file_name stringlengths 11 11 | content stringlengths 1.16k 56.6M |
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1100893.cif | #------------------------------------------------------------------------------
#$Date: 2018-09-01 22:50:30 +0300 (Sat, 01 Sep 2018) $
#$Revision: 210323 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100893.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_1100893
loop_
_publ_author_name
'Chase, Preston A.'
'Gagliardo, Marcella'
'Lutz, Martin'
'Spek, Anthony L.'
'van Klink, Gerard P. M.'
'van Koten, Gerard'
_publ_section_title
;
Electron-Poor Pentafluorophenyl-Substituted PCP--Palladium Pincer Complexes
;
_journal_coden_ASTM INOCAJ
_journal_issue 9
_journal_name_full Organometallics
_journal_page_first 2016
_journal_page_last 2019
_journal_paper_doi 10.1021/om0500063
_journal_volume 24
_journal_year 2005
_chemical_formula_moiety 'C34 H10 F20 N P2 Pd, B F4'
_chemical_formula_sum 'C34 H10 B F24 N P2 Pd'
_chemical_formula_weight 1067.58
_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 difmap
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 110.5437(8)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 10.1565(2)
_cell_length_b 25.6619(5)
_cell_length_c 16.1795(3)
_cell_measurement_reflns_used 72429
_cell_measurement_temperature 150(2)
_cell_measurement_theta_max 27.48
_cell_measurement_theta_min 1.02
_cell_volume 3948.77(13)
_diffrn_ambient_temperature 150(2)
_diffrn_measurement_device_type 'Nonius KappaCCD'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'rotating anode'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0659
_diffrn_reflns_av_sigmaI/netI 0.0473
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 31
_diffrn_reflns_limit_k_min -31
_diffrn_reflns_limit_l_max 20
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_number 40386
_diffrn_reflns_theta_max 26.14
_diffrn_reflns_theta_min 1.56
_exptl_absorpt_coefficient_mu 0.693
_exptl_absorpt_correction_T_max 0.96
_exptl_absorpt_correction_T_min 0.70
_exptl_absorpt_correction_type multi-scan
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.796
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description needle
_exptl_crystal_F_000 2072
_exptl_crystal_size_max 0.39
_exptl_crystal_size_mid 0.15
_exptl_crystal_size_min 0.06
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.040
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 623
_refine_ls_number_reflns 7802
_refine_ls_number_restraints 258
_refine_ls_restrained_S_all 1.152
_refine_ls_R_factor_all 0.0577
_refine_ls_R_factor_gt 0.0407
_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^)+(0.0335P)^2^+3.7955P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0931
_refine_ls_wR_factor_ref 0.1001
_reflns_number_gt 5863
_reflns_number_total 7802
_reflns_threshold_expression I>2\s(I)
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 1100893
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
Pd1 Pd 0.99146(3) 0.079376(12) 0.777666(18) 0.03873(10) Uani 1 1 d . . .
P1 P 0.85438(10) 0.00640(4) 0.74168(6) 0.0390(2) Uani 1 1 d . . .
P2 P 1.16523(10) 0.13583(4) 0.85151(7) 0.0405(2) Uani 1 1 d . . .
F1 F 0.7587(3) -0.10546(10) 0.69740(16) 0.0634(7) Uani 1 1 d . . .
F2 F 0.8422(4) -0.17527(11) 0.60229(19) 0.0893(10) Uani 1 1 d . . .
F3 F 1.0252(4) -0.14618(13) 0.52210(19) 0.0907(10) Uani 1 1 d . . .
F4 F 1.1306(3) -0.04839(13) 0.54302(17) 0.0780(9) Uani 1 1 d . . .
F5 F 1.0467(2) 0.02133(10) 0.63569(15) 0.0546(6) Uani 1 1 d . . .
F6 F 0.7092(2) 0.04411(9) 0.56105(13) 0.0467(5) Uani 1 1 d . . .
F7 F 0.4419(2) 0.07551(10) 0.48272(15) 0.0559(6) Uani 1 1 d . . .
F8 F 0.2546(2) 0.06177(12) 0.56484(17) 0.0697(8) Uani 1 1 d . . .
F9 F 0.3354(2) 0.01527(14) 0.72576(17) 0.0785(9) Uani 1 1 d . . .
F10 F 0.5978(2) -0.01669(12) 0.80310(15) 0.0681(8) Uani 1 1 d . . .
F11 F 1.1539(3) 0.14042(13) 0.66451(17) 0.0790(8) Uani 1 1 d . . .
F12 F 1.2845(3) 0.20632(15) 0.58995(18) 0.0966(11) Uani 1 1 d . . .
F13 F 1.4429(4) 0.28432(14) 0.6842(2) 0.1042(11) Uani 1 1 d . . .
F14 F 1.4762(4) 0.29627(13) 0.8579(2) 0.0994(11) Uani 1 1 d . . .
F15 F 1.3511(3) 0.22982(11) 0.93449(17) 0.0667(7) Uani 1 1 d . . .
F16 F 0.9616(3) 0.22089(11) 0.8062(2) 0.0744(8) Uani 1 1 d . . .
F17 F 0.8332(3) 0.26924(13) 0.9040(3) 0.1146(13) Uani 1 1 d . . .
F18 F 0.9136(4) 0.24872(15) 1.0799(3) 0.1304(15) Uani 1 1 d . . .
F19 F 1.1130(5) 0.17599(13) 1.1538(2) 0.1097(13) Uani 1 1 d . . .
F20 F 1.2389(3) 0.12658(10) 1.05758(17) 0.0697(7) Uani 1 1 d . . .
N1 N 0.8617(3) 0.12913(14) 0.6820(2) 0.0508(9) Uani 1 1 d . . .
C1 C 1.1078(4) 0.03157(14) 0.8755(2) 0.0359(8) Uani 1 1 d . . .
C2 C 1.0494(4) -0.01456(15) 0.8951(2) 0.0395(9) Uani 1 1 d . . .
C3 C 1.1301(4) -0.04845(17) 0.9604(2) 0.0458(9) Uani 1 1 d . . .
H3 H 1.0906 -0.0800 0.9719 0.055 Uiso 1 1 calc R . .
C4 C 1.2687(4) -0.03587(17) 1.0086(3) 0.0462(10) Uani 1 1 d . . .
H4 H 1.3250 -0.0593 1.0523 0.055 Uiso 1 1 calc R . .
C5 C 1.3250(4) 0.01017(16) 0.9935(2) 0.0403(9) Uani 1 1 d . . .
H5 H 1.4185 0.0192 1.0290 0.048 Uiso 1 1 calc R . .
C6 C 1.2474(3) 0.04371(15) 0.9271(2) 0.0359(8) Uani 1 1 d . . .
C7 C 0.8946(4) -0.02542(18) 0.8477(2) 0.0462(10) Uani 1 1 d . . .
H7A H 0.8375 -0.0107 0.8806 0.055 Uiso 1 1 calc R . .
H7B H 0.8766 -0.0634 0.8402 0.055 Uiso 1 1 calc R . .
C8 C 0.9033(4) -0.04013(16) 0.6730(2) 0.0407(9) Uani 1 1 d . . .
C9 C 0.8527(4) -0.09083(17) 0.6608(3) 0.0501(10) Uani 1 1 d . . .
C10 C 0.8946(5) -0.12662(18) 0.6121(3) 0.0596(12) Uani 1 1 d . . .
C11 C 0.9864(5) -0.1123(2) 0.5721(3) 0.0635(13) Uani 1 1 d . . .
C12 C 1.0393(4) -0.0625(2) 0.5819(3) 0.0556(11) Uani 1 1 d . . .
C13 C 0.9967(4) -0.02700(18) 0.6312(3) 0.0474(10) Uani 1 1 d . . .
C14 C 0.6652(4) 0.01407(16) 0.6864(2) 0.0404(9) Uani 1 1 d . . .
C15 C 0.6184(4) 0.03696(16) 0.6038(2) 0.0420(9) Uani 1 1 d . . .
C16 C 0.4818(4) 0.05286(17) 0.5619(2) 0.0460(10) Uani 1 1 d . . .
C17 C 0.3871(4) 0.04552(19) 0.6039(3) 0.0526(11) Uani 1 1 d . . .
C18 C 0.4269(4) 0.0218(2) 0.6844(3) 0.0557(12) Uani 1 1 d . . .
C19 C 0.5651(4) 0.00603(18) 0.7247(2) 0.0484(10) Uani 1 1 d . . .
C20 C 1.3117(4) 0.09339(16) 0.9104(3) 0.0439(9) Uani 1 1 d . . .
H20A H 1.3710 0.0866 0.8743 0.053 Uiso 1 1 calc R . .
H20B H 1.3706 0.1096 0.9668 0.053 Uiso 1 1 calc R . .
C21 C 1.2421(4) 0.18422(16) 0.8009(3) 0.0474(10) Uani 1 1 d . . .
C22 C 1.2312(4) 0.17948(19) 0.7136(3) 0.0563(11) Uani 1 1 d . . .
C23 C 1.2974(5) 0.2128(2) 0.6750(3) 0.0674(13) Uani 1 1 d . . .
C24 C 1.3781(5) 0.2524(2) 0.7232(4) 0.0727(15) Uani 1 1 d . . .
C25 C 1.3947(5) 0.2581(2) 0.8098(4) 0.0678(13) Uani 1 1 d . . .
C26 C 1.3273(4) 0.22436(18) 0.8480(3) 0.0530(11) Uani 1 1 d . . .
C27 C 1.1040(4) 0.17231(16) 0.9273(3) 0.0481(10) Uani 1 1 d . . .
C28 C 1.0002(5) 0.20903(19) 0.8929(3) 0.0591(12) Uani 1 1 d . . .
C29 C 0.9333(5) 0.2341(2) 0.9415(5) 0.0812(18) Uani 1 1 d . . .
C30 C 0.9744(7) 0.2232(2) 1.0305(5) 0.0856(18) Uani 1 1 d . . .
C31 C 1.0752(7) 0.1870(2) 1.0674(4) 0.0774(16) Uani 1 1 d . . .
C32 C 1.1408(5) 0.16180(18) 1.0174(3) 0.0576(12) Uani 1 1 d . . .
C33 C 0.7752(5) 0.1546(2) 0.6382(3) 0.0645(13) Uani 1 1 d . . .
C34 C 0.6595(6) 0.1876(2) 0.5822(4) 0.102(2) Uani 1 1 d . . .
H34A H 0.5695 0.1734 0.5815 0.153 Uiso 1 1 calc R . .
H34B H 0.6610 0.1881 0.5219 0.153 Uiso 1 1 calc R . .
H34C H 0.6711 0.2231 0.6058 0.153 Uiso 1 1 calc R . .
F22A F 0.6440(6) 0.3106(2) 0.2777(4) 0.0725(17) Uani 0.60 1 d PDU A 1
F23A F 0.5173(5) 0.3830(3) 0.2843(5) 0.079(2) Uani 0.60 1 d PDU A 1
F24A F 0.6247(7) 0.3360(3) 0.4050(3) 0.0907(19) Uani 0.60 1 d PDU A 1
F22B F 0.6022(12) 0.3346(6) 0.2365(7) 0.114(5) Uani 0.28 1 d PDU A 2
F23B F 0.5229(8) 0.3881(4) 0.3175(8) 0.056(4) Uani 0.28 1 d PDU A 2
F24B F 0.6417(14) 0.3160(5) 0.3805(10) 0.153(9) Uani 0.28 1 d PDU A 2
F22C F 0.5436(16) 0.3689(7) 0.2375(9) 0.070(7) Uani 0.12 1 d PDU A 3
F23C F 0.5668(19) 0.3614(9) 0.3812(13) 0.112(12) Uani 0.12 1 d PDU A 3
F24C F 0.6658(15) 0.3022(3) 0.3181(14) 0.058(8) Uani 0.12 1 d PDU A 3
F21 F 0.7533(3) 0.38395(13) 0.3426(2) 0.0999(11) Uani 1 1 d DU A .
B1 B 0.6333(5) 0.35424(18) 0.3225(3) 0.0769(19) Uani 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
Pd1 0.02894(15) 0.04466(19) 0.04048(17) -0.00277(13) 0.00955(12) -0.00210(12)
P1 0.0313(5) 0.0500(6) 0.0373(5) -0.0059(4) 0.0140(4) -0.0075(4)
P2 0.0327(5) 0.0422(6) 0.0462(6) -0.0038(5) 0.0132(4) -0.0044(4)
F1 0.0761(17) 0.0612(16) 0.0551(14) -0.0058(12) 0.0259(14) -0.0251(13)
F2 0.137(3) 0.0503(18) 0.0780(19) -0.0105(15) 0.0349(19) -0.0072(18)
F3 0.112(2) 0.093(2) 0.0692(18) -0.0183(17) 0.0349(18) 0.0362(19)
F4 0.0615(16) 0.119(3) 0.0673(17) -0.0106(17) 0.0400(15) 0.0121(16)
F5 0.0451(13) 0.0681(17) 0.0599(14) -0.0102(12) 0.0303(12) -0.0149(12)
F6 0.0359(11) 0.0690(16) 0.0389(11) -0.0035(11) 0.0177(10) -0.0058(11)
F7 0.0423(12) 0.0737(17) 0.0486(13) 0.0046(12) 0.0122(11) -0.0012(12)
F8 0.0320(12) 0.110(2) 0.0646(16) 0.0006(15) 0.0133(11) 0.0018(13)
F9 0.0344(12) 0.150(3) 0.0567(15) -0.0008(17) 0.0229(12) -0.0120(15)
F10 0.0366(12) 0.125(2) 0.0424(13) 0.0090(14) 0.0137(11) -0.0168(14)
F11 0.0846(19) 0.102(2) 0.0510(15) -0.0134(15) 0.0251(14) -0.0294(17)
F12 0.101(2) 0.137(3) 0.0525(17) 0.0167(18) 0.0281(17) -0.021(2)
F13 0.103(2) 0.112(3) 0.104(2) 0.039(2) 0.044(2) -0.028(2)
F14 0.103(2) 0.086(2) 0.112(3) -0.0060(19) 0.042(2) -0.053(2)
F15 0.0615(15) 0.0760(19) 0.0621(16) -0.0141(14) 0.0210(13) -0.0279(14)
F16 0.0494(15) 0.0652(18) 0.092(2) -0.0141(16) 0.0049(14) 0.0134(13)
F17 0.0642(19) 0.086(2) 0.185(4) -0.053(2) 0.033(2) 0.0154(18)
F18 0.152(3) 0.103(3) 0.184(4) -0.055(3) 0.120(3) 0.000(2)
F19 0.190(4) 0.082(2) 0.096(2) -0.0212(19) 0.098(3) -0.016(2)
F20 0.102(2) 0.0558(16) 0.0583(15) -0.0013(13) 0.0373(16) 0.0037(16)
N1 0.0411(18) 0.052(2) 0.049(2) 0.0017(17) 0.0028(16) -0.0075(17)
C1 0.0342(18) 0.042(2) 0.0346(18) -0.0051(16) 0.0158(16) 0.0029(16)
C2 0.0361(19) 0.048(2) 0.0365(19) -0.0086(17) 0.0152(16) -0.0051(17)
C3 0.048(2) 0.050(3) 0.044(2) -0.0034(19) 0.0225(19) -0.0031(19)
C4 0.044(2) 0.055(3) 0.041(2) 0.0019(19) 0.0170(18) 0.0115(19)
C5 0.0294(18) 0.055(3) 0.038(2) -0.0034(18) 0.0138(16) 0.0052(17)
C6 0.0290(17) 0.046(2) 0.0342(18) -0.0026(16) 0.0135(15) 0.0014(16)
C7 0.038(2) 0.065(3) 0.036(2) -0.0015(19) 0.0123(17) -0.0097(19)
C8 0.0320(19) 0.052(2) 0.0365(19) -0.0037(17) 0.0104(16) -0.0050(17)
C9 0.054(2) 0.057(3) 0.035(2) 0.0001(19) 0.0114(19) -0.006(2)
C10 0.079(3) 0.045(3) 0.047(2) -0.004(2) 0.011(2) 0.007(2)
C11 0.073(3) 0.066(3) 0.052(3) -0.007(2) 0.024(2) 0.021(3)
C12 0.047(2) 0.079(3) 0.043(2) -0.005(2) 0.018(2) 0.008(2)
C13 0.034(2) 0.063(3) 0.044(2) -0.007(2) 0.0127(18) -0.0006(19)
C14 0.0306(18) 0.054(2) 0.0357(19) -0.0121(18) 0.0099(16) -0.0079(17)
C15 0.0324(19) 0.057(3) 0.040(2) -0.0126(18) 0.0159(17) -0.0106(17)
C16 0.039(2) 0.060(3) 0.039(2) -0.0091(19) 0.0129(17) -0.0096(19)
C17 0.031(2) 0.075(3) 0.049(2) -0.014(2) 0.0102(18) -0.009(2)
C18 0.032(2) 0.094(4) 0.045(2) -0.010(2) 0.0179(19) -0.015(2)
C19 0.038(2) 0.074(3) 0.033(2) -0.006(2) 0.0119(17) -0.015(2)
C20 0.0305(18) 0.054(3) 0.046(2) -0.0020(19) 0.0123(17) -0.0016(17)
C21 0.034(2) 0.048(2) 0.058(2) 0.004(2) 0.0145(19) -0.0004(18)
C22 0.046(2) 0.068(3) 0.050(2) -0.001(2) 0.010(2) -0.008(2)
C23 0.060(3) 0.092(4) 0.051(3) 0.018(3) 0.019(2) 0.003(3)
C24 0.060(3) 0.075(4) 0.082(4) 0.028(3) 0.024(3) -0.012(3)
C25 0.056(3) 0.064(3) 0.078(3) 0.007(3) 0.017(3) -0.017(2)
C26 0.044(2) 0.059(3) 0.050(2) 0.003(2) 0.009(2) -0.007(2)
C27 0.041(2) 0.043(2) 0.063(3) -0.013(2) 0.021(2) -0.0095(18)
C28 0.044(2) 0.058(3) 0.071(3) -0.015(2) 0.013(2) -0.008(2)
C29 0.051(3) 0.055(3) 0.142(6) -0.038(4) 0.038(3) -0.005(2)
C30 0.093(4) 0.071(4) 0.119(5) -0.037(4) 0.070(4) -0.013(3)
C31 0.109(5) 0.055(3) 0.092(4) -0.026(3) 0.066(4) -0.019(3)
C32 0.069(3) 0.047(3) 0.070(3) -0.018(2) 0.039(3) -0.012(2)
C33 0.054(3) 0.062(3) 0.065(3) 0.010(2) 0.006(2) -0.015(2)
C34 0.065(3) 0.085(4) 0.116(5) 0.047(4) -0.019(3) -0.006(3)
F22A 0.067(3) 0.065(3) 0.079(4) -0.015(3) 0.018(3) 0.005(3)
F23A 0.074(4) 0.087(4) 0.085(5) 0.012(4) 0.041(3) 0.020(3)
F24A 0.119(5) 0.068(4) 0.090(4) -0.002(3) 0.043(4) -0.002(4)
F22B 0.094(8) 0.134(10) 0.137(9) -0.069(8) 0.070(7) -0.028(7)
F23B 0.043(5) 0.092(7) 0.034(6) -0.015(5) 0.015(4) 0.004(5)
F24B 0.147(12) 0.115(12) 0.185(13) 0.019(9) 0.043(9) 0.000(9)
F22C 0.053(10) 0.044(10) 0.094(11) 0.021(9) 0.001(8) 0.010(8)
F23C 0.092(14) 0.120(16) 0.134(16) -0.008(10) 0.053(11) 0.004(10)
F24C 0.064(11) 0.057(11) 0.037(10) 0.022(8) -0.002(8) 0.012(8)
F21 0.0701(19) 0.125(3) 0.121(3) -0.059(2) 0.0543(19) -0.0356(19)
B1 0.047(3) 0.085(5) 0.103(5) -0.029(4) 0.031(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'
B B 0.0013 0.0007 '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'
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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.316 0.631 0.288 128.4 42.3
2 0.316 0.869 0.788 128.4 42.4
3 0.684 0.131 0.212 128.5 42.0
4 0.684 0.369 0.712 128.5 42.2
|
1100894.cif | #------------------------------------------------------------------------------
#$Date: 2018-09-01 22:50:30 +0300 (Sat, 01 Sep 2018) $
#$Revision: 210323 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100894.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_1100894
loop_
_publ_author_name
'Chase, Preston A.'
'Gagliardo, Marcella'
'Lutz, Martin'
'Spek, Anthony L.'
'van Klink, Gerard P. M.'
'van Koten, Gerard'
_publ_section_title
;
Electron-Poor Pentafluorophenyl-Substituted PCP--Palladium Pincer Complexes
;
_journal_coden_ASTM INOCAJ
_journal_issue 9
_journal_name_full Organometallics
_journal_page_first 2016
_journal_page_last 2019
_journal_paper_doi 10.1021/om0500063
_journal_volume 24
_journal_year 2005
_chemical_formula_moiety 'C32 H7 Cl F20 P2 Pd, 2.1(C7 H8)'
_chemical_formula_sum 'C46.7 H23.8 Cl F20 P2 Pd'
_chemical_formula_weight 1168.65
_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 122.5592(3)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 15.4853(1)
_cell_length_b 13.6515(1)
_cell_length_c 26.0274(2)
_cell_measurement_reflns_used 83708
_cell_measurement_temperature 150(2)
_cell_measurement_theta_max 27.48
_cell_measurement_theta_min 1.02
_cell_volume 4637.39(6)
_diffrn_ambient_temperature 150(2)
_diffrn_measurement_device_type 'Nonius KappaCCD'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'rotating anode'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0539
_diffrn_reflns_av_sigmaI/netI 0.0284
_diffrn_reflns_limit_h_max 20
_diffrn_reflns_limit_h_min -20
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_l_max 33
_diffrn_reflns_limit_l_min -33
_diffrn_reflns_number 77297
_diffrn_reflns_theta_max 27.49
_diffrn_reflns_theta_min 1.56
_exptl_absorpt_coefficient_mu 0.642
_exptl_absorpt_correction_T_max 0.83
_exptl_absorpt_correction_T_min 0.74
_exptl_absorpt_correction_type multi-scan
_exptl_crystal_colour yellowish
_exptl_crystal_density_diffrn 1.674
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 2308
_exptl_crystal_size_max 0.55
_exptl_crystal_size_mid 0.50
_exptl_crystal_size_min 0.30
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.060
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 670
_refine_ls_number_reflns 10621
_refine_ls_number_restraints 114
_refine_ls_restrained_S_all 1.091
_refine_ls_R_factor_all 0.0542
_refine_ls_R_factor_gt 0.0430
_refine_ls_shift/su_max 0.022
_refine_ls_shift/su_mean 0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0781P)^2^+5.6672P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1286
_refine_ls_wR_factor_ref 0.1381
_reflns_number_gt 8624
_reflns_number_total 10621
_reflns_threshold_expression I>2\s(I)
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_original_formula_sum 'C46.70 H23.80 Cl F20 P2 Pd'
_cod_database_code 1100894
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
Pd1 Pd 0.355940(16) 0.444444(16) 0.243117(11) 0.02756(9) Uani 1 1 d . . .
Cl1 Cl 0.33698(7) 0.57661(6) 0.17926(4) 0.0436(2) Uani 1 1 d . . .
P1 P 0.19101(6) 0.41139(6) 0.21228(4) 0.03027(17) Uani 1 1 d . . .
P2 P 0.52958(6) 0.43899(5) 0.29732(4) 0.02710(17) Uani 1 1 d . . .
F1 F 0.09528(16) 0.49486(16) 0.08974(10) 0.0493(5) Uani 1 1 d . . .
F2 F -0.0455(2) 0.6367(2) 0.03487(14) 0.0775(8) Uani 1 1 d . . .
F3 F -0.1315(2) 0.7183(2) 0.09282(18) 0.0923(11) Uani 1 1 d . . .
F4 F -0.0710(2) 0.6594(2) 0.20662(18) 0.0830(10) Uani 1 1 d . . .
F5 F 0.0705(2) 0.52219(17) 0.26256(13) 0.0589(6) Uani 1 1 d . . .
F6 F 0.24911(15) 0.31678(16) 0.12764(10) 0.0448(5) Uani 1 1 d . . .
F7 F 0.15181(17) 0.17513(17) 0.04533(10) 0.0513(5) Uani 1 1 d . . .
F8 F -0.0173(2) 0.09113(18) 0.03062(11) 0.0618(6) Uani 1 1 d . . .
F9 F -0.09204(17) 0.15180(18) 0.09925(12) 0.0599(6) Uani 1 1 d . . .
F10 F -0.00200(15) 0.29930(16) 0.17763(10) 0.0441(5) Uani 1 1 d . . .
F11 F 0.45027(18) 0.62360(16) 0.32294(11) 0.0610(7) Uani 1 1 d . . .
F12 F 0.52641(19) 0.72322(17) 0.42567(12) 0.0618(7) Uani 1 1 d . . .
F13 F 0.70304(17) 0.66709(16) 0.52781(10) 0.0493(5) Uani 1 1 d . . .
F14 F 0.80590(18) 0.5100(2) 0.52458(11) 0.0668(7) Uani 1 1 d . . .
F15 F 0.73509(17) 0.41028(19) 0.42104(11) 0.0611(7) Uani 1 1 d . . .
F16 F 0.48248(16) 0.36702(16) 0.17988(10) 0.0464(5) Uani 1 1 d . . .
F17 F 0.5780(2) 0.39611(19) 0.12013(11) 0.0602(7) Uani 1 1 d . . .
F18 F 0.74966(17) 0.50650(15) 0.17049(10) 0.0450(5) Uani 1 1 d . . .
F19 F 0.81991(16) 0.59693(16) 0.27878(10) 0.0456(5) Uani 1 1 d . . .
F20 F 0.72620(18) 0.57221(17) 0.33808(10) 0.0516(6) Uani 1 1 d . . .
C1 C 0.3796(2) 0.3320(2) 0.30022(14) 0.0285(6) Uani 1 1 d . . .
C2 C 0.3051(2) 0.3061(2) 0.31274(14) 0.0323(6) Uani 1 1 d . . .
C3 C 0.3234(3) 0.2317(3) 0.35362(16) 0.0390(7) Uani 1 1 d . . .
H3 H 0.2725 0.2150 0.3619 0.047 Uiso 1 1 calc R . .
C4 C 0.4157(3) 0.1817(3) 0.38252(16) 0.0411(8) Uani 1 1 d . . .
H4 H 0.4282 0.1312 0.4109 0.049 Uiso 1 1 calc R . .
C5 C 0.4897(3) 0.2049(2) 0.37027(16) 0.0382(7) Uani 1 1 d . . .
H5 H 0.5524 0.1695 0.3895 0.046 Uiso 1 1 calc R . .
C6 C 0.4725(2) 0.2801(2) 0.32983(15) 0.0311(6) Uani 1 1 d . . .
C7 C 0.2069(2) 0.3651(3) 0.28294(15) 0.0362(7) Uani 1 1 d . . .
H7A H 0.2127 0.4199 0.3096 0.043 Uiso 1 1 calc R . .
H7B H 0.1482 0.3233 0.2741 0.043 Uiso 1 1 calc R . .
C8 C 0.0896(2) 0.5036(2) 0.17819(17) 0.0381(8) Uani 1 1 d . . .
C9 C 0.0566(3) 0.5354(3) 0.12012(19) 0.0444(9) Uani 1 1 d . . .
C10 C -0.0178(3) 0.6077(3) 0.0909(2) 0.0571(11) Uani 1 1 d . . .
C11 C -0.0605(3) 0.6487(3) 0.1205(3) 0.0650(14) Uani 1 1 d . . .
C12 C -0.0296(3) 0.6190(3) 0.1776(3) 0.0615(13) Uani 1 1 d . . .
C13 C 0.0446(3) 0.5471(3) 0.2068(2) 0.0473(9) Uani 1 1 d . . .
C14 C 0.1292(2) 0.3121(2) 0.15718(14) 0.0292(6) Uani 1 1 d . . .
C15 C 0.1649(2) 0.2785(2) 0.12183(15) 0.0332(6) Uani 1 1 d . . .
C16 C 0.1163(3) 0.2061(3) 0.07932(15) 0.0379(7) Uani 1 1 d . . .
C17 C 0.0295(3) 0.1620(3) 0.07149(17) 0.0427(8) Uani 1 1 d . . .
C18 C -0.0082(3) 0.1934(3) 0.10610(17) 0.0406(8) Uani 1 1 d . . .
C19 C 0.0398(2) 0.2679(2) 0.14691(15) 0.0335(7) Uani 1 1 d . . .
C20 C 0.5536(2) 0.3090(2) 0.31729(16) 0.0347(7) Uani 1 1 d . . .
H20A H 0.5469 0.2702 0.2832 0.042 Uiso 1 1 calc R . .
H20B H 0.6231 0.2990 0.3539 0.042 Uiso 1 1 calc R . .
C21 C 0.5878(2) 0.5095(2) 0.36783(14) 0.0301(6) Uani 1 1 d . . .
C22 C 0.5392(3) 0.5924(2) 0.37143(15) 0.0366(7) Uani 1 1 d . . .
C23 C 0.5771(3) 0.6460(2) 0.42426(17) 0.0410(8) Uani 1 1 d . . .
C24 C 0.6665(3) 0.6166(2) 0.47645(15) 0.0360(7) Uani 1 1 d . . .
C25 C 0.7169(3) 0.5365(3) 0.47454(16) 0.0413(8) Uani 1 1 d . . .
C26 C 0.6787(2) 0.4850(3) 0.42105(16) 0.0361(7) Uani 1 1 d . . .
C27 C 0.6003(2) 0.4678(2) 0.26146(14) 0.0280(6) Uani 1 1 d . . .
C28 C 0.5656(2) 0.4251(2) 0.20538(16) 0.0338(7) Uani 1 1 d . . .
C29 C 0.6137(3) 0.4381(2) 0.17408(16) 0.0378(7) Uani 1 1 d . . .
C30 C 0.7005(3) 0.4951(2) 0.19932(16) 0.0346(7) Uani 1 1 d . . .
C31 C 0.7362(2) 0.5402(2) 0.25437(16) 0.0336(7) Uani 1 1 d . . .
C32 C 0.6863(2) 0.5264(2) 0.28445(15) 0.0326(6) Uani 1 1 d . . .
C33 C 0.1617(3) 0.7892(3) 0.2430(2) 0.0572(10) Uani 1 1 d D . .
C34 C 0.0822(3) 0.8548(3) 0.2226(2) 0.0563(10) Uani 1 1 d . . .
H34 H 0.0586 0.8717 0.2485 0.068 Uiso 1 1 calc R . .
C35 C 0.0360(4) 0.8966(4) 0.1656(3) 0.0688(13) Uani 1 1 d . . .
H35 H -0.0193 0.9411 0.1523 0.083 Uiso 1 1 calc R . .
C36 C 0.0699(5) 0.8742(5) 0.1279(3) 0.0856(18) Uani 1 1 d . . .
H36 H 0.0390 0.9032 0.0887 0.103 Uiso 1 1 calc R . .
C37 C 0.1510(5) 0.8075(5) 0.1486(3) 0.087(2) Uani 1 1 d . . .
H37 H 0.1753 0.7910 0.1231 0.105 Uiso 1 1 calc R . .
C38 C 0.1950(4) 0.7665(3) 0.2046(3) 0.0672(14) Uani 1 1 d . . .
H38 H 0.2496 0.7213 0.2177 0.081 Uiso 1 1 calc R . .
C39 C 0.2081(4) 0.7446(4) 0.3035(3) 0.0855(17) Uani 1 1 d D . .
H39A H 0.2251 0.7959 0.3338 0.128 Uiso 1 1 calc R . .
H39B H 0.2707 0.7097 0.3136 0.128 Uiso 1 1 calc R . .
H39C H 0.1597 0.6984 0.3035 0.128 Uiso 1 1 calc R . .
C40 C 0.2306(3) 0.5956(4) 0.00933(18) 0.0473(15) Uani 0.60 1 d PDU . .
C41 C 0.2551(4) 0.5026(4) 0.0300(2) 0.0607(19) Uani 0.60 1 d PDU . .
H41 H 0.2282 0.4753 0.0521 0.073 Uiso 0.60 1 calc PR . .
C42 C 0.3167(5) 0.4477(6) 0.0199(3) 0.103(4) Uani 0.60 1 d PDU . .
H42 H 0.3335 0.3825 0.0347 0.123 Uiso 0.60 1 calc PR . .
C43 C 0.3543(6) 0.4876(8) -0.0118(4) 0.138(5) Uani 0.60 1 d PDU . .
H43 H 0.3968 0.4500 -0.0203 0.165 Uiso 0.60 1 calc PR . .
C44 C 0.3311(7) 0.5802(8) -0.0312(4) 0.125(4) Uani 0.60 1 d PDU . .
H44 H 0.3606 0.6084 -0.0518 0.151 Uiso 0.60 1 calc PR . .
C45 C 0.2682(6) 0.6346(7) -0.0228(3) 0.101(3) Uani 0.60 1 d PDU . .
H45 H 0.2501 0.6990 -0.0389 0.121 Uiso 0.60 1 calc PR . .
C46 C 0.1652(5) 0.6573(5) 0.0201(3) 0.0546(17) Uani 0.60 1 d PDU . .
H46A H 0.0932 0.6422 -0.0101 0.082 Uiso 0.60 1 calc PR . .
H46B H 0.1785 0.7264 0.0165 0.082 Uiso 0.60 1 calc PR . .
H46C H 0.1798 0.6449 0.0612 0.082 Uiso 0.60 1 calc PR . .
C47 C 0.5662(5) 0.4244(5) 0.5173(4) 0.130(3) Uani 1 1 d DU . .
H47 H 0.6123 0.3709 0.5290 0.156 Uiso 0.50 1 calc PR A 1
C48 C 0.4842(5) 0.4305(4) 0.4602(3) 0.0771(17) Uani 1 1 d DU B .
H48 H 0.4736 0.3804 0.4321 0.092 Uiso 1 1 calc R . .
C49 C 0.4169(5) 0.5039(6) 0.4413(3) 0.115(3) Uani 1 1 d DU . .
H49 H 0.3593 0.5064 0.4006 0.138 Uiso 1 1 calc R B .
C50 C 0.6412(12) 0.3476(11) 0.5401(10) 0.173(8) Uani 0.50 1 d PDU B 2
H50A H 0.6175 0.2949 0.5098 0.259 Uiso 0.50 1 calc PR B 2
H50B H 0.6510 0.3217 0.5780 0.259 Uiso 0.50 1 calc PR B 2
H50C H 0.7063 0.3736 0.5481 0.259 Uiso 0.50 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
Pd1 0.02295(13) 0.02292(13) 0.03634(15) 0.00071(8) 0.01564(11) -0.00186(8)
Cl1 0.0408(4) 0.0334(4) 0.0490(5) 0.0115(3) 0.0191(4) -0.0005(3)
P1 0.0237(4) 0.0265(4) 0.0413(4) -0.0033(3) 0.0179(3) -0.0023(3)
P2 0.0230(4) 0.0235(4) 0.0353(4) 0.0006(3) 0.0160(3) -0.0015(3)
F1 0.0436(12) 0.0460(12) 0.0485(12) 0.0094(10) 0.0184(10) 0.0101(9)
F2 0.0538(15) 0.0613(16) 0.0806(19) 0.0229(14) 0.0118(14) 0.0177(12)
F3 0.0480(15) 0.0568(16) 0.145(3) 0.0148(18) 0.0337(18) 0.0296(13)
F4 0.0676(17) 0.0515(15) 0.159(3) -0.0101(17) 0.080(2) 0.0113(13)
F5 0.0680(15) 0.0454(12) 0.0923(19) -0.0020(12) 0.0623(15) 0.0046(11)
F6 0.0370(11) 0.0534(12) 0.0533(12) -0.0039(10) 0.0304(10) -0.0024(9)
F7 0.0551(13) 0.0556(13) 0.0472(12) -0.0050(10) 0.0302(11) 0.0136(10)
F8 0.0614(15) 0.0507(13) 0.0589(15) -0.0251(11) 0.0227(12) -0.0116(12)
F9 0.0447(12) 0.0577(14) 0.0764(17) -0.0219(12) 0.0319(12) -0.0271(11)
F10 0.0342(10) 0.0500(12) 0.0568(13) -0.0122(10) 0.0302(10) -0.0106(9)
F11 0.0559(14) 0.0404(12) 0.0475(13) -0.0055(10) 0.0019(11) 0.0200(10)
F12 0.0639(15) 0.0401(12) 0.0643(15) -0.0142(11) 0.0231(13) 0.0114(11)
F13 0.0527(13) 0.0507(12) 0.0415(11) -0.0145(9) 0.0234(10) -0.0161(10)
F14 0.0455(13) 0.0782(17) 0.0414(13) -0.0014(12) 0.0001(10) 0.0152(12)
F15 0.0385(12) 0.0672(15) 0.0568(14) -0.0080(12) 0.0120(11) 0.0240(11)
F16 0.0391(11) 0.0530(12) 0.0471(12) -0.0197(10) 0.0232(10) -0.0219(9)
F17 0.0694(16) 0.0732(16) 0.0521(13) -0.0315(12) 0.0420(13) -0.0314(13)
F18 0.0552(12) 0.0449(11) 0.0543(13) -0.0042(9) 0.0423(11) -0.0057(10)
F19 0.0414(11) 0.0484(12) 0.0545(13) -0.0115(10) 0.0307(10) -0.0227(9)
F20 0.0550(13) 0.0667(14) 0.0422(12) -0.0252(10) 0.0321(11) -0.0360(11)
C1 0.0317(15) 0.0224(13) 0.0319(15) -0.0032(11) 0.0174(13) -0.0050(11)
C2 0.0306(15) 0.0330(16) 0.0333(16) -0.0079(12) 0.0173(13) -0.0088(12)
C3 0.0466(19) 0.0380(17) 0.0408(18) -0.0083(14) 0.0291(16) -0.0145(15)
C4 0.050(2) 0.0325(16) 0.0402(18) 0.0020(14) 0.0242(16) -0.0083(15)
C5 0.0418(18) 0.0268(15) 0.0435(19) 0.0019(13) 0.0213(16) -0.0005(13)
C6 0.0337(16) 0.0230(14) 0.0371(16) -0.0025(12) 0.0194(14) -0.0030(11)
C7 0.0327(16) 0.0401(17) 0.0405(18) -0.0083(14) 0.0227(15) -0.0063(13)
C8 0.0250(15) 0.0261(15) 0.059(2) -0.0021(14) 0.0202(15) -0.0010(12)
C9 0.0290(16) 0.0320(16) 0.065(2) -0.0022(16) 0.0203(17) 0.0014(13)
C10 0.0351(19) 0.043(2) 0.067(3) 0.0121(19) 0.0109(19) 0.0047(16)
C11 0.0304(19) 0.036(2) 0.114(4) 0.004(2) 0.029(2) 0.0103(15)
C12 0.042(2) 0.036(2) 0.116(4) -0.006(2) 0.049(3) 0.0026(16)
C13 0.0357(18) 0.0320(17) 0.080(3) -0.0074(17) 0.035(2) -0.0029(14)
C14 0.0262(14) 0.0240(13) 0.0346(16) 0.0008(12) 0.0145(13) 0.0021(11)
C15 0.0273(15) 0.0334(16) 0.0382(17) 0.0057(13) 0.0171(13) 0.0062(12)
C16 0.0374(17) 0.0363(17) 0.0370(17) 0.0009(14) 0.0180(15) 0.0116(14)
C17 0.0397(18) 0.0333(17) 0.0398(18) -0.0055(14) 0.0113(15) 0.0016(14)
C18 0.0303(16) 0.0376(18) 0.046(2) -0.0037(15) 0.0158(15) -0.0041(13)
C19 0.0281(15) 0.0302(15) 0.0423(18) -0.0012(13) 0.0190(14) 0.0005(12)
C20 0.0322(16) 0.0229(14) 0.0498(19) 0.0047(13) 0.0225(15) 0.0022(12)
C21 0.0292(15) 0.0290(15) 0.0338(16) 0.0004(12) 0.0182(13) -0.0043(12)
C22 0.0331(16) 0.0299(15) 0.0365(17) 0.0034(13) 0.0119(14) 0.0026(13)
C23 0.0419(18) 0.0307(16) 0.048(2) -0.0027(14) 0.0230(17) -0.0004(14)
C24 0.0332(16) 0.0398(17) 0.0343(16) -0.0052(13) 0.0177(14) -0.0120(13)
C25 0.0287(16) 0.052(2) 0.0344(17) 0.0026(15) 0.0111(14) 0.0000(14)
C26 0.0263(15) 0.0380(17) 0.0419(18) 0.0017(14) 0.0170(14) 0.0063(13)
C27 0.0249(14) 0.0263(13) 0.0329(15) -0.0013(12) 0.0156(12) -0.0018(11)
C28 0.0291(15) 0.0305(15) 0.0399(17) -0.0067(13) 0.0174(14) -0.0057(12)
C29 0.0449(19) 0.0340(17) 0.0372(18) -0.0082(13) 0.0241(16) -0.0073(14)
C30 0.0409(17) 0.0293(15) 0.0437(18) -0.0010(13) 0.0294(16) -0.0012(13)
C31 0.0311(16) 0.0282(14) 0.0426(18) -0.0012(13) 0.0206(14) -0.0074(12)
C32 0.0333(16) 0.0312(15) 0.0358(17) -0.0070(13) 0.0202(14) -0.0081(13)
C33 0.049(2) 0.045(2) 0.075(3) -0.005(2) 0.032(2) -0.0104(18)
C34 0.055(2) 0.051(2) 0.076(3) -0.008(2) 0.044(2) -0.0041(19)
C35 0.067(3) 0.055(3) 0.078(3) -0.001(2) 0.034(3) -0.005(2)
C36 0.112(5) 0.074(4) 0.069(3) -0.009(3) 0.047(3) -0.040(4)
C37 0.111(5) 0.084(4) 0.113(5) -0.054(4) 0.091(4) -0.055(4)
C38 0.060(3) 0.052(2) 0.110(4) -0.029(3) 0.058(3) -0.018(2)
C39 0.071(3) 0.069(3) 0.092(4) 0.014(3) 0.028(3) -0.007(3)
C40 0.035(3) 0.076(4) 0.020(2) -0.005(3) 0.007(2) -0.013(3)
C41 0.042(3) 0.071(4) 0.052(4) -0.021(3) 0.014(3) 0.004(3)
C42 0.078(6) 0.141(8) 0.057(5) -0.040(5) 0.016(4) 0.038(5)
C43 0.117(8) 0.202(10) 0.099(7) -0.056(7) 0.061(6) 0.040(7)
C44 0.125(8) 0.203(10) 0.074(6) -0.016(6) 0.070(6) -0.003(7)
C45 0.097(6) 0.167(8) 0.047(4) 0.011(5) 0.045(4) -0.007(6)
C46 0.059(4) 0.048(3) 0.036(3) 0.016(3) 0.013(3) 0.017(3)
C47 0.140(6) 0.142(6) 0.159(7) 0.007(5) 0.115(6) -0.042(5)
C48 0.103(4) 0.087(4) 0.072(3) -0.039(3) 0.067(3) -0.052(3)
C49 0.130(5) 0.134(6) 0.113(5) -0.025(4) 0.086(4) -0.062(5)
C50 0.164(11) 0.177(12) 0.181(12) 0.042(9) 0.095(9) -0.005(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'
Cl Cl 0.1484 0.1585 '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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100895.cif | #------------------------------------------------------------------------------
#$Date: 2023-04-20 14:53:48 +0300 (Thu, 20 Apr 2023) $
#$Revision: 282777 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100895.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_1100895
loop_
_publ_author_name
'Ward, Benjamin D.'
'Orde, Gavin'
'Clot, Eric'
'Cowley, Andrew R.'
'Gade, Lutz H.'
'Mountford, Philip'
_publ_section_title
;
Reactions of Neutral and Cationic Diamide-Supported Imido Complexes with
CO <sub>2</sub> and Other Heterocumulenes:  Issues of Site
Selectivity
;
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2368
_journal_page_last 2385
_journal_paper_doi 10.1021/om0500265
_journal_volume 24
_journal_year 2005
_chemical_formula_moiety ' C24 H47 Cl N5 Nb O Si2 '
_chemical_formula_sum 'C24 H47 Cl N5 Nb O Si2'
_chemical_formula_weight 606.21
_chemical_melting_point ?
_chemical_name_systematic
;
[Nb(NtBu){MeC(2-C5H4N)(CH2NSiMe3)(CH2NC(OSiMe3)NtBu)}Cl]
;
_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
_cell_angle_alpha 90
_cell_angle_beta 100.7414(6)
_cell_angle_gamma 90
_cell_formula_units_Z 16
_cell_length_a 16.8425(3)
_cell_length_b 21.5100(4)
_cell_length_c 36.4135(7)
_cell_measurement_reflns_used 70472
_cell_measurement_temperature 150
_cell_measurement_theta_max 28
_cell_measurement_theta_min 5
_cell_volume 12960.8
_diffrn_ambient_temperature 150
_diffrn_measured_fraction_theta_max 0.869
_diffrn_measurement_device_type
;
Nonius KappaCCD
;
_diffrn_measurement_method \w
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.056
_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 47
_diffrn_reflns_limit_l_min -47
_diffrn_reflns_number 70472
_diffrn_reflns_theta_max 27.50
_diffrn_reflns_theta_min 5.11
_diffrn_standards_decay_% 0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 0.551
_exptl_absorpt_correction_T_max 0.96
_exptl_absorpt_correction_T_min 0.85
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_exptl_crystal_colour ' pale yellow '
_exptl_crystal_density_diffrn 1.243
_exptl_crystal_density_meas ?
_exptl_crystal_description ' plate '
_exptl_crystal_F_000 5089.006
_exptl_crystal_size_max 0.30
_exptl_crystal_size_mid 0.20
_exptl_crystal_size_min 0.08
_refine_diff_density_max 1.02
_refine_diff_density_min -0.50
_refine_ls_goodness_of_fit_ref 1.0441
_refine_ls_hydrogen_treatment noref
_refine_ls_matrix_type full
_refine_ls_number_parameters 1225
_refine_ls_number_reflns 12358
_refine_ls_R_factor_gt 0.0433
_refine_ls_shift/su_max 0.041017
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Chebychev polynomial with 3 parameters (Carruthers & Watkin , 1979)
1.02 0.284 0.702
;
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_ref 0.0501
_reflns_limit_h_max 21
_reflns_limit_h_min -21
_reflns_limit_k_max 27
_reflns_limit_k_min 0
_reflns_limit_l_max 47
_reflns_limit_l_min 0
_reflns_number_gt 12358
_reflns_number_total 25778
_reflns_threshold_expression >3.00\s(I)
_cod_original_sg_symbol_H-M 'P 1 21/n 1 '
_cod_original_formula_sum ' C24 H47 Cl N5 Nb O Si2 '
_cod_database_code 1100895
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x+1/2,y+1/2,-z+1/2
x+1/2,-y+1/2,z+1/2
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
Nb1 0.79974(3) 0.26795(2) 0.126612(12) 0.0273 1.0000 Uani
Cl1 0.92105(8) 0.32630(6) 0.11987(4) 0.0375 1.0000 Uani
N1 0.7877(3) 0.2274(2) 0.08358(11) 0.0365 1.0000 Uani
C1 0.7930(4) 0.1869(3) 0.05177(15) 0.0508 1.0000 Uani
C2 0.8665(5) 0.2073(4) 0.0353(2) 0.0758 1.0000 Uani
C3 0.8047(5) 0.1206(3) 0.06555(19) 0.0639 1.0000 Uani
C4 0.7161(5) 0.1917(5) 0.0226(2) 0.0942 1.0000 Uani
N2 0.8563(2) 0.18880(18) 0.16359(11) 0.0288 1.0000 Uani
C5 0.7896(3) 0.1800(2) 0.17612(13) 0.0283 1.0000 Uani
N3 0.7288(2) 0.21555(19) 0.15901(11) 0.0286 1.0000 Uani
C6 0.6687(3) 0.2415(3) 0.17845(14) 0.0352 1.0000 Uani
C7 0.6793(3) 0.3130(2) 0.18543(15) 0.0351 1.0000 Uani
N4 0.8251(2) 0.31483(18) 0.18957(11) 0.0276 1.0000 Uani
C8 0.9008(3) 0.3261(2) 0.20783(14) 0.0331 1.0000 Uani
C9 0.9187(3) 0.3508(3) 0.24341(15) 0.0394 1.0000 Uani
C10 0.8560(4) 0.3645(3) 0.26141(15) 0.0416 1.0000 Uani
C11 0.7782(4) 0.3525(2) 0.24338(15) 0.0389 1.0000 Uani
C12 0.7633(3) 0.3274(2) 0.20735(14) 0.0302 1.0000 Uani
N5 0.7088(3) 0.3296(2) 0.11877(12) 0.0374 1.0000 Uani
C13 0.6651(3) 0.3494(3) 0.14832(16) 0.0415 1.0000 Uani
C14 0.9323(3) 0.1530(3) 0.17514(16) 0.0397 1.0000 Uani
C15 0.9915(3) 0.1769(3) 0.15160(18) 0.0491 1.0000 Uani
C16 0.9200(4) 0.0830(3) 0.16817(18) 0.0484 1.0000 Uani
C17 0.9674(4) 0.1650(3) 0.21633(17) 0.0495 1.0000 Uani
O1 0.7814(2) 0.13929(16) 0.20369(9) 0.0345 1.0000 Uani
Si1 0.71427(11) 0.08026(8) 0.19969(4) 0.0456 1.0000 Uani
C18 0.6895(5) 0.0572(3) 0.14996(18) 0.0708 1.0000 Uani
C19 0.7673(5) 0.0185(3) 0.2300(2) 0.0668 1.0000 Uani
C20 0.6223(4) 0.1027(3) 0.2169(2) 0.0633 1.0000 Uani
C21 0.6129(3) 0.3320(3) 0.20731(17) 0.0474 1.0000 Uani
Si2 0.6592(1) 0.35575(8) 0.07482(5) 0.0470 1.0000 Uani
C22 0.7320(4) 0.3644(3) 0.04205(19) 0.0654 1.0000 Uani
C23 0.5744(4) 0.3017(4) 0.0563(2) 0.0678 1.0000 Uani
C24 0.6146(5) 0.4342(3) 0.0797(2) 0.0709 1.0000 Uani
Nb2 0.59712(3) 0.20844(2) 0.369364(13) 0.0308 1.0000 Uani
Cl2 0.51504(9) 0.21630(7) 0.30638(4) 0.0488 1.0000 Uani
N6 0.6088(3) 0.2897(2) 0.37678(13) 0.0374 1.0000 Uani
C25 0.6296(4) 0.3552(3) 0.37781(19) 0.0497 1.0000 Uani
C26 0.6605(7) 0.3727(4) 0.3438(3) 0.1156 1.0000 Uani
C27 0.7031(5) 0.3633(4) 0.4110(3) 0.0942 1.0000 Uani
C28 0.5652(6) 0.3962(4) 0.3878(4) 0.1270 1.0000 Uani
N7 0.7224(3) 0.19004(19) 0.35647(11) 0.0326 1.0000 Uani
C29 0.7462(3) 0.1652(2) 0.38911(14) 0.0310 1.0000 Uani
N8 0.6907(3) 0.16836(19) 0.41086(11) 0.0320 1.0000 Uani
C30 0.6779(3) 0.1184(3) 0.43646(14) 0.0391 1.0000 Uani
C31 0.6006(3) 0.0806(3) 0.42179(15) 0.0388 1.0000 Uani
N9 0.5933(3) 0.0972(2) 0.35481(12) 0.0394 1.0000 Uani
C32 0.5944(4) 0.0771(3) 0.32031(16) 0.0468 1.0000 Uani
C33 0.6075(5) 0.0159(3) 0.31149(19) 0.0692 1.0000 Uani
C34 0.6199(6) -0.0269(3) 0.3401(2) 0.0819 1.0000 Uani
C35 0.6173(5) -0.0072(3) 0.37605(19) 0.0624 1.0000 Uani
C36 0.6045(4) 0.0549(3) 0.38315(16) 0.0417 1.0000 Uani
N10 0.5220(3) 0.18276(19) 0.40335(12) 0.0363 1.0000 Uani
C37 0.5238(3) 0.1200(3) 0.42052(16) 0.0420 1.0000 Uani
C38 0.7727(3) 0.1963(3) 0.32741(14) 0.0382 1.0000 Uani
C39 0.7195(4) 0.2246(3) 0.29294(16) 0.0519 1.0000 Uani
C40 0.8042(4) 0.1331(3) 0.31715(18) 0.0558 1.0000 Uani
C41 0.8438(4) 0.2408(3) 0.34024(17) 0.0500 1.0000 Uani
O2 0.8185(2) 0.13689(16) 0.4003(1) 0.0370 1.0000 Uani
Si3 0.89148(9) 0.15522(7) 0.43696(4) 0.0396 1.0000 Uani
C42 0.8764(4) 0.2353(3) 0.4512(2) 0.0664 1.0000 Uani
C43 0.8897(4) 0.1010(3) 0.47609(17) 0.0608 1.0000 Uani
C44 0.9859(4) 0.1437(5) 0.4192(2) 0.0815 1.0000 Uani
C45 0.5955(4) 0.0276(3) 0.44987(17) 0.0496 1.0000 Uani
Si4 0.46386(9) 0.23628(7) 0.42330(4) 0.0388 1.0000 Uani
C46 0.4102(4) 0.2884(3) 0.38589(18) 0.0501 1.0000 Uani
C47 0.5296(4) 0.2781(3) 0.46270(19) 0.0580 1.0000 Uani
C48 0.3838(4) 0.1949(3) 0.44323(17) 0.0483 1.0000 Uani
Nb3 0.19623(3) -0.07847(2) 0.365735(12) 0.0273 1.0000 Uani
Cl3 0.07225(8) -0.13205(6) 0.37370(4) 0.0403 1.0000 Uani
N11 0.2073(3) -0.0327(2) 0.40699(12) 0.0358 1.0000 Uani
C49 0.2023(4) 0.0116(3) 0.43623(16) 0.0546 1.0000 Uani
C50 0.1203(7) 0.0000(4) 0.4491(3) 0.0995 1.0000 Uani
C51 0.1983(4) 0.0764(3) 0.42026(18) 0.0528 1.0000 Uani
C52 0.2703(9) 0.0028(5) 0.4676(3) 0.1689 1.0000 Uani
N12 0.1436(3) -0.0007(2) 0.32599(12) 0.0335 1.0000 Uani
C53 0.2123(3) 0.0063(2) 0.31516(14) 0.0361 1.0000 Uani
N13 0.2716(2) -0.0296(2) 0.33381(11) 0.0346 1.0000 Uani
C54 0.3320(3) -0.0585(3) 0.31604(16) 0.0470 1.0000 Uani
C55 0.3189(3) -0.1293(3) 0.31003(15) 0.0433 1.0000 Uani
N14 0.1729(2) -0.13012(18) 0.30462(11) 0.0283 1.0000 Uani
C56 0.0976(3) -0.1407(2) 0.28569(14) 0.0339 1.0000 Uani
C57 0.0801(3) -0.1640(3) 0.25015(15) 0.0412 1.0000 Uani
C58 0.1438(4) -0.1765(3) 0.23223(15) 0.0428 1.0000 Uani
C59 0.2222(3) -0.1651(2) 0.25106(15) 0.0383 1.0000 Uani
C60 0.2356(3) -0.1424(2) 0.28726(14) 0.0320 1.0000 Uani
N15 0.2845(3) -0.1425(2) 0.37602(12) 0.0365 1.0000 Uani
C61 0.3301(3) -0.1648(3) 0.34778(15) 0.0458 1.0000 Uani
C62 0.0688(4) 0.0346(3) 0.31182(16) 0.0426 1.0000 Uani
C63 0.0059(4) 0.0136(3) 0.33416(19) 0.0573 1.0000 Uani
C64 0.0815(5) 0.1051(3) 0.31697(19) 0.0629 1.0000 Uani
C65 0.0392(4) 0.0207(3) 0.27012(17) 0.0567 1.0000 Uani
O3 0.2245(2) 0.04589(18) 0.2875(1) 0.0452 1.0000 Uani
Si5 0.29463(15) 0.1032(1) 0.29248(5) 0.0683 1.0000 Uani
C66 0.2451(7) 0.1667(4) 0.2619(2) 0.1081 1.0000 Uani
C67 0.3180(5) 0.1273(4) 0.3422(2) 0.0809 1.0000 Uani
C68 0.3871(6) 0.0767(5) 0.2768(2) 0.1014 1.0000 Uani
C69 0.3867(4) -0.1519(4) 0.28996(18) 0.0655 1.0000 Uani
Si6 0.3267(1) -0.17087(8) 0.42083(4) 0.0435 1.0000 Uani
C70 0.2488(4) -0.1745(3) 0.45141(17) 0.0558 1.0000 Uani
C71 0.4159(4) -0.1229(4) 0.44236(19) 0.0666 1.0000 Uani
C72 0.3632(5) -0.2524(3) 0.41659(18) 0.0697 1.0000 Uani
Nb4 0.40049(3) -0.02316(2) 0.127419(12) 0.0282 1.0000 Uani
Cl4 0.47817(8) -0.03074(6) 0.19146(4) 0.0426 1.0000 Uani
N16 0.3871(3) -0.1048(2) 0.12241(11) 0.0352 1.0000 Uani
C73 0.3677(3) -0.1706(2) 0.12600(17) 0.0412 1.0000 Uani
C74 0.3265(7) -0.1795(4) 0.1600(3) 0.1000 1.0000 Uani
C75 0.3016(6) -0.1882(5) 0.0932(3) 0.1182 1.0000 Uani
C76 0.4373(6) -0.2086(4) 0.1282(6) 0.1973 1.0000 Uani
N17 0.2740(2) 0.00015(19) 0.13781(11) 0.0302 1.0000 Uani
C77 0.2541(3) 0.0234(2) 0.10416(14) 0.0316 1.0000 Uani
N18 0.3113(2) 0.01628(18) 0.08376(11) 0.0297 1.0000 Uani
C78 0.3279(3) 0.0642(2) 0.05816(15) 0.0388 1.0000 Uani
C79 0.4060(3) 0.1017(2) 0.07312(15) 0.0371 1.0000 Uani
N19 0.4101(3) 0.08858(19) 0.14014(12) 0.0338 1.0000 Uani
C80 0.4094(3) 0.1106(3) 0.17471(15) 0.0384 1.0000 Uani
C81 0.4007(4) 0.1727(3) 0.18237(18) 0.0509 1.0000 Uani
C82 0.3928(5) 0.2139(3) 0.1534(2) 0.0682 1.0000 Uani
C83 0.3949(4) 0.1925(3) 0.11765(19) 0.0542 1.0000 Uani
C84 0.4030(3) 0.1286(3) 0.11148(16) 0.0397 1.0000 Uani
N20 0.4787(2) -0.00220(19) 0.09386(12) 0.0320 1.0000 Uani
C85 0.4809(3) 0.0589(3) 0.07524(17) 0.0431 1.0000 Uani
C86 0.2200(3) -0.0022(3) 0.16558(14) 0.0368 1.0000 Uani
C87 0.2681(4) -0.0309(3) 0.20086(16) 0.0503 1.0000 Uani
C88 0.1932(4) 0.0636(3) 0.17426(18) 0.0554 1.0000 Uani
C89 0.1454(3) -0.0434(3) 0.15200(16) 0.0476 1.0000 Uani
O4 0.1833(2) 0.05248(16) 0.09098(9) 0.0347 1.0000 Uani
Si7 0.11520(9) 0.03193(8) 0.05293(4) 0.0397 1.0000 Uani
C90 0.1213(4) -0.0534(3) 0.04628(17) 0.0530 1.0000 Uani
C91 0.1312(4) 0.0736(3) 0.01064(18) 0.0631 1.0000 Uani
C92 0.0177(4) 0.0566(4) 0.0649(2) 0.0644 1.0000 Uani
C93 0.4134(4) 0.1522(3) 0.04405(18) 0.0505 1.0000 Uani
Si8 0.53536(9) -0.05961(7) 0.07636(4) 0.0359 1.0000 Uani
C94 0.5910(3) -0.1065(3) 0.11618(17) 0.0440 1.0000 Uani
C95 0.4688(4) -0.1074(3) 0.04035(17) 0.0535 1.0000 Uani
C96 0.6141(3) -0.0239(3) 0.05247(17) 0.0476 1.0000 Uani
H21 0.8713 0.1802 0.0135 0.0969 1.0000 Uiso
H22 0.9166 0.2033 0.0548 0.0969 1.0000 Uiso
H23 0.8596 0.2515 0.0269 0.0969 1.0000 Uiso
H31 0.8084 0.0925 0.0441 0.0779 1.0000 Uiso
H32 0.8556 0.1176 0.0846 0.0779 1.0000 Uiso
H33 0.7577 0.1079 0.0771 0.0779 1.0000 Uiso
H41 0.7203 0.1639 0.0010 0.1079 1.0000 Uiso
H42 0.7084 0.2356 0.0136 0.1079 1.0000 Uiso
H43 0.6689 0.1787 0.0338 0.1079 1.0000 Uiso
H61 0.6732 0.2202 0.2031 0.0425 1.0000 Uiso
H62 0.6139 0.2338 0.1631 0.0425 1.0000 Uiso
H81 0.9467 0.3161 0.1949 0.0402 1.0000 Uiso
H91 0.9760 0.3586 0.2558 0.0468 1.0000 Uiso
H101 0.8667 0.3828 0.2871 0.0489 1.0000 Uiso
H111 0.7319 0.3617 0.2562 0.0481 1.0000 Uiso
H131 0.6804 0.3937 0.1545 0.0503 1.0000 Uiso
H132 0.6060 0.3470 0.1376 0.0503 1.0000 Uiso
H151 1.0438 0.1540 0.1584 0.0601 1.0000 Uiso
H152 1.0009 0.2223 0.1563 0.0601 1.0000 Uiso
H153 0.9686 0.1701 0.1245 0.0601 1.0000 Uiso
H161 0.9725 0.0608 0.1763 0.0580 1.0000 Uiso
H162 0.9000 0.0755 0.1409 0.0580 1.0000 Uiso
H163 0.8794 0.0671 0.1827 0.0580 1.0000 Uiso
H171 1.0185 0.1407 0.2238 0.0576 1.0000 Uiso
H172 0.9792 0.2103 0.2202 0.0576 1.0000 Uiso
H173 0.9274 0.1517 0.2320 0.0576 1.0000 Uiso
H181 0.6497 0.0223 0.1470 0.0853 1.0000 Uiso
H182 0.7398 0.0435 0.1414 0.0853 1.0000 Uiso
H183 0.6655 0.0935 0.1346 0.0853 1.0000 Uiso
H191 0.7312 -0.0186 0.2292 0.0807 1.0000 Uiso
H192 0.7817 0.0341 0.2562 0.0807 1.0000 Uiso
H193 0.8177 0.0066 0.2209 0.0807 1.0000 Uiso
H201 0.5839 0.0668 0.2142 0.0770 1.0000 Uiso
H202 0.6369 0.1147 0.2439 0.0770 1.0000 Uiso
H203 0.5961 0.1388 0.2021 0.0770 1.0000 Uiso
H211 0.6167 0.3776 0.2126 0.0571 1.0000 Uiso
H212 0.6205 0.3084 0.2314 0.0571 1.0000 Uiso
H213 0.5586 0.3221 0.1921 0.0571 1.0000 Uiso
H221 0.7025 0.3793 0.0172 0.0780 1.0000 Uiso
H222 0.7748 0.3952 0.0525 0.0780 1.0000 Uiso
H223 0.7577 0.3233 0.0389 0.0780 1.0000 Uiso
H231 0.5461 0.3166 0.0313 0.0785 1.0000 Uiso
H232 0.5964 0.2590 0.0539 0.0785 1.0000 Uiso
H233 0.5354 0.3006 0.0739 0.0785 1.0000 Uiso
H241 0.5864 0.4491 0.0546 0.0844 1.0000 Uiso
H242 0.6586 0.4641 0.0901 0.0844 1.0000 Uiso
H243 0.5750 0.4315 0.0969 0.0844 1.0000 Uiso
H261 0.6746 0.4179 0.3449 0.1408 1.0000 Uiso
H262 0.7098 0.3476 0.3424 0.1408 1.0000 Uiso
H263 0.6181 0.3643 0.3213 0.1408 1.0000 Uiso
H271 0.7200 0.4079 0.4129 0.1110 1.0000 Uiso
H272 0.6870 0.3499 0.4348 0.1110 1.0000 Uiso
H273 0.7492 0.3371 0.4063 0.1110 1.0000 Uiso
H281 0.5831 0.4406 0.3880 0.1577 1.0000 Uiso
H282 0.5550 0.3846 0.4131 0.1577 1.0000 Uiso
H283 0.5143 0.3909 0.3689 0.1577 1.0000 Uiso
H301 0.6732 0.1372 0.4611 0.0480 1.0000 Uiso
H302 0.7254 0.0898 0.4398 0.0480 1.0000 Uiso
H321 0.5851 0.1081 0.2995 0.0565 1.0000 Uiso
H331 0.6080 0.0031 0.2851 0.0850 1.0000 Uiso
H341 0.6306 -0.0715 0.3350 0.1016 1.0000 Uiso
H351 0.6248 -0.0380 0.3970 0.0752 1.0000 Uiso
H371 0.5159 0.1256 0.4469 0.0514 1.0000 Uiso
H372 0.4775 0.0959 0.4062 0.0514 1.0000 Uiso
H391 0.7517 0.2296 0.2727 0.0618 1.0000 Uiso
H392 0.6995 0.2662 0.2995 0.0618 1.0000 Uiso
H393 0.6724 0.1966 0.2841 0.0618 1.0000 Uiso
H401 0.8379 0.1389 0.2975 0.0698 1.0000 Uiso
H402 0.8378 0.1139 0.3399 0.0698 1.0000 Uiso
H403 0.7575 0.1053 0.3074 0.0698 1.0000 Uiso
H411 0.8769 0.2443 0.3202 0.0594 1.0000 Uiso
H412 0.8782 0.2244 0.3636 0.0594 1.0000 Uiso
H413 0.8226 0.2828 0.3453 0.0594 1.0000 Uiso
H421 0.9195 0.2465 0.4730 0.0759 1.0000 Uiso
H422 0.8222 0.2390 0.4585 0.0759 1.0000 Uiso
H423 0.8792 0.2641 0.4299 0.0759 1.0000 Uiso
H431 0.9333 0.1125 0.4976 0.0707 1.0000 Uiso
H432 0.8989 0.0576 0.4679 0.0707 1.0000 Uiso
H433 0.8360 0.1034 0.4840 0.0707 1.0000 Uiso
H441 1.0330 0.1537 0.4394 0.0985 1.0000 Uiso
H442 0.9895 0.0995 0.4113 0.0985 1.0000 Uiso
H443 0.9863 0.1718 0.3974 0.0985 1.0000 Uiso
H451 0.5458 0.0023 0.4410 0.0605 1.0000 Uiso
H452 0.5931 0.0457 0.4749 0.0605 1.0000 Uiso
H453 0.6444 0.0004 0.4519 0.0605 1.0000 Uiso
H461 0.3769 0.3191 0.3970 0.0597 1.0000 Uiso
H462 0.4507 0.3110 0.3740 0.0597 1.0000 Uiso
H463 0.3743 0.2630 0.3666 0.0597 1.0000 Uiso
H471 0.4963 0.3085 0.4740 0.0691 1.0000 Uiso
H472 0.5543 0.2473 0.4821 0.0691 1.0000 Uiso
H473 0.5734 0.3006 0.4530 0.0691 1.0000 Uiso
H481 0.3511 0.2259 0.4545 0.0579 1.0000 Uiso
H482 0.4097 0.1651 0.4629 0.0579 1.0000 Uiso
H483 0.3477 0.1716 0.4229 0.0579 1.0000 Uiso
H501 0.1147 0.0300 0.4695 0.1291 1.0000 Uiso
H502 0.1190 -0.0435 0.4587 0.1291 1.0000 Uiso
H503 0.0748 0.0062 0.4275 0.1291 1.0000 Uiso
H511 0.1948 0.1072 0.4405 0.0648 1.0000 Uiso
H512 0.2479 0.0847 0.4097 0.0648 1.0000 Uiso
H513 0.1494 0.0803 0.4000 0.0648 1.0000 Uiso
H521 0.2663 0.0337 0.4877 0.1839 1.0000 Uiso
H522 0.2684 -0.0403 0.4777 0.1839 1.0000 Uiso
H523 0.3224 0.0089 0.4586 0.1839 1.0000 Uiso
H541 0.3863 -0.0516 0.3321 0.0565 1.0000 Uiso
H542 0.3304 -0.0384 0.2912 0.0565 1.0000 Uiso
H561 0.0515 -0.1308 0.2984 0.0413 1.0000 Uiso
H571 0.0229 -0.1718 0.2375 0.0482 1.0000 Uiso
H581 0.1337 -0.1934 0.2062 0.0514 1.0000 Uiso
H591 0.2690 -0.1733 0.2384 0.0474 1.0000 Uiso
H611 0.3888 -0.1631 0.3593 0.0546 1.0000 Uiso
H612 0.3139 -0.2090 0.3420 0.0546 1.0000 Uiso
H631 -0.0458 0.0365 0.3254 0.0685 1.0000 Uiso
H632 0.0258 0.0225 0.3613 0.0685 1.0000 Uiso
H633 -0.0037 -0.0321 0.3305 0.0685 1.0000 Uiso
H641 0.0297 0.1273 0.3071 0.0733 1.0000 Uiso
H642 0.0989 0.1148 0.3442 0.0733 1.0000 Uiso
H643 0.1241 0.1192 0.3030 0.0733 1.0000 Uiso
H651 -0.0113 0.0448 0.2608 0.0642 1.0000 Uiso
H652 0.0278 -0.0248 0.2667 0.0642 1.0000 Uiso
H653 0.0818 0.0331 0.2557 0.0642 1.0000 Uiso
H66 0.2828 0.2029 0.2632 0.1293 1.0000 Uiso
H67 0.1947 0.1800 0.2705 0.1293 1.0000 Uiso
H68 0.2311 0.1515 0.2355 0.1293 1.0000 Uiso
H671 0.3594 0.1612 0.3454 0.0970 1.0000 Uiso
H672 0.3395 0.0909 0.3580 0.0970 1.0000 Uiso
H673 0.2676 0.1428 0.3500 0.0970 1.0000 Uiso
H681 0.4276 0.1112 0.2800 0.1262 1.0000 Uiso
H682 0.4102 0.0402 0.2922 0.1262 1.0000 Uiso
H683 0.3736 0.0645 0.2499 0.1262 1.0000 Uiso
H691 0.3811 -0.1976 0.2854 0.0796 1.0000 Uiso
H692 0.4405 -0.1430 0.3060 0.0796 1.0000 Uiso
H693 0.3825 -0.1296 0.2656 0.0796 1.0000 Uiso
H701 0.2742 -0.1907 0.4766 0.0671 1.0000 Uiso
H702 0.2267 -0.1319 0.4540 0.0671 1.0000 Uiso
H703 0.2040 -0.2028 0.4399 0.0671 1.0000 Uiso
H711 0.4391 -0.1397 0.4677 0.0782 1.0000 Uiso
H712 0.3986 -0.0789 0.4447 0.0782 1.0000 Uiso
H713 0.4579 -0.1247 0.4262 0.0782 1.0000 Uiso
H721 0.3872 -0.2686 0.4420 0.0823 1.0000 Uiso
H722 0.3168 -0.2793 0.4051 0.0823 1.0000 Uiso
H723 0.4051 -0.2527 0.4004 0.0823 1.0000 Uiso
H741 0.3133 -0.2245 0.1624 0.1250 1.0000 Uiso
H742 0.3639 -0.1654 0.1832 0.1250 1.0000 Uiso
H743 0.2757 -0.1544 0.1565 0.1250 1.0000 Uiso
H751 0.2874 -0.2330 0.0952 0.1362 1.0000 Uiso
H752 0.3211 -0.1810 0.0693 0.1362 1.0000 Uiso
H753 0.2526 -0.1621 0.0937 0.1362 1.0000 Uiso
H761 0.4220 -0.2531 0.1307 0.2416 1.0000 Uiso
H762 0.4785 -0.1963 0.1505 0.2416 1.0000 Uiso
H763 0.4605 -0.2032 0.1051 0.2416 1.0000 Uiso
H781 0.3337 0.0441 0.0341 0.0471 1.0000 Uiso
H782 0.2812 0.0937 0.0536 0.0471 1.0000 Uiso
H801 0.4155 0.0803 0.1959 0.0459 1.0000 Uiso
H811 0.4002 0.1871 0.2084 0.0631 1.0000 Uiso
H821 0.3855 0.2592 0.1579 0.0840 1.0000 Uiso
H831 0.3906 0.2224 0.0964 0.0665 1.0000 Uiso
H851 0.5288 0.0821 0.0890 0.0537 1.0000 Uiso
H852 0.4883 0.0508 0.0490 0.0537 1.0000 Uiso
H871 0.2335 -0.0333 0.2204 0.0611 1.0000 Uiso
H872 0.3166 -0.0047 0.2103 0.0611 1.0000 Uiso
H873 0.2858 -0.0737 0.1952 0.0611 1.0000 Uiso
H881 0.1568 0.0611 0.1930 0.0696 1.0000 Uiso
H882 0.2417 0.0892 0.1846 0.0696 1.0000 Uiso
H883 0.1634 0.0832 0.1508 0.0696 1.0000 Uiso
H891 0.1104 -0.0440 0.1714 0.0581 1.0000 Uiso
H892 0.1632 -0.0867 0.1477 0.0581 1.0000 Uiso
H893 0.1140 -0.0263 0.1281 0.0581 1.0000 Uiso
H901 0.0811 -0.0662 0.0238 0.0613 1.0000 Uiso
H902 0.1769 -0.0647 0.0427 0.0613 1.0000 Uiso
H903 0.1091 -0.0753 0.0688 0.0613 1.0000 Uiso
H911 0.0896 0.0600 -0.0112 0.0724 1.0000 Uiso
H912 0.1863 0.0639 0.0057 0.0724 1.0000 Uiso
H913 0.1263 0.1193 0.0145 0.0724 1.0000 Uiso
H921 -0.0273 0.0462 0.0437 0.0758 1.0000 Uiso
H922 0.0187 0.1024 0.0694 0.0758 1.0000 Uiso
H923 0.0092 0.0343 0.0880 0.0758 1.0000 Uiso
H931 0.4632 0.1774 0.0528 0.0628 1.0000 Uiso
H932 0.4167 0.1322 0.0196 0.0628 1.0000 Uiso
H933 0.3649 0.1799 0.0408 0.0628 1.0000 Uiso
H941 0.6235 -0.1394 0.1064 0.0527 1.0000 Uiso
H942 0.6279 -0.0788 0.1336 0.0527 1.0000 Uiso
H943 0.5515 -0.1265 0.1298 0.0527 1.0000 Uiso
H951 0.5019 -0.1399 0.0306 0.0634 1.0000 Uiso
H952 0.4260 -0.1278 0.0518 0.0634 1.0000 Uiso
H953 0.4428 -0.0800 0.0193 0.0634 1.0000 Uiso
H961 0.6455 -0.0576 0.0428 0.0584 1.0000 Uiso
H962 0.6515 0.0022 0.0707 0.0584 1.0000 Uiso
H963 0.5871 0.0026 0.0312 0.0584 1.0000 Uiso
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 International_Tables_Vol_IV_Table_2.2B
'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997
0.0030 International_Tables_Vol_IV_Table_2.2B
'Cl ' 0.1320 0.1590 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 International_Tables_Vol_IV_Table_2.2B
'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 International_Tables_Vol_IV_Table_2.2B
'Nb ' -2.1970 0.6210 17.6142 1.1887 12.0144 11.7660 4.0418 0.2048 3.5335
69.7957 3.7559 International_Tables_Vol_IV_Table_2.2B
'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 International_Tables_Vol_IV_Table_2.2B
'Si ' 0.0720 0.0710 6.2915 2.4386 3.0353 32.3337 1.9891 0.6785 1.5410 81.6937
1.1407 International_Tables_Vol_IV_Table_2.2B
|
1100896.cif | #------------------------------------------------------------------------------
#$Date: 2022-09-14 17:31:13 +0300 (Wed, 14 Sep 2022) $
#$Revision: 277831 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100896.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_1100896
loop_
_publ_author_name
'Hahn, F. Ekkehardt'
'Holtgrewe, Christian'
'Pape, Tania'
'Martin, Marta'
'Sola, Eduardo'
'Oro, Luis A.'
