977 0.3972 0.5617 0.155 Uiso 1.00 1 c R . . H(13) H 0.0297 0.1590 0.5860 0.156 Uiso 1.00 1 c R . . H(14) H 0.1455 0.0795 0.6153 0.156 Uiso 1.00 1 c R . . H(15) H 0.0677 0.0579 0.5431 0.156 Uiso 1.00 1 c R . . H(16) H 0.2535 0.0873 0.3459 0.037 Uiso 1.00 1 c R . . H(17) H 0.1757 -0.0958 0.3579 0.054 Uiso 1.00 1 c R . . H(18) H 0.1177 -0.0819 0.2827 0.054 Uiso 1.00 1 c R . . H(19) H 0.0459 -0.0460 0.3295 0.053 Uiso 1.00 1 c R . . H(20) H 0.0709 0.1141 0.2293 0.073 Uiso 1.00 1 c R . . H(21) H 0.2070 0.1213 0.2405 0.073 Uiso 1.00 1 c R . . H(22) H 0.1415 0.2374 0.2595 0.073 Uiso 1.00 1 c R . . H(23) H 0.8094 0.4905 0.6820 0.047 Uiso 1.00 1 c R . . H(24) H 0.8296 0.4412 0.7903 0.054 Uiso 1.00 1 c R . . H(25) H 0.7073 0.2855 0.8149 0.056 Uiso 1.00 1 c R . . H(26) H 0.6001 0.3532 0.5412 0.045 Uiso 1.00 1 c R . . H(27) H 0.5587 0.5581 0.5420 0.068 Uiso 1.00 1 c R . . H(28) H 0.6753 0.5701 0.5238 0.068 Uiso 1.00 1 c R . . H(29) H 0.6781 0.5881 0.5959 0.068 Uiso 1.00 1 c R . . H(30) H 0.8322 0.4295 0.5614 0.070 Uiso 1.00 1 c R . . H(31) H 0.7533 0.3430 0.5056 0.070 Uiso 1.00 1 c R . . H(32) H 0.8106 0.2862 0.5753 0.071 Uiso 1.00 1 c R . . H(33) H 0.5130 0.0762 0.7032 0.065 Uiso 1.00 1 c R . . H(34) H 0.6257 -0.0077 0.7908 0.234 Uiso 1.00 1 c R . . H(35) H 0.5228 0.0453 0.8138 0.234 Uiso 1.00 1 c R . . H(36) H 0.6387 0.1250 0.8257 0.234 Uiso 1.00 1 c R . . H(37) H 0.4334 0.2261 0.7844 0.249 Uiso 1.00 1 c R . . H(38) H 0.3640 0.1341 0.7284 0.249 Uiso 1.00 1 c R . . H(39) H 0.4054 0.2683 0.7118 0.249 Uiso 1.00 1 c R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 N(1) 0.0224(4) 0.0236(4) 0.0210(5) 0.0034(3) 0.0055(3) 0.0000(3) N(2) 0.0199(4) 0.0281(4) 0.0328(6) -0.0012(4) 0.0033(4) -0.0077(4) C(1) 0.0228(4) 0.0182(4) 0.0203(6) 0.0008(4) 0.0041(4) 0.0014(4) C(2) 0.0232(5) 0.0201(5) 0.0208(6) 0.0009(4) 0.0059(4) -0.0033(4) C(3) 0.0198(4) 0.0262(5) 0.0241(6) 0.0044(4) 0.0023(4) 0.0005(4) C(4) 0.0338(5) 0.0250(5) 0.0279(7) -0.0004(4) 0.0106(5) 0.0032(4) C(5) 0.0219(5) 0.0220(5) 0.0331(7) -0.0011(4) 0.0040(4) -0.0009(4) C(6) 0.0285(5) 0.0388(6) 0.0347(7) 0.0014(5) 0.0079(5) -0.0103(5) C(7) 0.0307(6) 0.0463(7) 0.0532(10) 0.0131(5) 0.0070(6) -0.0134(6) C(8) 0.0356(6) 0.0398(6) 0.0516(9) 0.0190(5) 0.0034(6) -0.0039(6) C(9) 0.0376(6) 0.0370(6) 0.0357(7) 0.0075(5) 0.0008(5) 0.0058(5) C(10) 0.0178(4) 0.0323(5) 0.0290(7) -0.0021(4) 0.0028(4) -0.0023(4) C(11) 0.0440(6) 0.0691(8) 0.0258(7) 0.0141(6) 0.0107(5) -0.0098(6) C(12) 0.227(3) 0.112(2) 0.0469(13) 0.016(2) 0.025(2) -0.0339(12) C(13) 0.148(2) 0.174(2) 0.068(2) -0.049(2) 0.007(2) 0.052(2) C(14) 0.0239(5) 0.0505(6) 0.0187(6) 0.0050(5) 0.0015(4) -0.0024(5) C(15) 0.0327(6) 0.0498(7) 0.0501(9) 0.0107(6) 0.0090(6) -0.0157(6) C(16) 0.0536(8) 0.0933(11) 0.0343(8) 0.0171(8) 0.0181(6) 0.0127(8) C(17) 0.0209(5) 0.0231(5) 0.0393(7) 0.0013(4) 0.0061(4) -0.0101(5) C(18) 0.0257(5) 0.0243(5) 0.0472(8) 0.0015(5) 0.0073(5) -0.0038(5) C(19) 0.0322(6) 0.0275(5) 0.0592(10) -0.0020(5) 0.0068(6) -0.0072(6) C(20) 0.0360(6) 0.0475(7) 0.0497(10) -0.0098(6) -0.0015(6) -0.0201(6) C(21) 0.0454(7) 0.0532(7) 0.0413(9) -0.0024(6) 0.0097(6) -0.0180(6) C(22) 0.0347(6) 0.0405(6) 0.0416(8) -0.0042(5) 0.0131(5) -0.0155(6) C(23) 0.0340(6) 0.0234(5) 0.0547(9) -0.0045(5) 0.0058(5) 0.0037(5) C(24) 0.0672(9) 0.0288(6) 0.0726(12) -0.0077(6) -0.0011(8) 0.0132(6) C(25) 0.0614(8) 0.0502(7) 0.0638(10) 0.0033(7) 0.0285(8) 0.0051(7) C(26) 0.0610(8) 0.0608(8) 0.0399(8) -0.0238(7) 0.0220(6) -0.0175(7) C(27) 0.0657(13) 0.114(2) 0.405(6) 0.0140(12) 0.044(2) 0.156(3) C(28) 0.119(2) 0.103(2) 0.400(6) 0.040(1) 0.182(3) 0.105(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 N(1) C(2) C(1) 123.26(8) ? . . . C(5) N(1) C(2) 117.65(8) ? . . . N(1) C(5) C(6) 118.8(1) ? . . . N(1) C(5) C(10) 119.9(1) ? . . . N(2) C(3) C(1) 121.71(8) ? . . . C(17) N(2) C(3) 117.78(8) ? . . . N(2) C(17) C(18) 118.2(1) ? . . . N(2) C(17) C(22) 120.4(1) ? . . . C(2) C(1) C(1) 110.46(8) ? . . 65603 C(3) C(1) C(1) 109.54(8) ? . . 65603 C(1) C(1) C(3) 109.54(8) ? . 65603 65603 C(4) C(1) C(1) 110.18(8) ? . . 65603 C(1) C(1) C(2) 110.46(8) ? . 65603 65603 C(1) C(1) C(4) 110.18(8) ? . 65603 65603 C(3) C(1) C(2) 108.19(7) ? . . . C(4) C(1) C(2) 110.28(8) ? . . . C(4) C(1) C(3) 108.11(8) ? . . . C(10) C(5) C(6) 121.28(9) ? . . . C(5) C(6) C(11) 121.8(1) ? . . . C(5) C(6) C(7) 118.3(1) ? . . . C(5) C(10) C(14) 120.07(8) ? . . . C(5) C(10) C(9) 117.4(1) ? . . . C(11) C(6) C(7) 119.9(1) ? . . . C(6) C(7) C(8) 120.8(1) ? . . . C(6) C(11) C(13) 111.8(1) ? . . . C(6) C(11) C(12) 111.6(1) ? . . . C(7) C(8) C(9) 120.0(1) ? . . . C(8) C(9) C(10) 122.1(1) ? . . . C(9) C(10) C(14) 122.5(1) ? . . . C(10) C(14) C(15) 109.7(1) ? . . . C(10) C(14) C(16) 113.1(1) ? . . . C(13) C(11) C(12) 109.7(2) ? . . . C(16) C(14) C(15) 111.3(1) ? . . . C(22) C(17) C(18) 121.41(9) ? . . . C(17) C(18) C(23) 122.86(9) ? . . . C(17) C(18) C(19) 116.8(1) ? . . . C(17) C(22) C(26) 120.3(1) ? . . . C(17) C(22) C(21) 119.4(1) ? . . . C(23) C(18) C(19) 120.3(1) ? . . . C(18) C(19) C(20) 122.2(1) ? . . . C(18) C(23) C(25) 112.7(1) ? . . . C(18) C(23) C(24) 111.4(1) ? . . . C(19) C(20) C(21) 120.0(1) ? . . . C(20) C(21) C(22) 120.2(1) ? . . . C(21) C(22) C(26) 120.3(1) ? . . . C(22) C(26) C(28) 112.2(1) ? . . . C(22) C(26) C(27) 114.5(1) ? . . . C(25) C(23) C(24) 109.2(1) ? . . . C(28) C(26) C(27) 107.5(2) ? . . . N(1) C(2) H(1) 118.6161 ? . . . N(2) C(3) H(2) 119.1735 ? . . . C(1) C(2) H(1) 118.1188 ? . . . C(1) C(3) H(2) 119.1157 ? . . . C(1) C(4) H(3) 108.7313 ? . . . C(1) C(4) H(5) 109.6302 ? . . . C(1) C(4) H(4) 110.0484 ? . . . H(5) C(4) H(3) 109.4684 ? . . . H(4) C(4) H(3) 109.4743 ? . . . H(5) C(4) H(4) 109.4719 ? . . . C(6) C(7) H(6) 119.5186 ? . . . C(6) C(11) H(9) 107.0199 ? . . . H(6) C(7) C(8) 119.5779 ? . . . C(7) C(8) H(7) 119.8606 ? . . . C(8) C(9) H(8) 119.0991 ? . . . H(7) C(8) C(9) 120.0828 ? . . . H(8) C(9) C(10) 118.7960 ? . . . C(10) C(14) H(16) 107.4218 ? . . . H(9) C(11) C(12) 108.6885 ? . . . C(11) C(12) H(10) 108.2447 ? . . . C(11) C(12) H(11) 110.3258 ? . . . C(11) C(12) H(12) 109.8289 ? . . . H(9) C(11) C(13) 107.8616 ? . . . C(11) C(13) H(15) 107.6162 ? . . . C(11) C(13) H(13) 110.4255 ? . . . C(11) C(13) H(14) 110.3529 ? . . . H(11) C(12) H(10) 109.4774 ? . . . H(12) C(12) H(10) 109.4696 ? . . . H(12) C(12) H(11) 109.4734 ? . . . H(15) C(13) H(13) 109.4675 ? . . . H(14) C(13) H(13) 109.4774 ? . . . H(15) C(13) H(14) 109.4715 ? . . . H(16) C(14) C(15) 107.5354 ? . . . C(14) C(15) H(17) 109.7627 ? . . . C(14) C(15) H(19) 110.6295 ? . . . C(14) C(15) H(18) 108.0054 ? . . . H(16) C(14) C(16) 107.5188 ? . . . C(14) C(16) H(20) 110.0313 ? . . . C(14) C(16) H(22) 108.9873 ? . . . C(14) C(16) H(21) 109.3830 ? . . . H(19) C(15) H(17) 109.4641 ? . . . H(18) C(15) H(17) 109.4770 ? . . . H(19) C(15) H(18) 109.4776 ? . . . H(22) C(16) H(20) 109.4743 ? . . . H(21) C(16) H(20) 109.4716 ? . . . H(22) C(16) H(21) 109.4781 ? . . . C(18) C(19) H(23) 118.9721 ? . . . C(18) C(23) H(26) 108.0889 ? . . . H(23) C(19) C(20) 118.8461 ? . . . C(19) C(20) H(24) 120.2658 ? . . . C(20) C(21) H(25) 119.9006 ? . . . H(24) C(20) C(21) 119.7689 ? . . . H(25) C(21) C(22) 119.9131 ? . . . C(22) C(26) H(33) 108.0490 ? . . . H(26) C(23) C(24) 106.7900 ? . . . C(23) C(24) H(27) 110.3168 ? . . . C(23) C(24) H(28) 109.4695 ? . . . C(23) C(24) H(29) 108.6206 ? . . . H(26) C(23) C(25) 108.3794 ? . . . C(23) C(25) H(32) 108.9309 ? . . . C(23) C(25) H(30) 110.2543 ? . . . C(23) C(25) H(31) 109.2180 ? . . . H(28) C(24) H(27) 109.4757 ? . . . H(29) C(24) H(27) 109.4706 ? . . . H(29) C(24) H(28) 109.4696 ? . . . H(32) C(25) H(30) 109.4736 ? . . . H(31) C(25) H(30) 109.4667 ? . . . H(32) C(25) H(31) 109.4809 ? . . . H(33) C(26) C(27) 103.4454 ? . . . C(26) C(27) H(34) 114.4488 ? . . . C(26) C(27) H(36) 106.4110 ? . . . C(26) C(27) H(35) 107.4430 ? . . . H(33) C(26) C(28) 110.8291 ? . . . C(26) C(28) H(39) 108.2602 ? . . . C(26) C(28) H(37) 112.4498 ? . . . C(26) C(28) H(38) 107.6592 ? . . . H(36) C(27) H(34) 109.4682 ? . . . H(35) C(27) H(34) 109.4733 ? . . . H(36) C(27) H(35) 109.4727 ? . . . H(39) C(28) H(37) 109.4693 ? . . . H(38) C(28) H(37) 109.4734 ? . . . H(39) C(28) H(38) 109.4753 ? . . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 N(1) C(2) 1.251(1) ? . . N(1) C(5) 1.430(1) ? . . N(2) C(3) 1.251(1) ? . . N(2) C(17) 1.439(1) ? . . C(1) C(1) 1.578(2) ? . 65603 C(1) C(2) 1.530(1) ? . . C(1) C(3) 1.513(1) ? . . C(1) C(4) 1.544(2) ? . . C(5) C(6) 1.394(2) ? . . C(5) C(10) 1.415(2) ? . . C(6) C(7) 1.395(2) ? . . C(6) C(11) 1.511(2) ? . . C(7) C(8) 1.366(2) ? . . C(8) C(9) 1.378(2) ? . . C(9) C(10) 1.372(1) ? . . C(10) C(14) 1.523(2) ? . . C(11) C(12) 1.518(3) ? . . C(11) C(13) 1.462(3) ? . . C(14) C(15) 1.514(2) ? . . C(14) C(16) 1.527(2) ? . . C(17) C(18) 1.424(2) ? . . C(17) C(22) 1.391(2) ? . . C(18) C(19) 1.394(2) ? . . C(18) C(23) 1.506(2) ? . . C(19) C(20) 1.382(2) ? . . C(20) C(21) 1.390(2) ? . . C(21) C(22) 1.393(2) ? . . C(22) C(26) 1.541(2) ? . . C(23) C(24) 1.530(2) ? . . C(23) C(25) 1.512(2) ? . . C(26) C(27) 1.456(4) ? . . C(26) C(28) 1.410(3) ? . . C(2) H(1) 0.9501 ? . . C(3) H(2) 0.9500 ? . . C(4) H(3) 0.9500 ? . . C(4) H(4) 0.9499 ? . . C(4) H(5) 0.9500 ? . . C(7) H(6) 0.9500 ? . . C(8) H(7) 0.9500 ? . . C(9) H(8) 0.9500 ? . . C(11) H(9) 0.9500 ? . . C(12) H(10) 0.9500 ? . . C(12) H(11) 0.9501 ? . . C(12) H(12) 0.9500 ? . . C(13) H(13) 0.9500 ? . . C(13) H(14) 0.9500 ? . . C(13) H(15) 0.9499 ? . . C(14) H(16) 0.9500 ? . . C(15) H(17) 0.9500 ? . . C(15) H(18) 0.9499 ? . . C(15) H(19) 0.9500 ? . . C(16) H(20) 0.9500 ? . . C(16) H(21) 0.9500 ? . . C(16) H(22) 0.9500 ? . . C(19) H(23) 0.9500 ? . . C(20) H(24) 0.9500 ? . . C(21) H(25) 0.9501 ? . . C(23) H(26) 0.9500 ? . . C(24) H(27) 0.9500 ? . . C(24) H(28) 0.9500 ? . . C(24) H(29) 0.9499 ? . . C(25) H(30) 0.9500 ? . . C(25) H(31) 0.9500 ? . . C(25) H(32) 0.9500 ? . . C(26) H(33) 0.9500 ? . . C(27) H(34) 0.9499 ? . . C(27) H(35) 0.9499 ? . . C(27) H(36) 0.9500 ? . . C(28) H(37) 0.9501 ? . . C(28) H(38) 0.9500 ? . . C(28) H(39) 0.9500 ? . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 N(1) C(1) 2.450(1) ? . . N(1) C(1) 3.359(1) ? . 65603 N(1) C(3) 3.580(1) ? . . N(1) C(3) 3.264(1) ? . 65603 N(1) C(4) 2.833(1) ? . . N(1) C(6) 2.431(1) ? . . N(1) C(10) 2.463(1) ? . . N(1) C(11) 2.878(2) ? . . N(1) C(13) 3.496(3) ? . . N(1) C(14) 2.892(1) ? . . N(1) C(15) 3.218(2) ? . . N(2) C(1) 2.418(1) ? . . N(2) C(2) 2.736(1) ? . . N(2) C(4) 3.237(1) ? . . N(2) C(18) 2.457(1) ? . . N(2) C(22) 2.456(2) ? . . N(2) C(23) 2.921(2) ? . . N(2) C(26) 2.899(2) ? . . N(2) C(28) 3.483(4) ? . . C(1) N(1) 3.359(1) ? . 65603 C(1) C(2) 2.553(1) ? . 65603 C(1) C(3) 2.526(1) ? . 65603 C(1) C(4) 2.560(2) ? . 65603 C(2) C(1) 2.553(1) ? . 65603 C(2) C(3) 2.465(1) ? . . C(2) C(3) 2.994(1) ? . 65603 C(2) C(4) 2.522(1) ? . . C(2) C(4) 2.991(2) ? . 65603 C(2) C(5) 2.296(1) ? . . C(2) C(6) 3.102(1) ? . . C(2) C(10) 3.243(1) ? . . C(2) C(11) 3.277(2) ? . . C(2) C(14) 3.517(1) ? . . C(3) N(1) 3.264(1) ? . 65603 C(3) C(1) 2.526(1) ? . 65603 C(3) C(2) 2.994(1) ? . 65603 C(3) C(4) 2.475(1) ? . . C(3) C(4) 2.999(2) ? . 65603 C(3) C(17) 2.305(1) ? . . C(3) C(18) 3.128(1) ? . . C(3) C(22) 3.239(2) ? . . C(3) C(23) 3.334(1) ? . . C(3) C(26) 3.525(2) ? . . C(4) C(1) 2.560(2) ? . 65603 C(4) C(2) 2.991(2) ? . 65603 C(4) C(3) 2.999(2) ? . 65603 C(5) C(7) 2.395(2) ? . . C(5) C(8) 2.757(1) ? . . C(5) C(9) 2.382(1) ? . . C(5) C(11) 2.539(2) ? . . C(5) C(13) 3.336(3) ? . . C(5) C(14) 2.545(2) ? . . C(5) C(15) 3.183(2) ? . . C(6) C(8) 2.401(2) ? . . C(6) C(9) 2.771(2) ? . . C(6) C(10) 2.448(2) ? . . C(6) C(12) 2.504(3) ? . . C(6) C(13) 2.462(3) ? . . C(7) C(9) 2.377(2) ? . . C(7) C(10) 2.790(2) ? . . C(7) C(11) 2.516(2) ? . . C(7) C(12) 2.885(3) ? . . C(7) C(13) 3.275(3) ? . . C(8) C(10) 2.406(2) ? . . C(9) C(14) 2.539(2) ? . . C(9) C(15) 3.437(2) ? . . C(9) C(16) 2.908(2) ? . . C(9) C(20) 3.449(2) ? . 45404 C(10) C(15) 2.483(2) ? . . C(10) C(16) 2.544(2) ? . . C(12) C(13) 2.437(4) ? . . C(15) C(16) 2.511(2) ? . . C(17) C(19) 2.401(1) ? . . C(17) C(20) 2.774(2) ? . . C(17) C(21) 2.404(2) ? . . C(17) C(23) 2.574(2) ? . . C(17) C(25) 3.587(2) ? . . C(17) C(26) 2.545(2) ? . . C(17) C(28) 3.302(4) ? . . C(18) C(20) 2.430(2) ? . . C(18) C(21) 2.818(2) ? . . C(18) C(22) 2.455(2) ? . . C(18) C(24) 2.509(2) ? . . C(18) C(25) 2.513(2) ? . . C(19) C(21) 2.399(2) ? . . C(19) C(22) 2.779(2) ? . . C(19) C(23) 2.517(2) ? . . C(19) C(24) 3.043(2) ? . . C(19) C(25) 3.141(3) ? . . C(20) C(9) 3.449(2) ? . 65504 C(20) C(22) 2.412(2) ? . . C(21) C(26) 2.545(2) ? . . C(21) C(27) 2.941(3) ? . . C(21) C(28) 3.289(3) ? . . C(22) C(27) 2.520(4) ? . . C(22) C(28) 2.451(3) ? . . C(24) C(24) 3.579(2) ? . 66603 C(24) C(25) 2.479(2) ? . . C(27) C(28) 2.312(3) ? . . N(1) H(1) 1.8988 ? . . N(1) H(2) 2.6105 ? . 65603 N(1) H(3) 3.2707 ? . . N(1) H(4) 3.5246 ? . 65603 N(1) H(5) 2.3820 ? . . N(1) H(9) 2.4707 ? . . N(1) H(15) 3.1484 ? . . N(1) H(16) 2.6080 ? . . N(1) H(17) 2.8230 ? . . N(1) H(19) 3.4332 ? . . N(2) H(1) 2.6074 ? . . N(2) H(2) 1.9042 ? . . N(2) H(3) 2.9366 ? . . N(2) H(4) 3.5270 ? . 65603 N(2) H(9) 3.1027 ? . . N(2) H(26) 2.4422 ? . . N(2) H(33) 2.5358 ? . . N(2) H(39) 3.1214 ? . . C(1) H(1) 2.1479 ? . . C(1) H(1) 3.0071 ? . 65603 C(1) H(2) 2.1430 ? . . C(1) H(2) 2.6681 ? . 65603 C(1) H(3) 2.0560 ? . . C(1) H(3) 3.3106 ? . 65603 C(1) H(4) 2.0714 ? . . C(1) H(4) 2.5413 ? . 65603 C(1) H(5) 2.0665 ? . . C(1) H(5) 2.9932 ? . 65603 C(1) H(9) 3.4739 ? . . C(2) H(2) 3.3158 ? . . C(2) H(2) 2.6620 ? . 65603 C(2) H(3) 2.9287 ? . . C(2) H(4) 3.2879 ? . . C(2) H(4) 2.5117 ? . 65603 C(2) H(5) 2.5163 ? . . C(2) H(9) 2.5900 ? . . C(2) H(16) 2.9344 ? . . C(2) H(28) 3.3373 ? . 66603 C(2) H(29) 3.5683 ? . 66603 C(3) H(1) 2.6102 ? . . C(3) H(3) 2.4396 ? . . C(3) H(4) 2.9101 ? . . C(3) H(4) 2.9085 ? . 65603 C(3) H(5) 3.2349 ? . . C(3) H(5) 2.9907 ? . 65603 C(3) H(16) 3.0971 ? . 65603 C(3) H(17) 3.0700 ? . 65603 C(3) H(26) 2.7812 ? . . C(3) H(32) 3.5827 ? . . C(3) H(33) 2.9041 ? . . C(4) H(1) 3.3596 ? . . C(4) H(1) 2.9692 ? . 65603 C(4) H(2) 2.9517 ? . . C(4) H(2) 3.0734 ? . 65603 C(4) H(26) 3.4202 ? . 65603 C(4) H(31) 3.3851 ? . 65603 C(4) H(33) 3.4233 ? . . C(5) H(1) 2.4098 ? . . C(5) H(6) 3.2539 ? . . C(5) H(8) 3.2431 ? . . C(5) H(9) 2.5805 ? . . C(5) H(15) 3.0090 ? . . C(5) H(16) 2.6453 ? . . C(5) H(17) 3.2009 ? . . C(5) H(19) 3.1613 ? . . C(5) H(28) 3.3270 ? . 66603 C(5) H(29) 3.4182 ? . 66603 C(6) H(1) 3.0617 ? . . C(6) H(6) 2.0380 ? . . C(6) H(7) 3.2573 ? . . C(6) H(9) 2.0065 ? . . C(6) H(10) 2.8975 ? . . C(6) H(11) 3.2746 ? . . C(6) H(12) 2.5161 ? . . C(6) H(13) 2.8797 ? . . C(6) H(14) 3.2316 ? . . C(6) H(15) 2.4328 ? . . C(6) H(28) 3.2220 ? . 66603 C(7) H(7) 2.0152 ? . . C(7) H(8) 3.2279 ? . . C(7) H(9) 3.2313 ? . . C(7) H(10) 3.3642 ? . . C(7) H(12) 2.4016 ? . . C(7) H(12) 3.2608 ? . 56603 C(7) H(13) 3.3082 ? . . C(7) H(15) 3.2782 ? . . C(7) H(30) 3.1807 ? . 66603 C(8) H(6) 2.0125 ? . . C(8) H(8) 2.0184 ? . . C(8) H(12) 3.2811 ? . 56603 C(8) H(18) 3.5332 ? . 55502 C(8) H(25) 3.3321 ? . 45404 C(8) H(30) 3.2843 ? . 66603 C(9) H(6) 3.2323 ? . . C(9) H(7) 2.0281 ? . . C(9) H(16) 3.1995 ? . . C(9) H(18) 3.1955 ? . 55502 C(9) H(19) 3.2054 ? . . C(9) H(20) 3.0823 ? . . C(9) H(22) 2.5972 ? . . C(9) H(23) 3.3674 ? . 66603 C(9) H(24) 3.0929 ? . 45404 C(10) H(1) 3.2361 ? . . C(10) H(7) 3.2572 ? . . C(10) H(8) 2.0102 ? . . C(10) H(16) 2.0216 ? . . C(10) H(17) 2.9002 ? . . C(10) H(18) 3.2398 ? . . C(10) H(19) 2.4934 ? . . C(10) H(20) 2.9570 ? . . C(10) H(21) 3.3002 ? . . C(10) H(22) 2.5532 ? . . C(10) H(24) 3.5238 ? . 45404 C(10) H(29) 3.3535 ? . 66603 C(11) H(1) 3.3359 ? . . C(11) H(6) 2.6607 ? . . C(11) H(10) 2.0269 ? . . C(11) H(11) 2.0512 ? . . C(11) H(12) 2.0454 ? . . C(11) H(13) 2.0021 ? . . C(11) H(14) 2.0012 ? . . C(11) H(15) 1.9696 ? . . C(12) H(6) 2.5898 ? . . C(12) H(6) 3.5561 ? . 56603 C(12) H(7) 3.1464 ? . 56603 C(12) H(9) 2.0321 ? . . C(12) H(13) 2.4612 ? . . C(12) H(14) 2.8273 ? . . C(12) H(15) 3.2097 ? . . C(12) H(20) 3.5432 ? . 55504 C(12) H(21) 3.1695 ? . 55504 C(12) H(34) 3.3726 ? . 65602 C(12) H(39) 3.3543 ? . . C(13) H(6) 3.2835 ? . . C(13) H(9) 1.9725 ? . . C(13) H(10) 3.1767 ? . . C(13) H(11) 2.4427 ? . . C(13) H(12) 2.8880 ? . . C(13) H(15) 3.2644 ? . 55603 C(13) H(19) 3.0914 ? . 55603 C(13) H(24) 3.2844 ? . 64602 C(14) H(2) 3.0212 ? . 65603 C(14) H(8) 2.6859 ? . . C(14) H(17) 2.0415 ? . . C(14) H(18) 2.0209 ? . . C(14) H(19) 2.0515 ? . . C(14) H(20) 2.0565 ? . . C(14) H(21) 2.0489 ? . . C(14) H(22) 2.0443 ? . . C(15) H(2) 2.8910 ? . 65603 C(15) H(8) 3.5714 ? . . C(15) H(8) 3.1992 ? . 54502 C(15) H(13) 3.2462 ? . 55603 C(15) H(16) 2.0153 ? . . C(15) H(20) 2.5465 ? . . C(15) H(21) 2.8877 ? . . C(15) H(22) 3.2834 ? . . C(15) H(24) 3.4829 ? . 45404 C(15) H(32) 3.2284 ? . 65603 C(16) H(8) 2.5435 ? . . C(16) H(11) 2.7792 ? . 55404 C(16) H(16) 2.0270 ? . . C(16) H(17) 3.2519 ? . . C(16) H(18) 2.4645 ? . . C(16) H(19) 2.9761 ? . . C(16) H(34) 3.4989 ? . 65603 C(16) H(37) 3.5349 ? . 55404 C(17) H(2) 2.4266 ? . . C(17) H(17) 3.2265 ? . 65603 C(17) H(23) 3.2638 ? . . C(17) H(25) 3.2621 ? . . C(17) H(26) 2.5938 ? . . C(17) H(32) 3.3955 ? . . C(17) H(33) 2.6180 ? . . C(17) H(35) 3.4143 ? . 65602 C(17) H(39) 2.9734 ? . . C(18) H(2) 3.0573 ? . . C(18) H(17) 3.2633 ? . 65603 C(18) H(23) 2.0320 ? . . C(18) H(24) 3.2828 ? . . C(18) H(26) 2.0151 ? . . C(18) H(27) 2.9229 ? . . C(18) H(28) 3.2696 ? . . C(18) H(29) 2.5068 ? . . C(18) H(30) 2.9240 ? . . C(18) H(31) 3.2714 ? . . C(18) H(32) 2.5243 ? . . C(18) H(35) 3.4135 ? . 65602 C(19) H(20) 3.5276 ? . 65504 C(19) H(24) 2.0334 ? . . C(19) H(25) 3.2560 ? . . C(19) H(26) 3.2711 ? . . C(19) H(29) 2.5927 ? . . C(19) H(30) 3.1613 ? . . C(19) H(32) 3.0924 ? . . C(19) H(35) 3.5392 ? . 65602 C(19) H(38) 3.3786 ? . 65602 C(20) H(8) 3.0758 ? . 65504 C(20) H(14) 3.2401 ? . 65602 C(20) H(19) 3.4845 ? . 65504 C(20) H(23) 2.0194 ? . . C(20) H(25) 2.0371 ? . . C(20) H(38) 3.0144 ? . 65602 C(21) H(7) 3.4348 ? . 65504 C(21) H(8) 3.4888 ? . 65504 C(21) H(18) 3.5974 ? . 65603 C(21) H(23) 3.2503 ? . . C(21) H(24) 2.0358 ? . . C(21) H(33) 3.2480 ? . . C(21) H(34) 3.4196 ? . . C(21) H(36) 2.4352 ? . . C(21) H(37) 3.3443 ? . . C(21) H(38) 3.4857 ? . 65602 C(21) H(39) 3.3180 ? . . C(22) H(2) 3.2746 ? . . C(22) H(18) 3.5926 ? . 65603 C(22) H(24) 3.2672 ? . . C(22) H(25) 2.0400 ? . . C(22) H(33) 2.0458 ? . . C(22) H(34) 2.9678 ? . . C(22) H(35) 3.2649 ? . . C(22) H(35) 3.5152 ? . 65602 C(22) H(36) 2.4982 ? . . C(22) H(37) 2.8846 ? . . C(22) H(38) 3.2092 ? . . C(22) H(39) 2.4309 ? . . C(23) H(2) 3.3309 ? . . C(23) H(23) 2.6566 ? . . C(23) H(27) 2.0620 ? . . C(23) H(27) 3.0038 ? . 66603 C(23) H(28) 2.0522 ? . . C(23) H(29) 2.0422 ? . . C(23) H(30) 2.0451 ? . . C(23) H(31) 2.0331 ? . . C(23) H(32) 2.0298 ? . . C(24) H(1) 2.7958 ? . 66603 C(24) H(23) 2.8518 ? . . C(24) H(26) 2.0205 ? . . C(24) H(26) 3.1614 ? . 66603 C(24) H(27) 2.8334 ? . 66603 C(24) H(30) 2.5054 ? . . C(24) H(31) 2.8419 ? . . C(24) H(32) 3.2643 ? . . C(25) H(2) 3.5656 ? . . C(25) H(5) 3.2422 ? . 65603 C(25) H(6) 3.3540 ? . 65501 C(25) H(13) 3.5407 ? . 65501 C(25) H(17) 3.3141 ? . 65603 C(25) H(23) 3.0247 ? . . C(25) H(26) 2.0233 ? . . C(25) H(27) 3.2373 ? . . C(25) H(28) 2.4519 ? . . C(25) H(29) 2.9130 ? . . C(26) H(3) 3.4911 ? . . C(26) H(25) 2.6917 ? . . C(26) H(34) 2.0412 ? . . C(26) H(35) 1.9623 ? . . C(26) H(36) 1.9502 ? . . C(26) H(37) 1.9787 ? . . C(26) H(38) 1.9247 ? . . C(26) H(39) 1.9317 ? . . C(27) H(10) 3.2351 ? . 64602 C(27) H(21) 3.4311 ? . 65603 C(27) H(25) 2.6413 ? . . C(27) H(33) 1.9144 ? . . C(27) H(37) 2.3782 ? . . C(27) H(38) 2.6484 ? . . C(27) H(39) 3.1113 ? . . C(27) H(39) 3.1135 ? . 64602 C(28) H(21) 3.1895 ? . 55504 C(28) H(22) 3.5628 ? . 55504 C(28) H(25) 3.3383 ? . . C(28) H(33) 1.9607 ? . . C(28) H(34) 3.1103 ? . . C(28) H(34) 3.1484 ? . 65602 C(28) H(35) 2.2607 ? . . C(28) H(36) 2.7107 ? . . H(1) C(1) 3.0071 ? . 65603 H(1) C(4) 2.9692 ? . 65603 H(1) C(24) 2.7958 ? . 66603 H(2) N(1) 2.6105 ? . 65603 H(2) C(1) 2.6681 ? . 65603 H(2) C(2) 2.6620 ? . 65603 H(2) C(4) 3.0734 ? . 65603 H(2) C(14) 3.0212 ? . 65603 H(2) C(15) 2.8910 ? . 65603 H(3) C(1) 3.3106 ? . 65603 H(4) N(1) 3.5246 ? . 65603 H(4) N(2) 3.5270 ? . 65603 H(4) C(1) 2.5413 ? . 65603 H(4) C(2) 2.5117 ? . 65603 H(4) C(3) 2.9085 ? . 65603 H(5) C(1) 2.9932 ? . 65603 H(5) C(3) 2.9907 ? . 65603 H(5) C(25) 3.2422 ? . 65603 H(6) C(12) 3.5561 ? . 56603 H(6) C(25) 3.3540 ? . 45501 H(7) C(12) 3.1464 ? . 56603 H(7) C(21) 3.4348 ? . 45404 H(8) C(15) 3.1992 ? . 55502 H(8) C(20) 3.0758 ? . 45404 H(8) C(21) 3.4888 ? . 45404 H(10) C(27) 3.2351 ? . 65602 H(11) C(16) 2.7792 ? . 55504 H(12) C(7) 3.2608 ? . 56603 H(12) C(8) 3.2811 ? . 56603 H(13) C(15) 3.2462 ? . 55603 H(13) C(25) 3.5407 ? . 45501 H(14) C(20) 3.2401 ? . 64602 H(15) C(13) 3.2644 ? . 55603 H(16) C(3) 3.0971 ? . 65603 H(17) C(3) 3.0700 ? . 65603 H(17) C(17) 3.2265 ? . 65603 H(17) C(18) 3.2633 ? . 65603 H(17) C(25) 3.3141 ? . 65603 H(18) C(8) 3.5332 ? . 54502 H(18) C(9) 3.1955 ? . 54502 H(18) C(21) 3.5974 ? . 65603 H(18) C(22) 3.5926 ? . 65603 H(19) C(13) 3.0914 ? . 55603 H(19) C(20) 3.4845 ? . 45404 H(20) C(12) 3.5432 ? . 55404 H(20) C(19) 3.5276 ? . 45404 H(21) C(12) 3.1695 ? . 55404 H(21) C(27) 3.4311 ? . 65603 H(21) C(28) 3.1895 ? . 55404 H(22) C(28) 3.5628 ? . 55404 H(23) C(9) 3.3674 ? . 66603 H(24) C(9) 3.0929 ? . 65504 H(24) C(10) 3.5238 ? . 65504 H(24) C(13) 3.2844 ? . 65602 H(24) C(15) 3.4829 ? . 65504 H(25) C(8) 3.3321 ? . 65504 H(26) C(4) 3.4202 ? . 65603 H(26) C(24) 3.1614 ? . 66603 H(27) C(23) 3.0038 ? . 66603 H(27) C(24) 2.8334 ? . 66603 H(28) C(2) 3.3373 ? . 66603 H(28) C(5) 3.3270 ? . 66603 H(28) C(6) 3.2220 ? . 66603 H(29) C(2) 3.5683 ? . 66603 H(29) C(5) 3.4182 ? . 66603 H(29) C(10) 3.3535 ? . 66603 H(30) C(7) 3.1807 ? . 66603 H(30) C(8) 3.2843 ? . 66603 H(31) C(4) 3.3851 ? . 65603 H(32) C(15) 3.2284 ? . 65603 H(34) C(12) 3.3726 ? . 64602 H(34) C(16) 3.4989 ? . 65603 H(34) C(28) 3.1484 ? . 64602 H(35) C(17) 3.4143 ? . 64602 H(35) C(18) 3.4135 ? . 64602 H(35) C(19) 3.5392 ? . 64602 H(35) C(22) 3.5152 ? . 64602 H(37) C(16) 3.5349 ? . 55504 H(38) C(19) 3.3786 ? . 64602 H(38) C(20) 3.0144 ? . 64602 H(38) C(21) 3.4857 ? . 64602 H(39) C(27) 3.1135 ? . 65602 loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 C(5) N(1) C(2) C(1) 175.63(9) ? . . . . C(2) N(1) C(5) C(6) -83.8(1) ? . . . . C(2) N(1) C(5) C(10) 98.6(1) ? . . . . C(17) N(2) C(3) C(1) 176.27(9) ? . . . . C(3) N(2) C(17) C(18) 84.2(1) ? . . . . C(3) N(2) C(17) C(22) -98.5(1) ? . . . . C(3) C(1) C(2) N(1) -143.7(1) ? . . . . C(4) C(1) C(2) N(1) -25.6(1) ? . . . . C(2) C(1) C(3) N(2) 26.3(1) ? . . . . C(4) C(1) C(3) N(2) -93.1(1) ? . . . . N(1) C(5) C(6) C(7) -177.9(1) ? . . . . N(1) C(5) C(6) C(11) 1.7(2) ? . . . . C(10) C(5) C(6) C(7) -0.4(2) ? . . . . C(10) C(5) C(6) C(11) 179.2(1) ? . . . . N(1) C(5) C(10) C(9) 178.39(9) ? . . . . N(1) C(5) C(10) C(14) 0.1(1) ? . . . . C(6) C(5) C(10) C(9) 0.9(1) ? . . . . C(6) C(5) C(10) C(14) -177.41(9) ? . . . . C(5) C(6) C(7) C(8) 0.3(2) ? . . . . C(11) C(6) C(7) C(8) -179.3(1) ? . . . . C(5) C(6) C(11) C(12) 144.7(2) ? . . . . C(5) C(6) C(11) C(13) -92.0(2) ? . . . . C(7) C(6) C(11) C(12) -35.7(2) ? . . . . C(7) C(6) C(11) C(13) 87.7(2) ? . . . . C(6) C(7) C(8) C(9) -0.7(2) ? . . . . C(7) C(8) C(9) C(10) 1.3(2) ? . . . . C(8) C(9) C(10) C(5) -1.3(2) ? . . . . C(8) C(9) C(10) C(14) 176.9(1) ? . . . . C(5) C(10) C(14) C(15) 74.7(1) ? . . . . C(5) C(10) C(14) C(16) -160.3(1) ? . . . . C(9) C(10) C(14) C(15) -103.5(1) ? . . . . C(9) C(10) C(14) C(16) 21.4(1) ? . . . . N(2) C(17) C(18) C(19) -179.8(1) ? . . . . N(2) C(17) C(18) C(23) -0.4(2) ? . . . . C(22) C(17) C(18) C(19) 3.0(2) ? . . . . C(22) C(17) C(18) C(23) -177.6(1) ? . . . . N(2) C(17) C(22) C(21) 179.7(1) ? . . . . N(2) C(17) C(22) C(26) -0.2(2) ? . . . . C(18) C(17) C(22) C(21) -3.1(2) ? . . . . C(18) C(17) C(22) C(26) 177.0(1) ? . . . . C(17) C(18) C(19) C(20) -0.9(2) ? . . . . C(23) C(18) C(19) C(20) 179.7(1) ? . . . . C(17) C(18) C(23) C(24) 124.0(1) ? . . . . C(17) C(18) C(23) C(25) -112.9(1) ? . . . . C(19) C(18) C(23) C(24) -56.6(1) ? . . . . C(19) C(18) C(23) C(25) 66.5(1) ? . . . . C(18) C(19) C(20) C(21) -1.0(2) ? . . . . C(19) C(20) C(21) C(22) 1.0(2) ? . . . . C(20) C(21) C(22) C(17) 1.0(2) ? . . . . C(20) C(21) C(22) C(26) -179.0(1) ? . . . . C(17) C(22) C(26) C(27) 146.3(2) ? . . . . C(17) C(22) C(26) C(28) -90.8(2) ? . . . . C(21) C(22) C(26) C(27) -33.6(2) ? . . . . C(21) C(22) C(26) C(28) 89.3(2) ? . . . .
1100781.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $ #$Revision: 176435 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100781.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100781 loop_ _publ_author_name 'Chizu Shimokawa' 'Shinobu Itoh' _publ_section_title ; The First \b-Diketiminate-Ag(I) Complexes. Macrocyclic Dinuclear and Tetranuclear Ag(I)-Complexes and Linear Coordination Polymer Ag(I)-Complex ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3010 _journal_page_last 3012 _journal_paper_doi 10.1021/ic0501014 _journal_volume 44 _journal_year 2005 _chemical_formula_moiety 'C56 H78 Ag2 Cl4 N4 ' _chemical_formula_sum 'C56 H78 Ag2 Cl4 N4' _chemical_formula_weight 1164.81 _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _cell_angle_alpha 82.84(3) _cell_angle_beta 83.35(3) _cell_angle_gamma 85.24(3) _cell_formula_units_Z 2 _cell_length_a 11.160(8) _cell_length_b 12.854(9) _cell_length_c 21.44(2) _cell_measurement_reflns_used 18481 _cell_measurement_temperature 153.1 _cell_measurement_theta_max 27.5 _cell_measurement_theta_min 3.1 _cell_volume 3024(4) _computing_cell_refinement PROCESS-AUTO _computing_data_collection PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_molecular_graphics ORTEP3 _computing_publication_material 'CrystalStructure 3.6.0' _computing_structure_refinement CRYSTALS _computing_structure_solution SIR92 _diffrn_detector_area_resol_mean 10.00 _diffrn_measured_fraction_theta_full 0.9758 _diffrn_measured_fraction_theta_max 0.9758 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents 0.064 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_number 29183 _diffrn_reflns_theta_full 27.48 _diffrn_reflns_theta_max 27.48 _exptl_absorpt_coefficient_mu 0.858 _exptl_absorpt_correction_T_max 0.918 _exptl_absorpt_correction_T_min 0.280 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.279 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 1208.00 _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _refine_diff_density_max 4.37 _refine_diff_density_min -1.89 _refine_ls_extinction_coef 248(57) _refine_ls_extinction_method 'Larson (1970) Crystallographic Computing eq. 22' _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_hydrogen_treatment refall _refine_ls_number_parameters 674 _refine_ls_number_reflns 7678 _refine_ls_R_factor_gt 0.0640 _refine_ls_shift/su_max 0.0000 _refine_ls_structure_factor_coef F _refine_ls_weighting_details 'w = 1/[0.0005Fo^2^ + 1.4000\s(Fo^2^)]' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.0650 _reflns_number_gt 7678 _reflns_number_total 27911 _reflns_threshold_expression F^2^>2.0\s(F^2^) _cod_data_source_file ic0501014si20050122_011347_2.cif _cod_data_source_block '__Ag2(L3)2(CH2Cl2)2' _cod_original_cell_volume 3023(3) _cod_original_formula_sum 'C56 H78 Ag2 Cl4 N4 ' _cod_database_code 1100781 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag(1) Ag 0.89202(7) 0.08546(6) 0.59391(4) 0.0249(2) Uani 1.00 1 d . . . Ag(2) Ag 0.59893(7) 0.39884(6) -0.08768(4) 0.0210(2) Uani 1.00 1 d . . . Cl(1) Cl 0.6423(3) 0.2296(3) 0.1523(1) 0.063(1) Uani 1.00 1 d . . . Cl(2) Cl 0.4944(4) 0.2488(3) 0.0492(1) 0.066(1) Uani 1.00 1 d . . . Cl(3) Cl 0.2371(3) 0.6838(3) 0.2111(1) 0.0508(9) Uani 1.00 1 d . . . Cl(4) Cl 0.2806(3) 0.8487(2) 0.2872(2) 0.058(1) Uani 1.00 1 d . . . N(1) N 0.8956(7) 0.2315(6) 0.5366(4) 0.033(2) Uani 1.00 1 d . . . N(2) N 1.1003(7) 0.0685(6) 0.3587(3) 0.029(2) Uani 1.00 1 d . . . N(3) N 0.7635(6) 0.4212(5) -0.0547(3) 0.025(2) Uani 1.00 1 d . . . N(4) N 0.5774(7) 0.6112(5) 0.1135(3) 0.024(2) Uani 1.00 1 d . . . C(1) C 1.0001(8) 0.1461(7) 0.4477(4) 0.024(3) Uani 1.00 1 d . . . C(2) C 0.9446(8) 0.2339(7) 0.4763(4) 0.025(3) Uani 1.00 1 d . . . C(3) C 1.0504(8) 0.1494(6) 0.3877(4) 0.024(3) Uani 1.00 1 d . . . C(4) C 0.8466(8) 0.3246(6) 0.5572(4) 0.022(2) Uani 1.00 1 d . . . C(5) C 0.913(1) 0.3874(7) 0.5842(4) 0.036(3) Uani 1.00 1 d . . . C(6) C 0.858(1) 0.4845(8) 0.6064(6) 0.051(4) Uani 1.00 1 d . . . C(7) C 0.740(1) 0.5161(7) 0.5959(5) 0.043(3) Uani 1.00 1 d . . . C(8) C 0.6701(9) 0.4491(8) 0.5705(5) 0.036(3) Uani 1.00 1 d . . . C(9) C 0.7227(8) 0.3556(7) 0.5515(4) 0.022(3) Uani 1.00 1 d . . . C(10) C 1.043(1) 0.3548(8) 0.5946(4) 0.030(3) Uani 1.00 1 d . . . C(11) C 1.053(1) 0.2959(9) 0.6646(6) 0.053(4) Uani 1.00 1 d . . . C(12) C 1.124(1) 0.439(1) 0.5876(6) 0.063(4) Uani 1.00 1 d . . . C(13) C 0.6440(8) 0.2830(9) 0.5202(5) 0.030(3) Uani 1.00 1 d . . . C(14) C 0.512(1) 0.282(1) 0.5553(7) 0.073(5) Uani 1.00 1 d . . . C(15) C 0.645(1) 0.319(1) 0.4505(5) 0.054(4) Uani 1.00 1 d . . . C(16) C 1.153(1) 0.0856(8) 0.2956(4) 0.031(3) Uani 1.00 1 d . . . C(17) C 1.0770(9) 0.0752(8) 0.2470(4) 0.036(3) Uani 1.00 1 d . . . C(18) C 1.133(1) 0.0935(7) 0.1833(4) 0.042(3) Uani 1.00 1 d . . . C(19) C 1.250(1) 0.1155(8) 0.1700(5) 0.040(3) Uani 1.00 1 d . . . C(20) C 1.319(1) 0.1210(8) 0.2158(5) 0.048(3) Uani 1.00 1 d . . . C(21) C 1.268(1) 0.1051(7) 0.2789(4) 0.038(3) Uani 1.00 1 d . . . C(22) C 0.948(1) 0.0485(7) 0.2625(5) 0.031(3) Uani 1.00 1 d . . . C(23) C 0.858(1) 0.1471(9) 0.2639(6) 0.061(4) Uani 1.00 1 d . . . C(24) C 0.916(1) -0.025(1) 0.2188(6) 0.061(4) Uani 1.00 1 d . . . C(25) C 1.3554(8) 0.1029(7) 0.3343(5) 0.030(3) Uani 1.00 1 d . . . C(26) C 1.485(1) 0.065(1) 0.3135(6) 0.072(5) Uani 1.00 1 d . . . C(27) C 1.343(1) 0.2110(9) 0.3574(6) 0.056(4) Uani 1.00 1 d . . . C(28) C 0.6659(7) 0.5151(6) 0.0286(4) 0.019(2) Uani 1.00 1 d . . . C(29) C 0.7725(7) 0.4785(6) -0.0033(4) 0.015(2) Uani 1.00 1 d . . . C(30) C 0.6763(8) 0.5737(6) 0.0828(4) 0.019(2) Uani 1.00 1 d . . . C(31) C 0.8808(9) 0.3839(7) -0.0884(4) 0.030(3) Uani 1.00 1 d . . . C(32) C 0.9362(9) 0.4476(8) -0.1353(4) 0.031(3) Uani 1.00 1 d . . . C(33) C 1.0395(8) 0.4054(8) -0.1675(5) 0.033(3) Uani 1.00 1 d . . . C(34) C 1.0889(9) 0.3008(7) -0.1579(5) 0.036(3) Uani 1.00 1 d . . . C(35) C 1.0137(8) 0.2339(8) -0.1057(5) 0.032(3) Uani 1.00 1 d . . . C(36) C 0.9155(8) 0.2777(8) -0.0718(4) 0.030(3) Uani 1.00 1 d . . . C(37) C 0.8971(9) 0.5620(7) -0.1493(5) 0.039(3) Uani 1.00 1 d . . . C(38) C 0.971(1) 0.6314(9) -0.1213(6) 0.058(4) Uani 1.00 1 d . . . C(39) C 0.899(1) 0.5933(9) -0.2219(5) 0.049(4) Uani 1.00 1 d . . . C(40) C 0.844(1) 0.2041(8) -0.0246(6) 0.045(4) Uani 1.00 1 d . . . C(41) C 0.785(1) 0.132(1) -0.0508(7) 0.075(5) Uani 1.00 1 d . . . C(42) C 0.925(1) 0.153(1) 0.0278(6) 0.068(4) Uani 1.00 1 d . . . C(43) C 0.6003(7) 0.6645(6) 0.1663(4) 0.013(2) Uani 1.00 1 d . . . C(44) C 0.6203(8) 0.6022(8) 0.2233(4) 0.027(3) Uani 1.00 1 d . . . C(45) C 0.6381(8) 0.6573(9) 0.2735(4) 0.038(3) Uani 1.00 1 d . . . C(46) C 0.6333(8) 0.7638(8) 0.2683(5) 0.033(3) Uani 1.00 1 d . . . C(47) C 0.6056(7) 0.8201(8) 0.2127(5) 0.031(3) Uani 1.00 1 d . . . C(48) C 0.5888(9) 0.7727(8) 0.1606(5) 0.034(3) Uani 1.00 1 d . . . C(49) C 0.6179(9) 0.4872(8) 0.2301(5) 0.034(3) Uani 1.00 1 d . . . C(50) C 0.695(1) 0.4283(9) 0.2853(5) 0.052(3) Uani 1.00 1 d . . . C(51) C 0.487(1) 0.4515(8) 0.2429(5) 0.039(3) Uani 1.00 1 d . . . C(52) C 0.562(1) 0.8392(8) 0.1004(5) 0.035(3) Uani 1.00 1 d . . . C(53) C 0.678(1) 0.851(1) 0.0575(5) 0.053(4) Uani 1.00 1 d . . . C(54) C 0.493(1) 0.9401(8) 0.1089(6) 0.052(4) Uani 1.00 1 d . . . C(55) C 0.523(1) 0.304(1) 0.1154(6) 0.074(5) Uani 1.00 1 d . . . C(56) C 0.315(1) 0.7124(8) 0.2765(4) 0.041(3) Uani 1.00 1 d . . . H(1) H 0.9971 0.0794 0.4723 0.031 Uiso 1.00 1 c R . . H(2) H 0.9446 0.2996 0.4506 0.029 Uiso 1.00 1 c R . . H(3) H 1.0544 0.2168 0.3640 0.027 Uiso 1.00 1 c R . . H(4) H 0.9017 0.5280 0.6268 0.060 Uiso 1.00 1 c R . . H(5) H 0.7039 0.5815 0.6074 0.050 Uiso 1.00 1 c R . . H(6) H 0.5882 0.4697 0.5643 0.043 Uiso 1.00 1 c R . . H(7) H 1.0729 0.3048 0.5665 0.038 Uiso 1.00 1 c R . . H(8) H 1.0540 0.3453 0.6939 0.064 Uiso 1.00 1 c R . . H(9) H 1.1202 0.2463 0.6679 0.064 Uiso 1.00 1 c R . . H(10) H 0.9801 0.2605 0.6738 0.064 Uiso 1.00 1 c R . . H(11) H 1.1586 0.4483 0.5448 0.077 Uiso 1.00 1 c R . . H(12) H 1.1865 0.4198 0.6143 0.077 Uiso 1.00 1 c R . . H(13) H 1.0828 0.5033 0.5982 0.077 Uiso 1.00 1 c R . . H(14) H 0.6811 0.2136 0.5233 0.038 Uiso 1.00 1 c R . . H(15) H 0.5086 0.2263 0.5887 0.087 Uiso 1.00 1 c R . . H(16) H 0.4588 0.2711 0.5254 0.087 Uiso 1.00 1 c R . . H(17) H 0.4872 0.3468 0.5718 0.087 Uiso 1.00 1 c R . . H(18) H 0.5800 0.3706 0.4454 0.066 Uiso 1.00 1 c R . . H(19) H 0.6355 0.2622 0.4277 0.066 Uiso 1.00 1 c R . . H(20) H 0.7193 0.3495 0.4348 0.066 Uiso 1.00 1 c R . . H(21) H 1.0851 0.0886 0.1499 0.049 Uiso 1.00 1 c R . . H(22) H 1.2836 0.1242 0.1271 0.046 Uiso 1.00 1 c R . . H(23) H 1.4007 0.1388 0.2057 0.057 Uiso 1.00 1 c R . . H(24) H 0.9405 0.0120 0.3039 0.038 Uiso 1.00 1 c R . . H(25) H 0.8503 0.1699 0.3047 0.074 Uiso 1.00 1 c R . . H(26) H 0.7794 0.1373 0.2530 0.074 Uiso 1.00 1 c R . . H(27) H 0.8946 0.1986 0.2338 0.074 Uiso 1.00 1 c R . . H(28) H 0.8835 0.0166 0.1841 0.072 Uiso 1.00 1 c R . . H(29) H 0.8580 -0.0714 0.2394 0.072 Uiso 1.00 1 c R . . H(30) H 0.9870 -0.0646 0.2040 0.072 Uiso 1.00 1 c R . . H(31) H 1.3188 0.0584 0.3687 0.035 Uiso 1.00 1 c R . . H(32) H 1.4907 -0.0100 0.3215 0.087 Uiso 1.00 1 c R . . H(33) H 1.5378 0.0925 0.3378 0.087 Uiso 1.00 1 c R . . H(34) H 1.5071 0.0851 0.2698 0.087 Uiso 1.00 1 c R . . H(35) H 1.4102 0.2445 0.3348 0.070 Uiso 1.00 1 c R . . H(36) H 1.3472 0.2088 0.4015 0.070 Uiso 1.00 1 c R . . H(37) H 1.2701 0.2491 0.3465 0.070 Uiso 1.00 1 c R . . H(38) H 0.5875 0.5048 0.0183 0.023 Uiso 1.00 1 c R . . H(39) H 0.8480 0.4923 0.0092 0.016 Uiso 1.00 1 c R . . H(40) H 0.7539 0.5813 0.0951 0.021 Uiso 1.00 1 c R . . H(41) H 1.0774 0.4484 -0.2023 0.041 Uiso 1.00 1 c R . . H(42) H 1.1615 0.2747 -0.1801 0.048 Uiso 1.00 1 c R . . H(43) H 1.0403 0.1619 -0.0976 0.037 Uiso 1.00 1 c R . . H(44) H 0.8173 0.5706 -0.1289 0.043 Uiso 1.00 1 c R . . H(45) H 0.9446 0.6362 -0.0780 0.072 Uiso 1.00 1 c R . . H(46) H 0.9731 0.7001 -0.1436 0.072 Uiso 1.00 1 c R . . H(47) H 1.0498 0.5969 -0.1251 0.072 Uiso 1.00 1 c R . . H(48) H 0.9738 0.6227 -0.2364 0.059 Uiso 1.00 1 c R . . H(49) H 0.8344 0.6448 -0.2295 0.059 Uiso 1.00 1 c R . . H(50) H 0.8911 0.5348 -0.2438 0.059 Uiso 1.00 1 c R . . H(51) H 0.7775 0.2451 -0.0058 0.053 Uiso 1.00 1 c R . . H(52) H 0.7077 0.1563 -0.0626 0.090 Uiso 1.00 1 c R . . H(53) H 0.7793 0.0686 -0.0228 0.090 Uiso 1.00 1 c R . . H(54) H 0.8380 0.1184 -0.0876 0.090 Uiso 1.00 1 c R . . H(55) H 0.9614 0.0877 0.0165 0.079 Uiso 1.00 1 c R . . H(56) H 0.8740 0.1419 0.0663 0.079 Uiso 1.00 1 c R . . H(57) H 0.9862 0.1976 0.0330 0.079 Uiso 1.00 1 c R . . H(58) H 0.6568 0.6183 0.3122 0.046 Uiso 1.00 1 c R . . H(59) H 0.6454 0.7971 0.3040 0.040 Uiso 1.00 1 c R . . H(60) H 0.5993 0.8945 0.2107 0.040 Uiso 1.00 1 c R . . H(61) H 0.6554 0.4642 0.1916 0.041 Uiso 1.00 1 c R . . H(62) H 0.7777 0.4156 0.2696 0.060 Uiso 1.00 1 c R . . H(63) H 0.6624 0.3636 0.3022 0.060 Uiso 1.00 1 c R . . H(64) H 0.6899 0.4735 0.3175 0.060 Uiso 1.00 1 c R . . H(65) H 0.4643 0.4403 0.2872 0.045 Uiso 1.00 1 c R . . H(66) H 0.4862 0.3872 0.2254 0.045 Uiso 1.00 1 c R . . H(67) H 0.4309 0.5021 0.2240 0.045 Uiso 1.00 1 c R . . H(68) H 0.5148 0.7994 0.0793 0.043 Uiso 1.00 1 c R . . H(69) H 0.7053 0.9157 0.0650 0.064 Uiso 1.00 1 c R . . H(70) H 0.6676 0.8529 0.0140 0.064 Uiso 1.00 1 c R . . H(71) H 0.7354 0.7952 0.0689 0.064 Uiso 1.00 1 c R . . H(72) H 0.4086 0.9300 0.1136 0.064 Uiso 1.00 1 c R . . H(73) H 0.5103 0.9937 0.0751 0.064 Uiso 1.00 1 c R . . H(74) H 0.5149 0.9601 0.1469 0.064 Uiso 1.00 1 c R . . H(75) H 0.4538 0.2931 0.1448 0.092 Uiso 1.00 1 c R . . H(76) H 0.5349 0.3766 0.1069 0.092 Uiso 1.00 1 c R . . H(77) H 0.2822 0.6721 0.3139 0.051 Uiso 1.00 1 c R . . H(78) H 0.3995 0.6962 0.2699 0.051 Uiso 1.00 1 c R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ag(1) 0.0335(5) 0.0194(5) 0.0202(5) 0.0013(4) 0.0025(4) -0.0032(4) Ag(2) 0.0184(5) 0.0219(5) 0.0233(5) 0.0007(3) -0.0007(4) -0.0077(4) Cl(1) 0.057(2) 0.082(2) 0.052(2) -0.010(2) -0.014(2) -0.003(2) Cl(2) 0.087(3) 0.070(2) 0.046(2) -0.026(2) -0.020(2) 0.002(2) Cl(3) 0.038(2) 0.083(2) 0.037(2) -0.004(2) -0.002(1) -0.031(2) Cl(4) 0.071(2) 0.033(2) 0.065(2) 0.000(1) 0.023(2) -0.018(1) N(1) 0.021(4) 0.040(5) 0.036(5) 0.006(4) -0.000(4) -0.005(4) N(2) 0.033(5) 0.030(4) 0.021(4) -0.012(4) 0.012(4) 0.002(3) N(3) 0.025(4) 0.020(4) 0.025(4) 0.009(3) 0.010(3) 0.002(3) N(4) 0.030(4) 0.021(4) 0.023(4) 0.003(3) -0.019(4) -0.003(3) C(1) 0.029(5) 0.016(5) 0.031(5) -0.004(4) -0.005(5) -0.010(4) C(2) 0.029(5) 0.030(5) 0.014(5) -0.004(4) -0.004(4) 0.005(4) C(3) 0.028(5) 0.006(4) 0.035(6) 0.001(4) 0.008(5) -0.000(4) C(4) 0.030(5) 0.014(5) 0.017(5) 0.010(4) 0.007(4) -0.004(4) C(5) 0.071(8) 0.023(5) 0.020(5) 0.002(5) -0.013(5) -0.016(4) C(6) 0.074(8) 0.019(6) 0.057(7) 0.006(6) 0.015(6) -0.014(5) C(7) 0.059(7) 0.017(5) 0.049(7) 0.015(5) 0.004(6) -0.013(5) C(8) 0.026(5) 0.049(7) 0.031(6) 0.010(5) -0.002(5) -0.008(5) C(9) 0.023(6) 0.024(5) 0.016(5) 0.008(4) 0.008(4) -0.007(4) C(10) 0.048(7) 0.030(6) 0.016(5) -0.013(5) 0.011(5) -0.020(4) C(11) 0.064(9) 0.043(7) 0.054(8) -0.005(6) -0.033(7) 0.013(6) C(12) 0.069(9) 0.068(9) 0.056(8) -0.028(7) -0.007(7) -0.007(7) C(13) 0.010(5) 0.055(7) 0.029(6) -0.001(5) -0.004(5) -0.016(5) C(14) 0.07(1) 0.058(9) 0.08(1) 0.006(7) 0.006(8) -0.023(7) C(15) 0.041(7) 0.074(8) 0.049(7) -0.012(6) -0.012(6) -0.002(6) C(16) 0.040(6) 0.039(6) 0.014(5) -0.010(5) 0.009(5) -0.009(4) C(17) 0.037(6) 0.043(6) 0.021(6) -0.006(5) 0.008(5) 0.012(5) C(18) 0.085(9) 0.026(6) 0.013(5) 0.007(6) -0.003(5) -0.001(4) C(19) 0.041(7) 0.043(6) 0.031(6) 0.002(5) 0.016(5) -0.009(5) C(20) 0.049(7) 0.036(6) 0.056(7) -0.008(5) 0.011(6) -0.010(5) C(21) 0.064(8) 0.024(5) 0.017(5) -0.001(5) 0.028(5) -0.002(4) C(22) 0.032(6) 0.036(6) 0.029(6) 0.005(5) -0.017(5) -0.005(5) C(23) 0.09(1) 0.051(7) 0.047(8) -0.025(7) 0.004(7) -0.004(6) C(24) 0.08(1) 0.047(7) 0.058(8) -0.008(7) 0.006(7) -0.003(6) C(25) 0.022(5) 0.028(6) 0.037(6) -0.007(4) 0.006(5) 0.001(4) C(26) 0.041(8) 0.13(1) 0.051(8) -0.022(8) 0.009(6) -0.020(8) C(27) 0.059(8) 0.058(8) 0.057(8) -0.021(6) -0.028(7) -0.007(6) C(28) 0.009(4) 0.025(5) 0.024(5) -0.004(4) 0.008(4) -0.013(4) C(29) 0.002(4) 0.029(5) 0.010(4) 0.013(3) 0.014(3) -0.002(3) C(30) 0.029(5) 0.014(4) 0.009(4) 0.012(4) 0.006(4) 0.006(3) C(31) 0.048(6) 0.021(5) 0.026(6) 0.015(5) -0.027(5) -0.014(4) C(32) 0.040(6) 0.048(6) 0.010(5) -0.006(5) -0.013(5) -0.005(5) C(33) 0.026(5) 0.035(6) 0.041(6) -0.012(4) 0.004(5) -0.015(5) C(34) 0.029(5) 0.019(5) 0.072(7) 0.016(4) -0.041(6) -0.030(5) C(35) 0.016(5) 0.040(6) 0.037(6) 0.011(4) 0.011(5) -0.012(5) C(36) 0.025(5) 0.043(6) 0.020(5) 0.001(5) 0.003(4) -0.007(5) C(37) 0.035(6) 0.040(6) 0.033(6) 0.029(5) 0.007(5) -0.002(5) C(38) 0.064(8) 0.039(7) 0.076(9) -0.002(6) -0.015(7) -0.021(6) C(39) 0.043(7) 0.049(7) 0.056(7) 0.003(6) -0.020(6) -0.008(6) C(40) 0.052(8) 0.023(6) 0.056(8) -0.004(6) -0.011(7) 0.010(6) C(41) 0.044(9) 0.09(1) 0.09(1) -0.012(8) -0.040(9) 0.031(9) C(42) 0.09(1) 0.063(8) 0.043(8) 0.016(8) -0.010(8) 0.012(6) C(43) -0.001(4) 0.018(5) 0.023(5) -0.002(3) 0.001(4) -0.010(4) C(44) 0.021(5) 0.045(6) 0.017(5) -0.012(4) 0.005(4) -0.012(4) C(45) 0.017(5) 0.069(8) 0.029(6) -0.008(5) -0.008(5) -0.006(5) C(46) 0.017(5) 0.048(7) 0.035(6) 0.004(4) 0.007(4) -0.023(5) C(47) 0.004(4) 0.043(6) 0.053(6) 0.007(4) -0.008(4) -0.029(5) C(48) 0.040(6) 0.038(6) 0.021(5) -0.009(5) 0.019(5) -0.009(4) C(49) 0.024(6) 0.053(7) 0.025(6) -0.001(5) -0.005(5) -0.004(5) C(50) 0.060(8) 0.054(7) 0.035(6) 0.011(6) -0.008(6) 0.015(5) C(51) 0.043(7) 0.022(5) 0.047(7) 0.003(5) 0.014(6) -0.005(5) C(52) 0.038(7) 0.028(6) 0.040(7) -0.016(5) -0.023(6) 0.018(5) C(53) 0.040(7) 0.082(9) 0.037(6) -0.040(6) -0.024(6) 0.032(6) C(54) 0.050(7) 0.052(7) 0.056(8) 0.007(6) -0.029(6) -0.007(6) C(55) 0.11(1) 0.060(9) 0.061(9) -0.038(8) -0.001(9) -0.028(7) C(56) 0.071(8) 0.035(6) 0.021(5) -0.019(5) 0.002(5) -0.014(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Ag Ag -0.897 1.101 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 N(2) Ag(1) N(1) 172.9(3) ? 75602 . . Ag(1) N(1) C(2) 118.8(6) ? . . . Ag(1) N(1) C(4) 123.4(6) ? . . . Ag(1) N(2) C(3) 121.3(6) ? . 75602 75602 Ag(1) N(2) C(16) 119.0(6) ? . 75602 75602 N(4) Ag(2) N(3) 173.2(3) ? 66502 . . Ag(2) N(3) C(29) 123.4(5) ? . . . Ag(2) N(3) C(31) 120.6(6) ? . . . Ag(2) N(4) C(30) 124.1(6) ? . 66502 66502 Ag(2) N(4) C(43) 122.9(5) ? . 66502 66502 Cl(1) C(55) Cl(2) 110.6(8) ? . . . Cl(3) C(56) Cl(4) 108.3(5) ? . . . N(1) C(2) C(1) 125.2(8) ? . . . C(4) N(1) C(2) 117.8(7) ? . . . N(1) C(4) C(5) 121.9(8) ? . . . N(1) C(4) C(9) 119.5(8) ? . . . C(3) N(2) Ag(1) 121.3(6) ? . . 75602 C(16) N(2) Ag(1) 119.0(6) ? . . 75602 N(2) C(3) C(1) 126.7(8) ? . . . C(16) N(2) C(3) 119.7(7) ? . . . N(2) C(16) C(17) 117.0(9) ? . . . N(2) C(16) C(21) 124.1(9) ? . . . N(3) C(29) C(28) 117.3(7) ? . . . C(31) N(3) C(29) 115.7(7) ? . . . N(3) C(31) C(32) 119.6(8) ? . . . N(3) C(31) C(36) 114.4(7) ? . . . C(30) N(4) Ag(2) 124.1(6) ? . . 66502 C(43) N(4) Ag(2) 122.9(5) ? . . 66502 N(4) C(30) C(28) 118.7(8) ? . . . C(43) N(4) C(30) 113.0(7) ? . . . N(4) C(43) C(44) 117.6(7) ? . . . N(4) C(43) C(48) 119.1(7) ? . . . C(3) C(1) C(2) 124.9(8) ? . . . C(9) C(4) C(5) 118.6(8) ? . . . C(4) C(5) C(10) 120.4(8) ? . . . C(4) C(5) C(6) 120(1) ? . . . C(4) C(9) C(13) 119.3(8) ? . . . C(4) C(9) C(8) 121.5(9) ? . . . C(10) C(5) C(6) 118(1) ? . . . C(5) C(6) C(7) 119(1) ? . . . C(5) C(10) C(11) 111.1(8) ? . . . C(5) C(10) C(12) 116.1(9) ? . . . C(6) C(7) C(8) 119.9(9) ? . . . C(7) C(8) C(9) 119.7(9) ? . . . C(8) C(9) C(13) 119.1(8) ? . . . C(9) C(13) C(15) 109.7(8) ? . . . C(9) C(13) C(14) 110.2(9) ? . . . C(12) C(10) C(11) 105.3(9) ? . . . C(15) C(13) C(14) 112.4(9) ? . . . C(21) C(16) C(17) 118.8(8) ? . . . C(16) C(17) C(22) 121.8(8) ? . . . C(16) C(17) C(18) 115(1) ? . . . C(16) C(21) C(25) 118.2(8) ? . . . C(16) C(21) C(20) 123(1) ? . . . C(22) C(17) C(18) 122(1) ? . . . C(17) C(18) C(19) 121(1) ? . . . C(17) C(22) C(23) 113.0(9) ? . . . C(17) C(22) C(24) 110.5(9) ? . . . C(18) C(19) C(20) 121(1) ? . . . C(19) C(20) C(21) 118(1) ? . . . C(20) C(21) C(25) 118(1) ? . . . C(21) C(25) C(27) 108.0(8) ? . . . C(21) C(25) C(26) 112.3(9) ? . . . C(24) C(22) C(23) 112(1) ? . . . C(27) C(25) C(26) 114(1) ? . . . C(30) C(28) C(29) 116.9(8) ? . . . C(36) C(31) C(32) 125.5(9) ? . . . C(31) C(32) C(37) 123.0(8) ? . . . C(31) C(32) C(33) 116.5(9) ? . . . C(31) C(36) C(40) 124.6(8) ? . . . C(31) C(36) C(35) 118.2(8) ? . . . C(37) C(32) C(33) 120.3(8) ? . . . C(32) C(33) C(34) 126.4(9) ? . . . C(32) C(37) C(38) 112.6(9) ? . . . C(32) C(37) C(39) 110.5(8) ? . . . C(33) C(34) C(35) 112.3(8) ? . . . C(34) C(35) C(36) 120.9(8) ? . . . C(35) C(36) C(40) 116.7(9) ? . . . C(36) C(40) C(41) 114(1) ? . . . C(36) C(40) C(42) 109(1) ? . . . C(39) C(37) C(38) 110.7(9) ? . . . C(42) C(40) C(41) 113(1) ? . . . C(48) C(43) C(44) 122.9(8) ? . . . C(43) C(44) C(49) 121.8(8) ? . . . C(43) C(44) C(45) 115.6(9) ? . . . C(43) C(48) C(52) 123.0(9) ? . . . C(43) C(48) C(47) 117.3(9) ? . . . C(49) C(44) C(45) 122.6(8) ? . . . C(44) C(45) C(46) 122.5(9) ? . . . C(44) C(49) C(51) 112.0(8) ? . . . C(44) C(49) C(50) 113.3(9) ? . . . C(45) C(46) C(47) 119(1) ? . . . C(46) C(47) C(48) 122.4(9) ? . . . C(47) C(48) C(52) 119.7(9) ? . . . C(48) C(52) C(53) 108.9(9) ? . . . C(48) C(52) C(54) 115.1(9) ? . . . C(51) C(49) C(50) 108.5(8) ? . . . C(54) C(52) C(53) 113.3(9) ? . . . Cl(1) C(55) H(75) 104.5030 ? . . . Cl(1) C(55) H(76) 113.7546 ? . . . Cl(2) C(55) H(75) 104.9240 ? . . . Cl(2) C(55) H(76) 112.8456 ? . . . Cl(3) C(56) H(77) 108.1743 ? . . . Cl(3) C(56) H(78) 112.3216 ? . . . Cl(4) C(56) H(77) 107.2035 ? . . . Cl(4) C(56) H(78) 111.2099 ? . . . N(1) C(2) H(2) 118.3285 ? . . . N(2) C(3) H(3) 116.3378 ? . . . N(3) C(29) H(39) 122.5759 ? . . . N(4) C(30) H(40) 121.6961 ? . . . H(1) C(1) C(2) 117.2564 ? . . . C(1) C(2) H(2) 116.4102 ? . . . H(1) C(1) C(3) 117.7305 ? . . . C(1) C(3) H(3) 116.8786 ? . . . C(5) C(6) H(4) 121.7563 ? . . . C(5) C(10) H(7) 108.6962 ? . . . H(4) C(6) C(7) 118.9011 ? . . . C(6) C(7) H(5) 120.8461 ? . . . C(7) C(8) H(6) 120.1390 ? . . . H(5) C(7) C(8) 119.2045 ? . . . H(6) C(8) C(9) 120.0644 ? . . . C(9) C(13) H(14) 108.7542 ? . . . H(7) C(10) C(11) 105.9393 ? . . . C(10) C(11) H(10) 103.3617 ? . . . C(10) C(11) H(8) 110.7210 ? . . . C(10) C(11) H(9) 114.1337 ? . . . H(7) C(10) C(12) 109.1896 ? . . . C(10) C(12) H(11) 108.0038 ? . . . C(10) C(12) H(12) 108.9533 ? . . . C(10) C(12) H(13) 111.4212 ? . . . H(10) C(11) H(8) 109.4672 ? . . . H(9) C(11) H(8) 109.4719 ? . . . H(10) C(11) H(9) 109.4734 ? . . . H(12) C(12) H(11) 109.4771 ? . . . H(13) C(12) H(11) 109.4744 ? . . . H(13) C(12) H(12) 109.4787 ? . . . H(14) C(13) C(14) 109.6007 ? . . . C(13) C(14) H(15) 109.0867 ? . . . C(13) C(14) H(17) 111.6944 ? . . . C(13) C(14) H(16) 107.6033 ? . . . H(14) C(13) C(15) 106.0155 ? . . . C(13) C(15) H(20) 110.1688 ? . . . C(13) C(15) H(18) 107.3454 ? . . . C(13) C(15) H(19) 110.8752 ? . . . H(17) C(14) H(15) 109.4750 ? . . . H(16) C(14) H(15) 109.4714 ? . . . H(17) C(14) H(16) 109.4704 ? . . . H(20) C(15) H(18) 109.4692 ? . . . H(19) C(15) H(18) 109.4716 ? . . . H(20) C(15) H(19) 109.4749 ? . . . C(17) C(18) H(21) 118.2035 ? . . . C(17) C(22) H(24) 107.1315 ? . . . H(21) C(18) C(19) 119.8148 ? . . . C(18) C(19) H(22) 119.0485 ? . . . C(19) C(20) H(23) 120.3094 ? . . . H(22) C(19) C(20) 119.6620 ? . . . H(23) C(20) C(21) 121.0619 ? . . . C(21) C(25) H(31) 104.5441 ? . . . C(22) C(23) H(26) 114.6268 ? . . . C(22) C(23) H(27) 104.4805 ? . . . H(24) C(22) C(23) 106.6460 ? . . . C(22) C(23) H(25) 109.1447 ? . . . H(24) C(22) C(24) 107.0102 ? . . . C(22) C(24) H(28) 107.4580 ? . . . C(22) C(24) H(29) 111.3411 ? . . . C(22) C(24) H(30) 109.5996 ? . . . H(26) C(23) H(25) 109.4660 ? . . . H(27) C(23) H(25) 109.4741 ? . . . H(27) C(23) H(26) 109.4778 ? . . . H(29) C(24) H(28) 109.4660 ? . . . H(30) C(24) H(28) 109.4676 ? . . . H(30) C(24) H(29) 109.4714 ? . . . H(31) C(25) C(26) 112.7476 ? . . . C(25) C(26) H(32) 107.6493 ? . . . C(25) C(26) H(34) 111.8894 ? . . . C(25) C(26) H(33) 108.8415 ? . . . H(31) C(25) C(27) 104.2302 ? . . . C(25) C(27) H(37) 111.4305 ? . . . C(25) C(27) H(36) 113.5717 ? . . . C(25) C(27) H(35) 103.2115 ? . . . H(34) C(26) H(32) 109.4741 ? . . . H(33) C(26) H(32) 109.4736 ? . . . H(34) C(26) H(33) 109.4707 ? . . . H(37) C(27) H(35) 109.4676 ? . . . H(36) C(27) H(35) 109.4744 ? . . . H(37) C(27) H(36) 109.4719 ? . . . H(38) C(28) C(29) 124.5203 ? . . . C(28) C(29) H(39) 120.1149 ? . . . H(38) C(28) C(30) 118.6174 ? . . . C(28) C(30) H(40) 119.6201 ? . . . C(32) C(33) H(41) 117.5293 ? . . . C(32) C(37) H(44) 105.9493 ? . . . H(41) C(33) C(34) 115.7995 ? . . . C(33) C(34) H(42) 124.3212 ? . . . C(34) C(35) H(43) 116.8073 ? . . . H(42) C(34) C(35) 123.3870 ? . . . H(43) C(35) C(36) 122.2786 ? . . . C(36) C(40) H(51) 107.1109 ? . . . H(44) C(37) C(38) 106.2861 ? . . . C(37) C(38) H(45) 111.8829 ? . . . C(37) C(38) H(47) 103.3842 ? . . . C(37) C(38) H(46) 112.9547 ? . . . H(44) C(37) C(39) 110.6567 ? . . . C(37) C(39) H(48) 107.4124 ? . . . C(37) C(39) H(49) 108.7990 ? . . . C(37) C(39) H(50) 112.1505 ? . . . H(47) C(38) H(45) 109.4671 ? . . . H(46) C(38) H(45) 109.4750 ? . . . H(47) C(38) H(46) 109.4785 ? . . . H(49) C(39) H(48) 109.4795 ? . . . H(50) C(39) H(48) 109.4749 ? . . . H(50) C(39) H(49) 109.4755 ? . . . H(51) C(40) C(41) 102.1717 ? . . . C(40) C(41) H(52) 114.3050 ? . . . C(40) C(41) H(54) 103.5998 ? . . . C(40) C(41) H(53) 110.3136 ? . . . H(51) C(40) C(42) 109.2845 ? . . . C(40) C(42) H(56) 107.5694 ? . . . C(40) C(42) H(57) 111.5868 ? . . . C(40) C(42) H(55) 109.2315 ? . . . H(54) C(41) H(52) 109.4671 ? . . . H(53) C(41) H(52) 109.4775 ? . . . H(54) C(41) H(53) 109.4755 ? . . . H(56) C(42) H(55) 109.4702 ? . . . H(57) C(42) H(55) 109.4677 ? . . . H(57) C(42) H(56) 109.4769 ? . . . C(44) C(45) H(58) 118.5680 ? . . . C(44) C(49) H(61) 107.1501 ? . . . H(58) C(45) C(46) 118.8795 ? . . . C(45) C(46) H(59) 118.9864 ? . . . C(46) C(47) H(60) 117.5540 ? . . . H(59) C(46) C(47) 121.9049 ? . . . H(60) C(47) C(48) 120.0732 ? . . . C(48) C(52) H(68) 106.6706 ? . . . H(61) C(49) C(50) 106.2109 ? . . . C(49) C(50) H(63) 110.2832 ? . . . C(49) C(50) H(64) 107.1750 ? . . . C(49) C(50) H(62) 110.9253 ? . . . H(61) C(49) C(51) 109.5345 ? . . . C(49) C(51) H(66) 107.4518 ? . . . C(49) C(51) H(67) 111.4595 ? . . . C(49) C(51) H(65) 109.4724 ? . . . H(63) C(50) H(62) 109.4688 ? . . . H(64) C(50) H(62) 109.4741 ? . . . H(64) C(50) H(63) 109.4755 ? . . . H(66) C(51) H(65) 109.4719 ? . . . H(67) C(51) H(65) 109.4777 ? . . . H(67) C(51) H(66) 109.4690 ? . . . H(68) C(52) C(53) 104.7094 ? . . . C(52) C(53) H(71) 109.8944 ? . . . C(52) C(53) H(69) 104.8609 ? . . . C(52) C(53) H(70) 113.5389 ? . . . H(68) C(52) C(54) 107.3275 ? . . . C(52) C(54) H(72) 109.5836 ? . . . C(52) C(54) H(74) 105.3527 ? . . . C(52) C(54) H(73) 113.3706 ? . . . H(71) C(53) H(69) 109.4722 ? . . . H(70) C(53) H(69) 109.4759 ? . . . H(71) C(53) H(70) 109.4655 ? . . . H(74) C(54) H(72) 109.4707 ? . . . H(73) C(54) H(72) 109.4719 ? . . . H(74) C(54) H(73) 109.4775 ? . . . H(76) C(55) H(75) 109.4539 ? . . . H(78) C(56) H(77) 109.4635 ? . . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Ag(1) N(1) 2.112(7) ? . . Ag(1) N(2) 2.110(7) ? . 75602 Ag(2) N(3) 2.097(8) ? . . Ag(2) N(4) 2.123(8) ? . 66502 Cl(1) C(55) 1.77(1) ? . . Cl(2) C(55) 1.74(2) ? . . Cl(3) C(56) 1.82(1) ? . . Cl(4) C(56) 1.80(1) ? . . N(1) C(2) 1.34(1) ? . . N(1) C(4) 1.38(1) ? . . N(2) Ag(1) 2.110(7) ? . 75602 N(2) C(3) 1.33(1) ? . . N(2) C(16) 1.41(1) ? . . N(3) C(29) 1.41(1) ? . . N(3) C(31) 1.49(1) ? . . N(4) Ag(2) 2.123(8) ? . 66502 N(4) C(30) 1.31(1) ? . . N(4) C(43) 1.45(1) ? . . C(1) C(2) 1.41(1) ? . . C(1) C(3) 1.34(1) ? . . C(4) C(5) 1.36(1) ? . . C(4) C(9) 1.42(1) ? . . C(5) C(6) 1.45(1) ? . . C(5) C(10) 1.51(2) ? . . C(6) C(7) 1.38(2) ? . . C(7) C(8) 1.40(2) ? . . C(8) C(9) 1.38(1) ? . . C(9) C(13) 1.59(1) ? . . C(10) C(11) 1.61(1) ? . . C(10) C(12) 1.46(2) ? . . C(13) C(14) 1.58(2) ? . . C(13) C(15) 1.51(2) ? . . C(16) C(17) 1.44(1) ? . . C(16) C(21) 1.33(2) ? . . C(17) C(18) 1.43(1) ? . . C(17) C(22) 1.50(2) ? . . C(18) C(19) 1.35(2) ? . . C(19) C(20) 1.33(2) ? . . C(20) C(21) 1.41(1) ? . . C(21) C(25) 1.62(1) ? . . C(22) C(23) 1.55(1) ? . . C(22) C(24) 1.50(2) ? . . C(25) C(26) 1.52(1) ? . . C(25) C(27) 1.52(2) ? . . C(28) C(29) 1.38(1) ? . . C(28) C(30) 1.48(1) ? . . C(31) C(32) 1.34(1) ? . . C(31) C(36) 1.40(1) ? . . C(32) C(33) 1.38(1) ? . . C(32) C(37) 1.50(1) ? . . C(33) C(34) 1.41(1) ? . . C(34) C(35) 1.53(1) ? . . C(35) C(36) 1.36(1) ? . . C(36) C(40) 1.50(1) ? . . C(37) C(38) 1.49(2) ? . . C(37) C(39) 1.56(1) ? . . C(40) C(41) 1.38(2) ? . . C(40) C(42) 1.57(2) ? . . C(43) C(44) 1.41(1) ? . . C(43) C(48) 1.38(1) ? . . C(44) C(45) 1.40(1) ? . . C(44) C(49) 1.47(1) ? . . C(45) C(46) 1.36(2) ? . . C(46) C(47) 1.37(1) ? . . C(47) C(48) 1.37(2) ? . . C(48) C(52) 1.50(1) ? . . C(49) C(50) 1.62(1) ? . . C(49) C(51) 1.55(2) ? . . C(52) C(53) 1.50(1) ? . . C(52) C(54) 1.47(1) ? . . C(1) H(1) 0.9500 ? . . C(2) H(2) 0.9500 ? . . C(3) H(3) 0.9500 ? . . C(6) H(4) 0.9500 ? . . C(7) H(5) 0.9499 ? . . C(8) H(6) 0.9500 ? . . C(10) H(7) 0.9500 ? . . C(11) H(8) 0.9499 ? . . C(11) H(9) 0.9500 ? . . C(11) H(10) 0.9500 ? . . C(12) H(11) 0.9499 ? . . C(12) H(12) 0.9500 ? . . C(12) H(13) 0.9500 ? . . C(13) H(14) 0.9500 ? . . C(14) H(15) 0.9501 ? . . C(14) H(16) 0.9499 ? . . C(14) H(17) 0.9500 ? . . C(15) H(18) 0.9500 ? . . C(15) H(19) 0.9500 ? . . C(15) H(20) 0.9500 ? . . C(18) H(21) 0.9502 ? . . C(19) H(22) 0.9500 ? . . C(20) H(23) 0.9500 ? . . C(22) H(24) 0.9500 ? . . C(23) H(25) 0.9499 ? . . C(23) H(26) 0.9500 ? . . C(23) H(27) 0.9501 ? . . C(24) H(28) 0.9500 ? . . C(24) H(29) 0.9499 ? . . C(24) H(30) 0.9500 ? . . C(25) H(31) 0.9501 ? . . C(26) H(32) 0.9500 ? . . C(26) H(33) 0.9500 ? . . C(26) H(34) 0.9501 ? . . C(27) H(35) 0.9500 ? . . C(27) H(36) 0.9501 ? . . C(27) H(37) 0.9500 ? . . C(28) H(38) 0.9500 ? . . C(29) H(39) 0.9500 ? . . C(30) H(40) 0.9500 ? . . C(33) H(41) 0.9500 ? . . C(34) H(42) 0.9500 ? . . C(35) H(43) 0.9499 ? . . C(37) H(44) 0.9500 ? . . C(38) H(45) 0.9501 ? . . C(38) H(46) 0.9500 ? . . C(38) H(47) 0.9500 ? . . C(39) H(48) 0.9500 ? . . C(39) H(49) 0.9500 ? . . C(39) H(50) 0.9500 ? . . C(40) H(51) 0.9500 ? . . C(41) H(52) 0.9500 ? . . C(41) H(53) 0.9501 ? . . C(41) H(54) 0.9499 ? . . C(42) H(55) 0.9500 ? . . C(42) H(56) 0.9500 ? . . C(42) H(57) 0.9500 ? . . C(45) H(58) 0.9500 ? . . C(46) H(59) 0.9501 ? . . C(47) H(60) 0.9500 ? . . C(49) H(61) 0.9500 ? . . C(50) H(62) 0.9500 ? . . C(50) H(63) 0.9500 ? . . C(50) H(64) 0.9500 ? . . C(51) H(65) 0.9499 ? . . C(51) H(66) 0.9499 ? . . C(51) H(67) 0.9500 ? . . C(52) H(68) 0.9500 ? . . C(53) H(69) 0.9500 ? . . C(53) H(70) 0.9501 ? . . C(53) H(71) 0.9500 ? . . C(54) H(72) 0.9500 ? . . C(54) H(73) 0.9500 ? . . C(54) H(74) 0.9501 ? . . C(55) H(75) 0.9500 ? . . C(55) H(76) 0.9501 ? . . C(56) H(77) 0.9499 ? . . C(56) H(78) 0.9500 ? . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Ag(1) Cl(4) 3.170(3) ? . 66602 Ag(1) C(1) 3.249(9) ? . . Ag(1) C(1) 3.306(9) ? . 75602 Ag(1) C(2) 2.997(9) ? . . Ag(1) C(3) 3.020(8) ? . 75602 Ag(1) C(4) 3.092(8) ? . . Ag(1) C(16) 3.050(9) ? . 75602 Ag(2) Cl(2) 3.444(3) ? . . Ag(2) Cl(3) 3.277(3) ? . 66502 Ag(2) C(28) 3.248(9) ? . . Ag(2) C(28) 3.241(8) ? . 66502 Ag(2) C(29) 3.110(8) ? . . Ag(2) C(30) 3.054(9) ? . 66502 Ag(2) C(31) 3.13(1) ? . . Ag(2) C(43) 3.155(8) ? . 66502 Cl(1) Cl(2) 2.884(5) ? . . Cl(1) C(23) 3.59(1) ? . . Cl(2) C(53) 3.57(1) ? . 66502 Cl(3) Ag(2) 3.277(3) ? . 66502 Cl(3) Cl(4) 2.933(5) ? . . Cl(3) C(31) 3.31(1) ? . 66502 Cl(3) C(32) 3.34(1) ? . 66502 Cl(3) C(36) 3.57(1) ? . 66502 Cl(4) Ag(1) 3.170(3) ? . 66602 Cl(4) C(16) 3.27(1) ? . 46501 Cl(4) C(21) 3.27(1) ? . 46501 N(1) C(1) 2.45(1) ? . . N(1) C(5) 2.39(1) ? . . N(1) C(9) 2.42(1) ? . . N(1) C(10) 2.85(1) ? . . N(1) C(13) 2.88(1) ? . . N(1) C(15) 3.55(1) ? . . N(2) C(1) 2.38(1) ? . . N(2) C(17) 2.43(1) ? . . N(2) C(21) 2.41(1) ? . . N(2) C(22) 2.87(1) ? . . N(2) C(23) 3.58(2) ? . . N(2) C(25) 2.89(1) ? . . N(2) C(27) 3.39(2) ? . . N(3) C(28) 2.39(1) ? . . N(3) C(32) 2.45(1) ? . . N(3) C(36) 2.43(1) ? . . N(3) C(37) 2.91(1) ? . . N(3) C(40) 2.88(1) ? . . N(4) C(28) 2.40(1) ? . . N(4) C(44) 2.44(1) ? . . N(4) C(48) 2.44(1) ? . . N(4) C(49) 2.85(1) ? . . N(4) C(51) 3.35(1) ? . . N(4) C(52) 2.90(1) ? . . N(4) C(53) 3.39(1) ? . . C(1) Ag(1) 3.306(9) ? . 75602 C(2) C(3) 2.44(1) ? . . C(2) C(4) 2.33(1) ? . . C(2) C(5) 3.19(1) ? . . C(2) C(9) 3.20(1) ? . . C(2) C(10) 3.46(1) ? . . C(2) C(13) 3.41(1) ? . . C(2) C(15) 3.51(2) ? . . C(3) Ag(1) 3.020(8) ? . 75602 C(3) C(16) 2.37(1) ? . . C(3) C(17) 3.25(1) ? . . C(3) C(21) 3.23(1) ? . . C(3) C(22) 3.47(1) ? . . C(3) C(25) 3.49(1) ? . . C(3) C(27) 3.39(2) ? . . C(4) C(6) 2.44(1) ? . . C(4) C(7) 2.82(1) ? . . C(4) C(8) 2.45(1) ? . . C(4) C(10) 2.49(1) ? . . C(4) C(11) 3.41(2) ? . . C(4) C(13) 2.60(1) ? . . C(4) C(15) 3.40(2) ? . . C(5) C(7) 2.44(1) ? . . C(5) C(8) 2.79(1) ? . . C(5) C(9) 2.39(2) ? . . C(5) C(11) 2.57(2) ? . . C(5) C(12) 2.52(2) ? . . C(6) C(8) 2.41(2) ? . . C(6) C(9) 2.78(2) ? . . C(6) C(10) 2.55(1) ? . . C(6) C(11) 3.34(2) ? . . C(6) C(12) 2.97(2) ? . . C(7) C(9) 2.41(1) ? . . C(8) C(13) 2.56(2) ? . . C(8) C(14) 2.96(2) ? . . C(8) C(15) 3.29(2) ? . . C(9) C(14) 2.60(2) ? . . C(9) C(15) 2.53(2) ? . . C(11) C(12) 2.44(2) ? . . C(14) C(15) 2.56(2) ? . . C(16) Ag(1) 3.050(9) ? . 75602 C(16) Cl(4) 3.27(1) ? . 64501 C(16) C(18) 2.43(1) ? . . C(16) C(19) 2.78(1) ? . . C(16) C(20) 2.41(1) ? . . C(16) C(22) 2.57(2) ? . . C(16) C(23) 3.45(2) ? . . C(16) C(25) 2.53(1) ? . . C(16) C(27) 3.26(2) ? . . C(17) C(19) 2.43(1) ? . . C(17) C(20) 2.80(2) ? . . C(17) C(21) 2.38(2) ? . . C(17) C(23) 2.55(2) ? . . C(17) C(24) 2.47(2) ? . . C(18) C(20) 2.34(2) ? . . C(18) C(21) 2.71(2) ? . . C(18) C(22) 2.57(1) ? . . C(18) C(23) 3.41(2) ? . . C(18) C(24) 2.94(2) ? . . C(19) C(21) 2.35(1) ? . . C(20) C(25) 2.60(2) ? . . C(20) C(26) 2.94(2) ? . . C(20) C(27) 3.42(2) ? . . C(21) Cl(4) 3.27(1) ? . 64501 C(21) C(26) 2.61(2) ? . . C(21) C(27) 2.54(2) ? . . C(23) C(24) 2.53(2) ? . . C(26) C(27) 2.56(2) ? . . C(28) Ag(2) 3.241(8) ? . 66502 C(28) C(55) 3.49(2) ? . . C(29) C(30) 2.44(1) ? . . C(29) C(31) 2.46(1) ? . . C(29) C(32) 3.23(1) ? . . C(29) C(36) 3.33(1) ? . . C(29) C(37) 3.36(1) ? . . C(30) Ag(2) 3.054(9) ? . 66502 C(30) C(43) 2.30(1) ? . . C(30) C(44) 3.07(1) ? . . C(30) C(48) 3.25(1) ? . . C(30) C(49) 3.23(1) ? . . C(30) C(52) 3.59(1) ? . . C(30) C(53) 3.54(1) ? . . C(31) Cl(3) 3.31(1) ? . 66502 C(31) C(33) 2.31(1) ? . . C(31) C(34) 2.82(1) ? . . C(31) C(35) 2.37(1) ? . . C(31) C(37) 2.50(1) ? . . C(31) C(38) 3.38(1) ? . . C(31) C(40) 2.57(1) ? . . C(31) C(41) 3.47(2) ? . . C(32) Cl(3) 3.34(1) ? . 66502 C(32) C(34) 2.49(1) ? . . C(32) C(35) 2.83(1) ? . . C(32) C(36) 2.44(1) ? . . C(32) C(38) 2.49(2) ? . . C(32) C(39) 2.51(1) ? . . C(33) C(35) 2.45(1) ? . . C(33) C(36) 2.77(1) ? . . C(33) C(37) 2.50(1) ? . . C(33) C(38) 3.19(2) ? . . C(33) C(39) 2.96(1) ? . . C(34) C(36) 2.52(1) ? . . C(34) C(43) 3.51(1) ? . 76502 C(35) C(40) 2.44(1) ? . . C(35) C(41) 3.01(2) ? . . C(35) C(42) 3.00(1) ? . . C(36) Cl(3) 3.57(1) ? . 66502 C(36) C(41) 2.43(2) ? . . C(36) C(42) 2.51(1) ? . . C(38) C(39) 2.50(2) ? . . C(41) C(42) 2.48(2) ? . . C(43) Ag(2) 3.155(8) ? . 66502 C(43) C(34) 3.51(1) ? . 76502 C(43) C(45) 2.37(1) ? . . C(43) C(46) 2.74(1) ? . . C(43) C(47) 2.35(1) ? . . C(43) C(49) 2.51(1) ? . . C(43) C(51) 3.28(1) ? . . C(43) C(52) 2.53(1) ? . . C(43) C(53) 3.23(1) ? . . C(44) C(46) 2.42(1) ? . . C(44) C(47) 2.77(1) ? . . C(44) C(48) 2.45(1) ? . . C(44) C(50) 2.58(1) ? . . C(44) C(51) 2.51(1) ? . . C(45) C(47) 2.35(1) ? . . C(45) C(48) 2.76(1) ? . . C(45) C(49) 2.52(2) ? . . C(45) C(50) 2.94(2) ? . . C(45) C(51) 3.42(2) ? . . C(46) C(48) 2.40(1) ? . . C(47) C(52) 2.49(1) ? . . C(47) C(53) 3.31(1) ? . . C(47) C(54) 2.90(1) ? . . C(48) C(53) 2.45(1) ? . . C(48) C(54) 2.51(1) ? . . C(50) C(51) 2.58(2) ? . . C(51) C(55) 3.49(2) ? . . C(53) Cl(2) 3.57(1) ? . 66502 C(53) C(54) 2.49(2) ? . . Ag(1) H(1) 2.7402 ? . . Ag(1) H(1) 2.8178 ? . 75602 Ag(1) H(7) 3.5532 ? . . Ag(1) H(10) 3.2676 ? . . Ag(1) H(14) 3.1793 ? . . Ag(1) H(24) 3.1203 ? . 75602 Ag(1) H(31) 3.0839 ? . 75602 Ag(2) H(38) 2.7762 ? . . Ag(2) H(38) 2.7188 ? . 66502 Ag(2) H(44) 3.3905 ? . . Ag(2) H(51) 3.2021 ? . . Ag(2) H(52) 3.2537 ? . . Ag(2) H(67) 3.0817 ? . 66502 Ag(2) H(68) 2.9167 ? . 66502 Ag(2) H(76) 3.1403 ? . 66502 Cl(1) H(23) 3.0689 ? . 45501 Cl(1) H(26) 2.8691 ? . . Cl(1) H(27) 3.4522 ? . . Cl(1) H(34) 3.2387 ? . 45501 Cl(1) H(51) 3.5353 ? . . Cl(1) H(56) 3.2066 ? . . Cl(1) H(61) 3.2496 ? . . Cl(1) H(66) 3.0283 ? . . Cl(1) H(75) 2.2094 ? . . Cl(1) H(76) 2.3226 ? . . Cl(2) H(22) 3.1509 ? . 45501 Cl(2) H(23) 3.5500 ? . 45501 Cl(2) H(38) 3.4954 ? . . Cl(2) H(38) 3.4124 ? . 66502 Cl(2) H(51) 3.2410 ? . . Cl(2) H(52) 3.4266 ? . . Cl(2) H(68) 2.9110 ? . 66502 Cl(2) H(70) 2.8648 ? . 66502 Cl(2) H(73) 3.2502 ? . 54501 Cl(2) H(75) 2.1835 ? . . Cl(2) H(76) 2.2801 ? . . Cl(3) H(10) 3.3525 ? . 66602 Cl(3) H(50) 3.2210 ? . 66502 Cl(3) H(52) 3.5868 ? . 66502 Cl(3) H(54) 3.5589 ? . 66502 Cl(3) H(67) 3.0578 ? . . Cl(3) H(77) 2.3002 ? . . Cl(3) H(78) 2.3508 ? . . Cl(4) H(10) 3.3100 ? . 66602 Cl(4) H(31) 3.4690 ? . 46501 Cl(4) H(32) 3.2824 ? . 46501 Cl(4) H(77) 2.2695 ? . . Cl(4) H(78) 2.3187 ? . . N(1) H(1) 2.6360 ? . . N(1) H(2) 1.9769 ? . . N(1) H(7) 2.4434 ? . . N(1) H(10) 3.2640 ? . . N(1) H(14) 2.4764 ? . . N(1) H(20) 3.2571 ? . . N(2) H(1) 2.5856 ? . . N(2) H(3) 1.9455 ? . . N(2) H(24) 2.4494 ? . . N(2) H(25) 3.2536 ? . . N(2) H(31) 2.4639 ? . . N(2) H(37) 3.0843 ? . . N(3) H(38) 2.6107 ? . . N(3) H(39) 2.0859 ? . . N(3) H(44) 2.4053 ? . . N(3) H(45) 3.5090 ? . . N(3) H(51) 2.3742 ? . . N(3) H(52) 3.5401 ? . . N(4) H(38) 2.5815 ? . . N(4) H(40) 1.9783 ? . . N(4) H(61) 2.5312 ? . . N(4) H(67) 2.9836 ? . . N(4) H(68) 2.5056 ? . . N(4) H(71) 3.0590 ? . . N(4) H(76) 3.1134 ? . . C(1) H(1) 3.1785 ? . 75602 C(1) H(2) 2.0243 ? . . C(1) H(3) 1.9619 ? . . C(2) H(1) 2.0331 ? . . C(2) H(3) 2.5992 ? . . C(2) H(7) 2.8134 ? . . C(2) H(13) 3.5583 ? . 76602 C(2) H(14) 3.0181 ? . . C(2) H(20) 2.9823 ? . . C(3) H(1) 1.9705 ? . . C(3) H(2) 2.6154 ? . . C(3) H(24) 3.0838 ? . . C(3) H(25) 2.9868 ? . . C(3) H(31) 3.1247 ? . . C(3) H(36) 3.5135 ? . . C(3) H(37) 2.8595 ? . . C(4) H(2) 2.4637 ? . . C(4) H(4) 3.2998 ? . . C(4) H(6) 3.3010 ? . . C(4) H(7) 2.5456 ? . . C(4) H(10) 3.0477 ? . . C(4) H(11) 3.4221 ? . 76602 C(4) H(14) 2.6435 ? . . C(4) H(20) 3.0965 ? . . C(4) H(77) 2.9670 ? . 66602 C(5) H(2) 3.1797 ? . . C(5) H(4) 2.1126 ? . . C(5) H(5) 3.3120 ? . . C(5) H(7) 2.0254 ? . . C(5) H(8) 2.9526 ? . . C(5) H(9) 3.3660 ? . . C(5) H(10) 2.5032 ? . . C(5) H(11) 2.9188 ? . . C(5) H(11) 3.3931 ? . 76602 C(5) H(12) 3.2665 ? . . C(5) H(13) 2.5740 ? . . C(5) H(77) 2.9735 ? . 66602 C(6) H(5) 2.0365 ? . . C(6) H(6) 3.2657 ? . . C(6) H(7) 3.3052 ? . . C(6) H(8) 3.3145 ? . . C(6) H(10) 3.3179 ? . . C(6) H(11) 3.4778 ? . . C(6) H(11) 3.2699 ? . 76602 C(6) H(13) 2.5258 ? . . C(6) H(50) 3.4224 ? . 55601 C(6) H(77) 2.9087 ? . 66602 C(7) H(4) 2.0175 ? . . C(7) H(6) 2.0529 ? . . C(7) H(11) 3.0875 ? . 76602 C(7) H(36) 3.5942 ? . 76602 C(7) H(37) 3.3892 ? . 76602 C(7) H(65) 3.2574 ? . 66602 C(7) H(77) 2.9117 ? . 66602 C(8) H(4) 3.2606 ? . . C(8) H(5) 2.0437 ? . . C(8) H(11) 3.1643 ? . 76602 C(8) H(14) 3.2978 ? . . C(8) H(15) 3.4662 ? . . C(8) H(17) 2.5127 ? . . C(8) H(18) 3.2681 ? . . C(8) H(18) 3.4967 ? . 66602 C(8) H(20) 3.2935 ? . . C(8) H(77) 2.8383 ? . 66602 C(9) H(2) 3.1908 ? . . C(9) H(5) 3.2592 ? . . C(9) H(6) 2.0299 ? . . C(9) H(11) 3.3149 ? . 