_publ_section_title
;
Iridium Complexes with N-Allyl-Substituted Benzimidazol-2-ylidene
Ligands and Their Application in Catalytic Transfer Hydrogenation
;
_journal_coden_ASTM ORGND7
_journal_issue 9
_journal_name_full Organometallics
_journal_page_first 2203
_journal_page_last 2209
_journal_paper_doi 10.1021/om0500873
_journal_volume 24
_journal_year 2005
_chemical_formula_moiety 'C21 H26 Br Ir N2'
_chemical_formula_sum 'C21 H26 Br Ir N2'
_chemical_formula_weight 578.55
_space_group_IT_number 2
_space_group_name_Hall '-P 1'
_space_group_name_H-M_alt 'P -1'
_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 heavy
_atom_sites_solution_secondary difmap
_cell_angle_alpha 64.4420(10)
_cell_angle_beta 75.631(2)
_cell_angle_gamma 88.124(2)
_cell_formula_units_Z 2
_cell_length_a 8.6482(8)
_cell_length_b 10.7943(10)
_cell_length_c 11.8122(11)
_cell_measurement_reflns_used 6787
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 28.69
_cell_measurement_theta_min 2.44
_cell_volume 960.17(15)
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measurement_device_type 'Bruker SMART APEX CCD system'
_diffrn_measurement_method '\w rotations with narrow frames'
_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 0.0231
_diffrn_reflns_av_sigmaI/netI 0.0392
_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 15
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_number 12008
_diffrn_reflns_theta_max 28.75
_diffrn_reflns_theta_min 1.98
_diffrn_standards_decay_% 'no decay'
_exptl_absorpt_coefficient_mu 9.039
_exptl_absorpt_correction_T_max 0.369
_exptl_absorpt_correction_T_min 0.271
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS: Area-Detector Absorption Correction. (1996) Bruker-AXS
within SAINT+ package, v. 6.01.
;
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 2.001
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description 'irregular block'
_exptl_crystal_F_000 556
_exptl_crystal_size_max 0.20
_exptl_crystal_size_mid 0.18
_exptl_crystal_size_min 0.10
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.942
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 275
_refine_ls_number_reflns 4562
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.942
_refine_ls_R_factor_all 0.0227
_refine_ls_R_factor_gt 0.0198
_refine_ls_shift/su_max 0.016
_refine_ls_shift/su_mean 0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0131P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0375
_refine_ls_wR_factor_ref 0.0380
_reflns_number_gt 4148
_reflns_number_total 4562
_reflns_threshold_expression >2sigma(I)
_cod_duplicate_entry 4060534
_cod_original_sg_symbol_H-M P-1
_cod_database_code 1100896
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
Ir1 Ir 0.778325(14) 0.747120(12) 0.706524(12) 0.01255(4) Uani 1 1 d . . .
Br1 Br 1.04840(3) 0.74599(3) 0.54361(3) 0.01678(7) Uani 1 1 d . . .
N1 N 0.5336(3) 0.6041(3) 0.6668(2) 0.0151(6) Uani 1 1 d . . .
N2 N 0.7248(3) 0.4685(2) 0.6904(2) 0.0128(5) Uani 1 1 d . . .
C1 C 0.6832(3) 0.5930(3) 0.6853(3) 0.0145(6) Uani 1 1 d . . .
C2 C 0.5993(3) 0.3998(3) 0.6790(3) 0.0137(6) Uani 1 1 d . . .
C3 C 0.4762(4) 0.4873(3) 0.6644(3) 0.0145(6) Uani 1 1 d . . .
C4 C 0.3317(4) 0.4504(3) 0.6512(3) 0.0195(7) Uani 1 1 d . . .
H4 H 0.2486 0.5108 0.6394 0.023 Uiso 1 1 calc R . .
C5 C 0.3156(4) 0.3212(3) 0.6562(3) 0.0207(7) Uani 1 1 d . . .
H5 H 0.2181 0.2915 0.6487 0.025 Uiso 1 1 calc R . .
C6 C 0.4387(4) 0.2329(3) 0.6722(3) 0.0200(7) Uani 1 1 d . . .
H6 H 0.4226 0.1446 0.6754 0.024 Uiso 1 1 calc R . .
C7 C 0.5828(4) 0.2711(3) 0.6832(3) 0.0169(7) Uani 1 1 d . . .
H7 H 0.6668 0.2115 0.6933 0.020 Uiso 1 1 calc R . .
C8 C 0.4441(4) 0.7190(3) 0.6722(4) 0.0210(7) Uani 1 1 d . . .
H8A H 0.387(4) 0.752(3) 0.603(3) 0.025 Uiso 1 1 d . . .
H8B H 0.371(4) 0.686(3) 0.750(3) 0.025 Uiso 1 1 d . . .
C9 C 0.5613(4) 0.8292(3) 0.6577(3) 0.0192(7) Uani 1 1 d . . .
H9 H 0.519(4) 0.882(3) 0.691(3) 0.021(9) Uiso 1 1 d . . .
C10 C 0.6923(4) 0.8907(4) 0.5481(4) 0.0198(7) Uani 1 1 d . . .
H10A H 0.730(4) 0.977(3) 0.521(3) 0.024(10) Uiso 1 1 d . . .
H10B H 0.703(4) 0.867(3) 0.490(3) 0.015(9) Uiso 1 1 d . . .
C11 C 0.8750(4) 0.4051(3) 0.7111(3) 0.0160(7) Uani 1 1 d . . .
H11A H 0.948(4) 0.478(3) 0.695(3) 0.019 Uiso 1 1 d . . .
H11B H 0.913(4) 0.377(3) 0.646(3) 0.019 Uiso 1 1 d . . .
C12 C 0.8496(4) 0.2872(3) 0.8435(3) 0.0194(7) Uani 1 1 d . . .
H12 H 0.807(4) 0.306(3) 0.911(3) 0.023 Uiso 1 1 d . . .
C13 C 0.8942(5) 0.1635(4) 0.8649(4) 0.0282(9) Uani 1 1 d . . .
H13A H 0.875(4) 0.093(3) 0.956(3) 0.021(9) Uiso 1 1 d . . .
H13B H 0.943(4) 0.141(3) 0.801(3) 0.023(10) Uiso 1 1 d . . .
C14 C 0.6938(4) 0.6255(3) 0.9107(3) 0.0221(8) Uani 1 1 d . . .
H14 H 0.632(4) 0.550(3) 0.928(3) 0.026 Uiso 1 1 d . . .
C15 C 0.8602(4) 0.6166(3) 0.8732(3) 0.0196(7) Uani 1 1 d . . .
H15 H 0.890(3) 0.534(3) 0.874(3) 0.015(8) Uiso 1 1 d . . .
C16 C 0.9846(4) 0.6870(3) 0.9034(3) 0.0234(8) Uani 1 1 d . . .
H16A H 1.0762 0.6295 0.9158 0.028 Uiso 1 1 calc R . .
H16B H 0.9362 0.6930 0.9859 0.028 Uiso 1 1 calc R . .
C17 C 1.0466(4) 0.8321(3) 0.7960(3) 0.0199(7) Uani 1 1 d . . .
H17A H 1.0770 0.8888 0.8356 0.024 Uiso 1 1 calc R . .
H17B H 1.1443 0.8256 0.7347 0.024 Uiso 1 1 calc R . .
C18 C 0.9267(4) 0.9036(3) 0.7215(3) 0.0168(7) Uani 1 1 d . . .
H18 H 0.959(3) 0.966(3) 0.638(3) 0.014(9) Uiso 1 1 d . . .
C19 C 0.7692(4) 0.9099(3) 0.7769(3) 0.0183(7) Uani 1 1 d . . .
H19 H 0.716(4) 0.978(3) 0.726(3) 0.022 Uiso 1 1 d . . .
C20 C 0.6966(4) 0.8533(3) 0.9227(3) 0.0260(8) Uani 1 1 d . . .
H20A H 0.6178 0.9157 0.9400 0.031 Uiso 1 1 calc R . .
H20B H 0.7822 0.8515 0.9654 0.031 Uiso 1 1 calc R . .
C21 C 0.6141(4) 0.7089(4) 0.9816(3) 0.0320(9) Uani 1 1 d . . .
H21A H 0.6160 0.6603 1.0739 0.038 Uiso 1 1 calc R . .
H21B H 0.5007 0.7155 0.9785 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
Ir1 0.01262(6) 0.01184(6) 0.01346(6) -0.00602(5) -0.00299(5) 0.00158(4)
Br1 0.01614(16) 0.01536(16) 0.01666(17) -0.00694(13) -0.00067(13) 0.00110(12)
N1 0.0132(13) 0.0137(13) 0.0197(15) -0.0080(12) -0.0057(11) 0.0033(10)
N2 0.0127(13) 0.0112(13) 0.0154(14) -0.0067(11) -0.0036(11) 0.0024(10)
C1 0.0163(16) 0.0146(16) 0.0114(16) -0.0045(13) -0.0040(13) 0.0025(12)
C2 0.0134(15) 0.0161(16) 0.0099(15) -0.0044(13) -0.0023(12) -0.0010(12)
C3 0.0161(16) 0.0131(16) 0.0132(16) -0.0055(13) -0.0025(13) 0.0007(12)
C4 0.0152(16) 0.0215(18) 0.0216(18) -0.0090(15) -0.0050(14) 0.0015(13)
C5 0.0162(17) 0.0242(18) 0.0219(18) -0.0096(15) -0.0056(14) -0.0022(14)
C6 0.0246(18) 0.0162(17) 0.0225(18) -0.0105(15) -0.0075(15) -0.0009(14)
C7 0.0190(17) 0.0155(16) 0.0170(17) -0.0077(14) -0.0050(14) 0.0024(13)
C8 0.0150(17) 0.0175(18) 0.032(2) -0.0121(16) -0.0061(15) 0.0048(13)
C9 0.0171(17) 0.0147(17) 0.030(2) -0.0126(16) -0.0088(15) 0.0079(13)
C10 0.0232(19) 0.0128(18) 0.027(2) -0.0092(16) -0.0121(16) 0.0048(14)
C11 0.0124(16) 0.0157(17) 0.0223(18) -0.0106(15) -0.0044(14) 0.0040(13)
C12 0.0193(17) 0.0213(18) 0.0203(18) -0.0093(15) -0.0090(14) 0.0008(14)
C13 0.035(2) 0.020(2) 0.032(2) -0.0104(18) -0.0152(19) 0.0028(16)
C14 0.030(2) 0.0195(18) 0.0144(17) -0.0078(15) 0.0002(15) -0.0065(15)
C15 0.030(2) 0.0113(16) 0.0184(18) -0.0065(14) -0.0084(15) 0.0019(14)
C16 0.034(2) 0.0180(18) 0.0219(19) -0.0087(15) -0.0144(16) 0.0033(15)
C17 0.0240(18) 0.0165(17) 0.0219(18) -0.0096(15) -0.0081(15) 0.0006(14)
C18 0.0227(18) 0.0125(16) 0.0175(18) -0.0085(15) -0.0051(14) 0.0008(13)
C19 0.0205(18) 0.0154(17) 0.0239(19) -0.0139(15) -0.0046(14) 0.0020(13)
C20 0.0273(19) 0.029(2) 0.026(2) -0.0196(17) 0.0017(16) -0.0006(15)
C21 0.035(2) 0.033(2) 0.026(2) -0.0177(18) 0.0061(17) -0.0097(17)
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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100897.cif | #------------------------------------------------------------------------------
#$Date: 2022-09-14 17:31:13 +0300 (Wed, 14 Sep 2022) $
#$Revision: 277831 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100897.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_1100897
loop_
_publ_author_name
'Hahn, F. Ekkehardt'
'Holtgrewe, Christian'
'Pape, Tania'
'Martin, Marta'
'Sola, Eduardo'
'Oro, Luis A.'
_publ_section_title
;
Iridium Complexes with N-Allyl-Substituted Benzimidazol-2-ylidene
Ligands and Their Application in Catalytic Transfer Hydrogenation
;
_journal_coden_ASTM ORGND7
_journal_issue 9
_journal_name_full Organometallics
_journal_page_first 2203
_journal_page_last 2209
_journal_paper_doi 10.1021/om0500873
_journal_volume 24
_journal_year 2005
_chemical_formula_moiety 'C21 H26 Ir N2, B F4, 2(C H Cl3)'
_chemical_formula_sum 'C23 H28 B Cl6 F4 Ir N2'
_chemical_formula_weight 824.18
_space_group_IT_number 15
_space_group_name_Hall '-C 2yc'
_space_group_name_H-M_alt 'C 1 2/c 1'
_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 heavy
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 97.5890(10)
_cell_angle_gamma 90.00
_cell_formula_units_Z 8
_cell_length_a 29.6219(12)
_cell_length_b 10.7321(4)
_cell_length_c 17.8342(7)
_cell_measurement_reflns_used 9443
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 28.49
_cell_measurement_theta_min 2.28
_cell_volume 5619.9(4)
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measurement_device_type 'Bruker SMART APEX CCD system'
_diffrn_measurement_method '\w rotations with narrow frames'
_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 0.0367
_diffrn_reflns_av_sigmaI/netI 0.0492
_diffrn_reflns_limit_h_max 38
_diffrn_reflns_limit_h_min -40
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 24
_diffrn_reflns_limit_l_min -24
_diffrn_reflns_number 32915
_diffrn_reflns_theta_max 28.87
_diffrn_reflns_theta_min 1.39
_diffrn_standards_decay_% 'no decay'
_exptl_absorpt_coefficient_mu 5.367
_exptl_absorpt_correction_T_max 0.597
_exptl_absorpt_correction_T_min 0.493
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS: Area-Detector Absorption Correction. (1996) Bruker-AXS
within SAINT+ package, v. 6.01.
;
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.948
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 3200
_exptl_crystal_size_max 0.14
_exptl_crystal_size_mid 0.14
_exptl_crystal_size_min 0.12
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.851
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 364
_refine_ls_number_reflns 6932
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.851
_refine_ls_R_factor_all 0.0312
_refine_ls_R_factor_gt 0.0231
_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^)+(0.0094P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0356
_refine_ls_wR_factor_ref 0.0367
_reflns_number_gt 5696
_reflns_number_total 6932
_reflns_threshold_expression >2sigma(I)
_cod_duplicate_entry 4060535
_cod_database_code 1100897
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
Ir1 Ir 0.135410(4) 0.359227(10) 0.871020(6) 0.01211(3) Uani 1 1 d . . .
Cl1 Cl 0.86272(3) 0.21106(8) 1.00794(5) 0.0357(2) Uani 1 1 d . . .
Cl2 Cl 0.95812(3) 0.15214(8) 1.01736(4) 0.03037(19) Uani 1 1 d . . .
Cl3 Cl 0.91489(3) 0.29879(8) 0.89236(5) 0.0356(2) Uani 1 1 d . . .
Cl4 Cl 0.91250(3) 0.85270(8) 0.70362(4) 0.0351(2) Uani 1 1 d . . .
Cl5 Cl 0.95922(3) 0.71001(8) 0.82809(5) 0.0328(2) Uani 1 1 d . . .
Cl6 Cl 0.96071(3) 0.97867(7) 0.83308(5) 0.0310(2) Uani 1 1 d . . .
F1 F 0.30309(6) 0.42149(16) 0.94218(9) 0.0295(4) Uani 1 1 d . . .
F2 F 0.27584(5) 0.43327(15) 0.81756(9) 0.0241(4) Uani 1 1 d . . .
F3 F 0.34913(5) 0.48946(14) 0.85843(9) 0.0222(4) Uani 1 1 d . . .
F4 F 0.32867(6) 0.28636(15) 0.85906(9) 0.0285(4) Uani 1 1 d . . .
N1 N 0.17093(8) 0.4603(2) 0.73860(12) 0.0132(5) Uani 1 1 d . . .
N2 N 0.18301(8) 0.2607(2) 0.75003(12) 0.0137(5) Uani 1 1 d . . .
C1 C 0.16285(8) 0.3585(3) 0.77795(14) 0.0116(5) Uani 1 1 d . . .
C2 C 0.20610(9) 0.3007(3) 0.69084(15) 0.0141(6) Uani 1 1 d . . .
C3 C 0.19793(9) 0.4285(3) 0.68276(15) 0.0139(6) Uani 1 1 d . . .
C4 C 0.21666(9) 0.4985(3) 0.62928(15) 0.0173(7) Uani 1 1 d . . .
H4 H 0.2105 0.5849 0.6229 0.021 Uiso 1 1 calc R . .
C5 C 0.24477(9) 0.4364(3) 0.58568(15) 0.0197(7) Uani 1 1 d . . .
H5 H 0.2586 0.4814 0.5489 0.024 Uiso 1 1 calc R . .
C6 C 0.25333(9) 0.3090(3) 0.59458(16) 0.0191(7) Uani 1 1 d . . .
H6 H 0.2731 0.2698 0.5640 0.023 Uiso 1 1 calc R . .
C7 C 0.23380(9) 0.2380(3) 0.64684(15) 0.0178(7) Uani 1 1 d . . .
H7 H 0.2392 0.1510 0.6521 0.021 Uiso 1 1 calc R . .
C8 C 0.15446(10) 0.5785(3) 0.76627(15) 0.0170(6) Uani 1 1 d . . .
H8A H 0.1259 0.6040 0.7349 0.020 Uiso 1 1 calc R . .
H8B H 0.1774 0.6449 0.7638 0.020 Uiso 1 1 calc R . .
C9 C 0.14610(10) 0.5580(3) 0.84798(16) 0.0157(6) Uani 1 1 d . . .
H9 H 0.1225(9) 0.603(2) 0.8636(14) 0.019 Uiso 1 1 d . . .
C10 C 0.18110(10) 0.5179(3) 0.90295(17) 0.0164(6) Uani 1 1 d . . .
H10A H 0.2108(9) 0.503(2) 0.8894(14) 0.020 Uiso 1 1 d . . .
H10B H 0.1806(9) 0.535(2) 0.9526(15) 0.020 Uiso 1 1 d . . .
C11 C 0.17958(9) 0.1416(3) 0.78899(14) 0.0167(6) Uani 1 1 d . . .
H11A H 0.2079 0.0929 0.7887 0.020 Uiso 1 1 calc R . .
H11B H 0.1538 0.0922 0.7634 0.020 Uiso 1 1 calc R . .
C12 C 0.17202(10) 0.1709(3) 0.86984(16) 0.0156(7) Uani 1 1 d . . .
H12 H 0.1570(9) 0.116(2) 0.8890(15) 0.019 Uiso 1 1 d . . .
C13 C 0.20001(10) 0.2524(3) 0.91499(17) 0.0182(7) Uani 1 1 d . . .
H13A H 0.2253(9) 0.292(2) 0.8943(15) 0.022 Uiso 1 1 d . . .
H13B H 0.2005(9) 0.250(2) 0.9649(15) 0.022 Uiso 1 1 d . . .
C14 C 0.06668(9) 0.3716(3) 0.80985(16) 0.0177(6) Uani 1 1 d . . .
H14 H 0.0682(9) 0.388(2) 0.7621(15) 0.021 Uiso 1 1 d . . .
C15 C 0.07480(10) 0.2466(3) 0.82906(17) 0.0181(7) Uani 1 1 d . . .
H15 H 0.0829(9) 0.200(3) 0.7913(15) 0.022 Uiso 1 1 d . . .
C16 C 0.05401(10) 0.1793(3) 0.89104(16) 0.0224(7) Uani 1 1 d . . .
H16A H 0.0504 0.0902 0.8773 0.027 Uiso 1 1 calc R . .
H16B H 0.0233 0.2139 0.8937 0.027 Uiso 1 1 calc R . .
C17 C 0.08218(10) 0.1892(3) 0.96981(16) 0.0226(7) Uani 1 1 d . . .
H17A H 0.0612 0.1858 1.0086 0.027 Uiso 1 1 calc R . .
H17B H 0.1026 0.1161 0.9776 0.027 Uiso 1 1 calc R . .
C18 C 0.11048(10) 0.3058(3) 0.98181(16) 0.0184(7) Uani 1 1 d . . .
H18 H 0.1368(9) 0.301(2) 1.0157(15) 0.022 Uiso 1 1 d . . .
C19 C 0.09462(10) 0.4233(3) 0.96335(16) 0.0184(7) Uani 1 1 d . . .
H19 H 0.1101(9) 0.488(3) 0.9865(15) 0.022 Uiso 1 1 d . . .
C20 C 0.04530(10) 0.4525(3) 0.93392(16) 0.0216(7) Uani 1 1 d . . .
H20A H 0.0370 0.5334 0.9550 0.026 Uiso 1 1 calc R . .
H20B H 0.0256 0.3876 0.9520 0.026 Uiso 1 1 calc R . .
C21 C 0.03618(10) 0.4585(3) 0.84740(16) 0.0227(7) Uani 1 1 d . . .
H21A H 0.0040 0.4365 0.8307 0.027 Uiso 1 1 calc R . .
H21B H 0.0410 0.5450 0.8308 0.027 Uiso 1 1 calc R . .
C22 C 0.90749(10) 0.1773(3) 0.95595(16) 0.0200(7) Uani 1 1 d . . .
H22 H 0.8998 0.0994 0.9263 0.024 Uiso 1 1 calc R . .
C23 C 0.92816(10) 0.8464(3) 0.80211(16) 0.0214(7) Uani 1 1 d . . .
H23 H 0.8999 0.8461 0.8271 0.026 Uiso 1 1 calc R . .
B1 B 0.31370(11) 0.4077(3) 0.86952(19) 0.0175(7) 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
Ir1 0.01149(5) 0.01255(5) 0.01249(5) -0.00016(5) 0.00235(4) 0.00015(5)
Cl1 0.0225(4) 0.0518(6) 0.0346(5) -0.0157(4) 0.0104(4) 0.0016(4)
Cl2 0.0206(4) 0.0410(5) 0.0285(4) 0.0063(4) -0.0003(3) 0.0003(4)
Cl3 0.0380(5) 0.0375(5) 0.0301(5) 0.0104(4) -0.0004(4) 0.0003(4)
Cl4 0.0488(5) 0.0297(5) 0.0252(4) -0.0015(4) -0.0007(4) -0.0107(4)
Cl5 0.0255(5) 0.0269(5) 0.0439(5) -0.0057(4) -0.0034(4) 0.0057(4)
Cl6 0.0263(5) 0.0275(5) 0.0396(5) -0.0147(4) 0.0060(4) -0.0071(4)
F1 0.0368(11) 0.0351(11) 0.0188(9) 0.0008(8) 0.0116(8) -0.0026(9)
F2 0.0159(9) 0.0278(10) 0.0274(10) 0.0033(8) -0.0014(8) -0.0001(8)
F3 0.0195(10) 0.0236(10) 0.0237(10) -0.0004(8) 0.0039(7) -0.0074(8)
F4 0.0336(11) 0.0158(9) 0.0350(11) -0.0008(8) 0.0005(9) 0.0043(8)
N1 0.0163(13) 0.0130(13) 0.0106(12) 0.0007(10) 0.0023(10) 0.0019(10)
N2 0.0150(13) 0.0120(12) 0.0146(13) -0.0003(10) 0.0031(10) 0.0002(10)
C1 0.0088(13) 0.0120(14) 0.0136(14) -0.0005(12) -0.0002(11) 0.0008(12)
C2 0.0114(15) 0.0178(15) 0.0128(15) -0.0011(12) -0.0001(12) -0.0022(12)
C3 0.0118(15) 0.0188(16) 0.0111(14) -0.0013(12) 0.0014(11) 0.0006(13)
C4 0.0175(16) 0.0192(16) 0.0145(15) 0.0022(12) -0.0006(12) -0.0018(13)
C5 0.0166(16) 0.0293(18) 0.0130(15) -0.0003(13) 0.0016(12) -0.0066(14)
C6 0.0127(15) 0.0255(17) 0.0199(17) -0.0059(13) 0.0056(13) -0.0018(13)
C7 0.0159(16) 0.0168(16) 0.0202(16) -0.0041(13) 0.0008(13) 0.0007(13)
C8 0.0209(16) 0.0122(15) 0.0183(16) 0.0006(12) 0.0047(13) 0.0027(13)
C9 0.0185(16) 0.0110(15) 0.0190(16) -0.0019(12) 0.0070(13) -0.0013(12)
C10 0.0181(16) 0.0156(16) 0.0153(16) -0.0018(13) 0.0016(13) -0.0035(13)
C11 0.0193(15) 0.0115(14) 0.0200(15) 0.0023(13) 0.0053(12) -0.0012(13)
C12 0.0152(16) 0.0119(16) 0.0203(16) 0.0060(12) 0.0048(13) 0.0020(12)
C13 0.0177(17) 0.0195(17) 0.0179(17) 0.0030(14) 0.0041(14) 0.0041(13)
C14 0.0126(14) 0.0265(18) 0.0138(15) 0.0010(14) 0.0008(12) 0.0017(14)
C15 0.0122(16) 0.0225(17) 0.0195(17) -0.0056(13) 0.0010(13) -0.0033(13)
C16 0.0182(17) 0.0196(17) 0.0304(18) -0.0037(13) 0.0067(14) -0.0052(13)
C17 0.0225(18) 0.0212(17) 0.0254(18) 0.0037(14) 0.0082(14) -0.0004(14)
C18 0.0175(17) 0.0262(17) 0.0124(16) 0.0013(13) 0.0049(13) -0.0014(14)
C19 0.0190(17) 0.0245(18) 0.0128(15) -0.0041(13) 0.0063(13) -0.0038(14)
C20 0.0185(17) 0.0219(17) 0.0254(17) -0.0035(14) 0.0072(14) 0.0020(13)
C21 0.0152(16) 0.0267(18) 0.0268(18) 0.0008(14) 0.0052(14) 0.0054(14)
C22 0.0209(17) 0.0218(17) 0.0171(16) -0.0034(13) 0.0019(13) -0.0022(13)
C23 0.0184(16) 0.0182(16) 0.0281(17) -0.0064(14) 0.0045(13) -0.0030(14)
B1 0.0161(18) 0.0189(18) 0.0176(18) 0.0004(15) 0.0030(14) -0.0015(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'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100898.cif | #------------------------------------------------------------------------------
#$Date: 2018-09-01 22:43:12 +0300 (Sat, 01 Sep 2018) $
#$Revision: 210322 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100898.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_1100898
loop_
_publ_author_name
'Hahn, F. Ekkehardt'
'Holtgrewe, Christian'
'Pape, Tania'
'Martin, Marta'
'Sola, Eduardo'
'Oro, Luis A.'
_publ_section_title
;
Iridium Complexes with N-Allyl-Substituted Benzimidazol-2-ylidene
Ligands and Their Application in Catalytic Transfer Hydrogenation
;
_journal_coden_ASTM ORGND7
_journal_issue 9
_journal_name_full Organometallics
_journal_page_first 2203
_journal_page_last 2209
_journal_paper_doi 10.1021/om0500873
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C28 H34 Br Ir N2'
_chemical_formula_weight 670.68
_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
_cell_angle_alpha 90.00
_cell_angle_beta 98.403(2)
_cell_angle_gamma 90.00
_cell_formula_units_Z 8
_cell_length_a 34.958(3)
_cell_length_b 7.5715(6)
_cell_length_c 17.7650(14)
_cell_measurement_reflns_used 900
_cell_measurement_temperature 173(2)
_cell_measurement_theta_max 22.5
_cell_measurement_theta_min 1
_cell_volume 4651.6(6)
_diffrn_ambient_temperature 173(2)
_diffrn_detector_area_resol_mean 80
_diffrn_measurement_device_type 'CCD area detector'
_diffrn_measurement_method 'Omega and Phi scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'rotating anode'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0524
_diffrn_reflns_av_sigmaI/netI 0.0532
_diffrn_reflns_limit_h_max 48
_diffrn_reflns_limit_h_min -48
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_l_max 24
_diffrn_reflns_limit_l_min -24
_diffrn_reflns_number 25955
_diffrn_reflns_theta_max 30.02
_diffrn_reflns_theta_min 1.18
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 7.478
_exptl_absorpt_correction_T_max 0.8648
_exptl_absorpt_correction_T_min 0.2900
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
Corrections were done with the SADABS program, utilizing the none merged
raw data obtained from the integration process. Integration and final cell
refinement were done with SAINT.
SADABS reports ratio of Tmin/Tmax = 0.641757
;
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.915
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description 'transparent needles'
_exptl_crystal_F_000 2624
_exptl_crystal_size_max 0.22
_exptl_crystal_size_mid 0.03
_exptl_crystal_size_min 0.02
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.016
_refine_ls_hydrogen_treatment noref
_refine_ls_matrix_type full
_refine_ls_number_parameters 272
_refine_ls_number_reflns 6760
_refine_ls_number_restraints 5
_refine_ls_restrained_S_all 1.022
_refine_ls_R_factor_all 0.0453
_refine_ls_R_factor_gt 0.0339
_refine_ls_shift/su_max 2.673
_refine_ls_shift/su_mean 0.187
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0271P)^2^+6.8059P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0729
_refine_ls_wR_factor_ref 0.0771
_reflns_number_gt 5587
_reflns_number_total 6760
_reflns_threshold_expression >2sigma(I)
_cod_duplicate_entry 4060536
_cod_original_sg_symbol_H-M C2/c
_cod_database_code 1100898
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
Br Br 0.112809(14) 1.09013(6) 0.18215(3) 0.03533(11) Uani 1 1 d . . .
C1 C 0.16400(11) 0.8034(5) 0.1095(2) 0.0195(7) Uani 1 1 d . . .
C2 C 0.21609(11) 0.6567(5) 0.1704(2) 0.0202(7) Uani 1 1 d . . .
C3 C 0.22934(11) 0.7777(5) 0.1208(2) 0.0186(7) Uani 1 1 d . . .
C4 C 0.26822(11) 0.7911(5) 0.1137(2) 0.0233(8) Uani 1 1 d . . .
H4 H 0.2771 0.8723 0.0793 0.028 Uiso 1 1 calc R . .
C5 C 0.29367(12) 0.6798(6) 0.1593(2) 0.0262(8) Uani 1 1 d . . .
H5 H 0.3206 0.6860 0.1566 0.031 Uiso 1 1 calc R . .
C6 C 0.28012(12) 0.5590(6) 0.2092(2) 0.0292(9) Uani 1 1 d . . .
H6 H 0.2982 0.4856 0.2398 0.035 Uiso 1 1 calc R . .
C7 C 0.24136(12) 0.5434(5) 0.2153(2) 0.0248(8) Uani 1 1 d . . .
H7 H 0.2323 0.4596 0.2484 0.030 Uiso 1 1 calc R . .
C8 C 0.19684(12) 1.0157(5) 0.0336(2) 0.0216(8) Uani 1 1 d . . .
H8A H 0.1715 1.0226 0.0006 0.026 Uiso 1 1 calc R . .
H8B H 0.2168 0.9962 0.0003 0.026 Uiso 1 1 calc R . .
C9 C 0.20471(13) 1.1897(5) 0.0745(2) 0.0262(8) Uani 1 1 d . . .
H9A H 0.2313 1.1899 0.1026 0.031 Uiso 1 1 calc R . .
H9B H 0.1865 1.2053 0.1118 0.031 Uiso 1 1 calc R . .
C10 C 0.20001(15) 1.3413(5) 0.0179(3) 0.0353(11) Uani 1 1 d . . .
H10A H 0.2174 1.3235 -0.0200 0.053 Uiso 1 1 calc R . .
H10B H 0.2064 1.4529 0.0447 0.053 Uiso 1 1 calc R . .
H10C H 0.1732 1.3453 -0.0077 0.053 Uiso 1 1 calc R . .
C11 C 0.15057(12) 0.5779(5) 0.2047(2) 0.0242(8) Uani 1 1 d . . .
H11A H 0.1580 0.4517 0.2067 0.029 Uiso 1 1 calc R . .
H11B H 0.1237 0.5866 0.1782 0.029 Uiso 1 1 calc R . .
C12 C 0.15224(13) 0.6477(6) 0.2855(2) 0.0307(9) Uani 1 1 d . . .
H12A H 0.1456 0.7748 0.2840 0.037 Uiso 1 1 calc R . .
H12B H 0.1788 0.6347 0.3130 0.037 Uiso 1 1 calc R . .
C13 C 0.12404(16) 0.5462(7) 0.3276(3) 0.0447(12) Uani 1 1 d . . .
H13A H 0.0976 0.5622 0.3012 0.067 Uiso 1 1 calc R . .
H13B H 0.1258 0.5911 0.3797 0.067 Uiso 1 1 calc R . .
H13C H 0.1306 0.4204 0.3289 0.067 Uiso 1 1 calc R . .
C14 C 0.11209(14) 0.7773(7) -0.0364(3) 0.0283(10) Uani 1 1 d . . .
H14 H 0.1389(14) 0.756(6) -0.047(2) 0.034 Uiso 1 1 calc . . .
C15 C 0.09857(14) 0.6472(7) 0.0107(3) 0.0283(10) Uani 1 1 d . . .
H15 H 0.1178(14) 0.552(6) 0.027(3) 0.034 Uiso 1 1 calc . . .
C16 C 0.05697(13) 0.5867(6) 0.0051(3) 0.0397(12) Uani 1 1 d . . .
H16A H 0.0544 0.5087 0.0488 0.048 Uiso 1 1 calc R . .
H16B H 0.0502 0.5166 -0.0420 0.048 Uiso 1 1 calc R . .
C17 C 0.02850(13) 0.7403(7) 0.0043(3) 0.0421(12) Uani 1 1 d . . .
H17A H 0.0186 0.7711 -0.0491 0.051 Uiso 1 1 calc R . .
H17B H 0.0062 0.7017 0.0289 0.051 Uiso 1 1 calc R . .
C18 C 0.04628(14) 0.9046(7) 0.0450(4) 0.0343(11) Uani 1 1 d . . .
H18 H 0.0330(15) 0.946(7) 0.088(3) 0.041 Uiso 1 1 calc . . .
C19 C 0.06366(15) 1.0379(7) 0.0081(3) 0.0337(11) Uani 1 1 d . . .
H19 H 0.0606(14) 1.158(7) 0.030(3) 0.040 Uiso 1 1 calc . . .
C20 C 0.06911(16) 1.0401(7) -0.0734(3) 0.0483(13) Uani 1 1 d . . .
H20A H 0.0865 1.1391 -0.0816 0.058 Uiso 1 1 calc R . .
H20B H 0.0438 1.0625 -0.1049 0.058 Uiso 1 1 calc R . .
C21 C 0.08600(16) 0.8688(7) -0.1002(3) 0.0435(12) Uani 1 1 d . . .
H21A H 0.0646 0.7883 -0.1204 0.052 Uiso 1 1 calc R . .
H21B H 0.1009 0.8957 -0.1420 0.052 Uiso 1 1 calc R . .
Ir1 Ir 0.109736(4) 0.882308(19) 0.072748(8) 0.01982(5) Uani 1 1 d . . .
N1 N 0.19658(9) 0.8649(4) 0.08462(18) 0.0199(6) Uani 1 1 d . . .
N2 N 0.17626(9) 0.6757(4) 0.16135(18) 0.0208(7) Uani 1 1 d . . .
H1XX H 0.04(13) 1.0(6) -0.7(3) 0.0(12) Uiso 0.01 1 d P . .
H1YY H -0.11(14) 0.6(7) -0.4(3) 0.0(14) Uiso 0.01 1 d P . .
C30 C 0.0000 0.844(3) 0.7500 0.0637(14) Uiso 0.546(8) 2 d SPD A 1
C31 C 0.0000 0.641(2) 0.7500 0.0637(14) Uiso 0.546(8) 2 d SPD . 1
C32 C -0.0267(4) 0.5741(19) 0.7911(9) 0.0637(14) Uiso 0.546(8) 1 d PD A 1
C33 C -0.0263(4) 0.3731(18) 0.7906(8) 0.0637(14) Uiso 0.546(8) 1 d PD A 1
C34 C 0.0000 0.300(2) 0.7500 0.0637(14) Uiso 0.546(8) 2 d SPD . 1
C40 C -0.0218(8) 0.280(3) 0.7746(16) 0.0637(14) Uiso 0.227(4) 1 d PD . 2
C41 C -0.0176(4) 0.471(2) 0.7757(8) 0.0637(14) Uiso 0.454(8) 1 d PD . 2
C42 C -0.0306(5) 0.634(2) 0.7971(11) 0.0637(14) Uiso 0.454(8) 1 d PD . 2
C43 C 0.0155(4) 0.766(2) 0.7274(9) 0.0637(14) Uiso 0.454(8) 1 d PD . 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
Br 0.0356(2) 0.0361(2) 0.0339(2) -0.01455(19) 0.00362(19) 0.00113(18)
C1 0.0202(18) 0.0165(17) 0.0215(19) -0.0033(14) 0.0018(15) -0.0017(14)
C2 0.0219(19) 0.0193(18) 0.0191(18) 0.0002(14) 0.0017(15) -0.0015(14)
C3 0.0195(18) 0.0197(17) 0.0158(17) -0.0012(14) 0.0000(14) 0.0020(14)
C4 0.024(2) 0.0233(19) 0.023(2) -0.0015(15) 0.0032(16) -0.0027(15)
C5 0.0184(19) 0.031(2) 0.028(2) -0.0032(17) 0.0023(16) 0.0012(16)
C6 0.027(2) 0.028(2) 0.031(2) 0.0018(18) -0.0007(18) 0.0071(17)
C7 0.029(2) 0.0232(19) 0.021(2) 0.0041(15) -0.0004(16) -0.0007(16)
C8 0.026(2) 0.0209(18) 0.0170(18) 0.0031(14) 0.0010(15) -0.0008(15)
C9 0.035(2) 0.0223(19) 0.022(2) 0.0002(16) 0.0076(17) -0.0002(17)
C10 0.051(3) 0.019(2) 0.037(3) 0.0074(18) 0.010(2) 0.0009(19)
C11 0.022(2) 0.026(2) 0.024(2) 0.0057(15) 0.0031(16) -0.0037(15)
C12 0.027(2) 0.037(2) 0.029(2) 0.0035(18) 0.0085(18) -0.0027(18)
C13 0.052(3) 0.048(3) 0.040(3) 0.014(2) 0.023(2) -0.001(3)
C14 0.024(2) 0.038(3) 0.021(2) -0.006(2) -0.0004(17) 0.0030(19)
C15 0.027(2) 0.025(2) 0.032(3) -0.006(2) -0.0002(19) -0.0013(18)
C16 0.028(2) 0.035(3) 0.056(3) -0.010(2) 0.003(2) -0.0079(19)
C17 0.023(2) 0.043(3) 0.060(3) -0.008(2) 0.004(2) -0.005(2)
C18 0.017(2) 0.040(3) 0.046(3) -0.005(3) 0.002(2) 0.004(2)
C19 0.032(3) 0.024(3) 0.041(3) -0.003(2) -0.006(2) 0.009(2)
C20 0.053(3) 0.048(3) 0.038(3) 0.011(2) -0.012(2) 0.011(3)
C21 0.043(3) 0.057(3) 0.029(2) 0.001(2) -0.002(2) 0.002(2)
Ir1 0.01773(8) 0.02039(8) 0.02067(8) -0.00151(6) 0.00054(5) 0.00037(6)
N1 0.0182(15) 0.0194(15) 0.0212(16) 0.0046(12) 0.0002(12) -0.0022(12)
N2 0.0179(15) 0.0228(16) 0.0219(16) 0.0050(13) 0.0034(13) -0.0014(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'
Ir Ir -1.4442 7.9887 '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'
|
1100899.cif | #------------------------------------------------------------------------------
#$Date: 2018-09-01 22:33:33 +0300 (Sat, 01 Sep 2018) $
#$Revision: 210321 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100899.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_1100899
loop_
_publ_author_name
'Izod, Keith'
'McFarlane, William'
'Allen, Ben'
'Clegg, William'
'Harrington, Ross W.'
_publ_section_title
;
An Intramolecularly Base-Stabilized Diphosphagermylene and Two Unusual
Germanium(II) Ate Complexes: A Structural, NMR, and DFT Study
;
_journal_coden_ASTM ORGND7
_journal_issue 9
_journal_name_full Organometallics
_journal_page_first 2157
_journal_page_last 2167
_journal_paper_doi 10.1021/om0501125
_journal_volume 24
_journal_year 2005
_chemical_formula_moiety 'C32 H62 Ge N2 P2 Si4, 0.5 C7 H14'
_chemical_formula_sum 'C35.5 H69 Ge N2 P2 Si4'
_chemical_formula_weight 770.82
_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 78.569(1)
_cell_angle_beta 89.576(1)
_cell_angle_gamma 75.536(1)
_cell_formula_units_Z 2
_cell_length_a 11.4596(5)
_cell_length_b 12.0029(5)
_cell_length_c 16.3524(7)
_cell_measurement_reflns_used 13588
_cell_measurement_temperature 150(2)
_cell_measurement_theta_max 28.9
_cell_measurement_theta_min 2.16
_cell_volume 2132.65(16)
_diffrn_ambient_temperature 150(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type 'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method '\w rotation with narrow frames'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0157
_diffrn_reflns_av_sigmaI/netI 0.0241
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_number 15612
_diffrn_reflns_theta_max 28.86
_diffrn_reflns_theta_min 1.84
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 0.931
_exptl_absorpt_correction_T_max 0.737
_exptl_absorpt_correction_T_min 0.653
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details SADABS
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.200
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 820
_exptl_crystal_size_max 0.50
_exptl_crystal_size_mid 0.40
_exptl_crystal_size_min 0.35
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.036
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 413
_refine_ls_number_reflns 9401
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.036
_refine_ls_R_factor_all 0.0299
_refine_ls_R_factor_gt 0.0268
_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^)+(0.0417P)^2^+0.8715P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0755
_refine_ls_wR_factor_ref 0.0776
_reflns_number_gt 8637
_reflns_number_total 9401
_reflns_threshold_expression I>2\s(I)
_cod_database_code 1100899
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
Ge Ge 0.339664(13) 0.041854(12) 0.179005(9) 0.01916(5) Uani 1 1 d . . .
P1 P 0.19237(3) 0.03927(3) 0.28420(2) 0.01874(8) Uani 1 1 d . . .
P2 P 0.47156(3) -0.13012(3) 0.26407(2) 0.01758(8) Uani 1 1 d . . .
Si1 Si -0.03479(4) 0.09811(4) 0.17835(3) 0.02998(10) Uani 1 1 d . . .
Si2 Si -0.02151(4) 0.25897(4) 0.30948(3) 0.02919(10) Uani 1 1 d . . .
Si3 Si 0.35557(4) -0.33940(4) 0.34097(3) 0.02924(10) Uani 1 1 d . . .
Si4 Si 0.40852(4) -0.30121(4) 0.14575(3) 0.02887(10) Uani 1 1 d . . .
N1 N 0.41870(12) 0.17393(11) 0.21553(8) 0.0244(3) Uani 1 1 d . . .
N2 N 0.81877(12) -0.38364(12) 0.37561(9) 0.0314(3) Uani 1 1 d . . .
C1 C 0.06320(13) 0.16638(13) 0.23583(9) 0.0224(3) Uani 1 1 d . . .
H1 H 0.0974 0.2195 0.1927 0.027 Uiso 1 1 calc R . .
C2 C -0.1314(2) 0.2119(2) 0.09383(16) 0.0634(7) Uani 1 1 d . . .
H2A H -0.1714 0.1733 0.0592 0.095 Uiso 1 1 calc R . .
H2B H -0.0809 0.2554 0.0591 0.095 Uiso 1 1 calc R . .
H2C H -0.1924 0.2663 0.1191 0.095 Uiso 1 1 calc R . .
C3 C -0.12808(17) 0.02272(19) 0.25303(14) 0.0437(5) Uani 1 1 d . . .
H3A H -0.1860 0.0811 0.2771 0.066 Uiso 1 1 calc R . .
H3B H -0.0755 -0.0335 0.2977 0.066 Uiso 1 1 calc R . .
H3C H -0.1717 -0.0191 0.2235 0.066 Uiso 1 1 calc R . .
C4 C 0.05627(17) -0.01435(19) 0.12280(12) 0.0403(4) Uani 1 1 d . . .
H4A H 0.1012 -0.0823 0.1639 0.060 Uiso 1 1 calc R . .
H4B H 0.1130 0.0198 0.0873 0.060 Uiso 1 1 calc R . .
H4C H 0.0023 -0.0394 0.0881 0.060 Uiso 1 1 calc R . .
C5 C -0.04985(18) 0.16944(19) 0.41147(12) 0.0441(5) Uani 1 1 d . . .
H5A H 0.0246 0.1423 0.4467 0.066 Uiso 1 1 calc R . .
H5B H -0.0761 0.1014 0.4015 0.066 Uiso 1 1 calc R . .
H5C H -0.1128 0.2177 0.4397 0.066 Uiso 1 1 calc R . .
C6 C 0.05901(17) 0.36965(16) 0.32954(13) 0.0400(4) Uani 1 1 d . . .
H6A H 0.0045 0.4284 0.3554 0.060 Uiso 1 1 calc R . .
H6B H 0.0849 0.4085 0.2766 0.060 Uiso 1 1 calc R . .
H6C H 0.1298 0.3299 0.3671 0.060 Uiso 1 1 calc R . .
C7 C -0.17277(17) 0.34883(19) 0.26168(15) 0.0492(5) Uani 1 1 d . . .
H7A H -0.2233 0.2964 0.2542 0.074 Uiso 1 1 calc R . .
H7B H -0.1620 0.3961 0.2073 0.074 Uiso 1 1 calc R . .
H7C H -0.2118 0.4008 0.2986 0.074 Uiso 1 1 calc R . .
C8 C 0.26477(13) 0.08112(12) 0.36949(9) 0.0206(3) Uani 1 1 d . . .
C9 C 0.25681(14) 0.01789(14) 0.45027(9) 0.0262(3) Uani 1 1 d . . .
H9 H 0.2091 -0.0374 0.4586 0.031 Uiso 1 1 calc R . .
C10 C 0.31723(16) 0.03437(16) 0.51840(10) 0.0328(4) Uani 1 1 d . . .
H10 H 0.3097 -0.0086 0.5727 0.039 Uiso 1 1 calc R . .
C11 C 0.38837(16) 0.11337(16) 0.50722(11) 0.0341(4) Uani 1 1 d . . .
H11 H 0.4314 0.1235 0.5535 0.041 Uiso 1 1 calc R . .
C12 C 0.39632(15) 0.17746(15) 0.42804(11) 0.0295(3) Uani 1 1 d . . .
H12 H 0.4446 0.2323 0.4205 0.035 Uiso 1 1 calc R . .
C13 C 0.33477(13) 0.16303(13) 0.35907(9) 0.0225(3) Uani 1 1 d . . .
C14 C 0.34186(14) 0.23746(12) 0.27455(10) 0.0238(3) Uani 1 1 d . . .
H14A H 0.2592 0.2702 0.2490 0.029 Uiso 1 1 calc R . .
H14B H 0.3739 0.3043 0.2820 0.029 Uiso 1 1 calc R . .
C15 C 0.4172(2) 0.26027(16) 0.13643(12) 0.0412(4) Uani 1 1 d . . .
H15A H 0.4517 0.3232 0.1472 0.062 Uiso 1 1 calc R . .
H15B H 0.3339 0.2938 0.1142 0.062 Uiso 1 1 calc R . .
H15C H 0.4652 0.2208 0.0957 0.062 Uiso 1 1 calc R . .
C16 C 0.54396(15) 0.12672(16) 0.25044(13) 0.0354(4) Uani 1 1 d . . .
H16A H 0.5954 0.0930 0.2087 0.053 Uiso 1 1 calc R . .
H16B H 0.5460 0.0656 0.3004 0.053 Uiso 1 1 calc R . .
H16C H 0.5736 0.1902 0.2654 0.053 Uiso 1 1 calc R . .
C17 C 0.38364(13) -0.23667(12) 0.24288(9) 0.0216(3) Uani 1 1 d . . .
H17 H 0.3012 -0.1828 0.2295 0.026 Uiso 1 1 calc R . .
C18 C 0.19067(19) -0.3334(2) 0.33874(15) 0.0562(6) Uani 1 1 d . . .
H18A H 0.1741 -0.3916 0.3855 0.084 Uiso 1 1 calc R . .
H18B H 0.1675 -0.3507 0.2860 0.084 Uiso 1 1 calc R . .
H18C H 0.1441 -0.2547 0.3436 0.084 Uiso 1 1 calc R . .
C19 C 0.4438(2) -0.49559(15) 0.34901(14) 0.0446(5) Uani 1 1 d . . .
H19A H 0.5299 -0.5010 0.3565 0.067 Uiso 1 1 calc R . .
H19B H 0.4297 -0.5220 0.2978 0.067 Uiso 1 1 calc R . .
H19C H 0.4179 -0.5455 0.3969 0.067 Uiso 1 1 calc R . .
C20 C 0.39359(19) -0.29639(17) 0.43906(11) 0.0392(4) Uani 1 1 d . . .
H20A H 0.3611 -0.3410 0.4866 0.059 Uiso 1 1 calc R . .
H20B H 0.3582 -0.2122 0.4351 0.059 Uiso 1 1 calc R . .
H20C H 0.4814 -0.3134 0.4470 0.059 Uiso 1 1 calc R . .
C21 C 0.55919(19) -0.40591(18) 0.14209(14) 0.0467(5) Uani 1 1 d . . .
H21A H 0.5599 -0.4423 0.0934 0.070 Uiso 1 1 calc R . .
H21B H 0.5743 -0.4671 0.1931 0.070 Uiso 1 1 calc R . .
H21C H 0.6223 -0.3632 0.1379 0.070 Uiso 1 1 calc R . .
C22 C 0.2886(2) -0.38089(18) 0.13589(14) 0.0485(5) Uani 1 1 d . . .
H22A H 0.2088 -0.3259 0.1328 0.073 Uiso 1 1 calc R . .
H22B H 0.2951 -0.4449 0.1846 0.073 Uiso 1 1 calc R . .
H22C H 0.2996 -0.4133 0.0851 0.073 Uiso 1 1 calc R . .
C23 C 0.38521(19) -0.18378(17) 0.04936(11) 0.0389(4) Uani 1 1 d . . .
H23A H 0.4531 -0.1471 0.0447 0.058 Uiso 1 1 calc R . .
H23B H 0.3101 -0.1242 0.0524 0.058 Uiso 1 1 calc R . .
H23C H 0.3802 -0.2183 0.0004 0.058 Uiso 1 1 calc R . .
C24 C 0.61238(13) -0.16292(12) 0.20656(9) 0.0196(3) Uani 1 1 d . . .
C25 C 0.62652(14) -0.09797(13) 0.12771(9) 0.0247(3) Uani 1 1 d . . .
H25 H 0.5606 -0.0365 0.1012 0.030 Uiso 1 1 calc R . .
C26 C 0.73447(16) -0.12081(15) 0.08702(10) 0.0304(3) Uani 1 1 d . . .
H26 H 0.7417 -0.0755 0.0335 0.036 Uiso 1 1 calc R . .
C27 C 0.83109(16) -0.21001(15) 0.12525(11) 0.0321(4) Uani 1 1 d . . .
H27 H 0.9048 -0.2267 0.0977 0.038 Uiso 1 1 calc R . .
C28 C 0.82011(15) -0.27496(14) 0.20372(10) 0.0286(3) Uani 1 1 d . . .
H28 H 0.8868 -0.3361 0.2295 0.034 Uiso 1 1 calc R . .
C29 C 0.71268(13) -0.25206(12) 0.24548(9) 0.0221(3) Uani 1 1 d . . .
C30 C 0.70313(14) -0.32623(14) 0.33028(10) 0.0270(3) Uani 1 1 d . . .
H30A H 0.6519 -0.2757 0.3646 0.032 Uiso 1 1 calc R . .
H30B H 0.6621 -0.3873 0.3230 0.032 Uiso 1 1 calc R . .
C31 C 0.87381(17) -0.29882(19) 0.40210(13) 0.0434(4) Uani 1 1 d . . .
H31A H 0.8222 -0.2600 0.4416 0.065 Uiso 1 1 calc R . .
H31B H 0.8830 -0.2399 0.3533 0.065 Uiso 1 1 calc R . .
H31C H 0.9532 -0.3395 0.4292 0.065 Uiso 1 1 calc R . .
C32 C 0.80028(18) -0.46803(18) 0.44877(12) 0.0469(5) Uani 1 1 d . . .
H32A H 0.8777 -0.5068 0.4792 0.070 Uiso 1 1 calc R . .
H32B H 0.7661 -0.5270 0.4310 0.070 Uiso 1 1 calc R . .
H32C H 0.7446 -0.4270 0.4853 0.070 Uiso 1 1 calc R . .
C33 C 0.1023(3) 0.4176(3) 0.0787(2) 0.0882(10) Uani 1 1 d . . .
H33A H 0.1755 0.4264 0.1058 0.106 Uiso 1 1 calc R . .
H33B H 0.0845 0.3414 0.1025 0.106 Uiso 1 1 calc R . .
C34 C 0.0014(3) 0.5166(3) 0.0706(3) 0.1000(12) Uani 1 1 d . . .
H34A H 0.0360 0.5852 0.0665 0.120 Uiso 1 1 calc R . .
H34B H -0.0368 0.5080 0.1252 0.120 Uiso 1 1 calc R . .
C35 C -0.0978(5) 0.5537(4) 0.0085(2) 0.1180(16) Uani 1 1 d . . .
H35A H -0.1416 0.4914 0.0215 0.142 Uiso 1 1 calc R . .
H35B H -0.1512 0.6237 0.0248 0.142 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
Ge 0.01867(8) 0.01913(8) 0.01761(8) -0.00237(5) -0.00083(5) -0.00200(6)
P1 0.01654(17) 0.01890(16) 0.01987(17) -0.00344(13) -0.00130(12) -0.00316(13)
P2 0.01724(17) 0.01717(16) 0.01701(16) -0.00235(12) 0.00033(12) -0.00281(13)
Si1 0.0210(2) 0.0333(2) 0.0349(2) -0.00705(19) -0.00836(17) -0.00520(17)
Si2 0.0189(2) 0.0289(2) 0.0363(2) -0.00865(18) 0.00046(17) 0.00189(16)
Si3 0.0286(2) 0.0239(2) 0.0327(2) 0.00559(17) -0.00149(17) -0.01072(17)
Si4 0.0323(2) 0.0244(2) 0.0304(2) -0.00985(17) -0.00574(17) -0.00457(17)
N1 0.0235(7) 0.0194(6) 0.0301(7) -0.0048(5) 0.0053(5) -0.0056(5)
N2 0.0234(7) 0.0299(7) 0.0292(7) 0.0058(5) 0.0034(5) 0.0056(5)
C1 0.0163(7) 0.0225(7) 0.0258(7) -0.0025(5) -0.0034(5) -0.0019(5)
C2 0.0628(15) 0.0570(14) 0.0616(15) -0.0044(11) -0.0413(12) -0.0036(11)
C3 0.0285(9) 0.0481(11) 0.0619(13) -0.0195(10) 0.0065(8) -0.0169(8)
C4 0.0317(10) 0.0567(12) 0.0400(10) -0.0225(9) -0.0021(7) -0.0152(8)
C5 0.0350(10) 0.0521(11) 0.0409(10) -0.0097(9) 0.0119(8) -0.0030(8)
C6 0.0305(9) 0.0348(9) 0.0556(12) -0.0226(8) 0.0023(8) 0.0008(7)
C7 0.0262(10) 0.0449(11) 0.0691(15) -0.0181(10) -0.0072(9) 0.0097(8)
C8 0.0173(7) 0.0214(6) 0.0212(7) -0.0062(5) -0.0013(5) 0.0001(5)
C9 0.0232(8) 0.0283(7) 0.0238(7) -0.0037(6) 0.0011(6) -0.0017(6)
C10 0.0316(9) 0.0415(9) 0.0202(7) -0.0065(6) -0.0014(6) 0.0008(7)
C11 0.0302(9) 0.0421(9) 0.0291(8) -0.0187(7) -0.0069(6) 0.0016(7)
C12 0.0244(8) 0.0299(8) 0.0363(9) -0.0165(7) -0.0038(6) -0.0027(6)
C13 0.0192(7) 0.0206(6) 0.0265(7) -0.0083(5) -0.0010(5) -0.0001(5)
C14 0.0229(7) 0.0169(6) 0.0319(8) -0.0072(6) 0.0018(6) -0.0041(5)
C15 0.0552(12) 0.0275(8) 0.0402(10) -0.0005(7) 0.0174(8) -0.0147(8)
C16 0.0202(8) 0.0340(9) 0.0576(11) -0.0203(8) 0.0038(7) -0.0083(7)
C17 0.0208(7) 0.0183(6) 0.0246(7) -0.0012(5) -0.0019(5) -0.0049(5)
C18 0.0354(11) 0.0667(14) 0.0589(13) 0.0202(11) -0.0011(9) -0.0249(10)
C19 0.0558(13) 0.0229(8) 0.0522(12) 0.0047(8) -0.0108(9) -0.0140(8)
C20 0.0507(11) 0.0367(9) 0.0277(8) 0.0026(7) 0.0082(7) -0.0140(8)
C21 0.0441(11) 0.0421(10) 0.0540(12) -0.0281(9) -0.0062(9) 0.0037(9)
C22 0.0562(13) 0.0399(10) 0.0540(12) -0.0107(9) -0.0182(10) -0.0192(9)
C23 0.0486(11) 0.0449(10) 0.0250(8) -0.0101(7) -0.0020(7) -0.0127(8)
C24 0.0201(7) 0.0184(6) 0.0204(7) -0.0051(5) 0.0023(5) -0.0042(5)
C25 0.0274(8) 0.0224(7) 0.0218(7) -0.0020(5) 0.0026(5) -0.0037(6)
C26 0.0343(9) 0.0303(8) 0.0243(7) -0.0022(6) 0.0099(6) -0.0067(7)
C27 0.0294(9) 0.0314(8) 0.0338(9) -0.0076(7) 0.0141(7) -0.0044(7)
C28 0.0237(8) 0.0252(7) 0.0331(8) -0.0049(6) 0.0065(6) -0.0003(6)
C29 0.0220(7) 0.0193(6) 0.0235(7) -0.0031(5) 0.0034(5) -0.0036(5)
C30 0.0203(7) 0.0269(7) 0.0269(7) 0.0033(6) 0.0030(6) -0.0005(6)
C31 0.0267(9) 0.0560(12) 0.0417(10) -0.0050(9) -0.0042(7) -0.0037(8)
C32 0.0388(10) 0.0443(11) 0.0366(10) 0.0157(8) 0.0064(8) 0.0089(8)
C33 0.089(2) 0.0638(18) 0.103(3) -0.0100(17) -0.0116(19) -0.0092(16)
C34 0.075(2) 0.073(2) 0.145(4) -0.026(2) 0.036(2) -0.0033(17)
C35 0.199(5) 0.114(3) 0.067(2) -0.048(2) 0.005(3) -0.065(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'
Ge Ge 0.1547 1.8001 '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'
|
1100900.cif | #------------------------------------------------------------------------------
#$Date: 2018-09-01 22:33:33 +0300 (Sat, 01 Sep 2018) $
#$Revision: 210321 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/09/1100900.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_1100900
loop_
_publ_author_name
'Izod, Keith'
'McFarlane, William'
'Allen, Ben'
'Clegg, William'
'Harrington, Ross W.'
_publ_section_title
;
An Intramolecularly Base-Stabilized Diphosphagermylene and Two Unusual
Germanium(II) Ate Complexes: A Structural, NMR, and DFT Study
;
_journal_coden_ASTM ORGND7
_journal_issue 9
_journal_name_full Organometallics
_journal_page_first 2157
_journal_page_last 2167
_journal_paper_doi 10.1021/om0501125
_journal_volume 24
_journal_year 2005
_chemical_formula_moiety 'C44 H92 Ge I2 Li2 N2 O3 P2 Si4'
_chemical_formula_sum 'C44 H92 Ge I2 Li2 N2 O3 P2 Si4'
_chemical_formula_weight 1211.77
_space_group_IT_number 33
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall 'P 2c -2n'
_symmetry_space_group_name_H-M 'P n a 21'
_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 90.00
_cell_formula_units_Z 4
_cell_length_a 48.748(3)
_cell_length_b 11.2312(6)
_cell_length_c 11.1410(6)
_cell_measurement_reflns_used 17640
_cell_measurement_temperature 160(2)
_cell_measurement_theta_max 28.41
_cell_measurement_theta_min 2.20
_cell_volume 6099.7(6)
_diffrn_ambient_temperature 160(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type 'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method 'thin-slice \w 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 0.0481
_diffrn_reflns_av_sigmaI/netI 0.0533
_diffrn_reflns_limit_h_max 65
_diffrn_reflns_limit_h_min -64
_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 49557
_diffrn_reflns_theta_max 28.48
_diffrn_reflns_theta_min 1.67
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 1.679
_exptl_absorpt_correction_T_max 0.730
_exptl_absorpt_correction_T_min 0.680
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details SADABS
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.320
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 2496
_exptl_crystal_size_max 0.25
_exptl_crystal_size_mid 0.25
_exptl_crystal_size_min 0.20
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack 0.052(11)
_refine_ls_extinction_coef 0.00012(5)
_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 1.106
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 561
_refine_ls_number_reflns 14270
_refine_ls_number_restraints 39
_refine_ls_restrained_S_all 1.104
_refine_ls_R_factor_all 0.0581
_refine_ls_R_factor_gt 0.0476
_refine_ls_shift/su_max 0.008
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0329P)^2^+9.7031P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0965
_refine_ls_wR_factor_ref 0.0998
_reflns_number_gt 12469
_reflns_number_total 14270
_reflns_threshold_expression I>2\s(I)
_cod_database_code 1100900
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
Ge Ge 0.067606(11) 0.41943(4) 0.14749(5) 0.02175(11) Uani 1 1 d . . .
P1 P 0.08465(3) 0.21787(11) 0.14584(12) 0.0207(2) Uani 1 1 d . . .
C1 C 0.07141(10) 0.1472(4) 0.0036(4) 0.0233(10) Uani 1 1 d . . .
H1 H 0.0706 0.2112 -0.0587 0.028 Uiso 1 1 calc R . .
Si1 Si 0.03499(3) 0.09611(14) 0.03171(13) 0.0292(3) Uani 1 1 d . . .
C2 C 0.01515(12) 0.1986(6) 0.1323(6) 0.0472(16) Uani 1 1 d . . .
H2A H 0.0146 0.2784 0.0967 0.071 Uiso 1 1 calc R . .
H2B H 0.0241 0.2024 0.2110 0.071 Uiso 1 1 calc R . .
H2C H -0.0036 0.1686 0.1416 0.071 Uiso 1 1 calc R . .
C3 C 0.01636(14) 0.0923(6) -0.1142(6) 0.0468(16) Uani 1 1 d . . .
H3A H 0.0171 0.1711 -0.1517 0.070 Uiso 1 1 calc R . .
H3B H -0.0028 0.0699 -0.1004 0.070 Uiso 1 1 calc R . .
H3C H 0.0250 0.0337 -0.1674 0.070 Uiso 1 1 calc R . .
C4 C 0.03451(13) -0.0518(5) 0.1089(6) 0.0457(15) Uani 1 1 d . . .
H4A H 0.0443 -0.0457 0.1855 0.068 Uiso 1 1 calc R . .
H4B H 0.0435 -0.1112 0.0580 0.068 Uiso 1 1 calc R . .
H4C H 0.0155 -0.0758 0.1235 0.068 Uiso 1 1 calc R . .
Si2 Si 0.09471(3) 0.02605(14) -0.05661(14) 0.0317(3) Uani 1 1 d . . .
C5 C 0.10606(15) -0.0780(5) 0.0645(6) 0.0473(17) Uani 1 1 d . . .
H5A H 0.0900 -0.1095 0.1065 0.071 Uiso 1 1 calc R . .
H5B H 0.1178 -0.0351 0.1215 0.071 Uiso 1 1 calc R . .
H5C H 0.1164 -0.1439 0.0290 0.071 Uiso 1 1 calc R . .
C6 C 0.07665(16) -0.0678(6) -0.1734(7) 0.0551(18) Uani 1 1 d . . .
H6A H 0.0600 -0.1024 -0.1385 0.083 Uiso 1 1 calc R . .
H6B H 0.0889 -0.1317 -0.2000 0.083 Uiso 1 1 calc R . .
H6C H 0.0717 -0.0178 -0.2421 0.083 Uiso 1 1 calc R . .
C7 C 0.12578(14) 0.0853(6) -0.1346(6) 0.0469(16) Uani 1 1 d . . .
H7A H 0.1201 0.1398 -0.1987 0.070 Uiso 1 1 calc R . .
H7B H 0.1362 0.0191 -0.1692 0.070 Uiso 1 1 calc R . .
H7C H 0.1373 0.1281 -0.0768 0.070 Uiso 1 1 calc R . .
C8 C 0.12226(10) 0.2446(4) 0.1215(4) 0.0238(11) Uani 1 1 d . . .
C9 C 0.14017(11) 0.1772(5) 0.1898(5) 0.0307(12) Uani 1 1 d . . .
H9 H 0.1331 0.1228 0.2474 0.037 Uiso 1 1 calc R . .
C10 C 0.16825(13) 0.1885(6) 0.1750(6) 0.0452(16) Uani 1 1 d . . .
H10 H 0.1803 0.1393 0.2202 0.054 Uiso 1 1 calc R . .
C11 C 0.17882(13) 0.2688(6) 0.0967(8) 0.0564(19) Uani 1 1 d . . .
H11 H 0.1981 0.2752 0.0867 0.068 Uiso 1 1 calc R . .
C12 C 0.16126(12) 0.3419(6) 0.0308(6) 0.0426(15) Uani 1 1 d . . .
H12 H 0.1687 0.4001 -0.0219 0.051 Uiso 1 1 calc R . .
C13 C 0.13281(11) 0.3301(5) 0.0418(5) 0.0279(11) Uani 1 1 d . . .
C14 C 0.11435(11) 0.4073(4) -0.0335(5) 0.0267(11) Uani 1 1 d . . .
H14A H 0.1255 0.4470 -0.0962 0.032 Uiso 1 1 calc R . .
H14B H 0.1006 0.3564 -0.0742 0.032 Uiso 1 1 calc R . .
N1 N 0.09980(9) 0.4994(4) 0.0378(4) 0.0257(9) Uani 1 1 d . . .
C15 C 0.11913(13) 0.5713(5) 0.1084(5) 0.0360(13) Uani 1 1 d . . .
H15A H 0.1090 0.6309 0.1548 0.054 Uiso 1 1 calc R . .
H15B H 0.1320 0.6114 0.0543 0.054 Uiso 1 1 calc R . .
H15C H 0.1293 0.5194 0.1634 0.054 Uiso 1 1 calc R . .
C16 C 0.08405(12) 0.5784(5) -0.0462(6) 0.0395(14) Uani 1 1 d . . .
H16A H 0.0712 0.5301 -0.0932 0.059 Uiso 1 1 calc R . .
H16B H 0.0968 0.6188 -0.1006 0.059 Uiso 1 1 calc R . .
H16C H 0.0738 0.6378 0.0001 0.059 Uiso 1 1 calc R . .
P2 P 0.08890(2) 0.42599(10) 0.34267(11) 0.0196(2) Uani 1 1 d . . .
C17 C 0.05755(9) 0.3584(4) 0.4195(4) 0.0195(9) Uani 1 1 d . . .
H17 H 0.0484 0.3144 0.3523 0.023 Uiso 1 1 calc R . .
Si3 Si 0.06812(3) 0.23417(12) 0.52358(13) 0.0248(3) Uani 1 1 d . . .
C18 C 0.10293(11) 0.1709(5) 0.4920(5) 0.0332(12) Uani 1 1 d . . .
H18A H 0.1038 0.1444 0.4083 0.050 Uiso 1 1 calc R . .
H18B H 0.1063 0.1031 0.5454 0.050 Uiso 1 1 calc R . .
H18C H 0.1169 0.2322 0.5059 0.050 Uiso 1 1 calc R . .
C19 C 0.04346(12) 0.1068(5) 0.5035(6) 0.0404(14) Uani 1 1 d . . .
H19A H 0.0435 0.0816 0.4193 0.061 Uiso 1 1 calc R . .
H19B H 0.0250 0.1325 0.5263 0.061 Uiso 1 1 calc R . .
H19C H 0.0491 0.0400 0.5545 0.061 Uiso 1 1 calc R . .
C20 C 0.06857(15) 0.2829(5) 0.6847(5) 0.0400(15) Uani 1 1 d . . .
H20A H 0.0507 0.3172 0.7058 0.060 Uiso 1 1 calc R . .
H20B H 0.0829 0.3430 0.6961 0.060 Uiso 1 1 calc R . .
H20C H 0.0723 0.2142 0.7363 0.060 Uiso 1 1 calc R . .
Si4 Si 0.02892(3) 0.45520(13) 0.47847(13) 0.0252(3) Uani 1 1 d . . .
C21 C 0.00092(12) 0.3560(6) 0.5366(6) 0.0415(15) Uani 1 1 d . . .
H21A H -0.0051 0.3020 0.4727 0.062 Uiso 1 1 calc R . .
H21B H -0.0146 0.4048 0.5628 0.062 Uiso 1 1 calc R . .
H21C H 0.0078 0.3094 0.6046 0.062 Uiso 1 1 calc R . .
C22 C 0.01165(13) 0.5443(6) 0.3572(6) 0.0431(16) Uani 1 1 d . . .
H22A H 0.0060 0.4910 0.2921 0.065 Uiso 1 1 calc R . .
H22B H 0.0245 0.6039 0.3258 0.065 Uiso 1 1 calc R . .
H22C H -0.0045 0.5844 0.3904 0.065 Uiso 1 1 calc R . .
C23 C 0.03974(12) 0.5569(5) 0.6012(5) 0.0328(12) Uani 1 1 d . . .
H23A H 0.0543 0.6096 0.5721 0.049 Uiso 1 1 calc R . .
H23B H 0.0466 0.5100 0.6691 0.049 Uiso 1 1 calc R . .
H23C H 0.0240 0.6049 0.6272 0.049 Uiso 1 1 calc R . .
C24 C 0.08948(10) 0.5831(4) 0.3960(4) 0.0217(10) Uani 1 1 d . . .
C25 C 0.07476(10) 0.6737(4) 0.3397(5) 0.0287(11) Uani 1 1 d . . .
H25 H 0.0646 0.6559 0.2691 0.034 Uiso 1 1 calc R . .
C26 C 0.07451(12) 0.7896(5) 0.3841(6) 0.0364(13) Uani 1 1 d . . .
H26 H 0.0643 0.8499 0.3444 0.044 Uiso 1 1 calc R . .
C27 C 0.08937(13) 0.8161(5) 0.4867(6) 0.0370(14) Uani 1 1 d . . .
H27 H 0.0891 0.8943 0.5192 0.044 Uiso 1 1 calc R . .
C28 C 0.10458(11) 0.7279(5) 0.5413(5) 0.0322(12) Uani 1 1 d . . .
H28 H 0.1148 0.7468 0.6114 0.039 Uiso 1 1 calc R . .
C29 C 0.10548(10) 0.6135(4) 0.4977(5) 0.0236(10) Uani 1 1 d . . .
C30 C 0.12325(10) 0.5237(4) 0.5644(4) 0.0234(10) Uani 1 1 d . . .
H30A H 0.1201 0.5328 0.6517 0.028 Uiso 1 1 calc R . .
H30B H 0.1174 0.4423 0.5415 0.028 Uiso 1 1 calc R . .
N2 N 0.15313(9) 0.5369(4) 0.5393(4) 0.0257(9) Uani 1 1 d . . .
C31 C 0.16730(12) 0.4469(5) 0.6132(6) 0.0392(15) Uani 1 1 d . . .
H31A H 0.1871 0.4524 0.5997 0.059 Uiso 1 1 calc R . .
H31B H 0.1609 0.3672 0.5907 0.059 Uiso 1 1 calc R . .
H31C H 0.1633 0.4611 0.6982 0.059 Uiso 1 1 calc R . .
C32 C 0.15920(12) 0.5123(5) 0.4123(5) 0.0365(13) Uani 1 1 d . . .
H32A H 0.1789 0.5216 0.3980 0.055 Uiso 1 1 calc R . .
H32B H 0.1490 0.5683 0.3615 0.055 Uiso 1 1 calc R . .
H32C H 0.1537 0.4307 0.3928 0.055 Uiso 1 1 calc R . .
Li1 Li 0.1722(2) 0.7017(8) 0.5861(10) 0.036(2) Uani 1 1 d . A .
O1 O 0.16528(10) 0.8385(4) 0.4840(4) 0.0468(11) Uani 1 1 d . . .
C33X C 0.1530(4) 0.8407(16) 0.3618(18) 0.049(5) Uani 0.45(3) 1 d PU A 1
H33A H 0.1432 0.9168 0.3484 0.059 Uiso 0.45(3) 1 calc PR A 1
H33B H 0.1397 0.7746 0.3525 0.059 Uiso 0.45(3) 1 calc PR A 1
C34X C 0.1761(6) 0.828(3) 0.273(3) 0.092(9) Uani 0.45(3) 1 d PU A 1
H34A H 0.1686 0.8262 0.1914 0.138 Uiso 0.45(3) 1 calc PR A 1
H34B H 0.1859 0.7532 0.2886 0.138 Uiso 0.45(3) 1 calc PR A 1
H34C H 0.1887 0.8949 0.2812 0.138 Uiso 0.45(3) 1 calc PR A 1
C33Y C 0.1765(4) 0.8267(16) 0.3624(18) 0.070(6) Uani 0.55(3) 1 d PU A 2
H33C H 0.1897 0.8921 0.3480 0.084 Uiso 0.55(3) 1 calc PR A 2
H33D H 0.1866 0.7506 0.3565 0.084 Uiso 0.55(3) 1 calc PR A 2
C34Y C 0.1555(5) 0.8299(18) 0.270(2) 0.090(8) Uani 0.55(3) 1 d PU A 2
H34D H 0.1641 0.8197 0.1911 0.136 Uiso 0.55(3) 1 calc PR A 2
H34E H 0.1460 0.9066 0.2728 0.136 Uiso 0.55(3) 1 calc PR A 2
H34F H 0.1423 0.7654 0.2837 0.136 Uiso 0.55(3) 1 calc PR A 2
C35 C 0.15790(16) 0.9477(7) 0.5369(10) 0.076(3) Uani 1 1 d . A .
H35A H 0.1530 0.9325 0.6218 0.091 Uiso 1 1 calc R . .
H35B H 0.1412 0.9773 0.4962 0.091 Uiso 1 1 calc R . .
C36 C 0.1782(2) 1.0411(8) 0.5343(11) 0.091(3) Uani 1 1 d . . .
H36A H 0.1708 1.1122 0.5740 0.137 Uiso 1 1 calc R A .
H36B H 0.1827 1.0602 0.4508 0.137 Uiso 1 1 calc R . .
H36C H 0.1947 1.0145 0.5762 0.137 Uiso 1 1 calc R . .
I1 I 0.159561(7) 0.72234(3) 0.82917(3) 0.03249(9) Uani 1 1 d . . .
I2 I 0.229618(8) 0.69550(3) 0.59322(4) 0.03822(10) Uani 1 1 d . . .
Li2 Li 0.2160(2) 0.7037(8) 0.8376(11) 0.038(2) Uani 1 1 d . A .
O2 O 0.23161(9) 0.8451(4) 0.9154(5) 0.0452(11) Uani 1 1 d . . .
C37 C 0.21423(16) 0.9428(7) 0.9532(8) 0.065(2) Uani 1 1 d . A .
H37A H 0.1965 0.9101 0.9814 0.078 Uiso 1 1 calc R . .
H37B H 0.2230 0.9835 1.0220 0.078 Uiso 1 1 calc R . .
C38 C 0.2090(2) 1.0286(8) 0.8608(11) 0.090(3) Uani 1 1 d . . .
H38A H 0.1972 1.0918 0.8925 0.135 Uiso 1 1 calc R A .
H38B H 0.1998 0.9896 0.7931 0.135 Uiso 1 1 calc R . .
H38C H 0.2264 1.0631 0.8337 0.135 Uiso 1 1 calc R . .
C39 C 0.25903(15) 0.8805(7) 0.8956(9) 0.065(2) Uani 1 1 d . A .
H39A H 0.2642 0.9413 0.9558 0.078 Uiso 1 1 calc R . .
H39B H 0.2605 0.9172 0.8151 0.078 Uiso 1 1 calc R . .
C40 C 0.27785(16) 0.7816(7) 0.9035(11) 0.080(3) Uani 1 1 d . . .
H40A H 0.2966 0.8096 0.8879 0.120 Uiso 1 1 calc R A .
H40B H 0.2728 0.7212 0.8440 0.120 Uiso 1 1 calc R . .
H40C H 0.2769 0.7468 0.9841 0.120 Uiso 1 1 calc R . .
O3 O 0.22979(10) 0.5587(4) 0.9186(4) 0.0490(12) Uani 1 1 d . . .
C41 C 0.23112(18) 0.5368(7) 1.0437(7) 0.065(2) Uani 1 1 d . A .
H41A H 0.2502 0.5488 1.0717 0.078 Uiso 1 1 calc R . .
H41B H 0.2261 0.4529 1.0595 0.078 Uiso 1 1 calc R . .
C42 C 0.2133(2) 0.6131(8) 1.1093(9) 0.089(3) Uani 1 1 d . . .
H42A H 0.2150 0.5960 1.1952 0.134 Uiso 1 1 calc R A .
H42B H 0.1943 0.5997 1.0835 0.134 Uiso 1 1 calc R . .
H42C H 0.2183 0.6963 1.0943 0.134 Uiso 1 1 calc R . .
C43 C 0.2467(2) 0.4701(7) 0.8530(8) 0.073(3) Uani 1 1 d . A .
H43A H 0.2547 0.5085 0.7812 0.087 Uiso 1 1 calc R . .
H43B H 0.2620 0.4443 0.9053 0.087 Uiso 1 1 calc R . .
C44 C 0.23139(19) 0.3673(9) 0.8162(10) 0.091(3) Uani 1 1 d . . .
H44A H 0.2435 0.3128 0.7723 0.137 Uiso 1 1 calc R A .
H44B H 0.2162 0.3921 0.7641 0.137 Uiso 1 1 calc R . .
H44C H 0.2240 0.3269 0.8872 0.137 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
Ge 0.0249(3) 0.0220(2) 0.0184(2) -0.0005(2) -0.0006(2) 0.0005(2)
P1 0.0226(6) 0.0204(6) 0.0190(6) -0.0018(5) 0.0007(5) 0.0001(5)
C1 0.032(3) 0.019(2) 0.019(2) -0.0099(19) -0.001(2) -0.005(2)
Si1 0.0321(8) 0.0308(8) 0.0246(7) 0.0001(6) -0.0046(6) -0.0094(6)
C2 0.024(3) 0.059(4) 0.058(4) -0.013(3) 0.005(3) -0.003(3)
C3 0.048(4) 0.054(4) 0.039(3) 0.007(3) -0.014(3) -0.020(3)
C4 0.043(3) 0.045(3) 0.049(4) 0.009(3) -0.005(3) -0.010(3)
Si2 0.0437(9) 0.0255(7) 0.0259(8) -0.0079(6) 0.0031(7) 0.0042(7)
C5 0.068(5) 0.028(3) 0.045(4) -0.009(3) 0.004(3) 0.016(3)
C6 0.080(5) 0.045(4) 0.040(4) -0.022(4) -0.003(4) 0.000(3)
C7 0.047(4) 0.051(4) 0.043(4) -0.010(3) 0.015(3) 0.009(3)
C8 0.026(2) 0.022(2) 0.024(3) -0.0028(18) -0.0007(19) 0.0027(19)
C9 0.027(3) 0.031(3) 0.034(3) 0.003(2) 0.001(2) 0.005(2)
C10 0.029(3) 0.048(4) 0.059(4) 0.009(3) -0.012(3) 0.006(3)
C11 0.022(3) 0.058(4) 0.089(6) 0.003(5) 0.001(3) 0.001(3)
C12 0.029(3) 0.047(4) 0.052(4) 0.005(3) 0.010(3) -0.006(3)
C13 0.029(3) 0.029(3) 0.026(3) -0.002(2) -0.001(2) -0.001(2)
C14 0.034(3) 0.025(3) 0.021(3) 0.001(2) 0.006(2) -0.004(2)
N1 0.031(2) 0.026(2) 0.020(2) 0.0006(17) 0.0016(18) -0.0010(18)
C15 0.049(3) 0.032(3) 0.027(3) -0.006(2) 0.006(3) -0.008(2)
C16 0.033(3) 0.044(3) 0.041(3) 0.017(3) 0.003(3) 0.008(3)
P2 0.0234(6) 0.0180(5) 0.0174(6) -0.0017(5) 0.0004(5) 0.0003(4)
C17 0.017(2) 0.021(2) 0.021(2) -0.0025(19) 0.0007(18) -0.0014(18)
Si3 0.0299(7) 0.0212(7) 0.0232(7) 0.0029(6) 0.0012(6) 0.0006(6)
C18 0.031(3) 0.033(3) 0.036(3) 0.005(2) -0.001(2) 0.004(2)
C19 0.027(3) 0.033(3) 0.061(4) 0.003(3) 0.001(3) -0.004(2)
C20 0.064(4) 0.031(3) 0.025(3) 0.007(2) 0.002(3) 0.008(3)
Si4 0.0211(7) 0.0289(7) 0.0256(7) -0.0007(6) 0.0014(6) 0.0025(5)
C21 0.027(3) 0.046(4) 0.052(4) -0.009(3) 0.012(3) 0.000(3)
C22 0.035(3) 0.056(4) 0.038(4) 0.006(3) -0.002(3) 0.015(3)
C23 0.041(3) 0.028(3) 0.029(3) -0.007(2) 0.005(3) 0.008(2)
C24 0.024(2) 0.016(2) 0.024(2) -0.0007(19) 0.003(2) -0.0024(19)
C25 0.032(3) 0.026(2) 0.028(3) 0.002(2) -0.006(2) 0.004(2)
C26 0.041(3) 0.025(3) 0.043(3) -0.002(2) -0.002(3) 0.007(2)
C27 0.045(3) 0.018(3) 0.047(4) -0.010(2) -0.003(3) 0.004(2)
C28 0.031(3) 0.030(3) 0.035(3) -0.009(2) -0.005(2) -0.005(2)
C29 0.022(2) 0.021(2) 0.028(3) -0.001(2) 0.004(2) 0.0003(19)
C30 0.025(3) 0.025(3) 0.020(3) 0.0002(19) -0.0031(19) 0.005(2)
N2 0.025(2) 0.027(2) 0.025(2) -0.0052(18) -0.0015(18) -0.0011(17)
C31 0.036(3) 0.030(3) 0.051(4) 0.001(3) -0.015(3) 0.004(2)
C32 0.029(3) 0.041(3) 0.040(3) -0.012(3) 0.003(3) 0.001(3)
Li1 0.052(6) 0.022(4) 0.034(5) -0.001(4) -0.001(5) 0.003(4)
O1 0.056(3) 0.042(3) 0.042(3) 0.003(2) 0.001(2) -0.005(2)
C33X 0.057(11) 0.046(9) 0.045(11) 0.010(7) -0.014(7) -0.011(7)
C34X 0.089(17) 0.117(19) 0.070(18) -0.005(15) 0.008(13) 0.032(16)
C33Y 0.083(13) 0.059(9) 0.068(12) 0.010(8) 0.000(9) -0.017(8)
C34Y 0.103(16) 0.075(12) 0.093(18) 0.037(11) -0.022(13) 0.016(11)
C35 0.049(5) 0.048(4) 0.130(9) 0.006(5) 0.002(5) 0.008(4)
C36 0.077(7) 0.064(6) 0.134(9) -0.007(6) 0.010(6) -0.021(5)
I1 0.02803(16) 0.04245(18) 0.02700(16) -0.00492(17) 0.00374(15) -0.00537(15)
I2 0.03205(18) 0.04015(19) 0.0425(2) -0.00060(19) 0.01002(17) -0.00186(16)
Li2 0.045(5) 0.025(5) 0.043(5) -0.006(5) 0.005(5) -0.004(4)
O2 0.036(2) 0.038(2) 0.062(3) -0.015(2) 0.005(2) -0.0046(19)
C37 0.041(4) 0.061(5) 0.093(6) -0.035(5) -0.008(4) -0.013(4)
C38 0.075(6) 0.053(5) 0.141(11) -0.007(6) -0.003(6) 0.015(4)
C39 0.047(4) 0.043(4) 0.106(7) -0.008(4) 0.005(4) -0.018(3)
C40 0.037(4) 0.056(5) 0.148(9) -0.018(6) 0.011(5) -0.002(4)
O3 0.064(3) 0.040(3) 0.043(3) 0.005(2) 0.001(2) 0.007(2)
C41 0.077(6) 0.061(5) 0.058(5) 0.025(4) 0.006(4) 0.007(4)
C42 0.123(9) 0.080(6) 0.065(6) 0.010(5) 0.009(6) 0.023(6)
C43 0.101(7) 0.049(5) 0.068(6) 0.019(4) 0.003(5) 0.011(5)
C44 0.083(7) 0.094(7) 0.098(8) 0.011(6) -0.045(6) 0.011(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'
Si Si 0.0817 0.0704 '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'
Ge Ge 0.1547 1.8001 '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'
Li Li -0.0003 0.0001 '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'
|
1100901.cif | #------------------------------------------------------------------------------
#$Date: 2018-09-01 22:33:33 +0300 (Sat, 01 Sep 2018) $
#$Revision: 210321 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/09/1100901.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_1100901
loop_
_publ_author_name
'Izod, Keith'
'McFarlane, William'
'Allen, Ben'
'Clegg, William'
'Harrington, Ross W.'
_publ_section_title
;
An Intramolecularly Base-Stabilized Diphosphagermylene and Two Unusual
Germanium(II) Ate Complexes: A Structural, NMR, and DFT Study
;
_journal_coden_ASTM ORGND7
_journal_issue 9
_journal_name_full Organometallics
_journal_page_first 2157
_journal_page_last 2167
_journal_paper_doi 10.1021/om0501125
_journal_volume 24
_journal_year 2005
_chemical_formula_moiety 'C48 H93 Ge K N3 P3 Si6'
_chemical_formula_sum 'C48 H93 Ge K N3 P3 Si6'
_chemical_formula_weight 1085.39
_space_group_IT_number 205
_symmetry_cell_setting cubic
_symmetry_space_group_name_Hall '-P 2ac 2ab 3'
_symmetry_space_group_name_H-M 'P a -3'
_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 90.00
_cell_formula_units_Z 8
_cell_length_a 23.4873(5)
_cell_length_b 23.4873(5)
_cell_length_c 23.4873(5)
_cell_measurement_reflns_used 30903
_cell_measurement_temperature 150(2)
_cell_measurement_theta_max 26.37
_cell_measurement_theta_min 2.50
_cell_volume 12956.8(5)
_diffrn_ambient_temperature 150(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type 'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method 'thin-slice \w 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 0.0556
_diffrn_reflns_av_sigmaI/netI 0.0123
_diffrn_reflns_limit_h_max 29
_diffrn_reflns_limit_h_min -29
_diffrn_reflns_limit_k_max 29
_diffrn_reflns_limit_k_min -29
_diffrn_reflns_limit_l_max 29
_diffrn_reflns_limit_l_min -29
_diffrn_reflns_number 202438
_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 0
_exptl_absorpt_coefficient_mu 0.753
_exptl_absorpt_correction_T_max 0.864
_exptl_absorpt_correction_T_min 0.806
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details SADABS
_exptl_crystal_colour red
_exptl_crystal_density_diffrn 1.113
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 4656
_exptl_crystal_size_max 0.30
_exptl_crystal_size_mid 0.30
_exptl_crystal_size_min 0.20
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.167
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 195
_refine_ls_number_reflns 4426
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.167
_refine_ls_R_factor_all 0.0548
_refine_ls_R_factor_gt 0.0402
_refine_ls_shift/su_max 0.256
_refine_ls_shift/su_mean 0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0617P)^2^+19.0115P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1185
_refine_ls_wR_factor_ref 0.1358
_reflns_number_gt 3729
_reflns_number_total 4426
_reflns_threshold_expression I>2\s(I)
_cod_database_code 1100901
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'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
'-z, -x, -y'
'-z-1/2, x-1/2, y'
'z-1/2, x, -y-1/2'
'z, -x-1/2, y-1/2'
'-y, -z, -x'
'y, -z-1/2, x-1/2'
'-y-1/2, z-1/2, x'
'y-1/2, z, -x-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
Ge Ge 0.819965(11) 0.319965(11) 0.180035(11) 0.02177(15) Uani 1 3 d S . .
K K 0.91096(2) 0.41096(2) 0.08904(2) 0.0253(2) Uani 1 3 d S . .
Si1 Si 0.89370(4) 0.17590(3) 0.23722(4) 0.0323(2) Uani 1 1 d . . .
Si2 Si 1.01585(4) 0.22601(4) 0.20647(4) 0.0345(2) Uani 1 1 d . . .
P P 0.91576(3) 0.28923(3) 0.15138(3) 0.02098(17) Uani 1 1 d . . .
N N 0.98000(11) 0.33927(12) 0.01621(11) 0.0333(6) Uani 1 1 d . . .
C1 C 0.93618(12) 0.23989(11) 0.21140(12) 0.0254(6) Uani 1 1 d . . .
H1 H 0.9340 0.2659 0.2451 0.030 Uiso 1 1 calc R . .
C2 C 0.90495(19) 0.17005(19) 0.31620(15) 0.0530(10) Uani 1 1 d . . .
H2A H 0.8899 0.2041 0.3350 0.079 Uiso 1 1 calc R . .
H2B H 0.9458 0.1667 0.3242 0.079 Uiso 1 1 calc R . .
H2C H 0.8851 0.1363 0.3306 0.079 Uiso 1 1 calc R . .
C3 C 0.91822(17) 0.10833(14) 0.20289(17) 0.0468(9) Uani 1 1 d . . .
H3A H 0.8951 0.0765 0.2167 0.070 Uiso 1 1 calc R . .
H3B H 0.9583 0.1016 0.2125 0.070 Uiso 1 1 calc R . .
H3C H 0.9142 0.1115 0.1615 0.070 Uiso 1 1 calc R . .
C4 C 0.81431(15) 0.17780(15) 0.23068(18) 0.0473(9) Uani 1 1 d . . .
H4A H 0.7975 0.1502 0.2571 0.071 Uiso 1 1 calc R . .
H4B H 0.8033 0.1681 0.1916 0.071 Uiso 1 1 calc R . .
H4C H 0.8005 0.2161 0.2399 0.071 Uiso 1 1 calc R . .
C5 C 1.03731(16) 0.18207(16) 0.14345(18) 0.0514(9) Uani 1 1 d . . .
H5A H 1.0147 0.1933 0.1103 0.077 Uiso 1 1 calc R . .
H5B H 1.0307 0.1417 0.1517 0.077 Uiso 1 1 calc R . .
H5C H 1.0778 0.1882 0.1354 0.077 Uiso 1 1 calc R . .
C6 C 1.04355(16) 0.18671(17) 0.27067(17) 0.0508(9) Uani 1 1 d . . .
H6A H 1.0246 0.1497 0.2735 0.076 Uiso 1 1 calc R . .
H6B H 1.0358 0.2090 0.3051 0.076 Uiso 1 1 calc R . .
H6C H 1.0847 0.1810 0.2668 0.076 Uiso 1 1 calc R . .
C7 C 1.05448(16) 0.29574(16) 0.20480(18) 0.0492(9) Uani 1 1 d . . .
H7A H 1.0956 0.2888 0.2052 0.074 Uiso 1 1 calc R . .
H7B H 1.0439 0.3183 0.2382 0.074 Uiso 1 1 calc R . .
H7C H 1.0442 0.3165 0.1701 0.074 Uiso 1 1 calc R . .
C8 C 0.90534(12) 0.24114(11) 0.08962(12) 0.0255(6) Uani 1 1 d . . .
C9 C 0.86135(14) 0.20096(12) 0.08822(14) 0.0337(7) Uani 1 1 d . . .
H9 H 0.8352 0.1994 0.1190 0.040 Uiso 1 1 calc R . .
C10 C 0.85485(17) 0.16348(15) 0.04325(17) 0.0473(9) Uani 1 1 d . . .
H10 H 0.8244 0.1369 0.0434 0.057 Uiso 1 1 calc R . .
C11 C 0.89260(19) 0.16460(17) -0.00189(17) 0.0556(10) Uani 1 1 d . . .
H11 H 0.8887 0.1386 -0.0326 0.067 Uiso 1 1 calc R . .
C12 C 0.93587(17) 0.20399(15) -0.00147(15) 0.0453(8) Uani 1 1 d . . .
H12 H 0.9619 0.2047 -0.0324 0.054 Uiso 1 1 calc R . .
C13 C 0.94279(13) 0.24276(12) 0.04270(12) 0.0310(6) Uani 1 1 d . . .
C14 C 0.99300(13) 0.28268(13) 0.03989(13) 0.0332(6) Uani 1 1 d . . .
H14A H 1.0085 0.2876 0.0788 0.040 Uiso 1 1 calc R . .
H14B H 1.0231 0.2648 0.0164 0.040 Uiso 1 1 calc R . .
C15 C 1.03105(16) 0.37408(17) 0.02015(18) 0.0514(9) Uani 1 1 d . . .
H15A H 1.0612 0.3572 -0.0033 0.077 Uiso 1 1 calc R . .
H15B H 1.0436 0.3759 0.0599 0.077 Uiso 1 1 calc R . .
H15C H 1.0227 0.4126 0.0065 0.077 Uiso 1 1 calc R . .
C16 C 0.96272(16) 0.33483(17) -0.04341(14) 0.0465(8) Uani 1 1 d . . .
H16A H 0.9543 0.3729 -0.0583 0.070 Uiso 1 1 calc R . .
H16B H 0.9287 0.3109 -0.0463 0.070 Uiso 1 1 calc R . .
H16C H 0.9936 0.3177 -0.0656 0.070 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
Ge 0.02177(15) 0.02177(15) 0.02177(15) 0.00194(10) 0.00194(10) -0.00194(10)
K 0.0253(2) 0.0253(2) 0.0253(2) 0.0034(2) 0.0034(2) -0.0034(2)
Si1 0.0370(5) 0.0249(4) 0.0350(5) 0.0092(3) -0.0045(3) -0.0036(3)
Si2 0.0271(4) 0.0316(4) 0.0448(5) 0.0084(4) -0.0102(4) -0.0003(3)
P 0.0224(3) 0.0184(3) 0.0221(3) 0.0012(2) -0.0007(2) 0.0000(2)
N 0.0315(13) 0.0386(14) 0.0298(13) 0.0017(11) 0.0070(10) -0.0009(11)
C1 0.0285(14) 0.0216(13) 0.0261(13) 0.0030(10) -0.0054(11) -0.0006(10)
C2 0.062(2) 0.061(2) 0.0365(19) 0.0144(17) -0.0016(17) -0.0064(19)
C3 0.055(2) 0.0267(16) 0.058(2) 0.0034(15) -0.0095(17) -0.0032(15)
C4 0.0382(18) 0.0411(19) 0.063(2) 0.0228(17) 0.0005(16) -0.0114(14)
C5 0.0409(19) 0.048(2) 0.066(3) 0.0043(18) 0.0014(18) 0.0158(16)
C6 0.045(2) 0.049(2) 0.058(2) 0.0168(17) -0.0231(17) -0.0026(16)
C7 0.0392(19) 0.047(2) 0.061(2) 0.0112(17) -0.0156(17) -0.0121(16)
C8 0.0297(14) 0.0201(12) 0.0267(13) -0.0010(10) -0.0061(11) 0.0036(10)
C9 0.0382(16) 0.0241(14) 0.0388(16) 0.0015(12) -0.0054(13) -0.0023(12)
C10 0.053(2) 0.0314(16) 0.058(2) -0.0057(15) -0.0158(18) -0.0109(15)
C11 0.073(3) 0.046(2) 0.048(2) -0.0233(17) -0.0084(19) -0.0005(19)
C12 0.058(2) 0.0452(19) 0.0327(17) -0.0152(15) 0.0003(15) 0.0031(16)
C13 0.0346(15) 0.0302(15) 0.0282(14) -0.0031(12) -0.0028(12) 0.0042(12)
C14 0.0285(14) 0.0424(17) 0.0286(14) -0.0014(13) 0.0051(12) 0.0059(13)
C15 0.0419(19) 0.053(2) 0.059(2) 0.0047(18) 0.0096(17) -0.0116(17)
C16 0.050(2) 0.058(2) 0.0306(17) 0.0076(15) 0.0032(15) 0.0016(17)
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'
Si Si 0.0817 0.0704 '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'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100902.cif | #------------------------------------------------------------------------------
#$Date: 2022-09-14 17:31:13 +0300 (Wed, 14 Sep 2022) $
#$Revision: 277831 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/09/1100902.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_1100902
loop_
_publ_author_name
'Yamada, Junji'
'Fujiki, Michiya'
'Nomura, Kotohiro'
_publ_section_title
;
A Vanadium(V) Alkylidene Complex Exhibiting Remarkable Catalytic
Activity for Ring-Opening Metathesis Polymerization (ROMP)
;
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2248
_journal_page_last 2250
_journal_paper_doi 10.1021/om0501834
_journal_volume 24
_journal_year 2005
_chemical_formula_moiety 'C17 H27 Cl2 N2 V '
_chemical_formula_sum 'C17 H27 Cl2 N2 V'
_chemical_formula_weight 381.26
_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 101.19(3)
_cell_angle_beta 111.44(4)
_cell_angle_gamma 101.37(3)
_cell_formula_units_Z 2
_cell_length_a 9.814(4)
_cell_length_b 9.861(4)
_cell_length_c 11.505(5)
_cell_measurement_reflns_used 10365
_cell_measurement_temperature 243.1
_cell_measurement_theta_max 27.5
_cell_measurement_theta_min 2.0
_cell_volume 971.9(7)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.9966
_diffrn_measured_fraction_theta_max 0.9966
_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 0.037
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -12
_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 9512
_diffrn_reflns_theta_full 27.48
_diffrn_reflns_theta_max 27.48
_exptl_absorpt_coefficient_mu 0.783
_exptl_absorpt_correction_T_max 0.791
_exptl_absorpt_correction_T_min 0.791
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
Higashi, T. (1995). Program for Absorption Correction.
Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour brown
_exptl_crystal_density_diffrn 1.303
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 400.00
_exptl_crystal_size_max 0.67
_exptl_crystal_size_mid 0.50
_exptl_crystal_size_min 0.30
_refine_diff_density_max 0.24
_refine_diff_density_min -0.65
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.056
_refine_ls_hydrogen_treatment mixed
_refine_ls_number_parameters 295
_refine_ls_number_reflns 3819
_refine_ls_R_factor_gt 0.0360
_refine_ls_shift/su_max 0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Chebychev polynomial with 3 parameters (Carruthers & Watkin, 1979)
19.2628 0.2819 15.7880
;
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_ref 0.0450
_reflns_number_gt 3819
_reflns_number_total 4443
_reflns_threshold_expression F^2^>2.0\s(F^2^)
_cod_original_formula_sum 'C17 H27 Cl2 N2 V '
_cod_database_code 1100902
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
V(1) V 0.95458(3) 0.37802(2) 1.31172(3) 0.03650(7) Uani 1.00 1 d . . .
Cl(1) Cl 0.96971(5) 0.60837(4) 1.40645(4) 0.0457(1) Uani 1.00 1 d . . .
Cl(2) Cl 1.16963(4) 0.31305(5) 1.35910(4) 0.0469(1) Uani 1.00 1 d . . .
N(1) N 0.8963(1) 0.3705(1) 1.1551(1) 0.0395(3) Uani 1.00 1 d . . .
N(2) N 0.7968(1) 0.2392(1) 1.2977(1) 0.0353(3) Uani 1.00 1 d . . .
C(1) C 0.8506(2) 0.3660(1) 1.0266(2) 0.0398(4) Uani 1.00 1 d . . .
C(2) C 0.7643(2) 0.4582(2) 0.9789(2) 0.0462(4) Uani 1.00 1 d . . .
C(3) C 0.7238(2) 0.4551(2) 0.8496(2) 0.0582(5) Uani 1.00 1 d . . .
C(4) C 0.7647(2) 0.3659(2) 0.7697(2) 0.0610(5) Uani 1.00 1 d . . .
C(5) C 0.8471(2) 0.2745(2) 0.8164(2) 0.0555(5) Uani 1.00 1 d . . .
C(6) C 0.8913(2) 0.2724(2) 0.9447(2) 0.0455(4) Uani 1.00 1 d . . .
C(7) C 0.7224(3) 0.5569(2) 1.0670(2) 0.0623(6) Uani 1.00 1 d . . .
C(8) C 0.9817(3) 0.1751(2) 0.9959(2) 0.0579(6) Uani 1.00 1 d . . .
C(9) C 0.6912(1) 0.1425(1) 1.2963(1) 0.0329(3) Uani 1.00 1 d . . .
C(10) C 0.5483(2) 0.1844(2) 1.2996(1) 0.0404(4) Uani 1.00 1 d . . .
C(11) C 0.4874(3) 0.1209(3) 1.3884(2) 0.0586(6) Uani 1.00 1 d . . .
C(12) C 0.4232(3) 0.1342(4) 1.1608(2) 0.0763(7) Uani 1.00 1 d . . .
C(13) C 0.5873(2) 0.3491(2) 1.3496(3) 0.0573(6) Uani 1.00 1 d . . .
C(14) C 0.7154(2) -0.0090(2) 1.2940(2) 0.0441(4) Uani 1.00 1 d . . .
C(15) C 0.7738(3) -0.0175(3) 1.4350(3) 0.0689(7) Uani 1.00 1 d . . .
C(16) C 0.5716(3) -0.1347(2) 1.2054(3) 0.0739(7) Uani 1.00 1 d . . .
C(17) C 0.8386(3) -0.0250(2) 1.2458(3) 0.0635(6) Uani 1.00 1 d . . .
H(1) H 0.665(3) 0.521(3) 0.815(2) 0.065(6) Uiso 1.00 1 c . . .
H(2) H 0.737(3) 0.362(3) 0.682(3) 0.071(7) Uiso 1.00 1 c . . .
H(3) H 0.874(3) 0.212(2) 0.764(2) 0.048(5) Uiso 1.00 1 c . . .
H(4) H 0.678(4) 0.618(4) 1.032(4) 0.11(1) Uiso 1.00 1 c . . .
H(5) H 0.6531 0.5013 1.0920 0.077 Uiso 1.00 1 c R . .
H(6) H 0.8122 0.6136 1.1426 0.077 Uiso 1.00 1 c R . .
H(7) H 1.077(3) 0.224(3) 1.058(2) 0.058(6) Uiso 1.00 1 c . . .
H(8) H 0.9308 0.1181 1.0340 0.078 Uiso 1.00 1 c R . .
H(9) H 0.9918 0.1136 0.9269 0.078 Uiso 1.00 1 c R . .
H(10) H 0.461(3) 0.011(3) 1.366(3) 0.086(9) Uiso 1.00 1 c . . .
H(11) H 0.399(3) 0.156(3) 1.390(3) 0.076(7) Uiso 1.00 1 c . . .
H(12) H 0.568(3) 0.154(3) 1.476(3) 0.070(7) Uiso 1.00 1 c . . .
H(13) H 0.334(5) 0.162(4) 1.152(4) 0.11(1) Uiso 1.00 1 c . . .
H(14) H 0.378(4) 0.025(3) 1.125(3) 0.081(8) Uiso 1.00 1 c . . .
H(15) H 0.465(3) 0.172(3) 1.108(3) 0.074(7) Uiso 1.00 1 c . . .
H(16) H 0.619(3) 0.398(2) 1.300(2) 0.054(6) Uiso 1.00 1 c . . .
H(17) H 0.497(3) 0.378(3) 1.357(3) 0.072(7) Uiso 1.00 1 c . . .
H(18) H 0.672(3) 0.394(3) 1.441(3) 0.074(7) Uiso 1.00 1 c . . .
H(19) H 0.801(3) -0.105(3) 1.428(3) 0.082(8) Uiso 1.00 1 c . . .
H(20) H 0.695(4) -0.026(3) 1.466(3) 0.091(9) Uiso 1.00 1 c . . .
H(21) H 0.876(4) 0.074(4) 1.498(4) 0.11(1) Uiso 1.00 1 c . . .
H(22) H 0.484(4) -0.132(3) 1.228(3) 0.089(9) Uiso 1.00 1 c . . .
H(23) H 0.598(3) -0.231(3) 1.210(3) 0.084(8) Uiso 1.00 1 c . . .
H(24) H 0.526(4) -0.139(4) 1.111(4) 0.10(1) Uiso 1.00 1 c . . .
H(25) H 0.936(3) 0.045(3) 1.297(3) 0.069(7) Uiso 1.00 1 c . . .
H(26) H 0.815(3) -0.009(3) 1.165(3) 0.061(6) Uiso 1.00 1 c . . .
H(27) H 0.853(5) -0.128(4) 1.243(4) 0.12(1) Uiso 1.00 1 c . . .
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)
;
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)
;
V V 0.300 0.529
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
|
1100903.cif | #------------------------------------------------------------------------------
#$Date: 2022-09-14 17:31:13 +0300 (Wed, 14 Sep 2022) $
#$Revision: 277831 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/09/1100903.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_1100903
loop_
_publ_author_name
'Yamada, Junji'
'Fujiki, Michiya'
'Nomura, Kotohiro'
_publ_section_title
;
A Vanadium(V) Alkylidene Complex Exhibiting Remarkable Catalytic
Activity for Ring-Opening Metathesis Polymerization (ROMP)
;
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2248
_journal_page_last 2250
_journal_paper_doi 10.1021/om0501834
_journal_volume 24
_journal_year 2005
_chemical_formula_moiety 'C20 H36 Cl2 N2 P V '
_chemical_formula_sum 'C20 H36 Cl2 N2 P V'
_chemical_formula_weight 457.34
_chemical_melting_point ?
_space_group_IT_number 14
_space_group_name_Hall '-P 2ybc'
_space_group_name_H-M_alt 'P 1 21/c 1'
_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 95.857(4)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 9.838(1)
_cell_length_b 12.565(2)
_cell_length_c 20.509(3)
_cell_measurement_reflns_used 14391
_cell_measurement_temperature 243.1
_cell_measurement_theta_max 27.5
_cell_measurement_theta_min 1.6
_cell_volume 2521.9(6)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.9214
_diffrn_measured_fraction_theta_max 0.9214
_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 ?
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min 0
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_l_max 26
_diffrn_reflns_limit_l_min -26
_diffrn_reflns_number 5592
_diffrn_reflns_theta_full 27.49
_diffrn_reflns_theta_max 27.49
_exptl_absorpt_coefficient_mu 0.675
_exptl_absorpt_correction_T_max 0.800
_exptl_absorpt_correction_T_min 0.800
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
Higashi, T. (1995). Program for Absorption Correction.
Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour brown
_exptl_crystal_density_diffrn 1.204
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 968.00
_exptl_crystal_size_max 0.42
_exptl_crystal_size_mid 0.33
_exptl_crystal_size_min 0.33
_refine_diff_density_max 0.52
_refine_diff_density_min -0.33
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.064
_refine_ls_hydrogen_treatment refall
_refine_ls_number_parameters 286
_refine_ls_number_reflns 2912
_refine_ls_R_factor_gt 0.0570
_refine_ls_shift/su_max 0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Chebychev polynomial with 3 parameters (Carruthers & Watkin, 1979)
0.1844 0.1470 0.0211
;
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_ref 0.0680
_reflns_number_gt 2912
_reflns_number_total 5398
_reflns_threshold_expression F^2^>2.0\s(F^2^)
_cod_original_formula_sum 'C20 H36 Cl2 N2 P V '
_cod_database_code 1100903
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
V(1) V 0.25896(7) 0.22387(6) 0.61893(3) 0.0365(2) Uani 1.00 1 d . . .
Cl(1) Cl 0.1138(1) 0.1022(1) 0.66058(7) 0.0608(4) Uani 1.00 1 d . . .
Cl(2) Cl 0.4525(1) 0.2961(1) 0.67386(7) 0.0692(4) Uani 1.00 1 d . . .
P(1) P 0.4086(1) 0.0601(1) 0.62988(6) 0.0565(4) Uani 1.00 1 d . . .
N(1) N 0.2666(4) 0.2218(3) 0.5389(1) 0.0375(9) Uani 1.00 1 d . . .
N(2) N 0.1443(4) 0.3378(3) 0.6266(2) 0.042(1) Uani 1.00 1 d . . .
C(1) C 0.2728(5) 0.2224(3) 0.4716(2) 0.041(1) Uani 1.00 1 d . . .
C(2) C 0.3773(5) 0.2821(4) 0.4462(2) 0.052(1) Uani 1.00 1 d . . .
C(3) C 0.3763(8) 0.2817(5) 0.3774(3) 0.078(2) Uani 1.00 1 d . . .
C(4) C 0.2853(9) 0.2261(6) 0.3382(3) 0.090(2) Uani 1.00 1 d . . .
C(5) C 0.1848(8) 0.1681(6) 0.3636(3) 0.081(2) Uani 1.00 1 d . . .
C(6) C 0.1773(5) 0.1645(4) 0.4314(2) 0.051(1) Uani 1.00 1 d . . .
C(7) C 0.4764(9) 0.3435(7) 0.4895(4) 0.081(2) Uani 1.00 1 d . . .
C(8) C 0.0686(8) 0.1026(6) 0.4603(4) 0.081(2) Uani 1.00 1 d . . .
C(9) C 0.5696(8) 0.0714(6) 0.5961(5) 0.097(3) Uani 1.00 1 d . . .
C(10) C 0.3337(8) -0.0592(5) 0.5888(4) 0.094(3) Uani 1.00 1 d . . .
C(11) C 0.453(1) 0.0154(8) 0.7126(4) 0.108(3) Uani 1.00 1 d . . .
C(12) C 0.0616(5) 0.4129(3) 0.6326(2) 0.041(1) Uani 1.00 1 d . . .
C(13) C -0.0914(6) 0.3825(4) 0.6351(3) 0.064(2) Uani 1.00 1 d . . .
C(14) C 0.1225(6) 0.5256(4) 0.6425(3) 0.066(2) Uani 1.00 1 d . . .
C(15) C -0.1282(7) 0.2919(6) 0.5872(4) 0.079(2) Uani 1.00 1 d . . .
C(16) C -0.1006 0.3407 0.7065 0.096 Uani 1.00 1 d R . .
C(17) C -0.1956(9) 0.4708(7) 0.6199(6) 0.151(4) Uani 1.00 1 d . . .
C(18) C 0.116(1) 0.5610(9) 0.7111(5) 0.200(6) Uani 1.00 1 d . . .
C(19) C 0.046(1) 0.6021(7) 0.5886(7) 0.175(5) Uani 1.00 1 d . . .
C(20) C 0.2660(8) 0.5285(6) 0.6270(5) 0.115(3) Uani 1.00 1 d . . .
H(1) H 0.4422 0.3240 0.3586 0.096 Uiso 1.00 1 c R . .
H(2) H 0.2914 0.2261 0.2922 0.109 Uiso 1.00 1 c R . .
H(3) H 0.1199 0.1299 0.3352 0.095 Uiso 1.00 1 c R . .
H(4) H 0.52(1) 0.317(8) 0.515(5) 0.12(4) Uiso 1.00 1 c . . .
H(5) H 0.5461 0.3701 0.4651 0.099 Uiso 1.00 1 c R . .
H(6) H 0.4312 0.4013 0.5079 0.099 Uiso 1.00 1 c R . .
H(7) H 0.101(9) 0.063(7) 0.491(4) 0.13(3) Uiso 1.00 1 c . . .
H(8) H 0.0009 0.1500 0.4731 0.096 Uiso 1.00 1 c R . .
H(9) H 0.0278 0.0539 0.4287 0.096 Uiso 1.00 1 c R . .
H(10) H 0.550(7) 0.093(5) 0.549(3) 0.09(2) Uiso 1.00 1 c . . .
H(11) H 0.6177 0.1310 0.6154 0.119 Uiso 1.00 1 c R . .
H(12) H 0.6223 0.0088 0.6051 0.119 Uiso 1.00 1 c R . .
H(14) H 0.3894 -0.1192 0.6010 0.113 Uiso 1.00 1 c R . .
H(15) H 0.2449 -0.0701 0.6018 0.113 Uiso 1.00 1 c R . .
H(16) H 0.51(1) -0.04(1) 0.717(7) 0.23(6) Uiso 1.00 1 c . . .
H(17) H 0.5101 0.0675 0.7348 0.128 Uiso 1.00 1 c R . .
H(18) H 0.3724 0.0072 0.7343 0.128 Uiso 1.00 1 c R . .
H(19) H -0.122(8) 0.315(6) 0.545(4) 0.11(3) Uiso 1.00 1 c . . .
H(20) H -0.0810 0.2291 0.6020 0.093 Uiso 1.00 1 c R . .
H(21) H -0.2239 0.2795 0.5841 0.093 Uiso 1.00 1 c R . .
H(23) H -0.1929 0.3261 0.7132 0.118 Uiso 1.00 1 c R . .
H(24) H -0.0482 0.2773 0.7126 0.118 Uiso 1.00 1 c R . .
H(25) H -0.2789 0.4405 0.6009 0.180 Uiso 1.00 1 c R . .
H(26) H -0.1626 0.5199 0.5900 0.180 Uiso 1.00 1 c R . .
H(27) H -0.2110 0.5066 0.6592 0.180 Uiso 1.00 1 c R . .
H(29) H 0.2031 0.5591 0.7358 0.249 Uiso 1.00 1 c R . .
H(30) H 0.0819 0.6318 0.7099 0.249 Uiso 1.00 1 c R . .
H(31) H 0.0927 0.6019 0.5503 0.208 Uiso 1.00 1 c R . .
H(32) H 0.0445 0.6723 0.6057 0.208 Uiso 1.00 1 c R . .
H(33) H -0.0452 0.5780 0.5778 0.208 Uiso 1.00 1 c R . .
H(34) H 0.3257 0.5122 0.6651 0.142 Uiso 1.00 1 c R . .
H(35) H 0.2875 0.5970 0.6114 0.142 Uiso 1.00 1 c R . .
H(36) H 0.2764 0.4769 0.5941 0.142 Uiso 1.00 1 c R . .
H(28) H 0.0597 0.5142 0.7329 0.249 Uiso 1.00 1 c R . .
H(22) H -0.0649 0.3929 0.7371 0.118 Uiso 1.00 1 c R . .
H(13) H 0.3287 -0.0493 0.5427 0.113 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)
;
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)
;
P P 0.102 0.094
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
V V 0.300 0.529
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
|
1100904.cif | #------------------------------------------------------------------------------
#$Date: 2022-09-14 17:31:13 +0300 (Wed, 14 Sep 2022) $
#$Revision: 277831 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/09/1100904.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_1100904
loop_
_publ_author_name
'Yamada, Junji'
'Fujiki, Michiya'
'Nomura, Kotohiro'
_publ_section_title
;
A Vanadium(V) Alkylidene Complex Exhibiting Remarkable Catalytic
Activity for Ring-Opening Metathesis Polymerization (ROMP)
;
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2248
_journal_page_last 2250
_journal_paper_doi 10.1021/om0501834
_journal_volume 24
_journal_year 2005
_chemical_formula_moiety 'C23 H43 Cl2 N2 P2 V '
_chemical_formula_sum 'C23 H43 Cl2 N2 P2 V'
_chemical_formula_weight 531.40
_chemical_melting_point ?
_space_group_IT_number 15
_space_group_name_Hall '-C 2yc'
_space_group_name_H-M_alt 'C 1 2/c 1'
_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 109.683(3)
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 29.520(3)
_cell_length_b 10.9241(5)
_cell_length_c 18.578(1)
_cell_measurement_reflns_used 20367
_cell_measurement_temperature 243.1
_cell_measurement_theta_max 27.5
_cell_measurement_theta_min 1.5
_cell_volume 5641.0(7)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.9966
_diffrn_measured_fraction_theta_max 0.9966
_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 ?
_diffrn_reflns_limit_h_max 38
_diffrn_reflns_limit_h_min 0
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_limit_l_min -24
_diffrn_reflns_number 6789
_diffrn_reflns_theta_full 27.48
_diffrn_reflns_theta_max 27.48
_exptl_absorpt_coefficient_mu 0.667
_exptl_absorpt_correction_T_max 0.917
_exptl_absorpt_correction_T_min 0.917
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
Higashi, T. (1995). Program for Absorption Correction.
Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour red
_exptl_crystal_density_diffrn 1.251
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 2256.00
_exptl_crystal_size_max 0.33
_exptl_crystal_size_mid 0.33
_exptl_crystal_size_min 0.13
_refine_diff_density_max 0.64
_refine_diff_density_min -0.32
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.094
_refine_ls_hydrogen_treatment refall
_refine_ls_number_parameters 347
_refine_ls_number_reflns 4052
_refine_ls_R_factor_gt 0.0430
_refine_ls_shift/su_max 0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Chebychev polynomial with 3 parameters (Carruthers & Watkin, 1979)
0.1433 0.1257 0.0305
;
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_ref 0.0480
_reflns_number_gt 4052
_reflns_number_total 6448
_reflns_threshold_expression F^2^>2.0\s(F^2^)
_cod_original_formula_sum 'C23 H43 Cl2 N2 P2 V '
_cod_database_code 1100904
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +X,+Y,+Z
2 -X,+Y,1/2-Z
3 -X,-Y,-Z
4 +X,-Y,1/2+Z
5 1/2+X,1/2+Y,+Z
6 1/2-X,1/2+Y,1/2-Z
7 1/2-X,1/2-Y,-Z
8 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
V(1) V 0.61663(1) 0.20092(4) 0.58471(2) 0.0292(1) Uani 1.00 1 d . . .
Cl(1) Cl 0.56840(2) 0.04786(6) 0.50503(4) 0.0424(2) Uani 1.00 1 d . . .
Cl(2) Cl 0.64000(3) 0.32338(7) 0.69690(4) 0.0444(2) Uani 1.00 1 d . . .
P(1) P 0.60019(3) 0.04666(7) 0.68304(4) 0.0426(2) Uani 1.00 1 d . . .
P(2) P 0.53576(2) 0.27008(6) 0.58667(4) 0.0368(2) Uani 1.00 1 d . . .
N(1) N 0.61361(8) 0.3074(2) 0.5182(1) 0.0339(5) Uani 1.00 1 d . . .
N(2) N 0.67579(8) 0.1308(2) 0.5990(1) 0.0357(5) Uani 1.00 1 d . . .
C(1) C 0.60587(9) 0.3965(3) 0.4633(2) 0.0381(7) Uani 1.00 1 d . . .
C(2) C 0.5836(1) 0.3662(3) 0.3854(2) 0.0496(9) Uani 1.00 1 d . . .
C(3) C 0.5770(1) 0.4571(4) 0.3315(2) 0.063(1) Uani 1.00 1 d . . .
C(4) C 0.5917(1) 0.5743(4) 0.3523(2) 0.071(1) Uani 1.00 1 d . . .
C(5) C 0.6130(1) 0.6039(3) 0.4278(3) 0.063(1) Uani 1.00 1 d . . .
C(6) C 0.6209(1) 0.5173(3) 0.4852(2) 0.0461(8) Uani 1.00 1 d . . .
C(7) C 0.5683(2) 0.2384(4) 0.3612(2) 0.072(1) Uani 1.00 1 d . . .
C(8) C 0.6452(2) 0.5504(3) 0.5665(3) 0.062(1) Uani 1.00 1 d . . .
C(9) C 0.7171(1) 0.0906(3) 0.6089(2) 0.0387(7) Uani 1.00 1 d . . .
C(10) C 0.7231(1) -0.0198(3) 0.5611(2) 0.0544(9) Uani 1.00 1 d . . .
C(11) C 0.6762(2) -0.0552(7) 0.5054(4) 0.138(2) Uani 1.00 1 d . . .
C(12) C 0.7541(3) 0.0148(7) 0.5128(5) 0.154(4) Uani 1.00 1 d . . .
C(13) C 0.7469(3) -0.1244(4) 0.6096(3) 0.120(2) Uani 1.00 1 d . . .
C(14) C 0.7591(1) 0.1533(3) 0.6719(2) 0.062(1) Uani 1.00 1 d . . .
C(15) C 0.7527(1) 0.2892(4) 0.6661(3) 0.073(1) Uani 1.00 1 d . . .
C(16) C 0.8091(2) 0.1185(7) 0.6801(5) 0.154(3) Uani 1.00 1 d . . .
C(17) C 0.7522(3) 0.1159(5) 0.7483(3) 0.114(2) Uani 1.00 1 d . . .
C(18) C 0.6271(2) 0.0659(4) 0.7857(2) 0.071(1) Uani 1.00 1 d . . .
C(19) C 0.6083(2) -0.1152(3) 0.6737(2) 0.066(1) Uani 1.00 1 d . . .
C(20) C 0.5353(1) 0.0558(3) 0.6657(2) 0.058(1) Uani 1.00 1 d . . .
C(21) C 0.5186(1) 0.1872(3) 0.6587(2) 0.059(1) Uani 1.00 1 d . . .
C(22) C 0.4853(1) 0.2515(3) 0.4995(2) 0.0519(8) Uani 1.00 1 d . . .
C(23) C 0.5301(1) 0.4293(3) 0.6080(2) 0.057(1) Uani 1.00 1 d . . .
H(1) H 0.5619 0.4379 0.2790 0.079 Uiso 1.00 1 c R . .
H(2) H 0.5871 0.6356 0.3142 0.089 Uiso 1.00 1 c R . .
H(3) H 0.6228 0.6859 0.4414 0.079 Uiso 1.00 1 c R . .
H(4) H 0.554(2) 0.231(5) 0.303(3) 0.10(2) Uiso 1.00 1 c . . .
H(5) H 0.5957 0.1863 0.3772 0.085 Uiso 1.00 1 c R . .
H(6) H 0.5456 0.2123 0.3840 0.085 Uiso 1.00 1 c R . .
H(7) H 0.630(2) 0.539(4) 0.593(3) 0.08(2) Uiso 1.00 1 c . . .
H(8) H 0.6709 0.4951 0.5888 0.073 Uiso 1.00 1 c R . .
H(9) H 0.6574 0.6314 0.5697 0.073 Uiso 1.00 1 c R . .
H(10) H 0.683(2) -0.122(6) 0.473(4) 0.14(2) Uiso 1.00 1 c . . .
H(11) H 0.6566 -0.0863 0.5325 0.154 Uiso 1.00 1 c R . .
H(12) H 0.6612 0.0144 0.4766 0.154 Uiso 1.00 1 c R . .
H(13) H 0.7344 0.0457 0.4646 0.211 Uiso 1.00 1 c R . .
H(14) H 0.7711 -0.0551 0.5052 0.211 Uiso 1.00 1 c R . .
H(15) H 0.7764 0.0760 0.5391 0.211 Uiso 1.00 1 c R . .
H(17) H 0.7256 -0.1583 0.6330 0.133 Uiso 1.00 1 c R . .
H(19) H 0.776(2) 0.328(5) 0.700(3) 0.11(2) Uiso 1.00 1 c . . .
H(20) H 0.7524 0.3140 0.6169 0.083 Uiso 1.00 1 c R . .
H(21) H 0.7232 0.3119 0.6725 0.083 Uiso 1.00 1 c R . .
H(22) H 0.815(2) 0.037(6) 0.677(4) 0.14(2) Uiso 1.00 1 c . . .
H(23) H 0.8142 0.1404 0.6339 0.168 Uiso 1.00 1 c R . .
H(24) H 0.8314 0.1612 0.7216 0.168 Uiso 1.00 1 c R . .
H(25) H 0.778(2) 0.151(5) 0.798(3) 0.11(2) Uiso 1.00 1 c . . .
H(26) H 0.7226 0.1474 0.7499 0.118 Uiso 1.00 1 c R . .
H(27) H 0.7520 0.0291 0.7515 0.118 Uiso 1.00 1 c R . .
H(28) H 0.614(2) 0.007(4) 0.815(3) 0.09(1) Uiso 1.00 1 c . . .
H(29) H 0.6608 0.0530 0.8007 0.082 Uiso 1.00 1 c R . .
H(30) H 0.6209 0.1465 0.7993 0.082 Uiso 1.00 1 c R . .
H(31) H 0.595(1) -0.135(4) 0.622(2) 0.07(1) Uiso 1.00 1 c . . .
H(32) H 0.6414 -0.1355 0.6960 0.076 Uiso 1.00 1 c R . .
H(33) H 0.5903 -0.1586 0.6992 0.076 Uiso 1.00 1 c R . .
H(34) H 0.527(2) 0.018(4) 0.711(3) 0.09(1) Uiso 1.00 1 c . . .
H(35) H 0.5184 0.0143 0.6195 0.071 Uiso 1.00 1 c R . .
H(36) H 0.5330 0.2260 0.7068 0.076 Uiso 1.00 1 c R . .
H(37) H 0.4846 0.1896 0.6454 0.076 Uiso 1.00 1 c R . .
H(38) H 0.459(2) 0.283(4) 0.506(2) 0.07(1) Uiso 1.00 1 c . . .
H(39) H 0.4899 0.3029 0.4612 0.058 Uiso 1.00 1 c R . .
H(40) H 0.4834 0.1686 0.4832 0.058 Uiso 1.00 1 c R . .
H(41) H 0.537(1) 0.481(4) 0.568(2) 0.07(1) Uiso 1.00 1 c . . .
H(42) H 0.4986 0.4439 0.6090 0.068 Uiso 1.00 1 c R . .
H(43) H 0.5530 0.4483 0.6565 0.068 Uiso 1.00 1 c R . .
H(16) H 0.7547 -0.1848 0.5789 0.133 Uiso 1.00 1 c R . .
H(18) H 0.7754 -0.0971 0.6479 0.133 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)
;
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)
;
P P 0.102 0.094
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
V V 0.300 0.529
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
|
1100905.cif | #------------------------------------------------------------------------------
#$Date: 2022-09-14 17:31:13 +0300 (Wed, 14 Sep 2022) $
#$Revision: 277831 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/09/1100905.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_1100905
loop_
_publ_author_name
'Yamada, Junji'
'Fujiki, Michiya'
'Nomura, Kotohiro'
_publ_section_title
;
A Vanadium(V) Alkylidene Complex Exhibiting Remarkable Catalytic
Activity for Ring-Opening Metathesis Polymerization (ROMP)
;
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2248
_journal_page_last 2250
_journal_paper_doi 10.1021/om0501834
_journal_volume 24
_journal_year 2005
_chemical_formula_moiety 'C24 H46 N2 P Si V '
_chemical_formula_sum 'C24 H46 N2 P Si V'
_chemical_formula_weight 472.64
_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 98.745(8)
_cell_angle_beta 92.067(9)
_cell_angle_gamma 98.33(1)
_cell_formula_units_Z 2
_cell_length_a 10.554(2)
_cell_length_b 10.944(2)
_cell_length_c 13.145(3)
_cell_measurement_reflns_used 5432
_cell_measurement_temperature 243.1
_cell_measurement_theta_max 27.4
_cell_measurement_theta_min 3.1
_cell_volume 1482.2(5)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.9913
_diffrn_measured_fraction_theta_max 0.9913
_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 0.034
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_number 14565
_diffrn_reflns_theta_full 27.49
_diffrn_reflns_theta_max 27.49
_exptl_absorpt_coefficient_mu 0.440
_exptl_absorpt_correction_T_max 0.896
_exptl_absorpt_correction_T_min 0.298
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
Higashi, T. (1995). Program for Absorption Correction.
Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour red
_exptl_crystal_density_diffrn 1.059
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 512.00
_exptl_crystal_size_max 0.80
_exptl_crystal_size_mid 0.50
_exptl_crystal_size_min 0.25
_refine_diff_density_max 0.31
_refine_diff_density_min -0.36
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.020
_refine_ls_hydrogen_treatment refall
_refine_ls_number_parameters 308
_refine_ls_number_reflns 5284
_refine_ls_R_factor_gt 0.0540
_refine_ls_shift/su_max 0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Chebychev polynomial with 3 parameters (Carruthers & Watkin, 1979)
13.3898 7.2647 9.6689
;
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_ref 0.0670
_reflns_number_gt 5284
_reflns_number_total 6743
_reflns_threshold_expression F^2^>2.0\s(F^2^)
_cod_original_formula_sum 'C24 H46 N2 P Si V '
_cod_database_code 1100905
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
V(1) V 0.78106(3) 0.23829(3) 0.71094(2) 0.04208(9) Uani 1.00 1 d . . .
P(1) P 1.00151(6) 0.19711(6) 0.71161(5) 0.0534(2) Uani 1.00 1 d . . .
Si(1) Si 0.72475(7) 0.17904(7) 0.93995(5) 0.0585(2) Uani 1.00 1 d . . .
N(1) N 0.7468(2) 0.1679(2) 0.5884(1) 0.0463(4) Uani 1.00 1 d . . .
N(2) N 0.7568(2) 0.4036(2) 0.7383(1) 0.0499(5) Uani 1.00 1 d . . .
C(1) C 0.7169(2) 0.1211(2) 0.4852(1) 0.0449(5) Uani 1.00 1 d . . .
C(2) C 0.7366(2) 0.2028(2) 0.4112(2) 0.0536(6) Uani 1.00 1 d . . .
C(3) C 0.7019(3) 0.1532(3) 0.3079(2) 0.0658(7) Uani 1.00 1 d . . .
C(4) C 0.6479(3) 0.0305(3) 0.2784(2) 0.0740(8) Uani 1.00 1 d . . .
C(5) C 0.6292(2) -0.0486(3) 0.3508(2) 0.0645(7) Uani 1.00 1 d . . .
C(6) C 0.6639(2) -0.0056(2) 0.4550(2) 0.0509(5) Uani 1.00 1 d . . .
C(7) C 0.7908(3) 0.3374(3) 0.4431(2) 0.0709(8) Uani 1.00 1 d . . .
C(8) C 0.6440(2) -0.0915(2) 0.5335(2) 0.0604(6) Uani 1.00 1 d . . .
C(9) C 0.7233(2) 0.5110(2) 0.7457(2) 0.0534(6) Uani 1.00 1 d . . .
C(10) C 0.5765(3) 0.5189(3) 0.7383(3) 0.0791(9) Uani 1.00 1 d . . .
C(11) C 0.5355(6) 0.6383(5) 0.7173(6) 0.181(3) Uani 1.00 1 d . . .
C(12) C 0.5129(4) 0.4201(5) 0.6539(6) 0.180(3) Uani 1.00 1 d . . .
C(13) C 0.5243(6) 0.488(1) 0.8371(7) 0.253(5) Uani 1.00 1 d . . .
C(14) C 0.8321(3) 0.6259(2) 0.7615(2) 0.0739(8) Uani 1.00 1 d . . .
C(15) C 0.8403(6) 0.6849(4) 0.6633(4) 0.141(2) Uani 1.00 1 d . . .
C(16) C 0.8144(6) 0.7199(5) 0.8555(5) 0.165(2) Uani 1.00 1 d . . .
C(17) C 0.9621(4) 0.5830(4) 0.7759(4) 0.103(1) Uani 1.00 1 d . . .
C(18) C 0.7205(2) 0.1282(2) 0.7991(2) 0.0548(6) Uani 1.00 1 d . . .
C(19) C 0.8077(4) 0.3439(3) 0.9827(2) 0.0805(9) Uani 1.00 1 d . . .
C(20) C 0.8108(4) 0.0725(3) 1.0087(2) 0.083(1) Uani 1.00 1 d . . .
C(21) C 0.5568(4) 0.1727(4) 0.9846(3) 0.090(1) Uani 1.00 1 d . . .
C(22) C 1.0991(3) 0.2662(4) 0.6178(3) 0.093(1) Uani 1.00 1 d . . .
C(23) C 1.1045(3) 0.2399(4) 0.8287(3) 0.100(1) Uani 1.00 1 d . . .
C(24) C 1.0059(3) 0.0313(3) 0.6747(4) 0.092(1) Uani 1.00 1 d . . .
H(1) H 0.7163 0.2064 0.2574 0.082 Uiso 1.00 1 c R . .
H(2) H 0.6225 -0.0005 0.2080 0.088 Uiso 1.00 1 c R . .
H(3) H 0.5926 -0.1337 0.3298 0.074 Uiso 1.00 1 c R . .
H(4) H 0.7227 0.3845 0.4572 0.088 Uiso 1.00 1 c R . .
H(5) H 0.8381 0.3671 0.3893 0.088 Uiso 1.00 1 c R . .
H(6) H 0.8458 0.3465 0.5034 0.088 Uiso 1.00 1 c R . .
H(7) H 0.7188 -0.1290 0.5413 0.073 Uiso 1.00 1 c R . .
H(8) H 0.5726 -0.1549 0.5120 0.073 Uiso 1.00 1 c R . .
H(9) H 0.6285 -0.0445 0.5976 0.073 Uiso 1.00 1 c R . .
H(10) H 0.5303 0.6910 0.7810 0.219 Uiso 1.00 1 c R . .
H(11) H 0.4540 0.6213 0.6808 0.219 Uiso 1.00 1 c R . .
H(12) H 0.5967 0.6790 0.6774 0.219 Uiso 1.00 1 c R . .
H(13) H 0.5129 0.4535 0.5912 0.202 Uiso 1.00 1 c R . .
H(14) H 0.4271 0.3923 0.6688 0.202 Uiso 1.00 1 c R . .
H(15) H 0.5596 0.3517 0.6472 0.202 Uiso 1.00 1 c R . .
H(16) H 0.4974 0.4002 0.8281 0.338 Uiso 1.00 1 c R . .
H(17) H 0.4532 0.5300 0.8538 0.338 Uiso 1.00 1 c R . .
H(18) H 0.5891 0.5114 0.8915 0.338 Uiso 1.00 1 c R . .
H(19) H 0.8974 0.6466 0.6190 0.169 Uiso 1.00 1 c R . .
H(20) H 0.8698 0.7722 0.6794 0.169 Uiso 1.00 1 c R . .
H(21) H 0.7570 0.6713 0.6297 0.169 Uiso 1.00 1 c R . .
H(22) H 0.7638 0.7785 0.8361 0.182 Uiso 1.00 1 c R . .
H(23) H 0.8951 0.7628 0.8851 0.182 Uiso 1.00 1 c R . .
H(24) H 0.7716 0.6758 0.9044 0.182 Uiso 1.00 1 c R . .
H(25) H 0.9813 0.5829 0.8470 0.121 Uiso 1.00 1 c R . .
H(26) H 1.0270 0.6378 0.7501 0.121 Uiso 1.00 1 c R . .
H(27) H 0.9584 0.5007 0.7390 0.121 Uiso 1.00 1 c R . .
H(28) H 0.6864 0.0442 0.7712 0.065 Uiso 1.00 1 c R . .
H(29) H 0.8964 0.3424 0.9969 0.094 Uiso 1.00 1 c R . .
H(30) H 0.7719 0.3803 1.0432 0.094 Uiso 1.00 1 c R . .
H(31) H 0.7978 0.3919 0.9293 0.094 Uiso 1.00 1 c R . .
H(32) H 0.7503 0.0051 1.0232 0.102 Uiso 1.00 1 c R . .
H(33) H 0.8521 0.1178 1.0714 0.102 Uiso 1.00 1 c R . .
H(34) H 0.8729 0.0405 0.9659 0.102 Uiso 1.00 1 c R . .
H(35) H 0.5279 0.2505 0.9820 0.108 Uiso 1.00 1 c R . .
H(36) H 0.5568 0.1562 1.0535 0.108 Uiso 1.00 1 c R . .
H(37) H 0.5011 0.1080 0.9414 0.108 Uiso 1.00 1 c R . .
H(38) H 1.0918 0.2082 0.5555 0.119 Uiso 1.00 1 c R . .
H(39) H 1.1863 0.2853 0.6430 0.119 Uiso 1.00 1 c R . .
H(40) H 1.0693 0.3407 0.6051 0.119 Uiso 1.00 1 c R . .
H(41) H 1.1483 0.3228 0.8320 0.119 Uiso 1.00 1 c R . .
H(42) H 1.1653 0.1838 0.8285 0.119 Uiso 1.00 1 c R . .
H(43) H 1.0541 0.2354 0.8868 0.119 Uiso 1.00 1 c R . .
H(44) H 1.0036 -0.0074 0.7347 0.112 Uiso 1.00 1 c R . .
H(45) H 1.0827 0.0199 0.6413 0.112 Uiso 1.00 1 c R . .
H(46) H 0.9340 -0.0054 0.6291 0.112 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)
;
Si Si 0.082 0.070
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
V V 0.300 0.529
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
|
1100906.cif | #------------------------------------------------------------------------------
#$Date: 2019-09-17 16:20:54 +0300 (Tue, 17 Sep 2019) $
#$Revision: 218380 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/09/1100906.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_1100906
loop_
_publ_author_name
'Shanmuga Sundara Raj, S.'
'Fun, Hoong-Kun'
'Wu, Ji'
'Tian, Yu-Peng'
'Xie, Fu-Xin'
'Shao, Ze-Huai'
'Li, Sheng-Li'
_publ_section_title
;
Intra- and intermolecular C---H...\p interactions in
bis[benzyl 3-(fluoren-9-ylidene)dithiocarbazato-N^3^,S]nickel(II)
;
_journal_coden_ASTM ACSCEE
_journal_issue 11
_journal_name_full
;
Acta Crystallographica, Section C: Crystal Structure Communications
;
_journal_page_first 1321
_journal_page_last 1322
_journal_paper_doi 10.1107/s0108270100011628
_journal_volume 56
_journal_year 2000
_chemical_formula_sum 'C42 H30 N4 Ni S4'
_chemical_formula_weight 777.65
_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'
_cell_angle_alpha 90.00
_cell_angle_beta 100.6900(10)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 8.94630(10)
_cell_length_b 21.76050(10)
_cell_length_c 19.0038(2)
_cell_measurement_reflns_used 7645
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 28.37
_cell_measurement_theta_min 1.44
_cell_volume 3635.38(6)
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full .999
_diffrn_measured_fraction_theta_max .999
_diffrn_measurement_device_type 'Siemens SMART CCD area-detector'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength .71073
_diffrn_reflns_av_R_equivalents .088
_diffrn_reflns_av_sigmaI/netI .0912
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min -25
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_number 20413
_diffrn_reflns_theta_full 25.00
_diffrn_reflns_theta_max 25.00
_diffrn_reflns_theta_min 1.44
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu .801
_exptl_absorpt_correction_T_max .910
_exptl_absorpt_correction_T_min .700
_exptl_absorpt_correction_type empirical
_exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour black
_exptl_crystal_density_diffrn 1.421
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description needle
_exptl_crystal_F_000 1608
_exptl_crystal_size_max .48
_exptl_crystal_size_mid .14
_exptl_crystal_size_min .12
_refine_diff_density_max .834
_refine_diff_density_min -1.240
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref .964
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 460
_refine_ls_number_reflns 6398
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all .964
_refine_ls_R_factor_all .082
_refine_ls_R_factor_gt .064
_refine_ls_shift/su_max .001
_refine_ls_shift/su_mean .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0796P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_ref .111
_reflns_number_gt 3886
_reflns_number_total 6398
_reflns_threshold_expression I>2\s(I)
_cod_duplicate_entry 2011575
_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
Marked entry as a duplicate of entry 2011575.
Copied multiple data items from entry 2011575.
Antanas Vaitkus,
2019-09-17
Updated bibliographical information.
Antanas Vaitkus,
2019-09-17
;
_cod_original_sg_symbol_H-M 'P 21/n'
_cod_database_code 1100906
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_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Ni1 .61154(7) .25498(2) .26099(3) .0377(2) Uani d . 1 . . Ni
S1 .76954(15) .33064(5) .27980(7) .0515(3) Uani d . 1 . . S
S2 1.07291(17) .32700(6) .36874(8) .0652(4) Uani d . 1 . . S
S3 .42692(15) .31907(5) .23103(7) .0503(4) Uani d . 1 . . S
S4 .12382(16) .28982(6) .14885(8) .0615(4) Uani d . 1 . . S
N1 .7907(4) .20327(15) .27254(18) .0375(9) Uani d . 1 . . N
N2 .9229(4) .22562(16) .3174(2) .0430(9) Uani d . 1 . . N
N3 .4546(4) .19324(15) .25885(18) .0378(9) Uani d . 1 . . N
N4 .3158(4) .20386(16) .2115(2) .0443(9) Uani d . 1 . . N
C1 .8017(5) .14592(19) .2528(2) .0374(10) Uani d . 1 . . C
C2 .9092(5) .09752(18) .2868(2) .0389(11) Uani d . 1 . . C
C3 1.0306(6) .0983(2) .3445(3) .0502(13) Uani d . 1 . . C
H3A 1.0668 .1354 .3655 .060 Uiso calc R 1 . . H
C4 1.0967(6) .0431(2) .3703(3) .0627(15) Uani d . 1 . . C
H4A 1.1776 .0432 .4089 .075 Uiso calc R 1 . . H
C5 1.0435(7) -.0121(2) .3391(3) .0699(16) Uani d . 1 . . C
H5A 1.0889 -.0487 .3573 .084 Uiso calc R 1 . . H
C6 .9252(6) -.0138(2) .2820(3) .0603(14) Uani d . 1 . . C
H6A .8912 -.0511 .2611 .072 Uiso calc R 1 . . H
C7 .8568(5) .04084(19) .2558(2) .0445(12) Uani d . 1 . . C
C8 .7294(5) .0522(2) .1965(2) .0453(12) Uani d . 1 . . C
C9 .6460(6) .0129(2) .1462(3) .0622(15) Uani d . 1 . . C
H9A .6648 -.0292 .1480 .075 Uiso calc R 1 . . H
C10 .5347(7) .0376(3) .0935(3) .0713(17) Uani d . 1 . . C
H10A .4762 .0115 .0605 .086 Uiso calc R 1 . . H
C11 .5085(6) .1002(3) .0887(3) .0661(15) Uani d . 1 . . C
H11A .4352 .1156 .0518 .079 Uiso calc R 1 . . H
C12 .5903(6) .1405(2) .1383(2) .0527(13) Uani d . 1 . . C
H12A .5743 .1827 .1346 .063 Uiso calc R 1 . . H
C13 .6968(5) .1154(2) .1937(2) .0412(11) Uani d . 1 . . C
C14 .9202(5) .28486(19) .3210(2) .0433(11) Uani d . 1 . . C
C15 1.2187(6) .2699(2) .3921(3) .0601(14) Uani d . 1 . . C
H15A 1.2162 .2435 .3507 .072 Uiso calc R 1 . . H
H15B 1.3160 .2909 .4002 .072 Uiso calc R 1 . . H
C16 1.2146(6) .2288(2) .4563(2) .0469(12) Uani d . 1 . . C
C17 1.3210(6) .1829(3) .4707(3) .0677(15) Uani d . 1 . . C
H17A 1.3924 .1783 .4412 .081 Uiso calc R 1 . . H
C18 1.3249(8) .1428(3) .5283(4) .0806(18) Uani d . 1 . . C
H18A 1.3968 .1115 .5366 .097 Uiso calc R 1 . . H
C19 1.2216(9) .1503(3) .5720(3) .083(2) Uani d . 1 . . C
H19A 1.2226 .1240 .6107 .100 Uiso calc R 1 . . H
C20 1.1182(7) .1958(3) .5595(3) .0754(18) Uani d . 1 . . C
H20A 1.0497 .2009 .5903 .090 Uiso calc R 1 . . H
C21 1.1110(6) .2360(2) .5007(3) .0613(14) Uani d . 1 . . C
H21A 1.0375 .2666 .4922 .074 Uiso calc R 1 . . H
C22 .4644(5) .13843(19) .2876(2) .0405(11) Uani d . 1 . . C
C23 .5801(5) .1219(2) .3520(2) .0457(12) Uani d . 1 . . C
C24 .6712(6) .1586(3) .4014(3) .0586(14) Uani d . 1 . . C
H24A .6710 .2011 .3962 .070 Uiso calc R 1 . . H
C25 .7629(7) .1304(3) .4590(3) .089(2) Uani d . 1 . . C
H25A .8255 .1546 .4926 .106 Uiso calc R 1 . . H
C26 .7643(10) .0689(4) .4677(4) .116(3) Uani d . 1 . . C
H26A .8305 .0515 .5060 .140 Uiso calc R 1 . . H
C27 .6683(9) .0310(3) .4203(4) .098(2) Uani d . 1 . . C
H27A .6674 -.0112 .4276 .118 Uiso calc R 1 . . H
C28 .5728(7) .0579(2) .3613(3) .0630(15) Uani d . 1 . . C
C29 .4559(6) .0327(2) .3045(3) .0589(15) Uani d . 1 . . C
C30 .4138(9) -.0277(2) .2863(4) .091(2) Uani d . 1 . . C
H30A .4630 -.0603 .3126 .110 Uiso calc R 1 . . H
C31 .2976(9) -.0384(3) .2288(4) .092(2) Uani d . 1 . . C
H31A .2683 -.0787 .2167 .111 Uiso calc R 1 . . H
C32 .2239(8) .0097(3) .1886(4) .085(2) Uani d . 1 . . C
H32A .1454 .0012 .1504 .102 Uiso calc R 1 . . H
C33 .2660(6) .0704(2) .2049(3) .0626(15) Uani d . 1 . . C
H33A .2174 .1026 .1777 .075 Uiso calc R 1 . . H
C34 .3816(5) .08162(19) .2625(3) .0464(12) Uani d . 1 . . C
C35 .2941(5) .2623(2) .1982(2) .0447(12) Uani d . 1 . . C
C36 .0096(6) .2219(2) .1299(3) .0552(13) Uani d . 1 . . C
H36A .0281 .1961 .1723 .066 Uiso calc R 1 . . H
H36B -.0964 .2342 .1222 .066 Uiso calc R 1 . . H
C37 .0327(6) .1824(2) .0659(3) .0509(12) Uani d . 1 . . C
C38 .1341(6) .1969(3) .0225(3) .0674(15) Uani d . 1 . . C
H38A .1950 .2317 .0321 .081 Uiso calc R 1 . . H
C39 .1460(7) .1594(3) -.0365(3) .0773(17) Uani d . 1 . . C
H39A .2142 .1697 -.0660 .093 Uiso calc R 1 . . H
C40 .0593(8) .1085(3) -.0506(3) .090(2) Uani d . 1 . . C
H40A .0679 .0839 -.0896 .108 Uiso calc R 1 . . H
C41 -.0410(9) .0933(3) -.0074(4) .107(2) Uani d . 1 . . C
H41A -.1008 .0582 -.0166 .128 Uiso calc R 1 . . H
C42 -.0529(7) .1305(3) .0500(3) .0820(19) Uani d . 1 . . C
H42A -.1218 .1199 .0791 .098 Uiso calc R 1 . . H
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
Ni1 .0558(4) .0275(3) .0339(3) .0009(3) .0195(3) .0011(2)
S1 .0728(9) .0306(6) .0522(8) -.0042(6) .0140(7) .0052(5)
S2 .0821(10) .0480(8) .0621(9) -.0234(7) .0043(8) .0056(7)
S3 .0659(9) .0298(6) .0585(8) .0073(5) .0203(7) .0006(5)
S4 .0689(9) .0537(8) .0603(9) .0145(7) .0076(7) .0027(7)
N1 .053(2) .032(2) .032(2) -.0064(17) .0184(18) .0006(16)
N2 .052(2) .035(2) .045(2) -.0080(18) .0181(19) -.0020(17)
N3 .050(2) .032(2) .035(2) .0102(17) .0190(18) .0029(16)
N4 .054(2) .036(2) .046(2) .0021(18) .0155(19) -.0030(18)
C1 .049(3) .036(2) .034(2) -.004(2) .025(2) .000(2)
C2 .049(3) .035(2) .039(3) .002(2) .026(2) -.002(2)
C3 .063(3) .037(3) .053(3) .001(2) .018(3) -.003(2)
C4 .078(4) .055(3) .056(3) .010(3) .014(3) .004(3)
C5 .097(5) .046(3) .069(4) .018(3) .022(4) .009(3)
C6 .083(4) .035(3) .068(4) .005(3) .028(3) -.007(3)
C7 .059(3) .039(3) .042(3) .004(2) .025(2) -.006(2)
C8 .060(3) .042(3) .042(3) -.005(2) .030(3) -.008(2)
C9 .085(4) .055(3) .054(3) -.012(3) .031(3) -.027(3)
C10 .094(5) .080(4) .042(3) -.011(4) .020(3) -.027(3)
C11 .076(4) .088(4) .037(3) -.002(3) .018(3) -.007(3)
C12 .071(4) .057(3) .038(3) -.003(3) .029(3) -.005(2)
C13 .052(3) .044(3) .034(3) -.002(2) .026(2) -.003(2)
C14 .061(3) .036(3) .037(3) -.010(2) .019(2) -.001(2)
C15 .059(3) .075(4) .050(3) -.018(3) .018(3) .000(3)
C16 .052(3) .057(3) .034(3) -.010(2) .012(2) -.007(2)
C17 .071(4) .076(4) .060(4) .000(3) .022(3) -.006(3)
C18 .095(5) .066(4) .076(5) .005(3) .004(4) .000(4)
C19 .122(6) .068(4) .053(4) -.017(4) -.001(4) .011(3)
C20 .103(5) .093(5) .036(3) -.022(4) .029(3) -.004(3)
C21 .068(4) .070(4) .051(3) .004(3) .027(3) .000(3)
C22 .053(3) .036(2) .041(3) .006(2) .029(2) .001(2)
C23 .061(3) .044(3) .041(3) .007(2) .030(2) .008(2)
C24 .065(3) .073(4) .041(3) .010(3) .019(3) .015(3)
C25 .096(5) .110(6) .061(4) .000(4) .018(4) .030(4)
C26 .134(7) .135(7) .077(5) .023(6) .011(5) .053(5)
C27 .132(6) .065(4) .105(6) .030(4) .040(5) .054(4)
C28 .084(4) .050(3) .066(4) .015(3) .043(3) .023(3)
C29 .084(4) .032(3) .075(4) .000(3) .050(3) .007(3)
C30 .125(6) .037(3) .135(7) -.006(4) .085(5) .010(4)
C31 .120(6) .048(4) .131(7) -.029(4) .079(5) -.025(4)
C32 .111(5) .063(4) .092(5) -.034(4) .052(4) -.027(4)
C33 .083(4) .051(3) .063(4) -.014(3) .039(3) -.013(3)
C34 .063(3) .030(2) .056(3) -.004(2) .039(3) -.003(2)
C35 .060(3) .044(3) .036(3) .010(2) .022(2) .001(2)
C36 .058(3) .063(3) .047(3) .012(3) .018(3) .001(3)
C37 .056(3) .061(3) .040(3) .006(3) .020(2) .006(2)
C38 .079(4) .078(4) .051(3) -.011(3) .027(3) .000(3)
C39 .083(4) .111(5) .047(3) .008(4) .034(3) .000(4)
C40 .104(5) .098(5) .069(5) .005(4) .022(4) -.032(4)
C41 .137(7) .101(6) .094(6) -.033(5) .055(5) -.034(4)
C42 .101(5) .080(4) .078(4) -.026(4) .050(4) -.018(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S .1246 .1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni .3393 1.1124 '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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni1 N1 . 1.937(3) y
Ni1 N3 . 1.938(4) y
Ni1 S3 . 2.1560(10) y
Ni1 S1 . 2.1560(10) y
S1 C14 . 1.741(5) y
S2 C14 . 1.752(4) y
S2 C15 . 1.796(5) y
S3 C35 . 1.746(5) y
S4 C35 . 1.740(5) y
S4 C36 . 1.796(5) y
N1 C1 . 1.312(5) ?