76602 C(9) H(14) 2.0958 ? . . C(9) H(15) 2.9986 ? . . C(9) H(16) 3.3500 ? . . C(9) H(17) 2.6225 ? . . C(9) H(18) 2.9007 ? . . C(9) H(19) 3.3190 ? . . C(9) H(20) 2.5167 ? . . C(9) H(77) 2.8587 ? . 66602 C(10) H(2) 3.5612 ? . . C(10) H(4) 2.7311 ? . . C(10) H(8) 2.1360 ? . . C(10) H(9) 2.1750 ? . . C(10) H(10) 2.0465 ? . . C(10) H(11) 1.9705 ? . . C(10) H(12) 1.9815 ? . . C(10) H(13) 2.0096 ? . . C(11) H(4) 3.3575 ? . . C(11) H(7) 2.0787 ? . . C(11) H(11) 3.2038 ? . . C(11) H(12) 2.3503 ? . . C(11) H(13) 2.8870 ? . . C(11) H(29) 3.4744 ? . 75602 C(11) H(59) 3.5905 ? . 76602 C(12) H(2) 3.4000 ? . 76602 C(12) H(4) 2.7314 ? . . C(12) H(7) 1.9843 ? . . C(12) H(8) 2.5150 ? . . C(12) H(9) 2.8379 ? . . C(12) H(10) 3.1853 ? . . C(12) H(20) 3.3049 ? . 76602 C(12) H(58) 3.4133 ? . 76602 C(12) H(64) 3.4098 ? . 76602 C(13) H(2) 3.5226 ? . . C(13) H(6) 2.6883 ? . . C(13) H(15) 2.0912 ? . . C(13) H(16) 2.0734 ? . . C(13) H(17) 2.1215 ? . . C(13) H(18) 2.0063 ? . . C(13) H(19) 2.0474 ? . . C(13) H(20) 2.0393 ? . . C(14) H(6) 2.6584 ? . . C(14) H(14) 2.0972 ? . . C(14) H(18) 2.5443 ? . . C(14) H(19) 2.9495 ? . . C(14) H(20) 3.3429 ? . . C(14) H(58) 3.5359 ? . 66602 C(14) H(59) 3.3952 ? . 66602 C(15) H(2) 3.3288 ? . . C(15) H(6) 3.2746 ? . . C(15) H(14) 1.9904 ? . . C(15) H(15) 3.3020 ? . . C(15) H(16) 2.5466 ? . . C(15) H(17) 3.0123 ? . . C(15) H(63) 3.1452 ? . . C(15) H(64) 3.2760 ? . . C(16) H(3) 2.4750 ? . . C(16) H(21) 3.2926 ? . . C(16) H(23) 3.2554 ? . . C(16) H(24) 2.6009 ? . . C(16) H(25) 3.4477 ? . . C(16) H(27) 3.4449 ? . . C(16) H(31) 2.5386 ? . . C(16) H(37) 2.9468 ? . . C(16) H(49) 3.5847 ? . 76502 C(17) H(3) 3.2523 ? . . C(17) H(21) 2.0592 ? . . C(17) H(22) 3.2845 ? . . C(17) H(24) 1.9997 ? . . C(17) H(25) 2.9250 ? . . C(17) H(26) 3.3422 ? . . C(17) H(27) 2.4958 ? . . C(17) H(28) 2.8716 ? . . C(17) H(29) 3.2380 ? . . C(17) H(30) 2.4531 ? . . C(17) H(46) 3.4635 ? . 76502 C(18) H(22) 1.9931 ? . . C(18) H(23) 3.1955 ? . . C(18) H(24) 3.2849 ? . . C(18) H(27) 3.0265 ? . . C(18) H(28) 3.0242 ? . . C(18) H(30) 2.6690 ? . . C(18) H(46) 2.8832 ? . 76502 C(18) H(54) 3.5814 ? . 75502 C(19) H(21) 2.0008 ? . . C(19) H(23) 1.9890 ? . . C(19) H(46) 3.3373 ? . 76502 C(19) H(49) 3.4966 ? . 76502 C(19) H(72) 3.1322 ? . 64501 C(19) H(74) 3.4522 ? . 64501 C(19) H(75) 3.3106 ? . 65501 C(20) H(21) 3.1901 ? . . C(20) H(22) 1.9828 ? . . C(20) H(31) 3.2760 ? . . C(20) H(32) 3.3384 ? . . C(20) H(34) 2.4936 ? . . C(20) H(35) 3.4551 ? . . C(20) H(37) 3.3921 ? . . C(20) H(49) 3.3675 ? . 76502 C(20) H(72) 3.5000 ? . 64501 C(20) H(74) 3.2386 ? . 64501 C(20) H(75) 2.9410 ? . 65501 C(21) H(3) 3.1815 ? . . C(21) H(22) 3.2198 ? . . C(21) H(23) 2.0631 ? . . C(21) H(31) 2.0739 ? . . C(21) H(32) 2.9666 ? . . C(21) H(33) 3.3860 ? . . C(21) H(34) 2.6510 ? . . C(21) H(35) 2.9371 ? . . C(21) H(36) 3.3281 ? . . C(21) H(37) 2.4916 ? . . C(21) H(49) 3.4022 ? . 76502 C(22) H(21) 2.7216 ? . . C(22) H(25) 2.0686 ? . . C(22) H(26) 2.1309 ? . . C(22) H(27) 2.0123 ? . . C(22) H(28) 2.0002 ? . . C(22) H(29) 2.0451 ? . . C(22) H(30) 2.0252 ? . . C(23) H(3) 3.4819 ? . . C(23) H(21) 3.4197 ? . . C(23) H(24) 2.0388 ? . . C(23) H(28) 2.5190 ? . . C(23) H(29) 2.9209 ? . . C(23) H(30) 3.3068 ? . . C(23) H(46) 3.5080 ? . 76502 C(23) H(48) 3.5879 ? . 76502 C(23) H(62) 3.5048 ? . . C(23) H(63) 3.5085 ? . . C(24) H(9) 3.5205 ? . 75602 C(24) H(21) 2.6740 ? . . C(24) H(24) 1.9948 ? . . C(24) H(25) 3.2771 ? . . C(24) H(26) 2.6089 ? . . C(24) H(27) 2.9193 ? . . C(24) H(43) 3.2845 ? . 75502 C(25) H(3) 3.5719 ? . . C(25) H(23) 2.7322 ? . . C(25) H(32) 2.0244 ? . . C(25) H(33) 2.0385 ? . . C(25) H(34) 2.0736 ? . . C(25) H(35) 1.9703 ? . . C(25) H(36) 2.0923 ? . . C(25) H(37) 2.0683 ? . . C(26) H(23) 2.6339 ? . . C(26) H(26) 3.5464 ? . 65501 C(26) H(31) 2.0833 ? . . C(26) H(35) 2.4724 ? . . C(26) H(36) 3.0153 ? . . C(26) H(37) 3.3105 ? . . C(26) H(60) 3.3675 ? . 64501 C(27) H(3) 3.2011 ? . . C(27) H(5) 2.8530 ? . 76602 C(27) H(23) 3.4657 ? . . C(27) H(31) 1.9829 ? . . C(27) H(32) 3.2944 ? . . C(27) H(33) 2.5744 ? . . C(27) H(34) 2.9942 ? . . C(27) H(65) 3.4465 ? . 65501 C(28) H(38) 3.1494 ? . 66502 C(28) H(39) 2.0303 ? . . C(28) H(40) 2.1180 ? . . C(28) H(61) 3.4638 ? . . C(28) H(76) 2.6905 ? . . C(29) H(38) 2.0718 ? . . C(29) H(40) 2.6060 ? . . C(29) H(44) 2.8087 ? . . C(29) H(45) 3.0792 ? . . C(29) H(47) 3.5677 ? . 76502 C(29) H(51) 3.0028 ? . . C(29) H(76) 3.5612 ? . . C(30) H(38) 2.1078 ? . . C(30) H(39) 2.5745 ? . . C(30) H(61) 2.5671 ? . . C(30) H(68) 3.2839 ? . . C(30) H(71) 2.9476 ? . . C(30) H(76) 3.0530 ? . . C(31) H(39) 2.6313 ? . . C(31) H(41) 3.1643 ? . . C(31) H(43) 3.2505 ? . . C(31) H(44) 2.5212 ? . . C(31) H(45) 3.4172 ? . . C(31) H(47) 3.4134 ? . . C(31) H(51) 2.5939 ? . . C(31) H(52) 3.5883 ? . . C(31) H(54) 3.4815 ? . . C(31) H(57) 3.5466 ? . . C(32) H(39) 3.2467 ? . . C(32) H(41) 2.0043 ? . . C(32) H(42) 3.3512 ? . . C(32) H(44) 1.9857 ? . . C(32) H(45) 2.8639 ? . . C(32) H(46) 3.2854 ? . . C(32) H(47) 2.4314 ? . . C(32) H(48) 2.9448 ? . . C(32) H(49) 3.2511 ? . . C(32) H(50) 2.5385 ? . . C(33) H(8) 3.1443 ? . 55401 C(33) H(40) 2.9518 ? . 76502 C(33) H(42) 2.0978 ? . . C(33) H(43) 3.2971 ? . . C(33) H(44) 3.2294 ? . . C(33) H(47) 2.7435 ? . . C(33) H(48) 3.0668 ? . . C(33) H(50) 2.7706 ? . . C(33) H(62) 3.5692 ? . 76502 C(34) H(8) 3.2196 ? . 55401 C(34) H(29) 3.5856 ? . 75502 C(34) H(30) 3.5041 ? . 75502 C(34) H(40) 2.9462 ? . 76502 C(34) H(41) 2.0140 ? . . C(34) H(43) 2.1386 ? . . C(34) H(71) 2.9799 ? . 76502 C(35) H(30) 3.2125 ? . 75502 C(35) H(41) 3.3087 ? . . C(35) H(42) 2.2053 ? . . C(35) H(51) 3.2032 ? . . C(35) H(54) 2.5217 ? . . C(35) H(55) 3.0558 ? . . C(35) H(57) 2.9358 ? . . C(35) H(71) 2.9775 ? . 76502 C(36) H(39) 3.4271 ? . . C(36) H(42) 3.3839 ? . . C(36) H(43) 2.0359 ? . . C(36) H(51) 2.0015 ? . . C(36) H(52) 2.8751 ? . . C(36) H(53) 3.2006 ? . . C(36) H(54) 2.3632 ? . . C(36) H(55) 2.9456 ? . . C(36) H(56) 3.2504 ? . . C(36) H(57) 2.5362 ? . . C(37) H(39) 3.3977 ? . . C(37) H(41) 2.6202 ? . . C(37) H(45) 2.0412 ? . . C(37) H(46) 2.0530 ? . . C(37) H(47) 1.9409 ? . . C(37) H(48) 2.0510 ? . . C(37) H(49) 2.0675 ? . . C(37) H(50) 2.1063 ? . . C(38) H(21) 3.5892 ? . 76502 C(38) H(27) 3.3507 ? . 76502 C(38) H(39) 3.3446 ? . . C(38) H(39) 3.4670 ? . 76502 C(38) H(41) 3.1673 ? . . C(38) H(44) 1.9762 ? . . C(38) H(48) 2.4801 ? . . C(38) H(49) 2.8998 ? . . C(38) H(50) 3.2816 ? . . C(38) H(57) 3.1721 ? . 76502 C(39) H(4) 3.4460 ? . 55401 C(39) H(41) 2.6460 ? . . C(39) H(44) 2.0892 ? . . C(39) H(45) 3.3037 ? . . C(39) H(46) 2.5434 ? . . C(39) H(47) 2.8269 ? . . C(40) H(43) 2.6049 ? . . C(40) H(52) 1.9756 ? . . C(40) H(53) 1.9322 ? . . C(40) H(54) 1.8543 ? . . C(40) H(55) 2.0881 ? . . C(40) H(56) 2.0683 ? . . C(40) H(57) 2.1155 ? . . C(41) H(43) 2.9445 ? . . C(41) H(51) 1.8370 ? . . C(41) H(55) 2.5550 ? . . C(41) H(56) 2.8250 ? . . C(41) H(57) 3.2545 ? . . C(41) H(68) 3.4974 ? . 66502 C(41) H(69) 3.5854 ? . 54501 C(41) H(72) 2.8906 ? . 66502 C(42) H(21) 3.3205 ? . . C(42) H(28) 3.5827 ? . . C(42) H(43) 2.8365 ? . . C(42) H(45) 3.5135 ? . 76502 C(42) H(51) 2.0887 ? . . C(42) H(52) 3.2698 ? . . C(42) H(53) 2.4491 ? . . C(42) H(54) 2.8567 ? . . C(42) H(55) 3.4503 ? . 75502 C(43) H(40) 2.4299 ? . . C(43) H(42) 2.8888 ? . 76502 C(43) H(58) 3.2362 ? . . C(43) H(60) 3.2168 ? . . C(43) H(61) 2.6018 ? . . C(43) H(67) 2.9882 ? . . C(43) H(68) 2.5940 ? . . C(43) H(71) 2.8753 ? . . C(43) H(78) 3.0079 ? . . C(44) H(40) 3.0028 ? . . C(44) H(41) 3.3709 ? . 76502 C(44) H(42) 3.0066 ? . 76502 C(44) H(58) 2.0333 ? . . C(44) H(59) 3.2633 ? . . C(44) H(61) 1.9716 ? . . C(44) H(62) 2.9889 ? . . C(44) H(63) 3.3373 ? . . C(44) H(64) 2.5957 ? . . C(44) H(65) 2.9283 ? . . C(44) H(66) 3.2441 ? . . C(44) H(67) 2.5616 ? . . C(44) H(78) 2.7870 ? . . C(45) H(8) 3.5806 ? . 76602 C(45) H(9) 3.4815 ? . 76602 C(45) H(12) 3.2812 ? . 76602 C(45) H(17) 3.4417 ? . 66602 C(45) H(41) 3.5967 ? . 76502 C(45) H(42) 2.9374 ? . 76502 C(45) H(59) 1.9982 ? . . C(45) H(60) 3.1927 ? . . C(45) H(61) 3.1948 ? . . C(45) H(62) 3.3640 ? . . C(45) H(64) 2.4798 ? . . C(45) H(65) 3.4901 ? . . C(45) H(67) 3.5082 ? . . C(45) H(78) 2.6763 ? . . C(46) H(9) 3.1978 ? . 76602 C(46) H(15) 3.2968 ? . 66602 C(46) H(29) 3.3696 ? . 56501 C(46) H(32) 3.4541 ? . 46501 C(46) H(42) 2.8468 ? . 76502 C(46) H(58) 1.9971 ? . . C(46) H(60) 1.9940 ? . . C(46) H(78) 2.8125 ? . . C(47) H(29) 3.3808 ? . 56501 C(47) H(32) 3.4590 ? . 46501 C(47) H(42) 2.8270 ? . 76502 C(47) H(58) 3.2032 ? . . C(47) H(59) 2.0366 ? . . C(47) H(68) 3.1915 ? . . C(47) H(69) 3.3489 ? . . C(47) H(71) 3.2915 ? . . C(47) H(72) 3.3415 ? . . C(47) H(74) 2.3775 ? . . C(47) H(78) 2.9662 ? . . C(48) H(40) 3.3058 ? . . C(48) H(42) 2.8687 ? . 76502 C(48) H(59) 3.2650 ? . . C(48) H(60) 2.0247 ? . . C(48) H(68) 1.9952 ? . . C(48) H(69) 2.8481 ? . . C(48) H(70) 3.2286 ? . . C(48) H(71) 2.4119 ? . . C(48) H(72) 2.9051 ? . . C(48) H(73) 3.2953 ? . . C(48) H(74) 2.4744 ? . . C(48) H(78) 3.0892 ? . . C(49) H(40) 3.2489 ? . . C(49) H(41) 3.5331 ? . 76502 C(49) H(58) 2.6782 ? . . C(49) H(62) 2.1511 ? . . C(49) H(63) 2.1436 ? . . C(49) H(64) 2.1063 ? . . C(49) H(65) 2.0738 ? . . C(49) H(66) 2.0499 ? . . C(49) H(67) 2.0969 ? . . C(49) H(76) 3.4007 ? . . C(49) H(78) 3.5904 ? . . C(50) H(12) 3.5090 ? . 76602 C(50) H(18) 3.5345 ? . . C(50) H(19) 3.5301 ? . . C(50) H(20) 3.2731 ? . . C(50) H(41) 3.3219 ? . 76502 C(50) H(58) 2.5695 ? . . C(50) H(61) 2.0945 ? . . C(50) H(65) 2.5651 ? . . C(50) H(66) 2.9059 ? . . C(50) H(67) 3.3844 ? . . C(51) H(35) 3.2197 ? . 45501 C(51) H(58) 3.5401 ? . . C(51) H(61) 2.0746 ? . . C(51) H(62) 3.3458 ? . . C(51) H(63) 2.5661 ? . . C(51) H(64) 2.9731 ? . . C(51) H(75) 3.1733 ? . . C(51) H(76) 3.1565 ? . . C(51) H(78) 3.3157 ? . . C(52) H(52) 3.2007 ? . 66502 C(52) H(60) 2.6398 ? . . C(52) H(69) 1.9734 ? . . C(52) H(70) 2.0743 ? . . C(52) H(71) 2.0331 ? . . C(52) H(72) 2.0025 ? . . C(52) H(73) 2.0450 ? . . C(52) H(74) 1.9527 ? . . C(53) H(40) 3.5140 ? . . C(53) H(42) 3.5036 ? . 76502 C(53) H(43) 3.3422 ? . 76502 C(53) H(53) 3.3097 ? . 56501 C(53) H(60) 3.4032 ? . . C(53) H(68) 1.9716 ? . . C(53) H(72) 3.2342 ? . . C(53) H(73) 2.5379 ? . . C(53) H(74) 2.8961 ? . . C(54) H(22) 3.2102 ? . 46501 C(54) H(23) 3.5052 ? . 46501 C(54) H(52) 2.9665 ? . 66502 C(54) H(60) 2.5879 ? . . C(54) H(68) 1.9762 ? . . C(54) H(69) 2.4580 ? . . C(54) H(70) 2.9129 ? . . C(54) H(71) 3.2493 ? . . C(55) H(23) 2.9926 ? . 45501 C(55) H(38) 3.1869 ? . . C(55) H(61) 3.3155 ? . . C(55) H(66) 2.6856 ? . . C(56) H(10) 3.3427 ? . 66602 C(56) H(67) 3.1765 ? . . H(1) Ag(1) 2.8178 ? . 75602 H(1) C(1) 3.1785 ? . 75602 H(2) C(12) 3.4000 ? . 76602 H(4) C(39) 3.4460 ? . 55601 H(5) C(27) 2.8530 ? . 76602 H(8) C(33) 3.1443 ? . 55601 H(8) C(34) 3.2196 ? . 55601 H(8) C(45) 3.5806 ? . 76602 H(9) C(24) 3.5205 ? . 75602 H(9) C(45) 3.4815 ? . 76602 H(9) C(46) 3.1978 ? . 76602 H(10) Cl(3) 3.3525 ? . 66602 H(10) Cl(4) 3.3100 ? . 66602 H(10) C(56) 3.3427 ? . 66602 H(11) C(4) 3.4221 ? . 76602 H(11) C(5) 3.3931 ? . 76602 H(11) C(6) 3.2699 ? . 76602 H(11) C(7) 3.0875 ? . 76602 H(11) C(8) 3.1643 ? . 76602 H(11) C(9) 3.3149 ? . 76602 H(12) C(45) 3.2812 ? . 76602 H(12) C(50) 3.5090 ? . 76602 H(13) C(2) 3.5583 ? . 76602 H(15) C(46) 3.2968 ? . 66602 H(17) C(45) 3.4417 ? . 66602 H(18) C(8) 3.4967 ? . 66602 H(20) C(12) 3.3049 ? . 76602 H(21) C(38) 3.5892 ? . 76502 H(22) Cl(2) 3.1509 ? . 65501 H(22) C(54) 3.2102 ? . 64501 H(23) Cl(1) 3.0689 ? . 65501 H(23) Cl(2) 3.5500 ? . 65501 H(23) C(54) 3.5052 ? . 64501 H(23) C(55) 2.9926 ? . 65501 H(24) Ag(1) 3.1203 ? . 75602 H(26) C(26) 3.5464 ? . 45501 H(27) C(38) 3.3507 ? . 76502 H(29) C(11) 3.4744 ? . 75602 H(29) C(34) 3.5856 ? . 75502 H(29) C(46) 3.3696 ? . 54501 H(29) C(47) 3.3808 ? . 54501 H(30) C(34) 3.5041 ? . 75502 H(30) C(35) 3.2125 ? . 75502 H(31) Ag(1) 3.0839 ? . 75602 H(31) Cl(4) 3.4690 ? . 64501 H(32) Cl(4) 3.2824 ? . 64501 H(32) C(46) 3.4541 ? . 64501 H(32) C(47) 3.4590 ? . 64501 H(34) Cl(1) 3.2387 ? . 65501 H(35) C(51) 3.2197 ? . 65501 H(36) C(7) 3.5942 ? . 76602 H(37) C(7) 3.3892 ? . 76602 H(38) Ag(2) 2.7188 ? . 66502 H(38) Cl(2) 3.4124 ? . 66502 H(38) C(28) 3.1494 ? . 66502 H(39) C(38) 3.4670 ? . 76502 H(40) C(33) 2.9518 ? . 76502 H(40) C(34) 2.9462 ? . 76502 H(41) C(44) 3.3709 ? . 76502 H(41) C(45) 3.5967 ? . 76502 H(41) C(49) 3.5331 ? . 76502 H(41) C(50) 3.3219 ? . 76502 H(42) C(43) 2.8888 ? . 76502 H(42) C(44) 3.0066 ? . 76502 H(42) C(45) 2.9374 ? . 76502 H(42) C(46) 2.8468 ? . 76502 H(42) C(47) 2.8270 ? . 76502 H(42) C(48) 2.8687 ? . 76502 H(42) C(53) 3.5036 ? . 76502 H(43) C(24) 3.2845 ? . 75502 H(43) C(53) 3.3422 ? . 76502 H(45) C(42) 3.5135 ? . 76502 H(46) C(17) 3.4635 ? . 76502 H(46) C(18) 2.8832 ? . 76502 H(46) C(19) 3.3373 ? . 76502 H(46) C(23) 3.5080 ? . 76502 H(47) C(29) 3.5677 ? . 76502 H(48) C(23) 3.5879 ? . 76502 H(49) C(16) 3.5847 ? . 76502 H(49) C(19) 3.4966 ? . 76502 H(49) C(20) 3.3675 ? . 76502 H(49) C(21) 3.4022 ? . 76502 H(50) Cl(3) 3.2210 ? . 66502 H(50) C(6) 3.4224 ? . 55401 H(52) Cl(3) 3.5868 ? . 66502 H(52) C(52) 3.2007 ? . 66502 H(52) C(54) 2.9665 ? . 66502 H(53) C(53) 3.3097 ? . 54501 H(54) Cl(3) 3.5589 ? . 66502 H(54) C(18) 3.5814 ? . 75502 H(55) C(42) 3.4503 ? . 75502 H(57) C(38) 3.1721 ? . 76502 H(58) C(12) 3.4133 ? . 76602 H(58) C(14) 3.5359 ? . 66602 H(59) C(11) 3.5905 ? . 76602 H(59) C(14) 3.3952 ? . 66602 H(60) C(26) 3.3675 ? . 46501 H(62) C(33) 3.5692 ? . 76502 H(64) C(12) 3.4098 ? . 76602 H(65) C(7) 3.2574 ? . 66602 H(65) C(27) 3.4465 ? . 45501 H(67) Ag(2) 3.0817 ? . 66502 H(68) Ag(2) 2.9167 ? . 66502 H(68) Cl(2) 2.9110 ? . 66502 H(68) C(41) 3.4974 ? . 66502 H(69) C(41) 3.5854 ? . 56501 H(70) Cl(2) 2.8648 ? . 66502 H(71) C(34) 2.9799 ? . 76502 H(71) C(35) 2.9775 ? . 76502 H(72) C(19) 3.1322 ? . 46501 H(72) C(20) 3.5000 ? . 46501 H(72) C(41) 2.8906 ? . 66502 H(73) Cl(2) 3.2502 ? . 56501 H(74) C(19) 3.4522 ? . 46501 H(74) C(20) 3.2386 ? . 46501 H(75) C(19) 3.3106 ? . 45501 H(75) C(20) 2.9410 ? . 45501 H(76) Ag(2) 3.1403 ? . 66502 H(77) C(4) 2.9670 ? . 66602 H(77) C(5) 2.9735 ? . 66602 H(77) C(6) 2.9087 ? . 66602 H(77) C(7) 2.9117 ? . 66602 H(77) C(8) 2.8383 ? . 66602 H(77) C(9) 2.8587 ? . 66602 loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 Ag(1) N(1) C(2) C(1) -2(1) ? . . . . C(4) N(1) C(2) C(1) 179.1(9) ? . . . . Ag(1) N(1) C(4) C(5) 90.7(9) ? . . . . Ag(1) N(1) C(4) C(9) -88.0(9) ? . . . . C(2) N(1) C(4) C(5) -91(1) ? . . . . C(2) N(1) C(4) C(9) 89(1) ? . . . . C(16) N(2) C(3) C(1) -178.2(9) ? . . . . C(3) N(2) C(16) C(17) -93(1) ? . . . . C(3) N(2) C(16) C(21) 89(1) ? . . . . Ag(2) N(3) C(29) C(28) 4.3(9) ? . . . . C(31) N(3) C(29) C(28) 179.4(6) ? . . . . Ag(2) N(3) C(31) C(32) 89(1) ? . . . . Ag(2) N(3) C(31) C(36) -83.8(9) ? . . . . C(29) N(3) C(31) C(32) -86(1) ? . . . . C(29) N(3) C(31) C(36) 100.9(9) ? . . . . C(43) N(4) C(30) C(28) 178.6(6) ? . . . . C(30) N(4) C(43) C(44) -82.0(8) ? . . . . C(30) N(4) C(43) C(48) 104.8(8) ? . . . . C(3) C(1) C(2) N(1) -179.0(9) ? . . . . C(2) C(1) C(3) N(2) -178.1(9) ? . . . . N(1) C(4) C(5) C(6) -179.1(8) ? . . . . N(1) C(4) C(5) C(10) -2(1) ? . . . . C(9) C(4) C(5) C(6) 0(1) ? . . . . C(9) C(4) C(5) C(10) 176.6(7) ? . . . . N(1) C(4) C(9) C(8) -178.9(8) ? . . . . N(1) C(4) C(9) C(13) -1(1) ? . . . . C(5) C(4) C(9) C(8) 2(1) ? . . . . C(5) C(4) C(9) C(13) -179.8(6) ? . . . . C(4) C(5) C(6) C(7) -4(1) ? . . . . C(10) C(5) C(6) C(7) 178.6(9) ? . . . . C(4) C(5) C(10) C(11) -94(1) ? . . . . C(4) C(5) C(10) C(12) 145(1) ? . . . . C(6) C(5) C(10) C(11) 82(1) ? . . . . C(6) C(5) C(10) C(12) -37(1) ? . . . . C(5) C(6) C(7) C(8) 7(1) ? . . . . C(6) C(7) C(8) C(9) -5(1) ? . . . . C(7) C(8) C(9) C(4) 0(1) ? . . . . C(7) C(8) C(9) C(13) -177.4(8) ? . . . . C(4) C(9) C(13) C(14) 142.5(9) ? . . . . C(4) C(9) C(13) C(15) -93(1) ? . . . . C(8) C(9) C(13) C(14) -39(1) ? . . . . C(8) C(9) C(13) C(15) 84(1) ? . . . . N(2) C(16) C(17) C(18) 179.8(6) ? . . . . N(2) C(16) C(17) C(22) 0(1) ? . . . . C(21) C(16) C(17) C(18) -3(1) ? . . . . C(21) C(16) C(17) C(22) 177.3(9) ? . . . . N(2) C(16) C(21) C(20) 179.3(9) ? . . . . N(2) C(16) C(21) C(25) 3(1) ? . . . . C(17) C(16) C(21) C(20) 2(1) ? . . . . C(17) C(16) C(21) C(25) -172.8(8) ? . . . . C(16) C(17) C(18) C(19) 2(1) ? . . . . C(22) C(17) C(18) C(19) -178.8(9) ? . . . . C(16) C(17) C(22) C(23) 91(1) ? . . . . C(16) C(17) C(22) C(24) -141(1) ? . . . . C(18) C(17) C(22) C(23) -86(1) ? . . . . C(18) C(17) C(22) C(24) 39(1) ? . . . . C(17) C(18) C(19) C(20) 0(1) ? . . . . C(18) C(19) C(20) C(21) -1(1) ? . . . . C(19) C(20) C(21) C(16) 0(1) ? . . . . C(19) C(20) C(21) C(25) 175.3(9) ? . . . . C(16) C(21) C(25) C(26) 147(1) ? . . . . C(16) C(21) C(25) C(27) -85(1) ? . . . . C(20) C(21) C(25) C(26) -28(1) ? . . . . C(20) C(21) C(25) C(27) 98(1) ? . . . . C(30) C(28) C(29) N(3) 179.2(6) ? . . . . C(29) C(28) C(30) N(4) 178.8(7) ? . . . . N(3) C(31) C(32) C(33) -175(1) ? . . . . N(3) C(31) C(32) C(37) 10(1) ? . . . . C(36) C(31) C(32) C(33) -3(1) ? . . . . C(36) C(31) C(32) C(37) -177(1) ? . . . . N(3) C(31) C(36) C(35) 172.3(9) ? . . . . N(3) C(31) C(36) C(40) 0(1) ? . . . . C(32) C(31) C(36) C(35) 0(1) ? . . . . C(32) C(31) C(36) C(40) -172(1) ? . . . . C(31) C(32) C(33) C(34) 3(1) ? . . . . C(37) C(32) C(33) C(34) 177(1) ? . . . . C(31) C(32) C(37) C(38) 98(1) ? . . . . C(31) C(32) C(37) C(39) -137(1) ? . . . . C(33) C(32) C(37) C(38) -75(1) ? . . . . C(33) C(32) C(37) C(39) 48(1) ? . . . . C(32) C(33) C(34) C(35) 0(1) ? . . . . C(33) C(34) C(35) C(36) -3(1) ? . . . . C(34) C(35) C(36) C(31) 3(1) ? . . . . C(34) C(35) C(36) C(40) 176(1) ? . . . . C(31) C(36) C(40) C(41) 106(1) ? . . . . C(31) C(36) C(40) C(42) -124(1) ? . . . . C(35) C(36) C(40) C(41) -65(1) ? . . . . C(35) C(36) C(40) C(42) 63(1) ? . . . . N(4) C(43) C(44) C(45) -178.0(7) ? . . . . N(4) C(43) C(44) C(49) -0.3(9) ? . . . . C(48) C(43) C(44) C(45) -5(1) ? . . . . C(48) C(43) C(44) C(49) 172.6(8) ? . . . . N(4) C(43) C(48) C(47) 176.9(7) ? . . . . N(4) C(43) C(48) C(52) -4(1) ? . . . . C(44) C(43) C(48) C(47) 4(1) ? . . . . C(44) C(43) C(48) C(52) -177.2(8) ? . . . . C(43) C(44) C(45) C(46) 1(1) ? . . . . C(49) C(44) C(45) C(46) -176.0(8) ? . . . . C(43) C(44) C(49) C(50) 155.7(8) ? . . . . C(43) C(44) C(49) C(51) -81(1) ? . . . . C(45) C(44) C(49) C(50) -26(1) ? . . . . C(45) C(44) C(49) C(51) 96(1) ? . . . . C(44) C(45) C(46) C(47) 2(1) ? . . . . C(45) C(46) C(47) C(48) -3(1) ? . . . . C(46) C(47) C(48) C(43) 0(1) ? . . . . C(46) C(47) C(48) C(52) -178.3(8) ? . . . . C(43) C(48) C(52) C(53) -81(1) ? . . . . C(43) C(48) C(52) C(54) 149(1) ? . . . . C(47) C(48) C(52) C(53) 96(1) ? . . . . C(47) C(48) C(52) C(54) -31(1) ? . . . .
1100782.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $ #$Revision: 176435 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100782.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100782 loop_ _publ_author_name 'Chizu Shimokawa' 'Shinobu Itoh' _publ_section_title ; The First \b-Diketiminate-Ag(I) Complexes. Macrocyclic Dinuclear and Tetranuclear Ag(I)-Complexes and Linear Coordination Polymer Ag(I)-Complex ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3010 _journal_page_last 3012 _journal_paper_doi 10.1021/ic0501014 _journal_volume 44 _journal_year 2005 _chemical_formula_moiety 'C113 H146 Ag4 Cl2 N12 ' _chemical_formula_sum 'C113 H146 Ag4 Cl2 N12' _chemical_formula_weight 2174.85 _space_group_IT_number 11 _symmetry_cell_setting monoclinic _symmetry_Int_Tables_number 11 _symmetry_space_group_name_Hall '-P 2yb' _symmetry_space_group_name_H-M 'P 1 21/m 1' _cell_angle_alpha 90 _cell_angle_beta 118.873(3) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 14.866(4) _cell_length_b 28.120(7) _cell_length_c 17.752(5) _cell_measurement_reflns_used 14115 _cell_measurement_temperature 153.1 _cell_measurement_theta_max 27.5 _cell_measurement_theta_min 4.1 _cell_volume 6498(3) _computing_cell_refinement CrystalClear _computing_data_collection CrystalClear _computing_data_reduction CrystalStructure _computing_molecular_graphics ORTEP3 _computing_publication_material 'CrystalStructure 3.6.0' _computing_structure_refinement CRYSTALS _computing_structure_solution SIR92 _diffrn_detector_area_resol_mean 7.31 _diffrn_measured_fraction_theta_full 0.9871 _diffrn_measured_fraction_theta_max 0.9871 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents 0.050 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 51621 _diffrn_reflns_theta_full 27.48 _diffrn_reflns_theta_max 27.48 _exptl_absorpt_coefficient_mu 0.676 _exptl_absorpt_correction_T_max 0.874 _exptl_absorpt_correction_T_min 0.845 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Higashi, T. (1999). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.111 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 2260.00 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _refine_diff_density_max 0.89 _refine_diff_density_min -0.66 _refine_ls_extinction_coef 588.7(67) _refine_ls_extinction_method 'Larson (1970) Crystallographic Computing eq. 22' _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_hydrogen_treatment refall _refine_ls_number_parameters 681 _refine_ls_number_reflns 13680 _refine_ls_R_factor_gt 0.0500 _refine_ls_shift/su_max 0.0000 _refine_ls_structure_factor_coef F _refine_ls_weighting_details 'w = 1/[0.0005Fo^2^ + 1.0000\s(Fo^2^)]' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.0520 _reflns_number_gt 13680 _reflns_number_total 44453 _reflns_threshold_expression F^2^>2.0\s(F^2^) _cod_data_source_file ic0501014si20050122_011347_3.cif _cod_data_source_block '__Ag4(L4)4(CH2Cl2)' _cod_original_cell_volume 6498.5(33) _cod_original_formula_sum 'C113 H146 Ag4 Cl2 N12 ' _cod_database_code 1100782 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,-Z 3 -X,-Y,-Z 4 +X,1/2-Y,+Z loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag(1) Ag 0.28805(2) 0.143710(10) 0.10556(2) 0.03869(8) Uani 1.00 1 d . . . Ag(2) Ag 0.20194(2) 0.145370(10) 0.40093(2) 0.03677(8) Uani 1.00 1 d . . . Cl(1) Cl -0.0339(6) 0.2500 0.1634(2) 0.232(2) Uani 1.00 2 d S . . Cl(2) Cl -0.0292(5) 0.2500 0.0118(5) 0.355(5) Uani 1.00 2 d S . . N(1) N 0.4003(2) 0.10064(10) 0.2029(2) 0.0350(7) Uani 1.00 1 d . . . N(2) N 0.3353(2) 0.10208(10) 0.4457(2) 0.0408(8) Uani 1.00 1 d . . . N(3) N 0.2127(3) 0.16576(13) 0.2359(2) 0.0553(11) Uani 1.00 1 d . . . N(4) N 0.1906(3) 0.16473(9) -0.0238(2) 0.0414(8) Uani 1.00 1 d . . . N(5) N 0.3268(4) 0.2500 0.1535(3) 0.058(2) Uani 1.00 2 d S . . N(6) N 0.0501(2) 0.16456(9) 0.3719(2) 0.0336(7) Uani 1.00 1 d . . . N(7) N 0.2574(3) 0.2500 0.4278(4) 0.058(2) Uani 1.00 2 d S . . C(1) C 0.3623(3) 0.10840(12) 0.3208(2) 0.0369(9) Uani 1.00 1 d . . . C(2) C 0.4170(3) 0.08970(11) 0.2808(2) 0.0353(9) Uani 1.00 1 d . . . C(3) C 0.3830(3) 0.09054(12) 0.4025(2) 0.0371(9) Uani 1.00 1 d . . . C(4) C 0.2793(3) 0.14085(12) 0.2747(2) 0.0379(9) Uani 1.00 1 d . . . C(5) C 0.4636(3) 0.07602(11) 0.1736(2) 0.0354(9) Uani 1.00 1 d . . . C(6) C 0.5560(3) 0.09668(13) 0.1865(3) 0.0462(11) Uani 1.00 1 d . . . C(7) C 0.6143(3) 0.0712(1) 0.1616(3) 0.0544(13) Uani 1.00 1 d . . . C(8) C 0.5864(3) 0.0282(1) 0.1212(3) 0.0465(11) Uani 1.00 1 d . . . C(9) C 0.4897(3) 0.0092(2) 0.1036(3) 0.0519(11) Uani 1.00 1 d . . . C(10) C 0.4279(3) 0.03259(13) 0.1299(2) 0.0397(9) Uani 1.00 1 d . . . C(11) C 0.5903(4) 0.1443(2) 0.2305(4) 0.073(2) Uani 1.00 1 d . . . C(12) C 0.615(2) 0.1774(3) 0.172(2) 0.347(13) Uani 1.00 1 d . . . C(13) C 0.6797(8) 0.1408(4) 0.3103(12) 0.290(7) Uani 1.00 1 d . . . C(14) C 0.3205(3) 0.0121(2) 0.1084(3) 0.0504(11) Uani 1.00 1 d . . . C(15) C 0.2622(4) -0.0023(2) 0.0161(3) 0.067(2) Uani 1.00 1 d . . . C(16) C 0.3351(5) -0.0285(3) 0.1696(4) 0.112(3) Uani 1.00 1 d . . . C(17) C 0.3570(3) 0.07412(13) 0.5194(2) 0.0412(10) Uani 1.00 1 d . . . C(18) C 0.3237(3) 0.0262(1) 0.5089(3) 0.0442(10) Uani 1.00 1 d . . . C(19) C 0.3404(3) 0.0001(2) 0.5831(3) 0.0584(13) Uani 1.00 1 d . . . C(20) C 0.3829(4) 0.0223(2) 0.6625(3) 0.067(2) Uani 1.00 1 d . . . C(21) C 0.4145(4) 0.0683(2) 0.6706(3) 0.072(2) Uani 1.00 1 d . . . C(22) C 0.4027(3) 0.0968(2) 0.6002(3) 0.0544(12) Uani 1.00 1 d . . . C(23) C 0.2705(4) 0.0018(2) 0.4235(3) 0.0577(13) Uani 1.00 1 d . . . C(24) C 0.3362(6) -0.0384(2) 0.4145(4) 0.105(2) Uani 1.00 1 d . . . C(25) C 0.1631(5) -0.0121(3) 0.4023(4) 0.115(3) Uani 1.00 1 d . . . C(26) C 0.4315(6) 0.1470(2) 0.6088(4) 0.085(2) Uani 1.00 1 d . . . C(27) C 0.5395(10) 0.1560(5) 0.6429(13) 0.257(7) Uani 1.00 1 d . . . C(28) C 0.3937(12) 0.1736(3) 0.6580(9) 0.202(6) Uani 1.00 1 d . . . C(29) C 0.1960(4) 0.2500 -0.0081(3) 0.0345(12) Uani 1.00 2 d S . . C(30) C 0.1649(3) 0.20670(11) -0.0543(2) 0.0368(9) Uani 1.00 1 d . . . C(31) C 0.2715(4) 0.2500 0.0829(3) 0.0375(13) Uani 1.00 2 d S . . C(32) C 0.1592(4) 0.12674(13) -0.0877(2) 0.0495(11) Uani 1.00 1 d . . . C(33) C 0.0652(4) 0.1029(1) -0.1100(3) 0.0630(13) Uani 1.00 1 d . . . C(34) C 0.0337(5) 0.0694(2) -0.1765(4) 0.076(2) Uani 1.00 1 d . . . C(35) C 0.0930(5) 0.0598(2) -0.2130(3) 0.066(2) Uani 1.00 1 d . . . C(36) C 0.1871(5) 0.0819(2) -0.1870(3) 0.068(2) Uani 1.00 1 d . . . C(37) C 0.2208(5) 0.11809(13) -0.1223(3) 0.0618(13) Uani 1.00 1 d . . . C(38) C -0.0007(5) 0.1107(2) -0.0682(5) 0.092(2) Uani 1.00 1 d . . . C(39) C -0.0259(7) 0.0656(3) -0.0385(5) 0.115(3) Uani 1.00 1 d . . . C(40) C -0.0954(6) 0.1368(3) -0.1249(9) 0.162(4) Uani 1.00 1 d . . . C(41) C 0.3214(5) 0.1425(2) -0.0948(3) 0.068(2) Uani 1.00 1 d . . . C(42) C 0.3164(9) 0.1788(3) -0.1586(6) 0.164(5) Uani 1.00 1 d . . . C(43) C 0.4156(6) 0.1105(2) -0.0733(4) 0.106(2) Uani 1.00 1 d . . . C(44) C 0.0631(3) 0.2500 0.3795(3) 0.0297(11) Uani 1.00 2 d S . . C(45) C 0.0114(3) 0.20606(11) 0.3680(2) 0.0347(9) Uani 1.00 1 d . . . C(46) C 0.1688(4) 0.2500 0.4037(3) 0.0330(12) Uani 1.00 2 d S . . C(47) C -0.0123(3) 0.12320(11) 0.3601(2) 0.0377(9) Uani 1.00 1 d . . . C(48) C -0.0241(3) 0.10494(13) 0.4298(3) 0.0503(12) Uani 1.00 1 d . . . C(49) C -0.0814(4) 0.0635(2) 0.4160(4) 0.063(2) Uani 1.00 1 d . . . C(50) C -0.1297(4) 0.0426(1) 0.3362(4) 0.061(1) Uani 1.00 1 d . . . C(51) C -0.1148(4) 0.05944(13) 0.2714(3) 0.0573(13) Uani 1.00 1 d . . . C(52) C -0.0541(3) 0.09943(12) 0.2812(3) 0.0488(11) Uani 1.00 1 d . . . C(53) C 0.0333(4) 0.1275(2) 0.5189(3) 0.065(2) Uani 1.00 1 d . . . C(54) C 0.1264(6) 0.0989(3) 0.5776(4) 0.136(3) Uani 1.00 1 d . . . C(55) C -0.0313(6) 0.1302(3) 0.5648(5) 0.106(3) Uani 1.00 1 d . . . C(56) C -0.0393(3) 0.1161(1) 0.2094(3) 0.0501(11) Uani 1.00 1 d . . . C(57) C -0.1359(5) 0.1262(2) 0.1230(3) 0.079(2) Uani 1.00 1 d . . . C(58) C 0.0278(5) 0.0781(2) 0.1943(4) 0.085(2) Uani 1.00 1 d . . . C(59) C 0.0443(10) 0.2500 0.1093(11) 0.125(5) Uani 1.00 2 d S . . H(1) H 0.4697 0.0672 0.3121 0.044 Uiso 1.00 1 c R . . H(2) H 0.4377 0.0683 0.4292 0.045 Uiso 1.00 1 c R . . H(3) H 0.6765 0.0848 0.1689 0.067 Uiso 1.00 1 c R . . H(4) H 0.6300 0.0107 0.1061 0.060 Uiso 1.00 1 c R . . H(5) H 0.4673 -0.0203 0.0743 0.062 Uiso 1.00 1 c R . . H(6) H 0.5355 0.1593 0.2346 0.087 Uiso 1.00 1 c R . . H(7) H 0.6874 0.1734 0.1990 0.547 Uiso 1.00 1 c R . . H(8) H 0.5995 0.2096 0.1773 0.547 Uiso 1.00 1 c R . . H(9) H 0.5854 0.1692 0.1131 0.547 Uiso 1.00 1 c R . . H(10) H 0.6591 0.1358 0.3527 0.262 Uiso 1.00 1 c R . . H(11) H 0.7201 0.1689 0.3237 0.262 Uiso 1.00 1 c R . . H(12) H 0.7190 0.1144 0.3094 0.262 Uiso 1.00 1 c R . . H(13) H 0.2824 0.0370 0.1162 0.055 Uiso 1.00 1 c R . . H(14) H 0.2218 0.0234 -0.0184 0.076 Uiso 1.00 1 c R . . H(15) H 0.2187 -0.0281 0.0117 0.076 Uiso 1.00 1 c R . . H(16) H 0.3088 -0.0122 -0.0031 0.076 Uiso 1.00 1 c R . . H(17) H 0.3413 -0.0579 0.1461 0.125 Uiso 1.00 1 c R . . H(18) H 0.2752 -0.0290 0.1760 0.125 Uiso 1.00 1 c R . . H(19) H 0.3938 -0.0237 0.2242 0.125 Uiso 1.00 1 c R . . H(20) H 0.3229 -0.0327 0.5772 0.065 Uiso 1.00 1 c R . . H(21) H 0.3875 0.0054 0.7106 0.080 Uiso 1.00 1 c R . . H(22) H 0.4469 0.0828 0.7258 0.086 Uiso 1.00 1 c R . . H(23) H 0.2640 0.0252 0.3826 0.067 Uiso 1.00 1 c R . . H(24) H 0.3792 -0.0262 0.3932 0.117 Uiso 1.00 1 c R . . H(25) H 0.2917 -0.0618 0.3760 0.117 Uiso 1.00 1 c R . . H(26) H 0.3774 -0.0523 0.4695 0.117 Uiso 1.00 1 c R . . H(27) H 0.1628 -0.0432 0.4233 0.134 Uiso 1.00 1 c R . . H(28) H 0.1185 -0.0113 0.3419 0.134 Uiso 1.00 1 c R . . H(29) H 0.1402 0.0101 0.4297 0.134 Uiso 1.00 1 c R . . H(30) H 0.4070 0.1600 0.5528 0.098 Uiso 1.00 1 c R . . H(31) H 0.5609 0.1591 0.7025 0.285 Uiso 1.00 1 c R . . H(32) H 0.5602 0.1833 0.6236 0.285 Uiso 1.00 1 c R . . H(33) H 0.5702 0.1285 0.6339 0.285 Uiso 1.00 1 c R . . H(34) H 0.3279 0.1858 0.6186 0.270 Uiso 1.00 1 c R . . H(35) H 0.4391 0.1992 0.6867 0.270 Uiso 1.00 1 c R . . H(36) H 0.3880 0.1539 0.6989 0.270 Uiso 1.00 1 c R . . H(37) H 0.1184 0.2092 -0.1141 0.038 Uiso 1.00 1 c R . . H(38) H -0.0278 0.0518 -0.1941 0.084 Uiso 1.00 1 c R . . H(39) H 0.0697 0.0379 -0.2595 0.074 Uiso 1.00 1 c R . . H(40) H 0.2276 0.0731 -0.2129 0.083 Uiso 1.00 1 c R . . H(41) H 0.0360 0.1306 -0.0195 0.105 Uiso 1.00 1 c R . . H(42) H -0.0891 0.0539 -0.0833 0.146 Uiso 1.00 1 c R . . H(43) H -0.0328 0.0718 0.0111 0.146 Uiso 1.00 1 c R . . H(44) H 0.0265 0.0426 -0.0250 0.146 Uiso 1.00 1 c R . . H(45) H -0.0862 0.1703 -0.1182 0.184 Uiso 1.00 1 c R . . H(46) H -0.1486 0.1274 -0.1130 0.184 Uiso 1.00 1 c R . . H(47) H -0.1134 0.1283 -0.1822 0.184 Uiso 1.00 1 c R . . H(48) H 0.3363 0.1594 -0.0438 0.092 Uiso 1.00 1 c R . . H(49) H 0.3363 0.1636 -0.1961 0.230 Uiso 1.00 1 c R . . H(50) H 0.3592 0.2056 -0.1328 0.230 Uiso 1.00 1 c R . . H(51) H 0.2469 0.1888 -0.1904 0.230 Uiso 1.00 1 c R . . H(52) H 0.4480 0.0991 -0.0158 0.130 Uiso 1.00 1 c R . . H(53) H 0.4632 0.1287 -0.0826 0.130 Uiso 1.00 1 c R . . H(54) H 0.3923 0.0843 -0.1119 0.130 Uiso 1.00 1 c R . . H(55) H -0.0586 0.2074 0.3548 0.045 Uiso 1.00 1 c R . . H(56) H -0.0886 0.0506 0.4622 0.083 Uiso 1.00 1 c R . . H(57) H -0.1723 0.0157 0.3273 0.076 Uiso 1.00 1 c R . . H(58) H -0.1456 0.0432 0.2178 0.072 Uiso 1.00 1 c R . . H(59) H 0.0537 0.1587 0.5130 0.087 Uiso 1.00 1 c R . . H(60) H 0.1078 0.0756 0.6062 0.149 Uiso 1.00 1 c R . . H(61) H 0.1763 0.1197 0.6189 0.149 Uiso 1.00 1 c R . . H(62) H 0.1541 0.0838 0.5455 0.149 Uiso 1.00 1 c R . . H(63) H -0.0706 0.1587 0.5495 0.135 Uiso 1.00 1 c R . . H(64) H 0.0141 0.1299 0.6251 0.135 Uiso 1.00 1 c R . . H(65) H -0.0760 0.1036 0.5495 0.135 Uiso 1.00 1 c R . . H(66) H -0.0013 0.1449 0.2271 0.057 Uiso 1.00 1 c R . . H(67) H -0.1579 0.0980 0.0894 0.095 Uiso 1.00 1 c R . . H(68) H -0.1251 0.1505 0.0910 0.095 Uiso 1.00 1 c R . . H(69) H -0.1870 0.1361 0.1371 0.095 Uiso 1.00 1 c R . . H(70) H 0.0987 0.0850 0.2299 0.117 Uiso 1.00 1 c R . . H(71) H 0.0117 0.0792 0.1356 0.117 Uiso 1.00 1 c R . . H(72) H 0.0132 0.0473 0.2076 0.117 Uiso 1.00 1 c R . . H(73) H 0.089(4) 0.279(2) 0.133(3) 0.056(12) Uiso 1.00 1 c . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ag(1) 0.0442(2) 0.0360(2) 0.0323(2) 0.01036(12) 0.01556(13) 0.00913(11) Ag(2) 0.0340(2) 0.0396(2) 0.0400(2) 0.01120(12) 0.02051(13) 0.00685(12) Cl(1) 0.537(10) 0.072(2) 0.119(2) 0.0000 0.183(4) 0.0000 Cl(2) 0.152(4) 0.77(2) 0.221(6) 0.0000 0.149(5) 0.0000 N(1) 0.030(1) 0.046(2) 0.0236(13) 0.0127(12) 0.0092(12) 0.0060(12) N(2) 0.040(2) 0.047(2) 0.041(2) 0.0146(13) 0.024(1) 0.0104(13) N(3) 0.062(2) 0.054(2) 0.058(2) 0.022(2) 0.035(2) 0.021(2) N(4) 0.054(2) 0.0233(13) 0.033(2) -0.0048(13) 0.010(1) -0.0043(11) N(5) 0.066(3) 0.061(3) 0.027(3) 0.0000 0.006(3) 0.0000 N(6) 0.032(1) 0.0283(13) 0.042(2) 0.0031(11) 0.0188(13) 0.0064(11) N(7) 0.030(3) 0.046(3) 0.099(5) 0.0000 0.031(3) 0.0000 C(1) 0.036(2) 0.042(2) 0.032(2) 0.009(2) 0.016(2) 0.013(1) C(2) 0.037(2) 0.036(2) 0.037(2) 0.008(1) 0.021(2) 0.009(1) C(3) 0.038(2) 0.042(2) 0.033(2) 0.011(2) 0.018(2) 0.002(1) C(4) 0.043(2) 0.040(2) 0.042(2) 0.011(2) 0.029(2) 0.010(2) C(5) 0.043(2) 0.033(2) 0.029(2) 0.012(1) 0.016(2) 0.0038(13) C(6) 0.048(2) 0.042(2) 0.054(2) 0.005(2) 0.029(2) -0.000(2) C(7) 0.047(2) 0.045(2) 0.077(3) 0.011(2) 0.034(2) 0.010(2) C(8) 0.053(2) 0.051(2) 0.046(2) 0.018(2) 0.032(2) 0.006(2) C(9) 0.049(2) 0.063(2) 0.043(2) 0.026(2) 0.022(2) 0.003(2) C(10) 0.038(2) 0.050(2) 0.029(2) 0.012(2) 0.014(2) 0.003(2) C(11) 0.042(2) 0.042(2) 0.133(5) -0.002(2) 0.042(3) -0.014(3) C(12) 0.65(4) 0.056(5) 0.66(4) -0.091(11) 0.58(3) -0.074(11) C(13) 0.124(8) 0.140(9) 0.39(2) 0.032(7) -0.047(11) -0.180(13) C(14) 0.041(2) 0.057(2) 0.039(2) 0.003(2) 0.009(2) 0.001(2) C(15) 0.054(3) 0.072(3) 0.063(3) -0.013(2) 0.019(2) -0.015(2) C(16) 0.078(4) 0.150(6) 0.084(5) -0.059(4) 0.020(4) 0.024(4) C(17) 0.040(2) 0.056(2) 0.031(2) 0.020(2) 0.020(2) 0.015(2) C(18) 0.034(2) 0.055(2) 0.042(2) 0.016(2) 0.018(2) 0.019(2) C(19) 0.038(2) 0.078(3) 0.047(3) 0.006(2) 0.010(2) 0.015(2) C(20) 0.074(3) 0.081(4) 0.046(3) 0.020(3) 0.030(3) 0.029(2) C(21) 0.069(3) 0.110(4) 0.035(2) 0.027(3) 0.023(2) 0.002(2) C(22) 0.051(2) 0.077(3) 0.032(2) 0.025(2) 0.018(2) 0.008(2) C(23) 0.067(3) 0.053(2) 0.047(2) 0.001(2) 0.024(2) 0.013(2) C(24) 0.117(6) 0.099(5) 0.078(4) 0.046(4) 0.029(4) 0.003(3) C(25) 0.084(4) 0.196(8) 0.056(4) -0.073(5) 0.027(3) -0.019(4) C(26) 0.119(5) 0.078(4) 0.049(3) 0.029(3) 0.034(3) 0.001(2) C(27) 0.144(9) 0.194(11) 0.37(2) -0.116(9) 0.079(12) -0.120(13) C(28) 0.30(2) 0.097(6) 0.28(2) 0.012(8) 0.20(1) -0.053(8) C(29) 0.049(3) 0.022(2) 0.032(2) 0.0000 0.019(2) 0.0000 C(30) 0.042(2) 0.026(2) 0.026(2) -0.0004(13) 0.004(2) -0.0009(12) C(31) 0.036(3) 0.039(3) 0.038(3) 0.0000 0.018(2) 0.0000 C(32) 0.077(3) 0.035(2) 0.029(2) 0.007(2) 0.019(2) 0.005(1) C(33) 0.069(3) 0.036(2) 0.060(3) -0.016(2) 0.012(2) -0.015(2) C(34) 0.097(4) 0.048(3) 0.064(3) -0.012(3) 0.024(3) -0.025(2) C(35) 0.093(4) 0.041(2) 0.050(3) -0.007(2) 0.022(3) -0.005(2) C(36) 0.119(5) 0.046(2) 0.042(2) 0.025(3) 0.042(3) -0.000(2) C(37) 0.111(4) 0.035(2) 0.033(2) 0.011(2) 0.029(3) 0.006(2) C(38) 0.071(4) 0.070(3) 0.122(5) -0.018(3) 0.036(4) -0.037(3) C(39) 0.147(6) 0.121(5) 0.098(5) -0.081(5) 0.075(5) -0.057(4) C(40) 0.071(4) 0.144(7) 0.245(13) 0.050(5) 0.057(6) 0.017(7) C(41) 0.107(4) 0.046(2) 0.076(3) -0.006(3) 0.065(3) -0.010(2) C(42) 0.265(12) 0.129(6) 0.181(8) 0.095(7) 0.174(9) 0.108(6) C(43) 0.169(7) 0.079(4) 0.077(4) 0.013(5) 0.064(5) 0.017(3) C(44) 0.025(2) 0.035(2) 0.029(2) 0.0000 0.013(2) 0.0000 C(45) 0.034(2) 0.037(2) 0.042(2) 0.005(1) 0.025(2) 0.006(1) C(46) 0.028(3) 0.025(2) 0.043(3) 0.0000 0.014(2) 0.0000 C(47) 0.044(2) 0.024(2) 0.047(2) -0.000(1) 0.023(2) 0.008(1) C(48) 0.052(2) 0.041(2) 0.074(3) 0.000(2) 0.043(2) 0.008(2) C(49) 0.077(3) 0.046(2) 0.085(4) -0.001(2) 0.054(3) 0.006(2) C(50) 0.057(3) 0.036(2) 0.097(4) -0.014(2) 0.042(3) -0.001(2) C(51) 0.057(3) 0.031(2) 0.092(3) -0.012(2) 0.042(3) -0.012(2) C(52) 0.056(2) 0.024(2) 0.072(3) 0.005(2) 0.035(2) 0.002(2) C(53) 0.085(3) 0.054(2) 0.078(3) -0.005(2) 0.058(3) 0.013(2) C(54) 0.133(6) 0.184(8) 0.055(4) 0.063(7) 0.017(4) 0.028(5) C(55) 0.120(6) 0.105(5) 0.112(6) 0.013(4) 0.073(5) 0.004(4) C(56) 0.047(2) 0.043(2) 0.053(2) -0.008(2) 0.018(2) -0.007(2) C(57) 0.093(4) 0.088(3) 0.058(3) -0.028(3) 0.038(3) -0.016(3) C(58) 0.111(5) 0.083(4) 0.098(4) -0.025(3) 0.080(4) -0.039(3) C(59) 0.121(9) 0.051(5) 0.21(2) 0.0000 0.090(10) 0.0000 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Ag Ag -0.897 1.101 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 N(4) Ag(1) N(1) 154.4(1) ? . . . Ag(1) N(1) C(2) 131.8(3) ? . . . Ag(1) N(1) C(5) 112.0(2) ? . . . Ag(1) N(4) C(30) 128.6(2) ? . . . Ag(1) N(4) C(32) 115.6(2) ? . . . N(6) Ag(2) N(2) 157.6(1) ? . . . Ag(2) N(2) C(3) 126.3(2) ? . . . Ag(2) N(2) C(17) 114.6(3) ? . . . Ag(2) N(6) C(45) 129.6(3) ? . . . Ag(2) N(6) C(47) 111.4(2) ? . . . Cl(1) C(59) Cl(2) 107.7(9) ? . . . N(1) C(2) C(1) 125.2(3) ? . . . C(5) N(1) C(2) 116.0(3) ? . . . N(1) C(5) C(6) 119.7(3) ? . . . N(1) C(5) C(10) 118.3(4) ? . . . N(2) C(3) C(1) 126.7(3) ? . . . C(17) N(2) C(3) 117.1(3) ? . . . N(2) C(17) C(18) 119.6(3) ? . . . N(2) C(17) C(22) 118.0(3) ? . . . N(3) C(4) C(1) 177.7(4) ? . . . N(4) C(30) C(29) 127.1(3) ? . . . C(32) N(4) C(30) 115.4(3) ? . . . N(4) C(32) C(33) 117.6(5) ? . . . N(4) C(32) C(37) 116.9(4) ? . . . N(5) C(31) C(29) 177.5(8) ? . . . N(6) C(45) C(44) 125.7(4) ? . . . C(47) N(6) C(45) 118.9(3) ? . . . N(6) C(47) C(52) 118.4(4) ? . . . N(6) C(47) C(48) 120.4(3) ? . . . N(7) C(46) C(44) 176.8(7) ? . . . C(4) C(1) C(2) 119.8(3) ? . . . C(3) C(1) C(2) 119.1(3) ? . . . C(4) C(1) C(3) 120.7(4) ? . . . C(10) C(5) C(6) 121.9(4) ? . . . C(5) C(6) C(11) 120.8(5) ? . . . C(5) C(6) C(7) 117.3(3) ? . . . C(5) C(10) C(14) 121.6(4) ? . . . C(5) C(10) C(9) 117.7(4) ? . . . C(11) C(6) C(7) 121.9(5) ? . . . C(6) C(7) C(8) 124.1(5) ? . . . C(6) C(11) C(13) 112.3(6) ? . . . C(6) C(11) C(12) 108.4(9) ? . . . C(7) C(8) C(9) 117.9(5) ? . . . C(8) C(9) C(10) 121.0(4) ? . . . C(9) C(10) C(14) 120.7(3) ? . . . C(10) C(14) C(16) 109.1(4) ? . . . C(10) C(14) C(15) 110.6(4) ? . . . C(13) C(11) C(12) 107(1) ? . . . C(16) C(14) C(15) 112.8(4) ? . . . C(22) C(17) C(18) 122.1(4) ? . . . C(17) C(18) C(23) 123.4(4) ? . . . C(17) C(18) C(19) 118.4(4) ? . . . C(17) C(22) C(26) 121.0(4) ? . . . C(17) C(22) C(21) 115.7(4) ? . . . C(23) C(18) C(19) 118.2(4) ? . . . C(18) C(19) C(20) 120.0(4) ? . . . C(18) C(23) C(25) 110.5(5) ? . . . C(18) C(23) C(24) 112.8(4) ? . . . C(19) C(20) C(21) 120.1(5) ? . . . C(20) C(21) C(22) 123.6(5) ? . . . C(21) C(22) C(26) 123.2(4) ? . . . C(22) C(26) C(27) 115.1(7) ? . . . C(22) C(26) C(28) 112.3(8) ? . . . C(25) C(23) C(24) 115.5(5) ? . . . C(28) C(26) C(27) 109(1) ? . . . C(31) C(29) C(30) 120.3(2) ? . . . C(30) C(29) C(30) 118.8(4) ? 55504 . . C(31) C(29) C(30) 120.3(2) ? . . 55504 C(29) C(30) N(4) 127.1(3) ? . 