N1 N2 . 1.410(5) ?
N2 C14 . 1.291(5) ?
N3 C22 . 1.308(5) ?
N3 N4 . 1.410(5) ?
N4 C35 . 1.305(5) ?
C1 C13 . 1.480(6) ?
C1 C2 . 1.490(6) ?
C2 C3 . 1.393(6) ?
C2 C7 . 1.410(6) ?
C3 C4 . 1.388(6) ?
C4 C5 . 1.386(7) ?
C5 C6 . 1.368(7) ?
C6 C7 . 1.387(6) ?
C7 C8 . 1.467(6) ?
C8 C9 . 1.393(6) ?
C8 C13 . 1.405(6) ?
C9 C10 . 1.384(7) ?
C10 C11 . 1.382(7) ?
C11 C12 . 1.392(6) ?
C12 C13 . 1.394(6) ?
C15 C16 . 1.519(7) ?
C16 C21 . 1.372(7) ?
C16 C17 . 1.373(7) ?
C17 C18 . 1.394(8) ?
C18 C19 . 1.363(9) ?
C19 C20 . 1.346(8) ?
C20 C21 . 1.410(7) ?
C22 C34 . 1.474(6) ?
C22 C23 . 1.493(6) ?
C23 C24 . 1.379(6) ?
C23 C28 . 1.406(6) ?
C24 C25 . 1.382(7) ?
C25 C26 . 1.349(9) ?
C26 C27 . 1.393(9) ?
C27 C28 . 1.405(8) ?
C28 C29 . 1.464(7) ?
C29 C30 . 1.392(7) ?
C29 C34 . 1.420(6) ?
C30 C31 . 1.382(10) ?
C31 C32 . 1.388(9) ?
C32 C33 . 1.394(7) ?
C33 C34 . 1.381(7) ?
C36 C37 . 1.534(6) ?
C37 C42 . 1.366(7) ?
C37 C38 . 1.371(7) ?
C38 C39 . 1.408(7) ?
C39 C40 . 1.350(8) ?
C40 C41 . 1.365(9) ?
C41 C42 . 1.378(8) ?
|
1100907.cif | #------------------------------------------------------------------------------
#$Date: 2015-01-27 21:58:39 +0200 (Tue, 27 Jan 2015) $
#$Revision: 130149 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100907.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_1100907
loop_
_publ_author_name
'Brady, Fiona'
'Gallagher, John F.'
_publ_section_title
;
Intermolecular O-H...O hydrogen bonding in the three independent molecules
of (2S)-3-(4-hydroxyphenyl)-2-(1-oxoisoindolin-2-yl)propanoic acid
;
_journal_name_full 'Acta Crystallographica, Section C'
_journal_page_first 1407
_journal_page_last 1410
_journal_paper_doi 10.1107/S010827010001163X
_journal_volume 56
_journal_year 2000
_chemical_formula_moiety 'C17 H15 N O4'
_chemical_formula_sum 'C17 H15 N O4'
_chemical_formula_weight 297.30
_chemical_melting_point 503
_chemical_name_systematic
;
(2S)-3-(4-hydroxyphenyl)-2-(1-oxoisoindolin-2-yl)propanoic acidd
;
_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'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 12
_cell_length_a 10.7589(9)
_cell_length_b 17.8696(17)
_cell_length_c 22.6670(18)
_cell_measurement_reflns_used 25
_cell_measurement_temperature 294.0(10)
_cell_measurement_theta_max 18.6
_cell_measurement_theta_min 9.6
_cell_volume 4357.9(7)
_diffrn_ambient_temperature 294.0(10)
_diffrn_measured_fraction_theta_full 1.00
_diffrn_measured_fraction_theta_max 1.00
_diffrn_measurement_device 'Enraf-Nonius CAD-4'
_diffrn_measurement_method \w/2\q
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'X-ray tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength .7107
_diffrn_reflns_av_R_equivalents .009
_diffrn_reflns_av_sigmaI/netI .045
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 21
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_l_max 26
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_number 8116
_diffrn_reflns_theta_full 25.0
_diffrn_reflns_theta_max 25.0
_diffrn_reflns_theta_min 2.1
_diffrn_standards_decay_% <1
_diffrn_standards_interval_time 120
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu .098
_exptl_absorpt_correction_T_max ?
_exptl_absorpt_correction_T_min ?
_exptl_absorpt_correction_type none
_exptl_absorpt_process_details none
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.359
_exptl_crystal_density_meas ?
_exptl_crystal_density_method .
_exptl_crystal_description block
_exptl_crystal_F_000 1872
_exptl_crystal_size_max .36
_exptl_crystal_size_mid .36
_exptl_crystal_size_min .28
_exptl_crystal_size_rad ?
_refine_diff_density_max .19
_refine_diff_density_min -.18
_refine_ls_extinction_coef .0013(3)
_refine_ls_extinction_method 'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref 1.02
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 602
_refine_ls_number_reflns 4272
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.02
_refine_ls_R_factor_all .086
_refine_ls_R_factor_gt .045
_refine_ls_shift/su_max <0.001
_refine_ls_shift/su_mean .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.063P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_ref .116
_reflns_number_gt 2782
_reflns_number_total 4272
_reflns_threshold_expression I>2\s(I)
_cod_database_code 1100907
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x+1/2, -y, z+1/2'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
O1A -.0896(3) .28650(16) .97414(15) .0590(9) Uani d . 1 . . O
O2A -.0106(3) .17910(18) 1.00576(15) .0627(10) Uani d . 1 . . O
O3A .2947(2) .19604(16) .92347(14) .0484(8) Uani d . 1 . . O
O4A .1472(3) .32560(18) .63561(15) .0631(9) Uani d . 1 . . O
N1A .1021(3) .15017(18) .90189(15) .0395(9) Uani d . 1 . . N
C1A -.0238(4) .2245(3) .9681(2) .0455(12) Uani d . 1 . . C
C2A .0365(4) .2207(2) .90756(19) .0407(11) Uani d . 1 . . C
C3A .2231(4) .1424(2) .9149(2) .0372(10) Uani d . 1 . . C
C4A .2515(4) .0627(2) .9164(2) .0446(11) Uani d . 1 . . C
C5A .3640(5) .0270(3) .9256(2) .0632(14) Uani d . 1 . . C
C6A .3638(7) -.0494(4) .9252(3) .0850(19) Uani d . 1 . . C
C7A .2564(8) -.0892(3) .9168(3) .091(2) Uani d . 1 . . C
C8A .1440(7) -.0540(3) .9068(3) .0809(18) Uani d . 1 . . C
C9A .1428(5) .0241(2) .9069(2) .0502(12) Uani d . 1 . . C
C10A .0381(4) .0781(2) .8977(2) .0510(13) Uani d . 1 . . C
C11A .0080(4) .2542(2) .7980(2) .0408(11) Uani d . 1 . . C
C12A .1052(4) .3053(2) .7926(2) .0470(11) Uani d . 1 . . C
C13A .1493(4) .3282(2) .7383(2) .0490(12) Uani d . 1 . . C
C14A .0992(4) .2996(2) .6878(2) .0472(11) Uani d . 1 . . C
C15A .0058(4) .2471(3) .6914(2) .0489(12) Uani d . 1 . . C
C16A -.0398(4) .2254(2) .7458(2) .0437(11) Uani d . 1 . . C
C21A -.0520(4) .2353(3) .85600(19) .0503(12) Uani d . 1 . . C
O1B -.1026(3) .2615(2) .18076(16) .0761(11) Uani d . 1 . . O
O2B .0525(4) .1887(2) .15264(18) .0895(13) Uani d . 1 . . O
O3B -.0604(3) .04789(15) .26555(14) .0487(8) Uani d . 1 . . O
O4B .0515(4) .25536(18) .53753(15) .0667(10) Uani d . 1 . . O
N1B .0906(3) .13819(17) .26492(16) .0403(9) Uani d . 1 . . N
C1B -.0103(5) .2147(3) .1905(2) .0527(13) Uani d . 1 . . C
C2B .0062(4) .2007(2) .2559(2) .0450(11) Uani d . 1 . . C
C3B .0517(4) .0663(2) .26483(18) .0372(10) Uani d . 1 . . C
C4B .1614(4) .0191(2) .26163(19) .0396(10) Uani d . 1 . . C
C5B .1698(5) -.0581(2) .2610(2) .0519(12) Uani d . 1 . . C
C6B .2856(5) -.0890(3) .2524(2) .0603(14) Uani d . 1 . . C
C7B .3897(5) -.0439(3) .2458(2) .0616(14) Uani d . 1 . . C
C8B .3808(4) .0322(3) .2480(2) .0597(14) Uani d . 1 . . C
C9B .2650(4) .0639(3) .2562(2) .0458(12) Uani d . 1 . . C
C10B .2253(4) .1444(2) .2581(2) .0524(13) Uani d . 1 . . C
C11B .0488(4) .2644(2) .3540(2) .0434(11) Uani d . 1 . . C
C12B -.0470(4) .2312(3) .3846(2) .0538(13) Uani d . 1 . . C
C13B -.0474(5) .2274(3) .4451(2) .0564(13) Uani d . 1 . . C
C14B .0478(4) .2586(2) .4766(2) .0454(11) Uani d . 1 . . C
C15B .1445(5) .2928(2) .4480(2) .0501(12) Uani d . 1 . . C
C16B .1435(4) .2955(2) .3870(2) .0477(12) Uani d . 1 . . C
C21B .0468(5) .2716(2) .2877(2) .0538(13) Uani d . 1 . . C
O1C -.3651(3) -.0029(3) .65872(17) .0956(15) Uani d . 1 . . O
O2C -.1767(3) .0045(3) .69273(17) .0879(13) Uani d . 1 . . O
O3C -.0623(3) .13484(15) .57332(15) .0518(8) Uani d . 1 . . O
O4C -.1461(5) -.08855(19) .31170(18) .0897(13) Uani d . 1 . . O
N1C -.0737(3) .00823(17) .58263(17) .0424(8) Uani d . 1 . . N
C1C -.2450(4) .0016(3) .6524(2) .0451(11) Uani d . 1 . . C
C2C -.2078(3) .0049(2) .5888(2) .0412(10) Uani d . 1 . . C
C3C -.0112(4) .0730(2) .5785(2) .0396(10) Uani d . 1 . . C
C4C .1223(4) .0541(2) .5814(2) .0419(10) Uani d . 1 . . C
C5C .2260(4) .1003(3) .5795(3) .0634(15) Uani d . 1 . . C
C6C .3410(5) .0666(4) .5835(3) .0818(18) Uani d . 1 . . C
C7C .3524(4) -.0096(3) .5888(3) .0745(17) Uani d . 1 . . C
C8C .2495(4) -.0553(3) .5910(3) .0655(16) Uani d . 1 . . C
C9C .1345(4) -.0219(2) .5872(2) .0473(11) Uani d . 1 . . C
C10C .0067(4) -.0566(2) .5902(3) .0534(13) Uani d . 1 . . C
C11C -.2282(4) -.0650(2) .4895(2) .0455(12) Uani d . 1 . . C
C12C -.2335(4) -.0041(3) .4522(2) .0536(13) Uani d . 1 . . C
C13C -.2069(5) -.0105(3) .3933(2) .0565(13) Uani d . 1 . . C
C14C -.1736(5) -.0789(3) .3702(2) .0598(14) Uani d . 1 . . C
C15C -.1684(4) -.1402(3) .4071(3) .0577(14) Uani d . 1 . . C
C16C -.1960(4) -.1329(2) .4646(2) .0505(12) Uani d . 1 . . C
C21C -.2641(4) -.0610(3) .5532(2) .0539(13) Uani d . 1 . . C
H1A -.1264 .2856 1.0058 .071 Uiso calc R 1 . . H
H4A .1213 .2999 .6083 .076 Uiso calc R 1 . . H
H2A .0996 .2602 .9064 .049 Uiso calc R 1 . . H
H5A .4368 .0539 .9317 .076 Uiso calc R 1 . . H
H6A .4381 -.0750 .9309 .102 Uiso calc R 1 . . H
H7A .2592 -.1412 .9178 .109 Uiso calc R 1 . . H
H8A .0718 -.0813 .9002 .097 Uiso calc R 1 . . H
H10A -.0002 .0714 .8594 .061 Uiso calc R 1 . . H
H10B -.0247 .0729 .9282 .061 Uiso calc R 1 . . H
H12A .1414 .3246 .8266 .056 Uiso calc R 1 . . H
H13A .2133 .3631 .7361 .059 Uiso calc R 1 . . H
H15A -.0267 .2262 .6572 .059 Uiso calc R 1 . . H
H16A -.1040 .1906 .7475 .052 Uiso calc R 1 . . H
H21A -.1033 .1912 .8505 .060 Uiso calc R 1 . . H
H21B -.1069 .2762 .8668 .060 Uiso calc R 1 . . H
H1B -.1022 .2743 .1460 .091 Uiso calc R 1 . . H
H4B -.0038 .2276 .5494 .080 Uiso calc R 1 . . H
H2B -.0749 .1862 .2718 .054 Uiso calc R 1 . . H
H5B .0999 -.0880 .2662 .062 Uiso calc R 1 . . H
H6B .2942 -.1408 .2509 .072 Uiso calc R 1 . . H
H7B .4670 -.0660 .2399 .074 Uiso calc R 1 . . H
H8B .4511 .0620 .2442 .072 Uiso calc R 1 . . H
H10C .2625 .1703 .2913 .063 Uiso calc R 1 . . H
H10D .2470 .1702 .2219 .063 Uiso calc R 1 . . H
H12B -.1132 .2108 .3637 .065 Uiso calc R 1 . . H
H13B -.1124 .2036 .4646 .068 Uiso calc R 1 . . H
H15B .2097 .3139 .4692 .060 Uiso calc R 1 . . H
H16B .2088 .3191 .3676 .057 Uiso calc R 1 . . H
H21C .1294 .2851 .2742 .065 Uiso calc R 1 . . H
H21D -.0091 .3119 .2769 .065 Uiso calc R 1 . . H
H1C -.3812 -.0272 .6884 .115 Uiso calc R 1 . . H
H4C -.1288 -.0480 .2969 .108 Uiso calc R 1 . . H
H2C -.2418 .0513 .5723 .049 Uiso calc R 1 . . H
H5C .2182 .1519 .5756 .076 Uiso calc R 1 . . H
H6C .4123 .0961 .5825 .098 Uiso calc R 1 . . H
H7C .4313 -.0307 .5910 .089 Uiso calc R 1 . . H
H8C .2574 -.1068 .5950 .079 Uiso calc R 1 . . H
H10E -.0054 -.0928 .5588 .064 Uiso calc R 1 . . H
H10F -.0074 -.0807 .6279 .064 Uiso calc R 1 . . H
H12C -.2557 .0424 .4674 .064 Uiso calc R 1 . . H
H13C -.2114 .0313 .3689 .068 Uiso calc R 1 . . H
H15C -.1457 -.1867 .3921 .069 Uiso calc R 1 . . H
H16C -.1934 -.1751 .4886 .061 Uiso calc R 1 . . H
H21E -.2396 -.1074 .5721 .065 Uiso calc R 1 . . H
H21F -.3540 -.0577 .5556 .065 Uiso calc R 1 . . H
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
O1A .078(2) .0446(17) .055(2) .0079(17) .0261(19) -.0007(16)
O2A .082(2) .058(2) .048(2) .0111(18) .0092(19) .0074(18)
O3A .0398(16) .0569(18) .048(2) -.0093(15) -.0046(15) -.0004(16)
O4A .067(2) .071(2) .051(2) -.0084(19) .007(2) -.0014(18)
N1A .0364(18) .0381(19) .044(2) -.0041(16) .0001(16) -.0048(16)
C1A .047(3) .039(3) .050(3) -.002(2) .000(2) -.009(2)
C2A .039(2) .039(2) .044(3) -.0004(18) .005(2) -.006(2)
C3A .037(2) .042(2) .032(3) -.002(2) -.004(2) .000(2)
C4A .051(3) .051(3) .032(3) .008(2) .006(2) -.005(2)
C5A .067(3) .071(3) .051(3) .026(3) -.004(3) .001(3)
C6A .112(5) .082(4) .061(4) .044(4) -.010(4) -.006(3)
C7A .152(7) .042(3) .078(5) .025(4) -.012(5) -.007(3)
C8A .113(5) .043(3) .087(5) -.005(3) .003(4) -.008(3)
C9A .068(3) .042(3) .040(3) .000(2) .007(2) -.008(2)
C10A .045(3) .046(2) .062(3) -.008(2) .004(2) -.010(2)
C11A .033(2) .044(2) .045(3) .013(2) -.001(2) .000(2)
C12A .048(3) .047(3) .046(3) .004(2) -.003(2) -.008(2)
C13A .044(2) .049(3) .054(3) -.004(2) .004(2) -.011(2)
C14A .043(3) .047(2) .051(3) .003(2) .004(2) -.004(2)
C15A .046(3) .056(3) .045(3) .005(2) -.004(2) -.012(2)
C16A .036(2) .044(2) .051(3) .0007(19) .000(2) .002(2)
C21A .041(2) .059(3) .051(3) .010(2) -.001(2) -.005(2)
O1B .075(2) .096(3) .057(2) .027(2) -.005(2) .018(2)
O2B .120(3) .090(3) .059(3) .050(3) -.003(3) .000(2)
O3B .0361(16) .0498(17) .060(2) -.0088(14) -.0008(15) .0030(16)
O4B .093(3) .056(2) .051(2) -.024(2) -.005(2) .0077(17)
N1B .0370(18) .0356(19) .048(2) -.0037(16) -.0065(17) .0085(17)
C1B .057(3) .044(3) .057(4) .013(2) -.004(3) .008(2)
C2B .049(2) .040(2) .046(3) .005(2) -.002(2) .006(2)
C3B .039(2) .035(2) .037(3) -.005(2) -.004(2) .004(2)
C4B .041(2) .042(2) .036(3) -.001(2) -.001(2) .003(2)
C5B .056(3) .038(2) .062(3) -.003(2) -.001(3) -.005(2)
C6B .066(3) .048(3) .067(4) .010(3) .011(3) .000(3)
C7B .051(3) .072(3) .061(4) .018(3) .009(3) .001(3)
C8B .039(3) .070(3) .070(4) -.004(2) .008(3) .013(3)
C9B .041(2) .048(3) .049(3) -.004(2) .000(2) .009(2)
C10B .045(3) .046(3) .066(4) -.012(2) -.004(2) .010(3)
C11B .049(3) .034(2) .047(3) .002(2) .002(2) .009(2)
C12B .046(3) .058(3) .057(3) -.009(2) -.007(3) -.007(3)
C13B .047(3) .066(3) .056(4) -.010(3) .002(3) .003(3)
C14B .056(3) .039(2) .041(3) -.001(2) -.004(2) .004(2)
C15B .054(3) .041(2) .055(3) -.012(2) -.014(3) .006(2)
C16B .044(3) .038(2) .061(3) -.004(2) .003(2) .009(2)
C21B .069(3) .040(3) .052(3) .002(2) .002(3) .008(2)
O1C .0411(19) .186(5) .059(3) -.029(3) .0045(17) .002(3)
O2C .051(2) .153(4) .060(3) -.021(3) -.011(2) -.002(3)
O3C .0435(16) .0371(16) .075(2) .0001(14) .0012(17) .0066(16)
O4C .137(4) .063(2) .069(3) -.005(3) .041(3) -.001(2)
N1C .0299(17) .0351(18) .062(2) -.0006(15) -.0020(18) -.0008(19)
C1C .033(2) .049(3) .053(3) -.009(2) -.003(2) -.002(2)
C2C .0257(19) .050(2) .048(3) -.0048(18) -.002(2) .008(2)
C3C .040(2) .041(2) .037(3) -.005(2) -.003(2) .003(2)
C4C .034(2) .055(3) .036(3) -.007(2) .000(2) .002(2)
C5C .038(3) .065(3) .087(4) -.013(2) .003(3) -.001(3)
C6C .036(3) .097(4) .112(5) -.020(3) -.007(3) .010(4)
C7C .027(2) .102(4) .095(5) .007(3) -.003(3) .016(4)
C8C .042(3) .071(3) .083(4) .014(3) .000(3) .015(3)
C9C .039(2) .049(3) .054(3) -.002(2) .002(2) .003(2)
C10C .038(2) .045(2) .078(4) .000(2) -.001(3) .005(3)
C11C .033(2) .047(3) .057(3) -.005(2) .003(2) .004(2)
C12C .052(3) .043(3) .066(4) -.005(2) .008(2) -.003(3)
C13C .074(3) .044(3) .051(3) .000(3) .017(3) .008(2)
C14C .056(3) .056(3) .067(4) -.007(3) .019(3) -.007(3)
C15C .051(3) .041(3) .081(5) -.004(2) .012(3) -.002(3)
C16C .046(3) .044(3) .062(4) -.006(2) .002(2) .004(2)
C21C .038(2) .059(3) .065(4) -.016(2) -.002(2) .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 .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
2 -8 2
-2 -7 4
3 3 9
|
1100908.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100908.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_1100908
loop_
_publ_author_name
'Baggio, Ricardo'
'Foxman, Bruce'
'Garland, Maria Teresa'
'Perec, Mireille'
'Shang, Wen'
_publ_section_title
;
Aquabis(crotonato)bis(pyridine)copper(II)
;
_journal_issue 11
_journal_name_full 'Acta Crystallographica Section C'
_journal_page_first e505
_journal_page_last e506
_journal_paper_doi 10.1107/S0108270100013937
_journal_volume 56
_journal_year 2000
_chemical_formula_iupac '[Cu (C4 H5 O2)2 (C5 H5 N)2 (H2 O)]'
_chemical_formula_moiety 'C18 H22 Cu N2 O5'
_chemical_formula_sum 'C18 H22 Cu N2 O5'
_chemical_formula_weight 409.92
_chemical_name_systematic
;
Aqua-bis(trans-2-butenoate)- bis(pyridine)copper(II)
;
_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'
_audit_creation_method SHELXL
_cell_angle_alpha 90.00
_cell_angle_beta 91.097(11)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 15.922(2)
_cell_length_b 5.7331(8)
_cell_length_c 21.341(3)
_cell_measurement_reflns_used 25
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 12.5
_cell_measurement_theta_min 7.5
_cell_volume 1947.6(5)
_computing_cell_refinement P3/P4-PC
_computing_data_collection 'P3/P4-PC (Siemens, 1991)'
_computing_data_reduction 'XDISK in SHELXTL/PC (Sheldrick, 1994)'
_computing_publication_material
'CIFTAB (Sheldrick, 1993) and PARST (Nardelli, 1983)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 293(2)
_diffrn_measured_fraction_theta_full .496
_diffrn_measured_fraction_theta_max .496
_diffrn_measurement_device_type 'Siemens R3m'
_diffrn_measurement_method \w/2\q
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength .71073
_diffrn_reflns_av_R_equivalents .026
_diffrn_reflns_av_sigmaI/netI .029
_diffrn_reflns_limit_h_max 18
_diffrn_reflns_limit_h_min 0
_diffrn_reflns_limit_k_max 6
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_l_max 25
_diffrn_reflns_limit_l_min -25
_diffrn_reflns_number 1866
_diffrn_reflns_theta_full 25.00
_diffrn_reflns_theta_max 25.00
_diffrn_reflns_theta_min 1.91
_diffrn_standards_decay_% <2
_diffrn_standards_interval_count 98
_diffrn_standards_number 2
_exptl_absorpt_coefficient_mu 1.15
_exptl_absorpt_correction_T_max .73
_exptl_absorpt_correction_T_min .50
_exptl_absorpt_correction_type psi-scan
_exptl_absorpt_process_details '(XEMP in SHELXTL/PC; Sheldrick, 1994)'
_exptl_crystal_colour blue
_exptl_crystal_density_diffrn 1.398
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plates
_exptl_crystal_F_000 852
_exptl_crystal_size_max .36
_exptl_crystal_size_mid .16
_exptl_crystal_size_min .08
_refine_diff_density_max .287
_refine_diff_density_min -.280
_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 123
_refine_ls_number_reflns 1699
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.068
_refine_ls_R_factor_all .041
_refine_ls_R_factor_gt .031
_refine_ls_shift/su_max .002
_refine_ls_shift/su_mean .001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
' w = 1/[\s^2^(Fo^2^)+(0.04P)^2^+2P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_ref .082
_reflns_number_gt 1476
_reflns_number_total 1699
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file qa0401sup1.cif
_cod_data_source_block I
_cod_original_sg_symbol_H-M 'C 2/c'
_cod_database_code 1100908
_cod_database_fobs_code 1100908
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_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Cu .0000 .38067(8) .2500 .02892(16) Uani d S 1 . . Cu
N1 .10999(12) .4139(4) .20392(9) .0329(5) Uani d . 1 . . N
C2 .16242(17) .5918(5) .21513(13) .0420(6) Uani d . 1 . . C
H2A .1464 .7078 .2429 .050 Uiso calc R 1 . . H
C3 .23942(18) .6096(6) .18688(15) .0503(7) Uani d . 1 . . C
H3A .2744 .7361 .1953 .060 Uiso calc R 1 . . H
C4 .26358(19) .4389(6) .14639(15) .0541(9) Uani d . 1 . . C
H4A .3153 .4469 .1270 .065 Uiso calc R 1 . . H
C5 .2103(2) .2561(6) .13483(16) .0564(9) Uani d . 1 . . C
H5A .2258 .1366 .1079 .068 Uiso calc R 1 . . H
C6 .13350(18) .2505(5) .16343(14) .0451(7) Uani d . 1 . . C
H6A .0968 .1285 .1542 .054 Uiso calc R 1 . . H
O7 -.03881(15) .7474(4) .14482(10) .0583(6) Uani d . 1 . . O
O8 -.05988(11) .3752(4) .17009(8) .0407(4) Uani d . 1 . . O
C9 -.05941(16) .5459(5) .13186(12) .0370(6) Uani d . 1 . . C
C10 -.0859(2) .4903(6) .06611(13) .0489(7) Uani d . 1 . . C
H10A -.0988 .6138 .0394 .059 Uiso calc R 1 . . H
C11 -.0920(2) .2790(6) .04387(14) .0518(8) Uani d . 1 . . C
H11A -.0801 .1568 .0713 .062 Uiso calc R 1 . . H
C12 -.1166(3) .2168(9) -.02215(17) .0879(14) Uani d . 1 . . C
H12A -.1159 .0503 -.0269 .132 Uiso calc R 1 . . H
H12B -.0776 .2857 -.0505 .132 Uiso calc R 1 . . H
H12C -.1721 .2745 -.0313 .132 Uiso calc R 1 . . H
O1W .0000 -.0050(6) .2500 .0499(8) Uani d S 1 . . O
H1W -.011(2) -.089(6) .2228(14) .052(10) Uiso d . 1 . . H
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
Cu .0280(2) .0293(3) .0294(2) .000 .00047(15) .000
N1 .0295(11) .0351(12) .0341(11) -.0002(9) .0000(8) .0006(9)
C2 .0392(14) .0396(16) .0473(15) -.0020(13) .0011(12) -.0036(13)
C3 .0362(14) .0516(18) .0632(19) -.0115(15) -.0023(13) .0060(17)
C4 .0342(15) .066(2) .0623(19) .0035(15) .0128(14) .0119(17)
C5 .059(2) .053(2) .0578(19) .0032(16) .0235(16) -.0103(16)
C6 .0454(16) .0422(17) .0480(16) -.0051(13) .0084(13) -.0092(14)
O7 .0891(17) .0386(13) .0470(12) .0084(12) -.0068(11) -.0065(10)
O8 .0386(10) .0495(11) .0338(9) -.0076(9) -.0041(7) .0067(9)
C9 .0343(14) .0415(17) .0352(14) .0084(12) .0024(11) -.0020(12)
C10 .0568(19) .0529(19) .0367(15) .0057(16) -.0045(13) .0069(15)
C11 .0584(19) .059(2) .0385(16) -.0125(16) .0033(13) -.0027(15)
C12 .102(3) .108(4) .053(2) -.028(3) -.005(2) -.026(2)
O1W .082(2) .0271(16) .0405(17) .000 -.0059(16) .000
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu .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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O8 Cu O8 6_556 . 178.13(12) y
O8 Cu N1 6_556 . 90.77(8) y
O8 Cu N1 . . 89.41(8) y
O8 Cu N1 6_556 6_556 89.41(8) n
O8 Cu N1 . 6_556 90.77(8) n
N1 Cu N1 . 6_556 169.26(12) y
O8 Cu O1W 6_556 . 89.07(6) n
O8 Cu O1W . . 89.07(6) y
N1 Cu O1W . . 95.37(6) y
N1 Cu O1W 6_556 . 95.37(6) n
C6 N1 C2 . . 118.0(2) ?
C6 N1 Cu . . 120.19(18) ?
C2 N1 Cu . . 121.69(18) ?
N1 C2 C3 . . 122.3(3) ?
C4 C3 C2 . . 119.1(3) ?
C3 C4 C5 . . 118.8(3) ?
C4 C5 C6 . . 119.4(3) ?
N1 C6 C5 . . 122.3(3) ?
C9 O8 Cu . . 122.82(18) ?
O7 C9 O8 . . 125.6(3) ?
O7 C9 C10 . . 118.8(3) ?
O8 C9 C10 . . 115.7(3) ?
C11 C10 C9 . . 124.0(3) ?
C10 C11 C12 . . 125.4(3) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cu O8 6_556 1.9381(17) ?
Cu O8 . 1.9381(17) y
Cu N1 . 2.034(2) y
Cu N1 6_556 2.034(2) ?
Cu O1W . 2.211(3) y
N1 C6 . 1.333(3) ?
N1 C2 . 1.337(3) ?
C2 C3 . 1.380(4) ?
C3 C4 . 1.365(5) ?
C4 C5 . 1.368(5) ?
C5 C6 . 1.378(4) ?
O7 C9 . 1.231(4) ?
O8 C9 . 1.274(3) ?
C9 C10 . 1.492(4) ?
C10 C11 . 1.304(5) ?
C11 C12 . 1.498(4) ?
|
1100909.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-30 15:18:45 +0300 (Wed, 30 Mar 2016) $
#$Revision: 180616 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100909.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_1100909
loop_
_publ_author_name
'Hergold-Brundi\'c, Antonija'
'Pavlovi\'c, Gordana'
'Mance, Ana Dunja'
'Jakop\<ci\'c, Kre\<simir'
_publ_section_title
;
N-(4-Methylphenyl)-N-(5-nitrofurfuryl)-N-prop-2-ynylamine
;
_journal_coden_ASTM ACSCEE
_journal_issue 11
_journal_name_full
;
Acta Crystallographica, Section C: Crystal Structure Communications
;
_journal_page_first e520
_journal_page_last e521
_journal_paper_doi 10.1107/s0108270100013068
_journal_volume 56
_journal_year 2000
_chemical_formula_moiety 'C15 H14 N2 O3'
_chemical_formula_sum 'C15 H14 N2 O3'
_chemical_formula_weight 270.28
_chemical_name_systematic
;
N-(4-Methylphenyl)-N-2-propynyl-N-5-nitro-2-furfurylamine
;
_space_group_IT_number 2
_symmetry_cell_setting triclinic
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_audit_creation_method SHELXL-97
_cell_angle_alpha 63.196(14)
_cell_angle_beta 76.908(15)
_cell_angle_gamma 73.937(13)
_cell_formula_units_Z 2
_cell_length_a 8.8490(18)
_cell_length_b 9.2060(13)
_cell_length_c 9.8438(19)
_cell_measurement_reflns_used 57
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 17.8
_cell_measurement_theta_min 8
_cell_volume 683.0(2)
_computing_cell_refinement STADI4
_computing_data_collection 'STADI4 (Stoe & Cie, 1995)'
_computing_data_reduction 'X-RED (Stoe & Cie, 1995)'
_computing_publication_material SHELXL97
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full .969
_diffrn_measured_fraction_theta_max .969
_diffrn_measurement_device_type 'Philips PW1100 updated by Stoe'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength .71073
_diffrn_reflns_av_R_equivalents .105
_diffrn_reflns_av_sigmaI/netI .1140
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_number 7040
_diffrn_reflns_theta_full 29.02
_diffrn_reflns_theta_max 29.02
_diffrn_reflns_theta_min 3.00
_diffrn_standards_decay_% 7.2
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time 90
_diffrn_standards_number 5
_exptl_absorpt_coefficient_mu .093
_exptl_absorpt_correction_T_max ?
_exptl_absorpt_correction_T_min ?
_exptl_absorpt_correction_type none
_exptl_crystal_colour 'pale orange'
_exptl_crystal_density_diffrn 1.314
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 284
_exptl_crystal_size_max .690
_exptl_crystal_size_mid .450
_exptl_crystal_size_min .135
_refine_diff_density_max .170
_refine_diff_density_min -.158
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref .973
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 186
_refine_ls_number_reflns 3520
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all .973
_refine_ls_R_factor_all .078
_refine_ls_R_factor_gt .039
_refine_ls_shift/su_max <0.001
_refine_ls_shift/su_mean .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0189P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_ref .101
_reflns_number_gt 1997
_reflns_number_total 3520
_reflns_threshold_expression I>2\s(I)
_cod_duplicate_entry 2011566
_cod_data_source_file qd0041sup1.cif
_cod_data_source_block 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
The following automatic conversions were performed:
'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0189P)^2^] 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^)+(0.0189P)^2^]
where P = (Fo^2^+2Fc^2^)/3'.
Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas
;
_cod_database_code 1100909
_cod_database_fobs_code 2011566
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
O1 .47394(9) .77179(11) .74520(9) .0474(2) Uani d . 1 . . O
O2 .67701(14) .47179(16) .61158(15) .0784(3) Uani d . 1 . . O
O3 .69057(13) .49415(15) .81856(14) .0769(3) Uani d . 1 . . O
N1 .11488(11) 1.07782(13) .75658(10) .0438(2) Uani d . 1 . . N
N2 .63536(13) .54186(15) .69909(14) .0569(3) Uani d . 1 . . N
C1 .28225(14) 1.01103(18) .76444(15) .0515(3) Uani d . 1 . . C
H1A .3005 .9498 .8712 .062 Uiso calc R 1 . . H
H1B .3380 1.1023 .7195 .062 Uiso calc R 1 . . H
C2 .34977(13) .89850(16) .68373(13) .0455(3) Uani d . 1 . . C
C3 .31406(15) .88957(18) .56119(15) .0536(3) Uani d . 1 . . C
H3 .2343 .9607 .5006 .064 Uiso calc R 1 . . H
C4 .42096(16) .75164(18) .54272(15) .0532(3) Uani d . 1 . . C
H4 .4259 .7136 .4685 .064 Uiso calc R 1 . . H
C5 .51347(14) .68762(17) .65516(14) .0473(3) Uani d . 1 . . C
C6 .00588(13) .97352(14) .83140(11) .0402(2) Uani d . 1 . . C
C7 .05328(16) .80830(16) .93425(12) .0477(3) Uani d . 1 . . C
H7 .1597 .7655 .9482 .057 Uiso calc R 1 . . H
C8 -.05664(19) .70851(18) 1.01507(13) .0578(3) Uani d . 1 . . C
H8 -.0224 .6001 1.0842 .069 Uiso calc R 1 . . H
C9 -.2166(2) .7646(2) .99655(15) .0607(4) Uani d . 1 . . C
C10 -.26237(16) .9274(2) .89053(15) .0578(3) Uani d . 1 . . C
H10 -.3684 .9682 .8744 .069 Uiso calc R 1 . . H
C11 -.15446(14) 1.03022(16) .80857(13) .0477(3) Uani d . 1 . . C
H11 -.1887 1.1378 .7378 .057 Uiso calc R 1 . . H
C12 -.3384(3) .6570(3) 1.0887(2) .0937(7) Uani d . 1 . . C
H12A -.3812 .6747 1.1800 .141 Uiso calc R 1 . . H
H12B -.2888 .5422 1.1161 .141 Uiso calc R 1 . . H
H12C -.4221 .6860 1.0283 .141 Uiso calc R 1 . . H
C13 .06416(15) 1.25034(16) .65162(14) .0490(3) Uani d . 1 . . C
H13A .1413 1.3133 .6403 .059 Uiso calc R 1 . . H
H13B -.0361 1.2966 .6958 .059 Uiso calc R 1 . . H
C14 .04568(16) 1.26957(17) .49896(14) .0538(3) Uani d . 1 . . C
C15 .0333(2) 1.2781(2) .37825(17) .0708(4) Uani d . 1 . . C
H15 .028(3) 1.283(3) .274(3) .110(7) Uiso d . 1 . . H
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
O1 .0400(4) .0548(5) .0483(4) -.0048(4) -.0038(3) -.0255(4)
O2 .0676(6) .0685(7) .1059(8) .0071(5) -.0089(5) -.0544(7)
O3 .0662(6) .0721(7) .0758(7) .0075(5) -.0223(5) -.0222(6)
N1 .0418(5) .0443(5) .0443(5) -.0058(4) -.0006(4) -.0212(4)
N2 .0455(6) .0521(6) .0673(7) -.0054(5) -.0025(5) -.0242(6)
C1 .0454(6) .0623(8) .0584(7) -.0062(5) -.0061(5) -.0377(7)
C2 .0375(5) .0527(7) .0491(6) -.0059(5) -.0017(4) -.0268(5)
C3 .0492(6) .0617(8) .0574(7) .0005(5) -.0122(5) -.0350(6)
C4 .0519(6) .0601(8) .0551(7) -.0056(5) -.0036(5) -.0349(6)
C5 .0404(6) .0490(7) .0542(7) -.0088(5) .0016(5) -.0264(6)
C6 .0467(6) .0439(6) .0341(5) -.0055(5) -.0022(4) -.0228(5)
C7 .0572(7) .0450(6) .0386(6) -.0025(5) -.0077(5) -.0188(5)
C8 .0892(10) .0459(7) .0386(6) -.0181(7) -.0033(6) -.0172(5)
C9 .0817(10) .0670(9) .0450(6) -.0349(8) .0080(6) -.0289(6)
C10 .0511(7) .0743(9) .0558(7) -.0192(6) .0012(5) -.0333(7)
C11 .0482(7) .0466(6) .0453(6) -.0046(5) -.0058(5) -.0189(5)
C12 .1217(16) .1020(16) .0717(10) -.0712(14) .0220(10) -.0360(11)
C13 .0564(7) .0421(6) .0487(6) -.0104(5) -.0010(5) -.0210(5)
C14 .0622(8) .0460(7) .0484(7) -.0119(6) -.0014(5) -.0172(6)
C15 .0973(12) .0591(9) .0513(8) -.0110(8) -.0133(7) -.0193(7)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O .0106 .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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C5 O1 C2 . . 105.10(10) no
C6 N1 C1 . . 120.36(10) no
C6 N1 C13 . . 120.47(10) no
C1 N1 C13 . . 118.57(9) no
O3 N2 O2 . . 124.40(14) no
O3 N2 C5 . . 119.20(12) no
O2 N2 C5 . . 116.39(13) no
N1 C1 C2 . . 113.50(9) no
N1 C1 H1A . . 108.9 no
C2 C1 H1A . . 108.9 no
N1 C1 H1B . . 108.9 no
C2 C1 H1B . . 108.9 no
H1A C1 H1B . . 107.7 no
C3 C2 O1 . . 109.95(11) no
C3 C2 C1 . . 134.27(13) no
O1 C2 C1 . . 115.77(10) no
C2 C3 C4 . . 107.15(12) no
C2 C3 H3 . . 126.4 no
C4 C3 H3 . . 126.4 no
C5 C4 C3 . . 105.19(11) no
C5 C4 H4 . . 127.4 no
C3 C4 H4 . . 127.4 no
C4 C5 O1 . . 112.60(12) no
C4 C5 N2 . . 130.32(12) no
O1 C5 N2 . . 116.90(12) no
N1 C6 C11 . . 121.51(11) no
N1 C6 C7 . . 120.79(11) no
C11 C6 C7 . . 117.70(10) no
C8 C7 C6 . . 120.58(13) no
C8 C7 H7 . . 119.7 no
C6 C7 H7 . . 119.7 no
C7 C8 C9 . . 122.24(14) no
C7 C8 H8 . . 118.9 no
C9 C8 H8 . . 118.9 no
C8 C9 C10 . . 116.94(12) no
C8 C9 C12 . . 122.35(18) no
C10 C9 C12 . . 120.70(18) no
C11 C10 C9 . . 121.90(14) no
C11 C10 H10 . . 119.1 no
C9 C10 H10 . . 119.1 no
C10 C11 C6 . . 120.58(13) no
C10 C11 H11 . . 119.7 no
C6 C11 H11 . . 119.7 no
C9 C12 H12A . . 109.5 no
C9 C12 H12B . . 109.5 no
H12A C12 H12B . . 109.5 no
C9 C12 H12C . . 109.5 no
H12A C12 H12C . . 109.5 no
H12B C12 H12C . . 109.5 no
N1 C13 C14 . . 113.17(10) no
N1 C13 H13A . . 108.9 no
C14 C13 H13A . . 108.9 no
N1 C13 H13B . . 108.9 no
C14 C13 H13B . . 108.9 no
H13A C13 H13B . . 107.8 no
C13 C14 C15 . . 177.26(15) yes
C14 C15 H15 . . 177.6(15) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
O1 C5 . 1.3555(15) no
O1 C2 . 1.3745(16) no
O2 N2 . 1.2328(16) no
O3 N2 . 1.2208(16) no
N1 C6 . 1.3956(14) yes
N1 C1 . 1.4432(16) yes
N1 C13 . 1.4584(16) yes
N2 C5 . 1.4276(19) no
C1 C2 . 1.4988(17) no
C1 H1A . .9700 no
C1 H1B . .9700 no
C2 C3 . 1.3558(17) no
C3 C4 . 1.416(2) no
C3 H3 . .9300 no
C4 C5 . 1.341(2) no
C4 H4 . .9300 no
C6 C11 . 1.4017(17) no
C6 C7 . 1.4017(17) no
C7 C8 . 1.3812(18) no
C7 H7 . .9300 no
C8 C9 . 1.390(2) no
C8 H8 . .9300 no
C9 C10 . 1.395(2) no
C9 C12 . 1.5175(19) no
C10 C11 . 1.3859(18) no
C10 H10 . .9300 no
C11 H11 . .9300 no
C12 H12A . .9600 no
C12 H12B . .9600 no
C12 H12C . .9600 no
C13 C14 . 1.4737(18) yes
C13 H13A . .9700 no
C13 H13B . .9700 no
C14 C15 . 1.183(2) yes
C15 H15 . 1.02(2) no
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C6 N1 C1 C2 . . . . 67.03(14) no
C13 N1 C1 C2 . . . . -104.13(12) no
C5 O1 C2 C3 . . . . .80(12) no
C5 O1 C2 C1 . . . . 179.56(9) no
N1 C1 C2 C3 . . . . 29.90(19) no
N1 C1 C2 O1 . . . . -148.47(10) no
O1 C2 C3 C4 . . . . -.44(14) no
C1 C2 C3 C4 . . . . -178.88(12) no
C2 C3 C4 C5 . . . . -.10(14) no
C3 C4 C5 O1 . . . . .63(13) no
C3 C4 C5 N2 . . . . 175.55(12) no
C2 O1 C5 C4 . . . . -.89(12) no
C2 O1 C5 N2 . . . . -176.55(10) no
O3 N2 C5 C4 . . . . -170.16(12) no
O2 N2 C5 C4 . . . . 9.45(19) no
O3 N2 C5 O1 . . . . 4.58(16) no
O2 N2 C5 O1 . . . . -175.82(9) no
C1 N1 C6 C11 . . . . -170.99(10) no
C13 N1 C6 C11 . . . . .01(14) no
C1 N1 C6 C7 . . . . 10.00(14) no
C13 N1 C6 C7 . . . . -179.00(9) no
N1 C6 C7 C8 . . . . 176.02(9) no
C11 C6 C7 C8 . . . . -3.02(16) no
C6 C7 C8 C9 . . . . 1.38(17) no
C7 C8 C9 C10 . . . . .63(18) no
C7 C8 C9 C12 . . . . -178.08(12) no
C8 C9 C10 C11 . . . . -.93(18) no
C12 C9 C10 C11 . . . . 177.81(12) no
C9 C10 C11 C6 . . . . -.79(18) no
N1 C6 C11 C10 . . . . -176.30(10) no
C7 C6 C11 C10 . . . . 2.74(16) no
C6 N1 C13 C14 . . . . -79.46(13) no
C1 N1 C13 C14 . . . . 91.70(12) no
N1 C13 C14 C15 . . . . -6(3) no
|
1100910.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100910.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_1100910
loop_
_publ_author_name
'Benabad, Aicha'
'Bakhous, Karima'
'Cherkaoui, Fatima'
'Holt, Elizabeth M.'
_publ_section_title
;
Bismuth(V) iron(III) tris(phosphate) oxide
;
_journal_name_full 'Acta Crystallographica, Section C'
_journal_page_first 1292
_journal_page_last 1293
_journal_paper_doi 10.1107/S010827010000977X
_journal_volume 56
_journal_year 2000
_chemical_formula_moiety 'Bi0.4 Fe3 O (PO4)3'
_chemical_formula_structural 'Bi0.4 Fe3 O (PO4)3'
_chemical_formula_sum 'Bi0.4 Fe3 O13 P3'
_chemical_formula_weight 552.04
_chemical_name_common 'Bismuth(V)iron(III) oxophosphate'
_chemical_name_systematic 'Bismuth(V) iron(III) tris(phosphate) oxide'
_space_group_IT_number 11
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2yb'
_symmetry_space_group_name_H-M 'P 1 21/m 1'
_cell_angle_alpha 90.00
_cell_angle_beta 100.110(10)
_cell_angle_gamma 90.00
_cell_formula_units_Z 2
_cell_length_a 7.4960(10)
_cell_length_b 6.3080(10)
_cell_length_c 10.125(2)
_cell_measurement_reflns_used 35
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 13.2
_cell_measurement_theta_min 8.5
_cell_volume 471.32(13)
_diffrn_ambient_temperature 293(2)
_diffrn_measured_fraction_theta_full .986
_diffrn_measured_fraction_theta_max .986
_diffrn_measurement_device_type 'Syntex P4 four-circle'
_diffrn_measurement_method \q/2\q
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength .71073
_diffrn_reflns_av_R_equivalents .088
_diffrn_reflns_av_sigmaI/netI .145
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -1
_diffrn_reflns_limit_k_max 8
_diffrn_reflns_limit_k_min -1
_diffrn_reflns_limit_l_max 14
_diffrn_reflns_limit_l_min -14
_diffrn_reflns_number 2030
_diffrn_reflns_theta_full 29.99
_diffrn_reflns_theta_max 30
_diffrn_reflns_theta_min 2.76
_diffrn_standards_decay_% .000
_diffrn_standards_interval_count 97
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 12.579
_exptl_absorpt_correction_T_max .284
_exptl_absorpt_correction_T_min .244
_exptl_absorpt_correction_type \y-scan
_exptl_absorpt_process_details '(XEMP; Siemens, 1990a)'
_exptl_crystal_colour red
_exptl_crystal_density_diffrn 3.890
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description chunk
_exptl_crystal_F_000 520.4
_exptl_crystal_size_max .1
_exptl_crystal_size_mid .1
_exptl_crystal_size_min .1
_refine_diff_density_max .25
_refine_diff_density_min -.72
_refine_ls_extinction_coef .0000(19)
_refine_ls_extinction_method 'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref .835
_refine_ls_hydrogen_treatment none
_refine_ls_matrix_type full
_refine_ls_number_parameters 115
_refine_ls_number_reflns 1468
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all .835
_refine_ls_R_factor_all .099
_refine_ls_R_factor_gt .058
_refine_ls_shift/su_max .056
_refine_ls_shift/su_mean .049
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0435P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_ref .128
_reflns_number_gt 867
_reflns_number_total 1468
_reflns_threshold_expression I>2\s(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0435P)^2^] 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^)+(0.0435P)^2^]
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 'P2 (1) /m'
_cod_database_code 1100910
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Bi1 .6591(2) 0.25 .19371(15) .0114(5) Uani d SP .40(3) . . Bi
Fe1 0 0 0 .0070(4) Uani d S 1 . . Fe
Fe2 .6496(2) 0.25 -.20185(16) .0060(4) Uani d S 1 . . Fe
Fe3 .2143(2) 0.25 -.43654(16) .0081(4) Uani d S 1 . . Fe
O1 .8762(11) 0.25 -.0928(7) .0088(16) Uani d S 1 . . O
P1 .7834(4) 0.25 .5116(3) .0072(6) Uani d S 1 . . P
O11 .9749(10) 0.25 .5901(8) .0120(18) Uani d S 1 . . O
O12 .6511(11) 0.25 .6076(8) .0129(18) Uani d S 1 . . O
O13 .7512(8) 0.0608(9) .4154(5) .0113(12) Uani d . 1 . . O
P2 .3173(4) 0.25 -.1129(3) .0061(6) Uani d S 1 . . P
O21 .3585(10) 0.25 -.2563(7) .0060(15) Uani d S 1 . . O
O22 .5078(11) 0.25 -.0310(7) .0091(16) Uani d S 1 . . O
O23 .2109(7) 0.0486(9) -.0936(5) .0088(12) Uani d . 1 . . O
P3 .2634(4) 0.25 .2394(3) .0064(6) Uani d S 1 . . P
O31 .2150(12) 0.25 .3744(8) .0161(19) Uani d S 1 . . O
O32 .0829(10) 0.25 .1343(7) .0083(16) Uani d S 1 . . O
O33 .3797(7) 0.4374(9) .2129(5) .0093(12) Uani d . 1 . . O
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
Bi1 .0118(8) .0106(9) .0121(8) 0 .0033(6) 0
Fe1 .0078(7) .0038(7) .0098(8) -.0015(6) .0030(6) -.0002(6)
Fe2 .0051(7) .0052(8) .0078(7) 0 .0018(6) 0
Fe3 .0107(8) .0064(8) .0074(8) 0 .0020(6) 0
O1 .013(4) .008(4) .003(3) 0 -.004(3) 0
P1 .0109(13) .0045(13) .0075(13) 0 .0051(11) 0
O11 .009(4) .015(5) .011(4) 0 -.002(3) 0
O12 .010(4) .021(5) .008(4) 0 .001(3) 0
O13 .020(3) .005(3) .009(3) .002(2) .003(2) .002(2)
P2 .0074(12) .0049(13) .0076(13) 0 .0059(10) 0
O21 .002(3) .010(4) .006(3) 0 .000(3) 0
O22 .013(4) .011(4) .002(3) 0 -.001(3) 0
O23 .011(3) .006(3) .011(3) .002(2) .004(2) .002(2)
P3 .0091(13) .0039(13) .0064(13) 0 .0023(10) 0
O31 .022(4) .020(5) .008(4) 0 .006(3) 0
O32 .022(3) .020(4) .007(4) 0 .006(3) 0
O33 .010(3) .005(3) .013(3) .000(2) .003(2) .001(2)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P .1023 .0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe .3010 .8450 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Bi Bi -4.8610 10.5590 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100911.cif | #------------------------------------------------------------------------------
#$Date: 2022-09-14 18:21:52 +0300 (Wed, 14 Sep 2022) $
#$Revision: 277833 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/09/1100911.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_1100911
loop_
_publ_author_name
'Schultz, Arthur J.'
'Figgis, Brian N.'
'Sobolev, Alexandre N.'
_publ_section_title
;
Na~2~Fe(CN)~5~NO.2D~2~O at 11 and 293 K
by X-ray and at 15 K by neutron diffraction
;
_journal_name_full 'Acta Crystallographica, Section C'
_journal_page_first 1289
_journal_page_last 1291
_journal_paper_doi 10.1107/S0108270100008763
_journal_volume 56
_journal_year 2000
_chemical_formula_moiety 'Na2 Fe (C N)5 N O , 2D2 O'
_chemical_formula_sum 'C5 D4 Fe N6 Na2 O3'
_chemical_formula_weight 301.97
_chemical_melting_point ?
_chemical_name_common 'Sodium nitroprusside, deuterated'
_chemical_name_systematic
;
disodium pentacyanonitrosylferrate(III) bis(dideuterium oxide)
;
_space_group_IT_number 58
_space_group_name_Hall '-P 2 2n'
_space_group_name_H-M_alt 'P n n m'
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall '-P 2 2n'
_symmetry_space_group_name_H-M 'P n n m'
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 6.207(3)
_cell_length_b 11.915(5)
_cell_length_c 15.583(6)
_cell_measurement_reflns_used 14
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 20.09
_cell_measurement_theta_min 18.62
_cell_volume 1152.5(9)
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type 'Huber 512 goniometer'
_diffrn_measurement_method \w/2\q
_diffrn_radiation_monochromator none
_diffrn_radiation_source 'normal-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength .71073
_diffrn_reflns_av_R_equivalents .022
_diffrn_reflns_av_sigmaI/netI .012
_diffrn_reflns_limit_h_max 7
_diffrn_reflns_limit_h_min -7
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_number 7566
_diffrn_reflns_theta_full 25.05
_diffrn_reflns_theta_max 25.05
_diffrn_reflns_theta_min 2.15
_diffrn_standards_decay_% 1
_diffrn_standards_interval_count 100
_diffrn_standards_interval_time ?
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 1.387
_exptl_absorpt_correction_T_max .608
_exptl_absorpt_correction_T_min .539
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details '(XTAL3.4; Hall et al., 1995)'
_exptl_crystal_colour 'dark red-brown'
_exptl_crystal_density_diffrn 1.740
_exptl_crystal_density_meas ?
_exptl_crystal_density_method .
_exptl_crystal_description prism
_exptl_crystal_F_000 592
_exptl_crystal_size_max .62
_exptl_crystal_size_mid .47
_exptl_crystal_size_min .41
_refine_diff_density_max .23
_refine_diff_density_min -.28
_refine_ls_extinction_coef .134(4)
_refine_ls_extinction_method 'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref 1.227
_refine_ls_hydrogen_treatment refall
_refine_ls_matrix_type full
_refine_ls_number_parameters 95
_refine_ls_number_reflns 1067
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.227
_refine_ls_R_factor_all .020
_refine_ls_R_factor_gt .019
_refine_ls_shift/su_max <0.001
_refine_ls_shift/su_mean .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0240P)^2^+0.3324P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_ref .051
_reflns_number_gt 1048
_reflns_number_total 1067
_reflns_threshold_expression I>2\s(I)
_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.
'_exptl_absorpt_correction_type' value 'Gaussian' changed to
'gaussian' 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:
'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.
Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana
;
_cod_original_sg_symbol_H-M Pnnm
_cod_database_code 1100911
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'x-1/2, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Fe1 0.49960(3) .279527(19) 0.5 .01590(14) Uani d S 1 . . Fe
Na1 0.5 0 0.24487(5) .0282(2) Uani d S 1 . . Na
Na2 0 0 0.37797(6) .0338(2) Uani d S 1 . . Na
O1 0.8776(3) .40583(13) 0.5 .0491(4) Uani d S 1 . . O
O2 0.1742(2) .12298(11) 0.26842(8) .0447(3) Uani d . 1 . . O
N1 0.7207(2) .35789(12) 0.5 .0227(3) Uani d S 1 . . N
N2 0.1065(3) .12264(15) 0.5 .0378(4) Uani d S 1 . . N
N3 0.6671(2) .12081(10) 0.35881(8) .0364(3) Uani d . 1 . . N
N4 0.2496(2) .40418(11) 0.35727(8) .0399(3) Uani d . 1 . . N
C1 0.2527(3) .18139(15) 0.5 .0232(4) Uani d S 1 . . C
C2 0.60727(19) .17954(10) 0.41187(8) .0229(3) Uani d . 1 . . C
C3 0.34422(19) .36084(10) 0.41117(8) .0236(3) Uani d . 1 . . C
D1 0.192(5) .187(2) 0.2853(18) .097(10) Uiso d . 1 . . D
D2 0.082(5) .128(2) 0.2365(19) .096(10) Uiso d . 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_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Fe1 .01572(19) .01722(19) .01476(19) -.00100(8) 0 0
Na1 .0291(4) .0324(4) .0231(4) -.0062(3) 0 0
Na2 .0316(5) .0378(5) .0320(5) .0021(3) 0 0
O1 .0308(8) .0434(9) .0733(12) -.0172(7) 0 0
O2 .0443(7) .0456(7) .0443(7) .0040(5) -.0078(5) .0039(5)
N1 .0207(8) .0215(7) .0258(7) -.0014(6) 0 0
N2 .0337(10) .0381(10) .0417(10) -.0142(8) 0 0
N3 .0358(7) .0414(7) .0320(6) .0051(5) -.0002(5) -.0130(5)
N4 .0395(7) .0510(8) .0292(6) .0100(6) -.0033(6) .0105(6)
C1 .0251(9) .0249(9) .0196(8) -.0012(8) 0 0
C2 .0212(6) .0256(6) .0218(6) .0003(5) -.0018(5) -.0011(5)
C3 .0231(6) .0274(6) .0205(6) .0013(5) .0024(5) .0009(5)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
D H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na .0362 .0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe .3463 .8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100912.cif | #------------------------------------------------------------------------------
#$Date: 2022-09-14 18:21:52 +0300 (Wed, 14 Sep 2022) $
#$Revision: 277833 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/09/1100912.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_1100912
loop_
_publ_author_name
'Schultz, Arthur J.'
'Figgis, Brian N.'
'Sobolev, Alexandre N.'
_publ_section_title
;
Na~2~Fe(CN)~5~NO.2D~2~O at 11 and 293 K
by X-ray and at 15 K by neutron diffraction
;
_journal_name_full 'Acta Crystallographica, Section C'
_journal_page_first 1289
_journal_page_last 1291
_journal_paper_doi 10.1107/S0108270100008763
_journal_volume 56
_journal_year 2000
_chemical_formula_moiety 'Na2 Fe (C N)5 N O , 2D2 O'
_chemical_formula_sum 'C5 D4 Fe N6 Na2 O3'
_chemical_formula_weight 301.97
_chemical_melting_point ?
_chemical_name_common 'Sodium nitroprusside, deuterated'
_chemical_name_systematic
;
disodium pentacyanonitrosylferrate(III) bis(dideuterium oxide)
;
_space_group_IT_number 58
_space_group_name_Hall '-P 2 2n'
_space_group_name_H-M_alt 'P n n m'
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall '-P 2 2n'
_symmetry_space_group_name_H-M 'P n n m'
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 6.124(2)
_cell_length_b 11.837(5)
_cell_length_c 15.547(6)
_cell_measurement_reflns_used 8
_cell_measurement_temperature 11.0(10)
_cell_measurement_theta_max 34.5
_cell_measurement_theta_min 34.5
_cell_volume 1127.0(7)
_diffrn_ambient_temperature 11(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full .990
_diffrn_measured_fraction_theta_max .990
_diffrn_measurement_device_type 'Huber 512 goniometer'
_diffrn_measurement_method \w/2\q
_diffrn_radiation_monochromator none
_diffrn_radiation_source 'normal-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength .71073
_diffrn_reflns_av_R_equivalents .028
_diffrn_reflns_av_sigmaI/netI .013
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 25
_diffrn_reflns_limit_k_min -25
_diffrn_reflns_limit_l_max 33
_diffrn_reflns_limit_l_min -33
_diffrn_reflns_number 44955
_diffrn_reflns_theta_full 50.13
_diffrn_reflns_theta_max 50.13
_diffrn_reflns_theta_min 2.16
_diffrn_standards_decay_% 1
_diffrn_standards_interval_count 100
_diffrn_standards_interval_time ?
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 1.419
_exptl_absorpt_correction_T_max .705
_exptl_absorpt_correction_T_min .641
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details '(XTAL3.4; Hall et al., 1995)'
_exptl_crystal_colour 'dark red-brown'
_exptl_crystal_density_diffrn 1.780
_exptl_crystal_density_meas ?
_exptl_crystal_density_method .
_exptl_crystal_description prism
_exptl_crystal_F_000 592
_exptl_crystal_size_max .38
_exptl_crystal_size_mid .32
_exptl_crystal_size_min .29
_refine_diff_density_max .98
_refine_diff_density_min -1.07
_refine_ls_extinction_coef .0096(6)
_refine_ls_extinction_method 'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref 1.081
_refine_ls_hydrogen_treatment refall
_refine_ls_matrix_type full
_refine_ls_number_parameters 95
_refine_ls_number_reflns 6020
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.081
_refine_ls_R_factor_all .025
_refine_ls_R_factor_gt .020
_refine_ls_shift/su_max .002
_refine_ls_shift/su_mean .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0230P)^2^+0.2957P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_ref .054
_reflns_number_gt 5342
_reflns_number_total 6020
_reflns_threshold_expression I>2\s(I)
_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.
'_exptl_absorpt_correction_type' value 'Gaussian' changed to
'gaussian' 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:
'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.
Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana
;
_cod_original_sg_symbol_H-M Pnnm
_cod_database_code 1100912
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'x-1/2, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Fe1 0.500791(12) .280406(6) 0.5 .00324(2) Uani d S 1 . . Fe
Na1 0.5 0 0.245992(17) .00649(4) Uani d S 1 . . Na
Na2 0 0 0.378142(18) .00712(4) Uani d S 1 . . Na
O1 0.88845(8) .40507(4) 0.5 .01010(6) Uani d S 1 . . O
O2 0.17170(6) .12253(3) 0.26872(2) .00956(4) Uani d . 1 . . O
N1 0.72761(7) .35799(4) 0.5 .00550(5) Uani d S 1 . . N
N2 0.09861(9) .12392(4) 0.5 .00859(6) Uani d S 1 . . N
N3 0.66704(6) .11951(3) 0.35800(2) .00868(4) Uani d . 1 . . N
N4 0.25023(6) .40559(3) 0.35539(2) .00944(5) Uani d . 1 . . N
C1 0.24954(9) .18302(4) 0.5 .00629(6) Uani d S 1 . . C
C2 0.60734(6) .17961(3) 0.41208(2) .00631(4) Uani d . 1 . . C
C3 0.34600(6) .36209(3) 0.41082(2) .00647(4) Uani d . 1 . . C
D1 0.180(2) .1871(11) 0.2860(9) .028(3) Uiso d . 1 . . D
D2 0.067(2) .1251(12) 0.2343(9) .033(3) Uiso d . 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_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Fe1 .00376(2) .00314(2) .00281(2) -.00007(2) 0 0
Na1 .00717(9) .00675(8) .00556(8) -.00082(7) 0 0
Na2 .00758(9) .00724(8) .00653(8) .00047(7) 0 0
O1 .00714(14) .00948(14) .01369(16) -.00352(11) 0 0
O2 .01005(11) .00910(9) .00953(10) .00055(8) -.00120(8) .00060(8)
N1 .00570(13) .00509(12) .00571(12) -.00035(10) 0 0
N2 .00811(15) .00843(14) .00923(14) -.00269(12) 0 0
N3 .00936(11) .00908(10) .00760(10) .00131(8) .00026(8) -.00294(8)
N4 .00994(12) .01124(11) .00715(10) .00196(9) -.00136(8) .00239(8)
C1 .00650(15) .00627(14) .00611(13) -.00100(11) 0 0
C2 .00701(11) .00636(10) .00556(9) .00050(8) .00009(8) -.00097(8)
C3 .00723(11) .00682(10) .00537(10) .00080(8) -.00038(8) .00079(8)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
D H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na .0362 .0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe .3463 .8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100913.cif | #------------------------------------------------------------------------------
#$Date: 2022-09-14 17:31:13 +0300 (Wed, 14 Sep 2022) $
#$Revision: 277831 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/09/1100913.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_1100913
loop_
_publ_author_name
'Schultz, Arthur J.'
'Figgis, Brian N.'
'Sobolev, Alexandre N.'
_publ_section_title
;
Na~2~Fe(CN)~5~NO.2D~2~O at 11 and 293 K
by X-ray and at 15 K by neutron diffraction
;
_journal_name_full 'Acta Crystallographica, Section C'
_journal_page_first 1289
_journal_page_last 1291
_journal_paper_doi 10.1107/S0108270100008763
_journal_volume 56
_journal_year 2000
_chemical_formula_moiety 'Na2 Fe (C N)5 N O , 1.45D2 O , 0.55H2 O'
_chemical_formula_sum 'C5 H1.1 D2.9 Fe N6 Na2 O3'
_chemical_formula_weight 300.87
_chemical_melting_point ?
_chemical_name_common 'Sodium nitroprusside, deuterated'
_chemical_name_systematic
;
disodium pentacyanonitrosylferrate(III) bis(dideuterium oxide)
;
_space_group_IT_number 58
_space_group_name_Hall '-P 2 2n'
_space_group_name_H-M_alt 'P n n m'
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall '-P 2 2n'
_symmetry_space_group_name_H-M 'P n n m'
_cell_angle_alpha 90.0
_cell_angle_beta 90.0
_cell_angle_gamma 90.0
_cell_formula_units_Z 4
_cell_length_a 6.124(2)
_cell_length_b 11.837(5)
_cell_length_c 15.547(6)
_cell_measurement_reflns_used 8
_cell_measurement_temperature 11
_cell_measurement_theta_max 34.5
_cell_measurement_theta_min 34.5
_cell_volume 1127.0(7)
_diffrn_ambient_temperature 15
_diffrn_measurement_device 'IPNS Single Crystal Diffractometer'
_diffrn_measurement_method 'Laue time of flight'
_diffrn_radiation_probe neutron
_diffrn_radiation_type 'pulsed neutron'
_diffrn_radiation_wavelength 0.7-4.2
_diffrn_reflns_av_R_equivalents 'not applicable to TOF Laue technique'
_diffrn_reflns_av_sigmaI/netI 'not applicable to TOF Laue technique'
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -1
_diffrn_reflns_limit_k_max 26
_diffrn_reflns_limit_k_min -26
_diffrn_reflns_limit_l_max 34
_diffrn_reflns_limit_l_min -7
_diffrn_reflns_number 8305
_diffrn_reflns_theta_full ?
_diffrn_standards_decay_% 'not applicable to TOF Laue technique'
_diffrn_standards_interval_count 'not applicable to TOF Laue technique'
_diffrn_standards_interval_time 'not applicable to TOF Laue technique'
_diffrn_standards_number 'not applicable to TOF Laue technique'
_exptl_absorpt_coefficient_mu '0.0559 +0.0029(\l) cm^-1^'
_exptl_absorpt_correction_T_max .940
_exptl_absorpt_correction_T_min .879
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details '(ANVRED; ref?)'
_exptl_crystal_colour 'dark red-brown'
_exptl_crystal_density_diffrn 1.774
_exptl_crystal_density_meas ?
_exptl_crystal_description prism
_exptl_crystal_size_max 3.0
_exptl_crystal_size_mid 2.0
_exptl_crystal_size_min 1.0
_refine_diff_density_max .563
_refine_diff_density_min -.512
_refine_ls_extinction_coef '8.4(1) \\times 10^-5^'
_refine_ls_extinction_method 'secondary Type I'
_refine_ls_goodness_of_fit_all 3.75
_refine_ls_hydrogen_treatment refall
_refine_ls_matrix_type full
_refine_ls_number_parameters 131
_refine_ls_number_reflns 6343
_refine_ls_R_factor_obs .058
_refine_ls_shift/esd_max .04
_refine_ls_shift/esd_mean .00
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details (2Fo/\sFo^2^)^2^
_refine_ls_weighting_scheme sigma
_refine_ls_wR_factor_obs .051
_reflns_number_gt 6343
_reflns_number_total 8305
_reflns_threshold_expression I>3\s(I)
_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.
'_exptl_absorpt_correction_type' value 'Gaussian' changed to
'gaussian' 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:
'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.
Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana
;
_cod_original_sg_symbol_H-M Pnnm
_cod_original_formula_sum 'C5 H1.1 D2.9 Fe1 N6 Na2 O3'
_cod_database_code 1100913
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'x-1/2, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z-1/2'
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Fe1 .00398(19) .0036(2) .0028(2) -.00022(19) 0 0
Na1 .0078(6) .0075(6) .0062(6) -.0007(6) 0 0
Na2 .0081(6) .0081(6) .0065(6) -.0010(6) 0 0
O1 .0070(4) .0098(4) .0133(5) -.0036(4) 0 0
O2 .0099(3) .0089(3) .0097(3) .0001(3) -.0014(3) .0007(3)
N1 .0048(2) .0052(2) .0065(3) -.00084(19) 0 0
N2 .0082(2) .0087(3) .0096(3) -.0034(2) 0 0
N3 .00948(18) .00953(19) .00764(19) .00118(17) .00106(17) -.00373(15)
N4 .01017(18) .0118(2) .00779(19) .00204(17) -.00160(18) .00265(16)
C1 .0066(3) .0071(3) .0068(4) -.0018(3) 0 0
C2 .0075(2) .0066(2) .0053(2) .0002(2) .0002(2) -.00160(19)
C3 .0069(2) .0071(2) .0061(3) .0008(2) -.0007(2) .00103(19)
D1 .0353(10) .0136(7) .0359(11) -.0007(7) -.0033(9) -.0052(7)
D2 .0250(8) .0307(9) .0216(9) .0024(7) -.0092(7) .0037(7)
H1 .0499(14) .0192(10) .0508(16) -.0009(10) -.0047(12) -.0073(9)
H2 .0353(11) .0434(13) .0305(12) .0034(10) -.0131(9) .0052(9)
loop_
_atom_site_label
_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
Fe1 0.50072(10) .28033(5) 0.5 .00348 Uani 1
Na1 0.5 0 0.24608(11) .00718 Uani 1
Na2 0 0 0.37830(11) .00755 Uani 1
O1 0.88842(18) .40463(10) 0.5 .01003 Uani 1
O2 0.17127(13) .12264(7) 0.26864(5) .00951 Uani 1
N1 0.72780(10) .35789(5) 0.5 .00551 Uani 1
N2 0.09869(11) .12397(6) 0.5 .00885 Uani 1
N3 0.66723(8) .11947(4) 0.35808(3) .00888 Uani 1
N4 0.25050(8) .40551(4) 0.35527(3) .00991 Uani 1
C1 0.24923(15) .18302(8) 0.5 .00681 Uani 1
C2 0.60718(11) .17967(6) 0.41219(4) .00646 Uani 1
C3 0.34569(10) .36206(5) 0.41079(4) .0067 Uani 1
D1 0.1885(3) .19915(13) 0.28574(13) .02825 Uani .719(3)
D2 0.0625(3) .12385(15) 0.22471(11) .02575 Uani .730(3)
H1 0.1885(3) .19915(13) 0.28574(13) .03997 Uani .281(3)
H2 0.0625(3) .12385(15) 0.22471(11) .03642 Uani .270(3)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_source
Fe Fe GSAS
Na Na GSAS
O O GSAS
N N GSAS
C C GSAS
D D GSAS
H H GSAS
|
1100914.cif | #------------------------------------------------------------------------------
#$Date: 2022-09-14 17:31:13 +0300 (Wed, 14 Sep 2022) $
#$Revision: 277831 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/09/1100914.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_1100914
loop_
_publ_author_name
'Willis, Anthony C.'
'Beckwith, Athelstan L. J.'
'Tozer, Matthew J.'
_publ_section_title
;
trans-3-Benzoyl-2-(tert-butyl)-4-(iso-butyl)-1,3-oxazolidin-5-one
;
_journal_issue 11
_journal_name_full 'Acta Crystallographica Section C'
_journal_page_first 2276
_journal_page_last 2277
_journal_paper_doi 10.1107/S0108270191009630
_journal_volume 47
_journal_year 1991
_chemical_formula_moiety 'C18 H25 N O3'
_chemical_formula_sum 'C18 H25 N O3'
_chemical_formula_weight 303.40
_chemical_name_systematic
;
trans-3-Benzoyl-2-(tert-butyl)-4-(iso-butyl)-1,3-oxazolidin-5-one
;
_space_group_IT_number 19
_space_group_name_Hall 'P 2ac 2ab'
_space_group_name_H-M_alt 'P 21 21 21'
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall 'P 2ac 2ab'
_symmetry_space_group_name_H-M 'P 21 21 21'
_audit_creation_method 'from xtal archive file using CIFIO'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 5.959(1)
_cell_length_b 14.956(1)
_cell_length_c 19.737(3)
_cell_measurement_reflns_used 25
_cell_measurement_temperature 293
_cell_measurement_theta_max 31
_cell_measurement_theta_min 25
_cell_volume 1759.0(3)
_computing_cell_refinement 'LATCON (Xtal: Schwarzenback & King)'
_computing_data_collection 'Philips PW1100/20 software 1976'
_computing_data_reduction 'pwredu (McLaughlin) ADDREF SORTRF (Xtal)'
_computing_publication_material 'BONDLA CIFIO (Xtal: Hall)'
_computing_structure_refinement 'SHELX76 (Sheldrick) CRYLSQ (Xtal: Olthof)'
_computing_structure_solution 'SHELXS86 (Sheldrick)'
_diffrn_ambient_temperature 293
_diffrn_measurement_device 'Philips PW1100/20 diffractometer'
_diffrn_measurement_method \q/2\q
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'X-ray tube'
_diffrn_radiation_type 'Cu K\a'
_diffrn_radiation_wavelength 1.5418
_diffrn_reflns_av_R_equivalents 0
_diffrn_reflns_av_sigmaI/netI .027
_diffrn_reflns_limit_h_max 6
_diffrn_reflns_limit_h_min 0
_diffrn_reflns_limit_k_max 0
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_number 1592
_diffrn_reflns_theta_max 61.97
_diffrn_reflns_theta_min 3.71
_diffrn_standards_decay_% 0
_diffrn_standards_interval_time 120
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 0.59
_exptl_absorpt_correction_T_max .824
_exptl_absorpt_correction_T_min .933
_exptl_absorpt_correction_type 'shelx76 gaussian'
_exptl_crystal_colour colourless
_exptl_crystal_density_meas 1.146
_exptl_crystal_description prism
_exptl_crystal_F_000 656
_exptl_crystal_size_max 0.32
_exptl_crystal_size_mid 0.27
_exptl_crystal_size_min 0.10
_refine_diff_density_max .131
_refine_diff_density_min -.108
_refine_ls_abs_structure_details
;
The absolute configuration was assigned to agree with the known chirality
at C(3) arising from its precursor l-leucine.
;
_refine_ls_abs_structure_Flack 0
_refine_ls_extinction_coef 3514(42)
_refine_ls_extinction_expression
'equ(22) p292 "Crystallographic Computing" (1970)'
_refine_ls_extinction_method Zachariasen
_refine_ls_goodness_of_fit_all 1.462
_refine_ls_goodness_of_fit_obs 1.515
_refine_ls_hydrogen_treatment 'refxyz except H332B noref'
_refine_ls_matrix_type full
_refine_ls_number_constraints 0
_refine_ls_number_parameters 272
_refine_ls_number_reflns 1408
_refine_ls_number_restraints 0
_refine_ls_R_factor_all .038
_refine_ls_R_factor_obs .034
_refine_ls_shift/esd_max .535
_refine_ls_shift/esd_mean .044
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details 'w = 1/(\s^2^(F)+0.0004F^2^)'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_all .044
_refine_ls_wR_factor_obs .042
_reflns_number_observed 1408
_reflns_number_total 1592
_reflns_observed_criterion 'refl observed if F > 6.0 sigma(F)'
_cod_duplicate_entry 2000169
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_thermal_displace_type' tag value 'Uij' was replaced with
'Uani' value 22 times.
Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana
The following automatic conversions were performed:
'_refine_ls_weighting_scheme' value '1/(\s^2^(F)+0.0004F^2^)' 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^(F)+0.0004F^2^)'.
Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas
;
_cod_database_code 1100914
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2-x,-y,1/2+z
1/2+x,1/2-y,-z
-x,1/2+y,1/2-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_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
_atom_site_aniso_type_symbol
O1 .071(1) .076(1) .0342(9) .008(1) .0051(9) -.0030(9) O
C2 .060(2) .072(2) .047(1) .002(2) .013(1) -.009(1) C
C3 .038(1) .060(2) .044(1) .007(1) .001(1) -.005(1) C
N4 .037(1) .048(1) .0325(9) .0025(9) .0011(9) -.0011(9) N
C5 .043(1) .060(1) .032(1) .001(1) -.001(1) .001(1) C
O21 .094(2) .109(2) .068(1) .023(2) .038(1) -.010(1) O
C31 .061(2) .056(2) .060(2) .015(2) .005(2) -.002(1) C
C32 .075(2) .057(2) .087(2) -.005(2) .002(2) -.018(2) C
C321 .100(4) .127(4) .107(3) -.026(3) -.027(3) -.016(3) C
C322 .192(7) .084(3) .171(5) -.046(4) -.027(6) .017(3) C
C41 .037(1) .046(1) .040(1) -.004(1) .001(1) -.005(1) C
O41 .0360(9) .071(1) .054(1) .0066(9) .0028(8) .0015(9) O
C411 .042(1) .054(1) .034(1) -.000(1) .002(1) -.003(1) C
C412 .048(2) .098(2) .045(1) -.016(2) .003(1) .007(2) C
C413 .074(2) .133(3) .052(2) -.022(2) .008(2) .031(2) C
C414 .075(2) .118(3) .040(2) -.002(2) -.004(2) .014(2) C
C415 .057(2) .096(2) .043(2) -.003(2) -.008(1) -.003(1) C
C416 .049(2) .069(2) .041(1) -.010(2) -.001(1) -.002(1) C
C51 .048(2) .059(2) .049(1) .002(1) -.000(1) .007(1) C
C511 .048(2) .071(2) .097(3) -.008(2) -.003(2) .010(2) C
C512 .078(2) .083(2) .075(2) .009(2) -.005(2) .033(2) C
C513 .074(2) .055(2) .075(2) .004(2) .001(2) -.010(2) C
loop_
_atom_site_label
_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_calc_flag
_atom_site_calc_attached_atom
_atom_site_type_symbol
O1 .4154(4) .5699(1) .3026(0) .060(1) Uani ? ? O
C2 .5630(5) .5087(2) .3246(1) .060(2) Uani ? ? C
C3 .5350(5) .4920(2) .3997(1) .048(1) Uani ? ? C
N4 .3570(3) .5558(1) .4167(0) .039(1) Uani ? ? N
C5 .3000(5) .6122(2) .3581(1) .045(1) Uani ? ? C
O21 .6958(5) .4738(2) .2874(1) .090(2) Uani ? ? O
C31 .4869(6) .3929(2) .4143(2) .059(2) Uani ? ? C
C32 .2552(7) .3558(2) .3953(2) .073(2) Uani ? ? C
C321 .209(1) .3542(4) .3211(3) .111(4) Uani ? ? C
C322 .230(1) .2626(3) .4264(3) .149(5) Uani ? ? C
C41 .2034(4) .5476(2) .4682(1) .041(1) Uani ? ? C
O41 .0124(3) .5776(1) .4624(0) .054(1) Uani ? ? O
C411 .2826(4) .5093(2) .5334(1) .043(1) Uani ? ? C
C412 .1315(5) .4613(2) .5725(1) .064(2) Uani ? ? C
C413 .1914(7) .4324(3) .6366(2) .086(2) Uani ? ? C
C414 .3987(6) .4522(3) .6620(1) .078(2) Uani ? ? C
C415 .5494(6) .4997(2) .6241(1) .065(2) Uani ? ? C
C416 .4920(5) .5279(2) .5594(1) .053(2) Uani ? ? C
C51 .3745(5) .7097(2) .3634(1) .052(2) Uani ? ? C
C511 .6299(6) .7166(3) .3669(2) .072(2) Uani ? ? C
C512 .2881(8) .7581(3) .3000(2) .079(2) Uani ? ? C
C513 .2757(7) .7522(2) .4267(2) .068(2) Uani ? ? C
H3 .679(5) .510(2) .422(1) .06000 Uiso ? ? H
H5 .135(5) .608(2) .350(1) .06000 Uiso ? ? H
H31A .507(5) .381(2) .461(2) .07000 Uiso ? ? H
H31B .593(6) .357(2) .390(2) .07000 Uiso ? ? H
H32 .129(6) .401(3) .417(2) .09000 Uiso ? ? H
H321A .330(9) .311(4) .306(3) .14000 Uiso ? ? H
H321B .22(1) .415(4) .298(2) .14000 Uiso ? ? H
H321C .04(1) .318(3) .320(2) .14000 Uiso ? ? H
H322A .25(1) .272(4) .475(3) .19000 Uiso ? ? H
H322B .34976 .22118 .40954 .19000 Uiso calc C322 H
H322C .08(1) .234(4) .397(3) .19000 Uiso ? ? H
H412 -.007(6) .447(2) .552(2) .08000 Uiso ? ? H
H413 .096(7) .392(3) .661(2) .11000 Uiso ? ? H
H414 .447(7) .433(2) .708(2) .10000 Uiso ? ? H
H415 .722(6) .521(2) .641(2) .08000 Uiso ? ? H
H416 .588(5) .564(2) .535(1) .07000 Uiso ? ? H
H511A .683(7) .692(2) .322(2) .09000 Uiso ? ? H
H511B .689(6) .681(2) .408(2) .09000 Uiso ? ? H
H511C .678(7) .781(3) .372(2) .09000 Uiso ? ? H
H512A .143(8) .759(3) .302(2) .10000 Uiso ? ? H
H512B .345(7) .726(3) .258(2) .10000 Uiso ? ? H
H512C .361(7) .820(3) .302(2) .10000 Uiso ? ? H
H513A .337(6) .717(2) .469(2) .09000 Uiso ? ? H
H513B .115(7) .757(3) .426(2) .09000 Uiso ? ? H
H513C .329(6) .817(2) .430(2) .09000 Uiso ? ? H
loop_
_atom_type_symbol
_atom_type_number_in_cell
_atom_type_oxidation_number
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 72 0 .017 .009 International_Tables_Vol_IV_Table_2.2B
H 100 0 0 0 International_Tables_Vol_IV_Table_2.2B
O 12 0 .047 .032 International_Tables_Vol_IV_Table_2.2B
N 4 0 .029 .018 International_Tables_Vol_IV_Table_2.2B
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
3 2 4
1 9 1
3 0 10
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 O1 C5 . . . 111.6(2) yes
O1 C2 C3 . . . 110.9(2) yes
O1 C2 O21 . . . 122.2(3) yes
C3 C2 O21 . . . 127.0(3) yes
C2 C3 N4 . . . 101.3(2) yes
C2 C3 C31 . . . 111.3(2) yes
C2 C3 H3 . . . 107.0(10) ?
N4 C3 C31 . . . 116.7(2) yes
N4 C3 H3 . . . 110.0(10) ?
C31 C3 H3 . . . 110.0(10) ?
C3 N4 C5 . . . 111.2(2) yes
C3 N4 C41 . . . 126.4(2) yes
C5 N4 C41 . . . 118.6(2) yes
O1 C5 N4 . . . 103.6(2) yes
O1 C5 C51 . . . 109.4(2) yes
O1 C5 H5 . . . 109.0(10) ?
N4 C5 C51 . . . 115.3(2) yes
N4 C5 H5 . . . 109.0(10) ?
C51 C5 H5 . . . 111.0(10) ?
C3 C31 C32 . . . 118.1(3) yes
C3 C31 H31A . . . 110.0(10) ?
C3 C31 H31B . . . 109.0(10) ?
C32 C31 H31A . . . 107.0(10) ?
C32 C31 H31B . . . 105.0(10) ?
H31A C31 H31B . . . 108.0(10) ?
C31 C32 C321 . . . 114.5(4) yes
C31 C32 C322 . . . 108.6(4) yes
C31 C32 H32 . . . 107.0(10) ?
C321 C32 C322 . . . 111.2(4) yes
C321 C32 H32 . . . 105.0(10) ?
C322 C32 H32 . . . 110.0(10) ?
C32 C321 H321A . . . 99.0(10) ?
C32 C321 H321B . . . 114.0(10) ?
C32 C321 H321C . . . 101.0(10) ?
H321A C321 H321B . . . 113.0(10) ?
H321A C321 H321C . . . 109.0(10) ?
H321B C321 H321C . . . 119.0(10) ?
C32 C322 H322A . . . 104.0(10) ?
C32 C322 H322B . . . 111.1 ?
C32 C322 H322C . . . 103.0(10) ?
H322A C322 H322B . . . 108 ?
H322A C322 H322C . . . 131.0(10) ?
H322B C322 H322C . . . 99 ?
N4 C41 O41 . . . 121.0(2) yes
N4 C41 C411 . . . 117.6(2) yes
O41 C41 C411 . . . 121.1(2) yes
C41 C411 C412 . . . 118.4(2) yes
C41 C411 C416 . . . 122.2(2) yes
C412 C411 C416 . . . 119.0(2) yes
C411 C412 C413 . . . 120.3(3) yes
C411 C412 H412 . . . 117.0(10) ?
C413 C412 H412 . . . 123.0(10) ?
C412 C413 C414 . . . 120.1(3) yes
C412 C413 H413 . . . 120.0(10) ?
C414 C413 H413 . . . 119.0(10) ?
C413 C414 C415 . . . 120.4(3) yes
C413 C414 H414 . . . 122.0(10) ?
C415 C414 H414 . . . 117.0(10) ?
C414 C415 C416 . . . 120.0(3) yes
C414 C415 H415 . . . 126.0(10) ?
C416 C415 H415 . . . 114.0(10) ?
C411 C416 C415 . . . 120.4(3) yes
C411 C416 H416 . . . 119.0(10) ?
C415 C416 H416 . . . 120.0(10) ?
C5 C51 C511 . . . 110.9(3) yes
C5 C51 C512 . . . 107.3(3) yes
C5 C51 C513 . . . 110.0(2) yes
C511 C51 C512 . . . 109.9(3) yes
C511 C51 C513 . . . 108.7(3) yes
C512 C51 C513 . . . 110.0(3) yes
C51 C511 H511A . . . 104.0(10) ?
C51 C511 H511B . . . 110.0(10) ?
C51 C511 H511C . . . 111.0(10) ?
H511A C511 H511B . . . 113.0(10) ?
H511A C511 H511C . . . 111.0(10) ?
H511B C511 H511C . . . 108.0(10) ?
C51 C512 H512A . . . 108.0(10) ?
C51 C512 H512B . . . 109.0(10) ?
C51 C512 H512C . . . 105.0(10) ?
H512A C512 H512B . . . 112.0(10) ?
H512A C512 H512C . . . 114.0(10) ?
H512B C512 H512C . . . 108.0(10) ?
C51 C513 H513A . . . 108.0(10) ?
C51 C513 H513B . . . 114.0(10) ?
C51 C513 H513C . . . 109.0(10) ?
H513A C513 H513B . . . 113.0(10) ?
H513A C513 H513C . . . 108.0(10) ?
H513B C513 H513C . . . 104.0(10) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
O1 C2 . . 1.342(4) yes
O1 C5 . . 1.439(3) yes
C2 C3 . . 1.512(4) yes
C2 O21 . . 1.199(4) yes
C3 N4 . . 1.465(3) yes
C3 C31 . . 1.537(4) yes
C3 H3 . . 1.00(3) ?
N4 C5 . . 1.472(3) yes
N4 C41 . . 1.374(3) yes
C5 C51 . . 1.528(4) yes
C5 H5 . . 1.00(3) ?
C31 C32 . . 1.535(5) yes
C31 H31A . . .95(3) ?
C31 H31B . . .96(3) ?
C32 C321 . . 1.490(7) yes
C32 C322 . . 1.531(6) yes
C32 H32 . . 1.10(4) ?
C321 H321A . . 1.01(5) ?
C321 H321B . . 1.02(5) ?
C321 H321C . . 1.14(6) ?
C322 H322A . . .98(5) ?
C322 H322B . . 1.002 ?
C322 H322C . . 1.15(7) ?
C41 O41 . . 1.229(3) yes
C41 C411 . . 1.485(3) yes
C411 C412 . . 1.386(4) yes
C411 C416 . . 1.378(4) yes
C412 C413 . . 1.383(4) yes
C412 H412 . . .94(4) ?
C413 C414 . . 1.366(5) yes
C413 H413 . . .96(4) ?
C414 C415 . . 1.368(5) yes
C414 H414 . . 1.00(4) ?
C415 C416 . . 1.387(4) yes
C415 H415 . . 1.12(4) ?
C416 H416 . . .93(3) ?
C51 C511 . . 1.527(5) yes
C51 C512 . . 1.533(5) yes
C51 C513 . . 1.520(5) yes
C511 H511A . . 1.00(4) ?
C511 H511B . . 1.03(4) ?
C511 H511C . . 1.01(4) ?
C512 H512A . . .87(5) ?
C512 H512B . . 1.03(4) ?
C512 H512C . . 1.03(4) ?
C513 H513A . . 1.06(3) ?
C513 H513B . . .96(4) ?
C513 H513C . . 1.02(4) ?
|
1100915.cif | #------------------------------------------------------------------------------
#$Date: 2015-01-27 21:58:39 +0200 (Tue, 27 Jan 2015) $
#$Revision: 130149 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100915.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_1100915
loop_
_publ_author_name
'Mario Nardelli'
_chemical_formula_analytical 'C15 H22 O3'
_chemical_formula_sum 'C15 H22 O3'
_chemical_formula_weight 250.34
_symmetry_space_group_name_H-M ' P 21 c n '
_cell_angle_alpha 90.00(0)
_cell_angle_beta 90.00(0)
_cell_angle_gamma 90.00(0)
_cell_formula_units_Z 4.00
_cell_length_a 11.891(6)
_cell_length_b 11.954(5)
_cell_length_c 9.387(6)
_cell_volume 1334.(1)
_computing_publication_material
;
PARST (Nardelli, 1983); PARSTCIF (Nardelli, 1991)
;
_diffrn_ambient_temperature ?
_diffrn_radiation_wavelength 0.71069
_exptl_absorpt_coefficient_mu 0.0851
_exptl_absorpt_correction_T_max ?
_exptl_absorpt_correction_T_min ?
_exptl_absorpt_correction_type ?
_exptl_crystal_density_diffrn 1.2462
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_F_000 544.0
_cod_database_code 1100915
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
O1 0.0568(12) 0.0651(11) 0.0650(10) 0.0143(9) -0.0125(10) 0.0181(10)
O2 0.0402(9) 0.0333(8) 0.0426(8) 0.0016(7) 0.0033(8) -0.0077(7)
O3 0.0601(12) 0.0618(10) 0.0528(10) -0.0004(9) 0.0156(9) -0.0075(9)
C1 0.0331(13) 0.0368(12) 0.0427(12) 0.0007(10) 0.0041(12) -0.0003(11)
C2 0.0375(14) 0.0377(11) 0.0497(13) 0.0064(11) -0.0016(12) -0.0053(11)
C3 0.0426(14) 0.0350(12) 0.0384(13) 0.0019(9) -0.0036(11) -0.0060(12)
C4 0.0659(19) 0.0502(16) 0.0411(14) 0.0062(12) 0.0068(15) -0.0031(14)
C5 0.0711(20) 0.0561(18) 0.0453(16) -0.0033(13) 0.0156(15) -0.0035(16)
C6 0.0522(16) 0.0493(16) 0.0606(17) -0.0059(12) 0.0135(15) 0.0031(15)
C7 0.0428(15) 0.0413(15) 0.0483(16) -0.0027(12) 0.0013(12) 0.0030(13)
C8 0.0347(13) 0.0321(12) 0.0394(13) 0.0001(10) -0.0003(10) -0.0041(11)
C9 0.0344(12) 0.0305(11) 0.0374(12) 0.0000(10) -0.0007(10) -0.0060(11)
C10 0.0455(15) 0.0408(13) 0.0405(14) 0.0042(11) -0.0032(12) -0.0031(13)
C11 0.0491(16) 0.0506(14) 0.0401(15) -0.0021(13) -0.0053(13) -0.0065(13)
C12 0.0607(18) 0.0476(16) 0.0481(15) -0.0105(12) 0.0065(14) -0.0069(13)
C13 0.0545(18) 0.0329(12) 0.0566(16) -0.0028(11) 0.0019(13) 0.0030(13)
C14 0.0406(14) 0.0449(13) 0.0417(12) 0.0121(10) -0.0038(13) -0.0027(12)
C15 0.0507(16) 0.0489(14) 0.0669(16) 0.0131(12) -0.0043(12) -0.0163(13)
loop_
_atom_site_label
_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_type_symbol
_atom_site_calc_flag
_atom_site_calc_attached_atom
_atom_site_aniso_ratio
O1 0.92230(0) 0.3802(1) 0.2549(2) 0.0623(6) aniso O . . 2.56
O2 0.8321(2) 0.6593(1) 0.0331(1) 0.0387(5) aniso O . . 1.68
O3 0.9534(2) 0.6357(1) -0.1497(2) 0.0582(6) aniso O . . 1.91
C1 0.8458(3) 0.4532(2) 0.0333(2) 0.0376(7) aniso C . . 1.40
C2 0.8584(2) 0.4434(2) 0.1943(2) 0.0416(7) aniso C . . 1.69
C3 0.7766(3) 0.5225(2) 0.2637(2) 0.0387(7) aniso C . . 1.50
C4 0.7183(3) 0.4911(2) 0.4015(3) 0.0524(9) aniso C . . 1.88
C5 0.6400(3) 0.5864(2) 0.4446(3) 0.0575(10) aniso C . . 2.10
C6 0.5594(3) 0.6196(2) 0.3259(3) 0.0540(10) aniso C . . 1.83
C7 0.6196(3) 0.6482(2) 0.1864(3) 0.0442(10) aniso C . . 1.29
C8 0.6938(3) 0.5496(2) 0.1450(2) 0.0354(7) aniso C . . 1.36
C9 0.7679(3) 0.5542(2) 0.0118(2) 0.0341(7) aniso C . . 1.49
C10 0.7058(3) 0.5596(2) -0.1301(3) 0.0422(8) aniso C . . 1.36
C11 0.6552(3) 0.4477(2) -0.1707(3) 0.0466(9) aniso C . . 1.57
C12 0.7439(3) 0.3563(2) -0.1701(3) 0.0521(9) aniso C . . 1.85
C13 0.7935(3) 0.3432(2) -0.0230(3) 0.0480(9) aniso C . . 1.80
C14 0.9193(3) 0.6887(2) -0.0503(2) 0.0424(8) aniso C . . 1.84
C15 0.9695(3) 0.7957(2) 0.0013(3) 0.0555(9) aniso C . . 2.47
H15A 0.9950(15) 0.7865(5) 0.0987(8) 0.1227(74) iso H . C15 1.00
H15B 0.9134(5) 0.8545(4) -0.0027(20) 0.1227(74) iso H . C15 1.00
H15C 1.0329(11) 0.8157(9) -0.0587(13) 0.1227(74) iso H . C15 1.00
H1 0.9143(19) 0.4632(14) -0.0121(18) 0.0304(51) iso H . C1 1.00
H3 0.8213(20) 0.5888(18) 0.2800(21) 0.0468(63) iso H . C3 1.00
H41 0.7745(21) 0.4744(20) 0.4779(28) 0.0672(79) iso H . C4 1.00
H42 0.6779(20) 0.4192(20) 0.3806(22) 0.0514(68) iso H . C4 1.00
H51 0.6858(21) 0.6505(20) 0.4681(22) 0.0488(68) iso H . C5 1.00
H52 0.5958(22) 0.5651(20) 0.5364(27) 0.0705(79) iso H . C5 1.00
H61 0.5075(21) 0.5566(20) 0.3076(24) 0.0638(80) iso H . C6 1.00
H62 0.5056(23) 0.6850(21) 0.3504(28) 0.0791(83) iso H . C6 1.00
H71 0.5629(22) 0.6660(17) 0.1103(22) 0.0492(63) iso H . C7 1.00
H72 0.6687(19) 0.7145(18) 0.2088(24) 0.0462(64) iso H . C7 1.00
H8 0.6450(17) 0.4830(16) 0.1330(20) 0.0302(55) iso H . C8 1.00
H101 0.6432(21) 0.6120(20) -0.1228(23) 0.0542(72) iso H . C10 1.00
H102 0.7641(20) 0.5837(17) -0.2048(24) 0.0514(65) iso H . C10 1.00
H111 0.6210(19) 0.4544(19) -0.2602(30) 0.0643(78) iso H . C11 1.00
H112 0.5981(20) 0.4261(18) -0.0991(25) 0.0516(72) iso H . C11 1.00
H121 0.8069(20) 0.3743(16) -0.2366(20) 0.0419(66) iso H . C12 1.00
H122 0.7124(21) 0.2790(21) -0.1924(27) 0.0624(74) iso H . C12 1.00
H131 0.8478(21) 0.2883(20) -0.0197(24) 0.0597(81) iso H . C13 1.00
H132 0.7309(23) 0.3176(20) 0.0497(25) 0.0697(83) iso H . C13 1.00
loop_
_atom_type_symbol
_atom_type_number_in_cell
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
'O ' 12 'Oxygen ' 0.0106 0.0060 'Int. Tab. C, 4.2.6.8, 6.1.1.4'
'C ' 60 'Carbon ' 0.0033 0.0016 'Int. Tab. C, 4.2.6.8, 6.1.1.4'
'H ' 88 'Hydrogen ' 0.0000 0.0000 'Int. Tab. C, 4.2.6.8, 6.1.1.4'
loop_
_diffrn_attenuator_code
_diffrn_attenuator_scale
? ?
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?
|
1100916.cif | #------------------------------------------------------------------------------
#$Date: 2015-04-02 14:22:18 +0300 (Thu, 02 Apr 2015) $
#$Revision: 134621 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100916.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_1100916
loop_
_publ_author_name
'Fabry, Jan'
'Zikmund, Zdenek'
'Kania, Antoni'
'Petricek, Vaclav'
_publ_section_title
;
Structural study of AgNbO~3~ at room temperature
;
_journal_name_full 'Acta Crystallographica, Section C'
_journal_page_first 916
_journal_page_last 918
_journal_paper_doi 10.1107/S0108270100006806
_journal_volume 56
_journal_year 2000
_chemical_formula_iupac 'Ag Nb O3'
_chemical_formula_moiety 'Ag Nb O3'
_chemical_formula_structural 'Ag Nb O3'
_chemical_formula_sum 'Ag Nb O3'
_chemical_formula_weight 248.77
_chemical_name_systematic
;
silver niobate
;
_space_group_IT_number 57
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall '-P 2c 2b'
_symmetry_space_group_name_H-M 'P b c m'
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 8
_cell_length_a 5.5462(3)
_cell_length_b 5.6028(4)
_cell_length_c 15.6365(13)
_cell_measurement_reflns_used 50
_cell_measurement_temperature 292.0(10)
_cell_measurement_theta_max 33
_cell_measurement_theta_min 5
_cell_volume 485.90(6)
_diffrn_measurement_device 'Hilger & Watts'
_diffrn_measurement_method \w/2\q
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength .71073
_diffrn_reflns_av_R_equivalents .025
_diffrn_reflns_limit_h_max 7
_diffrn_reflns_limit_h_min -7
_diffrn_reflns_limit_k_max 7
_diffrn_reflns_limit_k_min -7
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_number 5156
_diffrn_reflns_theta_full 30
_diffrn_reflns_theta_max 30
_diffrn_standards_decay_% 7.0
_diffrn_standards_interval_count 30
_diffrn_standards_interval_time ?
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 12.492
_exptl_absorpt_correction_T_max .356
_exptl_absorpt_correction_T_min .130
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details '(Templeton & Templeton, 1978)'
_exptl_crystal_colour 'light brown'
_exptl_crystal_density_diffrn 6.799
_exptl_crystal_density_meas ?
_exptl_crystal_density_method .
_exptl_crystal_description prism
_exptl_crystal_F_000 896
_exptl_crystal_size_max .31
_exptl_crystal_size_mid .17
_exptl_crystal_size_min .09
_refine_diff_density_max 1.20
_refine_diff_density_min -3.65
_refine_ls_extinction_coef .000228(4)
_refine_ls_extinction_method 'type II (Becker & Coppens, 1974)'
_refine_ls_goodness_of_fit_all 2.69
_refine_ls_goodness_of_fit_ref 2.84
_refine_ls_hydrogen_treatment none
_refine_ls_matrix_type fullcycle
_refine_ls_number_constraints 0
_refine_ls_number_parameters 52
_refine_ls_number_reflns 1689
_refine_ls_R_factor_gt .034
_refine_ls_shift/su_max .01
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details 'w = (\s^2^(F~o~)+0.0001(F~o~)^2^)^-1^'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_ref .053
_reflns_number_gt 1497
_reflns_number_total 1689
_reflns_threshold_expression I>3\s(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Gaussian' changed to 'gaussian'
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:
'_refine_ls_weighting_scheme' value 'w =
(\s^2^(F~o~)+0.0001(F~o~)^2^)^-1^' was changed to 'calc'. New tag
'_refine_ls_weighting_details' was created. The value of the new tag
was set to 'w = (\s^2^(F~o~)+0.0001(F~o~)^2^)^-1^'.
Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas
;
_cod_database_code 1100916
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, y, -z+1/2'
'-x, y+1/2, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'-x, -y, z+1/2'
'x, -y+1/2, -z'
'x, -y+1/2, z+1/2'
loop_
_atom_site_U_iso_or_equiv
_atom_site_label
_atom_site_fract_z
_atom_site_fract_x
_atom_site_fract_y
_atom_site_adp_type
_atom_site_occupancy
_atom_site_type_symbol
.01280(10) Ag1 0.75 .75770(3) 0.22738(7) Uani 1 Ag
.01280(10) Ag2 0.5 .75550(3) 0.25 Uani 1 Ag
.00590(10) Nb 0.625014(8) .74525(2) 0.72338(7) Uani 1 Nb
.0090(4) O1 0.75 .6978(2) 0.7664(2) Uani 1 O
.0095(4) O2 0.5 .8043(2) 0.75 Uani 1 O
.0088(3) O3 0.61132(6) .4662(2) 0.5364(2) Uani 1 O
.0092(3) O4 0.63865(7) -.0334(2) 0.4727(2) Uani 1 O
loop_
_atom_site_aniso_label
_atom_site_aniso_U_22
_atom_site_aniso_U_11
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
_atom_site_aniso_type_symbol
Ag1 .0123(2) .0128(2) .0133(2) -.00211(4) .0000 .0000 Ag
Ag2 .01410(10) .0113(2) .0130(2) .0000 .0000 .00107(7) Ag
Nb .0040(2) .0051(2) .0085(2) -.00014(3) -.00061(4) .00031(4) Nb
O1 .0119(7) .0118(6) .0031(7) .0009(4) .0000 .0000 O
O2 .0127(6) .0100(6) .0059(7) .0000 .0000 .0004(4) O
O3 .0084(5) .0064(4) .0115(5) -.0033(3) -.0013(3) .0014(3) O
O4 .0077(5) .0086(4) .0114(5) .0030(3) .0010(3) .0013(3) O
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ag -.897 1.102 International_Tables_vol_IV_Table_2.2A_and_2.3.1
Nb -2.073 .622 International_Tables_vol_IV_Table_2.2A_and_2.3.1
O .011 .006 International_Tables_vol_IV_Table_2.2A_and_2.3.1
|
1100917.cif | #------------------------------------------------------------------------------
#$Date: 2015-04-02 14:22:18 +0300 (Thu, 02 Apr 2015) $
#$Revision: 134621 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100917.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_1100917
loop_
_publ_author_name
'Fabry, Jan'
'Zikmund, Zdenek'
'Kania, Antoni'
'Petricek, Vaclav'
_publ_section_title
;
Structural study of AgNbO~3~ at room temperature
;
_journal_name_full 'Acta Crystallographica, Section C'
_journal_page_first 916
_journal_page_last 918
_journal_paper_doi 10.1107/S0108270100006806
_journal_volume 56
_journal_year 2000
_chemical_formula_iupac 'Ag Nb O3'
_chemical_formula_moiety 'Ag Nb O3'
_chemical_formula_structural 'Ag Nb O3'
_chemical_formula_sum 'Ag Nb O3'
_chemical_formula_weight 248.77
_chemical_name_systematic
;
silver niobate
;
_space_group_IT_number 57
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall '-P 2c 2b'
_symmetry_space_group_name_H-M 'P b c m'
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 8
_cell_length_a 5.5462(3)
_cell_length_b 5.6028(4)
_cell_length_c 15.6365(13)
_cell_measurement_reflns_used 50
_cell_measurement_temperature 292.0(10)
_cell_measurement_theta_max 33
_cell_measurement_theta_min 5
_cell_volume 485.90(6)
_diffrn_measurement_device 'Hilger & Watts'
_diffrn_measurement_method \w/2\q
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength .71073
_diffrn_reflns_av_R_equivalents .025
_diffrn_reflns_limit_h_max 7
_diffrn_reflns_limit_h_min -7
_diffrn_reflns_limit_k_max 7
_diffrn_reflns_limit_k_min -7
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_number 5156
_diffrn_reflns_theta_full 30
_diffrn_reflns_theta_max 30
_diffrn_standards_decay_% 7.0
_diffrn_standards_interval_count 30
_diffrn_standards_interval_time ?
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 12.492
_exptl_absorpt_correction_T_max .356
_exptl_absorpt_correction_T_min .130
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details '(Templeton & Templeton, 1978)'
_exptl_crystal_colour 'light brown'
_exptl_crystal_density_diffrn 6.799
_exptl_crystal_density_meas ?
_exptl_crystal_density_method .
_exptl_crystal_description prism
_exptl_crystal_F_000 896
_exptl_crystal_size_max .31
_exptl_crystal_size_mid .17
_exptl_crystal_size_min .09
_refine_diff_density_max 1.20
_refine_diff_density_min -3.65
_refine_ls_extinction_coef .000228(4)
_refine_ls_extinction_method 'type II (Becker & Coppens, 1974)'
_refine_ls_goodness_of_fit_all 2.69
_refine_ls_goodness_of_fit_ref 2.84
_refine_ls_hydrogen_treatment none
_refine_ls_matrix_type fullcycle
_refine_ls_number_constraints 0
_refine_ls_number_parameters 52
_refine_ls_number_reflns 1689
_refine_ls_R_factor_gt .034
_refine_ls_shift/su_max .01
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details 'w = (\s^2^(F~o~)+0.0001(F~o~)^2^)^-1^'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_ref .053
_reflns_number_gt 1497
_reflns_number_total 1689
_reflns_threshold_expression I>3\s(I)
_cod_duplicate_entry 1100916
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Gaussian' changed to 'gaussian'
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:
'_refine_ls_weighting_scheme' value 'w =
(\s^2^(F~o~)+0.0001(F~o~)^2^)^-1^' was changed to 'calc'. New tag
'_refine_ls_weighting_details' was created. The value of the new tag
was set to 'w = (\s^2^(F~o~)+0.0001(F~o~)^2^)^-1^'.
Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas
;
_cod_database_code 1100917
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, y, -z+1/2'
'-x, y+1/2, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'-x, -y, z+1/2'
'x, -y+1/2, -z'
'x, -y+1/2, z+1/2'
loop_
_atom_site_label
_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_type_symbol
Ag1 .75770(3) 0.22738(7) 0.75 .01280(10) Uani 1 Ag
Ag2 .75550(3) 0.25 0.5 .01280(10) Uani 1 Ag
Nb .74525(2) 0.72338(7) 0.625014(8) .00590(10) Uani 1 Nb
O1 .6978(2) 0.7664(2) 0.75 .0090(4) Uani 1 O
O2 .8043(2) 0.75 0.5 .0095(4) Uani 1 O
O3 .4662(2) 0.5364(2) 0.61132(6) .0088(3) Uani 1 O
O4 -.0334(2) 0.4727(2) 0.63865(7) .0092(3) Uani 1 O
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
_atom_site_aniso_type_symbol
Ag1 .0128(2) .0123(2) .0133(2) -.00211(4) .0000 .0000 Ag
Ag2 .0113(2) .01410(10) .0130(2) .0000 .0000 .00107(7) Ag
Nb .0051(2) .0040(2) .0085(2) -.00014(3) -.00061(4) .00031(4) Nb
O1 .0118(6) .0119(7) .0031(7) .0009(4) .0000 .0000 O
O2 .0100(6) .0127(6) .0059(7) .0000 .0000 .0004(4) O
O3 .0064(4) .0084(5) .0115(5) -.0033(3) -.0013(3) .0014(3) O
O4 .0086(4) .0077(5) .0114(5) .0030(3) .0010(3) .0013(3) O
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ag -.897 1.102 International_Tables_vol_IV_Table_2.2A_and_2.3.1
Nb -2.073 .622 International_Tables_vol_IV_Table_2.2A_and_2.3.1
O .011 .006 International_Tables_vol_IV_Table_2.2A_and_2.3.1
|
1100918.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100918.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_1100918
loop_
_publ_author_name
'Yuji Ohashi'
'Kazunori Yanagi'
'Toshiharu Kurihara'
'Yoshio Sasada'
'Yoshiaki Ohgo'
_publ_section_title
;
Crystalline state reaction of cobaloxime complexes by x-ray exposure.
1. Direct observation of cobalt-carbon bond cleavage in
[(R)-1-cyanoethyl][(S)-(-)-.alpha.-methylbenzylamine]
bis(dimethylglyoximato)cobalt(III)
;
_journal_name_full 'Journal of the American Chemical Society'
_journal_page_first 5805
_journal_page_last 5812
_journal_paper_doi 10.1021/ja00409a031
_journal_volume 103
_journal_year 1981
_chemical_formula_sum 'C19 H29 Co N6 O4'
_space_group_IT_number 4
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall 'P 2yb'
_symmetry_space_group_name_H-M 'P 1 21 1'
_cell_angle_alpha 90
_cell_angle_beta 99.06
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 8.638
_cell_length_b 13.833
_cell_length_c 9.537
_cod_original_sg_symbol_H-M 'P 21'
_cod_original_formula_sum 'C19 H29 Co1 N6 O4'
_cod_database_code 1100918
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
Co1 Co 0.00750 0.25000 0.26950
N1 N 0.16660 0.15510 0.29220
N2 N 0.01220 0.22320 0.46390
N3 N -0.15420 0.34340 0.24460
N4 N 0.00460 0.27750 0.07580
O1 O 0.24160 0.12700 0.18550
O2 O -0.09040 0.26160 0.54130
O3 O -0.23870 0.36410 0.34580
O4 O 0.10350 0.23370 -0.00340
C1 C 0.20390 0.11820 0.41730
C2 C 0.11090 0.15870 0.52000
C3 C -0.18660 0.38110 0.11970
C4 C -0.09170 0.34360 0.01840
C5 C 0.32810 0.04300 0.45440
C6 C 0.12490 0.12270 0.67060
C7 C -0.31870 0.44990 0.07540
C8 C -0.10440 0.37580 -0.13250
N5 N -0.16290 0.14220 0.23420
C9 C -0.20320 0.08780 0.10030
C10 C -0.28600 -0.00770 0.13100
C11 C -0.30360 0.14390 -0.01240
C12 C -0.44060 0.18960 0.00710
C13 C -0.53490 0.23640 -0.10150
C14 C -0.49120 0.23560 -0.23620
C15 C -0.36410 0.18950 -0.26090
C16 C -0.26810 0.14330 -0.15140
C17 C 0.17150 0.35600 0.31970
C18 C 0.13490 0.41510 0.43680
N6 N 0.10820 0.46550 0.51960
C19 C 0.33090 0.34040 0.30750
H1 H 0.14200 0.18300 0.03400
H2 H -0.16200 0.29900 0.46800
H3 H 0.33200 0.01000 0.53300
H4 H 0.40600 0.07600 0.42500
H5 H 0.32000 -0.00300 0.40000
H6 H 0.02500 0.09600 0.68000
H7 H 0.10800 0.17500 0.70900
H8 H 0.22800 0.13200 0.70800
H9 H -0.36300 0.47200 0.16300
H10 H -0.26800 0.51100 0.07200
H11 H -0.38600 0.44100 -0.00300
H12 H -0.10500 0.44300 -0.15100
H13 H -0.16500 0.33600 -0.20200
H14 H -0.04300 0.36200 -0.18400
H15 H -0.15000 0.08500 0.28900
H16 H -0.24900 0.17500 0.26800
H17 H -0.09800 0.07700 0.08400
H18 H -0.34600 0.00500 0.19500
H19 H -0.20400 -0.04500 0.20200
H20 H -0.30700 -0.04900 0.03100
H21 H -0.46900 0.17800 0.10000
H22 H -0.64700 0.27600 -0.08500
H23 H -0.55500 0.26600 -0.31700
H24 H -0.33800 0.18500 -0.34300
H25 H -0.17500 0.12000 -0.14700
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
Co 1.33
N 0.68
O 0.68
|
1100919.cif | #------------------------------------------------------------------------------
#$Date: 2020-03-17 13:52:12 +0200 (Tue, 17 Mar 2020) $
#$Revision: 249449 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/09/1100919.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_1100919
_chemical_formula_sum 'C2 O S'
_chemical_formula_weight 18.0218
_space_group_crystal_system hexagonal
_space_group_IT_number 178
_space_group_name_Hall 'P 61 2 (0 0 5)'
_space_group_name_H-M_alt 'P 61 2 2'
_cell_angle_alpha 90.000(10)
_cell_angle_beta 90.000(10)
_cell_angle_gamma 120.000(10)
_cell_formula_units_Z 6
_cell_length_a 8.530(10)
_cell_length_b 8.530(10)
_cell_length_c 20.370(10)
_cell_measurement_temperature 293
_cell_volume 1284(3)
_computing_data_reduction 'xtal ADDREF SORTRF'
_computing_molecular_graphics xtal
_computing_publication_material 'xtal BONDLA CIFIO'
_computing_structure_refinement 'xtal CRYLSQ'
_computing_structure_solution 'xtal GENTAN'
_diffrn_ambient_temperature 293
_diffrn_radiation_type 'Cu K\a'
_diffrn_radiation_wavelength 1.5418
_diffrn_reflns_av_sigmaI/netI .094
_diffrn_reflns_limit_h_max 2
_diffrn_reflns_limit_h_min 0
_diffrn_reflns_limit_k_max 4
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_l_max 12
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_number 92
_diffrn_reflns_theta_max 28.96
_diffrn_reflns_theta_min 5.99
_exptl_absorpt_coefficient_mu 2.549
_exptl_crystal_density_diffrn .56
_exptl_crystal_density_meas 1.234
_exptl_crystal_F_000 216
_refine_diff_density_max .182
_refine_diff_density_min -.182
_refine_ls_extinction_coef 5782(1247)
_refine_ls_extinction_expression 'Eq22 p292 "Cryst. Comp." Munksgaard 1970'
_refine_ls_extinction_method Zachariasen
_refine_ls_goodness_of_fit_all 1.42
_refine_ls_goodness_of_fit_ref .801
_refine_ls_matrix_type full
_refine_ls_number_constraints 0
_refine_ls_number_parameters 16
_refine_ls_number_reflns 81
_refine_ls_number_restraints 0
_refine_ls_R_factor_all .055
_refine_ls_R_factor_gt .045
_refine_ls_shift/su_max 2.032
_refine_ls_shift/su_mean .272
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme sigma
_refine_ls_wR_factor_all .114
_refine_ls_wR_factor_ref .061
_reflns_d_resolution_high 1.592
_reflns_d_resolution_low 7.376
_reflns_Friedel_coverage 0
_reflns_limit_h_max 2
_reflns_limit_h_min 0
_reflns_limit_k_max 4
_reflns_limit_k_min 0
_reflns_limit_l_max 12
_reflns_limit_l_min 0
_reflns_number_gt 81
_reflns_number_total 92
_reflns_threshold_expression 'F > .00 sig(F )'
_cod_data_source_file p6122.cif
_cod_data_source_block p6122
loop_
_cod_entry_issue_id
_cod_entry_issue_origin
_cod_entry_issue_severity
_cod_entry_issue_description
1 deposition error
;
This entry is one of the GNU Xtal software test files. It describes
a hypothetical structure in an awkward high symmetry. The original
'p6122.cif' file and a related 'p6122.dat' file that contains a short
description of the tests in the file header can be found at:
http://www.iucr.org/__data/iucr/cif/software/xtal/xtal/dat/p6122.cif
;
_cod_original_sg_symbol_Hall p_61_2_(0_0_5)
_cod_original_sg_symbol_H-M P_61_2_2
_cod_original_formula_sum 'C.5 O.25 S.25'
_cod_original_formula_units_Z 24
_cod_database_code 1100919
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +x,+y,+z
2 -x,-y,1/2+z
3 -y,-x,5/6-z
4 +y,+x,1/3-z
5 +x-y,-y,-z
6 -x+y,+y,1/2-z
7 +x,+x-y,1/6-z
8 -x,-x+y,2/3-z
9 -y,+x-y,1/3+z
10 +y,-x+y,5/6+z
11 +x-y,+x,1/6+z
12 -x+y,-x,2/3+z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S .2013(4) .7987(4) .91667 .030(6) Uani ? ? 1.00000 ? ?
O .501(2) .501(2) .66667 .082(14) Uani ? ? 1.00000 ? ?
C1 .492(3) .098(3) .0379(11) .03170 Uani ? ? .97(5) ? ?
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
S .042(8) .042(8) .011(7) .025(7) -.004(6) -.004(6)
O .087(18) .087(18) .09(2) .060(19) .011(8) -.011(8)
C1 .03170 .03170 .03170 .01585 .00000 .00000
loop_
_atom_type_symbol
_atom_type_description
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
S ? 0 6 .319 .557 'Int Tab Vol III p202 Tab. 3.3.1a'
O ? 0 6 .047 .032 'Int Tables Vol IV Tables 2.2B and 2.3.1'
C ? 0 12 .017 .009 'Int Tables Vol IV Tables 2.2B and 2.3.1'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C1 S O . . . 19.35(19) ?
C1 S C1 '2 665' '6 556' '8 665' 134.2(12) ?
C1 O C1 '12 665' . '8 665' 132(2) ?
O C1 S . '8 665' '6 556' 159(2) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 S . . 19.42(2) ?
S C1 '6 556' '2 665' 1.70(2) ?
S C1 '6 556' '8 665' 1.70(2) ?
O C1 . '12 665' 1.16(2) ?
O C1 . '8 665' 1.16(2) ?
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
S C1 1.70(2) 3 '8 665' ?
S C1 1.70(2) 3 '8 665' ?
S O 2.812(17) 3 . ?
S O 2.812(17) 3 . ?
S O 2.812(17) 3 . ?
S O 2.813(17) 3 . ?
C1 C1 2.11(3) '8 665' '12 665' ?
S O 2.81(3) '6 556' '7 566' ?
S O 2.813(15) '6 556' . ?
C1 C1 3.14(4) '8 665' '2 665' ?
S C1 3.53(4) '6 556' '6 665' ?
S C1 3.53(2) '6 556' '12 665' ?
O C1 4.29(4) . '3 665' ?
O C1 4.29(4) . '2 665' ?
S S 4.514(4) '6 556' '2 674' ?
S S 4.514(4) '6 556' '8 656' ?
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C1 S C1 O '2 665' '6 556' '8 665' . -164(6) ?
C1 O C1 S '12 665' . '8 665' '6 556' 7(9) ?
|
1100920.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100920.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_1100920
_chemical_formula_sum 'C64 H42.5 Cu1.5 N4 O9'
_chemical_formula_weight 1106.83
_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
_cell_angle_alpha 90.00
_cell_angle_beta 104.81(3)
_cell_angle_gamma 90.00
_cell_formula_units_Z 8
_cell_length_a 27.543(8)
_cell_length_b 13.226(6)
_cell_length_c 31.171(13)
_cell_measurement_reflns_used ?
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max ?
_cell_measurement_theta_min ?
_cell_volume 10977.9(75)
_diffrn_ambient_temperature 213
_diffrn_measurement_device ?
_diffrn_measurement_method ?
_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 0.0714
_diffrn_reflns_av_sigmaI/netI 0.1056
_diffrn_reflns_limit_h_max 29
_diffrn_reflns_limit_h_min -23
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 33
_diffrn_reflns_limit_l_min -34
_diffrn_reflns_number 12907
_diffrn_reflns_theta_max 23.46
_diffrn_reflns_theta_min 1.35
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 0.649
_exptl_absorpt_correction_T_max ?
_exptl_absorpt_correction_T_min ?
_exptl_absorpt_correction_type ?
_exptl_crystal_colour ?
_exptl_crystal_density_diffrn 1.339
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description ?
_exptl_crystal_F_000 4560
_exptl_crystal_size_max 0.20
_exptl_crystal_size_mid 0.20
_exptl_crystal_size_min 0.25
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_all 1.268
_refine_ls_goodness_of_fit_obs 1.490
_refine_ls_hydrogen_treatment ?
_refine_ls_matrix_type full
_refine_ls_number_parameters 688
_refine_ls_number_reflns 7560
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.284
_refine_ls_restrained_S_obs 1.490
_refine_ls_R_factor_all 0.1743
_refine_ls_R_factor_obs 0.0973
_refine_ls_shift/esd_max -1.322
_refine_ls_shift/esd_mean 0.098
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1282P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_all 0.2917
_refine_ls_wR_factor_obs 0.2448
_reflns_number_observed 4177
_reflns_number_total 7564
_reflns_observed_criterion >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
The following automatic conversions were performed:
'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1282P)^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^)+(0.1282P)^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 C2/c
_cod_original_formula_sum 'C64 H42.50 Cu1.50 N4 O9'
_cod_database_code 1100920
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_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 0.0581(7) 0.0923(10) 0.1146(11) -0.0274(8) 0.0275(7) 0.0282(7)
Cu2 0.0646(14) 0.077(2) 0.081(2) -0.0015(13) 0.0210(12) -0.0090(13)
O1 0.039(3) 0.057(3) 0.063(3) -0.008(3) 0.023(3) -0.012(3)
O2 0.051(3) 0.068(4) 0.064(4) -0.001(3) 0.025(3) 0.003(3)
O4 0.030(3) 0.087(4) 0.042(3) 0.000(3) 0.010(2) -0.007(3)
O5 0.044(3) 0.049(3) 0.048(3) -0.001(2) 0.004(3) -0.009(3)
O6 0.053(3) 0.043(3) 0.051(3) 0.005(2) 0.006(3) -0.009(3)
O7 0.047(3) 0.046(3) 0.051(3) 0.003(3) -0.001(3) -0.012(3)
N3 0.044(4) 0.071(5) 0.048(4) -0.004(3) 0.008(3) -0.001(4)
N4 0.056(4) 0.052(5) 0.075(5) -0.003(4) 0.015(4) 0.013(4)
C1 0.060(8) 0.308(23) 0.174(15) -0.137(16) -0.024(9) 0.042(11)
C2 0.115(14) 0.255(19) 0.137(12) -0.133(13) -0.023(11) 0.033(14)
C3 0.128(12) 0.205(16) 0.075(8) -0.060(9) 0.015(8) 0.036(12)
C4 0.083(7) 0.104(8) 0.066(7) -0.011(6) 0.023(6) 0.015(6)
C5 0.049(5) 0.081(6) 0.052(5) -0.012(5) 0.010(4) 0.019(5)
C6 0.049(5) 0.052(5) 0.053(5) 0.001(4) 0.023(4) 0.020(4)
C7 0.051(5) 0.066(6) 0.051(5) 0.005(4) 0.014(4) 0.016(4)
C8 0.054(5) 0.071(6) 0.077(7) 0.010(5) 0.005(5) 0.010(5)
C9 0.095(8) 0.072(6) 0.057(6) -0.001(5) 0.007(6) 0.016(6)
C10 0.079(7) 0.073(6) 0.063(6) 0.002(5) 0.022(5) 0.022(5)
C11 0.049(6) 0.114(10) 0.072(7) 0.014(6) 0.004(5) -0.013(6)
C12 0.089(8) 0.072(8) 0.088(8) 0.002(6) -0.008(7) -0.028(7)
C13 0.113(10) 0.049(7) 0.098(8) -0.006(6) -0.005(8) 0.005(7)
C14 0.066(6) 0.057(6) 0.064(6) -0.007(5) 0.000(5) 0.018(5)
C15 0.052(5) 0.056(5) 0.031(4) -0.003(4) -0.001(4) 0.012(4)
C16 0.043(5) 0.059(5) 0.037(4) 0.000(4) 0.012(4) 0.013(4)
C17 0.055(6) 0.071(6) 0.058(5) 0.011(5) 0.013(4) 0.006(5)
C18 0.057(6) 0.150(12) 0.068(7) 0.020(7) 0.010(5) 0.004(8)
C19 0.086(9) 0.091(9) 0.104(9) 0.021(7) 0.024(7) -0.012(7)
C200 0.089(9) 0.061(7) 0.107(9) 0.006(6) 0.014(7) 0.009(6)
C20 0.046(5) 0.062(5) 0.035(4) 0.004(4) 0.011(4) -0.004(4)
C21 0.035(4) 0.083(6) 0.039(4) -0.002(4) 0.003(4) -0.012(5)
C22 0.039(4) 0.074(6) 0.041(5) -0.005(4) 0.015(4) 0.003(4)
C23 0.049(5) 0.094(7) 0.059(6) -0.007(5) 0.010(5) 0.014(5)
C28 0.066(7) 0.137(11) 0.073(7) -0.004(7) 0.024(6) 0.043(7)
C24 0.047(6) 0.140(11) 0.064(6) 0.002(7) 0.022(5) 0.014(7)
C25 0.043(5) 0.125(9) 0.050(5) 0.002(5) 0.016(4) 0.008(6)
C26 0.030(4) 0.111(8) 0.031(4) 0.001(5) 0.006(3) -0.004(5)
C27 0.039(5) 0.073(6) 0.037(4) -0.004(4) 0.005(4) -0.012(4)
C29 0.050(5) 0.090(8) 0.092(7) 0.000(6) 0.020(5) -0.009(5)
C30 0.087(8) 0.071(7) 0.106(8) -0.001(6) 0.017(7) -0.025(6)
C31 0.070(7) 0.084(8) 0.087(7) -0.012(6) 0.022(6) -0.018(6)
C32 0.084(7) 0.076(7) 0.106(8) -0.017(6) 0.047(7) -0.011(6)
C33 0.072(6) 0.058(6) 0.080(6) -0.003(5) 0.033(5) -0.011(5)
C34 0.044(5) 0.066(6) 0.043(4) -0.005(4) 0.008(4) -0.018(4)
C35 0.037(4) 0.031(4) 0.053(5) -0.003(4) 0.013(4) 0.001(3)
C36 0.046(4) 0.035(4) 0.049(5) 0.007(4) 0.011(4) 0.004(4)
C37 0.043(4) 0.040(4) 0.046(5) -0.002(4) -0.002(4) -0.002(4)
C38 0.070(6) 0.046(5) 0.063(6) 0.003(4) -0.004(5) -0.007(5)
C39 0.080(7) 0.058(6) 0.064(6) 0.012(5) -0.018(5) -0.002(5)
C40 0.059(6) 0.061(6) 0.082(7) -0.005(5) -0.026(5) -0.009(5)
C41 0.048(5) 0.052(5) 0.067(6) -0.001(5) -0.005(4) -0.011(4)
C42 0.052(5) 0.039(4) 0.051(5) 0.002(4) 0.002(4) 0.000(4)
C43 0.042(4) 0.049(5) 0.046(5) -0.006(4) 0.012(4) 0.004(4)
C44 0.053(5) 0.055(5) 0.045(5) -0.001(4) 0.016(4) -0.012(4)
C45 0.089(7) 0.070(6) 0.057(6) 0.014(5) 0.022(5) -0.017(6)
C46 0.095(7) 0.076(7) 0.049(5) 0.020(5) 0.025(5) 0.000(6)
C47 0.066(6) 0.060(6) 0.053(5) -0.001(4) 0.008(5) 0.004(5)
C48 0.052(5) 0.041(4) 0.056(5) 0.009(4) 0.013(4) 0.001(4)
C49 0.050(5) 0.044(4) 0.033(4) 0.000(3) 0.012(4) 0.009(4)
C54 0.119(10) 0.056(6) 0.127(10) 0.008(6) 0.077(8) 0.003(6)
C55 0.210(17) 0.029(6) 0.348(24) 0.059(9) 0.231(18) 0.055(8)
C56 0.092(9) 0.081(9) 0.200(15) 0.069(10) 0.055(10) 0.034(8)
C57 0.103(10) 0.070(8) 0.162(13) -0.010(8) 0.073(10) -0.002(7)
C58 0.103(11) 0.077(9) 0.219(19) 0.059(11) -0.018(12) -0.048(8)
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
Cu1 Cu 0.36432(5) 0.41084(10) 0.08910(5) 0.0873(5) Uani 1 d . .
Cu2 Cu 0.39330(9) 0.0902(2) 0.36215(8) 0.0738(7) Uani 0.50 d P .
O1 O 0.4131(2) 0.2302(4) 0.3437(2) 0.0513(13) Uani 1 d . .
O2 O 0.4580(2) 0.0536(4) 0.3397(2) 0.0591(15) Uani 1 d . .
O4 O 0.5191(2) 0.3132(5) 0.3049(2) 0.0528(14) Uani 1 d . .
O5 O 0.3760(2) -0.0588(4) 0.3727(2) 0.0483(13) Uani 1 d . .
O6 O 0.3401(2) 0.0515(4) 0.3005(2) 0.0505(13) Uani 1 d . .
O7 O 0.2785(2) -0.2276(4) 0.3107(2) 0.0501(13) Uani 1 d . .
N1 N 0.3427(5) 0.4692(10) 0.1430(4) 0.055(3) Uiso 0.60 d P 1
N1X N 0.3486(7) 0.5123(15) 0.1304(6) 0.055(5) Uiso 0.40 d P 2
N2 N 0.2899(3) 0.4216(5) 0.0625(2) 0.055(2) Uiso 1 d . .
N3 N 0.3855(2) 0.2621(5) 0.0944(2) 0.055(2) Uani 1 d . .
N4 N 0.4276(3) 0.4247(5) 0.0700(2) 0.061(2) Uani 1 d . .
C1 C 0.3738(5) 0.5139(15) 0.1773(5) 0.190(9) Uani 1 d . .
H1 H 0.4081(5) 0.5137(15) 0.1797(5) 0.103(9) Uiso 1 calc R 1
C2 C 0.3554(7) 0.5608(14) 0.2093(5) 0.179(8) Uani 1 d . .
H2 H 0.3773(7) 0.5768(14) 0.2365(5) 0.103(9) Uiso 1 calc R .
C3 C 0.3077(6) 0.5830(13) 0.2020(4) 0.138(6) Uani 1 d . .
H3 H 0.2956(6) 0.6173(13) 0.2232(4) 0.103(9) Uiso 1 calc R .
C4 C 0.2762(4) 0.5545(8) 0.1626(3) 0.084(3) Uani 1 d . .
H4 H 0.2421(4) 0.5696(8) 0.1563(3) 0.103(9) Uiso 1 calc R .
C5 C 0.2957(3) 0.5029(7) 0.1319(3) 0.061(2) Uani 1 d . .
C6 C 0.2650(3) 0.4672(6) 0.0889(3) 0.050(2) Uani 1 d . .
C7 C 0.2128(3) 0.4717(6) 0.0774(3) 0.056(2) Uani 1 d . .
H7 H 0.1959(3) 0.5041(6) 0.0957(3) 0.103(9) Uiso 1 calc R .
C8 C 0.1870(3) 0.4282(7) 0.0389(3) 0.069(3) Uani 1 d . .
H8 H 0.1522(3) 0.4331(7) 0.0307(3) 0.103(9) Uiso 1 calc R .
C9 C 0.2101(4) 0.3782(7) 0.0122(3) 0.077(3) Uani 1 d . .
H9 H 0.1921(4) 0.3454(7) -0.0133(3) 0.103(9) Uiso 1 calc R .
C10 C 0.2635(4) 0.3778(7) 0.0250(3) 0.071(3) Uani 1 d . .
H10 H 0.2807(4) 0.3461(7) 0.0067(3) 0.103(9) Uiso 1 calc R .
C11 C 0.3602(4) 0.1806(9) 0.1037(3) 0.080(3) Uani 1 d . .
H11 H 0.3319(4) 0.1923(9) 0.1141(3) 0.103(9) Uiso 1 calc R .
C12 C 0.3737(5) 0.0805(9) 0.0987(4) 0.088(3) Uani 1 d . .
H12 H 0.3557(5) 0.0267(9) 0.1063(4) 0.103(9) Uiso 1 calc R .
C13 C 0.4149(5) 0.0653(8) 0.0822(4) 0.092(4) Uani 1 d . .
H13 H 0.4244(5) -0.0002(8) 0.0771(4) 0.103(9) Uiso 1 calc R .
C14 C 0.4419(4) 0.1450(7) 0.0731(3) 0.066(3) Uani 1 d . .
H14 H 0.4703(4) 0.1342(7) 0.0627(3) 0.103(9) Uiso 1 calc R .
C15 C 0.4263(3) 0.2445(6) 0.0796(2) 0.049(2) Uani 1 d . .
C16 C 0.4527(3) 0.3374(6) 0.0709(2) 0.046(2) Uani 1 d . .
C17 C 0.5005(3) 0.3350(7) 0.0651(3) 0.061(2) Uani 1 d . .
H17 H 0.5178(3) 0.2743(7) 0.0660(3) 0.103(9) Uiso 1 calc R .
C18 C 0.5217(4) 0.4233(11) 0.0580(3) 0.093(4) Uani 1 d . .
H18 H 0.5538(4) 0.4232(11) 0.0535(3) 0.103(9) Uiso 1 calc R .
C19 C 0.4960(5) 0.5157(10) 0.0572(4) 0.094(3) Uani 1 d . .
H19 H 0.5104(5) 0.5770(10) 0.0524(4) 0.103(9) Uiso 1 calc R .
C200 C 0.4503(5) 0.5106(8) 0.0637(4) 0.088(3) Uani 1 d . .
H200 H 0.4329(5) 0.5709(8) 0.0638(4) 0.103(9) Uiso 1 calc R .
C20 C 0.4536(3) 0.2309(6) 0.3308(2) 0.047(2) Uani 1 d . .
C21 C 0.4769(3) 0.1329(7) 0.3274(2) 0.054(2) Uani 1 d . .
C22 C 0.5203(3) 0.1285(7) 0.3094(2) 0.050(2) Uani 1 d . .
C23 C 0.5431(3) 0.0369(8) 0.3025(3) 0.068(3) Uani 1 d . .
H23 H 0.5303(3) -0.0244(8) 0.3094(3) 0.089(17) Uiso 1 calc R .
C28 C 0.5847(4) 0.0389(11) 0.2853(3) 0.091(4) Uani 1 d . .
H28 H 0.6000(4) -0.0209(11) 0.2801(3) 0.089(17) Uiso 1 calc R .
C24 C 0.6035(4) 0.1334(10) 0.2757(3) 0.082(3) Uani 1 d . .
H24 H 0.6313(4) 0.1347(10) 0.2640(3) 0.089(17) Uiso 1 calc R .
C25 C 0.5822(3) 0.2228(9) 0.2830(3) 0.072(3) Uani 1 d . .
H25 H 0.5956(3) 0.2840(9) 0.2769(3) 0.089(17) Uiso 1 calc R .
C26 C 0.5401(3) 0.2203(8) 0.2997(2) 0.058(2) Uani 1 d . .
C27 C 0.4763(3) 0.3210(7) 0.3190(2) 0.050(2) Uani 1 d . .
C29 C 0.4839(4) 0.5060(8) 0.3060(3) 0.077(3) Uani 1 d . .
H29 H 0.5111(4) 0.4930(8) 0.2942(3) 0.114(18) Uiso 1 calc R .
C30 C 0.4688(4) 0.6081(8) 0.3089(4) 0.089(3) Uani 1 d . .
H30 H 0.4868(4) 0.6594(8) 0.2995(4) 0.114(18) Uiso 1 calc R .
C31 C 0.4284(4) 0.6335(9) 0.3253(3) 0.080(3) Uani 1 d . .
H31 H 0.4182(4) 0.6999(9) 0.3274(3) 0.114(18) Uiso 1 calc R .
C32 C 0.4040(4) 0.5509(8) 0.3385(4) 0.085(3) Uani 1 d . .
H32 H 0.3760(4) 0.5636(8) 0.3491(4) 0.114(18) Uiso 1 calc R .
C33 C 0.4192(4) 0.4500(7) 0.3366(3) 0.067(2) Uani 1 d . .
H33 H 0.4015(4) 0.3996(7) 0.3469(3) 0.114(18) Uiso 1 calc R .
C34 C 0.4590(3) 0.4225(7) 0.3203(2) 0.052(2) Uani 1 d . .
C35 C 0.3403(3) -0.0990(5) 0.3413(2) 0.040(2) Uani 1 d . .
C36 C 0.3220(3) -0.0377(6) 0.3016(2) 0.043(2) Uani 1 d . .
C37 C 0.2834(3) -0.0801(5) 0.2656(2) 0.045(2) Uani 1 d . .
C38 C 0.2634(3) -0.0297(6) 0.2257(3) 0.064(2) Uani 1 d . .
H38 H 0.2758(3) 0.0335(6) 0.2208(3) 0.088(15) Uiso 1 calc R .
C39 C 0.2260(4) -0.0724(7) 0.1940(3) 0.074(3) Uani 1 d . .
H39 H 0.2129(4) -0.0387(7) 0.1674(3) 0.088(15) Uiso 1 calc R .
C40 C 0.2072(4) -0.1669(7) 0.2013(3) 0.075(3) Uani 1 d . .
H40 H 0.1825(4) -0.1967(7) 0.1789(3) 0.088(15) Uiso 1 calc R .
C41 C 0.2239(3) -0.2162(6) 0.2402(3) 0.059(2) Uani 1 d . .
H41 H 0.2099(3) -0.2775(6) 0.2454(3) 0.088(15) Uiso 1 calc R .
C42 C 0.2625(3) -0.1730(6) 0.2720(3) 0.050(2) Uani 1 d . .
C43 C 0.3174(3) -0.1913(6) 0.3448(2) 0.046(2) Uani 1 d . .
C44 C 0.2945(3) -0.3426(6) 0.3849(3) 0.051(2) Uani 1 d . .
H44 H 0.2646(3) -0.3484(6) 0.3630(3) 0.063(11) Uiso 1 calc R .
C45 C 0.3051(4) -0.4121(7) 0.4189(3) 0.071(3) Uani 1 d . .
H45 H 0.2829(4) -0.4647(7) 0.4196(3) 0.063(11) Uiso 1 calc R .
C46 C 0.3488(4) -0.4027(7) 0.4520(3) 0.072(3) Uani 1 d . .
H46 H 0.3560(4) -0.4481(7) 0.4755(3) 0.063(11) Uiso 1 calc R .
C47 C 0.3819(4) -0.3254(7) 0.4501(3) 0.061(2) Uani 1 d . .
H47 H 0.4116(4) -0.3200(7) 0.4724(3) 0.063(11) Uiso 1 calc R .
C48 C 0.3722(3) -0.2564(6) 0.4160(3) 0.050(2) Uani 1 d . .
H48 H 0.3951(3) -0.2052(6) 0.4152(3) 0.063(11) Uiso 1 calc R .
C49 C 0.3273(3) -0.2639(5) 0.3823(2) 0.042(2) Uani 1 d . .
O8 O 0.3284(5) 0.1678(8) 0.3734(4) 0.052(3) Uiso 0.50 d P 1
O9 O 0.4157(5) 0.1259(10) 0.4293(5) 0.061(3) Uiso 0.50 d P 1
O10 O 0.3520(5) 0.2755(9) 0.4964(4) 0.043(3) Uiso 0.50 d P 1
C50 C 0.3399(6) 0.1986(12) 0.4139(5) 0.048(4) Uiso 0.50 d P 1
C51 C 0.3748(3) 0.1816(7) 0.4395(3) 0.000(2) Uiso 0.50 d P 1
C52 C 0.3902(7) 0.2150(14) 0.4862(6) 0.064(5) Uiso 0.50 d P 1
C53 C 0.3080(5) 0.2993(10) 0.4655(4) 0.023(3) Uiso 0.50 d P 1
C59 C 0.4734 0.1357 0.5239 0.037(4) Uiso 0.50 d P 1
H59 H 0.4761 0.1128 0.4964 0.044(17) Uiso 0.50 calc PR 1
C61 C 0.5029(9) 0.1505(15) 0.5994(9) 0.073(6) Uiso 0.50 d P 1
H61 H 0.5257(9) 0.1401(15) 0.6267(9) 0.044(17) Uiso 0.50 calc PR 1
C60 C 0.5122(6) 0.1102(11) 0.5600(5) 0.037(4) Uiso 0.50 d P 1
H60 H 0.5402(6) 0.0722(11) 0.5588(5) 0.044(17) Uiso 0.50 calc PR 1
C62 C 0.4671(5) 0.1958(9) 0.5972(4) 0.100(4) Uiso 0.50 d P 1
H62 H 0.4672(5) 0.2215(9) 0.6250(4) 0.044(17) Uiso 0.50 calc PR 1
C63 C 0.4273(4) 0.2222(7) 0.5690(3) 0.074(3) Uiso 0.50 d P 1
H63 H 0.4001(4) 0.2553(7) 0.5753(3) 0.044(17) Uiso 0.50 calc PR 1
C64 C 0.4312(6) 0.1917(11) 0.5243(5) 0.032(4) Uiso 0.50 d P 1
O8X O 0.3483(5) 0.1584(9) 0.3938(4) 0.050(3) Uiso 0.50 d P 2
O9X O 0.4391(4) 0.0952(8) 0.4306(3) 0.044(3) Uiso 0.50 d P 2
O10X O 0.3716(6) 0.2520(11) 0.5086(5) 0.065(4) Uiso 0.50 d P 2
C50X C 0.4162(6) 0.1437(11) 0.4533(6) 0.042(4) Uiso 0.50 d P 2
C51X C 0.4397(6) 0.1544(12) 0.5018(5) 0.048(4) Uiso 0.50 d P 2
C52X C 0.4104(10) 0.2122(15) 0.5264(7) 0.057(6) Uiso 0.50 d P 2
C53X C 0.3453(6) 0.2382(13) 0.4628(6) 0.057(4) Uiso 0.50 d P 2
C59X C 0.4833 0.1301 0.5325 0.154(14) Uiso 0.50 d P 2
H59X H 0.5063 0.0965 0.5203 0.019(15) Uiso 0.50 calc PR 2
C61X C 0.4994(9) 0.1439(17) 0.5750(9) 0.078(7) Uiso 0.50 d P 2
H61X H 0.5309(9) 0.1209(17) 0.5905(9) 0.019(15) Uiso 0.50 calc PR 2
C62X C 0.4671(5) 0.1958(9) 0.5972(4) 0.100(4) Uiso 0.50 d P 2
H62X H 0.4743(5) 0.2080(7) 0.6275(4) 0.019(15) Uiso 0.50 calc PR 2
C63X C 0.4273(4) 0.2222(7) 0.5690(3) 0.074(3) Uiso 0.50 d P 2
H63X H 0.4051(5) 0.2567(7) 0.5818(4) 0.019(15) Uiso 0.50 calc PR 2
C54 C 0.2768(5) 0.3501(7) 0.4832(4) 0.092(4) Uani 1 d . .
H54 H 0.2876(5) 0.3716(7) 0.5125(4) 0.152(30) Uiso 1 calc R 1
C55 C 0.2195(6) 0.3759(8) 0.4550(7) 0.167(9) Uani 1 d . .
H55 H 0.1948(6) 0.4101(8) 0.4648(7) 0.152(30) Uiso 1 calc R .
C56 C 0.2156(5) 0.3325(9) 0.4099(6) 0.121(5) Uani 1 d . .
H56 H 0.1856(5) 0.3396(9) 0.3881(6) 0.152(30) Uiso 1 calc R .
C57 C 0.2554(5) 0.2821(9) 0.3999(5) 0.105(4) Uani 1 d . .
H57 H 0.2539(5) 0.2565(9) 0.3718(5) 0.152(30) Uiso 1 calc R .
C58 C 0.2945(6) 0.2736(10) 0.4327(7) 0.144(7) Uani 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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100921.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100921.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_1100921
_chemical_formula_sum 'C22 H25 Cl N2 O8'
_chemical_name_common 'tetracycline hydrochloride'
_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'
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 10.9300
_cell_length_b 12.7162
_cell_length_c 15.7085
_cod_duplicate_entry 1000006
_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_formula_sum 'C5 H5 O2 N2'
_cod_database_code 1100921
loop_
_symmetry_equiv_pos_as_xyz
' X, Y, Z'
' X+1/2,-Y+1/2,-Z'
'-X, Y+1/2,-Z+1/2'
'-X+1/2,-Y, Z+1/2'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
Cl1 0.92963 0.41939 -0.00197 0.01950 Uani
O1 0.00860 0.36560 0.43967 0.03923 Uani
H1 0.03900 0.43300 0.43500 0.04700 Uiso
O6 0.14530 0.46012 0.12979 0.01937 Uani
H6 0.08600 0.44900 0.08800 0.04500 Uiso
O11 0.75140 0.64335 0.07408 0.02683 Uani
O13 0.36340 0.71743 0.18883 0.02500 Uani
O14 0.58000 0.60174 0.29547 0.02120 Uani
H14 0.56500 0.61400 0.33800 0.03300 Uiso
O15 0.35060 0.60822 0.35612 0.01980 Uani
H15 0.28300 0.58000 0.38500 0.04500 Uiso
O17 0.16470 0.50211 0.38835 0.02337 Uani
O19 0.66230 0.81863 0.04211 0.02687 Uani
H19 0.73400 0.75700 0.05500 0.06100 Uiso
N10 0.74650 0.44880 0.14281 0.01933 Uani
H10 0.79300 0.46400 0.10000 0.03500 Uiso
N19 0.46940 0.85510 0.08138 0.02883 Uani
H19A 0.47500 0.92100 0.05800 0.03400 Uiso
H19B 0.40800 0.83300 0.11200 0.04900 Uiso
C1 0.02070 0.32040 0.36224 0.02710 Uani
C2 -0.05250 0.23450 0.34350 0.03147 Uani
H2 -0.11100 0.21100 0.38800 0.02600 Uiso
C3 -0.04360 0.18880 0.26570 0.03010 Uani
H3 -0.08400 0.13400 0.25300 0.04000 Uiso
C4 0.03780 0.22530 0.20360 0.02403 Uani
H4 0.03800 0.18900 0.14800 0.02800 Uiso
C5 0.11130 0.31050 0.22057 0.01830 Uani
C6 0.19620 0.36090 0.15436 0.01780 Uani
C7 0.31780 0.38720 0.19906 0.01443 Uani
H7 0.33700 0.31800 0.22200 0.02800 Uiso
C8 0.41480 0.43140 0.13903 0.01700 Uani
H8A 0.37800 0.48600 0.10700 0.03500 Uiso
H8B 0.44400 0.37800 0.10010 0.02500 Uiso
C9 0.52410 0.47660 0.18811 0.01407 Uani
H9 0.55400 0.42300 0.22920 0.02000 Uiso
C10 0.62830 0.50410 0.12622 0.01557 Uani
H10A 0.61500 0.48200 0.07150 0.00700 Uiso
C11 0.65260 0.62040 0.11090 0.01797 Uani
C12 0.55790 0.69230 0.12673 0.01703 Uani
C13 0.45880 0.66630 0.18199 0.01693 Uani
C14 0.48280 0.57050 0.24083 0.01503 Uani
C15 0.36900 0.54390 0.29061 0.01583 Uani
C16 0.29400 0.46240 0.27178 0.01493 Uani
C17 0.18670 0.44460 0.32353 0.01837 Uani
C18 0.10600 0.35780 0.30253 0.01867 Uani
C19 0.56220 0.79110 0.08265 0.02040 Uani
C20 0.21610 0.29190 0.07690 0.02463 Uani
H20A 0.13500 0.28400 0.04790 0.01500 Uiso
H20B 0.24500 0.22500 0.09000 0.03800 Uiso
H20C 0.25900 0.32900 0.03400 0.02500 Uiso
C21 0.73180 0.33240 0.13840 0.02610 Uani
H21A 0.68800 0.31100 0.18400 0.04100 Uiso
H21B 0.81000 0.30300 0.13120 0.01900 Uiso
H21C 0.69800 0.32100 0.08500 0.02800 Uiso
C22 0.80960 0.48110 0.22280 0.03057 Uani
H22A 0.82000 0.55900 0.22300 0.02800 Uiso
H22B 0.88500 0.45800 0.22200 0.03900 Uiso
H22C 0.76100 0.45700 0.26900 0.03000 Uiso
|
1100922.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100922.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_1100922
_chemical_formula_sum 'C22 H25 Cl N2 O8'
_chemical_formula_weight 480.89
_chemical_name_common 'tetracycline hydrochloride'
_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 difmap
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 10.9300(9)
_cell_length_b 12.7162(11)
_cell_length_c 15.7085(13)
_cell_measurement_reflns_used 6452
_cell_measurement_temperature 150(2)
_cell_measurement_theta_max 29.20
_cell_measurement_theta_min 2.51
_cell_volume 2183.3(3)
_diffrn_ambient_temperature 150(2)
_diffrn_measurement_device_type 'Siemens SMART CCD diffractometer'
_diffrn_measurement_method '\w rotation with narrow frames'
_diffrn_radiation_monochromator 'silicon 111'
_diffrn_radiation_source 'Daresbury SRS station 9.8'
_diffrn_radiation_type synchrotron
_diffrn_radiation_wavelength 0.6883
_diffrn_reflns_av_R_equivalents 0.0468
_diffrn_reflns_av_sigmaI/netI 0.0794
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_l_max 4
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_number 8955
_diffrn_reflns_theta_max 29.26
_diffrn_reflns_theta_min 2.20
_diffrn_standards_decay_% 15
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 0.228
_exptl_absorpt_correction_type none
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.463
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 1008
_exptl_crystal_size_max 0.04
_exptl_crystal_size_mid 0.03
_exptl_crystal_size_min 0.02
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack 0.02(8)
_refine_ls_extinction_coef 0.0038(12)
_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 0.969
_refine_ls_hydrogen_treatment refall
_refine_ls_matrix_type full
_refine_ls_number_parameters 399
_refine_ls_number_reflns 4915
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.969
_refine_ls_R_factor_all 0.0633
_refine_ls_R_factor_gt 0.0502
_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^)+(0.0579P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1116
_refine_ls_wR_factor_ref 0.1161
_reflns_number_gt 3937
_reflns_number_total 4915
_reflns_threshold_expression >2sigma(I)
_cod_duplicate_entry 1000006
_cod_original_sg_symbol_H-M P2(1)2(1)2(1)
_cod_database_code 1100922
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
Cl1 Cl 0.92963(7) 0.41939(6) -0.00197(4) 0.01949(17) Uani 1 1 d . . .