55504 55504 C(37) C(32) C(33) 125.5(4) ? . . . C(32) C(33) C(38) 125.5(4) ? . . . C(32) C(33) C(34) 115.7(6) ? . . . C(32) C(37) C(41) 124.1(4) ? . . . C(32) C(37) C(36) 116.2(5) ? . . . C(38) C(33) C(34) 118.8(5) ? . . . C(33) C(34) C(35) 120.7(6) ? . . . C(33) C(38) C(40) 111.8(8) ? . . . C(33) C(38) C(39) 112.6(6) ? . . . C(34) C(35) C(36) 122.5(5) ? . . . C(35) C(36) C(37) 119.4(6) ? . . . C(36) C(37) C(41) 119.6(6) ? . . . C(37) C(41) C(42) 112.9(5) ? . . . C(37) C(41) C(43) 117.2(4) ? . . . C(40) C(38) C(39) 110.3(7) ? . . . C(43) C(41) C(42) 106.9(8) ? . . . C(46) C(44) C(45) 119.3(2) ? . . . C(45) C(44) C(45) 121.3(4) ? 55504 . . C(46) C(44) C(45) 119.3(2) ? . . 55504 C(44) C(45) N(6) 125.7(4) ? . 55504 55504 C(52) C(47) C(48) 121.0(3) ? . . . C(47) C(48) C(53) 120.5(4) ? . . . C(47) C(48) C(49) 118.0(4) ? . . . C(47) C(52) C(56) 122.4(4) ? . . . C(47) C(52) C(51) 117.2(5) ? . . . C(53) C(48) C(49) 121.2(5) ? . . . C(48) C(49) C(50) 120.7(6) ? . . . C(48) C(53) C(54) 111.4(5) ? . . . C(48) C(53) C(55) 113.0(5) ? . . . C(49) C(50) C(51) 120.5(5) ? . . . C(50) C(51) C(52) 122.3(5) ? . . . C(51) C(52) C(56) 120.4(4) ? . . . C(52) C(56) C(58) 107.7(4) ? . . . C(52) C(56) C(57) 117.6(5) ? . . . C(55) C(53) C(54) 105.1(6) ? . . . C(58) C(56) C(57) 108.7(4) ? . . . Cl(1) C(59) H(73) 103(3) ? . . . Cl(1) C(59) H(73) 103(3) ? . . 55504 Cl(2) C(59) H(73) 115(2) ? . . . Cl(2) C(59) H(73) 115(2) ? . . 55504 N(1) C(2) H(1) 116.9596 ? . . . N(2) C(3) H(2) 116.3239 ? . . . N(4) C(30) H(37) 116.7760 ? . . . N(6) C(45) H(55) 117.2561 ? . . . C(1) C(2) H(1) 117.7931 ? . . . C(1) C(3) H(2) 117.0092 ? . . . C(6) C(7) H(3) 118.5814 ? . . . C(6) C(11) H(6) 110.1019 ? . . . H(3) C(7) C(8) 117.1965 ? . . . C(7) C(8) H(4) 122.2122 ? . . . C(8) C(9) H(5) 119.9090 ? . . . H(4) C(8) C(9) 119.8748 ? . . . H(5) C(9) C(10) 119.1216 ? . . . C(10) C(14) H(13) 107.7103 ? . . . H(6) C(11) C(12) 105.7341 ? . . . C(11) C(12) H(7) 99.7632 ? . . . C(11) C(12) H(8) 111.1320 ? . . . C(11) C(12) H(9) 116.9913 ? . . . H(6) C(11) C(13) 112.4901 ? . . . C(11) C(13) H(10) 107.4656 ? . . . C(11) C(13) H(12) 109.1383 ? . . . C(11) C(13) H(11) 111.7746 ? . . . H(8) C(12) H(7) 109.4711 ? . . . H(9) C(12) H(7) 109.4770 ? . . . H(9) C(12) H(8) 109.4761 ? . . . H(12) C(13) H(10) 109.4629 ? . . . H(11) C(13) H(10) 109.4742 ? . . . H(12) C(13) H(11) 109.4825 ? . . . H(13) C(14) C(15) 106.7238 ? . . . C(14) C(15) H(14) 110.6763 ? . . . C(14) C(15) H(16) 109.6860 ? . . . C(14) C(15) H(15) 108.0423 ? . . . H(13) C(14) C(16) 109.8021 ? . . . C(14) C(16) H(19) 111.5865 ? . . . C(14) C(16) H(17) 110.5599 ? . . . C(14) C(16) H(18) 106.2143 ? . . . H(16) C(15) H(14) 109.4662 ? . . . H(15) C(15) H(14) 109.4703 ? . . . H(16) C(15) H(15) 109.4753 ? . . . H(19) C(16) H(17) 109.4809 ? . . . H(18) C(16) H(17) 109.4662 ? . . . H(19) C(16) H(18) 109.4666 ? . . . C(18) C(19) H(20) 118.9499 ? . . . C(18) C(23) H(23) 105.4311 ? . . . H(20) C(19) C(20) 121.0465 ? . . . C(19) C(20) H(21) 119.2201 ? . . . C(20) C(21) H(22) 119.5850 ? . . . H(21) C(20) C(21) 120.6650 ? . . . H(22) C(21) C(22) 116.8129 ? . . . C(22) C(26) H(30) 108.5382 ? . . . H(23) C(23) C(24) 105.2442 ? . . . C(23) C(24) H(24) 110.9153 ? . . . C(23) C(24) H(25) 108.9341 ? . . . C(23) C(24) H(26) 108.5590 ? . . . H(23) C(23) C(25) 106.4935 ? . . . C(23) C(25) H(29) 107.4864 ? . . . C(23) C(25) H(27) 110.1669 ? . . . C(23) C(25) H(28) 110.7331 ? . . . H(25) C(24) H(24) 109.4667 ? . . . H(26) C(24) H(24) 109.4789 ? . . . H(26) C(24) H(25) 109.4636 ? . . . H(29) C(25) H(27) 109.4788 ? . . . H(28) C(25) H(27) 109.4784 ? . . . H(29) C(25) H(28) 109.4645 ? . . . H(30) C(26) C(27) 99.1353 ? . . . C(26) C(27) H(33) 108.4383 ? . . . C(26) C(27) H(31) 100.9266 ? . . . C(26) C(27) H(32) 118.5787 ? . . . H(30) C(26) C(28) 111.5046 ? . . . C(26) C(28) H(34) 107.5954 ? . . . C(26) C(28) H(36) 111.3743 ? . . . C(26) C(28) H(35) 109.4282 ? . . . H(33) C(27) H(31) 109.4791 ? . . . H(32) C(27) H(31) 109.4684 ? . . . H(33) C(27) H(32) 109.4649 ? . . . H(36) C(28) H(34) 109.4699 ? . . . H(35) C(28) H(34) 109.4695 ? . . . H(36) C(28) H(35) 109.4681 ? . . . C(29) C(30) H(37) 116.1410 ? . . . C(29) C(30) H(37) 116.1410 ? . 55504 55504 C(33) C(34) H(38) 120.2408 ? . . . C(33) C(38) H(41) 108.0402 ? . . . H(38) C(34) C(35) 118.9913 ? . . . C(34) C(35) H(39) 119.9160 ? . . . C(35) C(36) H(40) 119.7322 ? . . . H(39) C(35) C(36) 117.6008 ? . . . H(40) C(36) C(37) 120.9053 ? . . . C(37) C(41) H(48) 106.0186 ? . . . H(41) C(38) C(39) 108.2455 ? . . . C(38) C(39) H(44) 110.7494 ? . . . C(38) C(39) H(42) 108.4810 ? . . . C(38) C(39) H(43) 109.1793 ? . . . H(41) C(38) C(40) 105.5153 ? . . . C(38) C(40) H(45) 112.1565 ? . . . C(38) C(40) H(47) 106.7866 ? . . . C(38) C(40) H(46) 109.4207 ? . . . H(44) C(39) H(42) 109.4668 ? . . . H(43) C(39) H(42) 109.4694 ? . . . H(44) C(39) H(43) 109.4731 ? . . . H(47) C(40) H(45) 109.4756 ? . . . H(46) C(40) H(45) 109.4753 ? . . . H(47) C(40) H(46) 109.4679 ? . . . H(48) C(41) C(42) 106.4355 ? . . . C(41) C(42) H(51) 107.0887 ? . . . C(41) C(42) H(49) 107.7165 ? . . . C(41) C(42) H(50) 113.5339 ? . . . H(48) C(41) C(43) 106.7965 ? . . . C(41) C(43) H(52) 112.9323 ? . . . C(41) C(43) H(54) 107.5597 ? . . . C(41) C(43) H(53) 107.8665 ? . . . H(51) C(42) H(49) 109.4766 ? . . . H(50) C(42) H(49) 109.4693 ? . . . H(51) C(42) H(50) 109.4690 ? . . . H(54) C(43) H(52) 109.4608 ? . . . H(53) C(43) H(52) 109.4722 ? . . . H(54) C(43) H(53) 109.4830 ? . . . C(44) C(45) H(55) 116.9835 ? . . . C(44) C(45) H(55) 116.9835 ? . 55504 55504 C(48) C(49) H(56) 118.9526 ? . . . C(48) C(53) H(59) 108.5750 ? . . . H(56) C(49) C(50) 120.3311 ? . . . C(49) C(50) H(57) 119.1673 ? . . . C(50) C(51) H(58) 119.0579 ? . . . H(57) C(50) C(51) 120.3547 ? . . . H(58) C(51) C(52) 118.6601 ? . . . C(52) C(56) H(66) 107.3672 ? . . . C(53) C(54) H(62) 110.1031 ? . . . H(59) C(53) C(54) 109.5353 ? . . . C(53) C(54) H(61) 108.8411 ? . . . C(53) C(54) H(60) 109.4697 ? . . . H(59) C(53) C(55) 109.0537 ? . . . C(53) C(55) H(63) 110.2939 ? . . . C(53) C(55) H(64) 108.1992 ? . . . C(53) C(55) H(65) 109.8987 ? . . . H(62) C(54) H(60) 109.4597 ? . . . H(61) C(54) H(60) 109.4763 ? . . . H(62) C(54) H(61) 109.4750 ? . . . H(64) C(55) H(63) 109.4736 ? . . . H(65) C(55) H(63) 109.4796 ? . . . H(65) C(55) H(64) 109.4744 ? . . . H(66) C(56) C(57) 106.9716 ? . . . C(56) C(57) H(68) 112.4785 ? . . . C(56) C(57) H(69) 105.7570 ? . . . C(56) C(57) H(67) 110.1043 ? . . . H(66) C(56) C(58) 108.1494 ? . . . C(56) C(58) H(70) 109.9448 ? . . . C(56) C(58) H(71) 108.7328 ? . . . C(56) C(58) H(72) 109.7331 ? . . . H(68) C(57) H(67) 109.4738 ? . . . H(69) C(57) H(67) 109.4768 ? . . . H(69) C(57) H(68) 109.4631 ? . . . H(71) C(58) H(70) 109.4772 ? . . . H(72) C(58) H(70) 109.4609 ? . . . H(72) C(58) H(71) 109.4760 ? . . . H(73) C(59) H(73) 108(3) ? 55504 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Ag(1) N(1) 2.110(2) ? . . Ag(1) N(4) 2.123(3) ? . . Ag(2) N(2) 2.127(3) ? . . Ag(2) N(6) 2.128(3) ? . . Cl(1) C(59) 1.83(2) ? . . Cl(2) C(59) 1.54(2) ? . . N(1) C(2) 1.319(5) ? . . N(1) C(5) 1.451(6) ? . . N(2) C(3) 1.313(6) ? . . N(2) C(17) 1.424(5) ? . . N(3) C(4) 1.134(5) ? . . N(4) C(30) 1.277(4) ? . . N(4) C(32) 1.461(5) ? . . N(5) C(31) 1.119(6) ? . . N(6) C(45) 1.289(4) ? . . N(6) C(47) 1.439(4) ? . . N(7) C(46) 1.172(7) ? . . C(1) C(2) 1.414(6) ? . . C(1) C(3) 1.421(5) ? . . C(1) C(4) 1.431(5) ? . . C(5) C(6) 1.405(6) ? . . C(5) C(10) 1.406(5) ? . . C(6) C(7) 1.352(8) ? . . C(6) C(11) 1.509(6) ? . . C(7) C(8) 1.365(6) ? . . C(8) C(9) 1.420(7) ? . . C(9) C(10) 1.382(7) ? . . C(10) C(14) 1.561(6) ? . . C(11) C(12) 1.56(3) ? . . C(11) C(13) 1.40(1) ? . . C(14) C(15) 1.493(6) ? . . C(14) C(16) 1.517(9) ? . . C(17) C(18) 1.418(5) ? . . C(17) C(22) 1.408(5) ? . . C(18) C(19) 1.420(7) ? . . C(18) C(23) 1.495(6) ? . . C(19) C(18) 1.420(7) ? . . C(19) C(20) 1.386(7) ? . . C(20) C(19) 1.386(7) ? . . C(20) C(21) 1.359(8) ? . . C(21) C(22) 1.422(8) ? . . C(22) C(26) 1.464(8) ? . . C(23) C(24) 1.55(1) ? . . C(23) C(25) 1.505(9) ? . . C(26) C(27) 1.44(2) ? . . C(26) C(28) 1.45(2) ? . . C(29) C(30) 1.415(4) ? . . C(29) C(30) 1.415(4) ? . 55504 C(29) C(31) 1.456(6) ? . . C(32) C(33) 1.423(7) ? . . C(32) C(37) 1.348(9) ? . . C(33) C(34) 1.402(7) ? . . C(33) C(38) 1.50(1) ? . . C(34) C(35) 1.35(1) ? . . C(35) C(36) 1.390(9) ? . . C(36) C(37) 1.433(6) ? . . C(37) C(41) 1.496(9) ? . . C(38) C(39) 1.49(1) ? . . C(38) C(40) 1.47(1) ? . . C(41) C(42) 1.50(1) ? . . C(41) C(43) 1.55(1) ? . . C(44) C(45) 1.417(4) ? . . C(44) C(45) 1.417(4) ? . 55504 C(44) C(46) 1.414(7) ? . . C(44) C(46) 1.414(7) ? . 55504 C(45) C(44) 1.417(4) ? . . C(45) C(44) 1.417(4) ? . 55504 C(46) C(44) 1.414(7) ? . . C(46) C(44) 1.414(7) ? . 55504 C(47) C(48) 1.426(7) ? . . C(47) C(52) 1.397(6) ? . . C(48) C(49) 1.392(6) ? . . C(48) C(53) 1.526(7) ? . . C(49) C(50) 1.373(7) ? . . C(50) C(51) 1.36(1) ? . . C(51) C(52) 1.399(6) ? . . C(52) C(56) 1.473(8) ? . . C(53) C(54) 1.500(9) ? . . C(53) C(55) 1.53(1) ? . . C(56) C(57) 1.540(6) ? . . C(56) C(58) 1.569(9) ? . . C(2) H(1) 0.9500 ? . . C(3) H(2) 0.9500 ? . . C(7) H(3) 0.9501 ? . . C(8) H(4) 0.9499 ? . . C(9) H(5) 0.9500 ? . . C(11) H(6) 0.9500 ? . . C(12) H(7) 0.9500 ? . . C(12) H(8) 0.9501 ? . . C(12) H(9) 0.9500 ? . . C(13) H(10) 0.9500 ? . . C(13) H(11) 0.9500 ? . . C(13) H(12) 0.9500 ? . . C(14) H(13) 0.9501 ? . . C(15) H(14) 0.9499 ? . . C(15) H(15) 0.9500 ? . . C(15) H(16) 0.9499 ? . . C(16) H(17) 0.9499 ? . . C(16) H(18) 0.9500 ? . . C(16) H(19) 0.9500 ? . . C(19) H(20) 0.9500 ? . . C(20) H(21) 0.9500 ? . . C(21) H(22) 0.9501 ? . . C(23) H(23) 0.9500 ? . . C(24) H(24) 0.9500 ? . . C(24) H(25) 0.9501 ? . . C(24) H(26) 0.9501 ? . . C(25) H(27) 0.9499 ? . . C(25) H(28) 0.9500 ? . . C(25) H(29) 0.9500 ? . . C(26) H(30) 0.9500 ? . . C(27) H(31) 0.9500 ? . . C(27) H(32) 0.9499 ? . . C(27) H(33) 0.9500 ? . . C(28) H(34) 0.9500 ? . . C(28) H(35) 0.9500 ? . . C(28) H(36) 0.9500 ? . . C(30) H(37) 0.9500 ? . . C(34) H(38) 0.9501 ? . . C(35) H(39) 0.9500 ? . . C(36) H(40) 0.9500 ? . . C(38) H(41) 0.9501 ? . . C(39) H(42) 0.9500 ? . . C(39) H(43) 0.9500 ? . . C(39) H(44) 0.9500 ? . . C(40) H(45) 0.9501 ? . . C(40) H(46) 0.9501 ? . . C(40) H(47) 0.9500 ? . . C(41) H(48) 0.9499 ? . . C(42) H(49) 0.9501 ? . . C(42) H(50) 0.9501 ? . . C(42) H(51) 0.9500 ? . . C(43) H(52) 0.9500 ? . . C(43) H(53) 0.9500 ? . . C(43) H(54) 0.9500 ? . . C(45) H(55) 0.9501 ? . . C(49) H(56) 0.9500 ? . . C(50) H(57) 0.9501 ? . . C(51) H(58) 0.9500 ? . . C(53) H(59) 0.9500 ? . . C(54) H(60) 0.9500 ? . . C(54) H(61) 0.9499 ? . . C(54) H(62) 0.9499 ? . . C(55) H(63) 0.9501 ? . . C(55) H(64) 0.9500 ? . . C(55) H(65) 0.9500 ? . . C(56) H(66) 0.9500 ? . . C(57) H(67) 0.9499 ? . . C(57) H(68) 0.9500 ? . . C(57) H(69) 0.9501 ? . . C(58) H(70) 0.9500 ? . . C(58) H(71) 0.9500 ? . . C(58) H(72) 0.9500 ? . . C(59) H(73) 1.01(5) ? . . C(59) H(73) 1.01(5) ? . 55504 H(20) C(19) 0.9500 ? . . H(67) C(57) 0.9499 ? . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Ag(1) N(3) 3.081(5) ? . . Ag(1) N(5) 3.085(1) ? . . Ag(1) C(1) 3.568(4) ? . . Ag(1) C(2) 3.147(3) ? . . Ag(1) C(4) 3.070(5) ? . . Ag(1) C(5) 2.974(3) ? . . Ag(1) C(29) 3.494(2) ? . . Ag(1) C(30) 3.086(3) ? . . Ag(1) C(31) 3.0100(6) ? . . Ag(1) C(32) 3.053(4) ? . . Ag(2) N(3) 3.065(5) ? . . Ag(2) N(7) 3.030(1) ? . . Ag(2) C(1) 3.473(5) ? . . Ag(2) C(3) 3.091(4) ? . . Ag(2) C(4) 2.974(5) ? . . Ag(2) C(17) 3.012(3) ? . . Ag(2) C(44) 3.507(3) ? . . Ag(2) C(44) 3.507(3) ? . 55504 Ag(2) C(45) 3.112(4) ? . . Ag(2) C(46) 2.988(1) ? . . Ag(2) C(47) 2.971(4) ? . . Ag(2) C(52) 3.587(4) ? . . Cl(1) Cl(2) 2.72(1) ? . . Cl(1) C(44) 3.385(6) ? . . Cl(1) C(44) 3.385(6) ? . 55504 Cl(1) C(45) 3.579(6) ? . . Cl(1) C(45) 3.579(6) ? . 55504 Cl(2) C(29) 3.53(1) ? . . N(1) C(1) 2.427(6) ? . . N(1) C(4) 2.892(6) ? . . N(1) C(6) 2.470(6) ? . . N(1) C(10) 2.453(5) ? . . N(1) C(11) 2.897(6) ? . . N(1) C(14) 2.914(5) ? . . N(2) C(1) 2.443(6) ? . . N(2) C(4) 2.941(5) ? . . N(2) C(18) 2.457(5) ? . . N(2) C(22) 2.428(5) ? . . N(2) C(23) 2.945(5) ? . . N(2) C(26) 2.833(6) ? . . N(3) C(1) 2.565(5) ? . . N(3) C(2) 3.478(6) ? . . N(3) C(3) 3.521(5) ? . . N(3) C(58) 3.495(8) ? . . N(3) C(59) 3.390(9) ? . . N(4) C(29) 2.411(3) ? . . N(4) C(31) 2.930(4) ? . . N(4) C(33) 2.467(5) ? . . N(4) C(37) 2.395(7) ? . . N(4) C(38) 2.976(7) ? . . N(4) C(41) 2.851(9) ? . . N(5) Ag(1) 3.085(1) ? . 55504 N(5) C(29) 2.574(6) ? . . N(5) C(30) 3.508(5) ? . . N(5) C(30) 3.508(5) ? . 55504 N(6) C(44) 2.409(3) ? . . N(6) C(44) 2.409(3) ? . 55504 N(6) C(46) 2.871(4) ? . . N(6) C(48) 2.486(6) ? . . N(6) C(52) 2.437(4) ? . . N(6) C(53) 2.930(8) ? . . N(6) C(56) 2.871(5) ? . . N(7) Ag(2) 3.030(1) ? . 55504 N(7) C(44) 2.585(7) ? . . N(7) C(44) 2.585(7) ? . 55504 N(7) C(45) 3.505(6) ? . . N(7) C(45) 3.505(6) ? . 55504 C(2) C(3) 2.444(7) ? . . C(2) C(4) 2.462(6) ? . . C(2) C(5) 2.350(7) ? . . C(2) C(6) 3.233(8) ? . . C(2) C(10) 3.194(6) ? . . C(2) C(11) 3.467(8) ? . . C(2) C(14) 3.456(5) ? . . C(3) C(4) 2.479(5) ? . . C(3) C(17) 2.335(7) ? . . C(3) C(18) 3.039(6) ? . . C(3) C(22) 3.384(6) ? . . C(3) C(23) 3.126(6) ? . . C(5) C(7) 2.355(7) ? . . C(5) C(8) 2.765(7) ? . . C(5) C(9) 2.385(6) ? . . C(5) C(11) 2.534(5) ? . . C(5) C(13) 3.46(1) ? . . C(5) C(14) 2.591(5) ? . . C(5) C(16) 3.487(9) ? . . C(6) C(8) 2.400(6) ? . . C(6) C(9) 2.791(6) ? . . C(6) C(10) 2.457(5) ? . . C(6) C(12) 2.49(2) ? . . C(6) C(13) 2.42(1) ? . . C(7) C(9) 2.386(6) ? . . C(7) C(10) 2.770(7) ? . . C(7) C(11) 2.503(8) ? . . C(7) C(12) 2.99(1) ? . . C(7) C(13) 3.04(2) ? . . C(7) C(51) 3.542(6) ? . 65501 C(8) C(10) 2.438(7) ? . . C(9) C(14) 2.559(8) ? . . C(9) C(15) 2.980(7) ? . . C(9) C(16) 3.22(1) ? . . C(10) C(15) 2.511(6) ? . . C(10) C(16) 2.51(1) ? . . C(12) C(13) 2.39(3) ? . . C(15) C(16) 2.507(9) ? . . C(16) C(21) 3.600(8) ? . 65603 C(17) C(19) 2.438(7) ? . . C(17) C(20) 2.789(7) ? . . C(17) C(21) 2.396(6) ? . . C(17) C(23) 2.565(5) ? . . C(17) C(25) 3.568(8) ? . . C(17) C(26) 2.500(6) ? . . C(17) C(27) 3.42(1) ? . . C(17) C(28) 3.59(1) ? . . C(18) C(20) 2.430(7) ? . . C(18) C(21) 2.779(6) ? . . C(18) C(22) 2.472(6) ? . . C(18) C(24) 2.538(9) ? . . C(18) C(25) 2.465(7) ? . . C(19) C(17) 2.438(7) ? . . C(19) C(21) 2.378(7) ? . . C(19) C(22) 2.841(7) ? . . C(19) C(23) 2.502(7) ? . . C(19) C(24) 3.15(1) ? . . C(19) C(25) 3.032(6) ? . . C(20) C(22) 2.451(7) ? . . C(21) C(16) 3.600(8) ? . 65603 C(21) C(19) 2.378(7) ? . . C(21) C(26) 2.538(9) ? . . C(21) C(27) 3.27(2) ? . . C(21) C(28) 2.97(1) ? . . C(22) C(19) 2.841(7) ? . . C(22) C(27) 2.45(1) ? . . C(22) C(28) 2.42(1) ? . . C(23) C(19) 2.502(7) ? . . C(24) C(19) 3.15(1) ? . . C(24) C(25) 2.58(1) ? . . C(25) C(19) 3.032(6) ? . . C(27) C(28) 2.36(3) ? . . C(29) Ag(1) 3.494(2) ? . 55504 C(29) N(4) 2.411(3) ? . 55504 C(30) C(30) 2.435(4) ? . 55504 C(30) C(31) 2.489(5) ? . . C(30) C(32) 2.317(5) ? . . C(30) C(33) 3.207(5) ? . . C(30) C(37) 3.054(6) ? . . C(30) C(38) 3.581(8) ? . . C(30) C(41) 3.288(8) ? . . C(31) Ag(1) 3.0100(6) ? . 55504 C(31) N(4) 2.930(4) ? . 55504 C(31) C(30) 2.489(5) ? . 55504 C(32) C(34) 2.392(6) ? . . C(32) C(35) 2.710(6) ? . . C(32) C(36) 2.362(8) ? . . C(32) C(38) 2.60(1) ? . . C(32) C(40) 3.52(1) ? . . C(32) C(41) 2.514(9) ? . . C(32) C(42) 3.47(2) ? . . C(33) C(35) 2.391(9) ? . . C(33) C(36) 2.81(1) ? . . C(33) C(37) 2.464(9) ? . . C(33) C(39) 2.49(1) ? . . C(33) C(40) 2.46(1) ? . . C(34) C(36) 2.40(1) ? . . C(34) C(37) 2.820(9) ? . . C(34) C(38) 2.50(1) ? . . C(34) C(39) 2.98(1) ? . . C(34) C(40) 3.13(1) ? . . C(35) C(37) 2.437(6) ? . . C(35) C(51) 3.570(6) ? . 55503 C(36) C(41) 2.533(7) ? . . C(36) C(42) 3.23(1) ? . . C(36) C(43) 3.105(9) ? . . C(37) C(42) 2.50(1) ? . . C(37) C(43) 2.60(1) ? . . C(39) C(40) 2.43(1) ? . . C(42) C(43) 2.45(1) ? . . C(44) Ag(2) 3.507(3) ? . . C(44) Ag(2) 3.507(3) ? . 55504 C(44) Cl(1) 3.385(6) ? . . C(44) Cl(1) 3.385(6) ? . 55504 C(44) N(6) 2.409(3) ? . . C(44) N(6) 2.409(3) ? . 55504 C(44) N(7) 2.585(7) ? . . C(44) N(7) 2.585(7) ? . 55504 C(45) C(45) 2.471(4) ? . 55504 C(45) C(46) 2.444(6) ? . . C(45) C(47) 2.350(4) ? . . C(45) C(48) 3.182(6) ? . . C(45) C(52) 3.296(5) ? . . C(45) C(53) 3.364(7) ? . . C(45) C(56) 3.585(6) ? . . C(46) Ag(2) 2.988(1) ? . 55504 C(46) N(6) 2.871(4) ? . 55504 C(46) C(45) 2.444(6) ? . 55504 C(47) C(49) 2.416(7) ? . . C(47) C(50) 2.765(6) ? . . C(47) C(51) 2.387(5) ? . . C(47) C(53) 2.563(7) ? . . C(47) C(54) 3.455(7) ? . . C(47) C(56) 2.515(7) ? . . C(47) C(58) 3.51(1) ? . . C(48) C(50) 2.403(6) ? . . C(48) C(51) 2.774(7) ? . . C(48) C(52) 2.457(8) ? . . C(48) C(54) 2.501(7) ? . . C(48) C(55) 2.55(1) ? . . C(49) C(51) 2.369(9) ? . . C(49) C(52) 2.800(9) ? . . C(49) C(53) 2.543(6) ? . . C(49) C(54) 3.194(8) ? . . C(49) C(55) 3.02(1) ? . . C(50) C(52) 2.413(8) ? . . C(51) C(7) 3.542(6) ? . 45501 C(51) C(35) 3.570(6) ? . 55503 C(51) C(56) 2.492(8) ? . . C(51) C(57) 3.126(8) ? . . C(51) C(58) 3.07(1) ? . . C(52) C(57) 2.577(7) ? . . C(52) C(58) 2.46(1) ? . . C(54) C(55) 2.41(1) ? . . C(57) C(58) 2.526(9) ? . . C(59) N(3) 3.390(9) ? . 55504 Ag(1) H(6) 3.2918 ? . . Ag(1) H(13) 3.0114 ? . . Ag(1) H(41) 3.3273 ? . . Ag(1) H(48) 3.0938 ? . . Ag(2) H(23) 3.5589 ? . . Ag(2) H(30) 2.9662 ? . . Ag(2) H(34) 3.5688 ? . . Ag(2) H(62) 3.4431 ? . . Ag(2) H(66) 3.1060 ? . . Ag(2) H(70) 3.1562 ? . . Cl(1) H(66) 3.1174 ? . . Cl(1) H(66) 3.1174 ? . 55504 Cl(1) H(68) 3.1034 ? . . Cl(1) H(68) 3.1034 ? . 55504 Cl(1) H(73) 2.29(6) ? . . Cl(1) H(73) 2.29(6) ? . 55504 Cl(2) H(45) 3.0305 ? . . Cl(2) H(45) 3.0305 ? . 55504 Cl(2) H(73) 2.18(4) ? . . Cl(2) H(73) 2.18(4) ? . 55504 N(1) H(1) 1.9440 ? . . N(1) H(6) 2.4460 ? . . N(1) H(13) 2.4578 ? . . N(1) H(19) 3.5243 ? . . N(2) H(2) 1.9317 ? . . N(2) H(23) 2.4305 ? . . N(2) H(30) 2.3351 ? . . N(2) H(33) 3.5551 ? . . N(3) H(66) 3.1634 ? . . N(3) H(70) 2.8054 ? . . N(3) H(71) 3.5903 ? . . N(3) H(73) 2.42(4) ? . 55504 N(4) H(37) 1.9047 ? . . N(4) H(41) 2.5252 ? . . N(4) H(48) 2.3619 ? . . N(4) H(51) 3.5068 ? . . N(5) H(73) 3.48(6) ? . . N(5) H(73) 3.48(6) ? . 55504 N(6) H(55) 1.9194 ? . . N(6) H(59) 2.4856 ? . . N(6) H(62) 3.5281 ? . . N(6) H(66) 2.3663 ? . . N(7) H(30) 3.3920 ? . . N(7) H(30) 3.3920 ? . 55504 N(7) H(34) 3.5208 ? . . N(7) H(34) 3.5208 ? . 55504 C(1) H(1) 2.0382 ? . . C(1) H(2) 2.0363 ? . . C(1) H(23) 3.2196 ? . . C(1) H(70) 3.5053 ? . . C(2) H(2) 2.5711 ? . . C(2) H(6) 3.0004 ? . . C(2) H(10) 3.4383 ? . . C(2) H(13) 3.0164 ? . . C(2) H(19) 3.3122 ? . . C(3) H(1) 2.5805 ? . . C(3) H(23) 2.4560 ? . . C(3) H(24) 3.2865 ? . . C(3) H(26) 3.3454 ? . 65603 C(3) H(30) 3.1866 ? . . C(4) H(1) 3.3062 ? . . C(4) H(2) 3.3143 ? . . C(4) H(70) 2.8716 ? . . C(4) H(73) 3.54(4) ? . 55504 C(5) H(1) 2.4294 ? . . C(5) H(3) 3.2165 ? . . C(5) H(5) 3.2464 ? . . C(5) H(6) 2.5837 ? . . C(5) H(10) 3.5292 ? . . C(5) H(12) 3.5434 ? . . C(5) H(13) 2.6167 ? . . C(5) H(19) 3.2634 ? . . C(5) H(21) 3.1584 ? . 65603 C(5) H(52) 3.3207 ? . . C(6) H(1) 3.1730 ? . . C(6) H(3) 1.9903 ? . . C(6) H(4) 3.2577 ? . . C(6) H(6) 2.0411 ? . . C(6) H(7) 2.8465 ? . . C(6) H(8) 3.2615 ? . . C(6) H(9) 2.5675 ? . . C(6) H(10) 2.8095 ? . . C(6) H(11) 3.2042 ? . . C(6) H(12) 2.4030 ? . . C(6) H(21) 3.2866 ? . 65603 C(6) H(52) 3.1485 ? . . C(7) H(4) 2.0365 ? . . C(7) H(5) 3.2452 ? . . C(7) H(6) 3.2617 ? . . C(7) H(7) 3.0297 ? . . C(7) H(9) 2.8548 ? . . C(7) H(12) 2.6151 ? . . C(7) H(21) 3.1392 ? . 65603 C(7) H(52) 3.0207 ? . . C(7) H(57) 3.4849 ? . 65501 C(7) H(58) 3.3047 ? . 65501 C(8) H(3) 1.9876 ? . . C(8) H(5) 2.0649 ? . . C(8) H(5) 3.1717 ? . 65503 C(8) H(16) 3.1902 ? . 65503 C(8) H(21) 2.9727 ? . 65603 C(8) H(52) 3.0490 ? . . C(8) H(54) 3.1928 ? . 65503 C(8) H(58) 3.5211 ? . 65501 C(9) H(3) 3.2358 ? . . C(9) H(4) 2.0646 ? . . C(9) H(4) 3.3081 ? . 65503 C(9) H(5) 3.5262 ? . 65503 C(9) H(13) 3.2888 ? . . C(9) H(14) 3.5180 ? . . C(9) H(16) 2.5022 ? . . C(9) H(17) 3.2557 ? . . C(9) H(19) 3.2269 ? . . C(9) H(21) 2.9260 ? . 65603 C(9) H(52) 3.1631 ? . . C(9) H(54) 3.1252 ? . 65503 C(10) H(1) 3.1391 ? . . C(10) H(4) 3.2877 ? . . C(10) H(5) 2.0221 ? . . C(10) H(13) 2.0595 ? . . C(10) H(14) 2.9315 ? . . C(10) H(15) 3.2691 ? . . C(10) H(16) 2.5016 ? . . C(10) H(17) 2.9269 ? . . C(10) H(18) 3.2574 ? . . C(10) H(19) 2.5264 ? . . C(10) H(21) 3.0305 ? . 65603 C(10) H(52) 3.3211 ? . . C(11) H(1) 3.5394 ? . . C(11) H(3) 2.6435 ? . . C(11) H(7) 1.9605 ? . . C(11) H(8) 2.1001 ? . . C(11) H(9) 2.1649 ? . . C(11) H(10) 1.9148 ? . . C(11) H(11) 1.9635 ? . . C(11) H(12) 1.9341 ? . . C(12) H(3) 2.7698 ? . . C(12) H(6) 2.0359 ? . . C(12) H(8) 3.1889 ? . 55504 C(12) H(10) 3.1681 ? . . C(12) H(11) 2.3816 ? . . C(12) H(12) 2.7974 ? . . C(12) H(69) 3.4882 ? . 65501 C(13) H(3) 2.9446 ? . . C(13) H(6) 1.9713 ? . . C(13) H(7) 2.2310 ? . . C(13) H(8) 2.8326 ? . . C(13) H(9) 3.1808 ? . . C(14) H(1) 3.5564 ? . . C(14) H(5) 2.6902 ? . . C(14) H(14) 2.0331 ? . . C(14) H(15) 2.0027 ? . . C(14) H(16) 2.0217 ? . . C(14) H(17) 2.0531 ? . . C(14) H(18) 2.0020 ? . . C(14) H(19) 2.0649 ? . . C(15) H(4) 3.2698 ? . 65503 C(15) H(5) 2.7525 ? . . C(15) H(13) 1.9871 ? . . C(15) H(17) 2.5549 ? . . C(15) H(18) 2.8505 ? . . C(15) H(19) 3.2947 ? . . C(15) H(44) 3.4551 ? . . C(15) H(67) 3.2175 ? . 55503 C(16) H(1) 3.5715 ? . . C(16) H(5) 3.1604 ? . . C(16) H(13) 2.0445 ? . . C(16) H(14) 3.2670 ? . . C(16) H(15) 2.4839 ? . . C(16) H(16) 2.9340 ? . . C(16) H(22) 3.2360 ? . 65603 C(16) H(42) 3.2889 ? . 55503 C(17) H(2) 2.4267 ? . . C(17) H(20) 3.2921 ? . . C(17) H(22) 3.2462 ? . . C(17) H(23) 2.5420 ? . . C(17) H(29) 3.3483 ? . . C(17) H(30) 2.5132 ? . . C(17) H(33) 3.2085 ? . . C(17) H(62) 3.2763 ? . . C(18) H(2) 2.9323 ? . . C(18) H(20) 2.0556 ? . . C(18) H(21) 3.2834 ? . . C(18) H(23) 1.9730 ? . . C(18) H(24) 2.9509 ? . . C(18) H(25) 3.2908 ? . . C(18) H(26) 2.5556 ? . . C(18) H(27) 2.8841 ? . . C(18) H(28) 3.2353 ? . . C(18) H(29) 2.4331 ? . . C(18) H(62) 3.3153 ? . . C(19) H(1) 3.1517 ? . 65603 C(19) H(21) 2.0270 ? . . C(19) H(22) 3.2349 ? . . C(19) H(23) 3.2477 ? . . C(19) H(26) 2.7576 ? . . C(19) H(27) 3.0432 ? . . C(19) H(29) 2.9201 ? . . C(19) H(57) 3.5799 ? . 55603 C(19) H(62) 3.4469 ? . . C(20) H(1) 3.2233 ? . 65603 C(20) H(19) 2.9354 ? . 65603 C(20) H(20) 2.0448 ? . . C(20) H(22) 2.0062 ? . . C(20) H(57) 3.3944 ? . 55603 C(20) H(62) 3.4710 ? . . C(21) H(17) 3.5278 ? . 65603 C(21) H(19) 2.8345 ? . 65603 C(21) H(20) 3.2391 ? . . C(21) H(21) 2.0166 ? . . C(21) H(30) 3.2884 ? . . C(21) H(31) 3.2231 ? . . C(21) H(33) 3.1793 ? . . C(21) H(34) 3.5042 ? . . C(21) H(36) 2.5294 ? . . C(21) H(61) 3.5121 ? . . C(21) H(62) 3.4362 ? . . C(22) H(2) 3.4137 ? . . C(22) H(21) 3.3039 ? . . C(22) H(22) 2.0352 ? . . C(22) H(30) 1.9823 ? . . C(22) H(31) 2.7885 ? . . C(22) H(32) 3.2614 ? . . C(22) H(33) 2.4332 ? . . C(22) H(34) 2.8206 ? . . C(22) H(35) 3.1856 ? . . C(22) H(36) 2.4637 ? . . C(22) H(61) 3.5957 ? . . C(22) H(62) 3.3565 ? . . C(23) H(2) 3.0741 ? . . C(23) H(20) 2.6342 ? . . C(23) H(24) 2.0885 ? . . C(23) H(25) 2.0655 ? . . C(23) H(26) 2.0611 ? . . C(23) H(27) 2.0379 ? . . C(23) H(28) 2.0445 ? . . C(23) H(29) 2.0067 ? . . C(24) H(2) 3.3127 ? . . C(24) H(2) 3.2709 ? . 65603 C(24) H(20) 2.9939 ? . . C(24) H(23) 2.0210 ? . . C(24) H(27) 2.6597 ? . . C(24) H(28) 2.9485 ? . . C(24) H(29) 3.3445 ? . . C(24) H(33) 3.2001 ? . 65603 C(25) H(20) 2.9148 ? . . C(25) H(23) 1.9948 ? . . C(25) H(24) 3.3184 ? . . C(25) H(25) 2.5863 ? . . C(25) H(26) 3.0297 ? . . C(25) H(38) 3.4316 ? . 55503 C(25) H(39) 3.2335 ? . 55503 C(25) H(56) 3.2791 ? . 55603 C(25) H(65) 3.1761 ? . 55603 C(25) H(72) 3.5023 ? . . C(26) H(22) 2.6788 ? . . C(26) H(31) 1.8687 ? . . C(26) H(32) 2.0692 ? . . C(26) H(33) 1.9592 ? . . C(26) H(34) 1.9608 ? . . C(26) H(35) 1.9820 ? . . C(26) H(36) 2.0041 ? . . C(27) H(22) 3.2032 ? . . C(27) H(30) 1.8460 ? . . C(27) H(34) 3.0778 ? . . C(27) H(35) 2.3314 ? . . C(27) H(36) 2.8694 ? . . C(28) H(22) 2.7711 ? . . C(28) H(30) 2.0055 ? . . C(28) H(31) 2.2519 ? . . C(28) H(32) 2.8327 ? . . C(28) H(33) 3.1245 ? . . C(28) H(49) 3.1080 ? . 55601 C(28) H(61) 3.3261 ? . . C(29) H(37) 2.0219 ? . . C(29) H(37) 2.0219 ? . 55504 C(29) H(48) 3.5385 ? . . C(29) H(48) 3.5385 ? . 55504 C(30) H(37) 2.5465 ? . 55504 C(30) H(41) 3.1255 ? . . C(30) H(45) 3.4910 ? . . C(30) H(48) 2.7994 ? . . C(30) H(51) 3.2286 ? . . C(31) H(37) 3.3222 ? . . C(31) H(37) 3.3222 ? . 55504 C(31) H(73) 3.35(6) ? . . C(31) H(73) 3.35(6) ? . 55504 C(32) H(14) 3.1177 ? . . C(32) H(37) 2.3864 ? . . C(32) H(38) 3.2651 ? . . C(32) H(40) 3.2296 ? . . C(32) H(41) 2.6402 ? . . C(32) H(44) 3.5848 ? . . C(32) H(47) 3.5597 ? . . C(32) H(48) 2.5297 ? . . C(32) H(51) 3.2196 ? . . C(33) H(14) 3.0672 ? . . C(33) H(37) 3.1031 ? . . C(33) H(38) 2.0517 ? . . C(33) H(39) 3.2494 ? . . C(33) H(41) 2.0116 ? . . C(33) H(42) 2.9048 ? . . C(33) H(43) 3.2433 ? . . C(33) H(44) 2.5137 ? . . C(33) H(45) 2.8917 ? . . C(33) H(46) 3.2266 ? . . C(33) H(47) 2.4319 ? . . C(34) H(14) 3.1297 ? . . C(34) H(28) 3.1628 ? . 55503 C(34) H(39) 2.0006 ? . . C(34) H(40) 3.2462 ? . . C(34) H(41) 3.2612 ? . . C(34) H(42) 3.0306 ? . . C(34) H(44) 2.8448 ? . . C(34) H(47) 2.7045 ? . . C(34) H(72) 3.3468 ? . 55503 C(35) H(14) 3.2027 ? . . C(35) H(28) 3.1676 ? . 55503 C(35) H(38) 1.9917 ? . . C(35) H(40) 2.0357 ? . . C(35) H(57) 3.5108 ? . 55503 C(35) H(58) 3.0120 ? . 55503 C(35) H(60) 3.3504 ? . 55401 C(35) H(64) 3.2050 ? . 55401 C(35) H(72) 3.4231 ? . 55503 C(36) H(4) 3.5297 ? . 65503 C(36) H(14) 3.2303 ? . . C(36) H(38) 3.2470 ? . . C(36) H(39) 2.0144 ? . . C(36) H(48) 3.2696 ? . . C(36) H(49) 3.2518 ? . . C(36) H(51) 3.1447 ? . . C(36) H(54) 2.6771 ? . . C(36) H(58) 3.5674 ? . 55503 C(36) H(60) 3.2731 ? . 55401 C(36) H(61) 3.5347 ? . 55401 C(36) H(64) 3.3585 ? . 55401 C(37) H(14) 3.2346 ? . . C(37) H(37) 3.0207 ? . . C(37) H(39) 3.2827 ? . . C(37) H(40) 2.0868 ? . . C(37) H(48) 1.9814 ? . . C(37) H(49) 2.9111 ? . . C(37) H(50) 3.2704 ? . . C(37) H(51) 2.4538 ? . . C(37) H(52) 3.0160 ? . . C(37) H(53) 3.3348 ? . . C(37) H(54) 2.6430 ? . . C(38) H(37) 3.5869 ? . . C(38) H(38) 2.6518 ? . . C(38) H(42) 2.0039 ? . . C(38) H(43) 2.0120 ? . . C(38) H(44) 2.0300 ? . . C(38) H(45) 2.0301 ? . . C(38) H(46) 1.9991 ? . . C(38) H(47) 1.9682 ? . . C(39) H(15) 3.2973 ? . 55503 C(39) H(18) 3.4666 ? . 55503 C(39) H(38) 2.7754 ? . . C(39) H(41) 2.0011 ? . . C(39) H(44) 3.2462 ? . 55503 C(39) H(45) 3.2006 ? . . C(39) H(46) 2.4003 ? . . C(39) H(47) 2.8462 ? . . C(39) H(71) 2.8893 ? . . C(40) H(38) 3.0701 ? . . C(40) H(41) 1.9531 ? . . C(40) H(42) 2.4352 ? . . C(40) H(43) 2.8034 ? . . C(40) H(44) 3.2161 ? . . C(41) H(37) 3.4287 ? . . C(41) H(40) 2.7051 ? . . C(41) H(49) 2.0047 ? . . C(41) H(50) 2.0712 ? . . C(41) H(51) 1.9973 ? . . C(41) H(52) 2.1083 ? . . C(41) H(53) 2.0497 ? . . C(41) H(54) 2.0461 ? . . C(42) H(36) 3.2589 ? . 55401 C(42) H(37) 3.5033 ? . . C(42) H(40) 3.2050 ? . . C(42) H(48) 1.9894 ? . . C(42) H(50) 3.3006 ? . 55504 C(42) H(52) 3.2372 ? . . C(42) H(53) 2.3927 ? . . C(42) H(54) 2.8477 ? . . C(43) H(4) 3.4681 ? . 65503 C(43) H(5) 3.0821 ? . 65503 C(43) H(9) 3.4604 ? . . C(43) H(40) 2.8922 ? . . C(43) H(48) 2.0368 ? . . C(43) H(49) 2.4260 ? . . C(43) H(50) 2.8486 ? . . C(43) H(51) 3.2278 ? . . C(44) H(55) 2.0331 ? . . C(44) H(55) 2.0331 ? . 55504 C(44) H(59) 3.5427 ? . . C(44) H(59) 3.5427 ? . 55504 C(45) H(55) 2.6113 ? . 55504 C(45) H(59) 2.6897 ? . . C(45) H(66) 2.9658 ? . . C(46) H(55) 3.2833 ? . . C(46) H(55) 3.2833 ? . 55504 C(47) H(55) 2.4557 ? . . C(47) H(56) 3.2753 ? . . C(47) H(58) 3.2451 ? . . C(47) H(59) 2.5985 ? . . C(47) H(62) 3.2122 ? . . C(47) H(66) 2.5198 ? . . C(47) H(69) 3.5526 ? . . C(47) H(70) 3.5924 ? . . C(48) H(12) 3.3676 ? . 45501 C(48) H(55) 3.1115 ? . . C(48) H(56) 2.0302 ? . . C(48) H(57) 3.2539 ? . . C(48) H(59) 2.0381 ? . . C(48) H(60) 2.8999 ? . . C(48) H(61) 3.2652 ? . . C(48) H(62) 2.5176 ? . . C(48) H(63) 2.9493 ? . . C(48) H(64) 3.3070 ? . . C(48) H(65) 2.5885 ? . . C(49) H(12) 3.0017 ? . 45501 C(49) H(29) 3.5199 ? . . C(49) H(57) 2.0149 ? . . C(49) H(58) 3.2202 ? . . C(49) H(59) 3.2885 ? . . C(49) H(60) 3.2024 ? . . C(49) H(62) 3.1772 ? . . C(49) H(63) 3.5261 ? . . C(49) H(65) 2.5903 ? . . C(50) H(3) 3.2031 ? . 45501 C(50) H(12) 2.8849 ? . 45501 C(50) H(39) 2.9930 ? . 55503 C(50) H(56) 2.0262 ? . . C(50) H(58) 1.9982 ? . . C(50) H(60) 3.4463 ? . 55603 C(51) H(3) 2.8263 ? . 45501 C(51) H(12) 3.2484 ? . 45501 C(51) H(39) 2.8516 ? . 55503 C(51) H(56) 3.2256 ? . . C(51) H(57) 2.0109 ? . . C(51) H(66) 3.2450 ? . . C(51) H(67) 3.1670 ? . . C(51) H(69) 3.0025 ? . . C(51) H(72) 2.6655 ? . . C(52) H(3) 3.5306 ? . 45501 C(52) H(55) 3.3189 ? . . C(52) H(57) 3.2687 ? . . C(52) H(58) 2.0335 ? . . C(52) H(66) 1.9766 ? . . C(52) H(67) 2.9842 ? . . C(52) H(68) 3.3375 ? . . C(52) H(69) 2.5753 ? . . C(52) H(70) 2.8563 ? . . C(52) H(71) 3.2257 ? . . C(52) H(72) 2.4737 ? . . C(53) H(55) 3.4005 ? . . C(53) H(56) 2.6859 ? . . C(53) H(60) 2.0257 ? . . C(53) H(61) 2.0183 ? . . C(53) H(62) 2.0329 ? . . C(53) H(63) 2.0650 ? . . C(53) H(64) 2.0404 ? . . C(53) H(65) 2.0604 ? . . C(54) H(40) 3.3492 ? . 55601 C(54) H(56) 3.1528 ? . . C(54) H(57) 3.5493 ? . 55603 C(54) H(59) 2.0264 ? . . C(54) H(63) 3.1982 ? . . C(54) H(64) 2.3685 ? . . C(54) H(65) 2.8048 ? . . C(55) H(27) 3.2028 ? . 55603 C(55) H(56) 2.7496 ? . . C(55) H(59) 2.0505 ? . . C(55) H(60) 2.3885 ? . . C(55) H(61) 2.7693 ? . . C(55) H(62) 3.2129 ? . . C(56) H(58) 2.6359 ? . . C(56) H(67) 2.0684 ? . . C(56) H(68) 2.0955 ? . . C(56) H(69) 2.0168 ? . . C(56) H(70) 2.0931 ? . . C(56) H(71) 2.0789 ? . . C(56) H(72) 2.0906 ? . . C(57) H(3) 3.4627 ? . 45501 C(57) H(15) 3.4636 ? . 55503 C(57) H(43) 3.4022 ? . . C(57) H(58) 2.9215 ? . . C(57) H(66) 2.0314 ? . . C(57) H(70) 3.2733 ? . . C(57) H(71) 2.4774 ? . . C(57) H(72) 2.9790 ? . . C(58) H(28) 3.4044 ? . . C(58) H(43) 2.9322 ? . . C(58) H(58) 2.9696 ? . . C(58) H(66) 2.0719 ? . . C(58) H(67) 2.5375 ? . . C(58) H(68) 2.9414 ? . . C(58) H(69) 3.2799 ? . . H(1) C(19) 3.1517 ? . 65603 H(1) C(20) 3.2233 ? . 65603 H(2) C(24) 3.2709 ? . 65603 H(3) C(50) 3.2031 ? . 65501 H(3) C(51) 2.8263 ? . 65501 H(3) C(52) 3.5306 ? . 65501 H(3) C(57) 3.4627 ? . 65501 H(4) C(9) 3.3081 ? . 65503 H(4) C(15) 3.2698 ? . 65503 H(4) C(36) 3.5297 ? . 65503 H(4) C(43) 3.4681 ? . 65503 H(5) C(8) 3.1717 ? . 65503 H(5) C(9) 3.5262 ? . 65503 H(5) C(43) 3.0821 ? . 65503 H(8) C(12) 3.1889 ? . 55504 H(12) C(48) 3.3676 ? . 65501 H(12) C(49) 3.0017 ? . 65501 H(12) C(50) 2.8849 ? . 65501 H(12) C(51) 3.2484 ? . 65501 H(15) C(39) 3.2973 ? . 55503 H(15) C(57) 3.4636 ? . 55503 H(16) C(8) 3.1902 ? . 65503 H(17) C(21) 3.5278 ? . 65603 H(18) C(39) 3.4666 ? . 55503 H(19) C(20) 2.9354 ? . 65603 H(19) C(21) 2.8345 ? . 65603 H(21) C(5) 3.1584 ? . 65603 H(21) C(6) 3.2866 ? . 65603 H(21) C(7) 3.1392 ? . 65603 H(21) C(8) 2.9727 ? . 65603 H(21) C(9) 2.9260 ? . 65603 H(21) C(10) 3.0305 ? . 65603 H(21) C(19) 2.0270 ? . . H(22) C(16) 3.2360 ? . 65603 H(22) C(19) 3.2349 ? . . H(23) C(19) 3.2477 ? . . H(26) C(3) 3.3454 ? . 65603 H(26) C(19) 2.7576 ? . . H(27) C(19) 3.0432 ? . . H(27) C(55) 3.2028 ? . 55603 H(28) C(34) 3.1628 ? . 55503 H(28) C(35) 3.1676 ? . 55503 H(29) C(19) 2.9201 ? . . H(33) C(24) 3.2001 ? . 65603 H(36) C(42) 3.2589 ? . 55601 H(37) C(30) 2.5465 ? . 55504 H(38) C(25) 3.4316 ? . 55503 H(39) C(25) 3.2335 ? . 55503 H(39) C(50) 2.9930 ? . 55503 H(39) C(51) 2.8516 ? . 55503 H(40) C(54) 3.3492 ? . 55401 H(42) C(16) 3.2889 ? . 55503 H(44) C(39) 3.2462 ? . 55503 H(49) C(28) 3.1080 ? . 55401 H(50) C(42) 3.3006 ? . 55504 H(54) C(8) 3.1928 ? . 65503 H(54) C(9) 3.1252 ? . 65503 H(55) C(44) 2.0331 ? . . H(55) C(44) 2.0331 ? . 55504 H(55) C(45) 2.6113 ? . 55504 H(56) C(25) 3.2791 ? . 55603 H(57) C(7) 3.4849 ? . 45501 H(57) C(19) 3.5799 ? . 55603 H(57) C(20) 3.3944 ? . 55603 H(57) C(35) 3.5108 ? . 55503 H(57) C(54) 3.5493 ? . 55603 H(58) C(7) 3.3047 ? . 45501 H(58) C(8) 3.5211 ? . 45501 H(58) C(35) 3.0120 ? . 55503 H(58) C(36) 3.5674 ? . 55503 H(59) C(44) 3.5427 ? . . H(59) C(44) 3.5427 ? . 55504 H(60) C(35) 3.3504 ? . 55601 H(60) C(36) 3.2731 ? . 55601 H(60) C(50) 3.4463 ? . 55603 H(61) C(36) 3.5347 ? . 55601 H(62) C(19) 3.4469 ? . . H(64) C(35) 3.2050 ? . 55601 H(64) C(36) 3.3585 ? . 55601 H(65) C(25) 3.1761 ? . 55603 H(67) C(15) 3.2175 ? . 55503 H(67) C(51) 3.1670 ? . . H(67) C(52) 2.9842 ? . . H(67) C(56) 2.0684 ? . . H(67) C(58) 2.5375 ? . . H(69) C(12) 3.4882 ? . 45501 H(72) C(34) 3.3468 ? . 55503 H(72) C(35) 3.4231 ? . 55503 H(73) N(3) 2.42(4) ? . 55504 H(73) C(4) 3.54(4) ? . 55504 loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 N(4) Ag(1) N(1) C(2) -151.6(2) ? . . . . N(4) Ag(1) N(1) C(5) 22.4(3) ? . . . . N(1) Ag(1) N(4) C(30) -143.5(3) ? . . . . N(1) Ag(1) N(4) C(32) 28.1(5) ? . . . . N(6) Ag(2) N(2) C(3) 126.4(3) ? . . . . N(6) Ag(2) N(2) C(17) -36.6(4) ? . . . . N(2) Ag(2) N(6) C(45) 152.7(3) ? . . . . N(2) Ag(2) N(6) C(47) -23.7(4) ? . . . . Ag(1) N(1) C(2) C(1) -4.3(5) ? . . . . C(5) N(1) C(2) C(1) -178.1(3) ? . . . . Ag(1) N(1) C(5) C(6) 92.5(3) ? . . . . Ag(1) N(1) C(5) C(10) -85.2(3) ? . . . . C(2) N(1) C(5) C(6) -92.5(4) ? . . . . C(2) N(1) C(5) C(10) 89.8(3) ? . . . . Ag(2) N(2) C(3) C(1) 7.1(5) ? . . . . C(17) N(2) C(3) C(1) 169.8(3) ? . . . . Ag(2) N(2) C(17) C(18) 96.3(4) ? . . . . Ag(2) N(2) C(17) C(22) -77.8(4) ? . . . . C(3) N(2) C(17) C(18) -68.4(5) ? . . . . C(3) N(2) C(17) C(22) 117.4(4) ? . . . . Ag(1) N(4) C(30) C(29) 0.0(8) ? . . . . C(32) N(4) C(30) C(29) -171.6(6) ? . . . . Ag(1) N(4) C(32) C(33) 92.5(4) ? . . . . Ag(1) N(4) C(32) C(37) -89.1(4) ? . . . . C(30) N(4) C(32) C(33) -94.8(5) ? . . . . C(30) N(4) C(32) C(37) 83.6(5) ? . . . . Ag(2) N(6) C(45) C(44) 2.8(7) ? . . . . C(47) N(6) C(45) C(44) 178.9(5) ? . . . . Ag(2) N(6) C(47) C(48) 95.3(4) ? . . . . Ag(2) N(6) C(47) C(52) -79.8(3) ? . . . . C(45) N(6) C(47) C(48) -81.5(4) ? . . . . C(45) N(6) C(47) C(52) 103.4(5) ? . . . . C(3) C(1) C(2) N(1) 175.0(3) ? . . . . C(4) C(1) C(2) N(1) 2.0(5) ? . . . . C(2) C(1) C(3) N(2) -175.9(3) ? . . . . C(4) C(1) C(3) N(2) -3.0(5) ? . . . . N(1) C(5) C(6) C(7) 177.0(3) ? . . . . N(1) C(5) C(6) C(11) -0.1(4) ? . . . . C(10) C(5) C(6) C(7) -5.4(5) ? . . . . C(10) C(5) C(6) C(11) 177.5(4) ? . . . . N(1) C(5) C(10) C(9) -179.0(3) ? . . . . N(1) C(5) C(10) C(14) 3.3(5) ? . . . . C(6) C(5) C(10) C(9) 3.4(5) ? . . . . C(6) C(5) C(10) C(14) -174.3(3) ? . . . . C(5) C(6) C(7) C(8) 3.3(7) ? . . . . C(11) C(6) C(7) C(8) -179.6(4) ? . . . . C(5) C(6) C(11) C(12) -127(1) ? . . . . C(5) C(6) C(11) C(13) 113(1) ? . . . . C(7) C(6) C(11) C(12) 55(1) ? . . . . C(7) C(6) C(11) C(13) -63(1) ? . . . . C(6) C(7) C(8) C(9) 0.6(7) ? . . . . C(7) C(8) C(9) C(10) -2.8(6) ? . . . . C(8) C(9) C(10) C(5) 0.8(6) ? . . . . C(8) C(9) C(10) C(14) 178.5(4) ? . . . . C(5) C(10) C(14) C(15) 130.8(4) ? . . . . C(5) C(10) C(14) C(16) -104.6(5) ? . . . . C(9) C(10) C(14) C(15) -46.8(5) ? . . . . C(9) C(10) C(14) C(16) 77.8(5) ? . . . . N(2) C(17) C(18) C(19) -176.0(4) ? . . . . N(2) C(17) C(18) C(23) 3.2(7) ? . . . . C(22) C(17) C(18) C(19) -2.1(7) ? . . . . C(22) C(17) C(18) C(23) 177.0(4) ? . . . . N(2) C(17) C(22) C(21) 174.8(5) ? . . . . N(2) C(17) C(22) C(26) -2.8(8) ? . . . . C(18) C(17) C(22) C(21) 0.8(7) ? . . . . C(18) C(17) C(22) C(26) -176.7(5) ? . . . . C(17) C(18) C(19) C(20) 3.7(7) ? . . . . C(23) C(18) C(19) C(20) -175.5(5) ? . . . . C(17) C(18) C(23) C(24) 112.6(5) ? . . . . C(17) C(18) C(23) C(25) -116.4(6) ? . . . . C(19) C(18) C(23) C(24) -68.3(7) ? . . . . C(19) C(18) C(23) C(25) 62.7(6) ? . . . . C(18) C(19) C(20) C(21) -4.2(8) ? . . . . C(19) C(20) C(21) C(22) 2(1) ? . . . . C(20) C(21) C(22) C(17) -1.2(9) ? . . . . C(20) C(21) C(22) C(26) 176.3(6) ? . . . . C(17) C(22) C(26) C(27) -103(1) ? . . . . C(17) C(22) C(26) C(28) 130.3(7) ? . . . . C(21) C(22) C(26) C(27) 79(1) ? . . . . C(21) C(22) C(26) C(28) -47.1(8) ? . . . . C(31) C(29) C(30) N(4) 5(1) ? . . . . N(4) C(32) C(33) C(34) 175.0(4) ? . . . . N(4) C(32) C(33) C(38) -5.2(6) ? . . . . C(37) C(32) C(33) C(34) -3.3(6) ? . . . . C(37) C(32) C(33) C(38) 176.6(4) ? . . . . N(4) C(32) C(37) C(36) -177.9(3) ? . . . . N(4) C(32) C(37) C(41) 4.4(6) ? . . . . C(33) C(32) C(37) C(36) 0.3(6) ? . . . . C(33) C(32) C(37) C(41) -177.4(4) ? . . . . C(32) C(33) C(34) C(35) 2.9(6) ? . . . . C(38) C(33) C(34) C(35) -176.9(4) ? . . . . C(32) C(33) C(38) C(39) -127.8(5) ? . . . . C(32) C(33) C(38) C(40) 107.4(6) ? . . . . C(34) C(33) C(38) C(39) 52.0(6) ? . . . . C(34) C(33) C(38) C(40) -72.8(6) ? . . . . C(33) C(34) C(35) C(36) 0.2(6) ? . . . . C(34) C(35) C(36) C(37) -3.3(6) ? . . . . C(35) C(36) C(37) C(32) 3.0(6) ? . . . . C(35) C(36) C(37) C(41) -179.2(4) ? . . . . C(32) C(37) C(41) C(42) -105.7(7) ? . . . . C(32) C(37) C(41) C(43) 129.5(6) ? . . . . C(36) C(37) C(41) C(42) 76.7(7) ? . . . . C(36) C(37) C(41) C(43) -48.1(7) ? . . . . C(46) C(44) C(45) N(6) -5.0(7) ? . . . . N(6) C(47) C(48) C(49) -177.0(4) ? . . . . N(6) C(47) C(48) C(53) -3.0(6) ? . . . . C(52) C(47) C(48) C(49) -2.0(6) ? . . . . C(52) C(47) C(48) C(53) 172.0(4) ? . . . . N(6) C(47) C(52) C(51) -179.7(4) ? . . . . N(6) C(47) C(52) C(56) -2.0(6) ? . . . . C(48) C(47) C(52) C(51) 5.1(6) ? . . . . C(48) C(47) C(52) C(56) -177.1(4) ? . . . . C(47) C(48) C(49) C(50) -3.7(7) ? . . . . C(53) C(48) C(49) C(50) -177.7(5) ? . . . . C(47) C(48) C(53) C(54) -100.9(6) ? . . . . C(47) C(48) C(53) C(55) 141.0(5) ? . . . . C(49) C(48) C(53) C(54) 72.9(8) ? . . . . C(49) C(48) C(53) C(55) -45.2(6) ? . . . . C(48) C(49) C(50) C(51) 6.1(8) ? . . . . C(49) C(50) C(51) C(52) -2.8(7) ? . . . . C(50) C(51) C(52) C(47) -2.8(6) ? . . . . C(50) C(51) C(52) C(56) 179.3(4) ? . . . . C(47) C(52) C(56) C(57) -123.4(5) ? . . . . C(47) C(52) C(56) C(58) 113.5(4) ? . . . . C(51) C(52) C(56) C(57) 54.3(6) ? . . . . C(51) C(52) C(56) C(58) -68.8(5) ? . . . .