O1 O 0.0086(3) 0.3656(3) 0.43967(14) 0.0392(7) Uani 1 1 d . . .
H1 H 0.039(4) 0.433(4) 0.435(2) 0.047(13) Uiso 1 1 d . . .
O6 O 0.1453(2) 0.46012(16) 0.12979(12) 0.0194(5) Uani 1 1 d . . .
H6 H 0.086(4) 0.449(3) 0.088(2) 0.045(12) Uiso 1 1 d . . .
O11 O 0.7514(2) 0.64335(19) 0.07408(14) 0.0268(5) Uani 1 1 d . . .
O13 O 0.3634(2) 0.71743(18) 0.18883(13) 0.0250(5) Uani 1 1 d . . .
O14 O 0.5800(2) 0.60174(18) 0.29547(12) 0.0212(5) Uani 1 1 d . . .
H14 H 0.565(4) 0.614(3) 0.338(2) 0.033(11) Uiso 1 1 d . . .
O15 O 0.3506(2) 0.60822(17) 0.35612(12) 0.0198(5) Uani 1 1 d . . .
H15 H 0.283(4) 0.580(4) 0.385(2) 0.045(12) Uiso 1 1 d . . .
O17 O 0.1647(2) 0.50211(18) 0.38835(12) 0.0234(5) Uani 1 1 d . . .
O19 O 0.6623(3) 0.81863(18) 0.04211(13) 0.0269(6) Uani 1 1 d . . .
H19 H 0.734(5) 0.757(4) 0.055(3) 0.061(14) Uiso 1 1 d . . .
N10 N 0.7465(3) 0.4488(2) 0.14281(16) 0.0193(6) Uani 1 1 d . . .
H10 H 0.793(4) 0.464(3) 0.100(2) 0.035(11) Uiso 1 1 d . . .
N19 N 0.4694(3) 0.8551(2) 0.08138(17) 0.0288(7) Uani 1 1 d . . .
H19A H 0.475(4) 0.921(3) 0.058(2) 0.034(10) Uiso 1 1 d . . .
H19B H 0.408(4) 0.833(4) 0.112(2) 0.049(14) Uiso 1 1 d . . .
C1 C 0.0207(3) 0.3204(3) 0.36224(18) 0.0272(8) Uani 1 1 d . . .
C2 C -0.0525(4) 0.2345(3) 0.3435(2) 0.0314(9) Uani 1 1 d . . .
H2 H -0.111(3) 0.211(3) 0.388(2) 0.026(9) Uiso 1 1 d . . .
C3 C -0.0436(4) 0.1888(3) 0.2657(2) 0.0302(8) Uani 1 1 d . . .
H3 H -0.084(4) 0.134(3) 0.253(2) 0.040(12) Uiso 1 1 d . . .
C4 C 0.0378(3) 0.2253(3) 0.2036(2) 0.0240(7) Uani 1 1 d . . .
H4 H 0.038(3) 0.189(3) 0.148(2) 0.028(9) Uiso 1 1 d . . .
C5 C 0.1113(3) 0.3105(2) 0.22057(18) 0.0183(7) Uani 1 1 d . . .
C6 C 0.1962(3) 0.3609(2) 0.15436(17) 0.0178(7) Uani 1 1 d . . .
C7 C 0.3178(3) 0.3872(2) 0.19906(16) 0.0145(6) Uani 1 1 d . . .
H7 H 0.337(4) 0.318(3) 0.222(2) 0.028(9) Uiso 1 1 d . . .
C8 C 0.4148(3) 0.4314(2) 0.13903(16) 0.0170(6) Uani 1 1 d . . .
H8A H 0.378(4) 0.486(3) 0.107(2) 0.035(10) Uiso 1 1 d . . .
H8B H 0.444(3) 0.378(3) 0.1001(19) 0.025(9) Uiso 1 1 d . . .
C9 C 0.5241(3) 0.4766(2) 0.18811(16) 0.0141(6) Uani 1 1 d . . .
H9 H 0.554(3) 0.423(3) 0.2292(18) 0.020(8) Uiso 1 1 d . . .
C10 C 0.6283(3) 0.5041(2) 0.12622(17) 0.0156(6) Uani 1 1 d . . .
H10A H 0.615(3) 0.482(2) 0.0715(17) 0.007(7) Uiso 1 1 d . . .
C11 C 0.6526(3) 0.6204(2) 0.11090(16) 0.0180(6) Uani 1 1 d . . .
C12 C 0.5579(3) 0.6923(2) 0.12673(16) 0.0170(6) Uani 1 1 d . . .
C13 C 0.4588(3) 0.6663(2) 0.18199(15) 0.0171(7) Uani 1 1 d . . .
C14 C 0.4828(3) 0.5705(2) 0.24083(15) 0.0150(6) Uani 1 1 d . . .
C15 C 0.3690(3) 0.5439(2) 0.29061(15) 0.0158(6) Uani 1 1 d . . .
C16 C 0.2940(3) 0.4624(2) 0.27178(16) 0.0149(6) Uani 1 1 d . . .
C17 C 0.1867(3) 0.4446(2) 0.32353(16) 0.0184(7) Uani 1 1 d . . .
C18 C 0.1060(3) 0.3578(3) 0.30253(17) 0.0187(7) Uani 1 1 d . . .
C19 C 0.5622(3) 0.7911(2) 0.08265(16) 0.0204(7) Uani 1 1 d . . .
C20 C 0.2161(4) 0.2919(3) 0.0769(2) 0.0246(8) Uani 1 1 d . . .
H20A H 0.135(3) 0.284(3) 0.0479(18) 0.015(8) Uiso 1 1 d . . .
H20B H 0.245(4) 0.225(4) 0.090(2) 0.038(11) Uiso 1 1 d . . .
H20C H 0.259(3) 0.329(3) 0.034(2) 0.025(9) Uiso 1 1 d . . .
C21 C 0.7318(4) 0.3324(3) 0.1384(2) 0.0259(8) Uani 1 1 d . . .
H21A H 0.688(4) 0.311(3) 0.184(2) 0.041(11) Uiso 1 1 d . . .
H21B H 0.810(4) 0.303(3) 0.1312(19) 0.019(9) Uiso 1 1 d . . .
H21C H 0.698(3) 0.321(3) 0.085(2) 0.028(10) Uiso 1 1 d . . .
C22 C 0.8096(4) 0.4811(3) 0.2228(2) 0.0308(9) Uani 1 1 d . . .
H22A H 0.820(3) 0.559(3) 0.223(2) 0.028(9) Uiso 1 1 d . . .
H22B H 0.885(4) 0.458(4) 0.222(2) 0.039(12) Uiso 1 1 d . . .
H22C H 0.761(4) 0.457(3) 0.269(2) 0.030(10) 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
Cl1 0.0148(4) 0.0225(3) 0.0212(3) 0.0011(3) 0.0017(3) -0.0031(3)
O1 0.0359(18) 0.0553(19) 0.0265(11) 0.0003(11) 0.0098(10) -0.0166(16)
O6 0.0161(13) 0.0172(11) 0.0248(10) 0.0008(8) -0.0052(9) 0.0042(11)
O11 0.0167(14) 0.0226(12) 0.0412(11) 0.0072(10) 0.0086(10) -0.0041(11)
O13 0.0229(15) 0.0233(12) 0.0288(10) 0.0014(9) 0.0041(9) 0.0096(12)
O14 0.0140(13) 0.0322(13) 0.0174(9) -0.0005(8) -0.0032(8) -0.0055(11)
O15 0.0154(13) 0.0240(12) 0.0200(9) -0.0047(8) 0.0013(8) 0.0000(11)
O17 0.0180(13) 0.0292(12) 0.0229(9) -0.0026(9) 0.0037(8) 0.0002(12)
O19 0.0310(16) 0.0199(12) 0.0297(11) 0.0052(9) -0.0002(10) -0.0075(13)
N10 0.0132(15) 0.0194(13) 0.0254(11) 0.0042(10) 0.0046(10) -0.0001(12)
N19 0.038(2) 0.0166(14) 0.0319(14) 0.0069(11) -0.0021(13) 0.0056(15)
C1 0.020(2) 0.0351(19) 0.0262(14) 0.0090(13) 0.0011(13) -0.0004(17)
C2 0.017(2) 0.041(2) 0.0364(16) 0.0125(15) -0.0011(14) -0.0087(19)
C3 0.017(2) 0.0267(19) 0.0466(18) 0.0057(15) -0.0042(14) -0.0080(19)
C4 0.013(2) 0.0218(17) 0.0373(16) -0.0007(13) -0.0020(13) 0.0003(15)
C5 0.0084(18) 0.0178(15) 0.0287(13) 0.0034(11) -0.0015(11) 0.0039(14)
C6 0.0169(18) 0.0154(14) 0.0211(12) -0.0015(10) -0.0004(11) 0.0025(14)
C7 0.0061(16) 0.0135(14) 0.0237(12) -0.0006(10) 0.0003(10) 0.0009(13)
C8 0.0124(17) 0.0177(15) 0.0209(11) -0.0034(11) 0.0022(11) 0.0008(15)
C9 0.0079(16) 0.0132(14) 0.0211(11) 0.0015(10) 0.0011(10) 0.0007(13)
C10 0.0074(16) 0.0173(15) 0.0220(12) 0.0011(11) -0.0008(10) 0.0014(14)
C11 0.0153(18) 0.0184(15) 0.0202(12) 0.0031(11) -0.0013(11) -0.0003(15)
C12 0.0172(18) 0.0133(13) 0.0206(12) 0.0006(9) -0.0011(11) -0.0003(15)
C13 0.018(2) 0.0167(14) 0.0161(11) -0.0034(10) -0.0013(11) 0.0002(15)
C14 0.0119(16) 0.0151(14) 0.0181(11) -0.0005(10) -0.0024(10) -0.0015(14)
C15 0.0135(17) 0.0170(15) 0.0170(11) 0.0015(10) -0.0036(10) 0.0046(14)
C16 0.0123(17) 0.0153(14) 0.0172(11) 0.0024(10) -0.0009(10) 0.0040(14)
C17 0.0151(18) 0.0210(16) 0.0190(12) 0.0038(10) -0.0009(10) 0.0052(15)
C18 0.0111(18) 0.0209(16) 0.0240(13) 0.0045(11) -0.0007(11) 0.0031(14)
C19 0.026(2) 0.0143(14) 0.0209(12) 0.0000(10) -0.0036(12) -0.0055(17)
C20 0.019(2) 0.0250(19) 0.0299(15) -0.0109(13) 0.0012(13) -0.0014(18)
C21 0.024(2) 0.0177(17) 0.0366(17) 0.0046(13) 0.0117(15) 0.0050(17)
C22 0.017(2) 0.038(2) 0.0367(18) 0.0019(15) -0.0056(15) 0.002(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'
|
1100923.cif | #------------------------------------------------------------------------------
#$Date: 2022-09-14 17:31:13 +0300 (Wed, 14 Sep 2022) $
#$Revision: 277831 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/09/1100923.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_1100923
_chemical_formula_moiety ?
_chemical_formula_sum 'C22 H16 N2 S Se2'
_chemical_formula_weight 498.35
_space_group_IT_number 2
_space_group_name_Hall '-P 1'
_space_group_name_H-M_alt 'P -1'
_symmetry_cell_setting triclinic
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_type_scat_source IntTabC
_cell_angle_alpha 94.57(4)
_cell_angle_beta 92.31(4)
_cell_angle_gamma 100.58(4)
_cell_formula_units_Z 4
_cell_length_a 8.586(8)
_cell_length_b 15.286(11)
_cell_length_c 15.606(8)
_cell_measurement_reflns_used 25
_cell_measurement_temperature 295(2)
_cell_measurement_theta_max ?
_cell_measurement_theta_min ?
_cell_volume 2004(3)
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71067
_exptl_absorpt_coefficient_mu 3.804
_exptl_crystal_density_diffrn 1.652
_exptl_crystal_density_meas ?
_refine_diff_density_max 0.813
_refine_diff_density_min -0.715
_cod_original_formula_sum 'C22 H16 N2 S1 Se2'
_cod_database_code 1100923
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
Se(1A) .4853(1) -.0253(1) .2077(1) .065(1)
Se(2A) .6717(1) .1191(1) .2261(1) .050(1)
S(3A) .8539(2) .2668(1) .2273(1) .048(1)
C(4A) .7570(6) .2982(4) .1427(3) .038(1)
C(5A) .6144(7) .2423(4) .1061(3) .039(1)
C(6A) .5587(6) .1587(4) .1359(3) .034(1)
C(7A) .4228(6) .1001(4) .0982(3) .037(1)
C(8A) .3714(7) .0153(4) .1206(3) .035(1)
C(9A) .2337(6) -.0474(3) .0798(3) .036(1)
C(10A) .1409(7) -.1108(4) .1258(4) .049(2)
C(11A) .0128(8) -.1663(4) .0873(5) .057(2)
C(12A) -.0255(8) -.1657(5) .0022(5) .060(2)
C(13A) .0604(7) -.1074(5) -.0459(4) .054(2)
C(14A) .1893(7) -.0483(4) -.0068(4) .044(2)
C(15A) .5245(6) .2726(4) .0337(3) .036(1)
C(16A) .5193(7) .2353(4) -.0488(3) .043(2)
C(17A) .4361(7) .2653(5) -.1137(4) .056(2)
C(18A) .3630(7) .3357(5) -.0975(4) .058(2)
C(19A) .3670(8) .3760(5) -.0163(4) .059(2)
C(20A) .4454(7) .3442(4) .0503(4) .046(2)
N(21A) .8086(6) .3764(3) .1068(3) .047(1)
C(22A) .9429(7) .4426(4) .1246(4) .046(2)
N(23A) .9228(7) .5200(4) .0970(4) .060(2)
C(24A) 1.0458(10) .5859(5) .1086(5) .072(2)
C(25A) 1.1878(9) .5815(5) .1473(5) .068(2)
C(26A) 1.2084(8) .5019(6) .1726(4) .067(2)
C(27A) 1.0859(8) .4304(5) .1626(4) .058(2)
Se(1B) -.0913(1) -.0609(1) .2891(1) .059(1)
Se(2B) .1025(1) .0785(1) .2726(1) .045(1)
S(3B) .2876(2) .2246(1) .2703(1) .050(1)
C(4B) .2171(7) .2700(4) .3589(3) .041(1)
C(5B) .0873(7) .2215(4) .3991(3) .037(1)
C(6B) .0226(6) .1325(4) .3690(3) .034(1)
C(7B) -.1041(6) .0818(4) .4084(3) .039(1)
C(8B) -.1689(7) -.0057(4) .3846(3) .037(1)
C(9B) -.2936(7) -.0593(4) .4300(4) .038(1)
C(14B) -.3085(7) -.0420(4) .5184(4) .042(2)
C(13B) -.4268(8) -.0932(5) .5598(4) .056(2)
C(12B) -.5292(8) -.1616(5) .5154(5) .062(2)
C(11B) -.5164(8) -.1800(4) .4299(5) .060(2)
C(10B) -.4012(8) -.1308(4) .3874(4) .050(2)
C(15B) .0219(6) .2668(4) .4747(3) .037(1)
C(16B) .0407(7) .2423(4) .5557(4) .048(2)
C(17B) -.0233(8) .2846(5) .6247(4) .066(2)
C(18B) -.1015(8) .3515(5) .6131(5) .061(2)
C(19B) -.1177(8) .3793(5) .5328(5) .064(2)
C(20B) -.0590(7) .3359(4) .4624(4) .053(2)
N(21B) .2828(6) .3547(3) .3952(3) .054(1)
C(22B) .4085(7) .4167(4) .3732(4) .047(2)
N(23B) .3973(6) .5001(4) .4021(4) .059(2)
C(24B) .5169(10) .5645(5) .3882(5) .078(2)
C(25B) .6451(9) .5530(6) .3461(6) .083(2)
C(26B) .6596(9) .4691(6) .3185(5) .083(2)
C(27B) .5407(8) .3981(5) .3334(5) .070(2)
H(7A) .3641(6) .1204(4) .0552(3) .051(4)
H(10A) .1680(7) -.1145(4) .1835(4) .051(4)
H(11A) -.0505(8) -.2058(4) .1197(5) .051(4)
H(12A) -.1124(8) -.2062(5) -.0232(5) .051(4)
H(13A) .0335(7) -.1070(5) -.1042(4) .051(4)
H(14A) .2485(7) -.0075(4) -.0397(4) .051(4)
H(16A) .5731(7) .1887(4) -.0614(3) .051(4)
H(17A) .4298(7) .2371(5) -.1691(4) .051(4)
H(18A) .3097(7) .3567(5) -.1423(4) .051(4)
H(19A) .3175(8) .4247(5) -.0056(4) .051(4)
H(20A) .4456(7) .3703(4) .1062(4) .051(4)
H(21A) .7464(6) .3865(3) .0657(3) .051(4)
H(24A) 1.0344(10) .6402(5) .0885(5) .086
H(25A) 1.2683(9) .6316(5) .1562(5) .082
H(26A) 1.3061(8) .4958(6) .1969(4) .080
H(27A) 1.0976(8) .3753(8) .1806(4) .069
H(7B) -.1470(6) .1100(4) .4543(3) .051(4)
H(10B) -.2383(7) .0043(4) .5495(4) .051(4)
H(11B) -.4364(8) -.0809(5) .6184(4) .051(4)
H(12B) -.6085(8) -.1959(5) .5438(5) .051(4)
H(13B) -.5874(8) -.2268(4) .4000(5) .051(4)
H(14B) -.3937(8) -.1449(4) .3288(4) .051(4)
H(16B) .0967(7) .1970(4) .5653(4) .051(4)
H(17B) -.0115(8) .2661(5) .6796(4) .051(4)
H(18B) -.1444(8) .3788(5) .6595(5) .051(4)
H(19B) -.1679(8) .4272(5) .5250 .051(4)
H(20B) -.0742(7) .3533(4) .4074(4) .051(4)
H(21B) .2367(6) .3718(3) .4397(3) .051(4)
H(24B) .5114(10) .6224(5) .4095(5) .093
H(25B) .7225(9) .6016(6) .3360(6) .100
H(26B) .7483(9) .4589(6) .2898(5) .100
H(27B) .5499(8) .3395(5) .3170(5) .084
loop_
_atom_type_symbol
Se
S
C
N
H
|
1100924.cif | #------------------------------------------------------------------------------
#$Date: 2018-01-30 17:57:57 +0200 (Tue, 30 Jan 2018) $
#$Revision: 205901 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/09/1100924.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_1100924
loop_
_publ_author_name
'Ohishi, H.'
'Sakamoto, Y.'
'Harusawa, S.'
'Yoneda, R.'
'Kurihara, T.'
_publ_section_title
;(13-Methyl-1,4,7,8,13,13b-hexahydro[1',2']oxazepino[2',3':1,2]pyrido[3,4-<i>b</i>]indol-1-yl)methanol
and its Unusual Packing Style
;
_journal_issue 1
_journal_name_full 'Acta Crystallographica Section C'
_journal_page_first 135
_journal_page_last 139
_journal_paper_doi 10.1107/S0108270194000715
_journal_volume 51
_journal_year 1995
_chemical_formula_moiety 'C17 H20 N2 O2'
_chemical_formula_sum 'C17 H20 N2 O2'
_chemical_formula_weight 284.359
_space_group_crystal_system monoclinic
_space_group_IT_number 7
_space_group_name_Hall 'P -2yc'
_space_group_name_H-M_alt 'P 1 c 1'
_atom_type_scat_source IntTabIV
_cell_angle_alpha 90.
_cell_angle_beta 103.16(3)
_cell_angle_gamma 90.
_cell_formula_units_Z 8
_cell_length_a 18.499(4)
_cell_length_b 6.2149(9)
_cell_length_c 26.450(10)
_cell_measurement_reflns_used 20
_cell_measurement_temperature 293
_cell_measurement_theta_max 28.06
_cell_measurement_theta_min 23.83
_cell_volume 2961.1(14)
_diffrn_measurement_device 'Rigaku AFC'
_diffrn_measurement_method \w-2\q
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.5418
_diffrn_reflns_av_R_equivalents XX
_diffrn_reflns_limit_h_max 21
_diffrn_reflns_limit_h_min -21
_diffrn_reflns_limit_k_max 7
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_l_max 30
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_number 5706
_diffrn_reflns_theta_max 62.5
_diffrn_standards_decay_% 5
_diffrn_standards_interval_count 100
_diffrn_standards_number 4
_exptl_absorpt_coefficient_mu 0.638
_exptl_absorpt_correction_T_max 0.93
_exptl_absorpt_correction_T_min 0.83
_exptl_absorpt_correction_type empirical
_exptl_absorpt_process_details 'North, Phillips & Mathews, 1968'
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.2757
_exptl_crystal_description needles
_exptl_crystal_size_max 0.50
_exptl_crystal_size_mid 0.10
_exptl_crystal_size_min 0.10
_refine_diff_density_max 0.21
_refine_diff_density_min -0.05
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_obs 1.232
_refine_ls_hydrogen_treatment refxyz
_refine_ls_number_parameters 1078
_refine_ls_number_reflns 4021
_refine_ls_R_factor_obs 0.0615
_refine_ls_shift/esd_max 0.11
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
'w = 1.0/[\s(F~o~)^2^ - 0.09527F~o~ + 0.00606F~o~^2^]'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_obs 0.0675
_reflns_number_observed 4021
_reflns_number_total 5168
_reflns_observed_criterion F>3.0\s(F)
_cod_duplicate_entry 2010395
_cod_depositor_comments
;
Modifying the entry since it was initially mistakenly constructed by mixing
various data items from two other entries (2003785 and 2010395) and did not
result in a reasonable structure. Data values taken from entry 2003785 were
removed and the entry was marked as a duplicate of entry 2010395.
Antanas Vaitkus,
2018-01-30
The following automatic conversions were performed:
'_refine_ls_weighting_scheme' value ' w = 1.0/[\s(F~o~)^2^ -
0.09527F~o~ + 0.00606F~o~^2^]' was changed to 'calc'. New tag
'_refine_ls_weighting_details' was created. The value of the new tag
was set to 'w = 1.0/[\s(F~o~)^2^ - 0.09527F~o~ + 0.00606F~o~^2^]'.
Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas
;
_cod_database_code 1100924
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 x,-y,z+1/2
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
C1A .9428(3) .2564(8) .3598(2)
C2A .9883(3) .0971(8) .4011(2)
C3A .9693(3) -.0007(9) .4393(2)
C4A .8930(3) .0020(10) .4538(2)
O5A .8397(2) .1181(6) .41550(10)
N6A .8368(2) .0175(7) .36560(10)
C7A .7570(3) -.0460(9) .3458(2)
C8A .7562(3) -.1820(10) .2968(2)
C9A .8012(2) -.0687(8) .2650(2)
C10A .8027(3) -.1090(9) .2115(2)
C11A .7659(3) -.2632(9) .1738(2)
C12A .7761(4) -.2670(10) .1262(3)
C13A .8293(3) -.1050(10) .1121(2)
C14A .8658(3) .0460(10) .1482(2)
C15A .8518(3) .0404(8) .1991(2)
N16A .8787(2) .1659(6) .2394(2)
C17A .8504(2) .0960(8) .2789(2)
C18A .8645(2) .1903(7) .3354(2)
C19A .9248(4) .3630(10) .2396(2)
C20A .9440(3) .4801(7) .3855(2)
O21A .9246(2) .6266(5) .34580(10)
C1B .0252(2) .2531(7) .6218(2)
C2B -.0174(3) .4002(9) .5824(2)
C3B .0028(3) .4930(9) .5417(2)
C4B .0740(4) .5000(10) .5321(2)
O5B .1298(2) .3813(6) .5682(2)
N6B .1336(2) .4813(7) .6183(2)
C7B .2101(3) .5330(10) .6401(2)
C8B .2159(3) .6687(9) .6877(2)
C9B .1684(3) .5719(9) .7218(2)
C10B .1670(3) .6110(8) .7734(2)
C11B .1996(3) .7640(10) .8089(3)
C12B .1847(3) .7440(9) .8605(2)
C13B .1413(3) .5980(10) .8720(2)
C14B .1058(3) .4443(9) .8366(2)
C15B .1189(3) .4559(9) .7883(2)
N16B .0920(2) .3246(7) .74340(10)
C17B .1236(3) .3991(7) .7019(2)
C18B .1092(3) .3150(8) .6498(2)
C19B .0499(3) .1340(8) .7490(2)
C20B .0230(3) .0320(9) .5974(2)
O21B .0517(2) -.1269(6) .63950(10)
C1C .5396(3) .4937(8) .0947(2)
C2C .6091(3) .3420(9) .1034(2)
C3C .6475(3) .2500(9) .1425(2)
C4C .6294(3) .2380(10) .1926(2)
O5C .5605(2) .3619(7) .19820(10)
N6C .4988(3) .2570(9) .1612(2)
C7C .4418(3) .2130(10) .1893(2)
C8C .3837(3) .0660(10) .1510(2)
C9C .3688(3) .1793(8) .1010(2)
C10C .3049(3) .1523(8) .0575(2)
C11C .2440(3) -.0040(10) .0501(2)
C12C .1940(3) .0150(10) .0028(2)
C13C .1988(3) .1640(10) -.0308(2)
C14C .2574(3) .3101(9) -.0240(2)
C15C .3088(3) .2993(8) .0214(2)
N16C .3683(3) .4200(7) .0392(2)
C17C .4072(3) .3453(9) .0881(2)
C18C .4777(3) .4294(8) .1235(2)
C19C .3860(4) .6150(10) .0130(2)
C20C .5699(3) .7214(8) .1131(3)
O21C .5136(2) .8715(5) .0919(2)
C1D .4292(2) -.0070(9) .3884(2)
C2D .3652(3) -.1540(8) .3823(2)
C3D .3269(3) -.2560(9) .3359(3)
C4D .3442(4) -.2500(10) .2820(3)
O5D .4061(2) -.1436(6) .28420(10)
N6D .4658(2) -.2381(6) .3235(2)
C7D .5237(3) -.3180(10) .2955(2)
C8D .5794(3) -.4400(9) .3310(2)
C9D .6048(3) -.3323(9) .3834(2)
C10D .6657(3) -.3745(8) .4234(2)
C11D .7217(3) -.5190(10) .4343(2)
C12D .7775(4) -.5020(10) .4804(3)
C13D .7762(3) -.3280(10) .5200(2)
C14D .7168(3) -.1740(10) .5096(3)
C15D .6633(3) -.2020(9) .4623(2)
N16D .5985(2) -.0714(7) .4438(2)
C17D .5650(3) -.1553(8) .3962(2)
C18D .4946(3) -.0673(8) .3624(2)
C19D .5854(3) .1216(8) .4707(2)
C20D .4006(3) .2140(9) .3728(2)
O21D .4593(2) .3691(7) .3871(2)
H1A .970(3) .270(10) .330(2)
H2A 1.039(3) .070(9) .398(2)
H3A 1.010(3) -.091(9) .464(2)
H4A .872(3) -.160(10) .454(2)
H5A .897(3) .060(10) .489(2)
H6A .741(3) -.130(10) .373(2)
H7A .722(3) .089(9) .333(2)
H8A .776(3) -.330(10) .310(2)
H9A .704(3) -.200(9) .277(2)
H10A .728(3) -.360(9) .188(2)
H11A .751(3) -.399(9) .100(2)
H12A .838(3) -.100(9) .069(2)
H13A .902(3) .159(9) .137(2)
H14A .975(3) .310(9) .233(2)
H15A .933(3) .441(9) .275(2)
H16A .899(3) .470(10) .212(2)
H17A .833(3) .330(9) .338(2)
H18A .997(3) .511(9) .408(2)
H19A .878(3) .732(9) .353(2)
H20A .908(3) .470(10) .410(2)
H1B -.002(3) .250(10) .654(2)
H2B -.070(3) .420(10) .584(2)
H3B -.035(3) .600(10) .517(2)
H4B .071(3) .430(9) .496(2)
H5B .093(3) .660(10) .530(2)
H6B .244(3) .390(9) .648(2)
H7B .231(3) .621(9) .611(2)
H8B .267(3) .680(9) .709(2)
H9B .199(3) .820(10) .677(2)
H10B .233(3) .890(9) .797(2)
H11B .213(3) .831(9) .893(2)
H12B .072(3) .330(9) .849(2)
H13B .131(3) .590(9) .912(2)
H14B .074(3) .060(10) .784(2)
H15B .052(3) .020(10) .718(2)
H16B -.002(3) .170(9) .750(2)
H17B .143(3) .180(9) .651(2)
H18B .055(3) .029(9) .570(2)
H19B -.032(3) -.020(9) .578(2)
H20B .010(3) -.230(10) .638(2)
H1C .510(3) .480(10) .054(2)
H2C .630(3) .322(9) .069(2)
H3C .691(3) .179(9) .137(2)
H4C .624(3) .071(9) .203(2)
H5C .677(3) .310(10) .219(2)
H6C .415(3) .350(9) .199(2)
H7C .463(3) .140(10) .224(2)
H8C .411(3) -.100(9) .147(2)
H9C .335(3) .040(9) .164(2)
H10C .239(3) -.119(9) .079(2)
H11C .146(3) -.090(10) -.007(2)
H12C .156(3) .160(10) -.063(2)
H13C .252(3) .430(9) -.051(2)
H14C .401(3) .590(9) -.020(2)
H15C .426(3) .712(9) .039(2)
H16C .335(3) .708(9) .003(2)
H17C .469(3) .580(10) .144(2)
H18C .620(3) .760(10) .100(2)
H19C .583(3) .729(9) .155(2)
H20C .499(3) .982(9) .123(2)
H1D .453(3) -.010(10) .429(2)
H2D .350(3) -.200(10) .417(2)
H3D .279(4) -.330(9) .337(2)
H4D .356(3) -.429(9) .270(2)
H5D .303(3) -.190(9) .254(2)
H6D .493(3) -.400(9) .264(2)
H7D .541(3) -.179(9) .278(2)
H8D .561(3) -.600(9) .336(2)
H9D .631(3) -.450(9) .317(2)
H10D .697(3) -.670(10) .422(2)
H11D .822(3) -.620(9) .485(2)
H12D .818(3) -.310(10) .556(2)
H13D .714(3) -.040(10) .535(2)
H14D .573(3) .070(9) .506(2)
H15D .633(3) .200(10) .481(2)
H16D .540(3) .210(10) .450(2)
H17D .512(3) .079(9) .345(2)
H18D .378(3) .220(9) .331(2)
H19D .359(3) .260(9) .394(2)
H20D .480(3) .460(9) .419(2)
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
C2A C1A C18A 116.0(3) yes
C2A C1A C20A 108.0(3) yes
C18A C1A C20A 110.5(3) yes
C1A C2A C3A 129.9(3) yes
C2A C3A C4A 127.9(3) yes
C3A C4A O5A 110.5(3) yes
C4A O5A N6A 107.6(3) yes
O5A N6A C7A 105.1(3) yes
O5A N6A C18A 103.3(3) yes
C7A N6A C18A 115.5(3) yes
N6A C7A C8A 104.9(3) yes
C7A C8A C9A 108.4(3) yes
C8A C9A C10A 127.6(3) yes
C8A C9A C17A 128.9(3) yes
C10A C9A C17A 103.5(3) yes
C9A C10A C11A 133.1(3) yes
C9A C10A C15A 106.0(3) yes
C11A C10A C15A 120.9(3) yes
C10A C11A C12A 121.8(4) yes
C11A C12A C13A 117.9(4) yes
C12A C13A C14A 121.2(4) yes
C13A C14A C15A 117.7(4) yes
C10A C15A C14A 120.5(4) yes
C10A C15A N16A 110.5(3) yes
C14A C15A N16A 129.0(3) yes
C15A N16A C17A 107.1(3) yes
C15A N16A C19A 126.6(3) yes
C17A N16A C19A 125.9(3) yes
C9A C17A N16A 112.8(3) yes
C9A C17A C18A 119.5(3) yes
N16A C17A C18A 127.6(3) yes
C1A C18A N6A 112.4(3) yes
C1A C18A C17A 116.5(3) yes
N6A C18A C17A 103.7(3) yes
C1A C20A O21A 106.5(3) yes
C2B C1B C18B 118.9(3) yes
C2B C1B C20B 107.7(3) yes
C18B C1B C20B 110.0(3) yes
C1B C2B C3B 129.1(3) yes
C2B C3B C4B 127.1(4) yes
C3B C4B O5B 115.3(3) yes
C4B O5B N6B 105.3(3) yes
O5B N6B C7B 107.5(3) yes
O5B N6B C18B 105.1(3) yes
C7B N6B C18B 109.4(3) yes
N6B C7B C8B 109.8(3) yes
C7B C8B C9B 109.6(3) yes
C8B C9B C10B 130.9(3) yes
C8B C9B C17B 117.3(3) yes
C10B C9B C17B 111.4(3) yes
C9B C10B C11B 133.4(4) yes
C2C C1C C18C 116.2(3) yes
C2C C1C C20C 106.0(3) yes
C18C C1C C20C 109.3(3) yes
C1C C2C C3C 133.5(4) yes
C2C C3C C4C 125.2(4) yes
C3C C4C O5C 116.0(3) yes
C4C O5C N6C 104.5(3) yes
O5C N6C C7C 106.7(3) yes
O5C N6C C18C 100.1(3) yes
C7C N6C C18C 112.2(3) yes
N6C C7C C8C 104.3(3) yes
C7C C8C C9C 105.1(3) yes
C8C C9C C10C 127.4(3) yes
C8C C9C C17C 126.7(4) yes
C10C C9C C17C 105.6(3) yes
C9C C10C C11C 129.9(3) yes
C9C C10C C15C 108.6(3) yes
C11C C10C C15C 121.5(3) yes
C10C C11C C12C 113.6(3) yes
C11C C12C C13C 123.0(4) yes
C12C C13C C14C 123.2(4) yes
C13C C14C C15C 116.8(4) yes
C10C C15C C14C 121.8(3) yes
C10C C15C N16C 108.0(3) yes
C14C C15C N16C 130.2(3) yes
C15C N16C C17C 110.4(3) yes
C15C N16C C19C 123.7(4) yes
C17C N16C C19C 125.7(4) yes
C9C C17C N16C 107.3(3) yes
C9C C17C C18C 122.7(3) yes
N16C C17C C18C 129.9(3) yes
C1C C18C N6C 114.2(3) yes
C1C C18C C17C 114.2(3) yes
N6C C18C C17C 103.2(3) yes
C1C C20C O21C 107.1(3) yes
C2D C1D C18D 119.0(3) yes
C2D C1D C20D 108.3(3) yes
C18D C1D C20D 111.0(3) yes
C1D C2D C3D 127.0(3) yes
C2D C3D C4D 128.7(4) yes
C3D C4D O5D 109.7(3) yes
C4D O5D N6D 109.9(3) yes
O5D N6D C7D 106.8(3) yes
O5D N6D C18D 107.4(3) yes
C7D N6D C18D 112.9(3) yes
N6D C7D C8D 109.5(3) yes
C7D C8D C9D 113.0(4) yes
C8D C9D C10D 130.2(3) yes
C8D C9D C17D 119.7(3) yes
C10D C9D C17D 110.1(3) yes
C9D C10D C11D 137.7(4) yes
C9B C10B C15B 107.7(3) yes
C11B C10B C15B 118.9(4) yes
C10B C11B C12B 115.7(3) yes
C11B C12B C13B 122.7(4) yes
C12B C13B C14B 123.1(3) yes
C13B C14B C15B 116.0(4) yes
C10B C15B C14B 123.6(3) yes
C10B C15B N16B 106.0(3) yes
C14B C15B N16B 130.4(3) yes
C15B N16B C17B 109.0(3) yes
C15B N16B C19B 118.4(3) yes
C17B N16B C19B 131.9(3) yes
C9B C17B N16B 105.8(3) yes
C9B C17B C18B 127.5(3) yes
N16B C17B C18B 126.6(3) yes
C1B C18B N6B 107.3(3) yes
C1B C18B C17B 118.4(3) yes
N6B C18B C17B 105.9(3) yes
C1B C20B O21B 108.2(3) yes
C9D C10D C15D 104.1(3) yes
C11D C10D C15D 118.1(4) yes
C10D C11D C12D 120.4(4) yes
C11D C12D C13D 122.0(4) yes
C12D C13D C14D 118.7(4) yes
C13D C14D C15D 115.9(4) yes
C10D C15D C14D 124.9(4) yes
C10D C15D N16D 108.9(3) yes
C14D C15D N16D 126.2(3) yes
C15D N16D C17D 105.4(3) yes
C15D N16D C19D 121.5(3) yes
C17D N16D C19D 132.6(3) yes
C9D C17D N16D 111.5(3) yes
C9D C17D C18D 124.8(3) yes
N16D C17D C18D 123.8(3) yes
C1D C18D N6D 106.4(3) yes
C1D C18D C17D 118.5(3) yes
N6D C18D C17D 106.0(3) yes
C1D C20D O21D 110.2(3) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
C1A C2A 1.569(7) yes
C1A C18A 1.503(7) yes
C1A C20A 1.545(7) yes
C2A C3A 1.294(7) yes
C3A C4A 1.545(8) yes
C4A O5A 1.437(7) yes
O5A N6A 1.450(6) yes
N6A C7A 1.502(7) yes
N6A C18A 1.497(6) yes
C7A C8A 1.545(8) yes
C8A C9A 1.488(7) yes
C9A C10A 1.444(7) yes
C9A C17A 1.363(7) yes
C10A C11A 1.438(7) yes
C10A C15A 1.389(7) yes
C11A C12A 1.315(9) yes
C12A C13A 1.510(10) yes
C13A C14A 1.398(9) yes
C14A C15A 1.428(8) yes
C15A N16A 1.323(6) yes
N16A C17A 1.343(6) yes
N16A C19A 1.492(7) yes
C17A C18A 1.571(7) yes
C20A O21A 1.374(6) yes
C1B C2B 1.473(7) yes
C1B C18B 1.608(7) yes
C1B C20B 1.515(7) yes
C2B C3B 1.347(8) yes
C3B C4B 1.398(9) yes
C4B O5B 1.440(8) yes
O5B N6B 1.451(6) yes
N6B C7B 1.438(7) yes
N6B C18B 1.462(7) yes
C7B C8B 1.499(8) yes
C8B C9B 1.519(8) yes
C9B C10B 1.392(7) yes
C9B C17B 1.385(7) yes
C10B C11B 1.375(8) yes
C10B C15B 1.427(7) yes
C11B C12B 1.458(8) yes
C12B C13B 1.293(8) yes
C13B C14B 1.393(8) yes
C14B C15B 1.355(7) yes
C15B N16B 1.433(7) yes
N16B C17B 1.433(6) yes
N16B C19B 1.444(7) yes
C17B C18B 1.441(7) yes
C20B O21B 1.493(7) yes
C1C C2C 1.568(8) yes
C1C C18C 1.565(8) yes
C1C C20C 1.559(8) yes
C2C C3C 1.252(8) yes
C3C C4C 1.441(9) yes
C4C O5C 1.525(7) yes
O5C N6C 1.475(7) yes
N6C C7C 1.448(8) yes
N6C C18C 1.455(7) yes
C7C C8C 1.588(8) yes
C8C C9C 1.468(8) yes
C9C C10C 1.459(7) yes
C9C C17C 1.340(8) yes
C10C C11C 1.467(8) yes
C10C C15C 1.335(7) yes
C11C C12C 1.381(8) yes
C12C C13C 1.300(9) yes
C13C C14C 1.394(8) yes
C14C C15C 1.353(7) yes
C15C N16C 1.327(7) yes
N16C C17C 1.408(7) yes
N16C C19C 1.470(8) yes
C17C C18C 1.515(8) yes
C20C O21C 1.415(7) yes
C1D C2D 1.475(8) yes
C1D C18D 1.567(7) yes
C1D C20D 1.496(7) yes
C2D C3D 1.419(8) yes
C3D C4D 1.531(9) yes
C4D O5D 1.312(8) yes
O5D N6D 1.457(6) yes
N6D C7D 1.518(7) yes
N6D C18D 1.490(6) yes
C7D C8D 1.441(8) yes
C8D C9D 1.514(8) yes
C9D C10D 1.384(8) yes
C9D C17D 1.407(7) yes
C10D C11D 1.352(8) yes
C10D C15D 1.494(8) yes
C11D C12D 1.420(10) yes
C12D C13D 1.500(10) yes
C13D C14D 1.436(9) yes
C14D C15D 1.418(9) yes
C15D N16D 1.438(7) yes
N16D C17D 1.373(6) yes
N16D C19D 1.443(7) yes
C17D C18D 1.505(7) yes
C20D O21D 1.437(7) yes
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
C18A C1A C2A C3A -45.8(6) yes
C20A C1A C2A C3A 78.9(6) yes
C2A C1A C18A N6A 16.6(4) yes
C2A C1A C18A C17A -102.8(4) yes
C20A C1A C18A N6A -106.8(4) yes
C20A C1A C18A C17A 133.8(4) yes
C2A C1A C20A O21A 162.0(4) yes
C18A C1A C20A O21A -70.1(4) yes
C1A C2A C3A C4A 3.7(5) yes
C2A C3A C4A O5A 5.0(4) yes
C3A C4A O5A N6A 56.7(4) yes
C4A O5A N6A C7A 122.7(4) yes
C4A O5A N6A C18A -115.8(4) yes
O5A N6A C7A C8A -172.0(4) yes
C18A N6A C7A C8A 74.9(4) yes
O5A N6A C18A C1A 61.6(4) yes
O5A N6A C18A C17A -171.8(4) yes
C7A N6A C18A C1A 175.7(5) yes
C7A N6A C18A C17A -57.7(4) yes
N6A C7A C8A C9A -45.7(4) yes
C7A C8A C9A C10A -165.0(6) yes
C7A C8A C9A C17A 15.0(6) yes
C9A C17A C18A C1A 142.8(5) yes
C9A C17A C18A N6A 18.8(3) yes
N16A C17A C18A C1A -41.1(4) yes
N16A C17A C18A N6A -165.1(4) yes
C18B C1B C2B C3B 48.2(6) yes
C20B C1B C2B C3B -77.7(7) yes
C2B C1B C18B N6B -16.7(4) yes
C2B C1B C18B C17B 103.1(5) yes
C20B C1B C18B N6B 108.1(4) yes
C20B C1B C18B C17B -132.2(5) yes
C2B C1B C20B O21B -168.2(5) yes
C18B C1B C20B O21B 60.9(4) yes
C1B C2B C3B C4B -11.7(6) yes
C2B C3B C4B O5B 4.7(5) yes
C3B C4B O5B N6B -61.7(4) yes
C4B O5B N6B C7B -127.8(5) yes
C4B O5B N6B C18B 115.7(4) yes
O5B N6B C7B C8B 170.8(5) yes
C18B N6B C7B C8B -75.6(5) yes
O5B N6B C18B C1B -61.4(4) yes
O5B N6B C18B C17B 171.2(4) yes
C7B N6B C18B C1B -176.6(5) yes
C7B N6B C18B C17B 56.0(4) yes
N6B C7B C8B C9B 46.2(4) yes
C7B C8B C9B C10B 165.2(6) yes
C7B C8B C9B C17B -6.8(5) yes
C9B C17B C18B C1B -136.1(6) yes
C9B C17B C18B N6B -15.6(4) yes
N16B C17B C18B C1B 41.5(4) yes
N16B C17B C18B N6B 162.0(5) yes
C18C C1C C2C C3C -42.3(7) yes
C20C C1C C2C C3C 79.4(8) yes
C2C C1C C18C N6C 9.6(4) yes
C2C C1C C18C C17C -108.8(5) yes
C20C C1C C18C N6C -110.2(5) yes
C20C C1C C18C C17C 131.3(5) yes
C2C C1C C20C O21C 162.8(5) yes
C18C C1C C20C O21C -71.2(4) yes
C1C C2C C3C C4C 9.4(5) yes
C2C C3C C4C O5C -4.4(5) yes
C3C C4C O5C N6C 63.4(4) yes
C4C O5C N6C C7C 130.7(5) yes
C4C O5C N6C C18C -112.3(4) yes
O5C N6C C7C C8C -170.6(5) yes
C18C N6C C7C C8C 80.8(4) yes
O5C N6C C18C C1C 63.3(5) yes
O5C N6C C18C C17C -172.2(4) yes
C7C N6C C18C C1C 176.1(5) yes
C7C N6C C18C C17C -59.4(4) yes
N6C C7C C8C C9C -49.5(4) yes
C7C C8C C9C C10C -159.9(6) yes
C7C C8C C9C C17C 12.3(6) yes
C9C C17C C18C C1C 140.0(5) yes
C9C C17C C18C N6C 15.5(4) yes
N16C C17C C18C C1C -42.4(4) yes
N16C C17C C18C N6C -166.9(5) yes
C18D C1D C2D C3D -45.0(6) yes
C20D C1D C2D C3D 83.0(6) yes
C2D C1D C18D N6D 16.1(4) yes
C2D C1D C18D C17D -103.0(5) yes
C20D C1D C18D N6D -110.5(4) yes
C20D C1D C18D C17D 130.3(5) yes
C2D C1D C20D O21D 169.3(5) yes
C18D C1D C20D O21D -58.3(4) yes
C1D C2D C3D C4D 3.6(6) yes
C2D C3D C4D O5D 4.5(4) yes
C3D C4D O5D N6D 55.3(4) yes
C4D O5D N6D C7D 117.9(5) yes
C4D O5D N6D C18D -120.8(5) yes
O5D N6D C7D C8D -172.1(5) yes
C18D N6D C7D C8D 70.1(5) yes
O5D N6D C18D C1D 63.8(4) yes
O5D N6D C18D C17D -169.2(4) yes
C7D N6D C18D C1D 178.8(5) yes
C7D N6D C18D C17D -51.8(4) yes
N6D C7D C8D C9D -44.9(5) yes
C7D C8D C9D C10D -166.0(7) yes
C7D C8D C9D C17D 11.5(5) yes
C9D C17D C18D C1D 136.0(5) yes
C9D C17D C18D N6D 16.6(4) yes
N16D C17D C18D C1D -44.0(4) yes
N16D C17D C18D N6D -163.4(5) yes
|
1100925.cif | #------------------------------------------------------------------------------
#$Date: 2022-09-14 18:21:52 +0300 (Wed, 14 Sep 2022) $
#$Revision: 277833 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/09/1100925.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_1100925
loop_
_publ_author_name
'Emme, Holger'
'Valldor, Martin'
'P\"ottgen, Rainer'
'Huppertz, Hubert'
_publ_section_title
;
Associating Borate and Silicate Chemistry by Extreme Conditions:
High-Pressure Synthesis, Crystal Structure, and Properties of
the New Borates RE~3~B~5~O~12~ (RE = Er--Lu)
;
_journal_coden_ASTM CMATEX
_journal_issue 10
_journal_name_full 'Chemistry of Materials'
_journal_page_first 2707
_journal_page_last 2715
_journal_paper_doi 10.1021/cm047741+
_journal_volume 17
_journal_year 2005
_chemical_formula_moiety 'B5 Er3 O12'
_chemical_formula_sum 'B5 Er3 O12'
_chemical_formula_weight 747.83
_chemical_name_common Trierbiumpentaborate
_chemical_name_systematic Trierbiumpentaborate
_space_group_IT_number 53
_space_group_name_Hall '-P 2ac 2'
_space_group_name_H-M_alt 'P m n a'
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall '-P 2ac 2'
_symmetry_space_group_name_H-M 'P m n a'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_contact_author_address
;
'Department Chemie
Ludwig-Maximilians-Universitaet Muenchen
Butenandtstrasse 5-13 (Haus D)
81377 Muenchen
Germany'
;
_audit_contact_author_email huh@cup.uni-muenchen.de
_audit_contact_author_fax '+49 (0)89 2180 77440'
_audit_contact_author_phone '+49 (0)89 2180 77443'
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 12.8458(10)
_cell_length_b 4.6186(10)
_cell_length_c 12.5128(10)
_cell_measurement_reflns_used 4845
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 32.032
_cell_measurement_theta_min 3.134
_cell_volume 742.38(18)
_computing_cell_refinement 'HKL SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection 'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL DENZO (Otwinowski & Minor, 1997) and SCALEPACK'
_computing_molecular_graphics 'DIAMOND (Brandenburg & Berndt, 1999)'
_computing_publication_material 'enCIFer (Allen et al., 2004) and SHELXL97'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 293
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type KappaCCD
_diffrn_measurement_method '95mm CCD camera on \k-goniostat'
_diffrn_radiation_collimation 0.35
_diffrn_radiation_monochromator 'vertically mounted graphite crystal'
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0589
_diffrn_reflns_av_sigmaI/netI 0.0382
_diffrn_reflns_limit_h_max 19
_diffrn_reflns_limit_h_min -19
_diffrn_reflns_limit_k_max 6
_diffrn_reflns_limit_k_min -6
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_number 14145
_diffrn_reflns_theta_full 32.09
_diffrn_reflns_theta_max 32.09
_diffrn_reflns_theta_min 3.17
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 33.688
_exptl_absorpt_correction_T_max 0.5400
_exptl_absorpt_correction_T_min 0.3214
_exptl_absorpt_correction_type numerical
_exptl_absorpt_process_details 'Herrendorf,B\"arnighausen,HABITUS, 1993/1997'
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 6.691
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description Platelet
_exptl_crystal_F_000 1300
_exptl_crystal_size_max 0.04
_exptl_crystal_size_mid 0.03
_exptl_crystal_size_min 0.02
_refine_diff_density_max 2.166
_refine_diff_density_min -2.886
_refine_diff_density_rms 0.511
_refine_ls_extinction_coef 0.00172(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 1.033
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 90
_refine_ls_number_reflns 1301
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.033
_refine_ls_R_factor_all 0.0464
_refine_ls_R_factor_gt 0.0252
_refine_ls_shift/su_max 3.778
_refine_ls_shift/su_mean 0.042
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0224P)^2^+3.5070P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0571
_refine_ls_wR_factor_ref 0.0651
_reflns_number_gt 840
_reflns_number_total 1301
_reflns_threshold_expression >2sigma(I)
_cod_duplicate_entry 4000503
_cod_data_source_file cm047741+si20041223_064507.cif
_cod_data_source_block Er3B5O12
_cod_original_sg_symbol_H-M Pmna
_cod_database_code 1100925
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'
'-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
Er1 Er 0.13319(2) 0.0000 0.5000 0.00453(11) Uani 1 2 d S . .
Er2 Er 0.364648(17) 0.00062(7) 0.692420(19) 0.00526(10) Uani 1 1 d . . .
B1 B 0.3383(6) -0.5000 0.5000 0.0048(14) Uiso 1 2 d S . .
B2 B 0.2984(5) -0.5310(14) 0.8482(4) 0.0045(12) Uiso 1 1 d . . .
B3 B 0.0000 0.4597(17) 0.3496(6) 0.0000(15) Uiso 1 2 d S . .
B4 B 0.0000 0.541(2) 0.8756(8) 0.010(2) Uani 1 2 d S . .
O1 O 0.0000 0.2414(11) 0.4284(5) 0.0071(11) Uani 1 2 d S . .
O2 O 0.0000 0.2440(12) 0.8624(5) 0.0077(12) Uani 1 2 d S . .
O3 O 0.2958(3) -0.2217(8) 0.8480(3) 0.0064(8) Uani 1 1 d . . .
O4 O 0.4040(3) -0.6572(9) 0.8538(3) 0.0066(8) Uani 1 1 d . . .
O5 O 0.4041(3) -0.6650(8) 0.4271(3) 0.0069(8) Uani 1 1 d . . .
O6 O 0.2500 -0.6551(11) 0.7500 0.0063(11) Uani 1 2 d S . .
O7 O 0.5000 -0.3045(11) 0.7365(5) 0.0077(11) Uani 1 2 d S . .
O8 O 0.2662(3) -0.6885(8) 0.5655(3) 0.0061(8) 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
Er1 0.00358(17) 0.00573(18) 0.00429(18) 0.00051(18) 0.000 0.000
Er2 0.00400(14) 0.00607(15) 0.00571(16) -0.00042(13) 0.00039(8) -0.00005(11)
B4 0.010(4) 0.013(5) 0.009(4) -0.003(4) 0.000 0.000
O1 0.004(3) 0.006(3) 0.011(3) 0.003(2) 0.000 0.000
O2 0.009(3) 0.005(3) 0.008(3) -0.002(2) 0.000 0.000
O3 0.0055(19) 0.008(2) 0.006(2) 0.0011(15) -0.0011(16) -0.0011(16)
O4 0.0027(18) 0.009(2) 0.009(2) -0.0007(16) 0.0004(16) -0.0020(16)
O5 0.0059(18) 0.0075(18) 0.007(2) 0.0003(16) 0.0021(17) -0.0011(15)
O6 0.008(3) 0.009(3) 0.001(3) 0.000 0.000(2) 0.000
O7 0.006(3) 0.006(3) 0.012(3) 0.000(2) 0.000 0.000
O8 0.0063(18) 0.0073(18) 0.0048(19) -0.0016(16) 0.0010(16) -0.0023(15)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_audit_author_name
'Emme, H.'
'Huppertz, H.'
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 Er1 O1 79.8(2) 5_556 . ?
O1 Er1 O3 75.77(15) 5_556 4_556 ?
O1 Er1 O3 147.44(16) . 4_556 ?
O1 Er1 O3 147.44(16) 5_556 2_554 ?
O1 Er1 O3 75.77(15) . 2_554 ?
O3 Er1 O3 134.20(19) 4_556 2_554 ?
O1 Er1 O8 135.63(17) 5_556 1_565 ?
O1 Er1 O8 112.77(15) . 1_565 ?
O3 Er1 O8 72.86(13) 4_556 1_565 ?
O3 Er1 O8 74.68(13) 2_554 1_565 ?
O1 Er1 O8 112.77(15) 5_556 3_546 ?
O1 Er1 O8 135.63(17) . 3_546 ?
O3 Er1 O8 74.68(13) 4_556 3_546 ?
O3 Er1 O8 72.86(13) 2_554 3_546 ?
O8 Er1 O8 88.19(18) 1_565 3_546 ?
O1 Er1 O4 80.13(17) 5_556 2_544 ?
O1 Er1 O4 82.78(17) . 2_544 ?
O3 Er1 O4 113.36(14) 4_556 2_544 ?
O3 Er1 O4 75.77(13) 2_554 2_544 ?
O8 Er1 O4 141.51(13) 1_565 2_544 ?
O8 Er1 O4 59.69(13) 3_546 2_544 ?
O1 Er1 O4 82.79(17) 5_556 4_566 ?
O1 Er1 O4 80.13(17) . 4_566 ?
O3 Er1 O4 75.77(13) 4_556 4_566 ?
O3 Er1 O4 113.36(14) 2_554 4_566 ?
O8 Er1 O4 59.69(13) 1_565 4_566 ?
O8 Er1 O4 141.51(13) 3_546 4_566 ?
O4 Er1 O4 157.67(18) 2_544 4_566 ?
O1 Er1 B2 109.25(18) 5_556 4_566 ?
O1 Er1 B2 96.76(18) . 4_566 ?
O3 Er1 B2 71.88(15) 4_556 4_566 ?
O3 Er1 B2 94.82(14) 2_554 4_566 ?
O8 Er1 B2 30.52(15) 1_565 4_566 ?
O8 Er1 B2 116.27(15) 3_546 4_566 ?
O4 Er1 B2 170.43(15) 2_544 4_566 ?
O4 Er1 B2 29.17(15) 4_566 4_566 ?
O1 Er1 B2 96.76(18) 5_556 2_544 ?
O1 Er1 B2 109.25(19) . 2_544 ?
O3 Er1 B2 94.82(14) 4_556 2_544 ?
O3 Er1 B2 71.88(15) 2_554 2_544 ?
O8 Er1 B2 116.27(15) 1_565 2_544 ?
O8 Er1 B2 30.52(15) 3_546 2_544 ?
O4 Er1 B2 29.17(15) 2_544 2_544 ?
O4 Er1 B2 170.43(15) 4_566 2_544 ?
B2 Er1 B2 146.1(2) 4_566 2_544 ?
O1 Er1 Er1 39.90(10) 5_556 5_556 ?
O1 Er1 Er1 39.90(10) . 5_556 ?
O3 Er1 Er1 112.90(9) 4_556 5_556 ?
O3 Er1 Er1 112.90(9) 2_554 5_556 ?
O8 Er1 Er1 135.91(9) 1_565 5_556 ?
O8 Er1 Er1 135.91(9) 3_546 5_556 ?
O4 Er1 Er1 78.84(9) 2_544 5_556 ?
O4 Er1 Er1 78.84(9) 4_566 5_556 ?
B2 Er1 Er1 106.95(12) 4_566 5_556 ?
B2 Er1 Er1 106.95(12) 2_544 5_556 ?
O1 Er1 Er2 110.10(12) 5_556 . ?
O1 Er1 Er2 148.07(13) . . ?
O3 Er1 Er2 35.66(10) 4_556 . ?
O3 Er1 Er2 101.99(9) 2_554 . ?
O8 Er1 Er2 39.17(9) 1_565 . ?
O8 Er1 Er2 70.06(9) 3_546 . ?
O4 Er1 Er2 128.15(9) 2_544 . ?
O4 Er1 Er2 71.53(9) 4_566 . ?
B2 Er1 Er2 51.39(12) 4_566 . ?
B2 Er1 Er2 99.84(12) 2_544 . ?
Er1 Er1 Er2 140.999(6) 5_556 . ?
O2 Er2 O5 88.06(18) 6_657 3_546 ?
O2 Er2 O6 104.74(16) 6_657 1_565 ?
O5 Er2 O6 148.05(10) 3_546 1_565 ?
O2 Er2 O7 77.82(15) 6_657 . ?
O5 Er2 O7 63.95(17) 3_546 . ?
O6 Er2 O7 146.78(15) 1_565 . ?
O2 Er2 O3 148.65(17) 6_657 4_556 ?
O5 Er2 O3 75.52(13) 3_546 4_556 ?
O6 Er2 O3 78.89(12) 1_565 4_556 ?
O7 Er2 O3 116.38(15) . 4_556 ?
O2 Er2 O3 141.12(17) 6_657 . ?
O5 Er2 O3 109.68(14) 3_546 . ?
O6 Er2 O3 78.58(12) 1_565 . ?
O7 Er2 O3 79.65(16) . . ?
O3 Er2 O3 70.21(16) 4_556 . ?
O2 Er2 O8 84.65(14) 6_657 1_565 ?
O5 Er2 O8 95.11(13) 3_546 1_565 ?
O6 Er2 O8 58.10(9) 1_565 1_565 ?
O7 Er2 O8 152.80(16) . 1_565 ?
O3 Er2 O8 70.74(13) 4_556 1_565 ?
O3 Er2 O8 125.77(13) . 1_565 ?
O2 Er2 O4 77.13(17) 6_657 1_565 ?
O5 Er2 O4 154.38(13) 3_546 1_565 ?
O6 Er2 O4 57.31(10) 1_565 1_565 ?
O7 Er2 O4 92.24(17) . 1_565 ?
O3 Er2 O4 126.74(13) 4_556 1_565 ?
O3 Er2 O4 72.53(13) . 1_565 ?
O8 Er2 O4 104.04(13) 1_565 1_565 ?
O2 Er2 B4 78.80(18) 6_657 6_647 ?
O5 Er2 B4 31.09(19) 3_546 6_647 ?
O6 Er2 B4 176.46(17) 1_565 6_647 ?
O7 Er2 B4 33.1(2) . 6_647 ?
O3 Er2 B4 98.24(15) 4_556 6_647 ?
O3 Er2 B4 98.5(2) . 6_647 ?
O8 Er2 B4 123.1(2) 1_565 6_647 ?
O4 Er2 B4 123.97(18) 1_565 6_647 ?
O2 Er2 B2 93.32(19) 6_657 1_565 ?
O5 Er2 B2 176.41(15) 3_546 1_565 ?
O6 Er2 B2 28.36(12) 1_565 1_565 ?
O7 Er2 B2 119.59(19) . 1_565 ?
O3 Er2 B2 101.74(15) 4_556 1_565 ?
O3 Er2 B2 71.15(15) . 1_565 ?
O8 Er2 B2 81.72(15) 1_565 1_565 ?
O4 Er2 B2 29.13(15) 1_565 1_565 ?
B4 Er2 B2 152.49(19) 6_647 1_565 ?
O2 Er2 Er2 148.68(13) 6_657 4_556 ?
O5 Er2 Er2 120.17(10) 3_546 4_556 ?
O6 Er2 Er2 44.12(10) 1_565 4_556 ?
O7 Er2 Er2 124.92(12) . 4_556 ?
O3 Er2 Er2 46.29(9) 4_556 4_556 ?
O3 Er2 Er2 45.92(9) . 4_556 ?
O8 Er2 Er2 79.86(9) 1_565 4_556 ?
O4 Er2 Er2 80.45(9) 1_565 4_556 ?
B4 Er2 Er2 132.33(15) 6_647 4_556 ?
B2 Er2 Er2 57.71(12) 1_565 4_556 ?
O2 Er2 Er2 37.14(11) 6_657 7_655 ?
O5 Er2 Er2 76.77(10) 3_546 7_655 ?
O6 Er2 Er2 130.15(8) 1_565 7_655 ?
O7 Er2 Er2 41.04(10) . 7_655 ?
O3 Er2 Er2 150.95(9) 4_556 7_655 ?
O3 Er2 Er2 111.90(9) . 7_655 ?
O8 Er2 Er2 120.56(8) 1_565 7_655 ?
O4 Er2 Er2 78.86(9) 1_565 7_655 ?
B4 Er2 Er2 52.78(12) 6_647 7_655 ?
B2 Er2 Er2 106.28(12) 1_565 7_655 ?
Er2 Er2 Er2 153.931(9) 4_556 7_655 ?
O5 B1 O5 109.2(6) 3_546 . ?
O5 B1 O8 113.1(2) 3_546 3_546 ?
O5 B1 O8 108.5(2) . 3_546 ?
O5 B1 O8 108.5(2) 3_546 . ?
O5 B1 O8 113.1(2) . . ?
O8 B1 O8 104.5(6) 3_546 . ?
O3 B2 O4 114.6(5) . . ?
O3 B2 O6 111.9(5) . . ?
O4 B2 O6 105.7(4) . . ?
O3 B2 O8 117.3(5) . 4_556 ?
O4 B2 O8 105.9(4) . 4_556 ?
O6 B2 O8 99.8(4) . 4_556 ?
O3 B2 Er1 136.6(4) . 2_545 ?
O4 B2 Er1 54.5(3) . 2_545 ?
O6 B2 Er1 111.4(4) . 2_545 ?
O8 B2 Er1 51.5(2) 4_556 2_545 ?
O3 B2 Er2 135.9(4) . 1_545 ?
O4 B2 Er2 59.5(3) . 1_545 ?
O6 B2 Er2 46.7(2) . 1_545 ?
O8 B2 Er2 105.3(3) 4_556 1_545 ?
Er1 B2 Er2 79.09(16) 2_545 1_545 ?
O1 B3 O4 113.6(4) . 2_554 ?
O1 B3 O4 113.6(4) . 8 ?
O4 B3 O4 107.0(6) 2_554 8 ?
O1 B3 O7 107.5(6) . 2_554 ?
O4 B3 O7 107.4(4) 2_554 2_554 ?
O4 B3 O7 107.4(4) 8 2_554 ?
O2 B4 O5 115.5(4) . 2 ?
O2 B4 O5 115.5(4) . 8_556 ?
O5 B4 O5 109.9(7) 2 8_556 ?
O2 B4 O7 110.2(7) . 6_567 ?
O5 B4 O7 102.0(5) 2 6_567 ?
O5 B4 O7 102.0(5) 8_556 6_567 ?
O2 B4 Er2 134.3(4) . 4_566 ?
O5 B4 Er2 49.4(3) 2 4_566 ?
O5 B4 Er2 109.9(5) 8_556 4_566 ?
O7 B4 Er2 53.2(3) 6_567 4_566 ?
O2 B4 Er2 134.3(4) . 6_567 ?
O5 B4 Er2 109.9(5) 2 6_567 ?
O5 B4 Er2 49.4(3) 8_556 6_567 ?
O7 B4 Er2 53.2(3) 6_567 6_567 ?
Er2 B4 Er2 74.4(2) 4_566 6_567 ?
B3 O1 Er1 129.68(11) . 5_556 ?
B3 O1 Er1 129.68(11) . . ?
Er1 O1 Er1 100.2(2) 5_556 . ?
B4 O2 Er2 123.3(2) . 6_557 ?
B4 O2 Er2 123.3(2) . 4_556 ?
Er2 O2 Er2 105.7(2) 6_557 4_556 ?
B2 O3 Er1 115.2(3) . 2 ?
B2 O3 Er2 117.2(3) . 4_556 ?
Er1 O3 Er2 108.90(15) 2 4_556 ?
B2 O3 Er2 115.2(3) . . ?
Er1 O3 Er2 109.36(15) 2 . ?
Er2 O3 Er2 87.79(13) 4_556 . ?
B2 O4 B3 120.1(5) . 2 ?
B2 O4 Er1 96.4(3) . 2_545 ?
B3 O4 Er1 124.2(3) 2 2_545 ?
B2 O4 Er2 91.4(3) . 1_545 ?
B3 O4 Er2 119.2(3) 2 1_545 ?
Er1 O4 Er2 98.48(14) 2_545 1_545 ?
B1 O5 B4 122.9(5) . 2_554 ?
B1 O5 Er2 131.0(3) . 3_546 ?
B4 O5 Er2 99.5(4) 2_554 3_546 ?
B2 O6 B2 134.8(6) 4_556 . ?
B2 O6 Er2 105.0(3) 4_556 4_546 ?
B2 O6 Er2 106.1(3) . 4_546 ?
B2 O6 Er2 106.1(3) 4_556 1_545 ?
B2 O6 Er2 105.0(3) . 1_545 ?
Er2 O6 Er2 91.76(19) 4_546 1_545 ?
B4 O7 B3 126.1(6) 6_647 2 ?
B4 O7 Er2 93.7(3) 6_647 . ?
B3 O7 Er2 119.3(2) 2 . ?
B4 O7 Er2 93.7(3) 6_647 7_655 ?
B3 O7 Er2 119.3(2) 2 7_655 ?
Er2 O7 Er2 97.9(2) . 7_655 ?
B1 O8 B2 115.9(3) . 4_556 ?
B1 O8 Er1 126.9(3) . 1_545 ?
B2 O8 Er1 98.0(3) 4_556 1_545 ?
B1 O8 Er2 111.6(3) . 1_545 ?
B2 O8 Er2 95.7(3) 4_556 1_545 ?
Er1 O8 Er2 103.64(14) 1_545 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
Er1 O1 2.230(3) 5_556 ?
Er1 O1 2.230(3) . ?
Er1 O3 2.345(4) 4_556 ?
Er1 O3 2.345(4) 2_554 ?
Er1 O8 2.380(4) 1_565 ?
Er1 O8 2.380(4) 3_546 ?
Er1 O4 2.466(4) 2_544 ?
Er1 O4 2.466(4) 4_566 ?
Er1 B2 3.012(6) 4_566 ?
Er1 B2 3.012(6) 2_544 ?
Er1 Er1 3.4220(7) 5_556 ?
Er1 Er2 3.8259(9) . ?
Er2 O2 2.181(3) 6_657 ?
Er2 O5 2.213(4) 3_546 ?
Er2 O6 2.284(4) 1_565 ?
Er2 O7 2.305(4) . ?
Er2 O3 2.357(4) 4_556 ?
Er2 O3 2.372(4) . ?
Er2 O8 2.486(4) 1_565 ?
Er2 O4 2.614(4) 1_565 ?
Er2 B4 2.874(8) 6_647 ?
Er2 B2 3.033(6) 1_565 ?
Er2 Er2 3.2791(5) 4_556 ?
Er2 Er2 3.4774(5) 7_655 ?
B1 O5 1.459(6) 3_546 ?
B1 O5 1.459(6) . ?
B1 O8 1.512(6) 3_546 ?
B1 O8 1.512(6) . ?
B2 O3 1.429(7) . ?
B2 O4 1.477(8) . ?
B2 O6 1.492(6) . ?
B2 O8 1.545(7) 4_556 ?
B2 Er1 3.012(6) 2_545 ?
B2 Er2 3.033(6) 1_545 ?
B3 O1 1.410(9) . ?
B3 O4 1.535(6) 2_554 ?
B3 O4 1.535(6) 8 ?
B3 O7 1.586(9) 2_554 ?
B4 O2 1.380(11) . ?
B4 O5 1.505(7) 2 ?
B4 O5 1.505(7) 8_556 ?
B4 O7 1.574(11) 6_567 ?
B4 Er2 2.874(8) 4_566 ?
B4 Er2 2.874(8) 6_567 ?
O1 Er1 2.230(3) 5_556 ?
O2 Er2 2.181(3) 6_557 ?
O2 Er2 2.181(3) 4_556 ?
O3 Er1 2.345(4) 2 ?
O3 Er2 2.357(4) 4_556 ?
O4 B3 1.535(6) 2 ?
O4 Er1 2.466(4) 2_545 ?
O4 Er2 2.614(4) 1_545 ?
O5 B4 1.505(7) 2_554 ?
O5 Er2 2.213(4) 3_546 ?
O6 B2 1.492(6) 4_556 ?
O6 Er2 2.284(4) 4_546 ?
O6 Er2 2.284(4) 1_545 ?
O7 B4 1.574(11) 6_647 ?
O7 B3 1.586(9) 2 ?
O7 Er2 2.305(4) 7_655 ?
O8 B2 1.545(7) 4_556 ?
O8 Er1 2.380(4) 1_545 ?
O8 Er2 2.486(4) 1_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
O4 B3 O1 Er1 155.9(4) 2_554 . . 5_556 ?
O4 B3 O1 Er1 33.3(8) 8 . . 5_556 ?
O7 B3 O1 Er1 -85.4(4) 2_554 . . 5_556 ?
O4 B3 O1 Er1 -33.3(8) 2_554 . . . ?
O4 B3 O1 Er1 -155.9(4) 8 . . . ?
O7 B3 O1 Er1 85.4(4) 2_554 . . . ?
O1 Er1 O1 B3 -172.8(7) 5_556 . . . ?
O3 Er1 O1 B3 145.5(5) 4_556 . . . ?
O3 Er1 O1 B3 -14.5(5) 2_554 . . . ?
O8 Er1 O1 B3 51.8(6) 1_565 . . . ?
O8 Er1 O1 B3 -60.5(6) 3_546 . . . ?
O4 Er1 O1 B3 -91.6(6) 2_544 . . . ?
O4 Er1 O1 B3 102.9(6) 4_566 . . . ?
B2 Er1 O1 B3 78.8(6) 4_566 . . . ?
B2 Er1 O1 B3 -79.1(6) 2_544 . . . ?
Er1 Er1 O1 B3 -172.8(7) 5_556 . . . ?
Er2 Er1 O1 B3 75.4(6) . . . . ?
O1 Er1 O1 Er1 0.0 5_556 . . 5_556 ?
O3 Er1 O1 Er1 -41.8(4) 4_556 . . 5_556 ?
O3 Er1 O1 Er1 158.3(2) 2_554 . . 5_556 ?
O8 Er1 O1 Er1 -135.42(16) 1_565 . . 5_556 ?
O8 Er1 O1 Er1 112.2(2) 3_546 . . 5_556 ?
O4 Er1 O1 Er1 81.21(19) 2_544 . . 5_556 ?
O4 Er1 O1 Er1 -84.4(2) 4_566 . . 5_556 ?
B2 Er1 O1 Er1 -108.4(2) 4_566 . . 5_556 ?
B2 Er1 O1 Er1 93.7(2) 2_544 . . 5_556 ?
Er2 Er1 O1 Er1 -111.81(17) . . . 5_556 ?
O5 B4 O2 Er2 172.6(4) 2 . . 6_557 ?
O5 B4 O2 Er2 42.3(10) 8_556 . . 6_557 ?
O7 B4 O2 Er2 -72.6(4) 6_567 . . 6_557 ?
Er2 B4 O2 Er2 -130.3(3) 4_566 . . 6_557 ?
Er2 B4 O2 Er2 -14.8(10) 6_567 . . 6_557 ?
O5 B4 O2 Er2 -42.3(10) 2 . . 4_556 ?
O5 B4 O2 Er2 -172.6(4) 8_556 . . 4_556 ?
O7 B4 O2 Er2 72.6(4) 6_567 . . 4_556 ?
Er2 B4 O2 Er2 14.8(10) 4_566 . . 4_556 ?
Er2 B4 O2 Er2 130.3(3) 6_567 . . 4_556 ?
O4 B2 O3 Er1 -60.8(5) . . . 2 ?
O6 B2 O3 Er1 178.9(3) . . . 2 ?
O8 B2 O3 Er1 64.4(5) 4_556 . . 2 ?
Er1 B2 O3 Er1 2.7(7) 2_545 . . 2 ?
Er2 B2 O3 Er1 -131.6(4) 1_545 . . 2 ?
O4 B2 O3 Er2 169.1(3) . . . 4_556 ?
O6 B2 O3 Er2 48.7(5) . . . 4_556 ?
O8 B2 O3 Er2 -65.7(5) 4_556 . . 4_556 ?
Er1 B2 O3 Er2 -127.4(4) 2_545 . . 4_556 ?
Er2 B2 O3 Er2 98.3(5) 1_545 . . 4_556 ?
O4 B2 O3 Er2 67.9(5) . . . . ?
O6 B2 O3 Er2 -52.4(5) . . . . ?
O8 B2 O3 Er2 -166.9(3) 4_556 . . . ?
Er1 B2 O3 Er2 131.4(4) 2_545 . . . ?
Er2 B2 O3 Er2 -2.8(7) 1_545 . . . ?
O2 Er2 O3 B2 -106.9(4) 6_657 . . . ?
O5 Er2 O3 B2 5.8(4) 3_546 . . . ?
O6 Er2 O3 B2 153.7(4) 1_565 . . . ?
O7 Er2 O3 B2 -51.6(4) . . . . ?
O3 Er2 O3 B2 71.5(3) 4_556 . . . ?
O8 Er2 O3 B2 117.8(4) 1_565 . . . ?
O4 Er2 O3 B2 -147.3(4) 1_565 . . . ?
B4 Er2 O3 B2 -24.2(4) 6_647 . . . ?
B2 Er2 O3 B2 -177.9(5) 1_565 . . . ?
Er2 Er2 O3 B2 119.1(4) 4_556 . . . ?
Er2 Er2 O3 B2 -77.4(4) 7_655 . . . ?
O2 Er2 O3 Er1 24.6(3) 6_657 . . 2 ?
O5 Er2 O3 Er1 137.36(15) 3_546 . . 2 ?
O6 Er2 O3 Er1 -74.74(14) 1_565 . . 2 ?
O7 Er2 O3 Er1 80.01(19) . . . 2 ?
O3 Er2 O3 Er1 -156.91(17) 4_556 . . 2 ?
O8 Er2 O3 Er1 -110.65(16) 1_565 . . 2 ?
O4 Er2 O3 Er1 -15.68(14) 1_565 . . 2 ?
B4 Er2 O3 Er1 107.35(19) 6_647 . . 2 ?
B2 Er2 O3 Er1 -46.34(17) 1_565 . . 2 ?
Er2 Er2 O3 Er1 -109.27(19) 4_556 . . 2 ?
Er2 Er2 O3 Er1 54.15(16) 7_655 . . 2 ?
O2 Er2 O3 Er2 133.9(2) 6_657 . . 4_556 ?
O5 Er2 O3 Er2 -113.37(13) 3_546 . . 4_556 ?
O6 Er2 O3 Er2 34.52(9) 1_565 . . 4_556 ?
O7 Er2 O3 Er2 -170.72(16) . . . 4_556 ?
O3 Er2 O3 Er2 -47.64(16) 4_556 . . 4_556 ?
O8 Er2 O3 Er2 -1.38(19) 1_565 . . 4_556 ?
O4 Er2 O3 Er2 93.59(13) 1_565 . . 4_556 ?
B4 Er2 O3 Er2 -143.38(15) 6_647 . . 4_556 ?
B2 Er2 O3 Er2 62.93(15) 1_565 . . 4_556 ?
Er2 Er2 O3 Er2 163.41(6) 7_655 . . 4_556 ?
O3 B2 O4 B3 -5.0(7) . . . 2 ?
O6 B2 O4 B3 118.7(5) . . . 2 ?
O8 B2 O4 B3 -136.0(5) 4_556 . . 2 ?
Er1 B2 O4 B3 -136.0(5) 2_545 . . 2 ?
Er2 B2 O4 B3 125.3(5) 1_545 . . 2 ?
O3 B2 O4 Er1 131.0(4) . . . 2_545 ?
O6 B2 O4 Er1 -105.4(4) . . . 2_545 ?
O8 B2 O4 Er1 0.0(4) 4_556 . . 2_545 ?
Er2 B2 O4 Er1 -98.69(16) 1_545 . . 2_545 ?
O3 B2 O4 Er2 -130.4(4) . . . 1_545 ?
O6 B2 O4 Er2 -6.7(4) . . . 1_545 ?
O8 B2 O4 Er2 98.7(3) 4_556 . . 1_545 ?
Er1 B2 O4 Er2 98.69(16) 2_545 . . 1_545 ?
O5 B1 O5 B4 -42.5(5) 3_546 . . 2_554 ?
O8 B1 O5 B4 81.1(6) 3_546 . . 2_554 ?
O8 B1 O5 B4 -163.4(5) . . . 2_554 ?
O5 B1 O5 Er2 172.1(4) 3_546 . . 3_546 ?
O8 B1 O5 Er2 -64.2(4) 3_546 . . 3_546 ?
O8 B1 O5 Er2 51.2(5) . . . 3_546 ?
O3 B2 O6 B2 1.2(7) . . . 4_556 ?
O4 B2 O6 B2 -124.1(4) . . . 4_556 ?
O8 B2 O6 B2 126.1(4) 4_556 . . 4_556 ?
Er1 B2 O6 B2 178.5(3) 2_545 . . 4_556 ?
Er2 B2 O6 B2 -132.0(5) 1_545 . . 4_556 ?
O3 B2 O6 Er2 -130.4(4) . . . 4_546 ?
O4 B2 O6 Er2 104.2(4) . . . 4_546 ?
O8 B2 O6 Er2 -5.5(4) 4_556 . . 4_546 ?
Er1 B2 O6 Er2 46.8(3) 2_545 . . 4_546 ?
Er2 B2 O6 Er2 96.3(3) 1_545 . . 4_546 ?
O3 B2 O6 Er2 133.3(4) . . . 1_545 ?
O4 B2 O6 Er2 7.9(5) . . . 1_545 ?
O8 B2 O6 Er2 -101.9(3) 4_556 . . 1_545 ?
Er1 B2 O6 Er2 -49.5(3) 2_545 . . 1_545 ?
O2 Er2 O7 B4 -88.1(4) 6_657 . . 6_647 ?
O5 Er2 O7 B4 5.7(3) 3_546 . . 6_647 ?
O6 Er2 O7 B4 173.5(3) 1_565 . . 6_647 ?
O3 Er2 O7 B4 62.1(4) 4_556 . . 6_647 ?
O3 Er2 O7 B4 123.8(3) . . . 6_647 ?
O8 Er2 O7 B4 -37.0(5) 1_565 . . 6_647 ?
O4 Er2 O7 B4 -164.4(3) 1_565 . . 6_647 ?
B2 Er2 O7 B4 -175.0(3) 1_565 . . 6_647 ?
Er2 Er2 O7 B4 115.7(3) 4_556 . . 6_647 ?
Er2 Er2 O7 B4 -94.3(4) 7_655 . . 6_647 ?
O2 Er2 O7 B3 136.4(4) 6_657 . . 2 ?
O5 Er2 O7 B3 -129.8(4) 3_546 . . 2 ?
O6 Er2 O7 B3 38.0(5) 1_565 . . 2 ?
O3 Er2 O7 B3 -73.4(4) 4_556 . . 2 ?
O3 Er2 O7 B3 -11.8(4) . . . 2 ?
O8 Er2 O7 B3 -172.6(3) 1_565 . . 2 ?
O4 Er2 O7 B3 60.0(4) 1_565 . . 2 ?
B4 Er2 O7 B3 -135.5(5) 6_647 . . 2 ?
B2 Er2 O7 B3 49.5(4) 1_565 . . 2 ?
Er2 Er2 O7 B3 -19.9(5) 4_556 . . 2 ?
Er2 Er2 O7 B3 130.2(5) 7_655 . . 2 ?
O2 Er2 O7 Er2 6.2(2) 6_657 . . 7_655 ?
O5 Er2 O7 Er2 100.0(2) 3_546 . . 7_655 ?
O6 Er2 O7 Er2 -92.2(3) 1_565 . . 7_655 ?
O3 Er2 O7 Er2 156.41(15) 4_556 . . 7_655 ?
O3 Er2 O7 Er2 -141.9(2) . . . 7_655 ?
O8 Er2 O7 Er2 57.2(4) 1_565 . . 7_655 ?
O4 Er2 O7 Er2 -70.15(19) 1_565 . . 7_655 ?
B4 Er2 O7 Er2 94.3(4) 6_647 . . 7_655 ?
B2 Er2 O7 Er2 -80.7(2) 1_565 . . 7_655 ?
Er2 Er2 O7 Er2 -150.06(9) 4_556 . . 7_655 ?
O5 B1 O8 B2 53.3(6) 3_546 . . 4_556 ?
O5 B1 O8 B2 174.5(4) . . . 4_556 ?
O8 B1 O8 B2 -67.7(4) 3_546 . . 4_556 ?
O5 B1 O8 Er1 177.3(3) 3_546 . . 1_545 ?
O5 B1 O8 Er1 -61.5(6) . . . 1_545 ?
O8 B1 O8 Er1 56.3(2) 3_546 . . 1_545 ?
O5 B1 O8 Er2 -54.8(4) 3_546 . . 1_545 ?
O5 B1 O8 Er2 66.5(4) . . . 1_545 ?
O8 B1 O8 Er2 -175.7(3) 3_546 . . 1_545 ?
|
1100926.cif | #------------------------------------------------------------------------------
#$Date: 2022-09-14 18:21:52 +0300 (Wed, 14 Sep 2022) $
#$Revision: 277833 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/09/1100926.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_1100926
loop_
_publ_author_name
'Emme, Holger'
'Valldor, Martin'
'P\"ottgen, Rainer'
'Huppertz, Hubert'
_publ_section_title
;
Associating Borate and Silicate Chemistry by Extreme Conditions:
High-Pressure Synthesis, Crystal Structure, and Properties of
the New Borates RE~3~B~5~O~12~ (RE = Er--Lu)
;
_journal_coden_ASTM CMATEX
_journal_issue 10
_journal_name_full 'Chemistry of Materials'
_journal_page_first 2707
_journal_page_last 2715
_journal_paper_doi 10.1021/cm047741+
_journal_volume 17
_journal_year 2005
_chemical_formula_moiety 'B5 O12 Tm3'
_chemical_formula_sum 'B5 O12 Tm3'
_chemical_formula_weight 752.84
_chemical_name_common Trituliumpentaborate
_chemical_name_systematic Trituliumpentaborate
_space_group_IT_number 53
_space_group_name_Hall '-P 2ac 2'
_space_group_name_H-M_alt 'P m n a'
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall '-P 2ac 2'
_symmetry_space_group_name_H-M 'P m n a'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_contact_author_address
;
'Department Chemie und Biochemie
Ludwig-Maximilians-Universitaet Muenchen
Butenandtstrasse 5-13 (Haus D)
81377 Muenchen
Germany'
;
_audit_contact_author_email huh@cup.uni-muenchen.de
_audit_contact_author_fax '+49 (0)89 2180 77440'
_audit_contact_author_phone '+49 (0)89 2180 77442'
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 12.820(3)
_cell_length_b 4.6019(9)
_cell_length_c 12.477(3)
_cell_measurement_reflns_used 4232
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 32.85
_cell_measurement_theta_min 4.40
_cell_volume 736.1(3)
_computing_molecular_graphics 'DIAMOND (Brandenburg & Berndt, 1999)'
_computing_publication_material 'enCIFer (Allen et al., 2004) and SHELXL97'
_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 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type 'STOE IPDS'
_diffrn_measurement_method 'profile data from \f/\w-scans'
_diffrn_radiation_collimation 0.5
_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 0.0521
_diffrn_reflns_av_sigmaI/netI 0.0344
_diffrn_reflns_limit_h_max 19
_diffrn_reflns_limit_h_min -19
_diffrn_reflns_limit_k_max 6
_diffrn_reflns_limit_k_min -6
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 8905
_diffrn_reflns_theta_full 32.92
_diffrn_reflns_theta_max 32.92
_diffrn_reflns_theta_min 4.56
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 35.932
_exptl_absorpt_correction_T_max 0.2821
_exptl_absorpt_correction_T_min 0.1628
_exptl_absorpt_correction_type numerical
_exptl_absorpt_process_details 'Herrendorf,B\"arnighausen,HABITUS, 1993/1997'
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 6.793
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description platelet
_exptl_crystal_F_000 1312
_exptl_crystal_size_max 0.10
_exptl_crystal_size_mid 0.05
_exptl_crystal_size_min 0.04
_refine_diff_density_max 3.171
_refine_diff_density_min -5.779
_refine_diff_density_rms 0.805
_refine_ls_extinction_coef 0.0043(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 0.814
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 95
_refine_ls_number_reflns 1412
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.814
_refine_ls_R_factor_all 0.0642
_refine_ls_R_factor_gt 0.0376
_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^)+(0.0713P)^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 0.1001
_reflns_number_gt 751
_reflns_number_total 1412
_reflns_threshold_expression >2sigma(I)
_cod_duplicate_entry 4000576
_cod_data_source_file cm047741+si20041223_064526.cif
_cod_data_source_block Tm3B5O12
_cod_original_sg_symbol_H-M Pmna
_cod_database_code 1100926
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'
'-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
Tm1 Tm 0.13251(3) 0.0000 0.5000 0.00662(14) Uani 1 2 d S . .
Tm2 Tm 0.36474(2) 0.00032(15) 0.69281(2) 0.00717(14) Uani 1 1 d . . .
B1 B 0.3377(8) -0.5000 0.5000 0.0068(17) Uiso 1 2 d S . .
B2 B 0.2989(7) -0.524(3) 0.8488(6) 0.0074(18) Uani 1 1 d . . .
B3 B 0.0000 0.461(4) 0.3494(10) 0.010(3) Uani 1 2 d S . .
B4 B 0.0000 0.542(4) 0.8752(11) 0.011(3) Uani 1 2 d S . .
O1 O 0.0000 0.240(2) 0.4286(7) 0.0097(17) Uani 1 2 d S . .
O2 O 0.0000 0.241(2) 0.8624(7) 0.0093(17) Uani 1 2 d S . .
O3 O 0.2956(5) -0.2188(15) 0.8487(5) 0.0091(12) Uani 1 1 d . . .
O4 O 0.4046(5) -0.6584(15) 0.8543(5) 0.0089(11) Uani 1 1 d . . .
O5 O 0.4034(5) -0.6652(15) 0.4269(5) 0.0107(12) Uani 1 1 d . . .
O6 O 0.2500 -0.6541(19) 0.7500 0.0050(14) Uiso 1 2 d S . .
O7 O 0.5000 -0.304(2) 0.7374(7) 0.0082(16) Uani 1 2 d S . .
O8 O 0.2665(4) -0.6889(14) 0.5656(5) 0.0081(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
Tm1 0.0067(2) 0.0061(2) 0.0070(2) 0.0003(3) 0.000 0.000
Tm2 0.00659(18) 0.0061(2) 0.00878(19) -0.0002(2) 0.00035(9) 0.0003(2)
B2 0.006(3) 0.009(5) 0.007(3) 0.000(4) 0.001(2) -0.004(4)
B3 0.005(5) 0.016(10) 0.009(5) 0.002(5) 0.000 0.000
B4 0.013(5) 0.011(11) 0.010(5) 0.004(5) 0.000 0.000
O1 0.014(4) 0.006(4) 0.010(4) 0.003(3) 0.000 0.000
O2 0.014(4) 0.004(4) 0.010(3) 0.006(3) 0.000 0.000
O3 0.006(2) 0.008(3) 0.013(3) -0.001(2) -0.002(2) 0.003(2)
O4 0.011(3) 0.007(3) 0.008(2) -0.001(2) -0.001(2) -0.003(2)
O5 0.007(2) 0.013(3) 0.012(3) 0.003(3) 0.001(2) -0.003(2)
O7 0.016(4) 0.006(4) 0.003(3) 0.002(3) 0.000 0.000
O8 0.007(2) 0.006(3) 0.011(2) -0.002(3) -0.001(2) -0.002(2)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
Tm Tm -0.3139 5.2483 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_audit_author_name
'Emme, H.'
'Huppertz, H.'
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 Tm1 O1 79.7(4) 5_556 . ?
O1 Tm1 O3 147.7(2) 5_556 2_554 ?
O1 Tm1 O3 76.2(2) . 2_554 ?
O1 Tm1 O3 76.2(2) 5_556 4_556 ?
O1 Tm1 O3 147.7(2) . 4_556 ?
O3 Tm1 O3 133.4(3) 2_554 4_556 ?
O1 Tm1 O8 135.7(3) 5_556 1_565 ?
O1 Tm1 O8 113.1(3) . 1_565 ?
O3 Tm1 O8 74.5(2) 2_554 1_565 ?
O3 Tm1 O8 72.3(2) 4_556 1_565 ?
O1 Tm1 O8 113.1(3) 5_556 3_546 ?
O1 Tm1 O8 135.7(3) . 3_546 ?
O3 Tm1 O8 72.3(2) 2_554 3_546 ?
O3 Tm1 O8 74.5(2) 4_556 3_546 ?
O8 Tm1 O8 87.7(3) 1_565 3_546 ?
O1 Tm1 O4 80.2(3) 5_556 2_544 ?
O1 Tm1 O4 82.7(3) . 2_544 ?
O3 Tm1 O4 75.7(2) 2_554 2_544 ?
O3 Tm1 O4 113.6(2) 4_556 2_544 ?
O8 Tm1 O4 141.3(2) 1_565 2_544 ?
O8 Tm1 O4 59.9(2) 3_546 2_544 ?
O1 Tm1 O4 82.7(3) 5_556 4_566 ?
O1 Tm1 O4 80.2(3) . 4_566 ?
O3 Tm1 O4 113.6(2) 2_554 4_566 ?
O3 Tm1 O4 75.7(2) 4_556 4_566 ?
O8 Tm1 O4 59.9(2) 1_565 4_566 ?
O8 Tm1 O4 141.3(2) 3_546 4_566 ?
O4 Tm1 O4 157.6(3) 2_544 4_566 ?
O1 Tm1 B2 109.5(3) 5_556 4_566 ?
O1 Tm1 B2 96.5(3) . 4_566 ?
O3 Tm1 B2 94.4(2) 2_554 4_566 ?
O3 Tm1 B2 72.1(2) 4_556 4_566 ?
O8 Tm1 B2 30.7(2) 1_565 4_566 ?
O8 Tm1 B2 116.1(2) 3_546 4_566 ?
O4 Tm1 B2 170.0(2) 2_544 4_566 ?
O4 Tm1 B2 29.3(2) 4_566 4_566 ?
O1 Tm1 B2 96.5(3) 5_556 2_544 ?
O1 Tm1 B2 109.5(3) . 2_544 ?
O3 Tm1 B2 72.1(2) 2_554 2_544 ?
O3 Tm1 B2 94.4(2) 4_556 2_544 ?
O8 Tm1 B2 116.1(2) 1_565 2_544 ?
O8 Tm1 B2 30.7(2) 3_546 2_544 ?
O4 Tm1 B2 29.3(2) 2_544 2_544 ?
O4 Tm1 B2 170.0(2) 4_566 2_544 ?
B2 Tm1 B2 146.2(3) 4_566 2_544 ?
O1 Tm1 Tm1 39.83(18) 5_556 5_556 ?
O1 Tm1 Tm1 39.83(18) . 5_556 ?
O3 Tm1 Tm1 113.29(15) 2_554 5_556 ?
O3 Tm1 Tm1 113.29(15) 4_556 5_556 ?
O8 Tm1 Tm1 136.17(15) 1_565 5_556 ?
O8 Tm1 Tm1 136.17(15) 3_546 5_556 ?
O4 Tm1 Tm1 78.82(16) 2_544 5_556 ?
O4 Tm1 Tm1 78.82(16) 4_566 5_556 ?
B2 Tm1 Tm1 106.91(17) 4_566 5_556 ?
B2 Tm1 Tm1 106.91(17) 2_544 5_556 ?
O1 Tm1 Tm2 110.15(19) 5_556 . ?
O1 Tm1 Tm2 148.2(2) . . ?
O3 Tm1 Tm2 101.63(15) 2_554 . ?
O3 Tm1 Tm2 35.23(15) 4_556 . ?
O8 Tm1 Tm2 38.99(15) 1_565 . ?
O8 Tm1 Tm2 69.83(15) 3_546 . ?
O4 Tm1 Tm2 128.14(16) 2_544 . ?
O4 Tm1 Tm2 71.59(15) 4_566 . ?
B2 Tm1 Tm2 51.77(19) 4_566 . ?
B2 Tm1 Tm2 99.58(17) 2_544 . ?
Tm1 Tm1 Tm2 141.059(10) 5_556 . ?
O2 Tm2 O5 87.9(3) 6_657 3_546 ?
O2 Tm2 O6 104.9(3) 6_657 1_565 ?
O5 Tm2 O6 147.69(16) 3_546 1_565 ?
O2 Tm2 O7 77.6(3) 6_657 . ?
O5 Tm2 O7 64.4(3) 3_546 . ?
O6 Tm2 O7 146.7(2) 1_565 . ?
O2 Tm2 O3 148.1(3) 6_657 4_556 ?
O5 Tm2 O3 75.3(2) 3_546 4_556 ?
O6 Tm2 O3 78.7(2) 1_565 4_556 ?
O7 Tm2 O3 116.9(3) . 4_556 ?
O2 Tm2 O3 141.2(3) 6_657 . ?
O5 Tm2 O3 110.1(2) 3_546 . ?
O6 Tm2 O3 78.4(2) 1_565 . ?
O7 Tm2 O3 79.8(2) . . ?
O3 Tm2 O3 70.7(3) 4_556 . ?
O2 Tm2 O8 84.7(2) 6_657 1_565 ?
O5 Tm2 O8 94.8(2) 3_546 1_565 ?
O6 Tm2 O8 58.04(15) 1_565 1_565 ?
O7 Tm2 O8 152.9(2) . 1_565 ?
O3 Tm2 O8 70.2(2) 4_556 1_565 ?
O3 Tm2 O8 125.6(2) . 1_565 ?
O2 Tm2 O4 77.3(3) 6_657 1_565 ?
O5 Tm2 O4 154.4(2) 3_546 1_565 ?
O6 Tm2 O4 57.59(16) 1_565 1_565 ?
O7 Tm2 O4 91.8(3) . 1_565 ?
O3 Tm2 O4 126.9(2) 4_556 1_565 ?
O3 Tm2 O4 72.2(2) . 1_565 ?
O8 Tm2 O4 104.3(2) 1_565 1_565 ?
O2 Tm2 B4 78.4(3) 6_657 6_647 ?
O5 Tm2 B4 31.4(3) 3_546 6_647 ?
O6 Tm2 B4 176.7(3) 1_565 6_647 ?
O7 Tm2 B4 33.3(3) . 6_647 ?
O3 Tm2 B4 98.6(3) 4_556 6_647 ?
O3 Tm2 B4 99.0(3) . 6_647 ?
O8 Tm2 B4 122.9(3) 1_565 6_647 ?
O4 Tm2 B4 123.7(3) 1_565 6_647 ?
O2 Tm2 Tm2 149.0(2) 6_657 4_556 ?
O5 Tm2 Tm2 119.88(17) 3_546 4_556 ?
O6 Tm2 Tm2 44.21(16) 1_565 4_556 ?
O7 Tm2 Tm2 124.99(17) . 4_556 ?
O3 Tm2 Tm2 46.24(15) 4_556 4_556 ?
O3 Tm2 Tm2 45.85(15) . 4_556 ?
O8 Tm2 Tm2 79.78(14) 1_565 4_556 ?
O4 Tm2 Tm2 80.72(15) 1_565 4_556 ?
B4 Tm2 Tm2 132.5(3) 6_647 4_556 ?
O2 Tm2 Tm2 37.0(2) 6_657 7_655 ?
O5 Tm2 Tm2 77.01(16) 3_546 7_655 ?
O6 Tm2 Tm2 130.16(13) 1_565 7_655 ?
O7 Tm2 Tm2 40.98(17) . 7_655 ?
O3 Tm2 Tm2 151.13(16) 4_556 7_655 ?
O3 Tm2 Tm2 112.02(14) . 7_655 ?
O8 Tm2 Tm2 120.52(14) 1_565 7_655 ?
O4 Tm2 Tm2 78.70(15) 1_565 7_655 ?
B4 Tm2 Tm2 52.7(2) 6_647 7_655 ?
Tm2 Tm2 Tm2 154.120(12) 4_556 7_655 ?
O2 Tm2 Tm1 115.0(2) 6_657 . ?
O5 Tm2 Tm1 75.44(15) 3_546 . ?
O6 Tm2 Tm1 72.26(5) 1_565 . ?
O7 Tm2 Tm1 137.7(2) . . ?
O3 Tm2 Tm1 34.93(15) 4_556 . ?
O3 Tm2 Tm1 103.03(14) . . ?
O8 Tm2 Tm1 37.15(14) 1_565 . ?
O4 Tm2 Tm1 129.70(15) 1_565 . ?
B4 Tm2 Tm1 106.5(2) 6_647 . ?
Tm2 Tm2 Tm1 64.821(18) 4_556 . ?
Tm2 Tm2 Tm1 141.059(10) 7_655 . ?
O5 B1 O5 109.3(8) 3_546 . ?
O5 B1 O8 113.0(3) 3_546 3_546 ?
O5 B1 O8 108.2(3) . 3_546 ?
O5 B1 O8 108.2(3) 3_546 . ?
O5 B1 O8 113.0(3) . . ?
O8 B1 O8 105.2(8) 3_546 . ?
O3 B2 O4 116.3(8) . . ?
O3 B2 O6 112.6(8) . . ?
O4 B2 O6 104.5(7) . . ?
O3 B2 O8 118.2(7) . 4_556 ?
O4 B2 O8 104.7(8) . 4_556 ?
O6 B2 O8 98.2(7) . 4_556 ?
O3 B2 Tm1 137.2(5) . 2_545 ?
O4 B2 Tm1 53.5(4) . 2_545 ?
O6 B2 Tm1 110.0(7) . 2_545 ?
O8 B2 Tm1 51.2(4) 4_556 2_545 ?
O1 B3 O4 113.6(6) . 2_554 ?
O1 B3 O4 113.6(6) . 8 ?
O4 B3 O4 106.6(11) 2_554 8 ?
O1 B3 O7 106.8(12) . 2_554 ?
O4 B3 O7 108.0(6) 2_554 2_554 ?
O4 B3 O7 108.0(6) 8 2_554 ?
O2 B4 O5 115.0(7) . 2 ?
O2 B4 O5 115.0(7) . 8_556 ?
O5 B4 O5 110.5(11) 2 8_556 ?
O2 B4 O7 110.2(11) . 6_567 ?
O5 B4 O7 102.3(7) 2 6_567 ?
O5 B4 O7 102.3(7) 8_556 6_567 ?
O2 B4 Tm2 134.3(5) . 4_566 ?
O5 B4 Tm2 49.5(5) 2 4_566 ?
O5 B4 Tm2 110.3(9) 8_556 4_566 ?
O7 B4 Tm2 53.3(4) 6_567 4_566 ?
O2 B4 Tm2 134.3(5) . 6_567 ?
O5 B4 Tm2 110.3(9) 2 6_567 ?
O5 B4 Tm2 49.5(5) 8_556 6_567 ?
O7 B4 Tm2 53.3(4) 6_567 6_567 ?
Tm2 B4 Tm2 74.7(4) 4_566 6_567 ?
B3 O1 Tm1 129.63(19) . 5_556 ?
B3 O1 Tm1 129.63(19) . . ?
Tm1 O1 Tm1 100.3(4) 5_556 . ?
B4 O2 Tm2 123.0(3) . 6_557 ?
B4 O2 Tm2 123.0(3) . 4_556 ?
Tm2 O2 Tm2 106.0(4) 6_557 4_556 ?
B2 O3 Tm1 114.8(5) . 2 ?
B2 O3 Tm2 117.1(5) . 4_556 ?
Tm1 O3 Tm2 109.8(3) 2 4_556 ?
B2 O3 Tm2 114.6(5) . . ?
Tm1 O3 Tm2 109.5(3) 2 . ?
Tm2 O3 Tm2 87.9(2) 4_556 . ?
B2 O4 B3 118.6(8) . 2 ?
B2 O4 Tm1 97.2(5) . 2_545 ?
B3 O4 Tm1 124.6(6) 2 2_545 ?
B2 O4 Tm2 92.1(5) . 1_545 ?
B3 O4 Tm2 119.1(6) 2 1_545 ?
Tm1 O4 Tm2 98.6(2) 2_545 1_545 ?
B1 O5 B4 123.2(8) . 2_554 ?
B1 O5 Tm2 131.3(5) . 3_546 ?
B4 O5 Tm2 99.1(6) 2_554 3_546 ?
B2 O6 B2 133.1(11) 4_556 . ?
B2 O6 Tm2 106.9(4) 4_556 1_545 ?
B2 O6 Tm2 105.4(4) . 1_545 ?
B2 O6 Tm2 105.4(4) 4_556 4_546 ?
B2 O6 Tm2 106.9(4) . 4_546 ?
Tm2 O6 Tm2 91.6(3) 1_545 4_546 ?
B3 O7 B4 125.9(10) 2 6_647 ?
B3 O7 Tm2 119.7(4) 2 7_655 ?
B4 O7 Tm2 93.3(5) 6_647 7_655 ?
B3 O7 Tm2 119.7(4) 2 . ?
B4 O7 Tm2 93.3(5) 6_647 . ?
Tm2 O7 Tm2 98.0(3) 7_655 . ?
B1 O8 B2 114.7(6) . 4_556 ?
B1 O8 Tm1 126.8(4) . 1_545 ?
B2 O8 Tm1 98.1(5) 4_556 1_545 ?
B1 O8 Tm2 111.9(4) . 1_545 ?
B2 O8 Tm2 96.6(5) 4_556 1_545 ?
Tm1 O8 Tm2 103.9(2) 1_545 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
Tm1 O1 2.212(6) 5_556 ?
Tm1 O1 2.212(6) . ?
Tm1 O3 2.330(6) 2_554 ?
Tm1 O3 2.330(6) 4_556 ?
Tm1 O8 2.381(6) 1_565 ?
Tm1 O8 2.381(6) 3_546 ?
Tm1 O4 2.450(6) 2_544 ?
Tm1 O4 2.450(6) 4_566 ?
Tm1 B2 3.023(11) 4_566 ?
Tm1 B2 3.023(11) 2_544 ?
Tm1 Tm1 3.3975(10) 5_556 ?
Tm1 Tm2 3.8276(7) . ?
Tm2 O2 2.171(6) 6_657 ?
Tm2 O5 2.203(7) 3_546 ?
Tm2 O6 2.281(6) 1_565 ?
Tm2 O7 2.297(6) . ?
Tm2 O3 2.347(6) 4_556 ?
Tm2 O3 2.363(6) . ?
Tm2 O8 2.480(6) 1_565 ?
Tm2 O4 2.605(6) 1_565 ?
Tm2 B4 2.860(13) 6_647 ?
Tm2 Tm2 3.2697(8) 4_556 ?
Tm2 Tm2 3.4680(9) 7_655 ?
B1 O5 1.456(9) 3_546 ?
B1 O5 1.456(9) . ?
B1 O8 1.502(9) 3_546 ?
B1 O8 1.502(9) . ?
B2 O3 1.403(14) . ?
B2 O4 1.491(12) . ?
B2 O6 1.507(10) . ?
B2 O8 1.557(11) 4_556 ?
B2 Tm1 3.023(11) 2_545 ?
B3 O1 1.419(17) . ?
B3 O4 1.526(12) 2_554 ?
B3 O4 1.526(12) 8 ?
B3 O7 1.573(16) 2_554 ?
B4 O2 1.392(18) . ?
B4 O5 1.507(11) 2 ?
B4 O5 1.507(11) 8_556 ?
B4 O7 1.575(16) 6_567 ?
B4 Tm2 2.860(13) 4_566 ?
B4 Tm2 2.860(13) 6_567 ?
O1 Tm1 2.212(6) 5_556 ?
O2 Tm2 2.171(6) 6_557 ?
O2 Tm2 2.171(6) 4_556 ?
O3 Tm1 2.330(6) 2 ?
O3 Tm2 2.347(6) 4_556 ?
O4 B3 1.526(12) 2 ?
O4 Tm1 2.450(6) 2_545 ?
O4 Tm2 2.605(6) 1_545 ?
O5 B4 1.507(11) 2_554 ?
O5 Tm2 2.203(7) 3_546 ?
O6 B2 1.507(10) 4_556 ?
O6 Tm2 2.281(6) 1_545 ?
O6 Tm2 2.281(6) 4_546 ?
O7 B3 1.573(16) 2 ?
O7 B4 1.575(16) 6_647 ?
O7 Tm2 2.297(6) 7_655 ?
O8 B2 1.557(11) 4_556 ?
O8 Tm1 2.381(6) 1_545 ?
O8 Tm2 2.480(6) 1_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
O1 Tm1 Tm2 O2 -177.7(3) 5_556 . . 6_657 ?
O1 Tm1 Tm2 O2 -74.5(4) . . . 6_657 ?
O3 Tm1 Tm2 O2 8.1(3) 2_554 . . 6_657 ?
O3 Tm1 Tm2 O2 165.7(4) 4_556 . . 6_657 ?
O8 Tm1 Tm2 O2 -38.5(3) 1_565 . . 6_657 ?
O8 Tm1 Tm2 O2 74.2(3) 3_546 . . 6_657 ?
O4 Tm1 Tm2 O2 88.9(3) 2_544 . . 6_657 ?
O4 Tm1 Tm2 O2 -103.2(3) 4_566 . . 6_657 ?
B2 Tm1 Tm2 O2 -78.4(3) 4_566 . . 6_657 ?
B2 Tm1 Tm2 O2 81.6(3) 2_544 . . 6_657 ?
Tm1 Tm1 Tm2 O2 -145.7(2) 5_556 . . 6_657 ?
O1 Tm1 Tm2 O5 101.6(3) 5_556 . . 3_546 ?
O1 Tm1 Tm2 O5 -155.1(4) . . . 3_546 ?
O3 Tm1 Tm2 O5 -72.5(2) 2_554 . . 3_546 ?
O3 Tm1 Tm2 O5 85.1(3) 4_556 . . 3_546 ?
O8 Tm1 Tm2 O5 -119.1(3) 1_565 . . 3_546 ?
O8 Tm1 Tm2 O5 -6.5(2) 3_546 . . 3_546 ?
O4 Tm1 Tm2 O5 8.3(3) 2_544 . . 3_546 ?
O4 Tm1 Tm2 O5 176.2(2) 4_566 . . 3_546 ?
B2 Tm1 Tm2 O5 -159.0(3) 4_566 . . 3_546 ?
B2 Tm1 Tm2 O5 1.0(3) 2_544 . . 3_546 ?
Tm1 Tm1 Tm2 O5 133.72(18) 5_556 . . 3_546 ?
O1 Tm1 Tm2 O6 -79.1(3) 5_556 . . 1_565 ?
O1 Tm1 Tm2 O6 24.1(4) . . . 1_565 ?
O3 Tm1 Tm2 O6 106.7(2) 2_554 . . 1_565 ?
O3 Tm1 Tm2 O6 -95.6(3) 4_556 . . 1_565 ?
O8 Tm1 Tm2 O6 60.1(3) 1_565 . . 1_565 ?
O8 Tm1 Tm2 O6 172.8(2) 3_546 . . 1_565 ?
O4 Tm1 Tm2 O6 -172.4(2) 2_544 . . 1_565 ?
O4 Tm1 Tm2 O6 -4.5(2) 4_566 . . 1_565 ?
B2 Tm1 Tm2 O6 20.3(3) 4_566 . . 1_565 ?
B2 Tm1 Tm2 O6 -179.7(3) 2_544 . . 1_565 ?
Tm1 Tm1 Tm2 O6 -47.05(16) 5_556 . . 1_565 ?
O1 Tm1 Tm2 O7 83.1(4) 5_556 . . . ?
O1 Tm1 Tm2 O7 -173.7(4) . . . . ?
O3 Tm1 Tm2 O7 -91.1(3) 2_554 . . . ?
O3 Tm1 Tm2 O7 66.6(4) 4_556 . . . ?
O8 Tm1 Tm2 O7 -137.7(3) 1_565 . . . ?
O8 Tm1 Tm2 O7 -25.0(3) 3_546 . . . ?
O4 Tm1 Tm2 O7 -10.2(3) 2_544 . . . ?
O4 Tm1 Tm2 O7 157.7(3) 4_566 . . . ?
B2 Tm1 Tm2 O7 -177.5(3) 4_566 . . . ?
B2 Tm1 Tm2 O7 -17.5(3) 2_544 . . . ?
Tm1 Tm1 Tm2 O7 115.2(3) 5_556 . . . ?
O1 Tm1 Tm2 O3 16.5(4) 5_556 . . 4_556 ?
O1 Tm1 Tm2 O3 119.8(4) . . . 4_556 ?
O3 Tm1 Tm2 O3 -157.6(2) 2_554 . . 4_556 ?
O8 Tm1 Tm2 O3 155.8(4) 1_565 . . 4_556 ?
O8 Tm1 Tm2 O3 -91.6(3) 3_546 . . 4_556 ?
O4 Tm1 Tm2 O3 -76.8(3) 2_544 . . 4_556 ?
O4 Tm1 Tm2 O3 91.1(3) 4_566 . . 4_556 ?
B2 Tm1 Tm2 O3 115.9(3) 4_566 . . 4_556 ?
B2 Tm1 Tm2 O3 -84.1(3) 2_544 . . 4_556 ?
Tm1 Tm1 Tm2 O3 48.6(3) 5_556 . . 4_556 ?
O1 Tm1 Tm2 O3 -6.1(3) 5_556 . . . ?
O1 Tm1 Tm2 O3 97.2(4) . . . . ?
O3 Tm1 Tm2 O3 179.80(10) 2_554 . . . ?
O3 Tm1 Tm2 O3 -22.6(3) 4_556 . . . ?
O8 Tm1 Tm2 O3 133.2(3) 1_565 . . . ?
O8 Tm1 Tm2 O3 -114.2(2) 3_546 . . . ?
O4 Tm1 Tm2 O3 -99.4(3) 2_544 . . . ?
O4 Tm1 Tm2 O3 68.5(2) 4_566 . . . ?
B2 Tm1 Tm2 O3 93.3(3) 4_566 . . . ?
B2 Tm1 Tm2 O3 -106.7(3) 2_544 . . . ?
Tm1 Tm1 Tm2 O3 26.01(17) 5_556 . . . ?
O1 Tm1 Tm2 O8 -139.3(3) 5_556 . . 1_565 ?
O1 Tm1 Tm2 O8 -36.0(4) . . . 1_565 ?
O3 Tm1 Tm2 O8 46.6(3) 2_554 . . 1_565 ?
O3 Tm1 Tm2 O8 -155.8(4) 4_556 . . 1_565 ?
O8 Tm1 Tm2 O8 112.6(3) 3_546 . . 1_565 ?
O4 Tm1 Tm2 O8 127.4(3) 2_544 . . 1_565 ?
O4 Tm1 Tm2 O8 -64.7(3) 4_566 . . 1_565 ?
B2 Tm1 Tm2 O8 -39.9(3) 4_566 . . 1_565 ?
B2 Tm1 Tm2 O8 120.1(3) 2_544 . . 1_565 ?
Tm1 Tm1 Tm2 O8 -107.2(2) 5_556 . . 1_565 ?
O1 Tm1 Tm2 O4 -83.6(3) 5_556 . . 1_565 ?
O1 Tm1 Tm2 O4 19.7(4) . . . 1_565 ?
O3 Tm1 Tm2 O4 102.3(3) 2_554 . . 1_565 ?
O3 Tm1 Tm2 O4 -100.1(3) 4_556 . . 1_565 ?
O8 Tm1 Tm2 O4 55.6(3) 1_565 . . 1_565 ?
O8 Tm1 Tm2 O4 168.3(3) 3_546 . . 1_565 ?
O4 Tm1 Tm2 O4 -176.9(2) 2_544 . . 1_565 ?
O4 Tm1 Tm2 O4 -9.0(2) 4_566 . . 1_565 ?
B2 Tm1 Tm2 O4 15.8(3) 4_566 . . 1_565 ?
B2 Tm1 Tm2 O4 175.8(3) 2_544 . . 1_565 ?
Tm1 Tm1 Tm2 O4 -51.53(19) 5_556 . . 1_565 ?
O1 Tm1 Tm2 B4 97.6(4) 5_556 . . 6_647 ?
O1 Tm1 Tm2 B4 -159.1(5) . . . 6_647 ?
O3 Tm1 Tm2 B4 -76.5(4) 2_554 . . 6_647 ?
O3 Tm1 Tm2 B4 81.1(4) 4_556 . . 6_647 ?
O8 Tm1 Tm2 B4 -123.1(4) 1_565 . . 6_647 ?
O8 Tm1 Tm2 B4 -10.5(4) 3_546 . . 6_647 ?
O4 Tm1 Tm2 B4 4.3(4) 2_544 . . 6_647 ?
O4 Tm1 Tm2 B4 172.2(3) 4_566 . . 6_647 ?
B2 Tm1 Tm2 B4 -163.0(4) 4_566 . . 6_647 ?
B2 Tm1 Tm2 B4 -3.0(4) 2_544 . . 6_647 ?
Tm1 Tm1 Tm2 B4 129.7(3) 5_556 . . 6_647 ?
O1 Tm1 Tm2 Tm2 -32.1(2) 5_556 . . 4_556 ?
O1 Tm1 Tm2 Tm2 71.2(3) . . . 4_556 ?
O3 Tm1 Tm2 Tm2 153.80(17) 2_554 . . 4_556 ?
O3 Tm1 Tm2 Tm2 -48.6(3) 4_556 . . 4_556 ?
O8 Tm1 Tm2 Tm2 107.2(2) 1_565 . . 4_556 ?
O8 Tm1 Tm2 Tm2 -140.16(16) 3_546 . . 4_556 ?
O4 Tm1 Tm2 Tm2 -125.38(19) 2_544 . . 4_556 ?
O4 Tm1 Tm2 Tm2 42.53(17) 4_566 . . 4_556 ?
B2 Tm1 Tm2 Tm2 67.3(2) 4_566 . . 4_556 ?
B2 Tm1 Tm2 Tm2 -132.7(2) 2_544 . . 4_556 ?
Tm1 Tm1 Tm2 Tm2 0.017(8) 5_556 . . 4_556 ?
O1 Tm1 Tm2 Tm2 147.9(2) 5_556 . . 7_655 ?
O1 Tm1 Tm2 Tm2 -108.8(3) . . . 7_655 ?
O3 Tm1 Tm2 Tm2 -26.22(17) 2_554 . . 7_655 ?
O3 Tm1 Tm2 Tm2 131.4(3) 4_556 . . 7_655 ?
O8 Tm1 Tm2 Tm2 -72.8(2) 1_565 . . 7_655 ?
O8 Tm1 Tm2 Tm2 39.82(16) 3_546 . . 7_655 ?
O4 Tm1 Tm2 Tm2 54.60(19) 2_544 . . 7_655 ?
O4 Tm1 Tm2 Tm2 -137.49(17) 4_566 . . 7_655 ?
B2 Tm1 Tm2 Tm2 -112.7(2) 4_566 . . 7_655 ?
B2 Tm1 Tm2 Tm2 47.3(2) 2_544 . . 7_655 ?
Tm1 Tm1 Tm2 Tm2 180.0 5_556 . . 7_655 ?
O4 B3 O1 Tm1 155.4(6) 2_554 . . 5_556 ?
O4 B3 O1 Tm1 33.3(15) 8 . . 5_556 ?
O7 B3 O1 Tm1 -85.6(8) 2_554 . . 5_556 ?
O4 B3 O1 Tm1 -33.3(15) 2_554 . . . ?
O4 B3 O1 Tm1 -155.4(6) 8 . . . ?
O7 B3 O1 Tm1 85.6(8) 2_554 . . . ?
O1 Tm1 O1 B3 -173.2(12) 5_556 . . . ?
O3 Tm1 O1 B3 -14.9(10) 2_554 . . . ?
O3 Tm1 O1 B3 144.6(9) 4_556 . . . ?
O8 Tm1 O1 B3 51.3(11) 1_565 . . . ?
O8 Tm1 O1 B3 -60.6(11) 3_546 . . . ?
O4 Tm1 O1 B3 -91.9(10) 2_544 . . . ?
O4 Tm1 O1 B3 102.6(10) 4_566 . . . ?
B2 Tm1 O1 B3 78.1(10) 4_566 . . . ?
B2 Tm1 O1 B3 -79.9(10) 2_544 . . . ?
Tm1 Tm1 O1 B3 -173.2(12) 5_556 . . . ?
Tm2 Tm1 O1 B3 75.1(11) . . . . ?
O1 Tm1 O1 Tm1 0.0 5_556 . . 5_556 ?
O3 Tm1 O1 Tm1 158.3(4) 2_554 . . 5_556 ?
O3 Tm1 O1 Tm1 -42.2(7) 4_556 . . 5_556 ?
O8 Tm1 O1 Tm1 -135.5(3) 1_565 . . 5_556 ?
O8 Tm1 O1 Tm1 112.6(3) 3_546 . . 5_556 ?
O4 Tm1 O1 Tm1 81.3(3) 2_544 . . 5_556 ?
O4 Tm1 O1 Tm1 -84.2(3) 4_566 . . 5_556 ?
B2 Tm1 O1 Tm1 -108.7(3) 4_566 . . 5_556 ?
B2 Tm1 O1 Tm1 93.3(4) 2_544 . . 5_556 ?
Tm2 Tm1 O1 Tm1 -111.8(3) . . . 5_556 ?
O5 B4 O2 Tm2 172.9(6) 2 . . 6_557 ?
O5 B4 O2 Tm2 42.7(13) 8_556 . . 6_557 ?
O7 B4 O2 Tm2 -72.2(6) 6_567 . . 6_557 ?
Tm2 B4 O2 Tm2 -130.2(5) 4_566 . . 6_557 ?
Tm2 B4 O2 Tm2 -14.2(14) 6_567 . . 6_557 ?
O5 B4 O2 Tm2 -42.7(13) 2 . . 4_556 ?
O5 B4 O2 Tm2 -172.9(6) 8_556 . . 4_556 ?
O7 B4 O2 Tm2 72.2(6) 6_567 . . 4_556 ?
Tm2 B4 O2 Tm2 14.2(14) 4_566 . . 4_556 ?
Tm2 B4 O2 Tm2 130.2(5) 6_567 . . 4_556 ?
O4 B2 O3 Tm1 -60.4(7) . . . 2 ?
O6 B2 O3 Tm1 179.1(4) . . . 2 ?
O8 B2 O3 Tm1 65.6(8) 4_556 . . 2 ?
Tm1 B2 O3 Tm1 3.4(10) 2_545 . . 2 ?
O4 B2 O3 Tm2 168.6(4) . . . 4_556 ?
O6 B2 O3 Tm2 48.1(7) . . . 4_556 ?
O8 B2 O3 Tm2 -65.5(8) 4_556 . . 4_556 ?
Tm1 B2 O3 Tm2 -127.6(6) 2_545 . . 4_556 ?
O4 B2 O3 Tm2 67.7(7) . . . . ?
O6 B2 O3 Tm2 -52.8(7) . . . . ?
O8 B2 O3 Tm2 -166.4(5) 4_556 . . . ?
Tm1 B2 O3 Tm2 131.4(6) 2_545 . . . ?
O2 Tm2 O3 B2 -106.6(6) 6_657 . . . ?
O5 Tm2 O3 B2 6.4(6) 3_546 . . . ?
O6 Tm2 O3 B2 153.9(5) 1_565 . . . ?
O7 Tm2 O3 B2 -51.4(6) . . . . ?
O3 Tm2 O3 B2 72.0(5) 4_556 . . . ?
O8 Tm2 O3 B2 118.2(5) 1_565 . . . ?
O4 Tm2 O3 B2 -146.7(6) 1_565 . . . ?
B4 Tm2 O3 B2 -24.0(6) 6_647 . . . ?
Tm2 Tm2 O3 B2 119.0(6) 4_556 . . . ?
Tm2 Tm2 O3 B2 -77.3(5) 7_655 . . . ?
Tm1 Tm2 O3 B2 85.5(5) . . . . ?
O2 Tm2 O3 Tm1 24.0(5) 6_657 . . 2 ?
O5 Tm2 O3 Tm1 137.1(2) 3_546 . . 2 ?
O6 Tm2 O3 Tm1 -75.4(2) 1_565 . . 2 ?
O7 Tm2 O3 Tm1 79.3(3) . . . 2 ?
O3 Tm2 O3 Tm1 -157.4(3) 4_556 . . 2 ?
O8 Tm2 O3 Tm1 -111.1(3) 1_565 . . 2 ?
O4 Tm2 O3 Tm1 -16.0(2) 1_565 . . 2 ?
B4 Tm2 O3 Tm1 106.7(3) 6_647 . . 2 ?
Tm2 Tm2 O3 Tm1 -110.3(3) 4_556 . . 2 ?
Tm2 Tm2 O3 Tm1 53.4(3) 7_655 . . 2 ?
Tm1 Tm2 O3 Tm1 -143.89(19) . . . 2 ?
O2 Tm2 O3 Tm2 134.4(4) 6_657 . . 4_556 ?
O5 Tm2 O3 Tm2 -112.6(2) 3_546 . . 4_556 ?
O6 Tm2 O3 Tm2 34.91(16) 1_565 . . 4_556 ?
O7 Tm2 O3 Tm2 -170.4(3) . . . 4_556 ?
O3 Tm2 O3 Tm2 -47.0(3) 4_556 . . 4_556 ?
O8 Tm2 O3 Tm2 -0.8(3) 1_565 . . 4_556 ?
O4 Tm2 O3 Tm2 94.3(2) 1_565 . . 4_556 ?
B4 Tm2 O3 Tm2 -143.0(2) 6_647 . . 4_556 ?
Tm2 Tm2 O3 Tm2 163.74(9) 7_655 . . 4_556 ?
Tm1 Tm2 O3 Tm2 -33.56(19) . . . 4_556 ?
O3 B2 O4 B3 -5.3(10) . . . 2 ?
O6 B2 O4 B3 119.5(8) . . . 2 ?
O8 B2 O4 B3 -137.7(8) 4_556 . . 2 ?
Tm1 B2 O4 B3 -136.0(8) 2_545 . . 2 ?
O3 B2 O4 Tm1 130.8(6) . . . 2_545 ?
O6 B2 O4 Tm1 -104.4(6) . . . 2_545 ?
O8 B2 O4 Tm1 -1.7(7) 4_556 . . 2_545 ?
O3 B2 O4 Tm2 -130.3(6) . . . 1_545 ?
O6 B2 O4 Tm2 -5.5(7) . . . 1_545 ?
O8 B2 O4 Tm2 97.2(6) 4_556 . . 1_545 ?
Tm1 B2 O4 Tm2 98.9(3) 2_545 . . 1_545 ?
O5 B1 O5 B4 -42.3(7) 3_546 . . 2_554 ?
O8 B1 O5 B4 81.1(9) 3_546 . . 2_554 ?
O8 B1 O5 B4 -162.8(8) . . . 2_554 ?
O5 B1 O5 Tm2 172.1(6) 3_546 . . 3_546 ?
O8 B1 O5 Tm2 -64.5(6) 3_546 . . 3_546 ?
O8 B1 O5 Tm2 51.6(7) . . . 3_546 ?
O3 B2 O6 B2 1.6(5) . . . 4_556 ?
O4 B2 O6 B2 -125.5(7) . . . 4_556 ?
O8 B2 O6 B2 126.9(6) 4_556 . . 4_556 ?
Tm1 B2 O6 B2 178.5(4) 2_545 . . 4_556 ?
O3 B2 O6 Tm2 133.6(6) . . . 1_545 ?
O4 B2 O6 Tm2 6.5(8) . . . 1_545 ?
O8 B2 O6 Tm2 -101.1(5) 4_556 . . 1_545 ?
Tm1 B2 O6 Tm2 -49.5(4) 2_545 . . 1_545 ?
O3 B2 O6 Tm2 -129.9(6) . . . 4_546 ?
O4 B2 O6 Tm2 103.0(6) . . . 4_546 ?
O8 B2 O6 Tm2 -4.6(7) 4_556 . . 4_546 ?
Tm1 B2 O6 Tm2 47.0(4) 2_545 . . 4_546 ?
O2 Tm2 O7 B3 137.2(8) 6_657 . . 2 ?
O5 Tm2 O7 B3 -129.2(8) 3_546 . . 2 ?
O6 Tm2 O7 B3 38.8(9) 1_565 . . 2 ?
O3 Tm2 O7 B3 -73.1(8) 4_556 . . 2 ?
O3 Tm2 O7 B3 -10.9(8) . . . 2 ?
O8 Tm2 O7 B3 -172.2(7) 1_565 . . 2 ?
O4 Tm2 O7 B3 60.6(8) 1_565 . . 2 ?
B4 Tm2 O7 B3 -135.2(10) 6_647 . . 2 ?
Tm2 Tm2 O7 B3 -19.3(9) 4_556 . . 2 ?
Tm2 Tm2 O7 B3 131.0(9) 7_655 . . 2 ?
Tm1 Tm2 O7 B3 -109.2(8) . . . 2 ?
O2 Tm2 O7 B4 -87.6(6) 6_657 . . 6_647 ?
O5 Tm2 O7 B4 6.0(5) 3_546 . . 6_647 ?
O6 Tm2 O7 B4 173.9(6) 1_565 . . 6_647 ?
O3 Tm2 O7 B4 62.1(6) 4_556 . . 6_647 ?
O3 Tm2 O7 B4 124.2(6) . . . 6_647 ?
O8 Tm2 O7 B4 -37.1(8) 1_565 . . 6_647 ?
O4 Tm2 O7 B4 -164.2(5) 1_565 . . 6_647 ?
Tm2 Tm2 O7 B4 115.8(5) 4_556 . . 6_647 ?
Tm2 Tm2 O7 B4 -93.9(6) 7_655 . . 6_647 ?
Tm1 Tm2 O7 B4 26.0(6) . . . 6_647 ?
O2 Tm2 O7 Tm2 6.2(3) 6_657 . . 7_655 ?
O5 Tm2 O7 Tm2 99.8(3) 3_546 . . 7_655 ?
O6 Tm2 O7 Tm2 -92.2(4) 1_565 . . 7_655 ?
O3 Tm2 O7 Tm2 155.9(2) 4_556 . . 7_655 ?
O3 Tm2 O7 Tm2 -141.9(3) . . . 7_655 ?
O8 Tm2 O7 Tm2 56.8(6) 1_565 . . 7_655 ?
O4 Tm2 O7 Tm2 -70.4(3) 1_565 . . 7_655 ?
B4 Tm2 O7 Tm2 93.9(6) 6_647 . . 7_655 ?
Tm2 Tm2 O7 Tm2 -150.33(12) 4_556 . . 7_655 ?
Tm1 Tm2 O7 Tm2 119.8(2) . . . 7_655 ?
O5 B1 O8 B2 54.2(8) 3_546 . . 4_556 ?
O5 B1 O8 B2 175.4(6) . . . 4_556 ?
O8 B1 O8 B2 -66.8(5) 3_546 . . 4_556 ?
O5 B1 O8 Tm1 176.8(4) 3_546 . . 1_545 ?
O5 B1 O8 Tm1 -62.1(8) . . . 1_545 ?
O8 B1 O8 Tm1 55.8(4) 3_546 . . 1_545 ?
O5 B1 O8 Tm2 -54.6(6) 3_546 . . 1_545 ?
O5 B1 O8 Tm2 66.5(6) . . . 1_545 ?
O8 B1 O8 Tm2 -175.6(4) 3_546 . . 1_545 ?
|
1100927.cif | #------------------------------------------------------------------------------
#$Date: 2022-09-14 18:21:52 +0300 (Wed, 14 Sep 2022) $
#$Revision: 277833 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/09/1100927.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_1100927
loop_
_publ_author_name
'Emme, Holger'
'Valldor, Martin'
'P\"ottgen, Rainer'
'Huppertz, Hubert'
_publ_section_title
;
Associating Borate and Silicate Chemistry by Extreme Conditions:
High-Pressure Synthesis, Crystal Structure, and Properties of
the New Borates RE~3~B~5~O~12~ (RE = Er--Lu)
;
_journal_coden_ASTM CMATEX
_journal_issue 10
_journal_name_full 'Chemistry of Materials'
_journal_page_first 2707
_journal_page_last 2715
_journal_paper_doi 10.1021/cm047741+
_journal_volume 17
_journal_year 2005
_chemical_formula_moiety 'B5 O12 Yb3'
_chemical_formula_sum 'B5 O12 Yb3'
_chemical_formula_weight 765.17
_chemical_melting_point ?
_chemical_name_common Triytterbiumpentaborate
_chemical_name_systematic Triytterbiumpentaborate
_space_group_IT_number 53
_space_group_name_Hall '-P 2ac 2'
_space_group_name_H-M_alt 'P m n a'
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall '-P 2ac 2'
_symmetry_space_group_name_H-M 'P m n a'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_contact_author_address
;
'Department Chemie
Ludwig-Maximilians-Universitaet Muenchen
Butenandtstrasse 5-13 (Haus D)
81377 Muenchen
Germany'
;
_audit_contact_author_email hemch@cup.uni-muenchen.de
_audit_contact_author_fax '+49 (0)89 2180 77440'
_audit_contact_author_phone '+49 (0)89 2180 77443'
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 12.774(3)
_cell_length_b 4.5864(9)
_cell_length_c 12.451(3)
_cell_measurement_reflns_used 7337
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 35.5
_cell_measurement_theta_min 2.5
_cell_volume 729.5(3)
_computing_molecular_graphics 'DIAMOND (Brandenburg & Berndt, 1999)'
_computing_publication_material 'enCIFer (Allen et al., 2004) and SHELXL97'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_device_type 'STOE IPDS'
_diffrn_measurement_method 'profile data from \w-scans'
_diffrn_radiation_collimation 0.5
_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 0.0770
_diffrn_reflns_av_sigmaI/netI 0.0371
_diffrn_reflns_limit_h_max 20
_diffrn_reflns_limit_h_min -19
_diffrn_reflns_limit_k_max 7
_diffrn_reflns_limit_k_min -7
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_number 9635
_diffrn_reflns_theta_full 32.15
_diffrn_reflns_theta_max 34.91
_diffrn_reflns_theta_min 3.19
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 38.232
_exptl_absorpt_correction_T_max 0.2861
_exptl_absorpt_correction_T_min 0.1204
_exptl_absorpt_correction_type numerical
_exptl_absorpt_process_details 'Herrendorf,B\"arnighausen,HABITUS, 1993/1997'
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 6.967
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description platelet
_exptl_crystal_F_000 1324
_exptl_crystal_size_max 0.09
_exptl_crystal_size_mid 0.05
_exptl_crystal_size_min 0.035
_refine_diff_density_max 4.621
_refine_diff_density_min -2.715
_refine_diff_density_rms 0.637
_refine_ls_extinction_coef 0.0089(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 1.182
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 90
_refine_ls_number_reflns 1551
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.182
_refine_ls_R_factor_all 0.0670
_refine_ls_R_factor_gt 0.0445
_refine_ls_shift/su_max 0.018
_refine_ls_shift/su_mean 0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0465P)^2^+3.3757P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0982
_refine_ls_wR_factor_ref 0.1084
_reflns_number_gt 1061
_reflns_number_total 1551
_reflns_threshold_expression >2sigma(I)
_cod_duplicate_entry 4000577
_cod_data_source_file cm047741+si20041223_064541.cif
_cod_data_source_block Yb3B5O12
_cod_original_sg_symbol_H-M Pmna
_cod_database_code 1100927
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'
'-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
Yb1 Yb 0.13244(3) 0.0000 0.5000 0.00668(13) Uani 1 2 d S . .
Yb2 Yb 0.36459(2) 0.00046(9) 0.69297(2) 0.00715(13) Uani 1 1 d . . .
B1 B 0.3383(8) -0.5000 0.5000 0.0080(15) Uani 1 2 d S . .
B2 B 0.2986(6) -0.5295(17) 0.8489(6) 0.0056(12) Uiso 1 1 d . . .
B3 B 0.0000 0.456(2) 0.3508(11) 0.0080(19) Uani 1 2 d S . .
B4 B 0.0000 0.542(2) 0.8740(9) 0.0057(17) Uiso 1 2 d S . .
O1 O 0.0000 0.2388(15) 0.4295(8) 0.0075(13) Uani 1 2 d S . .
O2 O 0.0000 0.2395(16) 0.8612(8) 0.0065(13) Uani 1 2 d S . .
O3 O 0.2950(4) -0.2185(11) 0.8486(5) 0.0049(9) Uani 1 1 d . . .
O4 O 0.4049(5) -0.6577(11) 0.8542(5) 0.0063(9) Uani 1 1 d . . .
O5 O 0.4043(4) -0.6643(11) 0.4272(5) 0.0068(9) Uani 1 1 d . . .
O6 O 0.2500 -0.6564(15) 0.7500 0.0049(12) Uani 1 2 d S . .
O7 O 0.5000 -0.3032(15) 0.7368(7) 0.0052(12) Uiso 1 2 d S . .
O8 O 0.2662(4) -0.6896(10) 0.5645(5) 0.0052(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
Yb1 0.0065(2) 0.00540(19) 0.0081(2) 0.00058(18) 0.000 0.000
Yb2 0.00652(17) 0.00540(16) 0.0095(2) -0.00070(13) 0.00024(8) 0.00010(13)
B1 0.009(4) 0.004(3) 0.011(4) 0.000(5) 0.000 0.000
B3 0.012(5) 0.002(4) 0.010(5) -0.001(3) 0.000 0.000
O1 0.006(3) 0.003(3) 0.013(4) 0.003(2) 0.000 0.000
O2 0.004(3) 0.005(3) 0.010(4) -0.001(2) 0.000 0.000
O3 0.004(2) 0.0024(18) 0.008(3) 0.0018(15) 0.0025(16) 0.0009(16)
O4 0.007(2) 0.0016(17) 0.010(3) 0.0019(16) 0.0021(18) -0.0001(17)
O5 0.006(2) 0.0048(17) 0.009(3) 0.0005(17) 0.0040(19) 0.0029(15)
O6 0.006(3) 0.004(2) 0.005(3) 0.000 -0.002(2) 0.000
O8 0.0033(17) 0.0007(17) 0.012(3) 0.0001(17) -0.0043(19) 0.0006(14)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_audit_author_name
'Emme, H.'
'Huppertz, H.'
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 Yb1 O1 79.4(3) 5_556 . ?
O1 Yb1 O3 76.6(2) 5_556 4_556 ?
O1 Yb1 O3 147.6(2) . 4_556 ?
O1 Yb1 O3 147.6(2) 5_556 2_554 ?
O1 Yb1 O3 76.6(2) . 2_554 ?
O3 Yb1 O3 133.1(3) 4_556 2_554 ?
O1 Yb1 O8 136.1(3) 5_556 1_565 ?
O1 Yb1 O8 113.1(2) . 1_565 ?
O3 Yb1 O8 72.31(19) 4_556 1_565 ?
O3 Yb1 O8 74.2(2) 2_554 1_565 ?
O1 Yb1 O8 113.1(2) 5_556 3_546 ?
O1 Yb1 O8 136.1(3) . 3_546 ?
O3 Yb1 O8 74.2(2) 4_556 3_546 ?
O3 Yb1 O8 72.31(19) 2_554 3_546 ?
O8 Yb1 O8 87.5(3) 1_565 3_546 ?
O1 Yb1 O4 82.7(3) 5_556 4_566 ?
O1 Yb1 O4 80.0(3) . 4_566 ?
O3 Yb1 O4 75.70(19) 4_556 4_566 ?
O3 Yb1 O4 113.72(19) 2_554 4_566 ?
O8 Yb1 O4 60.2(2) 1_565 4_566 ?
O8 Yb1 O4 141.2(2) 3_546 4_566 ?
O1 Yb1 O4 80.0(3) 5_556 2_544 ?
O1 Yb1 O4 82.7(3) . 2_544 ?
O3 Yb1 O4 113.72(19) 4_556 2_544 ?
O3 Yb1 O4 75.70(19) 2_554 2_544 ?
O8 Yb1 O4 141.2(2) 1_565 2_544 ?
O8 Yb1 O4 60.2(2) 3_546 2_544 ?
O4 Yb1 O4 157.5(3) 4_566 2_544 ?
O1 Yb1 B2 109.5(3) 5_556 4_566 ?
O1 Yb1 B2 96.8(3) . 4_566 ?
O3 Yb1 B2 71.6(2) 4_556 4_566 ?
O3 Yb1 B2 94.7(2) 2_554 4_566 ?
O8 Yb1 B2 30.7(2) 1_565 4_566 ?
O8 Yb1 B2 115.7(2) 3_546 4_566 ?
O4 Yb1 B2 29.4(2) 4_566 4_566 ?
O4 Yb1 B2 170.2(2) 2_544 4_566 ?
O1 Yb1 B2 96.8(3) 5_556 2_544 ?
O1 Yb1 B2 109.5(3) . 2_544 ?
O3 Yb1 B2 94.7(2) 4_556 2_544 ?
O3 Yb1 B2 71.6(2) 2_554 2_544 ?
O8 Yb1 B2 115.7(2) 1_565 2_544 ?
O8 Yb1 B2 30.7(2) 3_546 2_544 ?
O4 Yb1 B2 170.2(2) 4_566 2_544 ?
O4 Yb1 B2 29.4(2) 2_544 2_544 ?
B2 Yb1 B2 145.8(3) 4_566 2_544 ?
O1 Yb1 B2 66.3(2) 5_556 4_556 ?
O1 Yb1 B2 145.7(2) . 4_556 ?
O3 Yb1 B2 23.96(19) 4_556 4_556 ?
O3 Yb1 B2 133.96(19) 2_554 4_556 ?
O8 Yb1 B2 93.33(19) 1_565 4_556 ?
O8 Yb1 B2 62.8(2) 3_546 4_556 ?
O4 Yb1 B2 96.0(2) 4_566 4_556 ?
O4 Yb1 B2 90.2(2) 2_544 4_556 ?
B2 Yb1 B2 95.5(2) 4_566 4_556 ?
B2 Yb1 B2 75.0(2) 2_544 4_556 ?
O1 Yb1 B2 145.7(2) 5_556 2_554 ?
O1 Yb1 B2 66.3(2) . 2_554 ?
O3 Yb1 B2 133.96(19) 4_556 2_554 ?
O3 Yb1 B2 23.96(19) 2_554 2_554 ?
O8 Yb1 B2 62.8(2) 1_565 2_554 ?
O8 Yb1 B2 93.33(19) 3_546 2_554 ?
O4 Yb1 B2 90.2(2) 4_566 2_554 ?
O4 Yb1 B2 96.0(2) 2_544 2_554 ?
B2 Yb1 B2 75.0(2) 4_566 2_554 ?
B2 Yb1 B2 95.5(2) 2_544 2_554 ?
B2 Yb1 B2 148.0(3) 4_556 2_554 ?
O2 Yb2 O5 87.6(3) 6_657 3_546 ?
O2 Yb2 O6 105.3(2) 6_657 1_565 ?
O5 Yb2 O6 147.86(15) 3_546 1_565 ?
O2 Yb2 O7 77.1(2) 6_657 . ?
O5 Yb2 O7 64.1(3) 3_546 . ?
O6 Yb2 O7 146.9(2) 1_565 . ?
O2 Yb2 O3 148.4(3) 6_657 4_556 ?
O5 Yb2 O3 75.49(19) 3_546 4_556 ?
O6 Yb2 O3 78.67(16) 1_565 4_556 ?
O7 Yb2 O3 116.9(2) . 4_556 ?
O2 Yb2 O3 140.9(3) 6_657 . ?
O5 Yb2 O3 110.3(2) 3_546 . ?
O6 Yb2 O3 78.13(16) 1_565 . ?
O7 Yb2 O3 80.2(2) . . ?
O3 Yb2 O3 70.7(3) 4_556 . ?
O2 Yb2 O8 85.0(2) 6_657 1_565 ?
O5 Yb2 O8 94.6(2) 3_546 1_565 ?
O6 Yb2 O8 58.43(15) 1_565 1_565 ?
O7 Yb2 O8 152.3(2) . 1_565 ?
O3 Yb2 O8 70.16(18) 4_556 1_565 ?
O3 Yb2 O8 125.67(19) . 1_565 ?
O2 Yb2 O4 77.0(3) 6_657 1_565 ?
O5 Yb2 O4 154.09(19) 3_546 1_565 ?
O6 Yb2 O4 57.74(14) 1_565 1_565 ?
O7 Yb2 O4 91.9(2) . 1_565 ?
O3 Yb2 O4 127.22(19) 4_556 1_565 ?
O3 Yb2 O4 72.33(18) . 1_565 ?
O8 Yb2 O4 104.63(18) 1_565 1_565 ?
O2 Yb2 B4 78.2(2) 6_657 6_647 ?
O5 Yb2 B4 31.4(2) 3_546 6_647 ?
O6 Yb2 B4 176.5(2) 1_565 6_647 ?
O7 Yb2 B4 32.9(3) . 6_647 ?
O3 Yb2 B4 98.53(18) 4_556 6_647 ?
O3 Yb2 B4 99.0(3) . 6_647 ?
O8 Yb2 B4 122.8(3) 1_565 6_647 ?
O4 Yb2 B4 123.5(2) 1_565 6_647 ?
O2 Yb2 B2 93.6(3) 6_657 1_565 ?
O5 Yb2 B2 176.4(2) 3_546 1_565 ?
O6 Yb2 B2 28.57(15) 1_565 1_565 ?
O7 Yb2 B2 119.5(3) . 1_565 ?
O3 Yb2 B2 101.9(2) 4_556 1_565 ?
O3 Yb2 B2 70.7(2) . 1_565 ?
O8 Yb2 B2 82.2(2) 1_565 1_565 ?
O4 Yb2 B2 29.4(2) 1_565 1_565 ?
B4 Yb2 B2 152.2(2) 6_647 1_565 ?
O2 Yb2 B2 97.8(2) 6_657 4_566 ?
O5 Yb2 B2 122.4(2) 3_546 4_566 ?
O6 Yb2 B2 28.16(15) 1_565 4_566 ?
O7 Yb2 B2 172.0(2) . 4_566 ?
O3 Yb2 B2 70.6(2) 4_556 4_566 ?
O3 Yb2 B2 100.6(2) . 4_566 ?
O8 Yb2 B2 30.4(2) 1_565 4_566 ?
O4 Yb2 B2 80.82(19) 1_565 4_566 ?
B4 Yb2 B2 152.7(3) 6_647 4_566 ?
B2 Yb2 B2 54.1(3) 1_565 4_566 ?
O2 Yb2 B4 22.0(2) 6_657 6_657 ?
O5 Yb2 B4 104.2(2) 3_546 6_657 ?
O6 Yb2 B4 83.65(19) 1_565 6_657 ?
O7 Yb2 B4 97.39(17) . 6_657 ?
O3 Yb2 B4 139.8(2) 4_556 6_657 ?
O3 Yb2 B4 139.8(3) . 6_657 ?
O8 Yb2 B4 69.78(19) 1_565 6_657 ?
O4 Yb2 B4 67.6(2) 1_565 6_657 ?
B4 Yb2 B4 99.88(15) 6_647 6_657 ?
B2 Yb2 B4 76.1(2) 1_565 6_657 ?
B2 Yb2 B4 76.77(18) 4_566 6_657 ?
O5 B1 O5 108.9(8) 3_546 . ?
O5 B1 O8 108.9(3) 3_546 . ?
O5 B1 O8 113.0(3) . . ?
O5 B1 O8 113.0(3) 3_546 3_546 ?
O5 B1 O8 108.9(3) . 3_546 ?
O8 B1 O8 104.2(7) . 3_546 ?
O3 B2 O4 115.2(6) . . ?
O3 B2 O6 112.0(6) . . ?
O4 B2 O6 105.2(5) . . ?
O3 B2 O8 117.3(6) . 4_556 ?
O4 B2 O8 105.7(5) . 4_556 ?
O6 B2 O8 99.6(5) . 4_556 ?
O3 B2 Yb1 136.9(5) . 2_545 ?
O4 B2 Yb1 54.3(3) . 2_545 ?
O6 B2 Yb1 111.0(4) . 2_545 ?
O8 B2 Yb1 51.4(3) 4_556 2_545 ?
O3 B2 Yb2 136.1(5) . 1_545 ?
O4 B2 Yb2 59.3(3) . 1_545 ?
O6 B2 Yb2 46.3(3) . 1_545 ?
O8 B2 Yb2 105.0(4) 4_556 1_545 ?
Yb1 B2 Yb2 78.90(19) 2_545 1_545 ?
O3 B2 Yb2 133.3(5) . 4_546 ?
O4 B2 Yb2 110.8(4) . 4_546 ?
O6 B2 Yb2 45.6(3) . 4_546 ?
O8 B2 Yb2 54.3(3) 4_556 4_546 ?
Yb1 B2 Yb2 78.39(19) 2_545 4_546 ?
Yb2 B2 Yb2 64.90(16) 1_545 4_546 ?
O4 B2 Yb1 91.3(4) . 2 ?
O6 B2 Yb1 153.4(5) . 2 ?
O8 B2 Yb1 95.6(4) 4_556 2 ?
Yb1 B2 Yb1 95.5(2) 2_545 2 ?
Yb2 B2 Yb1 147.5(3) 1_545 2 ?
Yb2 B2 Yb1 145.9(3) 4_546 2 ?
O4 B2 Yb2 94.9(4) . . ?
O6 B2 Yb2 84.6(4) . . ?
O8 B2 Yb2 156.8(5) 4_556 . ?
Yb1 B2 Yb2 147.6(3) 2_545 . ?
Yb2 B2 Yb2 94.5(2) 1_545 . ?
Yb2 B2 Yb2 127.6(2) 4_546 . ?
Yb1 B2 Yb2 73.11(17) 2 . ?
O4 B2 Yb2 153.3(5) . 4_556 ?
O6 B2 Yb2 83.9(4) . 4_556 ?
O8 B2 Yb2 97.1(4) 4_556 4_556 ?
Yb1 B2 Yb2 146.1(3) 2_545 4_556 ?
Yb2 B2 Yb2 127.7(2) 1_545 4_556 ?
Yb2 B2 Yb2 93.6(2) 4_546 4_556 ?
Yb1 B2 Yb2 72.69(17) 2 4_556 ?
Yb2 B2 Yb2 60.42(14) . 4_556 ?
O1 B3 O4 114.4(7) . 2_554 ?
O1 B3 O4 114.4(7) . 8 ?
O4 B3 O4 105.3(7) 2_554 8 ?
O1 B3 O7 108.4(8) . 2_554 ?
O4 B3 O7 107.0(7) 2_554 2_554 ?
O4 B3 O7 107.0(7) 8 2_554 ?
O2 B4 O5 114.9(5) . 8_556 ?
O2 B4 O5 114.9(5) . 2 ?
O5 B4 O5 109.3(8) 8_556 2 ?
O2 B4 O7 110.6(9) . 6_567 ?
O5 B4 O7 102.9(5) 8_556 6_567 ?
O5 B4 O7 102.9(5) 2 6_567 ?
O2 B4 Yb2 134.4(4) . 4_566 ?
O5 B4 Yb2 110.5(5) 8_556 4_566 ?
O5 B4 Yb2 50.1(3) 2 4_566 ?
O7 B4 Yb2 53.3(3) 6_567 4_566 ?
O2 B4 Yb2 134.4(4) . 6_567 ?
O5 B4 Yb2 50.1(3) 8_556 6_567 ?
O5 B4 Yb2 110.5(5) 2 6_567 ?
O7 B4 Yb2 53.3(3) 6_567 6_567 ?
Yb2 B4 Yb2 74.8(3) 4_566 6_567 ?
O5 B4 Yb2 87.9(3) 8_556 6_557 ?
O5 B4 Yb2 149.5(5) 2 6_557 ?
O7 B4 Yb2 97.2(5) 6_567 6_557 ?
Yb2 B4 Yb2 147.2(4) 4_566 6_557 ?
Yb2 B4 Yb2 99.88(15) 6_567 6_557 ?
O5 B4 Yb2 149.5(5) 8_556 4_556 ?
O5 B4 Yb2 87.9(3) 2 4_556 ?
O7 B4 Yb2 97.2(5) 6_567 4_556 ?
Yb2 B4 Yb2 99.88(15) 4_566 4_556 ?
Yb2 B4 Yb2 147.2(4) 6_567 4_556 ?
Yb2 B4 Yb2 66.8(2) 6_557 4_556 ?
B3 O1 Yb1 129.43(18) . 5_556 ?
B3 O1 Yb1 129.43(18) . . ?
Yb1 O1 Yb1 100.6(3) 5_556 . ?
B4 O2 Yb2 122.8(3) . 6_557 ?
B4 O2 Yb2 122.8(3) . 4_556 ?
Yb2 O2 Yb2 106.7(3) 6_557 4_556 ?
B2 O3 Yb1 114.6(4) . 2 ?
B2 O3 Yb2 117.3(5) . 4_556 ?
Yb1 O3 Yb2 110.1(2) 2 4_556 ?
B2 O3 Yb2 114.5(4) . . ?
Yb1 O3 Yb2 109.4(2) 2 . ?
Yb2 O3 Yb2 87.91(19) 4_556 . ?
B2 O4 B3 119.1(6) . 2 ?
B2 O4 Yb1 96.3(4) . 2_545 ?
B3 O4 Yb1 124.4(6) 2 2_545 ?
B2 O4 Yb2 91.3(4) . 1_545 ?
B3 O4 Yb2 120.1(6) 2 1_545 ?
Yb1 O4 Yb2 98.48(18) 2_545 1_545 ?
B1 O5 B4 123.8(6) . 2_554 ?
B1 O5 Yb2 130.8(5) . 3_546 ?