1100783.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $ #$Revision: 176435 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100783.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100783 loop_ _publ_author_name 'Chizu Shimokawa' 'Shinobu Itoh' _publ_section_title ; The First \b-Diketiminate-Ag(I) Complexes. Macrocyclic Dinuclear and Tetranuclear Ag(I)-Complexes and Linear Coordination Polymer Ag(I)-Complex ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3010 _journal_page_last 3012 _journal_paper_doi 10.1021/ic0501014 _journal_volume 44 _journal_year 2005 _chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk' _chemical_formula_moiety 'C28 H38 Ag Cl2 N3 O2 ' _chemical_formula_sum 'C28 H38 Ag Cl2 N3 O2' _chemical_formula_weight 627.40 _space_group_IT_number 4 _symmetry_cell_setting monoclinic _symmetry_Int_Tables_number 4 _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 1' _cell_angle_alpha 90 _cell_angle_beta 105.025(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.432(2) _cell_length_b 16.167(2) _cell_length_c 15.208(3) _cell_measurement_reflns_used 11477 _cell_measurement_temperature 153.1 _cell_measurement_theta_max 27.5 _cell_measurement_theta_min 4.0 _cell_volume 2952.1(8) _computing_cell_refinement CrystalClear _computing_data_collection CrystalClear _computing_data_reduction CrystalStructure _computing_molecular_graphics ORTEP3 _computing_publication_material 'CrystalStructure 3.6.0' _computing_structure_refinement CRYSTALS _computing_structure_solution SIR92 _diffrn_detector_area_resol_mean 7.31 _diffrn_measured_fraction_theta_full 0.9839 _diffrn_measured_fraction_theta_max 0.9839 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents 0.046 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 29107 _diffrn_reflns_theta_full 27.48 _diffrn_reflns_theta_max 27.48 _exptl_absorpt_coefficient_mu 0.890 _exptl_absorpt_correction_T_max 0.915 _exptl_absorpt_correction_T_min 0.839 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Higashi, T. (1999). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.412 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 1296.00 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _refine_diff_density_max 3.27 _refine_diff_density_min -5.42 _refine_ls_abs_structure_details 'Flack, H. D. (1983), Acta Cryst. A39, 876-881.' _refine_ls_abs_structure_Flack 0.43(2) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_hydrogen_treatment refall _refine_ls_number_parameters 726 _refine_ls_number_reflns 22778 _refine_ls_R_factor_gt 0.0470 _refine_ls_shift/su_max 0.0000 _refine_ls_structure_factor_coef F _refine_ls_weighting_details 'w = 1/[0.0005Fo^2^ + 2.0000\s(Fo^2^)]' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.0500 _reflns_number_gt 22778 _reflns_number_total 29066 _reflns_threshold_expression F^2^>2.0\s(F^2^) _cod_data_source_file ic0501014si20050122_011347_4.cif _cod_data_source_block '__(Ag(L5)(CH2Cl2))n' _cod_original_cell_volume 2952.0(8) _cod_original_formula_sum 'C28 H38 Ag Cl2 N3 O2 ' _cod_database_code 1100783 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,-Z loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag(1) Ag 0.61403(3) 0.29864(5) 0.96522(3) 0.02224(12) Uani 1.00 1 d . . . Ag(2) Ag 0.62376(3) 0.21630(5) 0.46799(3) 0.02101(12) Uani 1.00 1 d . . . Cl(1) Cl 0.9676(2) 0.39891(11) 0.7275(1) 0.0679(6) Uani 1.00 1 d . . . Cl(2) Cl 1.0221(2) 0.57345(11) 0.7540(2) 0.0780(7) Uani 1.00 1 d . . . Cl(3) Cl 1.0118(5) 0.0137(2) 0.7376(2) 0.1416(12) Uani 1.00 1 d . . . Cl(4) Cl 0.8956(2) 0.15403(13) 0.7856(2) 0.0969(8) Uani 1.00 1 d . . . O(1) O 0.5882(3) 0.2036(2) 0.6046(3) 0.0256(11) Uani 1.00 1 d . . . O(2) O 0.7109(3) 0.3015(3) 0.6214(3) 0.0302(10) Uani 1.00 1 d . . . O(3) O 0.5683(3) 0.3097(3) 1.0979(3) 0.0276(11) Uani 1.00 1 d . . . O(4) O 0.6782(3) 0.2034(3) 1.1103(3) 0.0326(11) Uani 1.00 1 d . . . N(1) N 0.5509(3) 0.2073(3) 0.8522(3) 0.0145(12) Uani 1.00 1 d . . . N(2) N 0.7090(3) 0.3569(3) 0.8746(4) 0.0163(13) Uani 1.00 1 d . . . N(3) N 0.6477(3) 0.2570(3) 0.6559(3) 0.0159(11) Uani 1.00 1 d . . . N(4) N 0.5459(3) 0.3044(3) 0.3513(3) 0.0166(12) Uani 1.00 1 d . . . N(5) N 0.7016(3) 0.1560(2) 0.3677(3) 0.0143(13) Uani 1.00 1 d . . . N(6) N 0.6245(4) 0.2517(3) 1.1471(3) 0.0201(12) Uani 1.00 1 d . . . C(1) C 0.6413(4) 0.2669(3) 0.7440(4) 0.014(1) Uani 1.00 1 d . . . C(2) C 0.5720(4) 0.2058(3) 0.7758(4) 0.016(1) Uani 1.00 1 d . . . C(3) C 0.7078(4) 0.3311(3) 0.7927(4) 0.014(1) Uani 1.00 1 d . . . C(4) C 0.4900(4) 0.1374(3) 0.8727(4) 0.014(2) Uani 1.00 1 d . . . C(5) C 0.5453(4) 0.0633(3) 0.8989(4) 0.019(2) Uani 1.00 1 d . . . C(6) C 0.4814(5) -0.0024(4) 0.9224(5) 0.026(2) Uani 1.00 1 d . . . C(7) C 0.3753(5) 0.0073(3) 0.9218(5) 0.030(2) Uani 1.00 1 d . . . C(8) C 0.3210(5) 0.0813(4) 0.8982(5) 0.033(2) Uani 1.00 1 d . . . C(9) C 0.3782(5) 0.1506(3) 0.8758(5) 0.025(2) Uani 1.00 1 d . . . C(10) C 0.6676(5) 0.0486(3) 0.9047(5) 0.025(2) Uani 1.00 1 d . . . C(11) C 0.6857(5) -0.0202(4) 0.8408(4) 0.039(2) Uani 1.00 1 d . . . C(12) C 0.7378(5) 0.0316(4) 1.0019(5) 0.037(2) Uani 1.00 1 d . . . C(13) C 0.3215(4) 0.2313(4) 0.8522(4) 0.029(2) Uani 1.00 1 d . . . C(14) C 0.2248(5) 0.2263(4) 0.7671(5) 0.062(2) Uani 1.00 1 d . . . C(15) C 0.2850(7) 0.2661(4) 0.9343(6) 0.061(3) Uani 1.00 1 d . . . C(16) C 0.7853(4) 0.4220(3) 0.9132(4) 0.016(2) Uani 1.00 1 d . . . C(17) C 0.7599(5) 0.5049(3) 0.8858(5) 0.021(2) Uani 1.00 1 d . . . C(18) C 0.8329(5) 0.5664(3) 0.9256(4) 0.023(2) Uani 1.00 1 d . . . C(19) C 0.9276(5) 0.5477(3) 0.9916(5) 0.029(2) Uani 1.00 1 d . . . C(20) C 0.9482(4) 0.4678(3) 1.0226(4) 0.026(2) Uani 1.00 1 d . . . C(21) C 0.8791(4) 0.4044(3) 0.9846(3) 0.0134(12) Uani 1.00 1 d . . . C(22) C 0.6537(5) 0.5270(3) 0.8121(4) 0.025(2) Uani 1.00 1 d . . . C(23) C 0.6748(5) 0.5388(4) 0.7192(4) 0.043(2) Uani 1.00 1 d . . . C(24) C 0.5972(5) 0.6040(4) 0.8389(5) 0.035(2) Uani 1.00 1 d . . . C(25) C 0.9070(4) 0.3157(3) 1.0196(4) 0.035(2) Uani 1.00 1 d . . . C(26) C 1.0144(5) 0.2895(4) 0.9983(6) 0.083(3) Uani 1.00 1 d . . . C(27) C 0.9132(5) 0.3117(3) 1.1193(4) 0.059(2) Uani 1.00 1 d . . . C(28) C 0.6243(4) 0.2442(3) 0.2372(4) 0.014(1) Uani 1.00 1 d . . . C(29) C 0.5618(4) 0.3025(4) 0.2706(3) 0.0157(13) Uani 1.00 1 d . . . C(30) C 0.6940(4) 0.1794(3) 0.2857(4) 0.018(2) Uani 1.00 1 d . . . C(31) C 0.4858(4) 0.3732(3) 0.3771(4) 0.017(2) Uani 1.00 1 d . . . C(32) C 0.3765(4) 0.3624(3) 0.3782(4) 0.015(2) Uani 1.00 1 d . . . C(33) C 0.3216(5) 0.4277(3) 0.4052(4) 0.020(2) Uani 1.00 1 d . . . C(34) C 0.3719(5) 0.5037(3) 0.4275(5) 0.029(2) Uani 1.00 1 d . . . C(35) C 0.4844(5) 0.5132(3) 0.4258(5) 0.026(2) Uani 1.00 1 d . . . C(36) C 0.5410(4) 0.4505(3) 0.3993(4) 0.017(2) Uani 1.00 1 d . . . C(37) C 0.3190(4) 0.2774(3) 0.3564(4) 0.021(2) Uani 1.00 1 d . . . C(38) C 0.2960(6) 0.2393(4) 0.4413(5) 0.043(2) Uani 1.00 1 d . . . C(39) C 0.2135(5) 0.2865(4) 0.2814(5) 0.049(2) Uani 1.00 1 d . . . C(40) C 0.6640(5) 0.4613(4) 0.4020(5) 0.026(2) Uani 1.00 1 d . . . C(41) C 0.7309(6) 0.4785(5) 0.4989(5) 0.059(3) Uani 1.00 1 d . . . C(42) C 0.6784(5) 0.5320(5) 0.3413(6) 0.069(3) Uani 1.00 1 d . . . C(43) C 0.7846(4) 0.0919(3) 0.4036(4) 0.017(2) Uani 1.00 1 d . . . C(44) C 0.8871(4) 0.1191(3) 0.4588(4) 0.0197(13) Uani 1.00 1 d . . . C(45) C 0.9643(4) 0.0578(3) 0.4986(4) 0.027(2) Uani 1.00 1 d . . . C(46) C 0.9406(5) -0.0257(4) 0.4809(5) 0.036(2) Uani 1.00 1 d . . . C(47) C 0.8415(5) -0.0487(4) 0.4232(5) 0.026(2) Uani 1.00 1 d . . . C(48) C 0.7576(4) 0.0094(3) 0.3819(4) 0.017(2) Uani 1.00 1 d . . . C(49) C 0.9131(4) 0.2106(3) 0.4737(3) 0.0253(12) Uani 1.00 1 d . . . C(50) C 0.9581(5) 0.2435(3) 0.3960(4) 0.049(2) Uani 1.00 1 d . . . C(51) C 0.9935(5) 0.2311(3) 0.5629(4) 0.059(2) Uani 1.00 1 d . . . C(52) C 0.6502(5) -0.0194(4) 0.3192(4) 0.024(2) Uani 1.00 1 d . . . C(53) C 0.6624(6) -0.0299(3) 0.2215(5) 0.043(2) Uani 1.00 1 d . . . C(54) C 0.5988(5) -0.0963(4) 0.3494(5) 0.043(2) Uani 1.00 1 d . . . C(55) C 1.0248(5) 0.4773(3) 0.8020(4) 0.056(2) Uani 1.00 1 d . . . C(56) C 0.8917(7) 0.0664(6) 0.7124(5) 0.121(3) Uani 1.00 1 d . . . H(1) H 0.5413 0.1618 0.7357 0.017 Uiso 1.00 1 c R . . H(2) H 0.7546 0.3598 0.7626 0.015 Uiso 1.00 1 c R . . H(3) H 0.5173 -0.0542 0.9385 0.033 Uiso 1.00 1 c R . . H(4) H 0.3351 -0.0385 0.9361 0.036 Uiso 1.00 1 c R . . H(5) H 0.2456 0.0883 0.8997 0.040 Uiso 1.00 1 c R . . H(6) H 0.6979 0.0970 0.8849 0.030 Uiso 1.00 1 c R . . H(7) H 0.6937 -0.0699 0.8753 0.048 Uiso 1.00 1 c R . . H(8) H 0.7498 -0.0122 0.8187 0.048 Uiso 1.00 1 c R . . H(9) H 0.6215 -0.0240 0.7909 0.048 Uiso 1.00 1 c R . . H(10) H 0.7643 0.0814 1.0333 0.043 Uiso 1.00 1 c R . . H(11) H 0.7990 -0.0034 1.0014 0.043 Uiso 1.00 1 c R . . H(12) H 0.6896 0.0042 1.0319 0.043 Uiso 1.00 1 c R . . H(13) H 0.3744 0.2690 0.8399 0.034 Uiso 1.00 1 c R . . H(14) H 0.2514 0.2397 0.7156 0.066 Uiso 1.00 1 c R . . H(15) H 0.1686 0.2646 0.7719 0.066 Uiso 1.00 1 c R . . H(16) H 0.1947 0.1720 0.7603 0.066 Uiso 1.00 1 c R . . H(17) H 0.2117 0.2474 0.9312 0.079 Uiso 1.00 1 c R . . H(18) H 0.2855 0.3248 0.9313 0.078 Uiso 1.00 1 c R . . H(19) H 0.3340 0.2485 0.9900 0.079 Uiso 1.00 1 c R . . H(20) H 0.8213 0.6209 0.9016 0.026 Uiso 1.00 1 c R . . H(21) H 0.9762 0.5906 1.0206 0.034 Uiso 1.00 1 c R . . H(22) H 1.0125 0.4554 1.0702 0.030 Uiso 1.00 1 c R . . H(23) H 0.6055 0.4806 0.8066 0.029 Uiso 1.00 1 c R . . H(24) H 0.6915 0.5954 0.7122 0.048 Uiso 1.00 1 c R . . H(25) H 0.6112 0.5233 0.6724 0.048 Uiso 1.00 1 c R . . H(26) H 0.7365 0.5057 0.7153 0.049 Uiso 1.00 1 c R . . H(27) H 0.5469 0.5832 0.8711 0.041 Uiso 1.00 1 c R . . H(28) H 0.5574 0.6361 0.7886 0.042 Uiso 1.00 1 c R . . H(29) H 0.6518 0.6375 0.8783 0.041 Uiso 1.00 1 c R . . H(30) H 0.8501 0.2796 0.9871 0.036 Uiso 1.00 1 c R . . H(31) H 1.0007 0.2642 0.9400 0.097 Uiso 1.00 1 c R . . H(32) H 1.0519 0.2514 1.0435 0.098 Uiso 1.00 1 c R . . H(33) H 1.0593 0.3372 0.9998 0.097 Uiso 1.00 1 c R . . H(34) H 0.9878 0.3216 1.1532 0.065 Uiso 1.00 1 c R . . H(35) H 0.8911 0.2579 1.1325 0.065 Uiso 1.00 1 c R . . H(36) H 0.8655 0.3516 1.1354 0.065 Uiso 1.00 1 c R . . H(37) H 0.5295 0.3458 0.2300 0.019 Uiso 1.00 1 c R . . H(38) H 0.7403 0.1523 0.2539 0.023 Uiso 1.00 1 c R . . H(39) H 0.2458 0.4211 0.4057 0.026 Uiso 1.00 1 c R . . H(40) H 0.3323 0.5486 0.4446 0.038 Uiso 1.00 1 c R . . H(41) H 0.5208 0.5642 0.4452 0.030 Uiso 1.00 1 c R . . H(42) H 0.3676 0.2422 0.3346 0.027 Uiso 1.00 1 c R . . H(43) H 0.3593 0.2080 0.4717 0.052 Uiso 1.00 1 c R . . H(44) H 0.2321 0.2046 0.4273 0.052 Uiso 1.00 1 c R . . H(45) H 0.2849 0.2832 0.4797 0.052 Uiso 1.00 1 c R . . H(46) H 0.1545 0.2946 0.3096 0.056 Uiso 1.00 1 c R . . H(47) H 0.2000 0.2377 0.2454 0.056 Uiso 1.00 1 c R . . H(48) H 0.2177 0.3326 0.2437 0.056 Uiso 1.00 1 c R . . H(49) H 0.6882 0.4106 0.3819 0.032 Uiso 1.00 1 c R . . H(50) H 0.7359 0.5364 0.5097 0.069 Uiso 1.00 1 c R . . H(51) H 0.8033 0.4566 0.5047 0.069 Uiso 1.00 1 c R . . H(52) H 0.6984 0.4528 0.5419 0.069 Uiso 1.00 1 c R . . H(53) H 0.6742 0.5088 0.2831 0.083 Uiso 1.00 1 c R . . H(54) H 0.7497 0.5562 0.3649 0.082 Uiso 1.00 1 c R . . H(55) H 0.6226 0.5732 0.3359 0.083 Uiso 1.00 1 c R . . H(56) H 1.0339 0.0733 0.5380 0.031 Uiso 1.00 1 c R . . H(57) H 0.9943 -0.0672 0.5048 0.041 Uiso 1.00 1 c R . . H(58) H 0.8231 -0.1058 0.4164 0.032 Uiso 1.00 1 c R . . H(59) H 0.8459 0.2390 0.4726 0.030 Uiso 1.00 1 c R . . H(60) H 1.0369 0.2378 0.4118 0.061 Uiso 1.00 1 c R . . H(61) H 0.9389 0.3002 0.3858 0.061 Uiso 1.00 1 c R . . H(62) H 0.9268 0.2129 0.3421 0.061 Uiso 1.00 1 c R . . H(63) H 0.9557 0.2398 0.6091 0.067 Uiso 1.00 1 c R . . H(64) H 1.0340 0.2795 0.5563 0.067 Uiso 1.00 1 c R . . H(65) H 1.0435 0.1859 0.5795 0.067 Uiso 1.00 1 c R . . H(66) H 0.5958 0.0221 0.3178 0.028 Uiso 1.00 1 c R . . H(67) H 0.6453 0.0203 0.1884 0.052 Uiso 1.00 1 c R . . H(68) H 0.6128 -0.0721 0.1920 0.052 Uiso 1.00 1 c R . . H(69) H 0.7368 -0.0457 0.2241 0.052 Uiso 1.00 1 c R . . H(70) H 0.6261 -0.1391 0.3182 0.048 Uiso 1.00 1 c R . . H(71) H 0.5198 -0.0950 0.3298 0.048 Uiso 1.00 1 c R . . H(72) H 0.6215 -0.1064 0.4131 0.048 Uiso 1.00 1 c R . . H(73) H 0.9822 0.4804 0.8456 0.068 Uiso 1.00 1 c R . . H(74) H 1.0996 0.4632 0.8318 0.068 Uiso 1.00 1 c R . . H(75) H 0.8726 0.0839 0.6506 0.143 Uiso 1.00 1 c R . . H(76) H 0.8358 0.0303 0.7222 0.143 Uiso 1.00 1 c R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ag(1) 0.0326(2) 0.0252(2) 0.0116(3) -0.0080(2) 0.0105(2) -0.0037(2) Ag(2) 0.0287(2) 0.0246(2) 0.0117(3) 0.0079(2) 0.0087(2) 0.0030(2) Cl(1) 0.0757(12) 0.0666(10) 0.0753(13) -0.0268(10) 0.0444(10) -0.0300(10) Cl(2) 0.096(2) 0.0534(9) 0.104(2) -0.0139(10) 0.061(1) 0.0046(11) Cl(3) 0.282(4) 0.0828(13) 0.058(2) 0.040(2) 0.042(2) 0.0115(12) Cl(4) 0.0748(13) 0.132(2) 0.087(2) 0.0411(12) 0.0269(12) 0.0346(13) O(1) 0.044(2) 0.020(2) 0.013(2) -0.018(2) 0.007(2) -0.006(2) O(2) 0.037(2) 0.037(2) 0.022(2) -0.014(2) 0.018(2) -0.001(2) O(3) 0.041(2) 0.027(2) 0.016(2) 0.011(2) 0.009(2) 0.006(2) O(4) 0.048(2) 0.039(2) 0.017(2) 0.022(2) 0.020(2) 0.003(2) N(1) 0.019(2) 0.019(2) 0.006(3) 0.008(2) 0.006(2) 0.008(2) N(2) 0.011(2) 0.017(2) 0.020(3) -0.002(2) 0.003(2) -0.005(2) N(3) 0.019(2) 0.014(2) 0.017(3) -0.003(2) 0.010(2) -0.006(2) N(4) 0.018(2) 0.012(2) 0.021(3) 0.014(2) 0.007(2) 0.004(3) N(5) 0.019(2) 0.013(2) 0.013(3) 0.001(2) 0.008(2) -0.002(2) N(6) 0.026(2) 0.021(2) 0.014(3) -0.001(2) 0.006(2) -0.006(2) C(1) 0.023(3) 0.012(3) 0.010(3) -0.003(2) 0.007(2) -0.002(2) C(2) 0.014(2) 0.005(2) 0.025(4) 0.002(2) -0.002(2) 0.005(2) C(3) 0.014(2) 0.011(3) 0.014(3) -0.004(2) -0.000(2) 0.002(2) C(4) 0.014(3) 0.021(3) 0.011(3) -0.008(2) 0.008(2) -0.003(2) C(5) 0.023(3) 0.021(3) 0.013(4) 0.002(3) 0.003(3) 0.004(3) C(6) 0.036(4) 0.019(3) 0.028(4) -0.004(3) 0.016(3) 0.008(3) C(7) 0.030(4) 0.020(4) 0.041(5) -0.015(3) 0.009(3) 0.005(3) C(8) 0.022(3) 0.047(4) 0.032(5) -0.008(3) 0.012(3) -0.001(3) C(9) 0.028(3) 0.015(3) 0.036(5) 0.001(3) 0.016(3) -0.000(3) C(10) 0.022(3) 0.022(3) 0.031(5) -0.001(3) 0.007(3) 0.007(3) C(11) 0.037(4) 0.055(4) 0.027(4) 0.001(3) 0.011(3) -0.019(3) C(12) 0.034(4) 0.034(3) 0.038(5) 0.011(3) 0.005(3) -0.010(3) C(13) 0.022(3) 0.030(4) 0.033(4) -0.003(3) 0.007(3) 0.003(3) C(14) 0.057(4) 0.032(3) 0.076(6) -0.009(4) -0.019(4) 0.021(4) C(15) 0.092(6) 0.047(4) 0.058(6) 0.042(4) 0.041(5) 0.008(4) C(16) 0.021(3) 0.017(3) 0.012(3) -0.001(2) 0.006(3) -0.003(2) C(17) 0.024(3) 0.017(4) 0.025(4) 0.005(3) 0.010(3) 0.000(3) C(18) 0.023(3) 0.014(3) 0.029(4) -0.007(2) 0.004(3) -0.004(3) C(19) 0.032(3) 0.024(3) 0.029(4) -0.010(2) 0.006(3) -0.006(2) C(20) 0.016(3) 0.034(3) 0.025(3) 0.004(2) -0.002(2) -0.000(2) C(21) 0.015(2) 0.013(2) 0.012(3) 0.002(2) 0.002(2) -0.001(2) C(22) 0.038(4) 0.007(2) 0.028(4) 0.005(2) 0.004(3) 0.002(2) C(23) 0.036(4) 0.065(4) 0.020(4) 0.002(3) -0.007(3) 0.031(3) C(24) 0.038(4) 0.033(3) 0.033(4) 0.019(3) 0.003(3) 0.005(3) C(25) 0.028(3) 0.022(3) 0.039(4) -0.009(2) -0.016(3) 0.006(2) C(26) 0.066(4) 0.039(3) 0.138(8) 0.037(3) 0.018(5) -0.002(4) C(27) 0.072(4) 0.038(3) 0.053(4) -0.005(3) -0.012(3) 0.025(3) C(28) 0.012(2) 0.018(3) 0.014(3) -0.000(2) 0.004(2) -0.002(2) C(29) 0.025(3) 0.024(3) -0.001(3) 0.004(3) 0.005(2) 0.004(3) C(30) 0.019(3) 0.018(3) 0.021(4) -0.005(2) 0.014(3) -0.007(2) C(31) 0.028(3) 0.015(3) 0.006(3) 0.004(2) 0.002(3) 0.003(2) C(32) 0.013(3) 0.021(3) 0.009(4) 0.008(2) 0.002(2) 0.002(3) C(33) 0.026(3) 0.011(3) 0.030(4) 0.004(2) 0.018(3) 0.007(2) C(34) 0.039(4) 0.026(4) 0.031(4) -0.002(3) 0.026(3) -0.003(3) C(35) 0.029(4) 0.017(3) 0.029(4) -0.003(3) 0.004(3) 0.000(3) C(36) 0.019(3) 0.015(3) 0.018(4) 0.004(3) 0.007(3) 0.003(3) C(37) 0.019(3) 0.016(3) 0.033(4) -0.005(2) 0.015(3) -0.003(2) C(38) 0.053(4) 0.028(3) 0.049(5) -0.005(3) 0.016(4) 0.006(3) C(39) 0.053(4) 0.046(4) 0.041(4) -0.030(3) -0.001(3) 0.006(3) C(40) 0.025(3) 0.023(4) 0.031(5) -0.004(3) 0.010(3) -0.009(3) C(41) 0.033(4) 0.090(5) 0.049(6) -0.002(4) 0.003(4) 0.023(5) C(42) 0.017(4) 0.122(6) 0.067(7) -0.017(4) 0.009(4) 0.043(6) C(43) 0.018(3) 0.016(3) 0.019(4) 0.006(2) 0.010(3) 0.003(2) C(44) 0.026(3) 0.024(2) 0.013(3) 0.003(2) 0.011(2) 0.007(2) C(45) 0.016(3) 0.026(3) 0.035(4) 0.002(2) 0.001(3) -0.001(2) C(46) 0.017(3) 0.027(3) 0.060(5) 0.009(2) 0.002(3) 0.011(3) C(47) 0.028(3) 0.019(3) 0.034(5) -0.005(3) 0.011(3) 0.003(3) C(48) 0.016(3) 0.023(4) 0.015(4) 0.001(3) 0.006(3) 0.000(3) C(49) 0.027(2) 0.026(2) 0.023(3) -0.013(2) 0.007(2) -0.012(2) C(50) 0.075(4) 0.032(3) 0.046(4) -0.026(3) 0.023(3) -0.010(2) C(51) 0.068(4) 0.054(4) 0.045(4) -0.034(3) -0.003(3) -0.014(3) C(52) 0.025(3) 0.026(3) 0.020(4) 0.009(3) 0.004(3) 0.003(3) C(53) 0.063(5) 0.020(3) 0.047(5) -0.007(3) 0.017(4) 0.005(3) C(54) 0.029(4) 0.030(3) 0.061(6) -0.006(3) -0.006(4) 0.015(3) C(55) 0.051(4) 0.066(4) 0.052(4) -0.021(3) 0.018(3) -0.014(3) C(56) 0.125(7) 0.197(8) 0.036(5) -0.141(7) 0.014(5) -0.015(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Ag Ag -0.897 1.101 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 N(1) Ag(1) O(3) 128.4(2) ? . . . N(2) Ag(1) O(3) 144.8(2) ? . . . Ag(1) O(3) N(6) 103.8(3) ? . . . N(2) Ag(1) N(1) 86.6(2) ? . . . Ag(1) N(1) C(2) 127.2(4) ? . . . Ag(1) N(1) C(4) 116.8(3) ? . . . Ag(1) N(2) C(3) 125.0(3) ? . . . Ag(1) N(2) C(16) 116.9(4) ? . . . Ag(2) O(1) N(3) 106.5(3) ? . . . N(4) Ag(2) O(1) 129.1(2) ? . . . N(5) Ag(2) O(1) 144.9(1) ? . . . N(5) Ag(2) N(4) 85.0(2) ? . . . Ag(2) N(4) C(29) 125.7(4) ? . . . Ag(2) N(4) C(31) 114.3(3) ? . . . Ag(2) N(5) C(30) 126.9(3) ? . . . Ag(2) N(5) C(43) 116.3(4) ? . . . Cl(1) C(55) Cl(2) 115.3(4) ? . . . Cl(3) C(56) Cl(4) 112.4(4) ? . . . O(1) N(3) C(1) 120.6(5) ? . . . O(1) N(3) O(2) 117.1(5) ? . . . O(2) N(3) C(1) 122.3(4) ? . . . O(3) N(6) O(4) 117.8(5) ? . . . O(3) N(6) C(28) 120.2(5) ? . . 55601 O(4) N(6) C(28) 122.0(4) ? . . 55601 N(1) C(2) C(1) 124.8(5) ? . . . C(4) N(1) C(2) 115.6(5) ? . . . N(1) C(4) C(5) 119.4(5) ? . . . N(1) C(4) C(9) 117.6(4) ? . . . N(2) C(3) C(1) 126.4(5) ? . . . C(16) N(2) C(3) 117.8(5) ? . . . N(2) C(16) C(17) 120.0(4) ? . . . N(2) C(16) C(21) 119.8(4) ? . . . N(3) C(1) C(2) 115.4(4) ? . . . N(3) C(1) C(3) 115.0(5) ? . . . N(4) C(29) C(28) 126.7(5) ? . . . C(31) N(4) C(29) 119.5(5) ? . . . N(4) C(31) C(32) 119.1(4) ? . . . N(4) C(31) C(36) 119.2(5) ? . . . N(5) C(30) C(28) 126.6(6) ? . . . C(43) N(5) C(30) 115.9(5) ? . . . N(5) C(43) C(44) 116.4(4) ? . . . N(5) C(43) C(48) 119.1(4) ? . . . N(6) C(28) C(29) 116.5(4) ? . 55601 55601 N(6) C(28) C(30) 114.8(5) ? . 55601 55601 C(3) C(1) C(2) 129.4(6) ? . . . C(9) C(4) C(5) 122.5(5) ? . . . C(4) C(5) C(10) 124.4(5) ? . . . C(4) C(5) C(6) 116.7(5) ? . . . C(4) C(9) C(13) 122.2(5) ? . . . C(4) C(9) C(8) 116.5(5) ? . . . C(10) C(5) C(6) 118.9(5) ? . . . C(5) C(6) C(7) 121.8(5) ? . . . C(5) C(10) C(12) 113.2(6) ? . . . C(5) C(10) C(11) 112.7(5) ? . . . C(6) C(7) C(8) 121.7(6) ? . . . C(7) C(8) C(9) 120.5(6) ? . . . C(8) C(9) C(13) 121.1(5) ? . . . C(9) C(13) C(14) 112.4(5) ? . . . C(9) C(13) C(15) 110.3(6) ? . . . C(12) C(10) C(11) 109.9(5) ? . . . C(15) C(13) C(14) 112.0(5) ? . . . C(21) C(16) C(17) 119.8(4) ? . . . C(16) C(17) C(22) 121.3(4) ? . . . C(16) C(17) C(18) 118.9(5) ? . . . C(16) C(21) C(25) 121.6(4) ? . . . C(16) C(21) C(20) 118.9(4) ? . . . C(22) C(17) C(18) 119.8(4) ? . . . C(17) C(18) C(19) 120.5(5) ? . . . C(17) C(22) C(23) 112.7(6) ? . . . C(17) C(22) C(24) 111.2(5) ? . . . C(18) C(19) C(20) 120.5(5) ? . . . C(19) C(20) C(21) 121.2(5) ? . . . C(20) C(21) C(25) 119.5(4) ? . . . C(21) C(25) C(27) 109.7(4) ? . . . C(21) C(25) C(26) 108.6(5) ? . . . C(24) C(22) C(23) 110.3(5) ? . . . C(27) C(25) C(26) 112.8(5) ? . . . C(29) C(28) N(6) 116.5(4) ? . . 55401 C(30) C(28) N(6) 114.8(5) ? . . 55401 C(28) N(6) O(3) 120.2(5) ? . 55401 55401 C(28) N(6) O(4) 122.0(4) ? . 55401 55401 C(30) C(28) C(29) 128.6(6) ? . . . C(36) C(31) C(32) 121.7(5) ? . . . C(31) C(32) C(37) 120.9(5) ? . . . C(31) C(32) C(33) 118.4(5) ? . . . C(31) C(36) C(40) 121.6(5) ? . . . C(31) C(36) C(35) 118.2(5) ? . . . C(37) C(32) C(33) 120.5(5) ? . . . C(32) C(33) C(34) 121.9(6) ? . . . C(32) C(37) C(38) 110.8(5) ? . . . C(32) C(37) C(39) 109.9(4) ? . . . C(33) C(34) C(35) 118.6(5) ? . . . C(34) C(35) C(36) 121.2(5) ? . . . C(35) C(36) C(40) 120.0(5) ? . . . C(36) C(40) C(41) 109.8(6) ? . . . C(36) C(40) C(42) 110.3(5) ? . . . C(39) C(37) C(38) 111.3(5) ? . . . C(42) C(40) C(41) 109.4(5) ? . . . C(43) C(44) C(49) 121.3(4) ? . . . C(43) C(44) C(45) 116.8(4) ? . . . C(48) C(43) C(44) 124.5(5) ? . . . C(43) C(48) C(52) 124.6(5) ? . . . C(43) C(48) C(47) 115.0(5) ? . . . C(49) C(44) C(45) 121.9(4) ? . . . C(44) C(45) C(46) 120.9(5) ? . . . C(44) C(49) C(50) 109.2(4) ? . . . C(44) C(49) C(51) 114.7(4) ? . . . C(45) C(46) C(47) 119.9(5) ? . . . C(46) C(47) C(48) 122.7(5) ? . . . C(47) C(48) C(52) 120.4(5) ? . . . C(48) C(52) C(53) 110.7(5) ? . . . C(48) C(52) C(54) 115.9(5) ? . . . C(51) C(49) C(50) 109.4(4) ? . . . C(54) C(52) C(53) 110.8(5) ? . . . Cl(1) C(55) H(73) 106.6870 ? . . . Cl(1) C(55) H(74) 108.8197 ? . . . Cl(2) C(55) H(73) 107.2377 ? . . . Cl(2) C(55) H(74) 109.1965 ? . . . Cl(3) C(56) H(75) 110.9641 ? . . . Cl(3) C(56) H(76) 107.2259 ? . . . Cl(4) C(56) H(75) 109.7618 ? . . . Cl(4) C(56) H(76) 106.9053 ? . . . N(1) C(2) H(1) 117.5276 ? . . . N(2) C(3) H(2) 116.4281 ? . . . N(4) C(29) H(37) 117.1111 ? . . . N(5) C(30) H(38) 117.2732 ? . . . C(1) C(2) H(1) 117.6666 ? . . . C(1) C(3) H(2) 117.1369 ? . . . C(5) C(6) H(3) 117.7145 ? . . . C(5) C(10) H(6) 109.0054 ? . . . H(3) C(6) C(7) 120.4553 ? . . . C(6) C(7) H(4) 119.1685 ? . . . C(7) C(8) H(5) 121.1915 ? . . . H(4) C(7) C(8) 119.1120 ? . . . H(5) C(8) C(9) 118.1964 ? . . . C(9) C(13) H(13) 107.6339 ? . . . H(6) C(10) C(11) 105.2513 ? . . . C(10) C(11) H(8) 113.5301 ? . . . C(10) C(11) H(9) 108.7777 ? . . . C(10) C(11) H(7) 106.0104 ? . . . H(6) C(10) C(12) 106.2511 ? . . . C(10) C(12) H(10) 111.6588 ? . . . C(10) C(12) H(12) 105.9274 ? . . . C(10) C(12) H(11) 110.7591 ? . . . H(8) C(11) H(7) 109.4697 ? . . . H(9) C(11) H(7) 109.4718 ? . . . H(9) C(11) H(8) 109.4804 ? . . . H(12) C(12) H(10) 109.4666 ? . . . H(11) C(12) H(10) 109.4745 ? . . . H(12) C(12) H(11) 109.4793 ? . . . H(13) C(13) C(14) 107.4497 ? . . . C(13) C(14) H(16) 110.0600 ? . . . C(13) C(14) H(14) 108.7930 ? . . . C(13) C(14) H(15) 109.5565 ? . . . H(13) C(13) C(15) 106.7805 ? . . . C(13) C(15) H(19) 110.9385 ? . . . C(13) C(15) H(17) 108.8536 ? . . . C(13) C(15) H(18) 108.5997 ? . . . H(16) C(14) H(14) 109.4677 ? . . . H(15) C(14) H(14) 109.4731 ? . . . H(16) C(14) H(15) 109.4746 ? . . . H(19) C(15) H(17) 109.4797 ? . . . H(18) C(15) H(17) 109.4726 ? . . . H(19) C(15) H(18) 109.4732 ? . . . C(17) C(18) H(20) 118.9104 ? . . . C(17) C(22) H(23) 106.4588 ? . . . H(20) C(18) C(19) 120.1845 ? . . . C(18) C(19) H(21) 120.1476 ? . . . C(19) C(20) H(22) 120.2987 ? . . . H(21) C(19) C(20) 119.1161 ? . . . H(22) C(20) C(21) 118.4641 ? . . . C(21) C(25) H(30) 108.7635 ? . . . C(22) C(23) H(26) 108.9337 ? . . . H(23) C(22) C(23) 106.0687 ? . . . C(22) C(23) H(24) 108.8055 ? . . . C(22) C(23) H(25) 110.6696 ? . . . H(23) C(22) C(24) 109.9737 ? . . . C(22) C(24) H(27) 104.9411 ? . . . C(22) C(24) H(28) 114.1104 ? . . . C(22) C(24) H(29) 109.2449 ? . . . H(26) C(23) H(24) 109.4731 ? . . . H(25) C(23) H(24) 109.4690 ? . . . H(26) C(23) H(25) 109.4699 ? . . . H(28) C(24) H(27) 109.4718 ? . . . H(29) C(24) H(27) 109.4531 ? . . . H(29) C(24) H(28) 109.4753 ? . . . H(30) C(25) C(26) 107.1876 ? . . . C(25) C(26) H(31) 111.4207 ? . . . C(25) C(26) H(33) 108.2890 ? . . . C(25) C(26) H(32) 108.6913 ? . . . H(30) C(25) C(27) 109.6482 ? . . . C(25) C(27) H(35) 108.1130 ? . . . C(25) C(27) H(36) 111.0901 ? . . . C(25) C(27) H(34) 109.1892 ? . . . H(33) C(26) H(31) 109.4654 ? . . . H(32) C(26) H(31) 109.4665 ? . . . H(33) C(26) H(32) 109.4772 ? . . . H(35) C(27) H(34) 109.4804 ? . . . H(36) C(27) H(34) 109.4685 ? . . . H(36) C(27) H(35) 109.4724 ? . . . C(28) C(29) H(37) 116.2161 ? . . . C(28) C(30) H(38) 116.0851 ? . . . C(32) C(33) H(39) 119.1360 ? . . . C(32) C(37) H(42) 107.8268 ? . . . H(39) C(33) C(34) 118.9398 ? . . . C(33) C(34) H(40) 120.9096 ? . . . C(34) C(35) H(41) 118.7723 ? . . . H(40) C(34) C(35) 120.5037 ? . . . H(41) C(35) C(36) 120.0425 ? . . . C(36) C(40) H(49) 106.8853 ? . . . H(42) C(37) C(38) 109.2796 ? . . . C(37) C(38) H(43) 108.2876 ? . . . C(37) C(38) H(45) 107.9435 ? . . . C(37) C(38) H(44) 112.1496 ? . . . H(42) C(37) C(39) 107.6189 ? . . . C(37) C(39) H(48) 111.1257 ? . . . C(37) C(39) H(46) 107.0673 ? . . . C(37) C(39) H(47) 110.1900 ? . . . H(45) C(38) H(43) 109.4692 ? . . . H(44) C(38) H(43) 109.4705 ? . . . H(45) C(38) H(44) 109.4744 ? . . . H(48) C(39) H(46) 109.4690 ? . . . H(47) C(39) H(46) 109.4729 ? . . . H(48) C(39) H(47) 109.4736 ? . . . H(49) C(40) C(41) 109.3521 ? . . . C(40) C(41) H(51) 106.8566 ? . . . C(40) C(41) H(52) 111.4226 ? . . . C(40) C(41) H(50) 110.1011 ? . . . H(49) C(40) C(42) 111.0561 ? . . . C(40) C(42) H(53) 106.5423 ? . . . C(40) C(42) H(55) 112.6423 ? . . . C(40) C(42) H(54) 109.1651 ? . . . H(51) C(41) H(50) 109.4741 ? . . . H(52) C(41) H(50) 109.4660 ? . . . H(52) C(41) H(51) 109.4721 ? . . . H(55) C(42) H(53) 109.4766 ? . . . H(54) C(42) H(53) 109.4745 ? . . . H(55) C(42) H(54) 109.4696 ? . . . C(44) C(45) H(56) 119.6966 ? . . . C(44) C(49) H(59) 108.3787 ? . . . H(56) C(45) C(46) 119.3547 ? . . . C(45) C(46) H(57) 121.1097 ? . . . C(46) C(47) H(58) 119.0195 ? . . . H(57) C(46) C(47) 118.8825 ? . . . H(58) C(47) C(48) 117.6980 ? . . . C(48) C(52) H(66) 107.8313 ? . . . H(59) C(49) C(50) 108.3712 ? . . . C(49) C(50) H(62) 109.5670 ? . . . C(49) C(50) H(60) 109.2795 ? . . . C(49) C(50) H(61) 109.5643 ? . . . H(59) C(49) C(51) 106.6229 ? . . . C(49) C(51) H(63) 111.1185 ? . . . C(49) C(51) H(64) 109.4698 ? . . . C(49) C(51) H(65) 107.8082 ? . . . H(62) C(50) H(60) 109.4697 ? . . . H(61) C(50) H(60) 109.4751 ? . . . H(62) C(50) H(61) 109.4715 ? . . . H(64) C(51) H(63) 109.4736 ? . . . H(65) C(51) H(63) 109.4748 ? . . . H(65) C(51) H(64) 109.4654 ? . . . H(66) C(52) C(53) 107.6802 ? . . . C(52) C(53) H(67) 110.6560 ? . . . C(52) C(53) H(69) 109.1102 ? . . . C(52) C(53) H(68) 108.6373 ? . . . H(66) C(52) C(54) 103.3976 ? . . . C(52) C(54) H(70) 102.2887 ? . . . C(52) C(54) H(72) 114.2685 ? . . . C(52) C(54) H(71) 111.5872 ? . . . H(69) C(53) H(67) 109.4660 ? . . . H(68) C(53) H(67) 109.4765 ? . . . H(69) C(53) H(68) 109.4746 ? . . . H(72) C(54) H(70) 109.4772 ? . . . H(71) C(54) H(70) 109.4680 ? . . . H(72) C(54) H(71) 109.4716 ? . . . H(74) C(55) H(73) 109.4606 ? . . . H(76) C(56) H(75) 109.4576 ? . . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Ag(1) O(3) 2.240(4) ? . . Ag(1) N(1) 2.247(4) ? . . Ag(1) N(2) 2.241(5) ? . . Ag(2) O(1) 2.243(4) ? . . Ag(2) N(4) 2.286(4) ? . . Ag(2) N(5) 2.231(5) ? . . Cl(1) C(55) 1.726(6) ? . . Cl(2) C(55) 1.714(6) ? . . Cl(3) C(56) 1.68(1) ? . . Cl(4) C(56) 1.795(9) ? . . O(1) N(3) 1.266(5) ? . . O(2) N(3) 1.275(6) ? . . O(3) N(6) 1.288(6) ? . . O(4) N(6) 1.250(7) ? . . N(1) C(2) 1.258(8) ? . . N(1) C(4) 1.438(7) ? . . N(2) C(3) 1.309(8) ? . . N(2) C(16) 1.437(6) ? . . N(3) C(1) 1.372(8) ? . . N(4) C(29) 1.293(7) ? . . N(4) C(31) 1.450(7) ? . . N(5) C(30) 1.283(8) ? . . N(5) C(43) 1.465(6) ? . . N(6) C(28) 1.376(8) ? . 55601 C(1) C(2) 1.471(8) ? . . C(1) C(3) 1.411(7) ? . . C(4) C(5) 1.387(7) ? . . C(4) C(9) 1.418(8) ? . . C(5) C(6) 1.426(9) ? . . C(5) C(10) 1.519(8) ? . . C(6) C(7) 1.326(9) ? . . C(7) C(8) 1.375(8) ? . . C(8) C(9) 1.415(9) ? . . C(9) C(13) 1.482(8) ? . . C(10) C(11) 1.532(9) ? . . C(10) C(12) 1.534(9) ? . . C(13) C(14) 1.523(8) ? . . C(13) C(15) 1.54(1) ? . . C(16) C(17) 1.415(7) ? . . C(16) C(21) 1.401(7) ? . . C(17) C(18) 1.377(7) ? . . C(17) C(22) 1.536(8) ? . . C(18) C(19) 1.368(8) ? . . C(19) C(20) 1.376(7) ? . . C(20) C(21) 1.365(7) ? . . C(21) C(25) 1.539(6) ? . . C(22) C(23) 1.51(1) ? . . C(22) C(24) 1.535(9) ? . . C(25) C(26) 1.513(9) ? . . C(25) C(27) 1.500(9) ? . . C(28) N(6) 1.376(8) ? . 55401 C(28) C(29) 1.398(8) ? . . C(28) C(30) 1.435(7) ? . . C(31) C(32) 1.374(8) ? . . C(31) C(36) 1.423(7) ? . . C(32) C(33) 1.376(8) ? . . C(32) C(37) 1.546(7) ? . . C(33) C(34) 1.381(7) ? . . C(34) C(35) 1.415(9) ? . . C(35) C(36) 1.352(8) ? . . C(36) C(40) 1.530(8) ? . . C(37) C(38) 1.52(1) ? . . C(37) C(39) 1.506(8) ? . . C(40) C(41) 1.517(9) ? . . C(40) C(42) 1.51(1) ? . . C(43) C(44) 1.403(7) ? . . C(43) C(48) 1.394(7) ? . . C(44) C(45) 1.404(7) ? . . C(44) C(49) 1.518(7) ? . . C(45) C(46) 1.393(8) ? . . C(46) C(47) 1.365(8) ? . . C(47) C(48) 1.423(7) ? . . C(48) C(52) 1.499(7) ? . . C(49) C(50) 1.529(8) ? . . C(49) C(51) 1.499(7) ? . . C(52) C(53) 1.54(1) ? . . C(52) C(54) 1.522(9) ? . . C(2) H(1) 0.9499 ? . . C(3) H(2) 0.9501 ? . . C(6) H(3) 0.9500 ? . . C(7) H(4) 0.9500 ? . . C(8) H(5) 0.9501 ? . . C(10) H(6) 0.9500 ? . . C(11) H(7) 0.9500 ? . . C(11) H(8) 0.9499 ? . . C(11) H(9) 0.9500 ? . . C(12) H(10) 0.9500 ? . . C(12) H(11) 0.9500 ? . . C(12) H(12) 0.9501 ? . . C(13) H(13) 0.9500 ? . . C(14) H(14) 0.9500 ? . . C(14) H(15) 0.9500 ? . . C(14) H(16) 0.9499 ? . . C(15) H(17) 0.9500 ? . . C(15) H(18) 0.9500 ? . . C(15) H(19) 0.9499 ? . . C(18) H(20) 0.9500 ? . . C(19) H(21) 0.9500 ? . . C(20) H(22) 0.9500 ? . . C(22) H(23) 0.9499 ? . . C(23) H(24) 0.9501 ? . . C(23) H(25) 0.9500 ? . . C(23) H(26) 0.9500 ? . . C(24) H(27) 0.9501 ? . . C(24) H(28) 0.9500 ? . . C(24) H(29) 0.9500 ? . . C(25) H(30) 0.9501 ? . . C(26) H(31) 0.9501 ? . . C(26) H(32) 0.9500 ? . . C(26) H(33) 0.9500 ? . . C(27) H(34) 0.9500 ? . . C(27) H(35) 0.9500 ? . . C(27) H(36) 0.9499 ? . . C(29) H(37) 0.9500 ? . . C(30) H(38) 0.9499 ? . . C(33) H(39) 0.9500 ? . . C(34) H(40) 0.9499 ? . . C(35) H(41) 0.9500 ? . . C(37) H(42) 0.9500 ? . . C(38) H(43) 0.9500 ? . . C(38) H(44) 0.9500 ? . . C(38) H(45) 0.9500 ? . . C(39) H(46) 0.9500 ? . . C(39) H(47) 0.9501 ? . . C(39) H(48) 0.9499 ? . . C(40) H(49) 0.9500 ? . . C(41) H(50) 0.9500 ? . . C(41) H(51) 0.9500 ? . . C(41) H(52) 0.9499 ? . . C(42) H(53) 0.9501 ? . . C(42) H(54) 0.9500 ? . . C(42) H(55) 0.9501 ? . . C(45) H(56) 0.9500 ? . . C(46) H(57) 0.9500 ? . . C(47) H(58) 0.9501 ? . . C(49) H(59) 0.9500 ? . . C(50) H(60) 0.9500 ? . . C(50) H(61) 0.9500 ? . . C(50) H(62) 0.9499 ? . . C(51) H(63) 0.9500 ? . . C(51) H(64) 0.9500 ? . . C(51) H(65) 0.9500 ? . . C(52) H(66) 0.9499 ? . . C(53) H(67) 0.9499 ? . . C(53) H(68) 0.9499 ? . . C(53) H(69) 0.9500 ? . . C(54) H(70) 0.9501 ? . . C(54) H(71) 0.9500 ? . . C(54) H(72) 0.9500 ? . . C(55) H(73) 0.9500 ? . . C(55) H(74) 0.9500 ? . . C(56) H(75) 0.9501 ? . . C(56) H(76) 0.9500 ? . . H(33) C(26) 0.9500 ? . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Ag(1) O(4) 2.638(4) ? . . Ag(1) N(6) 2.839(5) ? . . Ag(1) C(1) 3.505(6) ? . . Ag(1) C(2) 3.169(6) ? . . Ag(1) C(3) 3.178(6) ? . . Ag(1) C(4) 3.167(5) ? . . Ag(1) C(16) 3.163(6) ? . . Ag(1) C(25) 3.530(5) ? . . Ag(2) O(2) 2.684(4) ? . . Ag(2) N(3) 2.872(5) ? . . Ag(2) C(28) 3.540(6) ? . . Ag(2) C(29) 3.217(5) ? . . Ag(2) C(30) 3.171(7) ? . . Ag(2) C(31) 3.171(5) ? . . Ag(2) C(43) 3.165(6) ? . . Ag(2) C(49) 3.577(5) ? . . Cl(1) Cl(2) 2.906(3) ? . . Cl(1) O(2) 3.549(4) ? . . Cl(3) Cl(4) 2.884(5) ? . . Cl(3) C(45) 3.599(7) ? . . Cl(4) C(1) 3.562(5) ? . . O(1) O(2) 2.168(6) ? . . O(1) C(1) 2.292(7) ? . . O(1) C(2) 2.663(7) ? . . O(1) C(3) 3.527(6) ? . . O(1) C(34) 3.324(7) ? . 64602 O(1) C(35) 3.208(7) ? . 64602 O(2) C(1) 2.320(8) ? . . O(2) C(3) 2.660(7) ? . . O(2) C(41) 3.458(9) ? . . O(3) O(4) 2.173(6) ? . . O(3) C(28) 2.310(7) ? . 55601 O(3) C(29) 2.651(7) ? . 55601 O(3) C(30) 3.568(7) ? . 55601 O(4) C(12) 3.408(8) ? . . O(4) C(27) 3.378(7) ? . . O(4) C(28) 2.298(8) ? . 55601 O(4) C(29) 3.526(7) ? . 55601 O(4) C(30) 2.652(8) ? . 55601 N(1) N(2) 3.078(6) ? . . N(1) N(3) 3.588(7) ? . . N(1) C(1) 2.420(8) ? . . N(1) C(3) 3.089(7) ? . . N(1) C(5) 2.441(7) ? . . N(1) C(9) 2.444(8) ? . . N(1) C(10) 2.954(7) ? . . N(1) C(13) 2.877(7) ? . . N(2) N(3) 3.596(7) ? . . N(2) C(1) 2.429(7) ? . . N(2) C(2) 3.129(6) ? . . N(2) C(17) 2.470(6) ? . . N(2) C(21) 2.455(6) ? . . N(2) C(22) 2.933(7) ? . . N(2) C(25) 2.924(6) ? . . N(3) C(2) 2.404(8) ? . . N(3) C(3) 2.348(7) ? . . N(4) N(5) 3.051(6) ? . . N(4) N(6) 3.591(7) ? . 55401 N(4) C(28) 2.405(8) ? . . N(4) C(30) 3.069(7) ? . . N(4) C(32) 2.435(7) ? . . N(4) C(36) 2.478(7) ? . . N(4) C(37) 2.876(7) ? . . N(4) C(40) 2.932(7) ? . . N(5) N(6) 3.591(7) ? . 55401 N(5) C(28) 2.429(7) ? . . N(5) C(29) 3.078(7) ? . . N(5) C(44) 2.437(6) ? . . N(5) C(48) 2.465(6) ? . . N(5) C(49) 2.845(6) ? . . N(5) C(50) 3.413(7) ? . . N(5) C(52) 2.959(7) ? . . N(6) N(4) 3.591(7) ? . 55601 N(6) N(5) 3.591(7) ? . 55601 N(6) C(29) 2.359(8) ? . 55601 N(6) C(30) 2.369(7) ? . 55601 C(2) C(3) 2.606(7) ? . . C(2) C(4) 2.284(8) ? . . C(2) C(5) 3.041(8) ? . . C(2) C(9) 3.289(9) ? . . C(2) C(10) 3.241(8) ? . . C(3) C(16) 2.352(7) ? . . C(3) C(17) 3.137(7) ? . . C(3) C(21) 3.351(7) ? . . C(3) C(22) 3.268(7) ? . . C(3) C(23) 3.531(8) ? . . C(4) C(6) 2.395(8) ? . . C(4) C(7) 2.751(8) ? . . C(4) C(8) 2.410(9) ? . . C(4) C(10) 2.572(7) ? . . C(4) C(13) 2.540(7) ? . . C(4) C(14) 3.573(8) ? . . C(4) C(15) 3.60(1) ? . . C(5) C(7) 2.406(9) ? . . C(5) C(8) 2.801(9) ? . . C(5) C(9) 2.460(8) ? . . C(5) C(11) 2.540(9) ? . . C(5) C(12) 2.550(8) ? . . C(6) C(8) 2.359(9) ? . . C(6) C(9) 2.792(8) ? . . C(6) C(10) 2.537(9) ? . . C(6) C(11) 3.12(1) ? . . C(6) C(12) 3.150(8) ? . . C(7) C(9) 2.423(8) ? . . C(8) C(13) 2.523(8) ? . . C(8) C(14) 3.108(9) ? . . C(8) C(15) 3.091(9) ? . . C(9) C(14) 2.497(8) ? . . C(9) C(15) 2.48(1) ? . . C(11) C(12) 2.510(9) ? . . C(14) C(15) 2.54(1) ? . . C(16) C(18) 2.404(7) ? . . C(16) C(19) 2.755(7) ? . . C(16) C(20) 2.382(7) ? . . C(16) C(22) 2.573(7) ? . . C(16) C(23) 3.473(8) ? . . C(16) C(25) 2.567(7) ? . . C(16) C(26) 3.530(8) ? . . C(16) C(27) 3.597(8) ? . . C(17) C(19) 2.383(8) ? . . C(17) C(20) 2.765(7) ? . . C(17) C(21) 2.436(7) ? . . C(17) C(23) 2.539(9) ? . . C(17) C(24) 2.533(8) ? . . C(18) C(20) 2.382(7) ? . . C(18) C(21) 2.779(7) ? . . C(18) C(22) 2.521(8) ? . . C(18) C(23) 3.274(8) ? . . C(18) C(24) 2.948(8) ? . . C(19) C(21) 2.389(7) ? . . C(19) C(55) 3.59(1) ? . . C(20) C(25) 2.510(7) ? . . C(20) C(26) 3.047(8) ? . . C(20) C(27) 3.008(8) ? . . C(21) C(26) 2.479(8) ? . . C(21) C(27) 2.484(7) ? . . C(23) C(24) 2.50(1) ? . . C(24) C(28) 3.522(8) ? . 65602 C(26) C(27) 2.51(1) ? . . C(28) O(3) 2.310(7) ? . 55401 C(28) O(4) 2.298(8) ? . 55401 C(28) C(24) 3.522(8) ? . 64602 C(29) O(3) 2.651(7) ? . 55401 C(29) O(4) 3.526(7) ? . 55401 C(29) N(6) 2.359(8) ? . 55401 C(29) C(30) 2.553(7) ? . . C(29) C(31) 2.371(8) ? . . C(29) C(32) 3.299(8) ? . . C(29) C(36) 3.145(8) ? . . C(29) C(40) 3.299(8) ? . . C(30) O(3) 3.568(7) ? . 55401 C(30) O(4) 2.652(8) ? . 55401 C(30) N(6) 2.369(7) ? . 55401 C(30) C(43) 2.331(8) ? . . C(30) C(44) 3.219(7) ? . . C(30) C(48) 3.118(7) ? . . C(30) C(49) 3.436(7) ? . . C(30) C(50) 3.436(7) ? . . C(30) C(52) 3.322(8) ? . . C(30) C(53) 3.516(7) ? . . C(31) C(33) 2.361(8) ? . . C(31) C(34) 2.758(8) ? . . C(31) C(35) 2.382(7) ? . . C(31) C(37) 2.542(7) ? . . C(31) C(38) 3.521(9) ? . . C(31) C(40) 2.578(8) ? . . C(31) C(41) 3.561(8) ? . . C(32) C(34) 2.409(7) ? . . C(32) C(35) 2.785(7) ? . . C(32) C(36) 2.443(7) ? . . C(32) C(38) 2.526(9) ? . . C(32) C(39) 2.498(8) ? . . C(33) C(35) 2.404(8) ? . . C(33) C(36) 2.776(8) ? . . C(33) C(37) 2.538(7) ? . . C(33) C(38) 3.125(7) ? . . C(33) C(39) 3.042(8) ? . . C(33) C(56) 3.58(1) ? . 65602 C(34) O(1) 3.324(7) ? . 65602 C(34) C(36) 2.410(9) ? . . C(34) C(56) 3.561(9) ? . 65602 C(35) O(1) 3.208(7) ? . 65602 C(35) C(40) 2.497(9) ? . . C(35) C(41) 3.028(9) ? . . C(35) C(42) 3.03(1) ? . . C(36) C(41) 2.493(8) ? . . C(36) C(42) 2.49(1) ? . . C(38) C(39) 2.50(1) ? . . C(41) C(42) 2.47(1) ? . . C(43) C(45) 2.390(7) ? . . C(43) C(46) 2.753(7) ? . . C(43) C(47) 2.376(7) ? . . C(43) C(49) 2.547(7) ? . . C(43) C(50) 3.287(7) ? . . C(43) C(52) 2.562(7) ? . . C(43) C(53) 3.416(8) ? . . C(44) C(46) 2.434(8) ? . . C(44) C(47) 2.795(8) ? . . C(44) C(48) 2.475(7) ? . . C(44) C(50) 2.485(8) ? . . C(44) C(51) 2.540(7) ? . . C(45) C(47) 2.387(7) ? . . C(45) C(48) 2.828(7) ? . . C(45) C(49) 2.554(7) ? . . C(45) C(50) 3.376(7) ? . . C(45) C(51) 2.959(7) ? . . C(45) C(56) 3.59(1) ? . . C(46) C(48) 2.447(7) ? . . C(47) C(52) 2.535(8) ? . . C(47) C(53) 3.304(9) ? . . C(47) C(54) 3.033(8) ? . . C(48) C(53) 2.501(8) ? . . C(48) C(54) 2.560(8) ? . . C(50) C(51) 2.471(9) ? . . C(53) C(54) 2.52(1) ? . . C(56) C(33) 3.58(1) ? . 64602 C(56) C(34) 3.561(9) ? . 64602 Ag(1) H(13) 3.1297 ? . . Ag(1) H(30) 2.8838 ? . . Ag(2) H(40) 3.0068 ? . 64602 Ag(2) H(41) 3.5004 ? . 64602 Ag(2) H(42) 3.3284 ? . . Ag(2) H(43) 3.3052 ? . . Ag(2) H(49) 3.5731 ? . . Ag(2) H(59) 2.7680 ? . . Cl(1) H(2) 2.9030 ? . . Cl(1) H(15) 3.2467 ? . 65501 Cl(1) H(26) 3.3152 ? . . Cl(1) H(51) 3.5961 ? . . Cl(1) H(63) 3.1213 ? . . Cl(1) H(64) 3.5075 ? . . Cl(1) H(73) 2.1961 ? . . Cl(1) H(74) 2.2224 ? . . Cl(2) H(73) 2.1917 ? . . Cl(2) H(74) 2.2157 ? . . Cl(3) H(5) 3.5021 ? . 65501 Cl(3) H(16) 3.3808 ? . 65501 Cl(3) H(56) 3.2635 ? . . Cl(3) H(75) 2.2018 ? . . Cl(3) H(76) 2.1567 ? . . Cl(4) H(6) 3.3311 ? . . Cl(4) H(8) 3.3524 ? . . Cl(4) H(31) 2.9668 ? . . Cl(4) H(63) 3.2760 ? . . Cl(4) H(75) 2.2970 ? . . Cl(4) H(76) 2.2616 ? . . O(1) H(1) 2.3179 ? . . O(1) H(40) 2.8625 ? . 64602 O(1) H(41) 2.6381 ? . 64602 O(1) H(43) 3.0340 ? . . O(2) H(2) 2.2790 ? . . O(2) H(26) 3.5777 ? . . O(2) H(51) 3.4355 ? . . O(2) H(52) 2.7140 ? . . O(2) H(59) 3.3045 ? . . O(2) H(63) 3.2537 ? . . O(2) H(71) 3.5619 ? . 65602 O(3) H(19) 3.1109 ? . . O(3) H(37) 2.2612 ? . 55601 O(4) H(10) 2.6571 ? . . O(4) H(12) 3.4497 ? . . O(4) H(30) 3.4167 ? . . O(4) H(35) 2.7261 ? . . O(4) H(36) 3.2928 ? . . O(4) H(38) 2.2746 ? . 55601 O(4) H(67) 3.2551 ? . 55601 N(1) H(1) 1.8942 ? . . N(1) H(6) 2.5096 ? . . N(1) H(13) 2.3731 ? . . N(2) H(2) 1.9297 ? . . N(2) H(23) 2.4571 ? . . N(2) H(26) 3.4929 ? . . N(2) H(30) 2.4515 ? . . N(3) H(1) 2.5339 ? . . N(3) H(2) 2.4589 ? . . N(3) H(71) 3.2166 ? . 65602 N(4) H(28) 3.4873 ? . 64602 N(4) H(37) 1.9218 ? . . N(4) H(42) 2.3866 ? . . N(4) H(49) 2.4220 ? . . N(5) H(28) 3.4861 ? . 64602 N(5) H(38) 1.9144 ? . . N(5) H(40) 3.4595 ? . 64602 N(5) H(59) 2.4652 ? . . N(5) H(62) 3.0658 ? . . N(5) H(66) 2.5444 ? . . N(5) H(67) 3.4284 ? . . N(6) H(35) 3.3804 ? . . N(6) H(36) 3.4482 ? . . N(6) H(37) 2.4631 ? . 55601 N(6) H(38) 2.4657 ? . 55601 C(1) H(1) 2.0891 ? . . C(1) H(2) 2.0291 ? . . C(1) H(6) 3.4417 ? . . C(1) H(70) 3.5530 ? . 65602 C(1) H(71) 3.0155 ? . 65602 C(2) H(2) 3.4102 ? . . C(2) H(6) 2.6365 ? . . C(2) H(13) 3.0460 ? . . C(2) H(55) 3.3472 ? . 64602 C(2) H(70) 3.5453 ? . 65602 C(3) H(1) 3.4050 ? . . C(3) H(23) 2.7662 ? . . C(3) H(26) 3.1145 ? . . C(3) H(30) 3.1374 ? . . C(3) H(71) 3.1902 ? . 65602 C(4) H(1) 2.3646 ? . . C(4) H(3) 3.2453 ? . . C(4) H(5) 3.2677 ? . . C(4) H(6) 2.6252 ? . . C(4) H(9) 3.4757 ? . . C(4) H(13) 2.5439 ? . . C(4) H(19) 3.4590 ? . . C(4) H(53) 3.4051 ? . 64602 C(4) H(55) 3.2861 ? . 64602 C(5) H(1) 2.9386 ? . . C(5) H(3) 2.0486 ? . . C(5) H(4) 3.2595 ? . . C(5) H(6) 2.0375 ? . . C(5) H(7) 2.9175 ? . . C(5) H(8) 3.3231 ? . . C(5) H(9) 2.5278 ? . . C(5) H(10) 2.9657 ? . . C(5) H(11) 3.3154 ? . . C(5) H(12) 2.5182 ? . . C(5) H(53) 3.4590 ? . 64602 C(6) H(4) 1.9722 ? . . C(6) H(5) 3.2159 ? . . C(6) H(6) 3.3088 ? . . C(6) H(7) 3.1062 ? . . C(6) H(9) 2.9932 ? . . C(6) H(12) 2.6925 ? . . C(6) H(37) 3.3546 ? . 64602 C(6) H(53) 3.2266 ? . 64602 C(7) H(3) 1.9847 ? . . C(7) H(5) 2.0366 ? . . C(7) H(53) 3.0165 ? . 64602 C(8) H(3) 3.2186 ? . . C(8) H(4) 2.0163 ? . . C(8) H(13) 3.2768 ? . . C(8) H(16) 2.7017 ? . . C(8) H(17) 3.1082 ? . . C(8) H(19) 3.0266 ? . . C(8) H(53) 3.0110 ? . 64602 C(9) H(1) 3.3047 ? . . C(9) H(4) 3.2764 ? . . C(9) H(5) 2.0438 ? . . C(9) H(13) 1.9875 ? . . C(9) H(14) 2.9163 ? . . C(9) H(15) 3.2480 ? . . C(9) H(16) 2.5167 ? . . C(9) H(17) 2.8895 ? . . C(9) H(18) 3.2367 ? . . C(9) H(19) 2.5132 ? . . C(9) H(53) 3.2723 ? . 64602 C(9) H(55) 3.4527 ? . 64602 C(10) H(1) 3.2140 ? . . C(10) H(3) 2.6484 ? . . C(10) H(7) 2.0127 ? . . C(10) H(8) 2.0999 ? . . C(10) H(9) 2.0457 ? . . C(10) H(10) 2.0815 ? . . C(10) H(11) 2.0713 ? . . C(10) H(12) 2.0142 ? . . C(11) H(1) 3.5995 ? . . C(11) H(3) 2.9149 ? . . C(11) H(6) 2.0035 ? . . C(11) H(10) 3.2769 ? . . C(11) H(11) 2.4970 ? . . C(11) H(12) 2.9199 ? . . C(11) H(37) 3.3941 ? . 64602 C(11) H(48) 3.0916 ? . 64602 C(11) H(76) 3.0243 ? . . C(12) H(3) 2.9987 ? . . C(12) H(6) 2.0181 ? . . C(12) H(7) 2.4803 ? . . C(12) H(8) 2.9155 ? . . C(12) H(9) 3.2844 ? . . C(12) H(67) 3.3292 ? . 55601 C(13) H(5) 2.6658 ? . . C(13) H(14) 2.0386 ? . . C(13) H(15) 2.0475 ? . . C(13) H(16) 2.0533 ? . . C(13) H(17) 2.0552 ? . . C(13) H(18) 2.0522 ? . . C(13) H(19) 2.0794 ? . . C(13) H(68) 3.3932 ? . 65602 C(13) H(70) 3.5227 ? . 65602 C(14) H(5) 2.9730 ? . . C(14) H(13) 2.0227 ? . . C(14) H(17) 2.5651 ? . . C(14) H(18) 2.8917 ? . . C(14) H(19) 3.3282 ? . . C(14) H(54) 3.4678 ? . 64602 C(14) H(63) 3.5840 ? . 45501 C(14) H(64) 3.5639 ? . 45501 C(14) H(65) 3.2119 ? . 45501 C(14) H(70) 3.3314 ? . 65602 C(15) H(5) 2.9405 ? . . C(15) H(13) 2.0305 ? . . C(15) H(14) 3.2706 ? . . C(15) H(15) 2.5188 ? . . C(15) H(16) 3.0060 ? . . C(15) H(31) 3.5585 ? . 45501 C(15) H(33) 3.4105 ? . 45501 C(16) H(2) 2.4389 ? . . C(16) H(20) 3.2577 ? . . C(16) H(22) 3.2359 ? . . C(16) H(23) 2.5777 ? . . C(16) H(26) 3.2112 ? . . C(16) H(30) 2.5960 ? . . C(16) H(33) 3.5908 ? . . C(16) H(36) 3.4574 ? . . C(16) H(73) 3.0423 ? . . C(17) H(2) 2.9908 ? . . C(17) H(20) 2.0157 ? . . C(17) H(21) 3.2406 ? . . C(17) H(23) 2.0221 ? . . C(17) H(24) 2.9449 ? . . C(17) H(25) 3.3051 ? . . C(17) H(26) 2.5324 ? . . C(17) H(27) 2.8909 ? . . C(17) H(28) 3.3304 ? . . C(17) H(29) 2.5179 ? . . C(17) H(73) 3.0080 ? . . C(18) H(21) 2.0201 ? . . C(18) H(22) 3.2396 ? . . C(18) H(23) 3.2463 ? . . C(18) H(24) 3.3000 ? . . C(18) H(26) 3.2626 ? . . C(18) H(27) 3.4450 ? . . C(18) H(29) 2.4633 ? . . C(18) H(73) 2.8351 ? . . C(19) H(20) 2.0205 ? . . C(19) H(22) 2.0287 ? . . C(19) H(73) 2.7125 ? . . C(20) H(20) 3.2396 ? . . C(20) H(21) 2.0171 ? . . C(20) H(30) 3.2701 ? . . C(20) H(33) 2.5949 ? . . C(20) H(34) 3.0442 ? . . C(20) H(36) 2.9058 ? . . C(20) H(73) 2.8388 ? . . C(21) H(2) 3.4058 ? . . C(21) H(21) 3.2361 ? . . C(21) H(22) 2.0009 ? . . C(21) H(30) 2.0521 ? . . C(21) H(31) 2.9009 ? . . C(21) H(32) 3.2463 ? . . C(21) H(33) 2.4473 ? . . C(21) H(34) 2.8980 ? . . C(21) H(35) 3.2439 ? . . C(21) H(36) 2.4934 ? . . C(21) H(73) 3.0050 ? . . C(22) H(2) 3.1518 ? . . C(22) H(20) 2.6511 ? . . C(22) H(24) 2.0310 ? . . C(22) H(25) 2.0525 ? . . C(22) H(26) 2.0325 ? . . C(22) H(27) 2.0027 ? . . C(22) H(28) 2.1095 ? . . C(22) H(29) 2.0543 ? . . C(22) H(66) 3.2170 ? . 65602 C(22) H(71) 3.2834 ? . 65602 C(23) H(2) 3.0752 ? . . C(23) H(20) 3.1862 ? . . C(23) H(23) 1.9984 ? . . C(23) H(27) 3.2072 ? . . C(23) H(28) 2.5528 ? . . C(23) H(29) 2.9736 ? . . C(23) H(42) 3.3963 ? . 65602 C(23) H(47) 3.5515 ? . 65602 C(23) H(50) 3.4618 ? . . C(23) H(52) 3.1142 ? . . C(23) H(66) 3.2752 ? . 65602 C(23) H(71) 3.1868 ? . 65602 C(24) H(20) 2.7138 ? . . C(24) H(23) 2.0627 ? . . C(24) H(24) 2.5054 ? . . C(24) H(25) 2.8925 ? . . C(24) H(26) 3.2776 ? . . C(24) H(42) 3.5698 ? . 65602 C(24) H(66) 3.1969 ? . 65602 C(24) H(67) 3.2320 ? . 65602 C(25) H(22) 2.6248 ? . . C(25) H(31) 2.0596 ? . . C(25) H(32) 2.0281 ? . . C(25) H(33) 2.0234 ? . . C(25) H(34) 2.0221 ? . . C(25) H(35) 2.0095 ? . . C(25) H(36) 2.0439 ? . . C(26) H(17) 2.9696 ? . 65501 C(26) H(22) 2.8988 ? . . C(26) H(30) 2.0104 ? . . C(26) H(34) 2.5167 ? . . C(26) H(35) 2.8979 ? . . C(26) H(36) 3.2838 ? . . C(27) H(22) 2.8197 ? . . C(27) H(30) 2.0275 ? . . C(27) H(31) 3.2780 ? . . C(27) H(32) 2.5060 ? . . C(27) H(33) 2.9133 ? . . C(27) H(46) 3.5993 ? . 65601 C(28) H(27) 3.4920 ? . 64602 C(28) H(28) 2.8016 ? . 64602 C(28) H(37) 2.0078 ? . . C(28) H(38) 2.0398 ? . . C(28) H(49) 3.4364 ? . . C(29) H(9) 3.5827 ? . 65602 C(29) H(28) 3.0907 ? . 64602 C(29) H(38) 3.3432 ? . . C(29) H(42) 2.9910 ? . . C(29) H(49) 2.6473 ? . . C(30) H(28) 3.1159 ? . 64602 C(30) H(37) 3.3515 ? . . C(30) H(59) 3.1285 ? . . C(30) H(62) 2.8482 ? . . C(30) H(66) 2.9163 ? . . C(30) H(67) 2.9516 ? . . C(31) H(9) 3.0510 ? . 65602 C(31) H(37) 2.4757 ? . . C(31) H(39) 3.2189 ? . . C(31) H(41) 3.2493 ? . . C(31) H(42) 2.5628 ? . . C(31) H(43) 3.5844 ? . . C(31) H(45) 3.5787 ? . . C(31) H(48) 3.4859 ? . . C(31) H(49) 2.5703 ? . . C(31) H(52) 3.3887 ? . . C(32) H(9) 3.1661 ? . 65602 C(32) H(37) 3.3158 ? . . C(32) H(39) 2.0168 ? . . C(32) H(40) 3.2659 ? . . C(32) H(42) 2.0473 ? . . C(32) H(43) 2.9085 ? . . C(32) H(44) 3.3138 ? . . C(32) H(45) 2.4961 ? . . C(32) H(46) 2.9011 ? . . C(32) H(47) 3.2664 ? . . C(32) H(48) 2.4946 ? . . C(32) H(72) 3.2069 ? . 65602 C(33) H(8) 3.4297 ? . 65602 C(33) H(9) 3.3317 ? . 65602 C(33) H(40) 2.0387 ? . . C(33) H(41) 3.2544 ? . . C(33) H(42) 3.2846 ? . . C(33) H(45) 2.6866 ? . . C(33) H(46) 3.0808 ? . . C(33) H(48) 2.9010 ? . . C(33) H(72) 2.7251 ? . 65602 C(33) H(75) 3.4451 ? . 65602 C(33) H(76) 2.8925 ? . 65602 C(34) H(9) 3.3744 ? . 65602 C(34) H(39) 2.0195 ? . . C(34) H(41) 2.0489 ? . . C(34) H(72) 2.9906 ? . 65602 C(34) H(75) 3.2342 ? . 65602 C(34) H(76) 2.9977 ? . 65602 C(35) H(1) 3.3918 ? . 65602 C(35) H(9) 3.2723 ? . 65602 C(35) H(39) 3.2615 ? . . C(35) H(40) 2.0660 ? . . C(35) H(49) 3.2380 ? . . C(35) H(50) 3.0777 ? . . C(35) H(52) 2.9511 ? . . C(35) H(53) 3.5957 ? . . C(35) H(55) 2.6409 ? . . C(36) H(9) 3.0973 ? . 65602 C(36) H(37) 3.0542 ? . . C(36) H(40) 3.2624 ? . . C(36) H(41) 2.0040 ? . . C(36) H(49) 2.0217 ? . . C(36) H(50) 2.9169 ? . . C(36) H(51) 3.2406 ? . . C(36) H(52) 2.5163 ? . . C(36) H(53) 2.8763 ? . . C(36) H(54) 3.2606 ? . . C(36) H(55) 2.5301 ? . . C(37) H(24) 3.1124 ? . 64602 C(37) H(39) 2.6728 ? . . C(37) H(43) 2.0323 ? . . C(37) H(44) 2.0769 ? . . C(37) H(45) 2.0283 ? . . C(37) H(46) 2.0022 ? . . C(37) H(47) 2.0388 ? . . C(37) H(48) 2.0494 ? . . C(38) H(24) 3.3277 ? . 64602 C(38) H(39) 3.0240 ? . . C(38) H(42) 2.0440 ? . . C(38) H(46) 2.4647 ? . . C(38) H(47) 2.9091 ? . . C(38) H(48) 3.2763 ? . . C(38) H(50) 3.4098 ? . 64602 C(38) H(60) 3.1350 ? . 45501 C(38) H(72) 3.3165 ? . 65602 C(39) H(24) 3.2991 ? . 64602 C(39) H(34) 3.0269 ? . 45401 C(39) H(39) 2.8428 ? . . C(39) H(42) 2.0088 ? . . C(39) H(43) 3.2488 ? . . C(39) H(44) 2.5414 ? . . C(39) H(45) 2.9145 ? . . C(39) H(60) 3.4104 ? . 45501 C(40) H(37) 3.2950 ? . . C(40) H(41) 2.6407 ? . . C(40) H(50) 2.0482 ? . . C(40) H(51) 2.0101 ? . . C(40) H(52) 2.0633 ? . . C(40) H(53) 1.9982 ? . . C(40) H(54) 2.0291 ? . . C(40) H(55) 2.0688 ? . . C(41) H(25) 3.4261 ? . . C(41) H(26) 3.3036 ? . . C(41) H(41) 2.8802 ? . . C(41) H(49) 2.0396 ? . . C(41) H(53) 3.2093 ? . . C(41) H(54) 2.4555 ? . . C(41) H(55) 2.9266 ? . . C(42) H(1) 3.4025 ? . 65602 C(42) H(16) 3.3575 ? . 65602 C(42) H(41) 2.8647 ? . . C(42) H(49) 2.0509 ? . . C(42) H(50) 2.4736 ? . . C(42) H(51) 2.8409 ? . . C(42) H(52) 3.2577 ? . . C(43) H(38) 2.4057 ? . . C(43) H(40) 3.1105 ? . 64602 C(43) H(56) 3.2551 ? . . C(43) H(58) 3.2300 ? . . C(43) H(59) 2.6305 ? . . C(43) H(62) 2.9458 ? . . C(43) H(66) 2.6257 ? . . C(43) H(67) 3.4798 ? . . C(43) H(69) 3.4507 ? . . C(44) H(38) 3.2213 ? . . C(44) H(56) 2.0478 ? . . C(44) H(57) 3.2948 ? . . C(44) H(59) 2.0291 ? . . C(44) H(60) 2.8896 ? . . C(44) H(61) 3.2542 ? . . C(44) H(62) 2.4784 ? . . C(44) H(63) 2.9583 ? . . C(44) H(64) 3.2947 ? . . C(44) H(65) 2.5427 ? . . C(44) H(75) 3.0234 ? . . C(45) H(57) 2.0524 ? . . C(45) H(58) 3.2395 ? . . C(45) H(59) 3.2559 ? . . C(45) H(60) 3.4127 ? . . C(45) H(62) 3.4051 ? . . C(45) H(63) 3.4041 ? . . C(45) H(65) 2.4787 ? . . C(45) H(75) 2.8612 ? . . C(46) H(39) 3.3396 ? . 64602 C(46) H(56) 2.0353 ? . . C(46) H(58) 2.0059 ? . . C(46) H(75) 3.4138 ? . . C(47) H(39) 3.1065 ? . 64602 C(47) H(56) 3.2392 ? . . C(47) H(57) 2.0045 ? . . C(47) H(66) 3.2666 ? . . C(47) H(69) 2.9696 ? . . C(47) H(70) 3.1048 ? . . C(47) H(72) 2.8559 ? . . C(48) H(38) 2.9929 ? . . C(48) H(39) 3.5413 ? . 64602 C(48) H(40) 3.1850 ? . 64602 C(48) H(57) 3.2922 ? . . C(48) H(58) 2.0454 ? . . C(48) H(66) 2.0054 ? . . C(48) H(67) 2.9172 ? . . C(48) H(68) 3.2581 ? . . C(48) H(69) 2.5091 ? . . C(48) H(70) 2.9248 ? . . C(48) H(71) 3.3164 ? . . C(48) H(72) 2.6470 ? . . C(49) H(38) 3.5993 ? . . C(49) H(56) 2.7161 ? . . C(49) H(60) 2.0493 ? . . C(49) H(61) 2.0526 ? . . C(49) H(62) 2.0526 ? . . C(49) H(63) 2.0433 ? . . C(49) H(64) 2.0244 ? . . C(49) H(65) 2.0050 ? . . C(49) H(75) 3.5190 ? . . C(50) H(38) 3.3374 ? . . C(50) H(44) 3.3743 ? . 65501 C(50) H(46) 3.1670 ? . 65501 C(50) H(56) 3.4742 ? . . C(50) H(59) 2.0387 ? . . C(50) H(63) 3.2492 ? . . C(50) H(64) 2.4456 ? . . C(50) H(65) 2.8715 ? . . C(51) H(14) 3.4393 ? . 65501 C(51) H(15) 3.3972 ? . 65501 C(51) H(16) 3.5053 ? . 65501 C(51) H(56) 2.6470 ? . . C(51) H(59) 1.9909 ? . . C(51) H(60) 2.4962 ? . . C(51) H(61) 2.8315 ? . . C(51) H(62) 3.2574 ? . . C(51) H(75) 3.2764 ? . . C(52) H(23) 3.2578 ? . 64602 C(52) H(25) 3.3578 ? . 64602 C(52) H(38) 3.2444 ? . . C(52) H(58) 2.6655 ? . . C(52) H(67) 2.0763 ? . . C(52) H(68) 2.0528 ? . . C(52) H(69) 2.0584 ? . . C(52) H(70) 1.9581 ? . . C(52) H(71) 2.0694 ? . . C(52) H(72) 2.0993 ? . . C(53) H(12) 3.0398 ? . 55401 C(53) H(13) 3.3804 ? . 64602 C(53) H(18) 3.4803 ? . 64602 C(53) H(23) 3.2505 ? . 64602 C(53) H(27) 3.1946 ? . 64602 C(53) H(38) 3.1002 ? . . C(53) H(58) 3.3481 ? . . C(53) H(66) 2.0415 ? . . C(53) H(70) 2.4148 ? . . C(53) H(71) 2.9113 ? . . C(53) H(72) 3.3234 ? . . C(54) H(14) 3.5259 ? . 64602 C(54) H(23) 3.2407 ? . 64602 C(54) H(25) 3.1971 ? . 64602 C(54) H(45) 3.2707 ? . 64602 C(54) H(58) 2.7132 ? . . C(54) H(66) 1.9719 ? . . C(54) H(67) 3.2583 ? . . C(54) H(68) 2.4753 ? . . C(54) H(69) 2.9897 ? . . C(55) H(26) 3.5133 ? . . C(56) H(8) 2.9715 ? . . C(56) H(39) 3.1745 ? . 64602 C(56) H(40) 3.1762 ? . 64602 C(56) H(56) 3.5497 ? . . C(56) H(63) 3.4069 ? . . H(1) C(35) 3.3918 ? . 64602 H(1) C(42) 3.4025 ? . 64602 H(5) Cl(3) 3.5021 ? . 45501 H(8) C(33) 3.4297 ? . 64602 H(9) C(29) 3.5827 ? . 64602 H(9) C(31) 3.0510 ? . 64602 H(9) C(32) 3.1661 ? . 64602 H(9) C(33) 3.3317 ? . 64602 H(9) C(34) 3.3744 ? . 64602 H(9) C(35) 3.2723 ? . 64602 H(9) C(36) 3.0973 ? . 64602 H(12) C(53) 3.0398 ? . 55601 H(13) C(53) 3.3804 ? . 65602 H(14) C(51) 3.4393 ? . 45501 H(14) C(54) 3.5259 ? . 65602 H(15) Cl(1) 3.2467 ? . 45501 H(15) C(51) 3.3972 ? . 45501 H(16) Cl(3) 3.3808 ? . 45501 H(16) C(42) 3.3575 ? . 64602 H(16) C(51) 3.5053 ? . 45501 H(17) C(26) 2.9696 ? . 45501 H(18) C(53) 3.4803 ? . 65602 H(23) C(52) 3.2578 ? . 65602 H(23) C(53) 3.2505 ? . 65602 H(23) C(54) 3.2407 ? . 65602 H(24) C(37) 3.1124 ? . 65602 H(24) C(38) 3.3277 ? . 65602 H(24) C(39) 3.2991 ? . 65602 H(25) C(52) 3.3578 ? . 65602 H(25) C(54) 3.1971 ? . 65602 H(27) C(28) 3.4920 ? . 65602 H(27) C(53) 3.1946 ? . 65602 H(28) N(4) 3.4873 ? . 65602 H(28) N(5) 3.4861 ? . 65602 H(28) C(28) 2.8016 ? . 65602 H(28) C(29) 3.0907 ? . 65602 H(28) C(30) 3.1159 ? . 65602 H(31) C(15) 3.5585 ? . 65501 H(33) C(15) 3.4105 ? . 65501 H(33) C(16) 3.5908 ? . . H(33) C(20) 2.5949 ? . . H(33) C(21) 2.4473 ? . . H(33) C(25) 2.0234 ? . . H(33) C(27) 2.9133 ? . . H(34) C(39) 3.0269 ? . 65601 H(37) O(3) 2.2612 ? . 55401 H(37) N(6) 2.4631 ? . 55401 H(37) C(6) 3.3546 ? . 65602 H(37) C(11) 3.3941 ? . 65602 H(38) O(4) 2.2746 ? . 55401 H(38) N(6) 2.4657 ? . 55401 H(39) C(46) 3.3396 ? . 65602 H(39) C(47) 3.1065 ? . 65602 H(39) C(48) 3.5413 ? . 65602 H(39) C(56) 3.1745 ? . 65602 H(40) Ag(2) 3.0068 ? . 65602 H(40) O(1) 2.8625 ? . 65602 H(40) N(5) 3.4595 ? . 65602 H(40) C(43) 3.1105 ? . 65602 H(40) C(48) 3.1850 ? . 65602 H(40) C(56) 3.1762 ? . 65602 H(41) Ag(2) 3.5004 ? . 65602 H(41) O(1) 2.6381 ? . 65602 H(42) C(23) 3.3963 ? . 64602 H(42) C(24) 3.5698 ? . 64602 H(44) C(50) 3.3743 ? . 45501 H(45) C(54) 3.2707 ? . 65602 H(46) C(27) 3.5993 ? . 45401 H(46) C(50) 3.1670 ? . 45501 H(47) C(23) 3.5515 ? . 64602 H(48) C(11) 3.0916 ? . 65602 H(50) C(38) 3.4098 ? . 65602 H(53) C(4) 3.4051 ? . 65602 H(53) C(5) 3.4590 ? . 65602 H(53) C(6) 3.2266 ? . 65602 H(53) C(7) 3.0165 ? . 65602 H(53) C(8) 3.0110 ? . 65602 H(53) C(9) 3.2723 ? . 65602 H(54) C(14) 3.4678 ? . 65602 H(55) C(2) 3.3472 ? . 65602 H(55) C(4) 3.2861 ? . 65602 H(55) C(9) 3.4527 ? . 65602 H(60) C(38) 3.1350 ? . 65501 H(60) C(39) 3.4104 ? . 65501 H(63) C(14) 3.5840 ? . 65501 H(64) C(14) 3.5639 ? . 65501 H(65) C(14) 3.2119 ? . 65501 H(66) C(22) 3.2170 ? . 64602 H(66) C(23) 3.2752 ? . 64602 H(66) C(24) 3.1969 ? . 64602 H(67) O(4) 3.2551 ? . 55401 H(67) C(12) 3.3292 ? . 55401 H(67) C(24) 3.2320 ? . 64602 H(68) C(13) 3.3932 ? . 64602 H(70) C(1) 3.5530 ? . 64602 H(70) C(2) 3.5453 ? . 64602 H(70) C(13) 3.5227 ? . 64602 H(70) C(14) 3.3314 ? . 64602 H(71) O(2) 3.5619 ? . 64602 H(71) N(3) 3.2166 ? . 64602 H(71) C(1) 3.0155 ? . 64602 H(71) C(3) 3.1902 ? . 64602 H(71) C(22) 3.2834 ? . 64602 H(71) C(23) 3.1868 ? . 64602 H(72) C(32) 3.2069 ? . 64602 H(72) C(33) 2.7251 ? . 64602 H(72) C(34) 2.9906 ? . 64602 H(72) C(38) 3.3165 ? . 64602 H(75) C(33) 3.4451 ? . 64602 H(75) C(34) 3.2342 ? . 64602 H(76) C(33) 2.8925 ? . 64602 H(76) C(34) 2.9977 ? . 64602 loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 N(1) Ag(1) O(3) N(6) 78.4(3) ? . . . . N(2) Ag(1) O(3) N(6) -108.2(3) ? . . . . O(3) Ag(1) N(1) C(2) 174.7(4) ? . . . . O(3) Ag(1) N(1) C(4) -13.0(4) ? . . . . N(2) Ag(1) N(1) C(2) -1.4(4) ? . . . . N(2) Ag(1) N(1) C(4) 170.8(3) ? . . . . O(3) Ag(1) N(2) C(3) -174.8(3) ? . . . . O(3) Ag(1) N(2) C(16) 11.9(4) ? . . . . N(1) Ag(1) N(2) C(3) 0.0(3) ? . . . . N(1) Ag(1) N(2) C(16) -173.3(3) ? . . . . N(4) Ag(2) O(1) N(3) -85.1(3) ? . . . . N(5) Ag(2) O(1) N(3) 111.2(3) ? . . . . O(1) Ag(2) N(4) C(29) -172.2(4) ? . . . . O(1) Ag(2) N(4) C(31) 16.0(4) ? . . . . N(5) Ag(2) N(4) C(29) -1.5(4) ? . . . . N(5) Ag(2) N(4) C(31) -173.3(3) ? . . . . O(1) Ag(2) N(5) C(30) 170.6(3) ? . . . . O(1) Ag(2) N(5) C(43) -20.5(4) ? . . . . N(4) Ag(2) N(5) C(30) 3.2(4) ? . . . . N(4) Ag(2) N(5) C(43) 172.1(3) ? . . . . Ag(2) O(1) N(3) O(2) -1.1(5) ? . . . . Ag(2) O(1) N(3) C(1) 177.4(4) ? . . . . Ag(1) O(3) N(6) O(4) -5.6(5) ? . . . . Ag(1) N(1) C(2) C(1) -2.1(7) ? . . . . C(4) N(1) C(2) C(1) -174.4(4) ? . . . . Ag(1) N(1) C(4) C(5) -95.7(6) ? . . . . Ag(1) N(1) C(4) C(9) 76.7(6) ? . . . . C(2) N(1) C(4) C(5) 77.4(6) ? . . . . C(2) N(1) C(4) C(9) -110.2(6) ? . . . . Ag(1) N(2) C(3) C(1) 5.2(7) ? . . . . C(16) N(2) C(3) C(1) 178.5(4) ? . . . . Ag(1) N(2) C(16) C(17) -108.1(6) ? . . . . Ag(1) N(2) C(16) C(21) 65.4(6) ? . . . . C(3) N(2) C(16) C(17) 78.1(7) ? . . . . C(3) N(2) C(16) C(21) -108.4(6) ? . . . . O(1) N(3) C(1) C(2) 6.7(6) ? . . . . O(1) N(3) C(1) C(3) -177.1(4) ? . . . . O(2) N(3) C(1) C(2) -174.8(4) ? . . . . O(2) N(3) C(1) C(3) 1.3(7) ? . . . . Ag(2) N(4) C(29) C(28) 3.7(8) ? . . . . C(31) N(4) C(29) C(28) 175.2(4) ? . . . . Ag(2) N(4) C(31) C(32) -85.1(5) ? . . . . Ag(2) N(4) C(31) C(36) 95.9(5) ? . . . . C(29) N(4) C(31) C(32) 102.5(6) ? . . . . C(29) N(4) C(31) C(36) -76.5(6) ? . . . . Ag(2) N(5) C(30) C(28) -7.3(7) ? . . . . C(43) N(5) C(30) C(28) -176.2(4) ? . . . . Ag(2) N(5) C(43) C(44) -71.5(6) ? . . . . Ag(2) N(5) C(43) C(48) 108.1(6) ? . . . . C(30) N(5) C(43) C(44) 98.7(6) ? . . . . C(30) N(5) C(43) C(48) -81.8(7) ? . . . . N(3) C(1) C(2) N(1) -175.8(5) ? . . . . C(3) C(1) C(2) N(1) 8.7(8) ? . . . . N(3) C(1) C(3) N(2) 173.9(5) ? . . . . C(2) C(1) C(3) N(2) -10.6(8) ? . . . . N(1) C(4) C(5) C(6) 177.1(5) ? . . . . N(1) C(4) C(5) C(10) -2.3(9) ? . . . . C(9) C(4) C(5) C(6) 5.0(9) ? . . . . C(9) C(4) C(5) C(10) -174.4(6) ? . . . . N(1) C(4) C(9) C(8) -178.6(6) ? . . . . N(1) C(4) C(9) C(13) 4.7(9) ? . . . . C(5) C(4) C(9) C(8) -6.4(9) ? . . . . C(5) C(4) C(9) C(13) 176.8(6) ? . . . . C(4) C(5) C(6) C(7) -1.8(9) ? . . . . C(10) C(5) C(6) C(7) 177.6(6) ? . . . . C(4) C(5) C(10) C(11) -119.2(6) ? . . . . C(4) C(5) C(10) C(12) 115.3(6) ? . . . . C(6) C(5) C(10) C(11) 61.5(8) ? . . . . C(6) C(5) C(10) C(12) -64.1(7) ? . . . . C(5) C(6) C(7) C(8) 0.2(8) ? . . . . C(6) C(7) C(8) C(9) -1(1) ? . . . . C(7) C(8) C(9) C(4) 4(1) ? . . . . C(7) C(8) C(9) C(13) -178.6(6) ? . . . . C(4) C(9) C(13) C(14) 114.5(7) ? . . . . C(4) C(9) C(13) C(15) -119.8(7) ? . . . . C(8) C(9) C(13) C(14) -62.1(9) ? . . . . C(8) C(9) C(13) C(15) 63.6(8) ? . . . . N(2) C(16) C(17) C(18) 178.2(6) ? . . . . N(2) C(16) C(17) C(22) -2(1) ? . . . . C(21) C(16) C(17) C(18) 4(1) ? . . . . C(21) C(16) C(17) C(22) -176.0(6) ? . . . . N(2) C(16) C(21) C(20) -177.6(6) ? . . . . N(2) C(16) C(21) C(25) 3.7(9) ? . . . . C(17) C(16) C(21) C(20) -4.0(9) ? . . . . C(17) C(16) C(21) C(25) 177.3(6) ? . . . . C(16) C(17) C(18) C(19) 0(1) ? . . . . C(22) C(17) C(18) C(19) 179.8(6) ? . . . . C(16) C(17) C(22) C(23) -98.4(7) ? . . . . C(16) C(17) C(22) C(24) 137.2(7) ? . . . . C(18) C(17) C(22) C(23) 81.0(8) ? . . . . C(18) C(17) C(22) C(24) -43.4(9) ? . . . . C(17) C(18) C(19) C(20) -3(1) ? . . . . C(18) C(19) C(20) C(21) 4(1) ? . . . . C(19) C(20) C(21) C(16) -0.5(9) ? . . . . C(19) C(20) C(21) C(25) 178.3(6) ? . . . . C(16) C(21) C(25) C(26) 113.9(6) ? . . . . C(16) C(21) C(25) C(27) -122.4(5) ? . . . . C(20) C(21) C(25) C(26) -64.9(7) ? . . . . C(20) C(21) C(25) C(27) 58.9(6) ? . . . . C(30) C(28) C(29) N(4) -7.5(9) ? . . . . C(29) C(28) C(30) N(5) 9.5(9) ? . . . . N(4) C(31) C(32) C(33) 178.4(5) ? . . . . N(4) C(31) C(32) C(37) 2.6(8) ? . . . . C(36) C(31) C(32) C(33) -2.7(9) ? . . . . C(36) C(31) C(32) C(37) -178.4(5) ? . . . . N(4) C(31) C(36) C(35) -178.2(6) ? . . . . N(4) C(31) C(36) C(40) -3.7(8) ? . . . . C(32) C(31) C(36) C(35) 2.9(9) ? . . . . C(32) C(31) C(36) C(40) 177.4(6) ? . . . . C(31) C(32) C(33) C(34) 2.5(9) ? . . . . C(37) C(32) C(33) C(34) 178.2(6) ? . . . . C(31) C(32) C(37) C(38) 110.6(6) ? . . . . C(31) C(32) C(37) C(39) -125.9(6) ? . . . . C(33) C(32) C(37) C(38) -65.0(6) ? . . . . C(33) C(32) C(37) C(39) 58.4(8) ? . . . . C(32) C(33) C(34) C(35) -2(1) ? . . . . C(33) C(34) C(35) C(36) 2(1) ? . . . . C(34) C(35) C(36) C(31) -2.8(9) ? . . . . C(34) C(35) C(36) C(40) -177.4(6) ? . . . . C(31) C(36) C(40) C(41) -113.7(7) ? . . . . C(31) C(36) C(40) C(42) 125.6(6) ? . . . . C(35) C(36) C(40) C(41) 60.6(7) ? . . . . C(35) C(36) C(40) C(42) -60.0(8) ? . . . . N(5) C(43) C(44) C(45) 175.7(6) ? . . . . N(5) C(43) C(44) C(49) -4.9(9) ? . . . . C(48) C(43) C(44) C(45) -3(1) ? . . . . C(48) C(43) C(44) C(49) 175.6(6) ? . . . . N(5) C(43) C(48) C(47) -177.2(6) ? . . . . N(5) C(43) C(48) C(52) 3(1) ? . . . . C(44) C(43) C(48) C(47) 2(1) ? . . . . C(44) C(43) C(48) C(52) -176.8(7) ? . . . . C(43) C(44) C(45) C(46) 2.3(9) ? . . . . C(49) C(44) C(45) C(46) -177.2(6) ? . . . . C(43) C(44) C(49) C(50) -85.2(6) ? . . . . C(43) C(44) C(49) C(51) 151.7(6) ? . . . . C(45) C(44) C(49) C(50) 94.3(6) ? . . . . C(45) C(44) C(49) C(51) -28.9(8) ? . . . . C(44) C(45) C(46) C(47) 0(1) ? . . . . C(45) C(46) C(47) C(48) -2(1) ? . . . . C(46) C(47) C(48) C(43) 0(1) ? . . . . C(46) C(47) C(48) C(52) -179.9(5) ? . . . . C(43) C(48) C(52) C(53) 94.1(7) ? . . . . C(43) C(48) C(52) C(54) -138.7(7) ? . . . . C(47) C(48) C(52) C(53) -85.0(7) ? . . . . C(47) C(48) C(52) C(54) 42.2(9) ? . . . .
1100784.cif	#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100784.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100784 loop_ _publ_author_name 'Reger, Daniel L.' 'Semeniuc, Radu F.' 'Smith, Mark D.' _publ_section_title ; Supramolecular networks of silver(i) and iron(ii) complexes of the third generation tris(pyrazolyl)methane ligand Ph2(O)POCH2C(pz)3 (pz = pyrazolyl ring) ; _journal_issue 17 _journal_name_full 'Dalton Transactions' _journal_page_first 2253 _journal_page_last 2260 _journal_paper_doi 10.1039/B719023A _journal_year 2008 _chemical_formula_moiety ; C46 H42 Ag2 N12 O4 P2, 2(C4 H8 O), 2(B F4) ; _chemical_formula_sum 'C54 H58 Ag2 B2 F8 N12 O6 P2' _chemical_formula_weight 1422.42 _chemical_name_systematic ; ? ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 109.1080(10) _cell_angle_beta 98.4090(10) _cell_angle_gamma 102.7470(10) _cell_formula_units_Z 1 _cell_length_a 10.9754(8) _cell_length_b 11.4045(8) _cell_length_c 12.9314(9) _cell_measurement_reflns_used 8191 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 26.352 _cell_measurement_theta_min 2.347 _cell_volume 1449.22(18) _computing_cell_refinement 'SAINT+ NT V6.22 (Bruker, 2001)' _computing_data_collection 'SMART NT V5.625 (Bruker, 1998)' _computing_data_reduction 'SAINT+ NT V6.22' _computing_molecular_graphics 'SHELXTL V6.1 (Sheldrick, 2000)' _computing_publication_material 'SHELXTL V6.1' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0272 _diffrn_reflns_av_sigmaI/netI 0.0381 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 13216 _diffrn_reflns_theta_full 26.36 _diffrn_reflns_theta_max 26.36 _diffrn_reflns_theta_min 1.72 _diffrn_standards_decay_% 0 _exptl_absorpt_coefficient_mu 0.818 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.8619 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS, Bruker, 2001)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.630 _exptl_crystal_density_method 'not measured' _exptl_crystal_description parallelipiped _exptl_crystal_F_000 720 _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.06 _refine_diff_density_max 1.052 _refine_diff_density_min -0.777 _refine_diff_density_rms 0.083 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 388 _refine_ls_number_reflns 5923 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.047 _refine_ls_R_factor_all 0.0455 _refine_ls_R_factor_gt 0.0404 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0502P)^2^+1.3895P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0993 _refine_ls_wR_factor_ref 0.1027 _reflns_number_gt 5283 _reflns_number_total 5923 _reflns_threshold_expression >2sigma(I) _cod_data_source_file B719023A.txt _cod_data_source_block rs4001s _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_database_code 1100784 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.01038(2) 0.61081(2) 0.439324(18) 0.03641(10) Uani 1 1 d . . . P1 P 0.24883(7) 0.14220(7) 0.09866(6) 0.02744(17) Uani 1 1 d . . . C1 C 0.0132(2) 0.2717(2) 0.2750(2) 0.0212(5) Uani 1 1 d . . . C2 C 0.0548(3) 0.2193(3) 0.1643(2) 0.0248(6) Uani 1 1 d . . . H2A H -0.0147 0.1447 0.1082 0.030 Uiso 1 1 calc R . . H2B H 0.0749 0.2875 0.1326 0.030 Uiso 1 1 calc R . . C11 C 0.2172(3) 0.3706(3) 0.4270(2) 0.0288(6) Uani 1 1 d . . . H11 H 0.2200 0.2989 0.4484 0.035 Uiso 1 1 calc R . . C12 C 0.3115(3) 0.4850(3) 0.4618(3) 0.0378(7) Uani 1 1 d . . . H12 H 0.3923 0.5099 0.5133 0.045 Uiso 1 1 calc R . . C13 C 0.2646(3) 0.5576(3) 0.4060(3) 0.0378(7) Uani 1 1 d . . . H13 H 0.3104 0.6426 0.4146 0.045 Uiso 1 1 calc R . . C21 C -0.2021(3) 0.2461(3) 0.1602(2) 0.0315(6) Uani 1 1 d . . . H21 H -0.2075 0.1696 0.0990 0.038 Uiso 1 1 calc R . . C22 C -0.2956(3) 0.3068(3) 0.1754(3) 0.0335(7) Uani 1 1 d . . . H22 H -0.3781 0.2826 0.1267 0.040 Uiso 1 1 calc R . . C23 C -0.2451(3) 0.4109(3) 0.2764(3) 0.0323(6) Uani 1 1 d . . . H23 H -0.2898 0.4710 0.3084 0.039 Uiso 1 1 calc R . . C31 C -0.0410(3) 0.0427(3) 0.2706(2) 0.0278(6) Uani 1 1 d . . . H31 H -0.0293 -0.0012 0.1981 0.033 Uiso 1 1 calc R . . C32 C -0.0838(3) -0.0134(3) 0.3414(3) 0.0328(6) Uani 1 1 d . . . H32 H -0.1068 -0.1030 0.3294 0.039 Uiso 1 1 calc R . . C33 C -0.0867(3) 0.0890(3) 0.4359(2) 0.0299(6) Uani 1 1 d . . . H33 H -0.1131 0.0790 0.5000 0.036 Uiso 1 1 calc R . . C41 C 0.3030(3) 0.2873(3) 0.0721(2) 0.0313(6) Uani 1 1 d . . . C42 C 0.2806(3) 0.2829(4) -0.0383(3) 0.0414(8) Uani 1 1 d . . . H42 H 0.2440 0.2021 -0.0994 0.050 Uiso 1 1 calc R . . C43 C 0.3115(4) 0.3960(4) -0.0584(3) 0.0538(10) Uani 1 1 d . . . H43 H 0.2969 0.3930 -0.1335 0.065 Uiso 1 1 calc R . . C44 C 0.3638(4) 0.5141(4) 0.0309(3) 0.0529(9) Uani 1 1 d . . . H44 H 0.3828 0.5920 0.0166 0.064 Uiso 1 1 calc R . . C45 C 0.3886(3) 0.5192(4) 0.1407(3) 0.0459(8) Uani 1 1 d . . . H45 H 0.4261 0.6001 0.2016 0.055 Uiso 1 1 calc R . . C46 C 0.3587(3) 0.4064(3) 0.1612(3) 0.0344(7) Uani 1 1 d . . . H46 H 0.3761 0.4096 0.2363 0.041 Uiso 1 1 calc R . . C51 C 0.3765(3) 0.1109(3) 0.1785(3) 0.0319(6) Uani 1 1 d . . . C52 C 0.4345(3) 0.0217(3) 0.1201(3) 0.0450(8) Uani 1 1 d . . . H52 H 0.4073 -0.0183 0.0403 0.054 Uiso 1 1 calc R . . C53 C 0.5314(3) -0.0089(4) 0.1775(4) 0.0575(11) Uani 1 1 d . . . H53 H 0.5720 -0.0685 0.1371 0.069 Uiso 1 1 calc R . . C54 C 0.5695(3) 0.0478(4) 0.2945(4) 0.0567(11) Uani 1 1 d . . . H54 H 0.6353 0.0259 0.3343 0.068 Uiso 1 1 calc R . . C55 C 0.5118(3) 0.1354(4) 0.3525(3) 0.0524(9) Uani 1 1 d . . . H55 H 0.5376 0.1738 0.4324 0.063 Uiso 1 1 calc R . . C56 C 0.4159(3) 0.1679(3) 0.2949(3) 0.0423(8) Uani 1 1 d . . . H56 H 0.3772 0.2295 0.3353 0.051 Uiso 1 1 calc R . . N11 N 0.1477(2) 0.4934(2) 0.3389(2) 0.0318(5) Uani 1 1 d . . . N12 N 0.1183(2) 0.3790(2) 0.35582(19) 0.0240(5) Uani 1 1 d . . . N21 N -0.1269(2) 0.4172(2) 0.3236(2) 0.0292(5) Uani 1 1 d . . . N22 N -0.0994(2) 0.3155(2) 0.24931(18) 0.0233(5) Uani 1 1 d . . . N31 N -0.0481(2) 0.2019(2) 0.42484(19) 0.0250(5) Uani 1 1 d . . . N32 N -0.0180(2) 0.1727(2) 0.32210(18) 0.0219(4) Uani 1 1 d . . . O1 O 0.16698(17) 0.18014(18) 0.19128(15) 0.0255(4) Uani 1 1 d . . . O2 O 0.1775(2) 0.0312(2) -0.00628(18) 0.0369(5) Uani 1 1 d . . . B1 B -0.3393(5) 0.7587(4) 0.3868(4) 0.0533(11) Uani 1 1 d . . . F1 F -0.2436(3) 0.7021(2) 0.3493(2) 0.0714(7) Uani 1 1 d . . . F2 F -0.4276(2) 0.6668(3) 0.4062(2) 0.0769(8) Uani 1 1 d . . . F3 F -0.2767(2) 0.8613(2) 0.48579(19) 0.0641(6) Uani 1 1 d . . . F4 F -0.3886(3) 0.7949(3) 0.3035(3) 0.0917(10) Uani 1 1 d . . . O3 O 0.0937(3) 0.7421(3) 0.3025(3) 0.0689(8) Uani 1 1 d . . . C61 C 0.0219(5) 0.6598(6) 0.1972(5) 0.0852(17) Uani 1 1 d . . . H61B H -0.0673 0.6660 0.1897 0.102 Uiso 1 1 calc R . . H61A H 0.0192 0.5697 0.1887 0.102 Uiso 1 1 calc R . . C62 C 0.0718(8) 0.6878(9) 0.1091(6) 0.140(3) Uani 1 1 d . . . H62B H 0.0095 0.7139 0.0642 0.169 Uiso 1 1 calc R . . H62A H 0.0906 0.6112 0.0585 0.169 Uiso 1 1 calc R . . C63 C 0.1871(7) 0.7920(7) 0.1653(6) 0.112(2) Uani 1 1 d . . . H63B H 0.1796 0.8696 0.1494 0.134 Uiso 1 1 calc R . . H63A H 0.2613 0.7672 0.1390 0.134 Uiso 1 1 calc R . . C64 C 0.2054(6) 0.8200(6) 0.2883(5) 0.0892(16) Uani 1 1 d . . . H64B H 0.2828 0.7985 0.3170 0.107 Uiso 1 1 calc R . . H64A H 0.2159 0.9130 0.3300 0.107 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.05242(17) 0.02578(14) 0.02764(14) 0.00039(9) 0.01356(11) 0.01660(11) P1 0.0212(3) 0.0289(4) 0.0229(3) -0.0025(3) 0.0072(3) 0.0066(3) C1 0.0210(12) 0.0188(12) 0.0207(12) 0.0033(10) 0.0051(10) 0.0058(10) C2 0.0210(13) 0.0268(14) 0.0222(13) 0.0025(11) 0.0072(10) 0.0075(11) C11 0.0249(14) 0.0324(15) 0.0214(13) 0.0006(11) 0.0057(11) 0.0075(12) C12 0.0253(15) 0.0403(18) 0.0288(15) -0.0056(13) 0.0070(12) 0.0004(13) C13 0.0372(17) 0.0269(15) 0.0358(16) -0.0011(13) 0.0163(14) -0.0026(13) C21 0.0268(14) 0.0289(15) 0.0295(15) 0.0000(12) 0.0037(12) 0.0086(12) C22 0.0281(15) 0.0368(17) 0.0354(16) 0.0103(13) 0.0071(12) 0.0138(13) C23 0.0338(16) 0.0350(16) 0.0341(16) 0.0117(13) 0.0144(13) 0.0193(13) C31 0.0305(14) 0.0189(13) 0.0266(14) 0.0006(11) 0.0038(11) 0.0066(11) C32 0.0376(16) 0.0214(14) 0.0370(16) 0.0097(12) 0.0063(13) 0.0073(12) C33 0.0306(15) 0.0299(15) 0.0294(15) 0.0125(12) 0.0074(12) 0.0069(12) C41 0.0239(14) 0.0381(16) 0.0258(14) 0.0047(12) 0.0095(11) 0.0058(12) C42 0.0320(16) 0.055(2) 0.0257(15) 0.0069(14) 0.0065(13) 0.0034(15) C43 0.052(2) 0.072(3) 0.0357(19) 0.0244(19) 0.0117(16) 0.0077(19) C44 0.051(2) 0.056(2) 0.054(2) 0.028(2) 0.0166(18) 0.0059(18) C45 0.047(2) 0.0412(19) 0.0410(19) 0.0105(15) 0.0109(16) 0.0028(15) C46 0.0318(16) 0.0381(17) 0.0269(15) 0.0065(13) 0.0079(12) 0.0055(13) C51 0.0228(14) 0.0301(15) 0.0355(16) 0.0029(12) 0.0075(12) 0.0074(12) C52 0.0308(17) 0.0391(18) 0.054(2) 0.0000(16) 0.0136(15) 0.0118(14) C53 0.0350(19) 0.044(2) 0.086(3) 0.006(2) 0.0152(19) 0.0224(16) C54 0.0332(19) 0.048(2) 0.085(3) 0.022(2) 0.0004(19) 0.0149(16) C55 0.0395(19) 0.056(2) 0.053(2) 0.0141(18) -0.0026(16) 0.0155(17) C56 0.0363(17) 0.0431(19) 0.0390(18) 0.0024(15) 0.0042(14) 0.0176(15) N11 0.0340(13) 0.0204(12) 0.0368(14) 0.0051(10) 0.0141(11) 0.0042(10) N12 0.0245(11) 0.0169(11) 0.0245(11) 0.0009(9) 0.0071(9) 0.0038(9) N21 0.0354(13) 0.0257(12) 0.0268(12) 0.0034(10) 0.0128(10) 0.0154(10) N22 0.0256(11) 0.0205(11) 0.0237(11) 0.0045(9) 0.0100(9) 0.0095(9) N31 0.0270(12) 0.0255(12) 0.0223(11) 0.0066(9) 0.0093(9) 0.0084(9) N32 0.0224(11) 0.0207(11) 0.0212(11) 0.0049(9) 0.0074(9) 0.0067(9) O1 0.0221(9) 0.0286(10) 0.0232(9) 0.0031(8) 0.0082(8) 0.0102(8) O2 0.0300(11) 0.0356(12) 0.0298(11) -0.0053(9) 0.0073(9) 0.0064(9) B1 0.067(3) 0.035(2) 0.046(2) 0.0160(18) -0.001(2) 0.000(2) F1 0.112(2) 0.0491(14) 0.0564(14) 0.0211(12) 0.0303(14) 0.0208(14) F2 0.0592(15) 0.0772(18) 0.0768(17) 0.0419(15) -0.0076(13) -0.0192(13) F3 0.0675(15) 0.0503(13) 0.0507(13) 0.0000(11) 0.0160(11) -0.0017(11) F4 0.106(2) 0.0616(17) 0.090(2) 0.0452(16) -0.0226(17) -0.0050(15) O3 0.098(2) 0.0596(18) 0.066(2) 0.0308(16) 0.0357(18) 0.0335(18) C61 0.067(3) 0.120(5) 0.085(4) 0.072(4) 0.008(3) 0.011(3) C62 0.137(6) 0.176(8) 0.080(4) 0.041(5) 0.050(4) -0.015(6) C63 0.136(6) 0.092(4) 0.121(5) 0.050(4) 0.074(5) 0.016(4) C64 0.091(4) 0.071(3) 0.101(4) 0.025(3) 0.030(3) 0.021(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N31 Ag1 N21 149.94(9) 2_566 . ? N31 Ag1 N11 134.01(8) 2_566 . ? N21 Ag1 N11 75.79(8) . . ? N31 Ag1 O3 88.60(9) 2_566 . ? N21 Ag1 O3 106.87(10) . . ? N11 Ag1 O3 74.28(9) . . ? N31 Ag1 F1 80.23(7) 2_566 . ? N21 Ag1 F1 79.12(7) . . ? N11 Ag1 F1 132.39(8) . . ? O3 Ag1 F1 75.30(8) . . ? N31 Ag1 Ag1 106.42(6) 2_566 2_566 ? N21 Ag1 Ag1 68.25(6) . 2_566 ? N11 Ag1 Ag1 83.07(6) . 2_566 ? O3 Ag1 Ag1 157.29(6) . 2_566 ? F1 Ag1 Ag1 123.27(4) . 2_566 ? O2 P1 O1 114.91(11) . . ? O2 P1 C51 113.42(14) . . ? O1 P1 C51 100.00(12) . . ? O2 P1 C41 111.51(14) . . ? O1 P1 C41 104.25(12) . . ? C51 P1 C41 111.92(14) . . ? N32 C1 N12 108.6(2) . . ? N32 C1 N22 110.5(2) . . ? N12 C1 N22 110.6(2) . . ? N32 C1 C2 111.2(2) . . ? N12 C1 C2 108.8(2) . . ? N22 C1 C2 107.2(2) . . ? O1 C2 C1 106.6(2) . . ? O1 C2 H2A 110.4 . . ? C1 C2 H2A 110.4 . . ? O1 C2 H2B 110.4 . . ? C1 C2 H2B 110.4 . . ? H2A C2 H2B 108.6 . . ? N12 C11 C12 106.7(3) . . ? N12 C11 H11 126.6 . . ? C12 C11 H11 126.6 . . ? C11 C12 C13 105.6(3) . . ? C11 C12 H12 127.2 . . ? C13 C12 H12 127.2 . . ? N11 C13 C12 111.9(3) . . ? N11 C13 H13 124.1 . . ? C12 C13 H13 124.1 . . ? N22 C21 C22 107.2(3) . . ? N22 C21 H21 126.4 . . ? C22 C21 H21 126.4 . . ? C21 C22 C23 105.5(3) . . ? C21 C22 H22 127.3 . . ? C23 C22 H22 127.3 . . ? N21 C23 C22 112.1(3) . . ? N21 C23 H23 124.0 . . ? C22 C23 H23 124.0 . . ? N32 C31 C32 107.7(3) . . ? N32 C31 H31 126.2 . . ? C32 C31 H31 126.2 . . ? C31 C32 C33 105.2(3) . . ? C31 C32 H32 127.4 . . ? C33 C32 H32 127.4 . . ? N31 C33 C32 111.6(3) . . ? N31 C33 H33 124.2 . . ? C32 C33 H33 124.2 . . ? C42 C41 C46 119.5(3) . . ? C42 C41 P1 119.7(2) . . ? C46 C41 P1 120.6(2) . . ? C43 C42 C41 119.8(3) . . ? C43 C42 H42 120.1 . . ? C41 C42 H42 120.1 . . ? C42 C43 C44 120.2(3) . . ? C42 C43 H43 119.9 . . ? C44 C43 H43 119.9 . . ? C45 C44 C43 120.4(4) . . ? C45 C44 H44 119.8 . . ? C43 C44 H44 119.8 . . ? C46 C45 C44 119.7(3) . . ? C46 C45 H45 120.2 . . ? C44 C45 H45 120.2 . . ? C45 C46 C41 120.4(3) . . ? C45 C46 H46 119.8 . . ? C41 C46 H46 119.8 . . ? C56 C51 C52 119.5(3) . . ? C56 C51 P1 122.8(2) . . ? C52 C51 P1 117.7(3) . . ? C53 C52 C51 120.3(4) . . ? C53 C52 H52 119.9 . . ? C51 C52 H52 119.9 . . ? C52 C53 C54 119.9(3) . . ? C52 C53 H53 120.0 . . ? C54 C53 H53 120.0 . . ? C55 C54 C53 119.9(3) . . ? C55 C54 H54 120.1 . . ? C53 C54 H54 120.1 . . ? C54 C55 C56 120.3(4) . . ? C54 C55 H55 119.9 . . ? C56 C55 H55 119.9 . . ? C51 C56 C55 120.1(3) . . ? C51 C56 H56 119.9 . . ? C55 C56 H56 119.9 . . ? C13 N11 N12 103.9(3) . . ? C13 N11 Ag1 102.43(19) . . ? N12 N11 Ag1 102.83(16) . . ? C11 N12 N11 111.8(2) . . ? C11 N12 C1 126.4(2) . . ? N11 N12 C1 118.6(2) . . ? C23 N21 N22 104.6(2) . . ? C23 N21 Ag1 119.55(19) . . ? N22 N21 Ag1 127.89(18) . . ? C21 N22 N21 110.6(2) . . ? C21 N22 C1 124.4(2) . . ? N21 N22 C1 123.7(2) . . ? C33 N31 N32 105.1(2) . . ? C33 N31 Ag1 124.01(19) . 2_566 ? N32 N31 Ag1 129.99(17) . 2_566 ? C31 N32 N31 110.5(2) . . ? C31 N32 C1 128.2(2) . . ? N31 N32 C1 120.6(2) . . ? C2 O1 P1 119.43(16) . . ? F4 B1 F3 113.4(4) . . ? F4 B1 F2 113.7(4) . . ? F3 B1 F2 110.5(4) . . ? F4 B1 F1 105.8(4) . . ? F3 B1 F1 105.5(4) . . ? F2 B1 F1 107.3(3) . . ? B1 F1 Ag1 142.5(2) . . ? C61 O3 C64 107.3(4) . . ? C61 O3 Ag1 102.6(3) . . ? C64 O3 Ag1 142.2(3) . . ? O3 C61 C62 112.8(5) . . ? O3 C61 H61B 109.0 . . ? C62 C61 H61B 109.0 . . ? O3 C61 H61A 109.0 . . ? C62 C61 H61A 109.0 . . ? H61B C61 H61A 107.8 . . ? C61 C62 C63 105.1(6) . . ? C61 C62 H62B 110.7 . . ? C63 C62 H62B 110.7 . . ? C61 C62 H62A 110.7 . . ? C63 C62 H62A 110.7 . . ? H62B C62 H62A 108.8 . . ? C62 C63 C64 107.4(5) . . ? C62 C63 H63B 110.2 . . ? C64 C63 H63B 110.2 . . ? C62 C63 H63A 110.2 . . ? C64 C63 H63A 110.2 . . ? H63B C63 H63A 108.5 . . ? O3 C64 C63 106.8(5) . . ? O3 C64 H64B 110.4 . . ? C63 C64 H64B 110.4 . . ? O3 C64 H64A 110.4 . . ? C63 C64 H64A 110.4 . . ? H64B C64 H64A 108.6 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N31 2.182(2) 2_566 ? Ag1 N21 2.257(2) . ? Ag1 N11 2.464(2) . ? Ag1 O3 2.795(3) . ? Ag1 F1 3.366(3) . ? Ag1 Ag1 3.3690(5) 2_566 ? P1 O2 1.478(2) . ? P1 O1 1.6048(19) . ? P1 C51 1.788(3) . ? P1 C41 1.791(3) . ? C1 N32 1.450(3) . ? C1 N12 1.452(3) . ? C1 N22 1.466(3) . ? C1 C2 1.540(3) . ? C2 O1 1.434(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C11 N12 1.358(4) . ? C11 C12 1.363(4) . ? C11 H11 0.9500 . ? C12 C13 1.394(5) . ? C12 H12 0.9500 . ? C13 N11 1.334(4) . ? C13 H13 0.9500 . ? C21 N22 1.361(4) . ? C21 C22 1.362(4) . ? C21 H21 0.9500 . ? C22 C23 1.381(4) . ? C22 H22 0.9500 . ? C23 N21 1.326(4) . ? C23 H23 0.9500 . ? C31 N32 1.359(3) . ? C31 C32 1.359(4) . ? C31 H31 0.9500 . ? C32 C33 1.396(4) . ? C32 H32 0.9500 . ? C33 N31 1.325(4) . ? C33 H33 0.9500 . ? C41 C42 1.394(4) . ? C41 C46 1.395(4) . ? C42 C43 1.378(5) . ? C42 H42 0.9500 . ? C43 C44 1.387(6) . ? C43 H43 0.9500 . ? C44 C45 1.386(5) . ? C44 H44 0.9500 . ? C45 C46 1.377(5) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C51 C56 1.386(5) . ? C51 C52 1.390(4) . ? C52 C53 1.381(5) . ? C52 H52 0.9500 . ? C53 C54 1.393(6) . ? C53 H53 0.9500 . ? C54 C55 1.375(6) . ? C54 H54 0.9500 . ? C55 C56 1.387(5) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? N11 N12 1.369(3) . ? N21 N22 1.367(3) . ? N31 N32 1.368(3) . ? N31 Ag1 2.182(2) 2_566 ? B1 F4 1.357(5) . ? B1 F3 1.374(5) . ? B1 F2 1.377(5) . ? B1 F1 1.414(6) . ? O3 C61 1.371(6) . ? O3 C64 1.420(6) . ? C61 C62 1.429(7) . ? C61 H61B 0.9900 . ? C61 H61A 0.9900 . ? C62 C63 1.430(9) . ? C62 H62B 0.9900 . ? C62 H62A 0.9900 . ? C63 C64 1.489(8) . ? C63 H63B 0.9900 . ? C63 H63A 0.9900 . ? C64 H64B 0.9900 . ? C64 H64A 0.9900 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N32 C1 C2 O1 -60.7(3) . . . . ? N12 C1 C2 O1 58.8(3) . . . . ? N22 C1 C2 O1 178.4(2) . . . . ? N12 C11 C12 C13 -1.5(3) . . . . ? C11 C12 C13 N11 -0.4(4) . . . . ? N22 C21 C22 C23 -1.3(3) . . . . ? C21 C22 C23 N21 0.0(4) . . . . ? N32 C31 C32 C33 0.8(3) . . . . ? C31 C32 C33 N31 -0.1(3) . . . . ? O2 P1 C41 C42 -2.9(3) . . . . ? O1 P1 C41 C42 -127.4(2) . . . . ? C51 P1 C41 C42 125.4(3) . . . . ? O2 P1 C41 C46 172.2(2) . . . . ? O1 P1 C41 C46 47.7(3) . . . . ? C51 P1 C41 C46 -59.5(3) . . . . ? C46 C41 C42 C43 -1.1(5) . . . . ? P1 C41 C42 C43 174.1(3) . . . . ? C41 C42 C43 C44 -0.5(6) . . . . ? C42 C43 C44 C45 1.7(6) . . . . ? C43 C44 C45 C46 -1.3(6) . . . . ? C44 C45 C46 C41 -0.4(5) . . . . ? C42 C41 C46 C45 1.5(5) . . . . ? P1 C41 C46 C45 -173.6(3) . . . . ? O2 P1 C51 C56 -149.4(3) . . . . ? O1 P1 C51 C56 -26.6(3) . . . . ? C41 P1 C51 C56 83.3(3) . . . . ? O2 P1 C51 C52 28.2(3) . . . . ? O1 P1 C51 C52 151.1(3) . . . . ? C41 P1 C51 C52 -99.0(3) . . . . ? C56 C51 C52 C53 -0.6(5) . . . . ? P1 C51 C52 C53 -178.4(3) . . . . ? C51 C52 C53 C54 1.3(6) . . . . ? C52 C53 C54 C55 -0.9(6) . . . . ? C53 C54 C55 C56 -0.2(6) . . . . ? C52 C51 C56 C55 -0.5(5) . . . . ? P1 C51 C56 C55 177.1(3) . . . . ? C54 C55 C56 C51 0.9(6) . . . . ? C12 C13 N11 N12 2.0(3) . . . . ? C12 C13 N11 Ag1 108.8(2) . . . . ? N31 Ag1 N11 C13 15.2(3) 2_566 . . . ? N21 Ag1 N11 C13 -160.2(2) . . . . ? O3 Ag1 N11 C13 87.3(2) . . . . ? F1 Ag1 N11 C13 139.46(19) . . . . ? Ag1 Ag1 N11 C13 -91.0(2) 2_566 . . . ? N31 Ag1 N11 N12 122.89(16) 2_566 . . . ? N21 Ag1 N11 N12 -52.54(16) . . . . ? O3 Ag1 N11 N12 -165.01(19) . . . . ? F1 Ag1 N11 N12 -112.88(16) . . . . ? Ag1 Ag1 N11 N12 16.71(15) 2_566 . . . ? C12 C11 N12 N11 2.8(3) . . . . ? C12 C11 N12 C1 162.0(2) . . . . ? C13 N11 N12 C11 -3.0(3) . . . . ? Ag1 N11 N12 C11 -109.5(2) . . . . ? C13 N11 N12 C1 -164.0(2) . . . . ? Ag1 N11 N12 C1 89.5(2) . . . . ? N32 C1 N12 C11 34.3(3) . . . . ? N22 C1 N12 C11 155.7(2) . . . . ? C2 C1 N12 C11 -86.8(3) . . . . ? N32 C1 N12 N11 -167.7(2) . . . . ? N22 C1 N12 N11 -46.4(3) . . . . ? C2 C1 N12 N11 71.1(3) . . . . ? C22 C23 N21 N22 1.4(3) . . . . ? C22 C23 N21 Ag1 152.8(2) . . . . ? N31 Ag1 N21 C23 42.6(3) 2_566 . . . ? N11 Ag1 N21 C23 -144.0(2) . . . . ? O3 Ag1 N21 C23 -75.7(2) . . . . ? F1 Ag1 N21 C23 -4.8(2) . . . . ? Ag1 Ag1 N21 C23 127.9(2) 2_566 . . . ? N31 Ag1 N21 N22 -173.39(19) 2_566 . . . ? N11 Ag1 N21 N22 0.0(2) . . . . ? O3 Ag1 N21 N22 68.4(2) . . . . ? F1 Ag1 N21 N22 139.2(2) . . . . ? Ag1 Ag1 N21 N22 -88.1(2) 2_566 . . . ? C22 C21 N22 N21 2.2(3) . . . . ? C22 C21 N22 C1 169.4(3) . . . . ? C23 N21 N22 C21 -2.2(3) . . . . ? Ag1 N21 N22 C21 -150.4(2) . . . . ? C23 N21 N22 C1 -169.5(2) . . . . ? Ag1 N21 N22 C1 42.3(3) . . . . ? N32 C1 N22 C21 -74.7(3) . . . . ? N12 C1 N22 C21 165.1(2) . . . . ? C2 C1 N22 C21 46.7(3) . . . . ? N32 C1 N22 N21 90.9(3) . . . . ? N12 C1 N22 N21 -29.3(3) . . . . ? C2 C1 N22 N21 -147.7(2) . . . . ? C32 C33 N31 N32 -0.7(3) . . . . ? C32 C33 N31 Ag1 -170.64(19) . . . 2_566 ? C32 C31 N32 N31 -1.3(3) . . . . ? C32 C31 N32 C1 -171.6(2) . . . . ? C33 N31 N32 C31 1.3(3) . . . . ? Ag1 N31 N32 C31 170.35(19) 2_566 . . . ? C33 N31 N32 C1 172.3(2) . . . . ? Ag1 N31 N32 C1 -18.6(3) 2_566 . . . ? N12 C1 N32 C31 -135.2(3) . . . . ? N22 C1 N32 C31 103.4(3) . . . . ? C2 C1 N32 C31 -15.6(4) . . . . ? N12 C1 N32 N31 55.4(3) . . . . ? N22 C1 N32 N31 -66.0(3) . . . . ? C2 C1 N32 N31 175.1(2) . . . . ? C1 C2 O1 P1 -170.14(16) . . . . ? O2 P1 O1 C2 -60.9(2) . . . . ? C51 P1 O1 C2 177.3(2) . . . . ? C41 P1 O1 C2 61.4(2) . . . . ? F4 B1 F1 Ag1 164.3(2) . . . . ? F3 B1 F1 Ag1 43.8(5) . . . . ? F2 B1 F1 Ag1 -74.0(4) . . . . ? N31 Ag1 F1 B1 -43.3(4) 2_566 . . . ? N21 Ag1 F1 B1 114.7(4) . . . . ? N11 Ag1 F1 B1 173.8(3) . . . . ? O3 Ag1 F1 B1 -134.4(4) . . . . ? Ag1 Ag1 F1 B1 60.0(4) 2_566 . . . ? N31 Ag1 O3 C61 -149.2(3) 2_566 . . . ? N21 Ag1 O3 C61 4.7(3) . . . . ? N11 Ag1 O3 C61 74.0(3) . . . . ? F1 Ag1 O3 C61 -68.9(3) . . . . ? Ag1 Ag1 O3 C61 78.5(4) 2_566 . . . ? N31 Ag1 O3 C64 69.1(5) 2_566 . . . ? N21 Ag1 O3 C64 -137.1(5) . . . . ? N11 Ag1 O3 C64 -67.7(5) . . . . ? F1 Ag1 O3 C64 149.3(5) . . . . ? Ag1 Ag1 O3 C64 -63.3(6) 2_566 . . . ? C64 O3 C61 C62 -7.0(8) . . . . ? Ag1 O3 C61 C62 -163.7(6) . . . . ? O3 C61 C62 C63 2.9(10) . . . . ? C61 C62 C63 C64 2.2(9) . . . . ? C61 O3 C64 C63 8.0(6) . . . . ? Ag1 O3 C64 C63 148.8(4) . . . . ? C62 C63 C64 O3 -6.4(8) . . . . ?