B4 O5 Yb2 98.5(5) 2_554 3_546 ?
B2 O6 B2 134.2(8) . 4_556 ?
B2 O6 Yb2 106.3(3) . 4_546 ?
B2 O6 Yb2 105.1(3) 4_556 4_546 ?
B2 O6 Yb2 105.1(3) . 1_545 ?
B2 O6 Yb2 106.3(3) 4_556 1_545 ?
Yb2 O6 Yb2 91.9(2) 4_546 1_545 ?
B4 O7 B3 126.6(7) 6_647 2 ?
B4 O7 Yb2 93.8(4) 6_647 . ?
B3 O7 Yb2 118.9(3) 2 . ?
B4 O7 Yb2 93.8(4) 6_647 7_655 ?
B3 O7 Yb2 118.9(3) 2 7_655 ?
Yb2 O7 Yb2 98.3(3) . 7_655 ?
B1 O8 B2 115.3(4) . 4_556 ?
B1 O8 Yb1 127.7(4) . 1_545 ?
B2 O8 Yb1 97.8(4) 4_556 1_545 ?
B1 O8 Yb2 111.5(4) . 1_545 ?
B2 O8 Yb2 95.4(4) 4_556 1_545 ?
Yb1 O8 Yb2 103.89(18) 1_545 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
Yb1 O1 2.198(5) 5_556 ?
Yb1 O1 2.198(5) . ?
Yb1 O3 2.327(6) 4_556 ?
Yb1 O3 2.327(6) 2_554 ?
Yb1 O8 2.365(5) 1_565 ?
Yb1 O8 2.365(5) 3_546 ?
Yb1 O4 2.447(6) 4_566 ?
Yb1 O4 2.447(6) 2_544 ?
Yb1 B2 2.996(8) 4_566 ?
Yb1 B2 2.996(8) 2_544 ?
Yb1 B2 3.196(8) 4_556 ?
Yb1 B2 3.196(8) 2_554 ?
Yb2 O2 2.156(5) 6_657 ?
Yb2 O5 2.208(6) 3_546 ?
Yb2 O6 2.264(5) 1_565 ?
Yb2 O7 2.287(5) . ?
Yb2 O3 2.331(6) 4_556 ?
Yb2 O3 2.357(6) . ?
Yb2 O8 2.481(5) 1_565 ?
Yb2 O4 2.599(6) 1_565 ?
Yb2 B4 2.847(8) 6_647 ?
Yb2 B2 3.021(8) 1_565 ?
Yb2 B2 3.043(8) 4_566 ?
Yb2 B4 3.141(9) 6_657 ?
B1 O5 1.449(8) 3_546 ?
B1 O5 1.449(8) . ?
B1 O8 1.500(9) . ?
B1 O8 1.500(9) 3_546 ?
B2 O3 1.427(10) . ?
B2 O4 1.481(10) . ?
B2 O6 1.496(8) . ?
B2 O8 1.545(10) 4_556 ?
B2 Yb1 2.996(8) 2_545 ?
B2 Yb2 3.021(8) 1_545 ?
B2 Yb2 3.043(8) 4_546 ?
B2 Yb1 3.196(8) 2 ?
B2 Yb2 3.244(8) 4_556 ?
B3 O1 1.397(14) . ?
B3 O4 1.529(9) 2_554 ?
B3 O4 1.529(8) 8 ?
B3 O7 1.582(15) 2_554 ?
B4 O2 1.398(13) . ?
B4 O5 1.499(8) 8_556 ?
B4 O5 1.499(9) 2 ?
B4 O7 1.552(14) 6_567 ?
B4 Yb2 2.847(8) 4_566 ?
B4 Yb2 2.847(8) 6_567 ?
B4 Yb2 3.141(9) 6_557 ?
B4 Yb2 3.141(9) 4_556 ?
O1 Yb1 2.198(5) 5_556 ?
O2 Yb2 2.156(5) 6_557 ?
O2 Yb2 2.156(5) 4_556 ?
O3 Yb1 2.327(6) 2 ?
O3 Yb2 2.331(6) 4_556 ?
O4 B3 1.529(9) 2 ?
O4 Yb1 2.447(6) 2_545 ?
O4 Yb2 2.599(6) 1_545 ?
O5 B4 1.499(8) 2_554 ?
O5 Yb2 2.208(6) 3_546 ?
O6 B2 1.496(8) 4_556 ?
O6 Yb2 2.264(5) 4_546 ?
O6 Yb2 2.264(5) 1_545 ?
O7 B4 1.552(14) 6_647 ?
O7 B3 1.582(15) 2 ?
O7 Yb2 2.287(5) 7_655 ?
O8 B2 1.545(10) 4_556 ?
O8 Yb1 2.365(5) 1_545 ?
O8 Yb2 2.481(5) 1_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
O2 Yb2 B2 O3 104.0(6) 6_657 . . . ?
O5 Yb2 B2 O3 -174.0(5) 3_546 . . . ?
O6 Yb2 B2 O3 -25.8(5) 1_565 . . . ?
O7 Yb2 B2 O3 122.9(5) . . . . ?
O3 Yb2 B2 O3 -98.5(5) 4_556 . . . ?
O8 Yb2 B2 O3 -80.9(5) 1_565 . . . ?
O4 Yb2 B2 O3 31.9(5) 1_565 . . . ?
B4 Yb2 B2 O3 155.7(5) 6_647 . . . ?
B2 Yb2 B2 O3 2.6(6) 1_565 . . . ?
B2 Yb2 B2 O3 -49.0(5) 4_566 . . . ?
B4 Yb2 B2 O3 69.5(7) 6_657 . . . ?
O2 Yb2 B2 O4 -19.0(6) 6_657 . . . ?
O5 Yb2 B2 O4 62.9(4) 3_546 . . . ?
O6 Yb2 B2 O4 -148.8(4) 1_565 . . . ?
O7 Yb2 B2 O4 -0.1(4) . . . . ?
O3 Yb2 B2 O4 138.5(4) 4_556 . . . ?
O3 Yb2 B2 O4 -123.0(7) . . . . ?
O8 Yb2 B2 O4 156.1(4) 1_565 . . . ?
O4 Yb2 B2 O4 -91.1(4) 1_565 . . . ?
B4 Yb2 B2 O4 32.7(4) 6_647 . . . ?
B2 Yb2 B2 O4 -120.5(3) 1_565 . . . ?
B2 Yb2 B2 O4 -172.0(4) 4_566 . . . ?
B4 Yb2 B2 O4 -53.6(7) 6_657 . . . ?
O2 Yb2 B2 O6 -123.9(5) 6_657 . . . ?
O5 Yb2 B2 O6 -41.9(3) 3_546 . . . ?
O6 Yb2 B2 O6 106.3(3) 1_565 . . . ?
O7 Yb2 B2 O6 -105.0(4) . . . . ?
O3 Yb2 B2 O6 33.6(3) 4_556 . . . ?
O3 Yb2 B2 O6 132.1(7) . . . . ?
O8 Yb2 B2 O6 51.2(4) 1_565 . . . ?
O4 Yb2 B2 O6 164.0(3) 1_565 . . . ?
B4 Yb2 B2 O6 -72.2(3) 6_647 . . . ?
B2 Yb2 B2 O6 134.7(2) 1_565 . . . ?
B2 Yb2 B2 O6 83.1(4) 4_566 . . . ?
B4 Yb2 B2 O6 -158.4(4) 6_657 . . . ?
O2 Yb2 B2 O8 134.1(12) 6_657 . . 4_556 ?
O5 Yb2 B2 O8 -143.9(12) 3_546 . . 4_556 ?
O6 Yb2 B2 O8 4.4(12) 1_565 . . 4_556 ?
O7 Yb2 B2 O8 153.1(12) . . . 4_556 ?
O3 Yb2 B2 O8 -68.3(12) 4_556 . . 4_556 ?
O3 Yb2 B2 O8 30.1(10) . . . 4_556 ?
O8 Yb2 B2 O8 -50.8(13) 1_565 . . 4_556 ?
O4 Yb2 B2 O8 62.0(12) 1_565 . . 4_556 ?
B4 Yb2 B2 O8 -174.1(12) 6_647 . . 4_556 ?
B2 Yb2 B2 O8 32.7(13) 1_565 . . 4_556 ?
B2 Yb2 B2 O8 -18.9(12) 4_566 . . 4_556 ?
B4 Yb2 B2 O8 99.6(12) 6_657 . . 4_556 ?
O2 Yb2 B2 Yb1 -2.3(7) 6_657 . . 2_545 ?
O5 Yb2 B2 Yb1 79.7(5) 3_546 . . 2_545 ?
O6 Yb2 B2 Yb1 -132.1(5) 1_565 . . 2_545 ?
O7 Yb2 B2 Yb1 16.7(5) . . . 2_545 ?
O3 Yb2 B2 Yb1 155.3(6) 4_556 . . 2_545 ?
O3 Yb2 B2 Yb1 -106.3(7) . . . 2_545 ?
O8 Yb2 B2 Yb1 172.8(4) 1_565 . . 2_545 ?
O4 Yb2 B2 Yb1 -74.4(5) 1_565 . . 2_545 ?
B4 Yb2 B2 Yb1 49.4(5) 6_647 . . 2_545 ?
B2 Yb2 B2 Yb1 -103.7(5) 1_565 . . 2_545 ?
B2 Yb2 B2 Yb1 -155.3(5) 4_566 . . 2_545 ?
B4 Yb2 B2 Yb1 -36.8(8) 6_657 . . 2_545 ?
O2 Yb2 B2 Yb2 -78.6(4) 6_657 . . 1_545 ?
O5 Yb2 B2 Yb2 3.4(2) 3_546 . . 1_545 ?
O6 Yb2 B2 Yb2 151.66(15) 1_565 . . 1_545 ?
O7 Yb2 B2 Yb2 -59.6(3) . . . 1_545 ?
O3 Yb2 B2 Yb2 79.0(2) 4_556 . . 1_545 ?
O3 Yb2 B2 Yb2 177.4(6) . . . 1_545 ?
O8 Yb2 B2 Yb2 96.5(3) 1_565 . . 1_545 ?
O4 Yb2 B2 Yb2 -150.7(2) 1_565 . . 1_545 ?
B4 Yb2 B2 Yb2 -26.8(2) 6_647 . . 1_545 ?
B2 Yb2 B2 Yb2 180.0 1_565 . . 1_545 ?
B2 Yb2 B2 Yb2 128.4(3) 4_566 . . 1_545 ?
B4 Yb2 B2 Yb2 -113.1(4) 6_657 . . 1_545 ?
O2 Yb2 B2 Yb2 -140.1(4) 6_657 . . 4_546 ?
O5 Yb2 B2 Yb2 -58.1(3) 3_546 . . 4_546 ?
O6 Yb2 B2 Yb2 90.1(3) 1_565 . . 4_546 ?
O7 Yb2 B2 Yb2 -121.2(4) . . . 4_546 ?
O3 Yb2 B2 Yb2 17.4(3) 4_556 . . 4_546 ?
O3 Yb2 B2 Yb2 115.9(6) . . . 4_546 ?
O8 Yb2 B2 Yb2 35.0(4) 1_565 . . 4_546 ?
O4 Yb2 B2 Yb2 147.8(3) 1_565 . . 4_546 ?
B4 Yb2 B2 Yb2 -88.4(3) 6_647 . . 4_546 ?
B2 Yb2 B2 Yb2 118.5(3) 1_565 . . 4_546 ?
B2 Yb2 B2 Yb2 66.9(4) 4_566 . . 4_546 ?
B4 Yb2 B2 Yb2 -174.6(3) 6_657 . . 4_546 ?
O2 Yb2 B2 Yb1 70.8(4) 6_657 . . 2 ?
O5 Yb2 B2 Yb1 152.78(18) 3_546 . . 2 ?
O6 Yb2 B2 Yb1 -58.97(13) 1_565 . . 2 ?
O7 Yb2 B2 Yb1 89.7(2) . . . 2 ?
O3 Yb2 B2 Yb1 -131.7(2) 4_556 . . 2 ?
O3 Yb2 B2 Yb1 -33.2(4) . . . 2 ?
O8 Yb2 B2 Yb1 -114.1(2) 1_565 . . 2 ?
O4 Yb2 B2 Yb1 -1.30(17) 1_565 . . 2 ?
B4 Yb2 B2 Yb1 122.5(2) 6_647 . . 2 ?
B2 Yb2 B2 Yb1 -30.6(3) 1_565 . . 2 ?
B2 Yb2 B2 Yb1 -82.20(14) 4_566 . . 2 ?
B4 Yb2 B2 Yb1 36.3(5) 6_657 . . 2 ?
O2 Yb2 B2 Yb2 150.1(4) 6_657 . . 4_556 ?
O5 Yb2 B2 Yb2 -127.90(16) 3_546 . . 4_556 ?
O6 Yb2 B2 Yb2 20.35(11) 1_565 . . 4_556 ?
O7 Yb2 B2 Yb2 169.1(3) . . . 4_556 ?
O3 Yb2 B2 Yb2 -52.35(16) 4_556 . . 4_556 ?
O3 Yb2 B2 Yb2 46.1(4) . . . 4_556 ?
O8 Yb2 B2 Yb2 -34.8(3) 1_565 . . 4_556 ?
O4 Yb2 B2 Yb2 78.02(15) 1_565 . . 4_556 ?
B4 Yb2 B2 Yb2 -158.2(2) 6_647 . . 4_556 ?
B2 Yb2 B2 Yb2 48.7(2) 1_565 . . 4_556 ?
B2 Yb2 B2 Yb2 -2.87(16) 4_566 . . 4_556 ?
B4 Yb2 B2 Yb2 115.6(4) 6_657 . . 4_556 ?
O4 B3 O1 Yb1 155.6(5) 2_554 . . 5_556 ?
O4 B3 O1 Yb1 34.1(13) 8 . . 5_556 ?
O7 B3 O1 Yb1 -85.1(7) 2_554 . . 5_556 ?
O4 B3 O1 Yb1 -34.1(13) 2_554 . . . ?
O4 B3 O1 Yb1 -155.6(5) 8 . . . ?
O7 B3 O1 Yb1 85.1(7) 2_554 . . . ?
O1 Yb1 O1 B3 -172.4(11) 5_556 . . . ?
O3 Yb1 O1 B3 145.0(8) 4_556 . . . ?
O3 Yb1 O1 B3 -14.3(9) 2_554 . . . ?
O8 Yb1 O1 B3 51.8(10) 1_565 . . . ?
O8 Yb1 O1 B3 -60.1(10) 3_546 . . . ?
O4 Yb1 O1 B3 103.2(9) 4_566 . . . ?
O4 Yb1 O1 B3 -91.2(9) 2_544 . . . ?
B2 Yb1 O1 B3 78.9(9) 4_566 . . . ?
B2 Yb1 O1 B3 -78.9(9) 2_544 . . . ?
B2 Yb1 O1 B3 -170.8(7) 4_556 . . . ?
B2 Yb1 O1 B3 8.6(8) 2_554 . . . ?
O1 Yb1 O1 Yb1 0.0 5_556 . . 5_556 ?
O3 Yb1 O1 Yb1 -42.6(6) 4_556 . . 5_556 ?
O3 Yb1 O1 Yb1 158.1(3) 2_554 . . 5_556 ?
O8 Yb1 O1 Yb1 -135.8(3) 1_565 . . 5_556 ?
O8 Yb1 O1 Yb1 112.3(3) 3_546 . . 5_556 ?
O4 Yb1 O1 Yb1 -84.4(3) 4_566 . . 5_556 ?
O4 Yb1 O1 Yb1 81.2(3) 2_544 . . 5_556 ?
B2 Yb1 O1 Yb1 -108.7(3) 4_566 . . 5_556 ?
B2 Yb1 O1 Yb1 93.5(3) 2_544 . . 5_556 ?
B2 Yb1 O1 Yb1 1.6(7) 4_556 . . 5_556 ?
B2 Yb1 O1 Yb1 -179.0(4) 2_554 . . 5_556 ?
O5 B4 O2 Yb2 43.4(12) 8_556 . . 6_557 ?
O5 B4 O2 Yb2 171.5(6) 2 . . 6_557 ?
O7 B4 O2 Yb2 -72.5(6) 6_567 . . 6_557 ?
Yb2 B4 O2 Yb2 -130.8(4) 4_566 . . 6_557 ?
Yb2 B4 O2 Yb2 -14.3(13) 6_567 . . 6_557 ?
Yb2 B4 O2 Yb2 -145.1(12) 4_556 . . 6_557 ?
O5 B4 O2 Yb2 -171.5(6) 8_556 . . 4_556 ?
O5 B4 O2 Yb2 -43.4(12) 2 . . 4_556 ?
O7 B4 O2 Yb2 72.5(6) 6_567 . . 4_556 ?
Yb2 B4 O2 Yb2 14.3(13) 4_566 . . 4_556 ?
Yb2 B4 O2 Yb2 130.8(4) 6_567 . . 4_556 ?
Yb2 B4 O2 Yb2 145.1(12) 6_557 . . 4_556 ?
O4 B2 O3 Yb1 -60.3(7) . . . 2 ?
O6 B2 O3 Yb1 179.5(3) . . . 2 ?
O8 B2 O3 Yb1 65.2(7) 4_556 . . 2 ?
Yb1 B2 O3 Yb1 3.5(9) 2_545 . . 2 ?
Yb2 B2 O3 Yb1 -131.4(5) 1_545 . . 2 ?
Yb2 B2 O3 Yb1 130.6(5) 4_546 . . 2 ?
Yb2 B2 O3 Yb1 -127.7(5) . . . 2 ?
Yb2 B2 O3 Yb1 131.4(6) 4_556 . . 2 ?
O4 B2 O3 Yb2 168.4(4) . . . 4_556 ?
O6 B2 O3 Yb2 48.2(7) . . . 4_556 ?
O8 B2 O3 Yb2 -66.1(7) 4_556 . . 4_556 ?
Yb1 B2 O3 Yb2 -127.8(5) 2_545 . . 4_556 ?
Yb2 B2 O3 Yb2 97.3(7) 1_545 . . 4_556 ?
Yb2 B2 O3 Yb2 -0.7(8) 4_546 . . 4_556 ?
Yb1 B2 O3 Yb2 -131.4(6) 2 . . 4_556 ?
Yb2 B2 O3 Yb2 101.0(5) . . . 4_556 ?
O4 B2 O3 Yb2 67.4(7) . . . . ?
O6 B2 O3 Yb2 -52.8(7) . . . . ?
O8 B2 O3 Yb2 -167.1(4) 4_556 . . . ?
Yb1 B2 O3 Yb2 131.2(5) 2_545 . . . ?
Yb2 B2 O3 Yb2 -3.7(9) 1_545 . . . ?
Yb2 B2 O3 Yb2 -101.7(6) 4_546 . . . ?
Yb1 B2 O3 Yb2 127.7(5) 2 . . . ?
Yb2 B2 O3 Yb2 -101.0(5) 4_556 . . . ?
O2 Yb2 O3 B2 -106.3(6) 6_657 . . . ?
O5 Yb2 O3 B2 6.4(5) 3_546 . . . ?
O6 Yb2 O3 B2 154.0(5) 1_565 . . . ?
O7 Yb2 O3 B2 -51.1(5) . . . . ?
O3 Yb2 O3 B2 72.0(4) 4_556 . . . ?
O8 Yb2 O3 B2 118.1(5) 1_565 . . . ?
O4 Yb2 O3 B2 -146.3(5) 1_565 . . . ?
B4 Yb2 O3 B2 -23.9(5) 6_647 . . . ?
B2 Yb2 O3 B2 -177.3(6) 1_565 . . . ?
B2 Yb2 O3 B2 137.0(4) 4_566 . . . ?
B4 Yb2 O3 B2 -141.0(4) 6_657 . . . ?
O2 Yb2 O3 Yb1 23.9(4) 6_657 . . 2 ?
O5 Yb2 O3 Yb1 136.6(2) 3_546 . . 2 ?
O6 Yb2 O3 Yb1 -75.73(19) 1_565 . . 2 ?
O7 Yb2 O3 Yb1 79.1(3) . . . 2 ?
O3 Yb2 O3 Yb1 -157.7(2) 4_556 . . 2 ?
O8 Yb2 O3 Yb1 -111.7(2) 1_565 . . 2 ?
O4 Yb2 O3 Yb1 -16.1(2) 1_565 . . 2 ?
B4 Yb2 O3 Yb1 106.3(2) 6_647 . . 2 ?
B2 Yb2 O3 Yb1 -47.0(2) 1_565 . . 2 ?
B2 Yb2 O3 Yb1 -92.8(2) 4_566 . . 2 ?
B4 Yb2 O3 Yb1 -10.8(4) 6_657 . . 2 ?
O2 Yb2 O3 Yb2 134.5(3) 6_657 . . 4_556 ?
O5 Yb2 O3 Yb2 -112.83(19) 3_546 . . 4_556 ?
O6 Yb2 O3 Yb2 34.82(13) 1_565 . . 4_556 ?
O7 Yb2 O3 Yb2 -170.4(2) . . . 4_556 ?
O3 Yb2 O3 Yb2 -47.2(2) 4_556 . . 4_556 ?
O8 Yb2 O3 Yb2 -1.1(3) 1_565 . . 4_556 ?
O4 Yb2 O3 Yb2 94.45(19) 1_565 . . 4_556 ?
B4 Yb2 O3 Yb2 -143.15(19) 6_647 . . 4_556 ?
B2 Yb2 O3 Yb2 63.51(19) 1_565 . . 4_556 ?
B2 Yb2 O3 Yb2 17.8(2) 4_566 . . 4_556 ?
B4 Yb2 O3 Yb2 99.8(3) 6_657 . . 4_556 ?
O3 B2 O4 B3 -4.3(10) . . . 2 ?
O6 B2 O4 B3 119.5(8) . . . 2 ?
O8 B2 O4 B3 -135.6(8) 4_556 . . 2 ?
Yb1 B2 O4 B3 -135.3(8) 2_545 . . 2 ?
Yb2 B2 O4 B3 126.0(8) 1_545 . . 2 ?
Yb2 B2 O4 B3 167.2(7) 4_546 . . 2 ?
Yb1 B2 O4 B3 -39.4(8) 2 . . 2 ?
Yb2 B2 O4 B3 33.7(8) . . . 2 ?
Yb2 B2 O4 B3 12.4(15) 4_556 . . 2 ?
O3 B2 O4 Yb1 131.0(5) . . . 2_545 ?
O6 B2 O4 Yb1 -105.2(5) . . . 2_545 ?
O8 B2 O4 Yb1 -0.3(5) 4_556 . . 2_545 ?
Yb2 B2 O4 Yb1 -98.7(2) 1_545 . . 2_545 ?
Yb2 B2 O4 Yb1 -57.5(4) 4_546 . . 2_545 ?
Yb1 B2 O4 Yb1 95.9(2) 2 . . 2_545 ?
Yb2 B2 O4 Yb1 169.04(19) . . . 2_545 ?
Yb2 B2 O4 Yb1 147.7(9) 4_556 . . 2_545 ?
O3 B2 O4 Yb2 -130.3(5) . . . 1_545 ?
O6 B2 O4 Yb2 -6.5(5) . . . 1_545 ?
O8 B2 O4 Yb2 98.4(5) 4_556 . . 1_545 ?
Yb1 B2 O4 Yb2 98.7(2) 2_545 . . 1_545 ?
Yb2 B2 O4 Yb2 41.2(3) 4_546 . . 1_545 ?
Yb1 B2 O4 Yb2 -165.43(19) 2 . . 1_545 ?
Yb2 B2 O4 Yb2 -92.3(2) . . . 1_545 ?
Yb2 B2 O4 Yb2 -113.6(9) 4_556 . . 1_545 ?
O5 B1 O5 B4 -43.3(6) 3_546 . . 2_554 ?
O8 B1 O5 B4 -164.4(7) . . . 2_554 ?
O8 B1 O5 B4 80.3(8) 3_546 . . 2_554 ?
O5 B1 O5 Yb2 172.1(5) 3_546 . . 3_546 ?
O8 B1 O5 Yb2 51.0(7) . . . 3_546 ?
O8 B1 O5 Yb2 -64.3(6) 3_546 . . 3_546 ?
O3 B2 O6 B2 1.7(9) . . . 4_556 ?
O4 B2 O6 B2 -124.1(5) . . . 4_556 ?
O8 B2 O6 B2 126.5(5) 4_556 . . 4_556 ?
Yb1 B2 O6 B2 178.8(4) 2_545 . . 4_556 ?
Yb2 B2 O6 B2 -131.9(6) 1_545 . . 4_556 ?
Yb2 B2 O6 B2 131.5(6) 4_546 . . 4_556 ?
Yb1 B2 O6 B2 2.4(8) 2 . . 4_556 ?
Yb2 B2 O6 B2 -30.5(6) . . . 4_556 ?
Yb2 B2 O6 B2 30.3(6) 4_556 . . 4_556 ?
O3 B2 O6 Yb2 -129.8(5) . . . 4_546 ?
O4 B2 O6 Yb2 104.3(5) . . . 4_546 ?
O8 B2 O6 Yb2 -5.0(5) 4_556 . . 4_546 ?
Yb1 B2 O6 Yb2 47.3(4) 2_545 . . 4_546 ?
Yb2 B2 O6 Yb2 96.6(4) 1_545 . . 4_546 ?
Yb1 B2 O6 Yb2 -129.1(9) 2 . . 4_546 ?
Yb2 B2 O6 Yb2 -161.98(19) . . . 4_546 ?
Yb2 B2 O6 Yb2 -101.2(2) 4_556 . . 4_546 ?
O3 B2 O6 Yb2 133.6(5) . . . 1_545 ?
O4 B2 O6 Yb2 7.7(6) . . . 1_545 ?
O8 B2 O6 Yb2 -101.6(4) 4_556 . . 1_545 ?
Yb1 B2 O6 Yb2 -49.3(4) 2_545 . . 1_545 ?
Yb2 B2 O6 Yb2 -96.6(4) 4_546 . . 1_545 ?
Yb1 B2 O6 Yb2 134.3(9) 2 . . 1_545 ?
Yb2 B2 O6 Yb2 101.4(2) . . . 1_545 ?
Yb2 B2 O6 Yb2 162.18(19) 4_556 . . 1_545 ?
O2 Yb2 O7 B4 -88.2(4) 6_657 . . 6_647 ?
O5 Yb2 O7 B4 5.5(4) 3_546 . . 6_647 ?
O6 Yb2 O7 B4 173.5(4) 1_565 . . 6_647 ?
O3 Yb2 O7 B4 61.5(4) 4_556 . . 6_647 ?
O3 Yb2 O7 B4 123.9(4) . . . 6_647 ?
O8 Yb2 O7 B4 -37.0(6) 1_565 . . 6_647 ?
O4 Yb2 O7 B4 -164.4(4) 1_565 . . 6_647 ?
B2 Yb2 O7 B4 -175.0(4) 1_565 . . 6_647 ?
B4 Yb2 O7 B4 -96.8(5) 6_657 . . 6_647 ?
O2 Yb2 O7 B3 135.9(6) 6_657 . . 2 ?
O5 Yb2 O7 B3 -130.5(6) 3_546 . . 2 ?
O6 Yb2 O7 B3 37.6(7) 1_565 . . 2 ?
O3 Yb2 O7 B3 -74.4(6) 4_556 . . 2 ?
O3 Yb2 O7 B3 -12.1(5) . . . 2 ?
O8 Yb2 O7 B3 -172.9(5) 1_565 . . 2 ?
O4 Yb2 O7 B3 59.6(6) 1_565 . . 2 ?
B4 Yb2 O7 B3 -136.0(7) 6_647 . . 2 ?
B2 Yb2 O7 B3 49.1(6) 1_565 . . 2 ?
B4 Yb2 O7 B3 127.3(6) 6_657 . . 2 ?
O2 Yb2 O7 Yb2 6.2(3) 6_657 . . 7_655 ?
O5 Yb2 O7 Yb2 99.9(3) 3_546 . . 7_655 ?
O6 Yb2 O7 Yb2 -92.1(4) 1_565 . . 7_655 ?
O3 Yb2 O7 Yb2 155.9(2) 4_556 . . 7_655 ?
O3 Yb2 O7 Yb2 -141.7(3) . . . 7_655 ?
O8 Yb2 O7 Yb2 57.4(5) 1_565 . . 7_655 ?
O4 Yb2 O7 Yb2 -70.0(3) 1_565 . . 7_655 ?
B4 Yb2 O7 Yb2 94.4(5) 6_647 . . 7_655 ?
B2 Yb2 O7 Yb2 -80.6(3) 1_565 . . 7_655 ?
B4 Yb2 O7 Yb2 -2.4(3) 6_657 . . 7_655 ?
O5 B1 O8 B2 53.4(7) 3_546 . . 4_556 ?
O5 B1 O8 B2 174.4(5) . . . 4_556 ?
O8 B1 O8 B2 -67.5(4) 3_546 . . 4_556 ?
O5 B1 O8 Yb1 177.1(4) 3_546 . . 1_545 ?
O5 B1 O8 Yb1 -61.9(7) . . . 1_545 ?
O8 B1 O8 Yb1 56.2(3) 3_546 . . 1_545 ?
O5 B1 O8 Yb2 -53.9(5) 3_546 . . 1_545 ?
O5 B1 O8 Yb2 67.2(6) . . . 1_545 ?
O8 B1 O8 Yb2 -174.8(4) 3_546 . . 1_545 ?
|
1100928.cif | #------------------------------------------------------------------------------
#$Date: 2022-09-14 18:21:52 +0300 (Wed, 14 Sep 2022) $
#$Revision: 277833 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/09/1100928.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_1100928
loop_
_publ_author_name
'Emme, Holger'
'Valldor, Martin'
'P\"ottgen, Rainer'
'Huppertz, Hubert'
_publ_section_title
;
Associating Borate and Silicate Chemistry by Extreme Conditions:
High-Pressure Synthesis, Crystal Structure, and Properties of
the New Borates RE~3~B~5~O~12~ (RE = Er--Lu)
;
_journal_coden_ASTM CMATEX
_journal_issue 10
_journal_name_full 'Chemistry of Materials'
_journal_page_first 2707
_journal_page_last 2715
_journal_paper_doi 10.1021/cm047741+
_journal_volume 17
_journal_year 2005
_chemical_formula_moiety 'B5 Lu3 O12'
_chemical_formula_sum 'B5 Lu3 O12'
_chemical_formula_weight 770.96
_chemical_melting_point ?
_chemical_name_common Trilutetiumpentaborate
_chemical_name_systematic Trilutetiumpentaborate
_space_group_IT_number 53
_space_group_name_Hall '-P 2ac 2'
_space_group_name_H-M_alt 'P m n a'
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall '-P 2ac 2'
_symmetry_space_group_name_H-M 'P m n a'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_contact_author_address
;
'Department Chemie und Biochemie
Ludwig-Maximilians-Universitaet Muenchen
Butenandtstrasse 5-13 (Haus D)
81377 Muenchen
Germany'
;
_audit_contact_author_email huh@cup.uni-muenchen.de
_audit_contact_author_fax '+49 (0)89 2180 77440'
_audit_contact_author_phone '+49 (0)89 2180 77442'
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 12.76510(40)
_cell_length_b 4.57500(20)
_cell_length_c 12.44180(40)
_cell_measurement_reflns_used 4810
_cell_measurement_temperature 200(2)
_cell_measurement_theta_max 40.250
_cell_measurement_theta_min 3.134
_cell_volume 726.605(45)
_computing_cell_refinement 'HKL SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection 'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL DENZO (Otwinowski & Minor, 1997) and SCALEPACK'
_computing_molecular_graphics 'DIAMOND (Brandenburg & Berndt, 1999)'
_computing_publication_material 'enCIFer (Allen et al., 2004) and SHELXL97'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 200(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type KappaCCD
_diffrn_measurement_method '95mm CCD camera on \k-goniostat'
_diffrn_radiation_collimation 0.35
_diffrn_radiation_monochromator 'vertically mounted graphite crystal'
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0569
_diffrn_reflns_av_sigmaI/netI 0.0365
_diffrn_reflns_limit_h_max 21
_diffrn_reflns_limit_h_min -21
_diffrn_reflns_limit_k_max 7
_diffrn_reflns_limit_k_min -7
_diffrn_reflns_limit_l_max 21
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_number 14453
_diffrn_reflns_theta_full 37.48
_diffrn_reflns_theta_max 37.48
_diffrn_reflns_theta_min 3.19
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 40.530
_exptl_absorpt_correction_T_max 0.5091
_exptl_absorpt_correction_T_min 0.1714
_exptl_absorpt_correction_type numerical
_exptl_absorpt_process_details 'Herrendorf,B\"arnighausen,HABITUS, 1993/1997'
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 7.048
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description platelet
_exptl_crystal_F_000 1336
_exptl_crystal_size_max 0.11
_exptl_crystal_size_mid 0.04
_exptl_crystal_size_min 0.02
_refine_diff_density_max 6.425
_refine_diff_density_min -5.022
_refine_diff_density_rms 0.591
_refine_ls_extinction_coef 0.00070(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 0.957
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 101
_refine_ls_number_reflns 1928
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.957
_refine_ls_R_factor_all 0.0566
_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^)+(0.0455P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0776
_refine_ls_wR_factor_ref 0.0850
_reflns_number_gt 1141
_reflns_number_total 1928
_reflns_threshold_expression >2sigma(I)
_cod_duplicate_entry 4000578
_cod_data_source_file cm047741+si20041223_064556.cif
_cod_data_source_block Lu3B5O12
_cod_original_sg_symbol_H-M Pmna
_cod_database_code 1100928
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'
'-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
Lu1 Lu 0.13248(2) 0.0000 0.5000 0.00495(8) Uani 1 2 d S . .
Lu2 Lu 0.364559(15) -0.00123(6) 0.693646(15) 0.00552(7) Uani 1 1 d . . .
B1 B 0.3381(5) -0.5000 0.5000 0.0060(11) Uani 1 2 d S . .
B2 B 0.2980(5) -0.5285(14) 0.8497(4) 0.0077(11) Uani 1 1 d . . .
B3 B 0.0000 0.4610(16) 0.3516(6) 0.0049(14) Uani 1 2 d S . .
B4 B 0.0000 0.5409(17) 0.8744(7) 0.0075(16) Uani 1 2 d S . .
O1 O 0.0000 0.2450(11) 0.4303(4) 0.0087(9) Uani 1 2 d S . .
O2 O 0.0000 0.2384(11) 0.8617(4) 0.0093(10) Uani 1 2 d S . .
O3 O 0.2963(3) -0.2201(8) 0.8485(2) 0.0079(7) Uani 1 1 d . . .
O4 O 0.4049(3) -0.6634(9) 0.8546(3) 0.0090(7) Uani 1 1 d . . .
O5 O 0.4042(2) -0.6674(8) 0.4266(3) 0.0079(6) Uani 1 1 d . . .
O6 O 0.2500 -0.6615(11) 0.7500 0.0078(9) Uani 1 2 d S . .
O7 O 0.5000 -0.3046(11) 0.7388(4) 0.0077(9) Uani 1 2 d S . .
O8 O 0.2664(2) -0.6907(7) 0.5644(3) 0.0079(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
Lu1 0.00498(12) 0.00504(13) 0.00483(12) 0.00016(15) 0.000 0.000
Lu2 0.00511(10) 0.00541(11) 0.00605(10) -0.00023(11) 0.00024(6) 0.00002(9)
B1 0.005(2) 0.009(3) 0.005(2) 0.000(4) 0.000 0.000
B2 0.004(2) 0.013(3) 0.006(2) -0.004(2) -0.0009(15) 0.003(2)
B3 0.004(3) 0.005(4) 0.006(3) -0.003(2) 0.000 0.000
B4 0.010(3) 0.006(5) 0.006(3) 0.003(3) 0.000 0.000
O1 0.009(2) 0.012(3) 0.005(2) 0.000(2) 0.000 0.000
O2 0.011(2) 0.006(2) 0.012(2) 0.004(2) 0.000 0.000
O3 0.0087(16) 0.0085(18) 0.0066(15) -0.0001(13) -0.0001(12) 0.0002(14)
O4 0.0079(16) 0.0072(18) 0.0119(16) 0.0014(15) 0.0008(13) 0.0006(14)
O5 0.0053(14) 0.0078(17) 0.0106(16) 0.0006(15) 0.0014(14) -0.0011(13)
O6 0.009(2) 0.006(2) 0.008(2) 0.000 0.0021(18) 0.000
O7 0.008(2) 0.008(2) 0.007(2) 0.0004(19) 0.000 0.000
O8 0.0083(15) 0.0070(17) 0.0083(15) -0.0015(14) 0.0007(13) 0.0013(13)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_audit_author_name
'Emme, H.'
'Huppertz, H.'
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 Lu1 O1 79.91(19) 5_556 . ?
O1 Lu1 O3 76.16(13) 5_556 4_556 ?
O1 Lu1 O3 147.05(14) . 4_556 ?
O1 Lu1 O3 147.05(14) 5_556 2_554 ?
O1 Lu1 O3 76.16(13) . 2_554 ?
O3 Lu1 O3 133.92(17) 4_556 2_554 ?
O1 Lu1 O8 136.61(14) 5_556 1_565 ?
O1 Lu1 O8 112.59(14) . 1_565 ?
O3 Lu1 O8 72.59(12) 4_556 1_565 ?
O3 Lu1 O8 74.45(12) 2_554 1_565 ?
O1 Lu1 O8 112.59(14) 5_556 3_546 ?
O1 Lu1 O8 136.61(14) . 3_546 ?
O3 Lu1 O8 74.45(12) 4_556 3_546 ?
O3 Lu1 O8 72.59(12) 2_554 3_546 ?
O8 Lu1 O8 87.13(16) 1_565 3_546 ?
O1 Lu1 O4 83.03(15) 5_556 4_566 ?
O1 Lu1 O4 79.60(15) . 4_566 ?
O3 Lu1 O4 75.33(13) 4_556 4_566 ?
O3 Lu1 O4 114.04(13) 2_554 4_566 ?
O8 Lu1 O4 60.53(12) 1_565 4_566 ?
O8 Lu1 O4 141.02(12) 3_546 4_566 ?
O1 Lu1 O4 79.60(15) 5_556 2_544 ?
O1 Lu1 O4 83.02(15) . 2_544 ?
O3 Lu1 O4 114.04(13) 4_556 2_544 ?
O3 Lu1 O4 75.33(13) 2_554 2_544 ?
O8 Lu1 O4 141.02(12) 1_565 2_544 ?
O8 Lu1 O4 60.53(12) 3_546 2_544 ?
O4 Lu1 O4 157.28(17) 4_566 2_544 ?
O1 Lu1 B2 110.38(16) 5_556 4_566 ?
O1 Lu1 B2 96.12(17) . 4_566 ?
O3 Lu1 B2 71.89(13) 4_556 4_566 ?
O3 Lu1 B2 94.51(13) 2_554 4_566 ?
O8 Lu1 B2 30.67(14) 1_565 4_566 ?
O8 Lu1 B2 115.48(14) 3_546 4_566 ?
O4 Lu1 B2 29.88(14) 4_566 4_566 ?
O4 Lu1 B2 169.74(14) 2_544 4_566 ?
O1 Lu1 B2 96.12(17) 5_556 2_544 ?
O1 Lu1 B2 110.38(16) . 2_544 ?
O3 Lu1 B2 94.51(13) 4_556 2_544 ?
O3 Lu1 B2 71.89(13) 2_554 2_544 ?
O8 Lu1 B2 115.48(14) 1_565 2_544 ?
O8 Lu1 B2 30.67(14) 3_546 2_544 ?
O4 Lu1 B2 169.74(14) 4_566 2_544 ?
O4 Lu1 B2 29.88(14) 2_544 2_544 ?
B2 Lu1 B2 145.5(2) 4_566 2_544 ?
O1 Lu1 Lu1 39.96(10) 5_556 5_556 ?
O1 Lu1 Lu1 39.96(10) . 5_556 ?
O3 Lu1 Lu1 113.04(9) 4_556 5_556 ?
O3 Lu1 Lu1 113.04(9) 2_554 5_556 ?
O8 Lu1 Lu1 136.43(8) 1_565 5_556 ?
O8 Lu1 Lu1 136.43(8) 3_546 5_556 ?
O4 Lu1 Lu1 78.64(8) 4_566 5_556 ?
O4 Lu1 Lu1 78.64(8) 2_544 5_556 ?
B2 Lu1 Lu1 107.26(12) 4_566 5_556 ?
B2 Lu1 Lu1 107.26(12) 2_544 5_556 ?
O1 Lu1 Lu2 67.29(11) 5_556 4_556 ?
O1 Lu1 Lu2 113.65(11) . 4_556 ?
O3 Lu1 Lu2 35.30(9) 4_556 4_556 ?
O3 Lu1 Lu2 143.94(9) 2_554 4_556 ?
O8 Lu1 Lu2 69.77(8) 1_565 4_556 ?
O8 Lu1 Lu2 109.36(8) 3_546 4_556 ?
O4 Lu1 Lu2 41.96(9) 4_566 4_556 ?
O4 Lu1 Lu2 138.38(9) 2_544 4_556 ?
B2 Lu1 Lu2 51.15(10) 4_566 4_556 ?
B2 Lu1 Lu2 128.42(10) 2_544 4_556 ?
Lu1 Lu1 Lu2 90.567(4) 5_556 4_556 ?
O2 Lu2 O5 87.04(16) 6_657 3_546 ?
O2 Lu2 O6 105.64(15) 6_657 1_565 ?
O5 Lu2 O6 147.46(9) 3_546 1_565 ?
O2 Lu2 O7 77.36(15) 6_657 . ?
O5 Lu2 O7 64.69(15) 3_546 . ?
O6 Lu2 O7 146.67(12) 1_565 . ?
O2 Lu2 O3 141.06(15) 6_657 . ?
O5 Lu2 O3 110.64(13) 3_546 . ?
O6 Lu2 O3 78.27(11) 1_565 . ?
O7 Lu2 O3 79.61(14) . . ?
O2 Lu2 O3 147.85(15) 6_657 4_556 ?
O5 Lu2 O3 75.76(12) 3_546 4_556 ?
O6 Lu2 O3 78.17(11) 1_565 4_556 ?
O7 Lu2 O3 117.25(14) . 4_556 ?
O3 Lu2 O3 71.05(14) . 4_556 ?
O2 Lu2 O8 84.67(14) 6_657 1_565 ?
O5 Lu2 O8 94.03(12) 3_546 1_565 ?
O6 Lu2 O8 58.54(8) 1_565 1_565 ?
O7 Lu2 O8 152.50(13) . 1_565 ?
O3 Lu2 O8 126.15(11) . 1_565 ?
O3 Lu2 O8 69.98(12) 4_556 1_565 ?
O2 Lu2 O4 77.51(15) 6_657 1_565 ?
O5 Lu2 O4 153.96(12) 3_546 1_565 ?
O6 Lu2 O4 58.23(9) 1_565 1_565 ?
O7 Lu2 O4 91.27(15) . 1_565 ?
O3 Lu2 O4 72.04(12) . 1_565 ?
O3 Lu2 O4 127.17(12) 4_556 1_565 ?
O8 Lu2 O4 105.09(12) 1_565 1_565 ?
O2 Lu2 B4 78.01(16) 6_657 6_647 ?
O5 Lu2 B4 31.38(16) 3_546 6_647 ?
O6 Lu2 B4 176.35(15) 1_565 6_647 ?
O7 Lu2 B4 33.56(19) . 6_647 ?
O3 Lu2 B4 98.98(19) . 6_647 ?
O3 Lu2 B4 98.71(13) 4_556 6_647 ?
O8 Lu2 B4 122.34(18) 1_565 6_647 ?
O4 Lu2 B4 123.39(15) 1_565 6_647 ?
O2 Lu2 B2 93.81(18) 6_657 1_565 ?
O5 Lu2 B2 176.09(14) 3_546 1_565 ?
O6 Lu2 B2 28.73(11) 1_565 1_565 ?
O7 Lu2 B2 119.22(16) . 1_565 ?
O3 Lu2 B2 70.92(14) . 1_565 ?
O3 Lu2 B2 101.71(14) 4_556 1_565 ?
O8 Lu2 B2 82.26(13) 1_565 1_565 ?
O4 Lu2 B2 29.64(13) 1_565 1_565 ?
B4 Lu2 B2 152.51(16) 6_647 1_565 ?
O2 Lu2 Lu2 149.28(12) 6_657 4_556 ?
O5 Lu2 Lu2 120.27(9) 3_546 4_556 ?
O6 Lu2 Lu2 43.78(9) 1_565 4_556 ?
O7 Lu2 Lu2 125.14(10) . 4_556 ?
O3 Lu2 Lu2 46.23(9) . 4_556 ?
O3 Lu2 Lu2 46.12(8) 4_556 4_556 ?
O8 Lu2 Lu2 79.93(8) 1_565 4_556 ?
O4 Lu2 Lu2 81.06(8) 1_565 4_556 ?
B4 Lu2 Lu2 132.58(12) 6_647 4_556 ?
B2 Lu2 Lu2 57.99(12) 1_565 4_556 ?
O2 Lu2 Lu2 36.83(11) 6_657 7_655 ?
O5 Lu2 Lu2 76.62(8) 3_546 7_655 ?
O6 Lu2 Lu2 130.62(8) 1_565 7_655 ?
O7 Lu2 Lu2 40.89(10) . 7_655 ?
O3 Lu2 Lu2 111.86(9) . 7_655 ?
O3 Lu2 Lu2 151.17(9) 4_556 7_655 ?
O8 Lu2 Lu2 120.28(8) 1_565 7_655 ?
O4 Lu2 Lu2 78.49(8) 1_565 7_655 ?
B4 Lu2 Lu2 52.57(9) 6_647 7_655 ?
B2 Lu2 Lu2 106.28(11) 1_565 7_655 ?
Lu2 Lu2 Lu2 154.384(7) 4_556 7_655 ?
O5 B1 O5 109.4(5) 3_546 . ?
O5 B1 O8 108.93(19) 3_546 . ?
O5 B1 O8 112.48(19) . . ?
O5 B1 O8 112.48(19) 3_546 3_546 ?
O5 B1 O8 108.93(19) . 3_546 ?
O8 B1 O8 104.6(5) . 3_546 ?
O3 B2 O4 115.2(5) . . ?
O3 B2 O6 112.8(4) . . ?
O4 B2 O6 103.7(4) . . ?
O3 B2 O8 118.8(4) . 4_556 ?
O4 B2 O8 105.1(4) . 4_556 ?
O6 B2 O8 99.1(4) . 4_556 ?
O3 B2 Lu1 137.1(3) . 2_545 ?
O4 B2 Lu1 53.7(2) . 2_545 ?
O6 B2 Lu1 110.1(3) . 2_545 ?
O8 B2 Lu1 51.4(2) 4_556 2_545 ?
O3 B2 Lu2 135.4(3) . 1_545 ?
O4 B2 Lu2 58.4(2) . 1_545 ?
O6 B2 Lu2 45.57(19) . 1_545 ?
O8 B2 Lu2 104.5(3) 4_556 1_545 ?
Lu1 B2 Lu2 78.61(15) 2_545 1_545 ?
O1 B3 O4 114.4(4) . 2_554 ?
O1 B3 O4 114.4(4) . 8 ?
O4 B3 O4 105.3(6) 2_554 8 ?
O1 B3 O7 107.8(5) . 2_554 ?
O4 B3 O7 107.3(4) 2_554 2_554 ?
O4 B3 O7 107.3(4) 8 2_554 ?
O2 B4 O5 115.6(4) . 2 ?
O2 B4 O5 115.6(4) . 8_556 ?
O5 B4 O5 109.1(6) 2 8_556 ?
O2 B4 O7 110.2(6) . 6_567 ?
O5 B4 O7 102.4(4) 2 6_567 ?
O5 B4 O7 102.4(4) 8_556 6_567 ?
O2 B4 Lu2 134.3(3) . 4_566 ?
O5 B4 Lu2 49.4(2) 2 4_566 ?
O5 B4 Lu2 109.9(4) 8_556 4_566 ?
O7 B4 Lu2 53.4(2) 6_567 4_566 ?
O2 B4 Lu2 134.3(3) . 6_567 ?
O5 B4 Lu2 109.9(4) 2 6_567 ?
O5 B4 Lu2 49.4(2) 8_556 6_567 ?
O7 B4 Lu2 53.4(2) 6_567 6_567 ?
Lu2 B4 Lu2 74.86(18) 4_566 6_567 ?
B3 O1 Lu1 129.60(10) . 5_556 ?
B3 O1 Lu1 129.60(10) . . ?
Lu1 O1 Lu1 100.09(19) 5_556 . ?
B4 O2 Lu2 122.70(17) . 6_557 ?
B4 O2 Lu2 122.70(17) . 4_556 ?
Lu2 O2 Lu2 106.3(2) 6_557 4_556 ?
B2 O3 Lu1 114.8(3) . 2 ?
B2 O3 Lu2 115.5(3) . . ?
Lu1 O3 Lu2 109.70(15) 2 . ?
B2 O3 Lu2 116.3(3) . 4_556 ?
Lu1 O3 Lu2 109.83(14) 2 4_556 ?
Lu2 O3 Lu2 87.65(11) . 4_556 ?
B2 O4 B3 118.2(5) . 2 ?
B2 O4 Lu1 96.5(3) . 2_545 ?
B3 O4 Lu1 124.1(3) 2 2_545 ?
B2 O4 Lu2 91.9(3) . 1_545 ?
B3 O4 Lu2 120.2(3) 2 1_545 ?
Lu1 O4 Lu2 99.17(14) 2_545 1_545 ?
B1 O5 B4 122.6(4) . 2_554 ?
B1 O5 Lu2 131.1(3) . 3_546 ?
B4 O5 Lu2 99.2(3) 2_554 3_546 ?
B2 O6 B2 132.5(6) . 4_556 ?
B2 O6 Lu2 106.6(3) . 4_546 ?
B2 O6 Lu2 105.7(2) 4_556 4_546 ?
B2 O6 Lu2 105.7(2) . 1_545 ?
B2 O6 Lu2 106.6(2) 4_556 1_545 ?
Lu2 O6 Lu2 92.44(18) 4_546 1_545 ?
B4 O7 B3 126.3(5) 6_647 2 ?
B4 O7 Lu2 93.0(3) 6_647 . ?
B3 O7 Lu2 119.6(2) 2 . ?
B4 O7 Lu2 93.0(3) 6_647 7_655 ?
B3 O7 Lu2 119.6(2) 2 7_655 ?
Lu2 O7 Lu2 98.21(19) . 7_655 ?
B1 O8 B2 114.7(3) . 4_556 ?
B1 O8 Lu1 127.7(2) . 1_545 ?
B2 O8 Lu1 97.9(3) 4_556 1_545 ?
B1 O8 Lu2 111.8(3) . 1_545 ?
B2 O8 Lu2 95.5(3) 4_556 1_545 ?
Lu1 O8 Lu2 104.02(13) 1_545 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
Lu1 O1 2.206(3) 5_556 ?
Lu1 O1 2.206(3) . ?
Lu1 O3 2.322(3) 4_556 ?
Lu1 O3 2.322(3) 2_554 ?
Lu1 O8 2.359(3) 1_565 ?
Lu1 O8 2.359(3) 3_546 ?
Lu1 O4 2.423(4) 4_566 ?
Lu1 O4 2.423(4) 2_544 ?
Lu1 B2 2.989(6) 4_566 ?
Lu1 B2 2.989(6) 2_544 ?
Lu1 Lu1 3.3824(6) 5_556 ?
Lu1 Lu2 3.8118(4) 4_556 ?
Lu2 O2 2.160(3) 6_657 ?
Lu2 O5 2.189(4) 3_546 ?
Lu2 O6 2.246(3) 1_565 ?
Lu2 O7 2.287(3) . ?
Lu2 O3 2.340(3) . ?
Lu2 O3 2.344(4) 4_556 ?
Lu2 O8 2.485(3) 1_565 ?
Lu2 O4 2.582(4) 1_565 ?
Lu2 B4 2.845(6) 6_647 ?
Lu2 B2 3.028(6) 1_565 ?
Lu2 Lu2 3.2435(4) 4_556 ?
Lu2 Lu2 3.4578(5) 7_655 ?
B1 O5 1.460(5) 3_546 ?
B1 O5 1.460(5) . ?
B1 O8 1.497(5) . ?
B1 O8 1.497(5) 3_546 ?
B2 O3 1.411(7) . ?
B2 O4 1.499(7) . ?
B2 O6 1.512(6) . ?
B2 O8 1.539(7) 4_556 ?
B2 Lu1 2.989(6) 2_545 ?
B2 Lu2 3.028(6) 1_545 ?
B3 O1 1.392(9) . ?
B3 O4 1.527(6) 2_554 ?
B3 O4 1.527(6) 8 ?
B3 O7 1.575(8) 2_554 ?
B4 O2 1.393(9) . ?
B4 O5 1.501(6) 2 ?
B4 O5 1.501(6) 8_556 ?
B4 O7 1.575(9) 6_567 ?
B4 Lu2 2.845(6) 4_566 ?
B4 Lu2 2.845(6) 6_567 ?
O1 Lu1 2.206(3) 5_556 ?
O2 Lu2 2.160(3) 6_557 ?
O2 Lu2 2.160(3) 4_556 ?
O3 Lu1 2.322(3) 2 ?
O3 Lu2 2.344(4) 4_556 ?
O4 B3 1.527(6) 2 ?
O4 Lu1 2.423(4) 2_545 ?
O4 Lu2 2.582(4) 1_545 ?
O5 B4 1.501(6) 2_554 ?
O5 Lu2 2.189(4) 3_546 ?
O6 B2 1.512(6) 4_556 ?
O6 Lu2 2.246(3) 4_546 ?
O6 Lu2 2.246(3) 1_545 ?
O7 B4 1.575(9) 6_647 ?
O7 B3 1.575(8) 2 ?
O7 Lu2 2.287(3) 7_655 ?
O8 B2 1.539(7) 4_556 ?
O8 Lu1 2.359(3) 1_545 ?
O8 Lu2 2.485(3) 1_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
O4 B3 O1 Lu1 156.7(3) 2_554 . . 5_556 ?
O4 B3 O1 Lu1 35.1(8) 8 . . 5_556 ?
O7 B3 O1 Lu1 -84.1(4) 2_554 . . 5_556 ?
O4 B3 O1 Lu1 -35.1(8) 2_554 . . . ?
O4 B3 O1 Lu1 -156.7(3) 8 . . . ?
O7 B3 O1 Lu1 84.1(4) 2_554 . . . ?
O1 Lu1 O1 B3 -170.8(6) 5_556 . . . ?
O3 Lu1 O1 B3 145.3(5) 4_556 . . . ?
O3 Lu1 O1 B3 -13.7(5) 2_554 . . . ?
O8 Lu1 O1 B3 52.7(6) 1_565 . . . ?
O8 Lu1 O1 B3 -58.5(6) 3_546 . . . ?
O4 Lu1 O1 B3 104.5(5) 4_566 . . . ?
O4 Lu1 O1 B3 -90.2(5) 2_544 . . . ?
B2 Lu1 O1 B3 79.5(5) 4_566 . . . ?
B2 Lu1 O1 B3 -78.0(5) 2_544 . . . ?
Lu1 Lu1 O1 B3 -170.8(6) 5_556 . . . ?
Lu2 Lu1 O1 B3 129.6(5) 4_556 . . . ?
O1 Lu1 O1 Lu1 0.0 5_556 . . 5_556 ?
O3 Lu1 O1 Lu1 -43.9(3) 4_556 . . 5_556 ?
O3 Lu1 O1 Lu1 157.2(2) 2_554 . . 5_556 ?
O8 Lu1 O1 Lu1 -136.50(14) 1_565 . . 5_556 ?
O8 Lu1 O1 Lu1 112.32(18) 3_546 . . 5_556 ?
O4 Lu1 O1 Lu1 -84.68(17) 4_566 . . 5_556 ?
O4 Lu1 O1 Lu1 80.62(17) 2_544 . . 5_556 ?
B2 Lu1 O1 Lu1 -109.68(18) 4_566 . . 5_556 ?
B2 Lu1 O1 Lu1 92.83(19) 2_544 . . 5_556 ?
Lu2 Lu1 O1 Lu1 -59.61(18) 4_556 . . 5_556 ?
O5 B4 O2 Lu2 172.6(3) 2 . . 6_557 ?
O5 B4 O2 Lu2 43.4(8) 8_556 . . 6_557 ?
O7 B4 O2 Lu2 -72.0(3) 6_567 . . 6_557 ?
Lu2 B4 O2 Lu2 -130.1(3) 4_566 . . 6_557 ?
Lu2 B4 O2 Lu2 -14.0(8) 6_567 . . 6_557 ?
O5 B4 O2 Lu2 -43.4(8) 2 . . 4_556 ?
O5 B4 O2 Lu2 -172.6(3) 8_556 . . 4_556 ?
O7 B4 O2 Lu2 72.0(3) 6_567 . . 4_556 ?
Lu2 B4 O2 Lu2 14.0(8) 4_566 . . 4_556 ?
Lu2 B4 O2 Lu2 130.1(3) 6_567 . . 4_556 ?
O4 B2 O3 Lu1 -61.7(4) . . . 2 ?
O6 B2 O3 Lu1 179.5(2) . . . 2 ?
O8 B2 O3 Lu1 64.2(5) 4_556 . . 2 ?
Lu1 B2 O3 Lu1 1.2(6) 2_545 . . 2 ?
Lu2 B2 O3 Lu1 -131.5(3) 1_545 . . 2 ?
O4 B2 O3 Lu2 67.5(4) . . . . ?
O6 B2 O3 Lu2 -51.4(5) . . . . ?
O8 B2 O3 Lu2 -166.6(3) 4_556 . . . ?
Lu1 B2 O3 Lu2 130.4(4) 2_545 . . . ?
Lu2 B2 O3 Lu2 -2.3(6) 1_545 . . . ?
O4 B2 O3 Lu2 168.1(3) . . . 4_556 ?
O6 B2 O3 Lu2 49.3(5) . . . 4_556 ?
O8 B2 O3 Lu2 -66.0(5) 4_556 . . 4_556 ?
Lu1 B2 O3 Lu2 -128.9(4) 2_545 . . 4_556 ?
Lu2 B2 O3 Lu2 98.4(5) 1_545 . . 4_556 ?
O2 Lu2 O3 B2 -106.7(4) 6_657 . . . ?
O5 Lu2 O3 B2 5.5(4) 3_546 . . . ?
O6 Lu2 O3 B2 152.8(3) 1_565 . . . ?
O7 Lu2 O3 B2 -52.2(3) . . . . ?
O3 Lu2 O3 B2 71.5(3) 4_556 . . . ?
O8 Lu2 O3 B2 117.1(3) 1_565 . . . ?
O4 Lu2 O3 B2 -147.0(4) 1_565 . . . ?
B4 Lu2 O3 B2 -24.7(4) 6_647 . . . ?
B2 Lu2 O3 B2 -178.3(4) 1_565 . . . ?
Lu2 Lu2 O3 B2 118.2(4) 4_556 . . . ?
Lu2 Lu2 O3 B2 -77.9(3) 7_655 . . . ?
O2 Lu2 O3 Lu1 24.9(3) 6_657 . . 2 ?
O5 Lu2 O3 Lu1 137.12(14) 3_546 . . 2 ?
O6 Lu2 O3 Lu1 -75.55(13) 1_565 . . 2 ?
O7 Lu2 O3 Lu1 79.36(17) . . . 2 ?
O3 Lu2 O3 Lu1 -156.92(15) 4_556 . . 2 ?
O8 Lu2 O3 Lu1 -111.28(15) 1_565 . . 2 ?
O4 Lu2 O3 Lu1 -15.41(13) 1_565 . . 2 ?
B4 Lu2 O3 Lu1 106.89(16) 6_647 . . 2 ?
B2 Lu2 O3 Lu1 -46.69(16) 1_565 . . 2 ?
Lu2 Lu2 O3 Lu1 -110.24(18) 4_556 . . 2 ?
Lu2 Lu2 O3 Lu1 53.73(15) 7_655 . . 2 ?
O2 Lu2 O3 Lu2 135.1(2) 6_657 . . 4_556 ?
O5 Lu2 O3 Lu2 -112.64(12) 3_546 . . 4_556 ?
O6 Lu2 O3 Lu2 34.69(9) 1_565 . . 4_556 ?
O7 Lu2 O3 Lu2 -170.40(15) . . . 4_556 ?
O3 Lu2 O3 Lu2 -46.68(15) 4_556 . . 4_556 ?
O8 Lu2 O3 Lu2 -1.04(18) 1_565 . . 4_556 ?
O4 Lu2 O3 Lu2 94.83(13) 1_565 . . 4_556 ?
B4 Lu2 O3 Lu2 -142.87(13) 6_647 . . 4_556 ?
B2 Lu2 O3 Lu2 63.55(14) 1_565 . . 4_556 ?
Lu2 Lu2 O3 Lu2 163.97(5) 7_655 . . 4_556 ?
O3 B2 O4 B3 -3.3(6) . . . 2 ?
O6 B2 O4 B3 120.5(5) . . . 2 ?
O8 B2 O4 B3 -135.9(5) 4_556 . . 2 ?
Lu1 B2 O4 B3 -134.5(5) 2_545 . . 2 ?
Lu2 B2 O4 B3 126.1(4) 1_545 . . 2 ?
O3 B2 O4 Lu1 131.2(4) . . . 2_545 ?
O6 B2 O4 Lu1 -105.0(3) . . . 2_545 ?
O8 B2 O4 Lu1 -1.4(4) 4_556 . . 2_545 ?
Lu2 B2 O4 Lu1 -99.45(17) 1_545 . . 2_545 ?
O3 B2 O4 Lu2 -129.3(4) . . . 1_545 ?
O6 B2 O4 Lu2 -5.6(4) . . . 1_545 ?
O8 B2 O4 Lu2 98.0(3) 4_556 . . 1_545 ?
Lu1 B2 O4 Lu2 99.45(17) 2_545 . . 1_545 ?
O5 B1 O5 B4 -42.9(4) 3_546 . . 2_554 ?
O8 B1 O5 B4 -164.1(4) . . . 2_554 ?
O8 B1 O5 B4 80.4(6) 3_546 . . 2_554 ?
O5 B1 O5 Lu2 173.0(4) 3_546 . . 3_546 ?
O8 B1 O5 Lu2 51.8(4) . . . 3_546 ?
O8 B1 O5 Lu2 -63.6(4) 3_546 . . 3_546 ?
O3 B2 O6 B2 0.6(7) . . . 4_556 ?
O4 B2 O6 B2 -124.8(4) . . . 4_556 ?
O8 B2 O6 B2 127.2(4) 4_556 . . 4_556 ?
Lu1 B2 O6 B2 179.3(3) 2_545 . . 4_556 ?
Lu2 B2 O6 B2 -131.4(4) 1_545 . . 4_556 ?
O3 B2 O6 Lu2 -130.5(4) . . . 4_546 ?
O4 B2 O6 Lu2 104.1(4) . . . 4_546 ?
O8 B2 O6 Lu2 -3.9(4) 4_556 . . 4_546 ?
Lu1 B2 O6 Lu2 48.2(3) 2_545 . . 4_546 ?
Lu2 B2 O6 Lu2 97.5(3) 1_545 . . 4_546 ?
O3 B2 O6 Lu2 132.0(4) . . . 1_545 ?
O4 B2 O6 Lu2 6.7(5) . . . 1_545 ?
O8 B2 O6 Lu2 -101.4(3) 4_556 . . 1_545 ?
Lu1 B2 O6 Lu2 -49.3(3) 2_545 . . 1_545 ?
O2 Lu2 O7 B4 -87.3(3) 6_657 . . 6_647 ?
O5 Lu2 O7 B4 5.4(3) 3_546 . . 6_647 ?
O6 Lu2 O7 B4 173.4(3) 1_565 . . 6_647 ?
O3 Lu2 O7 B4 124.3(3) . . . 6_647 ?
O3 Lu2 O7 B4 62.1(3) 4_556 . . 6_647 ?
O8 Lu2 O7 B4 -36.9(4) 1_565 . . 6_647 ?
O4 Lu2 O7 B4 -164.2(3) 1_565 . . 6_647 ?
B2 Lu2 O7 B4 -174.6(3) 1_565 . . 6_647 ?
Lu2 Lu2 O7 B4 115.8(3) 4_556 . . 6_647 ?
Lu2 Lu2 O7 B4 -93.5(3) 7_655 . . 6_647 ?
O2 Lu2 O7 B3 137.2(4) 6_657 . . 2 ?
O5 Lu2 O7 B3 -130.1(4) 3_546 . . 2 ?
O6 Lu2 O7 B3 37.9(5) 1_565 . . 2 ?
O3 Lu2 O7 B3 -11.2(4) . . . 2 ?
O3 Lu2 O7 B3 -73.4(4) 4_556 . . 2 ?
O8 Lu2 O7 B3 -172.3(3) 1_565 . . 2 ?
O4 Lu2 O7 B3 60.3(4) 1_565 . . 2 ?
B4 Lu2 O7 B3 -135.5(5) 6_647 . . 2 ?
B2 Lu2 O7 B3 49.9(4) 1_565 . . 2 ?
Lu2 Lu2 O7 B3 -19.6(4) 4_556 . . 2 ?
Lu2 Lu2 O7 B3 131.0(5) 7_655 . . 2 ?
O2 Lu2 O7 Lu2 6.20(18) 6_657 . . 7_655 ?
O5 Lu2 O7 Lu2 98.92(19) 3_546 . . 7_655 ?
O6 Lu2 O7 Lu2 -93.1(2) 1_565 . . 7_655 ?
O3 Lu2 O7 Lu2 -142.18(18) . . . 7_655 ?
O3 Lu2 O7 Lu2 155.58(12) 4_556 . . 7_655 ?
O8 Lu2 O7 Lu2 56.6(4) 1_565 . . 7_655 ?
O4 Lu2 O7 Lu2 -70.70(16) 1_565 . . 7_655 ?
B4 Lu2 O7 Lu2 93.5(3) 6_647 . . 7_655 ?
B2 Lu2 O7 Lu2 -81.1(2) 1_565 . . 7_655 ?
Lu2 Lu2 O7 Lu2 -150.65(7) 4_556 . . 7_655 ?
O5 B1 O8 B2 53.3(5) 3_546 . . 4_556 ?
O5 B1 O8 B2 174.8(4) . . . 4_556 ?
O8 B1 O8 B2 -67.1(3) 3_546 . . 4_556 ?
O5 B1 O8 Lu1 176.4(2) 3_546 . . 1_545 ?
O5 B1 O8 Lu1 -62.1(5) . . . 1_545 ?
O8 B1 O8 Lu1 55.9(2) 3_546 . . 1_545 ?
O5 B1 O8 Lu2 -54.0(3) 3_546 . . 1_545 ?
O5 B1 O8 Lu2 67.5(4) . . . 1_545 ?
O8 B1 O8 Lu2 -174.4(2) 3_546 . . 1_545 ?
|
1100929.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-17 15:57:14 +0200 (Thu, 17 Mar 2016) $
#$Revision: 178241 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100929.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_1100929
loop_
_publ_author_name
'Uchida, Sayaka'
'Kawamoto, Ryosuke'
'Akatsuka, Takeo'
'Hikichi, Shiro'
'Mizuno, Noritaka'
_publ_contact_author_address
;
Department of Applied Chemistry,
School of Engineering,
The University of Tokyo,
7-3-1 Hongo, Bunkyo, Tokyo 113-8656
Japan
;
_publ_contact_author_email tmizuno@mail.ecc.u-tokyo.ac.jp
_publ_contact_author_fax 81(3)58417220
_publ_contact_author_name 'Prof. Noritaka Mizuno'
_publ_contact_author_phone 81(3)58417272
_publ_section_title
;
Structures and Sorption Properties of Ionic Crystals of
Macrocation-Dawson-Type Polyoxometalates with Different Charges
;
_journal_coden_ASTM CMATEX
_journal_issue 6
_journal_name_full 'Chemistry of Materials'
_journal_page_first 1367
_journal_page_last 1375
_journal_paper_doi 10.1021/cm047879s
_journal_volume 17
_journal_year 2005
_chemical_formula_sum 'C12 Cr6 N4 O100 P2 W18'
_chemical_formula_weight 5483.32
_space_group_IT_number 176
_symmetry_cell_setting hexagonal
_symmetry_Int_Tables_number 176
_symmetry_space_group_name_Hall '-P 6c'
_symmetry_space_group_name_H-M 'P 63/m'
_audit_creation_method 'CrystalStructure 3.6.0'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 2
_cell_length_a 16.009(4)
_cell_length_b 16.009(4)
_cell_length_c 21.785(9)
_cell_measurement_reflns_used 25
_cell_measurement_temperature 296.1
_cell_measurement_theta_max 15.0
_cell_measurement_theta_min 14.5
_cell_volume 4835(2)
_computing_cell_refinement 'MSC/AFC Diffractometer Control'
_computing_data_collection 'MSC/AFC Diffractometer Control'
_computing_data_reduction CrystalStructure
_computing_publication_material 'CrystalStructure 3.6.0'
_computing_structure_refinement CRYSTALS
_computing_structure_solution 'DIRDIF99 (PATTY)'
_diffrn_measured_fraction_theta_full 0.9987
_diffrn_measured_fraction_theta_max 0.9987
_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 0.046
_diffrn_reflns_limit_h_max 18
_diffrn_reflns_limit_h_min 0
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_l_max 0
_diffrn_reflns_limit_l_min -28
_diffrn_reflns_number 4220
_diffrn_reflns_theta_full 27.53
_diffrn_reflns_theta_max 27.53
_diffrn_standards_decay_% 1.50
_diffrn_standards_interval_count 0
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 22.136
_exptl_absorpt_correction_T_max 0.012
_exptl_absorpt_correction_T_min 0.005
_exptl_absorpt_correction_type psi-scan
_exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour green
_exptl_crystal_density_diffrn 3.766
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 4812.00
_exptl_crystal_size_max 0.20
_exptl_crystal_size_mid 0.20
_exptl_crystal_size_min 0.01
_refine_diff_density_max 1.76
_refine_diff_density_min -1.59
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.128
_refine_ls_hydrogen_treatment ?
_refine_ls_number_parameters 190
_refine_ls_number_reflns 2320
_refine_ls_R_factor_gt 0.0420
_refine_ls_shift/su_max 0.1240
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details 'w = 1.0'
_refine_ls_weighting_scheme unit
_refine_ls_wR_factor_ref 0.0450
_reflns_number_gt 2320
_reflns_number_total 3812
_reflns_threshold_expression F^2^>2.0\s(F^2^)
_cod_duplicate_entry 4000556
_cod_data_source_file cm047879ssi20041206_095001.cif
_cod_data_source_block '_1a'
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'psiscan' changed to 'psi-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 1100929
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +X,+Y,+Z
2 +X-Y,+X,1/2+Z
3 -Y,+X-Y,+Z
4 -X,-Y,1/2+Z
5 -X+Y,-X,+Z
6 +Y,-X+Y,1/2+Z
7 -X,-Y,-Z
8 -X+Y,-X,1/2-Z
9 +Y,-X+Y,-Z
10 +X,+Y,1/2-Z
11 +X-Y,+X,-Z
12 -Y,+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
W(1) W 0.33200(5) 0.44567(5) 0.16398(4) 0.0230(2) Uani 1.00 1 d . . .
W(2) W 0.55865(5) 0.67845(5) 0.16419(4) 0.0225(2) Uani 1.00 1 d . . .
W(3) W 0.40632(6) 0.59872(6) 0.02479(3) 0.0324(2) Uani 1.00 1 d . . .
Cr(1) Cr 0.5328(3) 0.2853(3) 0.2500 0.031(1) Uani 1.00 2 d S . .
Cr(2) Cr 0.9246(4) 0.8614(4) 0.1535(3) 0.022(1) Uiso 0.50 1 d P . .
P(1) P 0.3333 0.6667 0.1590(3) 0.020(1) Uani 1.00 3 d S . .
O(1) O 0.4573(9) 0.5514(9) 0.1782(6) 0.025(3) Uani 1.00 1 d . . .
O(2) O 0.350(1) 0.495(1) 0.0816(6) 0.034(4) Uani 1.00 1 d . . .
O(3) O 0.283(1) 0.5625(8) 0.1802(5) 0.022(3) Uani 1.00 1 d . . .
O(4) O 0.315(1) 0.431(1) 0.2500 0.023(4) Uani 1.00 2 d S . .
O(5) O 0.1958(9) 0.3801(9) 0.1502(6) 0.028(3) Uani 1.00 1 d . . .
O(6) O 0.349(1) 0.3508(9) 0.1478(8) 0.039(4) Uani 1.00 1 d . . .
O(7) O 0.5099(9) 0.661(1) 0.0813(6) 0.028(4) Uani 1.00 1 d . . .
O(8) O 0.575(1) 0.698(1) 0.2500 0.027(5) Uani 1.00 2 d S . .
O(9) O 0.6545(9) 0.6626(9) 0.1488(7) 0.032(4) Uani 1.00 1 d . . .
O(10) O 0.3333 0.6667 0.0872(8) 0.020(4) Uani 1.00 3 d S . .
O(11) O 0.454(1) 0.557(1) -0.0291(7) 0.052(5) Uani 1.00 1 d . . .
O(12) O 0.279(1) 0.555(1) -0.0083(5) 0.031(4) Uani 1.00 1 d . . .
O(13) O 0.6667 0.3333 0.2500 0.032(7) Uiso 1.00 6 d S . .
O(14) O 0.503(1) 0.188(1) 0.1872(9) 0.057(5) Uiso 1.00 1 d . . .
O(15) O 0.385(2) 0.234(2) 0.2500 0.059(7) Uiso 1.00 2 d S . .
O(16) O 0.538(1) 0.373(1) 0.1842(8) 0.054(4) Uiso 1.00 1 d . . .
O(17) O 0.842(2) 0.715(2) 0.156(1) 0.031(6) Uiso 0.50 1 d P . .
O(18) O 1.002(2) 0.846(2) 0.090(1) 0.038(7) Uiso 0.50 1 d P . .
O(19) O 1.001(2) 0.846(2) 0.220(1) 0.027(6) Uiso 0.50 1 d P . .
O(20) O 0.837(2) 0.858(2) 0.091(1) 0.036(7) Uiso 0.50 1 d P . .
O(21) O 0.834(2) 0.855(2) 0.220(1) 0.032(6) Uiso 0.50 1 d P . .
O(22) O 1.0000 1.0000 0.152(2) 0.021(8) Uiso 0.50 3 d SP . .
O(23) O 0.825(3) 0.631(3) 0.063(2) 0.19(2) Uiso 1.00 1 d . . .
N(1) N 0.321(2) 0.332(2) -0.004(1) 0.031(5) Uiso 0.67 1 d P . .
C(1) C 0.602(1) 0.452(1) 0.164(1) 0.035(4) Uiso 1.00 1 d . . .
C(2) C 1.087(4) 0.896(4) 0.2500 0.07(1) Uiso 1.00 2 d S . .
C(3) C 0.814(3) 0.914(3) 0.077(2) 0.026(8) Uiso 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_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
W(1) 0.0211(3) 0.0190(3) 0.0295(4) 0.0106(3) -0.0010(3) -0.0041(3)
W(2) 0.0193(3) 0.0213(3) 0.0274(4) 0.0104(3) 0.0038(3) -0.0008(3)
W(3) 0.0407(5) 0.0425(5) 0.0171(3) 0.0231(4) 0.0034(4) -0.0046(4)
Cr(1) 0.025(2) 0.028(2) 0.038(3) 0.011(2) 0.0000 0.0000
P(1) 0.024(2) 0.024(2) 0.010(3) 0.012(1) 0.0000 0.0000
O(1) 0.026(6) 0.024