1100785.cif	#------------------------------------------------------------------------------ #$Date: 2016-03-28 07:01:53 +0300 (Mon, 28 Mar 2016) $ #$Revision: 180559 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100785.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100785 loop_ _publ_author_name 'Vecchi, Paul A.' 'Ellern, Arkady' 'Angelici, Robert J.' _publ_section_title ; Steric Effects in the Binding of Hindered Dibenzothiophene Ligands in [Cp'Ru(CO)~2~(\h^1^(S)-DBTh)]^+^ Complexes ; _journal_coden_ASTM ORGND7 _journal_issue 9 _journal_name_full Organometallics _journal_page_first 2168 _journal_page_last 2176 _journal_paper_doi 10.1021/om048973l _journal_volume 24 _journal_year 2005 _chemical_formula_sum 'C20 H15 B F4 O2 Ru S' _chemical_formula_weight 507.26 _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 94.534(6) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 11.699(4) _cell_length_b 12.520(5) _cell_length_c 13.149(5) _cell_measurement_reflns_used 988 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 27.39 _cell_measurement_theta_min 2.39 _cell_volume 1920.0(12) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 173(2) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0422 _diffrn_reflns_av_sigmaI/netI 0.0357 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 13529 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_min 1.75 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _exptl_absorpt_coefficient_mu 0.977 _exptl_absorpt_correction_T_max 0.88 _exptl_absorpt_correction_T_min 0.76 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Bruker SADABS' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.755 _exptl_crystal_density_meas 0 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 1008 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _refine_diff_density_max 4.094 _refine_diff_density_min -0.874 _refine_diff_density_rms 0.198 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 262 _refine_ls_number_reflns 3341 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.100 _refine_ls_R_factor_all 0.0744 _refine_ls_R_factor_gt 0.0677 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1092P)^2^+21.7858P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2006 _refine_ls_wR_factor_ref 0.2083 _reflns_number_gt 2955 _reflns_number_total 3341 _reflns_threshold_expression >2sigma(I) _cod_duplicate_entry 4060277 _cod_data_source_file om048973lsi20050303_083418.cif _cod_data_source_block complex2 _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_sg_symbol_H-M P2(1)/c _cod_database_code 1100785 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.64089(5) 0.42801(5) 0.75372(5) 0.0223(3) Uani 1 1 d . . . S1 S 0.81129(16) 0.50452(15) 0.83292(15) 0.0252(4) Uani 1 1 d . . . C1 C 1.0608(8) 0.3244(7) 0.9602(7) 0.038(2) Uani 1 1 d . . . H1 H 1.1345 0.3033 0.9419 0.046 Uiso 1 1 calc R . . C2 C 1.0232(9) 0.2930(7) 1.0519(7) 0.042(2) Uani 1 1 d . . . H2 H 1.0706 0.2488 1.0963 0.050 Uiso 1 1 calc R . . C3 C 0.9176(9) 0.3246(8) 1.0803(7) 0.043(2) Uani 1 1 d . . . H3 H 0.8939 0.3022 1.1444 0.052 Uiso 1 1 calc R . . C4 C 0.8429(8) 0.3899(7) 1.0161(6) 0.0347(19) Uani 1 1 d . . . C6 C 0.9370(8) 0.5571(7) 0.6663(7) 0.037(2) Uani 1 1 d . . . H6 H 0.8759 0.6011 0.6392 0.044 Uiso 1 1 calc R . . C7 C 1.0374(8) 0.5490(8) 0.6184(7) 0.041(2) Uani 1 1 d . . . H7 H 1.0462 0.5891 0.5582 0.049 Uiso 1 1 calc R . . C8 C 1.1255(8) 0.4831(8) 0.6573(7) 0.038(2) Uani 1 1 d . . . H8 H 1.1935 0.4777 0.6225 0.046 Uiso 1 1 calc R . . C9 C 1.1163(7) 0.4251(7) 0.7455(8) 0.038(2) Uani 1 1 d . . . H9 H 1.1770 0.3800 0.7716 0.046 Uiso 1 1 calc R . . C10 C 1.0163(7) 0.4340(6) 0.7956(7) 0.0311(19) Uani 1 1 d . . . C11 C 0.9904(7) 0.3876(7) 0.8940(7) 0.0308(18) Uani 1 1 d . . . C12 C 0.9277(6) 0.4986(6) 0.7559(6) 0.0266(16) Uani 1 1 d . . . C13 C 0.8835(7) 0.4175(6) 0.9240(6) 0.0281(17) Uani 1 1 d . . . C14 C 0.7307(9) 0.4252(9) 1.0500(7) 0.046(2) Uani 1 1 d . . . H14A H 0.6909 0.4693 0.9967 0.069 Uiso 1 1 calc R . . H14B H 0.7435 0.4672 1.1129 0.069 Uiso 1 1 calc R . . H14C H 0.6838 0.3626 1.0629 0.069 Uiso 1 1 calc R . . C17 C 0.7034(9) 0.4001(7) 0.6263(7) 0.039(2) Uani 1 1 d . . . C18 C 0.6807(7) 0.2876(7) 0.7994(6) 0.0307(18) Uani 1 1 d . . . C19 C 0.5379(7) 0.5385(8) 0.8426(7) 0.040(2) Uani 1 1 d . . . H19 H 0.5655 0.5759 0.9071 0.047 Uiso 1 1 calc R . . C20 C 0.4821(8) 0.4403(8) 0.8359(7) 0.040(2) Uani 1 1 d . . . H20 H 0.4630 0.3951 0.8949 0.048 Uiso 1 1 calc R . . C21 C 0.4510(7) 0.4182(8) 0.7320(8) 0.040(2) Uani 1 1 d . . . H21 H 0.4053 0.3556 0.7046 0.048 Uiso 1 1 calc R . . C22 C 0.4887(7) 0.5048(8) 0.6746(8) 0.040(2) Uani 1 1 d . . . H22 H 0.4741 0.5143 0.5992 0.048 Uiso 1 1 calc R . . C23 C 0.5428(8) 0.5792(7) 0.7429(8) 0.041(2) Uani 1 1 d . . . H23 H 0.5733 0.6507 0.7245 0.050 Uiso 1 1 calc R . . O1 O 0.7386(6) 0.3827(6) 0.5504(5) 0.0445(16) Uani 1 1 d . . . O2 O 0.7016(6) 0.2031(5) 0.8265(5) 0.0471(17) Uani 1 1 d . . . B1 B 0.3654(9) 0.2098(9) 0.9872(9) 0.040(2) Uani 1 1 d . . . F1 F 0.3188(6) 0.2595(6) 1.0683(5) 0.070(2) Uani 1 1 d . . . F2 F 0.3206(5) 0.2528(5) 0.8957(5) 0.0602(17) Uani 1 1 d . . . F3 F 0.4827(5) 0.2247(7) 0.9968(6) 0.083(2) Uani 1 1 d . . . F4 F 0.3406(7) 0.1033(5) 0.9901(5) 0.0678(19) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0171(4) 0.0246(4) 0.0249(4) -0.0006(2) 0.0001(2) 0.0001(2) S1 0.0206(9) 0.0265(10) 0.0281(10) -0.0023(8) 0.0006(7) -0.0007(7) C1 0.032(4) 0.035(5) 0.046(5) 0.002(4) -0.010(4) 0.001(4) C2 0.051(6) 0.031(5) 0.042(5) 0.004(4) -0.010(4) -0.001(4) C3 0.054(6) 0.043(5) 0.031(5) 0.005(4) -0.009(4) -0.019(5) C4 0.038(5) 0.038(5) 0.028(4) -0.006(4) -0.002(4) -0.009(4) C6 0.029(4) 0.044(5) 0.036(5) 0.001(4) 0.001(4) -0.009(4) C7 0.044(5) 0.048(6) 0.032(5) -0.002(4) 0.006(4) -0.007(4) C8 0.033(5) 0.047(5) 0.035(5) -0.004(4) 0.010(4) -0.009(4) C9 0.016(4) 0.039(5) 0.060(6) -0.013(4) 0.009(4) -0.001(3) C10 0.025(4) 0.026(4) 0.041(5) -0.006(3) 0.000(4) -0.003(3) C11 0.032(4) 0.025(4) 0.034(4) -0.005(3) -0.005(3) -0.002(3) C12 0.019(4) 0.028(4) 0.033(4) -0.003(3) 0.000(3) -0.005(3) C13 0.025(4) 0.026(4) 0.032(4) -0.002(3) -0.006(3) -0.004(3) C14 0.046(6) 0.065(7) 0.027(5) -0.002(4) 0.005(4) 0.001(5) C17 0.059(6) 0.033(5) 0.024(4) -0.001(4) 0.005(4) -0.016(4) C18 0.028(4) 0.030(5) 0.034(4) -0.002(4) -0.004(3) -0.006(3) C19 0.025(4) 0.050(5) 0.045(5) -0.013(4) 0.006(4) 0.012(4) C20 0.027(4) 0.056(6) 0.038(5) 0.008(4) 0.006(4) 0.007(4) C21 0.013(4) 0.051(6) 0.056(6) -0.004(4) -0.002(4) 0.000(3) C22 0.022(4) 0.046(5) 0.052(6) 0.003(4) -0.001(4) 0.011(4) C23 0.033(5) 0.028(5) 0.062(6) 0.003(4) 0.001(4) 0.010(4) O1 0.050(4) 0.047(4) 0.037(4) -0.003(3) 0.009(3) 0.004(3) O2 0.050(4) 0.031(4) 0.058(4) 0.009(3) -0.008(3) -0.001(3) B1 0.038(5) 0.032(5) 0.051(6) 0.000(5) 0.006(5) 0.004(4) F1 0.060(4) 0.072(5) 0.074(4) -0.035(4) -0.010(3) 0.024(3) F2 0.040(3) 0.068(4) 0.072(4) 0.024(3) 0.000(3) 0.015(3) F3 0.029(3) 0.118(7) 0.099(6) 0.028(5) -0.003(3) 0.002(4) F4 0.107(6) 0.041(3) 0.055(4) -0.002(3) 0.008(4) -0.009(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C18 Ru1 C17 90.4(4) . . ? C18 Ru1 C22 135.9(3) . . ? C17 Ru1 C22 91.0(4) . . ? C18 Ru1 C23 157.4(4) . . ? C17 Ru1 C23 109.4(4) . . ? C22 Ru1 C23 37.1(4) . . ? C18 Ru1 C21 101.9(4) . . ? C17 Ru1 C21 109.0(4) . . ? C22 Ru1 C21 37.1(4) . . ? C23 Ru1 C21 62.0(4) . . ? C18 Ru1 C19 122.5(4) . . ? C17 Ru1 C19 146.5(4) . . ? C22 Ru1 C19 61.8(4) . . ? C23 Ru1 C19 37.1(4) . . ? C21 Ru1 C19 61.6(4) . . ? C18 Ru1 C20 96.0(4) . . ? C17 Ru1 C20 146.0(4) . . ? C22 Ru1 C20 61.7(4) . . ? C23 Ru1 C20 61.6(4) . . ? C21 Ru1 C20 37.0(4) . . ? C19 Ru1 C20 36.4(4) . . ? C18 Ru1 S1 93.3(2) . . ? C17 Ru1 S1 95.3(3) . . ? C22 Ru1 S1 130.4(3) . . ? C23 Ru1 S1 95.5(3) . . ? C21 Ru1 S1 151.0(3) . . ? C19 Ru1 S1 89.4(3) . . ? C20 Ru1 S1 117.6(3) . . ? C12 S1 C13 90.8(4) . . ? C12 S1 Ru1 113.0(3) . . ? C13 S1 Ru1 112.6(3) . . ? C2 C1 C11 119.7(9) . . ? C2 C1 H1 120.1 . . ? C11 C1 H1 120.1 . . ? C1 C2 C3 120.8(9) . . ? C1 C2 H2 119.6 . . ? C3 C2 H2 119.6 . . ? C2 C3 C4 121.7(9) . . ? C2 C3 H3 119.1 . . ? C4 C3 H3 119.1 . . ? C13 C4 C3 115.2(8) . . ? C13 C4 C14 124.2(8) . . ? C3 C4 C14 120.5(8) . . ? C7 C6 C12 118.1(9) . . ? C7 C6 H6 120.9 . . ? C12 C6 H6 120.9 . . ? C6 C7 C8 120.7(9) . . ? C6 C7 H7 119.6 . . ? C8 C7 H7 119.6 . . ? C9 C8 C7 121.1(8) . . ? C9 C8 H8 119.4 . . ? C7 C8 H8 119.4 . . ? C8 C9 C10 118.7(9) . . ? C8 C9 H9 120.6 . . ? C10 C9 H9 120.6 . . ? C12 C10 C9 120.1(9) . . ? C12 C10 C11 111.3(7) . . ? C9 C10 C11 128.6(8) . . ? C13 C11 C1 118.4(8) . . ? C13 C11 C10 113.2(7) . . ? C1 C11 C10 128.3(8) . . ? C10 C12 C6 121.2(8) . . ? C10 C12 S1 113.4(6) . . ? C6 C12 S1 125.2(6) . . ? C4 C13 C11 124.1(8) . . ? C4 C13 S1 124.4(7) . . ? C11 C13 S1 111.3(6) . . ? C4 C14 H14A 109.5 . . ? C4 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C4 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O1 C17 Ru1 178.8(9) . . ? O2 C18 Ru1 178.2(7) . . ? C20 C19 C23 108.3(9) . . ? C20 C19 Ru1 71.9(5) . . ? C23 C19 Ru1 70.9(5) . . ? C20 C19 H19 125.8 . . ? C23 C19 H19 125.8 . . ? Ru1 C19 H19 125.8 . . ? C19 C20 C21 108.5(9) . . ? C19 C20 Ru1 71.7(5) . . ? C21 C20 Ru1 71.2(5) . . ? C19 C20 H20 125.7 . . ? C21 C20 H20 125.7 . . ? Ru1 C20 H20 125.7 . . ? C22 C21 C20 107.4(9) . . ? C22 C21 Ru1 71.0(5) . . ? C20 C21 Ru1 71.7(5) . . ? C22 C21 H21 126.2 . . ? C20 C21 H21 126.2 . . ? Ru1 C21 H21 126.2 . . ? C23 C22 C21 108.1(9) . . ? C23 C22 Ru1 71.5(5) . . ? C21 C22 Ru1 71.8(5) . . ? C23 C22 H22 125.9 . . ? C21 C22 H22 125.9 . . ? Ru1 C22 H22 125.9 . . ? C22 C23 C19 107.7(9) . . ? C22 C23 Ru1 71.4(5) . . ? C19 C23 Ru1 72.0(5) . . ? C22 C23 H23 126.1 . . ? C19 C23 H23 126.1 . . ? Ru1 C23 H23 126.1 . . ? F4 B1 F3 109.9(9) . . ? F4 B1 F2 109.7(9) . . ? F3 B1 F2 109.5(9) . . ? F4 B1 F1 108.6(9) . . ? F3 B1 F1 108.5(9) . . ? F2 B1 F1 110.5(8) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C18 1.903(9) . ? Ru1 C17 1.912(9) . ? Ru1 C22 2.210(9) . ? Ru1 C23 2.212(8) . ? Ru1 C21 2.221(8) . ? Ru1 C19 2.225(8) . ? Ru1 C20 2.227(9) . ? Ru1 S1 2.377(2) . ? S1 C12 1.763(8) . ? S1 C13 1.782(8) . ? C1 C2 1.373(14) . ? C1 C11 1.395(12) . ? C1 H1 0.9500 . ? C2 C3 1.377(15) . ? C2 H2 0.9500 . ? C3 C4 1.424(13) . ? C3 H3 0.9500 . ? C4 C13 1.379(12) . ? C4 C14 1.487(14) . ? C6 C7 1.379(13) . ? C6 C12 1.398(12) . ? C6 H6 0.9500 . ? C7 C8 1.386(14) . ? C7 H7 0.9500 . ? C8 C9 1.380(13) . ? C8 H8 0.9500 . ? C9 C10 1.391(12) . ? C9 H9 0.9500 . ? C10 C12 1.384(11) . ? C10 C11 1.472(12) . ? C11 C13 1.392(12) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C17 O1 1.131(11) . ? C18 O2 1.137(10) . ? C19 C20 1.392(14) . ? C19 C23 1.412(14) . ? C19 H19 1.0000 . ? C20 C21 1.413(14) . ? C20 H20 1.0000 . ? C21 C22 1.411(14) . ? C21 H21 1.0000 . ? C22 C23 1.408(14) . ? C22 H22 1.0000 . ? C23 H23 1.0000 . ? B1 F4 1.367(13) . ? B1 F3 1.380(12) . ? B1 F2 1.382(13) . ? B1 F1 1.384(12) . ?
1100786.cif	#------------------------------------------------------------------------------ #$Date: 2016-03-28 07:01:53 +0300 (Mon, 28 Mar 2016) $ #$Revision: 180559 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100786.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100786 loop_ _publ_author_name 'Vecchi, Paul A.' 'Ellern, Arkady' 'Angelici, Robert J.' _publ_section_title ; Steric Effects in the Binding of Hindered Dibenzothiophene Ligands in [Cp'Ru(CO)~2~(\h^1^(S)-DBTh)]^+^ Complexes ; _journal_coden_ASTM ORGND7 _journal_issue 9 _journal_name_full Organometallics _journal_page_first 2168 _journal_page_last 2176 _journal_paper_doi 10.1021/om048973l _journal_volume 24 _journal_year 2005 _chemical_formula_sum 'C21 H17 B F4 O2 Ru S' _chemical_formula_weight 521.29 _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 73.4480(10) _cell_angle_beta 69.5040(10) _cell_angle_gamma 88.382(2) _cell_formula_units_Z 2 _cell_length_a 9.3637(8) _cell_length_b 10.4141(9) _cell_length_c 11.7381(9) _cell_measurement_temperature 293(2) _cell_volume 1024.48(15) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.981 _diffrn_measured_fraction_theta_max 0.981 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0183 _diffrn_reflns_av_sigmaI/netI 0.0385 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 6757 _diffrn_reflns_theta_full 26.37 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_min 1.94 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _exptl_absorpt_coefficient_mu 0.918 _exptl_absorpt_correction_T_max 0.86 _exptl_absorpt_correction_T_min 0.76 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details ? _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.690 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 520 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.21 _refine_diff_density_max 0.785 _refine_diff_density_min -0.782 _refine_diff_density_rms 0.077 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 271 _refine_ls_number_reflns 4112 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.018 _refine_ls_R_factor_all 0.0380 _refine_ls_R_factor_gt 0.0311 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0471P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0775 _refine_ls_wR_factor_ref 0.0803 _reflns_number_gt 3522 _reflns_number_total 4112 _reflns_threshold_expression >2sigma(I) _cod_duplicate_entry 4060278 _cod_data_source_file om048973lsi20050303_083418.cif _cod_data_source_block complex3 _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_sg_symbol_H-M P-1 _cod_database_code 1100786 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.68945(3) 0.72355(2) 0.68625(2) 0.02390(9) Uani 1 1 d . . . S1 S 0.69906(8) 0.86947(7) 0.81000(6) 0.02462(16) Uani 1 1 d . . . C1 C 0.3619(3) 0.7819(3) 1.1461(3) 0.0327(7) Uani 1 1 d . . . H1 H 0.3513 0.7344 1.2291 0.039 Uiso 1 1 calc R . . C2 C 0.2388(3) 0.8406(3) 1.1186(3) 0.0359(7) Uani 1 1 d . . . H2 H 0.1445 0.8315 1.1838 0.043 Uiso 1 1 calc R . . C3 C 0.2538(3) 0.9124(3) 0.9957(3) 0.0347(7) Uani 1 1 d . . . H3 H 0.1691 0.9518 0.9809 0.042 Uiso 1 1 calc R . . C4 C 0.3907(3) 0.9281(3) 0.8934(3) 0.0288(6) Uani 1 1 d . . . C6 C 0.9176(3) 0.7591(3) 0.9153(3) 0.0314(7) Uani 1 1 d . . . C7 C 0.9472(4) 0.6891(3) 1.0234(3) 0.0367(7) Uani 1 1 d . . . H7 H 1.0467 0.6676 1.0152 0.044 Uiso 1 1 calc R . . C8 C 0.8340(4) 0.6502(3) 1.1428(3) 0.0380(8) Uani 1 1 d . . . H8 H 0.8587 0.6032 1.2128 0.046 Uiso 1 1 calc R . . C9 C 0.6842(4) 0.6802(3) 1.1595(3) 0.0323(7) Uani 1 1 d . . . H9 H 0.6087 0.6554 1.2401 0.039 Uiso 1 1 calc R . . C10 C 0.6487(3) 0.7484(3) 1.0531(3) 0.0265(6) Uani 1 1 d . . . C11 C 0.5027(3) 0.7953(3) 1.0465(3) 0.0262(6) Uani 1 1 d . . . C12 C 0.7658(3) 0.7839(3) 0.9338(3) 0.0266(6) Uani 1 1 d . . . C13 C 0.5122(3) 0.8665(3) 0.9228(3) 0.0253(6) Uani 1 1 d . . . C14 C 0.4056(4) 1.0063(3) 0.7608(3) 0.0358(7) Uani 1 1 d . . . H14A H 0.5084 1.0059 0.7041 0.054 Uiso 1 1 calc R . . H14B H 0.3822 1.0972 0.7581 0.054 Uiso 1 1 calc R . . H14C H 0.3358 0.9659 0.7350 0.054 Uiso 1 1 calc R . . C16 C 1.0430(4) 0.8058(4) 0.7858(3) 0.0431(8) Uani 1 1 d . . . H16A H 1.1391 0.7783 0.7930 0.065 Uiso 1 1 calc R . . H16B H 1.0487 0.9019 0.7539 0.065 Uiso 1 1 calc R . . H16C H 1.0211 0.7666 0.7284 0.065 Uiso 1 1 calc R . . C17 C 0.7800(4) 0.5829(3) 0.7751(3) 0.0323(7) Uani 1 1 d . . . C18 C 0.4898(4) 0.6478(3) 0.8027(3) 0.0337(7) Uani 1 1 d . . . C19 C 0.6237(4) 0.8222(3) 0.5189(3) 0.0350(7) Uani 1 1 d . . . H19 H 0.5230 0.8537 0.5224 0.042 Uiso 1 1 calc R . . C20 C 0.6705(4) 0.6921(3) 0.5136(3) 0.0358(7) Uani 1 1 d . . . H20 H 0.6092 0.6192 0.5107 0.043 Uiso 1 1 calc R . . C21 C 0.8263(4) 0.6923(3) 0.5008(3) 0.0360(7) Uani 1 1 d . . . H21 H 0.8914 0.6183 0.4890 0.043 Uiso 1 1 calc R . . C22 C 0.8749(4) 0.8197(4) 0.5015(3) 0.0382(8) Uani 1 1 d . . . H22 H 0.9788 0.8495 0.4897 0.046 Uiso 1 1 calc R . . C23 C 0.7480(4) 0.8999(3) 0.5113(3) 0.0380(8) Uani 1 1 d . . . H23 H 0.7490 0.9947 0.5091 0.046 Uiso 1 1 calc R . . O1 O 0.8360(3) 0.4973(2) 0.8229(2) 0.0491(6) Uani 1 1 d . . . O2 O 0.3707(3) 0.6054(3) 0.8718(2) 0.0506(6) Uani 1 1 d . . . B1 B 0.7388(4) 0.3320(4) 0.4785(4) 0.0391(9) Uani 1 1 d . . . F1 F 0.7532(3) 0.1998(2) 0.5304(3) 0.0813(9) Uani 1 1 d . . . F2 F 0.6927(3) 0.3465(4) 0.3761(2) 0.1048(12) Uani 1 1 d . . . F3 F 0.8767(2) 0.4037(2) 0.4331(2) 0.0623(6) Uani 1 1 d . . . F4 F 0.6271(2) 0.3771(2) 0.56677(18) 0.0552(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.02841(14) 0.02158(14) 0.02569(13) -0.00777(9) -0.01386(9) 0.00367(9) S1 0.0276(4) 0.0239(4) 0.0250(3) -0.0079(3) -0.0120(3) 0.0020(3) C1 0.0372(17) 0.0336(17) 0.0276(15) -0.0095(13) -0.0110(13) -0.0030(14) C2 0.0272(16) 0.044(2) 0.0386(17) -0.0223(15) -0.0053(13) -0.0005(14) C3 0.0297(16) 0.0366(18) 0.0456(18) -0.0217(15) -0.0154(14) 0.0072(14) C4 0.0329(16) 0.0245(15) 0.0354(16) -0.0133(12) -0.0163(13) 0.0018(12) C6 0.0320(16) 0.0338(17) 0.0343(16) -0.0142(13) -0.0156(13) 0.0016(13) C7 0.0373(18) 0.0380(19) 0.0433(18) -0.0132(15) -0.0239(15) 0.0073(15) C8 0.049(2) 0.0340(18) 0.0394(18) -0.0080(14) -0.0280(15) 0.0048(15) C9 0.0409(18) 0.0288(16) 0.0289(15) -0.0063(13) -0.0161(13) 0.0006(13) C10 0.0343(16) 0.0218(15) 0.0280(14) -0.0084(12) -0.0154(12) 0.0005(12) C11 0.0309(15) 0.0225(15) 0.0285(14) -0.0113(12) -0.0111(12) 0.0003(12) C12 0.0340(16) 0.0240(15) 0.0265(14) -0.0080(12) -0.0158(12) 0.0008(12) C13 0.0268(14) 0.0244(15) 0.0277(14) -0.0113(12) -0.0103(11) 0.0020(12) C14 0.0402(18) 0.0343(18) 0.0396(17) -0.0115(14) -0.0222(14) 0.0091(14) C16 0.0300(17) 0.060(2) 0.0407(18) -0.0160(17) -0.0128(14) 0.0018(16) C17 0.0394(17) 0.0276(17) 0.0330(16) -0.0076(13) -0.0178(14) 0.0035(14) C18 0.0403(19) 0.0289(17) 0.0383(17) -0.0154(14) -0.0174(15) 0.0019(14) C19 0.0474(19) 0.0375(18) 0.0269(15) -0.0095(13) -0.0223(14) 0.0148(15) C20 0.051(2) 0.0382(19) 0.0319(16) -0.0174(14) -0.0253(15) 0.0069(15) C21 0.0444(19) 0.0399(19) 0.0272(15) -0.0145(14) -0.0138(13) 0.0106(15) C22 0.0370(17) 0.048(2) 0.0273(15) -0.0076(14) -0.0102(13) -0.0052(15) C23 0.065(2) 0.0261(17) 0.0243(15) -0.0048(13) -0.0202(15) 0.0043(16) O1 0.0635(16) 0.0342(14) 0.0535(15) -0.0052(11) -0.0324(13) 0.0142(12) O2 0.0403(14) 0.0503(16) 0.0550(15) -0.0211(13) -0.0039(12) -0.0116(12) B1 0.033(2) 0.046(2) 0.038(2) -0.0156(17) -0.0102(16) 0.0037(17) F1 0.0710(16) 0.0287(12) 0.103(2) -0.0144(12) 0.0144(14) 0.0037(11) F2 0.0584(16) 0.211(4) 0.0598(16) -0.059(2) -0.0237(13) 0.0093(19) F3 0.0435(12) 0.0478(13) 0.0882(17) -0.0132(12) -0.0196(12) -0.0026(10) F4 0.0582(13) 0.0549(14) 0.0427(11) -0.0160(10) -0.0065(10) 0.0227(11) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C17 Ru1 C18 90.44(13) . . ? C17 Ru1 C20 113.86(13) . . ? C18 Ru1 C20 98.02(13) . . ? C17 Ru1 C21 91.82(12) . . ? C18 Ru1 C21 129.99(13) . . ? C20 Ru1 C21 37.27(11) . . ? C17 Ru1 C22 105.20(13) . . ? C18 Ru1 C22 158.63(13) . . ? C20 Ru1 C22 62.56(12) . . ? C21 Ru1 C22 37.24(12) . . ? C17 Ru1 C19 150.98(13) . . ? C18 Ru1 C19 97.44(13) . . ? C20 Ru1 C19 37.47(12) . . ? C21 Ru1 C19 61.87(12) . . ? C22 Ru1 C19 61.92(12) . . ? C17 Ru1 C23 141.81(13) . . ? C18 Ru1 C23 127.47(13) . . ? C20 Ru1 C23 62.04(12) . . ? C21 Ru1 C23 61.74(12) . . ? C22 Ru1 C23 37.19(12) . . ? C19 Ru1 C23 36.53(12) . . ? C17 Ru1 S1 93.66(9) . . ? C18 Ru1 S1 91.30(9) . . ? C20 Ru1 S1 150.71(9) . . ? C21 Ru1 S1 138.30(9) . . ? C22 Ru1 S1 101.92(9) . . ? C19 Ru1 S1 113.92(9) . . ? C23 Ru1 S1 90.32(8) . . ? C12 S1 C13 90.88(13) . . ? C12 S1 Ru1 109.96(10) . . ? C13 S1 Ru1 108.42(10) . . ? C2 C1 C11 118.7(3) . . ? C3 C2 C1 121.1(3) . . ? C2 C3 C4 122.5(3) . . ? C13 C4 C3 115.5(3) . . ? C13 C4 C14 122.5(3) . . ? C3 C4 C14 122.0(3) . . ? C7 C6 C12 115.8(3) . . ? C7 C6 C16 122.0(3) . . ? C12 C6 C16 122.3(3) . . ? C8 C7 C6 122.3(3) . . ? C7 C8 C9 120.8(3) . . ? C8 C9 C10 118.8(3) . . ? C9 C10 C12 118.7(3) . . ? C9 C10 C11 129.1(3) . . ? C12 C10 C11 112.2(2) . . ? C1 C11 C13 118.5(3) . . ? C1 C11 C10 128.5(3) . . ? C13 C11 C10 113.0(2) . . ? C6 C12 C10 123.6(3) . . ? C6 C12 S1 124.2(2) . . ? C10 C12 S1 112.2(2) . . ? C4 C13 C11 123.7(3) . . ? C4 C13 S1 124.8(2) . . ? C11 C13 S1 111.5(2) . . ? O1 C17 Ru1 176.8(3) . . ? O2 C18 Ru1 178.7(3) . . ? C23 C19 C20 108.5(3) . . ? C23 C19 Ru1 72.24(17) . . ? C20 C19 Ru1 70.61(16) . . ? C21 C20 C19 107.1(3) . . ? C21 C20 Ru1 71.66(17) . . ? C19 C20 Ru1 71.93(16) . . ? C20 C21 C22 108.7(3) . . ? C20 C21 Ru1 71.07(17) . . ? C22 C21 Ru1 71.65(17) . . ? C21 C22 C23 107.2(3) . . ? C21 C22 Ru1 71.11(17) . . ? C23 C22 Ru1 72.00(18) . . ? C19 C23 C22 108.4(3) . . ? C19 C23 Ru1 71.23(17) . . ? C22 C23 Ru1 70.81(17) . . ? F3 B1 F1 110.1(3) . . ? F3 B1 F4 113.5(3) . . ? F1 B1 F4 109.1(3) . . ? F3 B1 F2 107.0(3) . . ? F1 B1 F2 109.6(4) . . ? F4 B1 F2 107.4(3) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C17 1.906(3) . ? Ru1 C18 1.915(3) . ? Ru1 C20 2.208(3) . ? Ru1 C21 2.216(3) . ? Ru1 C22 2.223(3) . ? Ru1 C19 2.226(3) . ? Ru1 C23 2.239(3) . ? Ru1 S1 2.4051(7) . ? S1 C12 1.778(3) . ? S1 C13 1.781(3) . ? C1 C2 1.384(4) . ? C1 C11 1.401(4) . ? C2 C3 1.381(4) . ? C3 C4 1.391(4) . ? C4 C13 1.390(4) . ? C4 C14 1.496(4) . ? C6 C7 1.388(4) . ? C6 C12 1.389(4) . ? C6 C16 1.512(4) . ? C7 C8 1.383(5) . ? C8 C9 1.387(4) . ? C9 C10 1.395(4) . ? C10 C12 1.397(4) . ? C10 C11 1.460(4) . ? C11 C13 1.402(4) . ? C17 O1 1.131(4) . ? C18 O2 1.134(4) . ? C19 C23 1.399(5) . ? C19 C20 1.424(4) . ? C20 C21 1.414(4) . ? C21 C22 1.417(5) . ? C22 C23 1.423(5) . ? B1 F3 1.362(4) . ? B1 F1 1.362(5) . ? B1 F4 1.371(4) . ? B1 F2 1.381(4) . ?
1100787.cif	#------------------------------------------------------------------------------ #$Date: 2016-03-28 07:01:53 +0300 (Mon, 28 Mar 2016) $ #$Revision: 180559 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100787.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100787 loop_ _publ_author_name 'Vecchi, Paul A.' 'Ellern, Arkady' 'Angelici, Robert J.' _publ_section_title ; Steric Effects in the Binding of Hindered Dibenzothiophene Ligands in [Cp'Ru(CO)~2~(\h^1^(S)-DBTh)]^+^ Complexes ; _journal_coden_ASTM ORGND7 _journal_issue 9 _journal_name_full Organometallics _journal_page_first 2168 _journal_page_last 2176 _journal_paper_doi 10.1021/om048973l _journal_volume 24 _journal_year 2005 _chemical_formula_sum 'C21 H17 B F4 O2 Ru S' _chemical_formula_weight 521.29 _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 98.660(8) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 9.394(4) _cell_length_b 11.003(5) _cell_length_c 19.963(9) _cell_measurement_reflns_used 968 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 27.98 _cell_measurement_theta_min 3.72 _cell_volume 2039.7(16) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 173(2) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.928 _diffrn_measured_fraction_theta_max 0.928 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0394 _diffrn_reflns_av_sigmaI/netI 0.0317 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 19275 _diffrn_reflns_theta_full 28.29 _diffrn_reflns_theta_max 28.29 _diffrn_reflns_theta_min 2.06 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _exptl_absorpt_coefficient_mu 0.922 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_correction_T_min 0.88 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ? _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.698 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 1040 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.23 _refine_diff_density_max 2.791 _refine_diff_density_min -1.821 _refine_diff_density_rms 0.187 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.222 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 271 _refine_ls_number_reflns 4706 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.222 _refine_ls_R_factor_all 0.0833 _refine_ls_R_factor_gt 0.0787 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0184P)^2^+37.5477P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1925 _refine_ls_wR_factor_ref 0.1945 _reflns_number_gt 4286 _reflns_number_total 4706 _reflns_threshold_expression >2sigma(I) _cod_duplicate_entry 4060279 _cod_data_source_file om048973lsi20050303_083418.cif _cod_data_source_block complex4 _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'none' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas ; _cod_original_sg_symbol_H-M P2(1)/n _cod_database_code 1100787 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.72984(7) 0.35635(5) 0.86245(3) 0.02182(18) Uani 1 1 d . . . S1 S 0.91539(19) 0.23719(15) 0.92743(9) 0.0189(4) Uani 1 1 d . . . C1 C 1.0391(7) -0.0675(6) 0.8479(4) 0.0190(14) Uani 1 1 d . . . H1 H 1.0181 -0.1513 0.8527 0.023 Uiso 1 1 calc R . . C2 C 1.1427(9) -0.0296(7) 0.8066(4) 0.0240(15) Uani 1 1 d . . . C3 C 1.1724(8) 0.0952(7) 0.8011(4) 0.0230(15) Uani 1 1 d . . . H3 H 1.2417 0.1201 0.7738 0.028 Uiso 1 1 calc R . . C4 C 1.1033(8) 0.1823(7) 0.8343(4) 0.0234(15) Uani 1 1 d . . . H4 H 1.1240 0.2663 0.8304 0.028 Uiso 1 1 calc R . . C6 C 0.7383(8) 0.1110(7) 1.0068(4) 0.0228(15) Uani 1 1 d . . . H6 H 0.7166 0.1849 1.0277 0.027 Uiso 1 1 calc R . . C7 C 0.6799(8) 0.0015(7) 1.0239(4) 0.0238(15) Uani 1 1 d . . . H7 H 0.6163 0.0012 1.0567 0.029 Uiso 1 1 calc R . . C8 C 0.7122(8) -0.1085(7) 0.9942(4) 0.0237(15) Uani 1 1 d . . . C9 C 0.8076(8) -0.1086(7) 0.9477(4) 0.0242(15) Uani 1 1 d . . . H9 H 0.8329 -0.1832 0.9286 0.029 Uiso 1 1 calc R . . C10 C 0.8667(7) -0.0003(6) 0.9284(4) 0.0192(14) Uani 1 1 d . . . C11 C 0.9700(8) 0.0199(6) 0.8808(4) 0.0210(14) Uani 1 1 d . . . C12 C 0.8293(8) 0.1090(6) 0.9582(4) 0.0192(14) Uani 1 1 d . . . C13 C 1.0026(8) 0.1426(7) 0.8738(4) 0.0210(14) Uani 1 1 d . . . C14 C 1.2231(11) -0.1213(7) 0.7710(5) 0.0334(19) Uani 1 1 d . . . H14A H 1.2888 -0.0791 0.7451 0.050 Uiso 1 1 calc R . . H14B H 1.1545 -0.1699 0.7402 0.050 Uiso 1 1 calc R . . H14C H 1.2785 -0.1748 0.8045 0.050 Uiso 1 1 calc R . . C16 C 0.6447(9) -0.2260(7) 1.0136(5) 0.0320(18) Uani 1 1 d . . . H16A H 0.5810 -0.2091 1.0471 0.048 Uiso 1 1 calc R . . H16B H 0.7206 -0.2824 1.0329 0.048 Uiso 1 1 calc R . . H16C H 0.5888 -0.2625 0.9731 0.048 Uiso 1 1 calc R . . C17 C 0.6132(10) 0.2152(8) 0.8415(5) 0.0347(19) Uani 1 1 d . . . C18 C 0.8069(11) 0.3413(9) 0.7797(5) 0.038(2) Uani 1 1 d . . . C19 C 0.7813(10) 0.5105(7) 0.9349(5) 0.0315(18) Uani 1 1 d . . . H19 H 0.8713 0.5192 0.9684 0.038 Uiso 1 1 calc R . . C20 C 0.7582(10) 0.5590(7) 0.8695(5) 0.035(2) Uani 1 1 d . . . H20 H 0.8278 0.6088 0.8478 0.041 Uiso 1 1 calc R . . C21 C 0.6127(11) 0.5295(8) 0.8408(5) 0.041(2) Uani 1 1 d . . . H21 H 0.5624 0.5564 0.7955 0.049 Uiso 1 1 calc R . . C22 C 0.5492(11) 0.4669(8) 0.8900(6) 0.044(2) Uani 1 1 d . . . H22 H 0.4462 0.4407 0.8854 0.053 Uiso 1 1 calc R . . C23 C 0.6514(10) 0.4534(8) 0.9475(5) 0.036(2) Uani 1 1 d . . . H23 H 0.6346 0.4162 0.9913 0.043 Uiso 1 1 calc R . . O1 O 0.5427(9) 0.1317(7) 0.8311(4) 0.053(2) Uani 1 1 d . . . O2 O 0.8472(11) 0.3373(9) 0.7286(4) 0.068(3) Uani 1 1 d . . . B1 B 0.8510(12) 0.4150(9) 0.1187(5) 0.033(2) Uani 1 1 d . . . F1 F 0.7126(6) 0.3663(6) 0.1154(4) 0.0534(16) Uani 1 1 d . . . F2 F 0.9183(6) 0.3607(5) 0.0698(3) 0.0409(12) Uani 1 1 d . . . F3 F 0.8387(9) 0.5391(5) 0.1073(3) 0.0614(19) Uani 1 1 d . . . F4 F 0.9278(7) 0.3924(6) 0.1826(3) 0.0495(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0229(3) 0.0176(3) 0.0244(3) 0.0005(2) 0.0019(2) 0.0038(2) S1 0.0209(8) 0.0144(8) 0.0221(8) -0.0008(6) 0.0051(7) 0.0022(6) C1 0.015(3) 0.015(3) 0.028(4) 0.001(3) 0.006(3) 0.002(3) C2 0.031(4) 0.016(3) 0.026(4) -0.005(3) 0.007(3) 0.001(3) C3 0.021(4) 0.027(4) 0.022(3) 0.007(3) 0.004(3) -0.003(3) C4 0.023(4) 0.019(3) 0.026(4) 0.006(3) 0.000(3) 0.000(3) C6 0.023(4) 0.024(4) 0.022(3) -0.002(3) 0.002(3) 0.003(3) C7 0.023(4) 0.026(4) 0.024(4) 0.000(3) 0.007(3) -0.002(3) C8 0.021(4) 0.021(3) 0.029(4) 0.004(3) 0.002(3) 0.000(3) C9 0.026(4) 0.017(3) 0.028(4) -0.002(3) 0.000(3) -0.001(3) C10 0.015(3) 0.019(3) 0.024(3) 0.004(3) 0.003(3) 0.003(3) C11 0.023(4) 0.016(3) 0.023(4) 0.001(3) 0.000(3) -0.001(3) C12 0.020(3) 0.015(3) 0.021(3) 0.002(3) 0.002(3) 0.004(3) C13 0.023(3) 0.018(3) 0.021(3) -0.002(3) 0.002(3) 0.005(3) C14 0.048(5) 0.022(4) 0.033(4) 0.001(3) 0.016(4) 0.009(4) C16 0.031(4) 0.024(4) 0.044(5) 0.003(4) 0.012(4) -0.006(3) C17 0.033(5) 0.035(5) 0.034(5) -0.003(4) -0.001(4) 0.006(4) C18 0.050(6) 0.037(5) 0.028(4) 0.006(4) 0.004(4) 0.013(4) C19 0.032(4) 0.021(4) 0.040(5) -0.005(3) 0.002(4) 0.003(3) C20 0.039(5) 0.017(4) 0.047(5) 0.004(3) 0.002(4) 0.003(3) C21 0.046(5) 0.020(4) 0.051(6) -0.002(4) -0.012(4) 0.015(4) C22 0.031(5) 0.027(4) 0.075(7) -0.012(5) 0.008(5) 0.008(4) C23 0.040(5) 0.025(4) 0.045(5) -0.011(4) 0.019(4) 0.001(4) O1 0.055(5) 0.035(4) 0.064(5) -0.003(4) -0.009(4) -0.014(3) O2 0.089(7) 0.080(6) 0.039(4) 0.013(4) 0.024(4) 0.024(5) B1 0.049(6) 0.020(4) 0.031(5) 0.000(4) 0.011(4) 0.000(4) F1 0.037(3) 0.054(4) 0.072(4) 0.007(3) 0.018(3) 0.003(3) F2 0.043(3) 0.040(3) 0.041(3) -0.011(2) 0.011(2) -0.001(3) F3 0.105(6) 0.022(3) 0.058(4) 0.003(3) 0.016(4) 0.006(3) F4 0.057(4) 0.060(4) 0.031(3) 0.005(3) 0.006(3) -0.005(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C18 Ru1 C17 91.1(4) . . ? C18 Ru1 C21 98.5(4) . . ? C17 Ru1 C21 113.9(4) . . ? C18 Ru1 C23 156.3(4) . . ? C17 Ru1 C23 108.2(4) . . ? C21 Ru1 C23 61.5(4) . . ? C18 Ru1 C22 131.7(4) . . ? C17 Ru1 C22 93.7(4) . . ? C21 Ru1 C22 37.0(4) . . ? C23 Ru1 C22 36.4(4) . . ? C18 Ru1 C19 123.6(4) . . ? C17 Ru1 C19 145.1(4) . . ? C21 Ru1 C19 61.7(3) . . ? C23 Ru1 C19 37.4(3) . . ? C22 Ru1 C19 61.5(4) . . ? C18 Ru1 C20 94.8(4) . . ? C17 Ru1 C20 151.5(4) . . ? C21 Ru1 C20 37.6(3) . . ? C23 Ru1 C20 61.6(4) . . ? C22 Ru1 C20 61.9(4) . . ? C19 Ru1 C20 36.3(3) . . ? C18 Ru1 S1 94.7(3) . . ? C17 Ru1 S1 91.2(3) . . ? C21 Ru1 S1 151.2(3) . . ? C23 Ru1 S1 98.4(3) . . ? C22 Ru1 S1 133.2(3) . . ? C19 Ru1 S1 89.8(2) . . ? C20 Ru1 S1 116.0(2) . . ? C13 S1 C12 91.1(3) . . ? C13 S1 Ru1 110.9(2) . . ? C12 S1 Ru1 106.8(2) . . ? C11 C1 C2 118.7(7) . . ? C11 C1 H1 120.6 . . ? C2 C1 H1 120.6 . . ? C3 C2 C1 119.3(7) . . ? C3 C2 C14 119.9(7) . . ? C1 C2 C14 120.8(7) . . ? C4 C3 C2 121.7(7) . . ? C4 C3 H3 119.1 . . ? C2 C3 H3 119.1 . . ? C3 C4 C13 117.6(7) . . ? C3 C4 H4 121.2 . . ? C13 C4 H4 121.2 . . ? C12 C6 C7 117.8(7) . . ? C12 C6 H6 121.1 . . ? C7 C6 H6 121.1 . . ? C6 C7 C8 121.8(7) . . ? C6 C7 H7 119.1 . . ? C8 C7 H7 119.1 . . ? C9 C8 C7 119.2(7) . . ? C9 C8 C16 120.5(7) . . ? C7 C8 C16 120.3(7) . . ? C8 C9 C10 120.6(7) . . ? C8 C9 H9 119.7 . . ? C10 C9 H9 119.7 . . ? C9 C10 C12 118.6(7) . . ? C9 C10 C11 129.5(7) . . ? C12 C10 C11 111.9(6) . . ? C1 C11 C13 120.1(7) . . ? C1 C11 C10 127.1(7) . . ? C13 C11 C10 112.7(6) . . ? C6 C12 C10 121.9(7) . . ? C6 C12 S1 126.0(6) . . ? C10 C12 S1 112.0(5) . . ? C4 C13 C11 122.6(7) . . ? C4 C13 S1 124.9(6) . . ? C11 C13 S1 112.2(6) . . ? C2 C14 H14A 109.5 . . ? C2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C8 C16 H16A 109.5 . . ? C8 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C8 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O1 C17 Ru1 177.7(9) . . ? O2 C18 Ru1 176.0(9) . . ? C20 C19 C23 108.4(8) . . ? C20 C19 Ru1 72.4(5) . . ? C23 C19 Ru1 70.9(5) . . ? C20 C19 H19 125.7 . . ? C23 C19 H19 125.7 . . ? Ru1 C19 H19 125.7 . . ? C19 C20 C21 106.9(9) . . ? C19 C20 Ru1 71.3(5) . . ? C21 C20 Ru1 69.8(5) . . ? C19 C20 H20 126.5 . . ? C21 C20 H20 126.5 . . ? Ru1 C20 H20 126.5 . . ? C22 C21 C20 108.0(9) . . ? C22 C21 Ru1 72.0(5) . . ? C20 C21 Ru1 72.6(5) . . ? C22 C21 H21 125.9 . . ? C20 C21 H21 125.9 . . ? Ru1 C21 H21 125.9 . . ? C23 C22 C21 108.5(9) . . ? C23 C22 Ru1 71.8(5) . . ? C21 C22 Ru1 71.0(5) . . ? C23 C22 H22 125.7 . . ? C21 C22 H22 125.7 . . ? Ru1 C22 H22 125.7 . . ? C22 C23 C19 108.1(9) . . ? C22 C23 Ru1 71.8(5) . . ? C19 C23 Ru1 71.8(5) . . ? C22 C23 H23 125.9 . . ? C19 C23 H23 125.9 . . ? Ru1 C23 H23 125.9 . . ? F2 B1 F3 110.2(8) . . ? F2 B1 F4 110.1(8) . . ? F3 B1 F4 110.3(8) . . ? F2 B1 F1 108.9(8) . . ? F3 B1 F1 108.4(9) . . ? F4 B1 F1 109.0(8) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C18 1.909(9) . ? Ru1 C17 1.910(10) . ? Ru1 C21 2.211(8) . ? Ru1 C23 2.223(8) . ? Ru1 C22 2.223(9) . ? Ru1 C19 2.235(8) . ? Ru1 C20 2.248(8) . ? Ru1 S1 2.400(2) . ? S1 C13 1.779(7) . ? S1 C12 1.781(7) . ? C1 C11 1.380(10) . ? C1 C2 1.430(10) . ? C1 H1 0.9500 . ? C2 C3 1.409(10) . ? C2 C14 1.501(10) . ? C3 C4 1.382(11) . ? C3 H3 0.9500 . ? C4 C13 1.389(11) . ? C4 H4 0.9500 . ? C6 C12 1.387(10) . ? C6 C7 1.387(11) . ? C6 H6 0.9500 . ? C7 C8 1.401(11) . ? C7 H7 0.9500 . ? C8 C9 1.386(11) . ? C8 C16 1.515(10) . ? C9 C10 1.392(10) . ? C9 H9 0.9500 . ? C10 C12 1.409(10) . ? C10 C11 1.475(10) . ? C11 C13 1.396(10) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 O1 1.134(11) . ? C18 O2 1.140(11) . ? C19 C20 1.397(13) . ? C19 C23 1.427(12) . ? C19 H19 1.0000 . ? C20 C21 1.438(13) . ? C20 H20 1.0000 . ? C21 C22 1.406(15) . ? C21 H21 1.0000 . ? C22 C23 1.389(15) . ? C22 H22 1.0000 . ? C23 H23 1.0000 . ? B1 F2 1.378(11) . ? B1 F3 1.387(11) . ? B1 F4 1.389(12) . ? B1 F1 1.398(12) . ?
1100788.cif	#------------------------------------------------------------------------------ #$Date: 2022-09-14 17:31:13 +0300 (Wed, 14 Sep 2022) $ #$Revision: 277831 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/10/07/1100788.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100788 loop_ _publ_author_name 'Hidenobu Kajitani' 'Yoshiaki Tanabe' 'Shigeki Kuwata' 'Masakazu Iwasaki' 'Youichi Ishii' _publ_section_title ; Cyanamido-Bridged Diiridium Complex: a Reactive Building Block for Polynuclear Cyanamido Complexes ; _journal_issue 10 _journal_name_full Organometallics _journal_page_first 2251 _journal_page_last 2254 _journal_paper_doi 10.1021/om048978i _journal_volume 24 _journal_year 2005 _chemical_formula_moiety 'C22 H30 Ir2 N4 ' _chemical_formula_sum 'C22 H30 Ir2 N4' _chemical_formula_weight 734.95 _space_group_IT_number 62 _space_group_name_Hall '-P 2ac 2n' _space_group_name_H-M_alt 'P n m a' _symmetry_cell_setting orthorhombic _symmetry_Int_Tables_number 62 _symmetry_space_group_name_Hall '-P 2ac 2n' _symmetry_space_group_name_H-M 'P n m a' _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 21.365(6) _cell_length_b 15.428(5) _cell_length_c 6.697(5) _cell_measurement_reflns_used 25 _cell_measurement_temperature 294.1 _cell_measurement_theta_max 20.0 _cell_measurement_theta_min 19.8 _cell_volume 2207(1) _diffrn_measured_fraction_theta_full 0.9898 _diffrn_measured_fraction_theta_max 0.9898 _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_number 2908 _diffrn_reflns_theta_full 27.51 _diffrn_reflns_theta_max 27.51 _diffrn_standards_decay_% 0.27 _diffrn_standards_interval_count 0 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 12.093 _exptl_absorpt_correction_T_max 0.089 _exptl_absorpt_correction_T_min 0.033 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_crystal_colour 'dark red' _exptl_crystal_density_diffrn 2.211 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 1376.00 _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _refine_diff_density_max 5.93 _refine_diff_density_min -3.41 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_hydrogen_treatment refall _refine_ls_number_parameters 156 _refine_ls_number_reflns 1731 _refine_ls_R_factor_gt 0.0520 _refine_ls_shift/su_max 0.0000 _refine_ls_structure_factor_coef F _refine_ls_weighting_details 'w = 1/[0.0004Fo^2^ + 4.0000\s(Fo^2^) + 0.5000]' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.0540 _reflns_number_gt 1731 _reflns_number_total 2519 _reflns_threshold_expression F^2^>3.0\s(F^2^) _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_absorpt_correction_type' tag value 'psi-scans' was replaced with 'psi-scan' value. Automatic conversion script Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana ; _cod_original_formula_sum 'C22 H30 Ir2 N4 ' _cod_database_code 1100788 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2-X,1/2+Y,1/2+Z 3 +X,1/2-Y,+Z 4 1/2-X,-Y,1/2+Z 5 -X,-Y,-Z 6 1/2+X,1/2-Y,1/2-Z 7 -X,1/2+Y,-Z 8 1/2+X,+Y,1/2-Z loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir(1) Ir 0.43198(3) 0.2500 0.31218(9) 0.0270(2) Uani 1.00 2 d S . . Ir(2) Ir 0.30015(3) 0.2500 0.3253(1) 0.0288(2) Uani 1.00 2 d S . . N(1) N 0.3668(5) 0.1705(9) 0.429(2) 0.048(4) Uani 1.00 1 d . . . N(2) N 0.3667(7) 0.013(1) 0.365(4) 0.098(6) Uani 1.00 1 d . . . C(1) C 0.3660(7) 0.087(1) 0.391(3) 0.066(5) Uani 1.00 1 d . . . C(2) C 0.4793(7) 0.2032(8) 0.057(2) 0.039(4) Uani 1.00 1 d . . . C(3) C 0.5140(7) 0.1755(9) 0.228(2) 0.042(4) Uani 1.00 1 d . . . C(4) C 0.5311(7) 0.2500 0.335(2) 0.032(5) Uani 1.00 2 d S . . C(5) C 0.4509(9) 0.148(1) -0.104(3) 0.076(6) Uani 1.00 1 d . . . C(6) C 0.524(1) 0.081(1) 0.275(3) 0.087(7) Uani 1.00 1 d . . . C(7) C 0.569(1) 0.25000(1) 0.514(3) 0.079(9) Uani 1.00 2 d S . . C(8) C 0.2485(6) 0.2026(8) 0.070(2) 0.036(4) Uani 1.00 1 d . . . C(9) C 0.2178(6) 0.1756(9) 0.253(2) 0.045(4) Uani 1.00 1 d . . . C(10) C 0.1997(8) 0.2500 0.364(3) 0.036(5) Uani 1.00 2 d S . . C(11) C 0.2749(8) 0.144(1) -0.087(2) 0.055(5) Uani 1.00 1 d . . . C(12) C 0.2074(9) 0.080(1) 0.306(3) 0.076(6) Uani 1.00 1 d . . . C(13) C 0.163(1) 0.25000(1) 0.555(4) 0.077(9) Uani 1.00 2 d S . . H(1) H 0.4218 0.1100 -0.0410 0.091 Uiso 1.00 1 c R . . H(2) H 0.4298 0.1814 -0.2020 0.091 Uiso 1.00 1 c R . . H(3) H 0.4827 0.1142 -0.1668 0.091 Uiso 1.00 1 c R . . H(4) H 0.5041 0.0692 0.3989 0.104 Uiso 1.00 1 c R . . H(5) H 0.5063 0.0455 0.1738 0.104 Uiso 1.00 1 c R . . H(6) H 0.5676 0.0685 0.2864 0.104 Uiso 1.00 1 c R . . H(7) H 0.5475 0.2192 0.6147 0.095 Uiso 0.50 1 c R . . H(8) H 0.6086 0.2227 0.4899 0.095 Uiso 0.50 1 c R . . H(9) H 0.5762 0.3080 0.5561 0.095 Uiso 0.50 1 c R . . H(10) H 0.2423 0.1093 -0.1403 0.066 Uiso 1.00 1 c R . . H(11) H 0.2932 0.1774 -0.1918 0.066 Uiso 1.00 1 c R . . H(12) H 0.3059 0.1082 -0.0288 0.066 Uiso 1.00 1 c R . . H(13) H 0.1639 0.0697 0.3234 0.092 Uiso 1.00 1 c R . . H(14) H 0.2233 0.0430 0.2051 0.092 Uiso 1.00 1 c R . . H(15) H 0.2286 0.0692 0.4282 0.092 Uiso 1.00 1 c R . . H(16) H 0.1571 0.3080 0.5995 0.092 Uiso 0.50 1 c R . . H(17) H 0.1230 0.2236 0.5356 0.092 Uiso 0.50 1 c R . . H(18) H 0.1855 0.2184 0.6527 0.092 Uiso 0.50 1 c R . . loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ir Ir -1.444 7.990 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ;
1100789.cif	#------------------------------------------------------------------------------ #$Date: 2022-09-14 17:31:13 +0300 (Wed, 14 Sep 2022) $ #$Revision: 277831 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/10/07/1100789.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100789 loop_ _publ_author_name 'Hidenobu Kajitani' 'Yoshiaki Tanabe' 'Shigeki Kuwata' 'Masakazu Iwasaki' 'Youichi Ishii' _publ_section_title ; Cyanamido-Bridged Diiridium Complex: a Reactive Building Block for Polynuclear Cyanamido Complexes ; _journal_issue 10 _journal_name_full Organometallics _journal_page_first 2251 _journal_page_last 2254 _journal_paper_doi 10.1021/om048978i _journal_volume 24 _journal_year 2005 _chemical_formula_moiety 'C24 H30 Ir2 N4 O2 ' _chemical_formula_sum 'C24 H30 Ir2 N4 O2' _chemical_formula_weight 790.97 _chemical_melting_point ? _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_cell_setting triclinic _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _cell_angle_alpha 88.75(3) _cell_angle_beta 86.05(4) _cell_angle_gamma 76.30(4) _cell_formula_units_Z 2 _cell_length_a 8.888(5) _cell_length_b 11.704(4) _cell_length_c 12.696(4) _cell_measurement_reflns_used 25 _cell_measurement_temperature 294.1 _cell_measurement_theta_max 20.0 _cell_measurement_theta_min 19.9 _cell_volume 1280.2(9) _diffrn_measured_fraction_theta_full 0.9959 _diffrn_measured_fraction_theta_max 0.9959 _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents 0.021 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 6165 _diffrn_reflns_theta_full 27.51 _diffrn_reflns_theta_max 27.51 _diffrn_standards_decay_% 0.01 _diffrn_standards_interval_count 0 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 10.440 _exptl_absorpt_correction_T_max 0.352 _exptl_absorpt_correction_T_min 0.144 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_crystal_colour 'dark brown' _exptl_crystal_density_diffrn 2.052 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 744.00 _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _refine_diff_density_max 1.21 _refine_diff_density_min -1.35 _refine_ls_extinction_coef 38(3) _refine_ls_extinction_method 'Larson (1970) Crystallographic Computing eq. 22' _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_hydrogen_treatment refall _refine_ls_number_parameters 320 _refine_ls_number_reflns 4755 _refine_ls_R_factor_gt 0.0260 _refine_ls_shift/su_max 0.0000 _refine_ls_structure_factor_coef F _refine_ls_weighting_details 'w = 1/[0.0001Fo^2^ + 1.8000\s(Fo^2^) + 0.5000]' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.0260 _reflns_number_gt 4755 _reflns_number_total 5779 _reflns_threshold_expression F^2^>3.0\s(F^2^) _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_absorpt_correction_type' tag value 'psi-scans' was replaced with 'psi-scan' value. Automatic conversion script Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana ; _cod_original_formula_sum 'C24 H30 Ir2 N4 O2 ' _cod_database_code 1100789 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir(1) Ir 0.75251(3) 0.64738(2) 0.76861(2) 0.04492(7) Uani 1.00 1 d . . . Ir(2) Ir 0.66854(2) 0.96071(2) 0.77909(1) 0.03169(6) Uani 1.00 1 d . . . O(1) O 0.4675(5) 0.7028(5) 0.6589(5) 0.090(2) Uani 1.00 1 d . . . O(2) O 0.550(1) 0.5936(7) 0.9517(7) 0.185(4) Uani 1.00 1 d . . . N(1) N 0.5312(5) 0.8681(4) 0.7117(4) 0.045(1) Uani 1.00 1 d . . . N(2) N 0.2909(7) 0.9836(6) 0.6348(5) 0.084(2) Uani 1.00 1 d . . . N(3) N 0.7620(5) 0.8053(4) 0.8366(3) 0.041(1) Uani 1.00 1 d . . . N(4) N 0.9530(7) 0.7755(5) 0.9740(4) 0.064(2) Uani 1.00 1 d . . . C(1) C 0.5558(7) 0.7451(6) 0.7048(5) 0.055(2) Uani 1.00 1 d . . . C(2) C 0.4020(7) 0.9287(6) 0.6686(5) 0.055(2) Uani 1.00 1 d . . . C(3) C 0.8637(7) 0.7898(5) 0.9090(4) 0.044(1) Uani 1.00 1 d . . . C(4) C 0.630(1) 0.6151(7) 0.8821(7) 0.096(3) Uani 1.00 1 d . . . C(5) C 0.8825(7) 0.6176(5) 0.6097(4) 0.053(2) Uani 1.00 1 d . . . C(6) C 0.9921(7) 0.6261(5) 0.6832(5) 0.054(2) Uani 1.00 1 d . . . C(7) C 1.0015(8) 0.5352(6) 0.7591(6) 0.066(2) Uani 1.00 1 d . . . C(8) C 0.896(1) 0.4674(5) 0.7326(6) 0.070(2) Uani 1.00 1 d . . . C(9) C 0.8193(8) 0.5174(6) 0.6400(5) 0.064(2) Uani 1.00 1 d . . . C(10) C 0.845(1) 0.6928(8) 0.5139(6) 0.095(3) Uani 1.00 1 d . . . C(11) C 1.0834(8) 0.7184(7) 0.6812(7) 0.085(3) Uani 1.00 1 d . . . C(12) C 1.114(1) 0.5056(8) 0.8448(7) 0.107(3) Uani 1.00 1 d . . . C(13) C 0.872(2) 0.3563(7) 0.7861(8) 0.129(4) Uani 1.00 1 d . . . C(14) C 0.711(1) 0.4690(8) 0.5789(7) 0.102(3) Uani 1.00 1 d . . . C(15) C 0.7708(6) 1.0918(5) 0.7028(4) 0.040(1) Uani 1.00 1 d . . . C(16) C 0.8218(6) 1.0733(4) 0.8096(4) 0.037(1) Uani 1.00 1 d . . . C(17) C 0.6868(6) 1.1019(4) 0.8792(4) 0.041(1) Uani 1.00 1 d . . . C(18) C 0.5512(6) 1.1408(5) 0.8164(4) 0.046(1) Uani 1.00 1 d . . . C(19) C 0.6068(6) 1.1381(5) 0.7080(4) 0.046(2) Uani 1.00 1 d . . . C(20) C 0.8761(8) 1.0735(6) 0.6044(4) 0.058(2) Uani 1.00 1 d . . . C(21) C 0.9854(6) 1.0350(5) 0.8390(5) 0.048(2) Uani 1.00 1 d . . . C(22) C 0.6838(8) 1.0992(6) 0.9975(4) 0.061(2) Uani 1.00 1 d . . . C(23) C 0.3867(8) 1.1828(7) 0.8595(6) 0.076(2) Uani 1.00 1 d . . . C(24) C 0.5117(8) 1.1785(6) 0.6159(5) 0.071(2) Uani 1.00 1 d . . . H(1) H 0.8071 0.7733 0.5321 0.105 Uiso 1.00 1 c R . . H(2) H 0.9345 0.6844 0.4666 0.105 Uiso 1.00 1 c R . . H(3) H 0.7671 0.6659 0.4809 0.105 Uiso 1.00 1 c R . . H(4) H 1.1474 0.7046 0.7393 0.102 Uiso 1.00 1 c R . . H(5) H 1.1467 0.7123 0.6172 0.102 Uiso 1.00 1 c R . . H(6) H 1.0171 0.7950 0.6865 0.102 Uiso 1.00 1 c R . . H(7) H 1.0630 0.4980 0.9120 0.120 Uiso 1.00 1 c R . . H(8) H 1.1884 0.4345 0.8281 0.120 Uiso 1.00 1 c R . . H(9) H 1.1647 0.5684 0.8465 0.120 Uiso 1.00 1 c R . . H(10) H 0.8265 0.3794 0.8546 0.154 Uiso 1.00 1 c R . . H(11) H 0.8015 0.3259 0.7483 0.154 Uiso 1.00 1 c R . . H(12) H 0.9651 0.2975 0.7920 0.154 Uiso 1.00 1 c R . . H(13) H 0.6194 0.5294 0.5740 0.126 Uiso 1.00 1 c R . . H(14) H 0.7560 0.4471 0.5100 0.126 Uiso 1.00 1 c R . . H(15) H 0.6869 0.4027 0.6142 0.126 Uiso 1.00 1 c R . . H(16) H 0.9811 1.0426 0.6197 0.072 Uiso 1.00 1 c R . . H(17) H 0.8436 1.0198 0.5611 0.072 Uiso 1.00 1 c R . . H(18) H 0.8669 1.1466 0.5684 0.072 Uiso 1.00 1 c R . . H(19) H 0.9987 0.9655 0.8808 0.060 Uiso 1.00 1 c R . . H(20) H 1.0506 1.0198 0.7760 0.060 Uiso 1.00 1 c R . . H(21) H 1.0120 1.0953 0.8776 0.060 Uiso 1.00 1 c R . . H(22) H 0.5799 1.1242 1.0262 0.073 Uiso 1.00 1 c R . . H(23) H 0.7263 1.0209 1.0198 0.073 Uiso 1.00 1 c R . . H(24) H 0.7438 1.1496 1.0213 0.073 Uiso 1.00 1 c R . . H(25) H 0.3478 1.2625 0.8395 0.086 Uiso 1.00 1 c R . . H(26) H 0.3266 1.1353 0.8308 0.086 Uiso 1.00 1 c R . . H(27) H 0.3805 1.1763 0.9343 0.086 Uiso 1.00 1 c R . . H(28) H 0.5468 1.2403 0.5800 0.085 Uiso 1.00 1 c R . . H(29) H 0.5232 1.1141 0.5693 0.085 Uiso 1.00 1 c R . . H(30) H 0.4054 1.2055 0.6390 0.085 Uiso 1.00 1 c R . . loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ir Ir -1.444 7.990 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ;
1100790.cif	#------------------------------------------------------------------------------ #$Date: 2022-09-14 17:31:13 +0300 (Wed, 14 Sep 2022) $ #$Revision: 277831 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/10/07/1100790.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100790 loop_ _publ_author_name 'Hidenobu Kajitani' 'Yoshiaki Tanabe' 'Shigeki Kuwata' 'Masakazu Iwasaki' 'Youichi Ishii' _publ_section_title ; Cyanamido-Bridged Diiridium Complex: a Reactive Building Block for Polynuclear Cyanamido Complexes ; _journal_issue 10 _journal_name_full Organometallics _journal_page_first 2251 _journal_page_last 2254 _journal_paper_doi 10.1021/om048978i _journal_volume 24 _journal_year 2005 _chemical_formula_moiety 'C25 H39 Ir2 N4 P ' _chemical_formula_sum 'C25 H39 Ir2 N4 P' _chemical_formula_weight 811.02 _chemical_melting_point ? _space_group_IT_number 62 _space_group_name_Hall '-P 2ac 2n' _space_group_name_H-M_alt 'P n m a' _symmetry_cell_setting orthorhombic _symmetry_Int_Tables_number 62 _symmetry_space_group_name_Hall '-P 2ac 2n' _symmetry_space_group_name_H-M 'P n m a' _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 19.199(5) _cell_length_b 13.714(5) _cell_length_c 9.781(3) _cell_measurement_reflns_used 22586 _cell_measurement_temperature 108.1 _cell_measurement_theta_max 27.5 _cell_measurement_theta_min 3.2 _cell_volume 2575(1) _diffrn_detector_area_resol_mean 10.00 _diffrn_measured_fraction_theta_full 0.9958 _diffrn_measured_fraction_theta_max 0.9958 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents 0.103 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 24765 _diffrn_reflns_theta_full 27.45 _diffrn_reflns_theta_max 27.45 _exptl_absorpt_coefficient_mu 10.435 _exptl_absorpt_correction_T_max 0.593 _exptl_absorpt_correction_T_min 0.261 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Higashi, T. (1999). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_crystal_colour purple _exptl_crystal_density_diffrn 2.092 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 1544.00 _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _refine_diff_density_max 3.60 _refine_diff_density_min -2.21 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_hydrogen_treatment refall _refine_ls_number_parameters 184 _refine_ls_number_reflns 2557 _refine_ls_R_factor_gt 0.0580 _refine_ls_shift/su_max 0.0000 _refine_ls_structure_factor_coef F _refine_ls_weighting_details 'w = 1/[1.3500\s(Fo^2^) + 0.5000]' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.0680 _reflns_number_gt 2557 _reflns_number_total 3028 _reflns_threshold_expression F^2^>3.0\s(F^2^) _cod_original_formula_sum 'C25 H39 Ir2 N4 P ' _cod_database_code 1100790 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2-X,1/2+Y,1/2+Z 3 +X,1/2-Y,+Z 4 1/2-X,-Y,1/2+Z 5 -X,-Y,-Z 6 1/2+X,1/2-Y,1/2-Z 7 -X,1/2+Y,-Z 8 1/2+X,+Y,1/2-Z loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir(1) Ir 0.22217(2) 0.2500 0.03820(4) 0.0080(1) Uani 1.00 2 d S . . Ir(2) Ir 0.06294(2) 0.2500 0.16486(4) 0.0086(1) Uani 1.00 2 d S . . P(1) P 0.1780(2) 0.2500 -0.1769(3) 0.0119(7) Uani 1.00 2 d S . . N(1) N 0.1370(4) 0.1611(5) 0.0944(6) 0.012(2) Uani 1.00 1 d . . . N(2) N 0.1437(4) -0.0171(5) 0.1324(7) 0.019(2) Uani 1.00 1 d . . . C(1) C 0.1404(4) 0.0682(6) 0.1149(7) 0.009(2) Uani 1.00 1 d . . . C(2) C 0.3336(7) 0.2500 -0.015(1) 0.017(3) Uani 1.00 2 d S . . C(3) C 0.3171(4) 0.1658(6) 0.0665(8) 0.015(2) Uani 1.00 1 d . . . C(4) C 0.2956(4) 0.1986(6) 0.2009(8) 0.012(2) Uani 1.00 1 d . . . C(5) C 0.3673(8) 0.25000(1) -0.152(1) 0.026(4) Uani 1.00 2 d S . . C(6) C 0.3268(5) 0.0617(7) 0.0210(8) 0.020(2) Uani 1.00 1 d . . . C(7) C 0.2720(5) 0.1323(6) 0.3161(9) 0.017(2) Uani 1.00 1 d . . . C(8) C 0.0018(4) 0.1963(6) 0.3332(7) 0.010(2) Uani 1.00 1 d . . . C(9) C -0.0306(5) 0.1631(6) 0.2084(8) 0.014(2) Uani 1.00 1 d . . . C(10) C -0.0474(6) 0.2500 0.128(1) 0.016(3) Uani 1.00 2 d S . . C(11) C 0.0313(5) 0.1312(6) 0.4429(7) 0.018(2) Uani 1.00 1 d . . . C(12) C -0.0406(4) 0.0609(6) 0.1676(8) 0.016(2) Uani 1.00 1 d . . . C(13) C -0.0815(8) 0.25000(1) -0.007(1) 0.025(4) Uani 1.00 2 d S . . C(14) C 0.0839(6) 0.25000(1) -0.191(1) 0.023(3) Uani 1.00 2 d S . . C(15) C 0.2034(5) 0.1464(6) -0.279(1) 0.025(2) Uani 1.00 1 d . . . H(1) H 0.3726 0.1844 -0.1826 0.032 Uiso 0.50 1 c R . . H(2) H 0.3400 0.2858 -0.2156 0.032 Uiso 0.50 1 c R . . H(3) H 0.4118 0.2798 -0.1432 0.032 Uiso 0.50 1 c R . . H(4) H 0.3750 0.0507 0.0059 0.024 Uiso 1.00 1 c R . . H(5) H 0.3018 0.0491 -0.0610 0.024 Uiso 1.00 1 c R . . H(6) H 0.3107 0.0192 0.0912 0.024 Uiso 1.00 1 c R . . H(7) H 0.3092 0.0895 0.3396 0.020 Uiso 1.00 1 c R . . H(8) H 0.2327 0.0947 0.2893 0.020 Uiso 1.00 1 c R . . H(9) H 0.2603 0.1716 0.3929 0.020 Uiso 1.00 1 c R . . H(10) H -0.0056 0.0926 0.4785 0.021 Uiso 1.00 1 c R . . H(11) H 0.0505 0.1704 0.5140 0.021 Uiso 1.00 1 c R . . H(12) H 0.0664 0.0894 0.4069 0.021 Uiso 1.00 1 c R . . H(13) H -0.0688 0.0291 0.2340 0.019 Uiso 1.00 1 c R . . H(14) H -0.0630 0.0583 0.0810 0.019 Uiso 1.00 1 c R . . H(15) H 0.0032 0.0288 0.1621 0.019 Uiso 1.00 1 c R . . H(16) H -0.0886 0.3157 -0.0360 0.030 Uiso 0.50 1 c R . . H(17) H -0.0522 0.2172 -0.0704 0.030 Uiso 0.50 1 c R . . H(18) H -0.1250 0.2172 -0.0017 0.029 Uiso 0.50 1 c R . . H(19) H 0.0660 0.3100 -0.1560 0.027 Uiso 0.50 1 c R . . H(20) H 0.0712 0.2500 -0.2842 0.027 Uiso 1.00 2 c R . . H(21) H 0.0653 0.1969 -0.1395 0.027 Uiso 0.50 1 c R . . H(22) H 0.2526 0.1386 -0.2786 0.030 Uiso 1.00 1 c R . . H(23) H 0.1879 0.1559 -0.3705 0.030 Uiso 1.00 1 c R . . H(24) H 0.1822 0.0893 -0.2422 0.030 Uiso 1.00 1 c R . . loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; P P 0.102 0.094 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ir Ir -1.444 7.990 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ;
1100791.cif	#------------------------------------------------------------------------------ #$Date: 2022-09-14 17:31:13 +0300 (Wed, 14 Sep 2022) $ #$Revision: 277831 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/10/07/1100791.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100791 loop_ _publ_author_name 'Hidenobu Kajitani' 'Yoshiaki Tanabe' 'Shigeki Kuwata' 'Masakazu Iwasaki' 'Youichi Ishii' _publ_section_title ; Cyanamido-Bridged Diiridium Complex: a Reactive Building Block for Polynuclear Cyanamido Complexes ; _journal_issue 10 _journal_name_full Organometallics _journal_page_first 2251 _journal_page_last 2254 _journal_paper_doi 10.1021/om048978i _journal_volume 24 _journal_year 2005 _chemical_formula_moiety 'C56 H61 Ir2 N4 P2 ' _chemical_formula_sum 'C56 H61 Ir2 N4 P2' _chemical_formula_weight 1236.51 _chemical_melting_point ? _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_cell_setting triclinic _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _cell_angle_alpha 99.37(1) _cell_angle_beta 91.82(1) _cell_angle_gamma 118.88(1) _cell_formula_units_Z 2 _cell_length_a 12.084(4) _cell_length_b 12.105(4) _cell_length_c 19.525(7) _cell_measurement_reflns_used 20891 _cell_measurement_temperature 294.1 _cell_measurement_theta_max 27.5 _cell_measurement_theta_min 1.9 _cell_volume 2447(1) _diffrn_detector_area_resol_mean 10.00 _diffrn_measured_fraction_theta_full 0.9851 _diffrn_measured_fraction_theta_max 0.9851 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents 0.033 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 24110 _diffrn_reflns_theta_full 27.46 _diffrn_reflns_theta_max 27.46 _exptl_absorpt_coefficient_mu 5.555 _exptl_absorpt_correction_T_max 0.108 _exptl_absorpt_correction_T_min 0.040 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_crystal_colour dark _exptl_crystal_density_diffrn 1.678 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1218.00 _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.70 _exptl_crystal_size_min 0.40 _refine_diff_density_max 1.71 _refine_diff_density_min -1.67 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_hydrogen_treatment refall _refine_ls_number_parameters 638 _refine_ls_number_reflns 8788 _refine_ls_R_factor_gt 0.0310 _refine_ls_shift/su_max 0.0000 _refine_ls_structure_factor_coef F _refine_ls_weighting_details 'w = 1/[1.8500\s(Fo^2^) + 0.5000]' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.0360 _reflns_number_gt 8788 _reflns_number_total 10868 _reflns_threshold_expression F^2^>2.0\s(F^2^) _cod_original_formula_sum 'C56 H61 Ir2 N4 P2 ' _cod_database_code 1100791 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir(1) Ir 0.10772(1) 0.47498(1) 0.27106(1) 0.02367(5) Uani 1.00 1 d . . . Ir(2) Ir 0.40851(1) 0.70784(1) 0.33470(1) 0.02686(5) Uani 1.00 1 d . . . P(1) P 0.1919(1) 0.3908(1) 0.19052(5) 0.0254(3) Uani 1.00 1 d . . . P(2) P 0.4710(1) 0.6056(1) 0.25112(6) 0.0280(3) Uani 1.00 1 d . . . N(1) N 0.2496(3) 0.6599(4) 0.2662(2) 0.030(1) Uani 1.00 1 d . . . N(2) N 0.2553(6) 0.7590(5) 0.1646(3) 0.060(2) Uani 1.00 1 d . . . N(3) N 0.2708(4) 0.5171(4) 0.3376(2) 0.031(1) Uani 1.00 1 d . . . N(4) N 0.2490(5) 0.4371(5) 0.4468(3) 0.066(2) Uani 1.00 1 d . . . C(1) C 0.2524(5) 0.7100(4) 0.2125(3) 0.035(1) Uani 1.00 1 d . . . C(2) C 0.2588(5) 0.4762(5) 0.3951(3) 0.038(1) Uani 1.00 1 d . . . C(3) C -0.0940(4) 0.3236(5) 0.2482(3) 0.040(1) Uani 1.00 1 d . . . C(4) C -0.0569(4) 0.3560(5) 0.3221(3) 0.040(1) Uani 1.00 1 d . . . C(5) C -0.0246(5) 0.4878(5) 0.3453(3) 0.041(1) Uani 1.00 1 d . . . C(6) C -0.0396(5) 0.5354(5) 0.2871(3) 0.040(1) Uani 1.00 1 d . . . C(7) C -0.0782(5) 0.4362(5) 0.2264(3) 0.041(1) Uani 1.00 1 d . . . C(8) C -0.1504(6) 0.1918(6) 0.2041(4) 0.073(2) Uani 1.00 1 d . . . C(9) C -0.0648(7) 0.2695(7) 0.3708(4) 0.066(2) Uani 1.00 1 d . . . C(10) C 0.0071(6) 0.5578(7) 0.4193(3) 0.068(2) Uani 1.00 1 d . . . C(11) C -0.0191(7) 0.6675(7) 0.2884(4) 0.075(3) Uani 1.00 1 d . . . C(12) C -0.1168(6) 0.4477(8) 0.1551(3) 0.074(2) Uani 1.00 1 d . . . C(13) C 0.5956(5) 0.8672(5) 0.3851(3) 0.042(1) Uani 1.00 1 d . . . C(14) C 0.5305(5) 0.7998(5) 0.4373(3) 0.044(1) Uani 1.00 1 d . . . C(15) C 0.4205(5) 0.8167(5) 0.4435(3) 0.046(1) Uani 1.00 1 d . . . C(16) C 0.4170(5) 0.8869(5) 0.3946(3) 0.049(2) Uani 1.00 1 d . . . C(17) C 0.5240(5) 0.9166(5) 0.3554(3) 0.042(1) Uani 1.00 1 d . . . C(18) C 0.7266(5) 0.8932(6) 0.3699(4) 0.063(2) Uani 1.00 1 d . . . C(19) C 0.5758(7) 0.7437(7) 0.4865(3) 0.072(2) Uani 1.00 1 d . . . C(20) C 0.3322(7) 0.7696(6) 0.4977(3) 0.073(2) Uani 1.00 1 d . . . C(21) C 0.3187(7) 0.9263(6) 0.3831(4) 0.080(3) Uani 1.00 1 d . . . C(22) C 0.5627(7) 1.0021(5) 0.3034(3) 0.067(2) Uani 1.00 1 d . . . C(23) C 0.1070(4) 0.3336(5) 0.1013(2) 0.032(1) Uani 1.00 1 d . . . C(24) C 0.0314(5) 0.2041(5) 0.0717(3) 0.049(1) Uani 1.00 1 d . . . C(25) C -0.0349(6) 0.1652(7) 0.0060(3) 0.070(2) Uani 1.00 1 d . . . C(26) C -0.0301(7) 0.2510(8) -0.0317(3) 0.071(2) Uani 1.00 1 d . . . C(27) C 0.0458(6) 0.3818(7) -0.0036(3) 0.059(2) Uani 1.00 1 d . . . C(28) C 0.1122(5) 0.4228(6) 0.0634(3) 0.045(2) Uani 1.00 1 d . . . C(29) C 0.2070(5) 0.2537(4) 0.2046(2) 0.033(1) Uani 1.00 1 d . . . C(30) C 0.1744(7) 0.2061(6) 0.2639(3) 0.059(2) Uani 1.00 1 d . . . C(31) C 0.1802(9) 0.0973(7) 0.2721(4) 0.090(3) Uani 1.00 1 d . . . C(32) C 0.2211(8) 0.0379(7) 0.2213(4) 0.081(3) Uani 1.00 1 d . . . C(33) C 0.2558(6) 0.0855(6) 0.1623(4) 0.059(2) Uani 1.00 1 d . . . C(34) C 0.2509(5) 0.1944(5) 0.1548(3) 0.047(2) Uani 1.00 1 d . . . C(35) C 0.3514(4) 0.5069(4) 0.1751(2) 0.029(1) Uani 1.00 1 d . . . C(36) C 0.5263(4) 0.5015(4) 0.2788(3) 0.034(1) Uani 1.00 1 d . . . C(37) C 0.5549(6) 0.5126(5) 0.3489(3) 0.046(2) Uani 1.00 1 d . . . C(38) C 0.6101(6) 0.4472(6) 0.3724(3) 0.057(2) Uani 1.00 1 d . . . C(39) C 0.6347(6) 0.3667(6) 0.3251(4) 0.060(2) Uani 1.00 1 d . . . C(40) C 0.6029(6) 0.3514(6) 0.2551(4) 0.059(2) Uani 1.00 1 d . . . C(41) C 0.5500(5) 0.4202(6) 0.2311(3) 0.049(2) Uani 1.00 1 d . . . C(42) C 0.6015(4) 0.7104(5) 0.2063(2) 0.035(1) Uani 1.00 1 d . . . C(43) C 0.7201(5) 0.7188(5) 0.2129(3) 0.052(2) Uani 1.00 1 d . . . C(44) C 0.8165(5) 0.8014(6) 0.1793(4) 0.064(2) Uani 1.00 1 d . . . C(45) C 0.7952(6) 0.8750(6) 0.1411(4) 0.069(2) Uani 1.00 1 d . . . C(46) C 0.6798(6) 0.8688(5) 0.1341(3) 0.055(2) Uani 1.00 1 d . . . C(47) C 0.5828(5) 0.7873(4) 0.1679(3) 0.042(1) Uani 1.00 1 d . . . C(48) C 0.592(1) 0.474(1) 0.0217(4) 0.101(4) Uani 1.00 1 d . . . C(49) C 0.6249(9) 0.594(1) 0.0125(5) 0.102(4) Uani 1.00 1 d . . . C(50) C 0.530(1) 0.618(1) -0.0110(5) 0.111(4) Uani 1.00 1 d . . . C(51) C 0.0366(8) -0.0409(8) 0.4405(4) 0.081(3) Uani 1.00 1 d . . . C(52) C 0.0715(6) 0.0873(7) 0.4602(4) 0.066(2) Uani 1.00 1 d . . . C(53) C 0.0360(8) 0.1267(7) 0.5194(4) 0.076(3) Uani 1.00 1 d . . . C(54) C 0.569(2) 1.106(2) 0.050(1) 0.165(7) Uani 1.00 1 d . . . C(55) C 0.478(3) 0.994(3) 0.0650(8) 0.156(8) Uani 1.00 1 d . . . C(56) C 0.413(1) 0.893(2) 0.015(2) 0.150(6) Uani 1.00 1 d . . . H(1) H -0.2355 0.1639 0.1861 0.070 Uiso 1.00 1 c R . . H(2) H -0.1020 0.1932 0.1666 0.070 Uiso 1.00 1 c R . . H(3) H -0.1498 0.1342 0.2316 0.070 Uiso 1.00 1 c R . . H(4) H -0.1263 0.2625 0.4015 0.083 Uiso 1.00 1 c R . . H(5) H -0.0887 0.1868 0.3440 0.083 Uiso 1.00 1 c R . . H(6) H 0.0160 0.3039 0.3973 0.083 Uiso 1.00 1 c R . . H(7) H 0.0793 0.5583 0.4402 0.080 Uiso 1.00 1 c R . . H(8) H 0.0253 0.6438 0.4210 0.080 Uiso 1.00 1 c R . . H(9) H -0.0633 0.5160 0.4440 0.080 Uiso 1.00 1 c R . . H(10) H 0.0669 0.7276 0.3068 0.103 Uiso 1.00 1 c R . . H(11) H -0.0352 0.6767 0.2425 0.103 Uiso 1.00 1 c R . . H(12) H -0.0741 0.6829 0.3173 0.103 Uiso 1.00 1 c R . . H(13) H -0.0483 0.5177 0.1406 0.095 Uiso 1.00 1 c R . . H(14) H -0.1385 0.3699 0.1234 0.095 Uiso 1.00 1 c R . . H(15) H -0.1884 0.4604 0.1560 0.095 Uiso 1.00 1 c R . . H(16) H 0.7256 0.8140 0.3550 0.065 Uiso 1.00 1 c R . . H(17) H 0.7498 0.9409 0.3338 0.065 Uiso 1.00 1 c R . . H(18) H 0.7867 0.9412 0.4105 0.065 Uiso 1.00 1 c R . . H(19) H 0.5119 0.7030 0.5152 0.082 Uiso 1.00 1 c R . . H(20) H 0.5942 0.6822 0.4607 0.082 Uiso 1.00 1 c R . . H(21) H 0.6507 0.8105 0.5151 0.082 Uiso 1.00 1 c R . . H(22) H 0.3800 0.8105 0.5426 0.072 Uiso 1.00 1 c R . . H(23) H 0.2654 0.7892 0.4934 0.072 Uiso 1.00 1 c R . . H(24) H 0.2971 0.6792 0.4919 0.072 Uiso 1.00 1 c R . . H(25) H 0.3164 0.9772 0.4249 0.097 Uiso 1.00 1 c R . . H(26) H 0.3396 0.9746 0.3472 0.097 Uiso 1.00 1 c R . . H(27) H 0.2377 0.8513 0.3693 0.097 Uiso 1.00 1 c R . . H(28) H 0.6362 1.0062 0.2851 0.072 Uiso 1.00 1 c R . . H(29) H 0.4946 0.9669 0.2666 0.072 Uiso 1.00 1 c R . . H(30) H 0.5807 1.0863 0.3247 0.072 Uiso 1.00 1 c R . . H(31) H 0.0278 0.1420 0.0969 0.051 Uiso 1.00 1 c R . . H(32) H -0.0872 0.0762 -0.0135 0.071 Uiso 1.00 1 c R . . H(33) H -0.0774 0.2239 -0.0767 0.085 Uiso 1.00 1 c R . . H(34) H 0.0515 0.4430 -0.0301 0.078 Uiso 1.00 1 c R . . H(35) H 0.1626 0.5122 0.0826 0.057 Uiso 1.00 1 c R . . H(36) H 0.1488 0.2492 0.2995 0.077 Uiso 1.00 1 c R . . H(37) H 0.1545 0.0626 0.3126 0.128 Uiso 1.00 1 c R . . H(38) H 0.2254 -0.0365 0.2267 0.107 Uiso 1.00 1 c R . . H(39) H 0.2858 0.0457 0.1275 0.076 Uiso 1.00 1 c R . . H(40) H 0.2748 0.2285 0.1139 0.058 Uiso 1.00 1 c R . . H(41) H 0.3832 0.4605 0.1461 0.036 Uiso 1.00 1 c R . . H(42) H 0.3420 0.5643 0.1508 0.036 Uiso 1.00 1 c R . . H(43) H 0.5334 0.5644 0.3815 0.060 Uiso 1.00 1 c R . . H(44) H 0.6321 0.4589 0.4211 0.072 Uiso 1.00 1 c R . . H(45) H 0.6732 0.3222 0.3416 0.078 Uiso 1.00 1 c R . . H(46) H 0.6172 0.2931 0.2230 0.076 Uiso 1.00 1 c R . . H(47) H 0.5310 0.4119 0.1824 0.063 Uiso 1.00 1 c R . . H(48) H 0.7347 0.6674 0.2398 0.061 Uiso 1.00 1 c R . . H(49) H 0.8972 0.8059 0.1830 0.074 Uiso 1.00 1 c R . . H(50) H 0.8626 0.9328 0.1194 0.080 Uiso 1.00 1 c R . . H(51) H 0.6652 0.9192 0.1064 0.066 Uiso 1.00 1 c R . . H(52) H 0.5022 0.7830 0.1638 0.049 Uiso 1.00 1 c R . . H(53) H 0.6563 0.4560 0.0366 0.124 Uiso 1.00 1 c R . . H(54) H 0.7119 0.6594 0.0196 0.115 Uiso 1.00 1 c R . . H(55) H 0.5530 0.7024 -0.0161 0.135 Uiso 1.00 1 c R . . H(56) H 0.0651 -0.0687 0.3999 0.105 Uiso 1.00 1 c R . . H(57) H 0.1175 0.1464 0.4316 0.078 Uiso 1.00 1 c R . . H(58) H 0.0599 0.2146 0.5349 0.095 Uiso 1.00 1 c R . . H(59) H 0.5812 1.1578 0.0945 0.197 Uiso 1.00 1 c R . . H(60) H 0.4321 0.9493 0.0992 0.253 Uiso 1.00 1 c R . . H(61) H 0.3384 0.8122 -0.0016 0.186 Uiso 1.00 1 c R . . loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; P P 0.102 0.094 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ir Ir -1.444 7.990 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ;
1100792.cif	#------------------------------------------------------------------------------ #$Date: 2022-09-14 17:31:13 +0300 (Wed, 14 Sep 2022) $ #$Revision: 277831 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/10/07/1100792.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100792 loop_ _publ_author_name 'Hidenobu Kajitani' 'Yoshiaki Tanabe' 'Shigeki Kuwata' 'Masakazu Iwasaki' 'Youichi Ishii' _publ_section_title ; Cyanamido-Bridged Diiridium Complex: a Reactive Building Block for Polynuclear Cyanamido Complexes ; _journal_issue 10 _journal_name_full Organometallics _journal_page_first 2251 _journal_page_last 2254 _journal_paper_doi 10.1021/om048978i _journal_volume 24 _journal_year 2005 _chemical_formula_moiety 'C55 H64 B Cl2 Ir2 N4 Rh ' _chemical_formula_sum 'C55 H64 B Cl2 Ir2 N4 Rh' _chemical_formula_weight 1350.20 _chemical_melting_point ? _space_group_IT_number 56 _space_group_name_Hall '-P 2ab 2ac' _space_group_name_H-M_alt 'P c c n' _symmetry_cell_setting orthorhombic _symmetry_Int_Tables_number 56 _symmetry_space_group_name_Hall '-P 2ab 2ac' _symmetry_space_group_name_H-M 'P c c n' _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.680(2) _cell_length_b 12.734(2) _cell_length_c 32.297(4) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293.1 _cell_measurement_theta_max 19.9 _cell_measurement_theta_min 18.6 _cell_volume 5214(1) _diffrn_measured_fraction_theta_full 0.9976 _diffrn_measured_fraction_theta_max 0.9965 _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method \w-2\q _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 6641 _diffrn_reflns_theta_full 27.50 _diffrn_reflns_theta_max 27.51 _diffrn_standards_decay_% -2.52 _diffrn_standards_interval_count 0 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 5.559 _exptl_absorpt_correction_T_max 0.574 _exptl_absorpt_correction_T_min 0.175 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_crystal_colour 'dark red' _exptl_crystal_density_diffrn 1.720 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 2640.00 _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.10 _refine_diff_density_max 2.68 _refine_diff_density_min -1.58 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_hydrogen_treatment refall _refine_ls_number_parameters 329 _refine_ls_number_reflns 3844 _refine_ls_R_factor_gt 0.0510 _refine_ls_shift/su_max 0.0000 _refine_ls_structure_factor_coef F _refine_ls_weighting_details 'w = 1/[0.0002Fo^2^ + 2.2000\s(Fo^2^) + 0.5000]' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.0520 _reflns_number_gt 3844 _reflns_number_total 5934 _reflns_threshold_expression F^2^>3.0\s(F^2^) _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_absorpt_correction_type' tag value 'psi-scans' was replaced with 'psi-scan' value. Automatic conversion script Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana ; _cod_original_formula_sum 'C55 H64 B Cl2 Ir2 N4 Rh ' _cod_database_code 1100792 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2-X,+Y,1/2+Z 3 +X,1/2-Y,1/2+Z 4 1/2-X,1/2-Y,+Z 5 -X,-Y,-Z 6 1/2+X,-Y,1/2-Z 7 -X,1/2+Y,1/2-Z 8 1/2+X,1/2+Y,-Z loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir(1) Ir 0.20707(3) 0.14770(3) 0.14925(1) 0.03278(9) Uani 1.00 1 d . . . Rh(1) Rh 0.2500 0.2500 0.22609(3) 0.0347(3) Uani 1.00 2 d S . . Cl(1) Cl 0.6712(4) 0.3303(5) 0.2349(2) 0.131(2) Uani 1.00 1 d . . . N(1) N 0.3370(6) 0.2123(6) 0.1749(3) 0.033(2) Uani 1.00 1 d . . . N(2) N 0.5160(8) 0.132(1) 0.1764(4) 0.076(4) Uani 1.00 1 d . . . C(1) C 0.4328(8) 0.1701(9) 0.1752(4) 0.045(3) Uani 1.00 1 d . . . C(2) C 0.0696(9) 0.0641(9) 0.1274(4) 0.049(3) Uani 1.00 1 d . . . C(3) C 0.133(1) 0.092(1) 0.0929(4) 0.055(4) Uani 1.00 1 d . . . C(4) C 0.2330(9) 0.0436(9) 0.0981(3) 0.048(3) Uani 1.00 1 d . . . C(5) C 0.232(1) -0.0135(9) 0.1352(4) 0.055(4) Uani 1.00 1 d . . . C(6) C 0.132(1) -0.001(1) 0.1534(5) 0.069(4) Uani 1.00 1 d . . . C(7) C -0.043(1) 0.098(1) 0.1347(5) 0.086(5) Uani 1.00 1 d . . . C(8) C 0.098(1) 0.158(1) 0.0577(5) 0.081(5) Uani 1.00 1 d . . . C(9) C 0.325(1) 0.049(1) 0.0686(5) 0.082(5) Uani 1.00 1 d . . . C(10) C 0.319(1) -0.087(1) 0.1518(6) 0.113(7) Uani 1.00 1 d . . . C(11) C 0.093(1) -0.053(1) 0.1928(5) 0.107(7) Uani 1.00 1 d . . . C(12) C 0.249(2) 0.118(2) 0.3037(6) 0.138(9) Uani 1.00 1 d . . . C(13) C 0.329(1) 0.155(1) 0.2712(4) 0.074(5) Uani 1.00 1 d . . . C(14) C 0.374(1) 0.251(1) 0.2713(4) 0.070(4) Uani 1.00 1 d . . . C(15) C 0.356(2) 0.338(2) 0.3025(6) 0.131(9) Uani 1.00 1 d . . . C(16) C 0.6452(7) 0.2351(7) -0.0215(3) 0.036(3) Uani 1.00 1 d . . . C(17) C 0.5607(8) 0.1686(8) -0.0120(3) 0.043(3) Uani 1.00 1 d . . . C(18) C 0.4711(8) 0.1584(9) -0.0367(4) 0.051(3) Uani 1.00 1 d . . . C(19) C 0.4629(9) 0.2140(9) -0.0729(4) 0.054(4) Uani 1.00 1 d . . . C(20) C 0.5430(9) 0.2820(9) -0.0834(4) 0.056(4) Uani 1.00 1 d . . . C(21) C 0.6309(9) 0.2919(8) -0.0586(4) 0.044(3) Uani 1.00 1 d . . . C(22) C 0.7621(8) 0.1450(8) 0.0364(3) 0.040(3) Uani 1.00 1 d . . . C(23) C 0.8270(9) 0.0584(9) 0.0259(4) 0.049(3) Uani 1.00 1 d . . . C(24) C 0.829(1) -0.0335(9) 0.0474(4) 0.051(3) Uani 1.00 1 d . . . C(25) C 0.766(1) -0.0463(9) 0.0822(4) 0.057(4) Uani 1.00 1 d . . . C(26) C 0.703(1) 0.036(1) 0.0948(4) 0.058(4) Uani 1.00 1 d . . . C(27) C 0.7026(8) 0.1269(9) 0.0724(4) 0.049(3) Uani 1.00 1 d . . . C(28) C 0.75000(1) 0.25000(1) 0.2028(9) 0.11(1) Uani 1.00 2 d S . . B(1) B 0.7500 0.2500 0.0070(5) 0.040(4) Uani 1.00 2 d S . . H(1) H -0.0464 0.1723 0.1363 0.103 Uiso 1.00 1 c R . . H(2) H -0.0863 0.0741 0.1126 0.103 Uiso 1.00 1 c R . . H(3) H -0.0672 0.0684 0.1600 0.103 Uiso 1.00 1 c R . . H(4) H 0.0784 0.2253 0.0675 0.097 Uiso 1.00 1 c R . . H(5) H 0.1545 0.1645 0.0386 0.097 Uiso 1.00 1 c R . . H(6) H 0.0395 0.1258 0.0444 0.097 Uiso 1.00 1 c R . . H(7) H 0.3424 -0.0193 0.0591 0.098 Uiso 1.00 1 c R . . H(8) H 0.3078 0.0925 0.0457 0.098 Uiso 1.00 1 c R . . H(9) H 0.3841 0.0783 0.0828 0.098 Uiso 1.00 1 c R . . H(10) H 0.2942 -0.1573 0.1519 0.135 Uiso 1.00 1 c R . . H(11) H 0.3788 -0.0814 0.1343 0.135 Uiso 1.00 1 c R . . H(12) H 0.3376 -0.0666 0.1791 0.135 Uiso 1.00 1 c R . . H(13) H 0.0709 -0.0005 0.2120 0.128 Uiso 1.00 1 c R . . H(14) H 0.0357 -0.0976 0.1865 0.128 Uiso 1.00 1 c R . . H(15) H 0.1488 -0.0927 0.2047 0.128 Uiso 1.00 1 c R . . H(16) H 0.2416 0.0445 0.3005 0.166 Uiso 1.00 1 c R . . H(17) H 0.2796 0.1330 0.3300 0.166 Uiso 1.00 1 c R . . H(18) H 0.3461 0.1082 0.2494 0.089 Uiso 1.00 1 c R . . H(19) H 0.4218 0.2670 0.2495 0.083 Uiso 1.00 1 c R . . H(20) H 0.3693 0.3084 0.3290 0.157 Uiso 1.00 1 c R . . H(21) H 0.4056 0.3931 0.2975 0.157 Uiso 1.00 1 c R . . H(22) H 0.5645 0.1280 0.0126 0.051 Uiso 1.00 1 c R . . H(23) H 0.4156 0.1129 -0.0284 0.061 Uiso 1.00 1 c R . . H(24) H 0.4035 0.2054 -0.0905 0.065 Uiso 1.00 1 c R . . H(25) H 0.5374 0.3229 -0.1079 0.068 Uiso 1.00 1 c R . . H(26) H 0.6847 0.3393 -0.0670 0.053 Uiso 1.00 1 c R . . H(27) H 0.8713 0.0647 0.0023 0.058 Uiso 1.00 1 c R . . H(28) H 0.8742 -0.0889 0.0386 0.061 Uiso 1.00 1 c R . . H(29) H 0.7664 -0.1105 0.0972 0.069 Uiso 1.00 1 c R . . H(30) H 0.6603 0.0291 0.1187 0.070 Uiso 1.00 1 c R . . H(31) H 0.6589 0.1823 0.0821 0.059 Uiso 1.00 1 c R . . H(32) H 0.7062 0.2075 0.1858 0.136 Uiso 1.00 1 c R . . loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; B B 0.001 0.001 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Rh Rh -1.118 0.919 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ir Ir -1.444 7.990 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ;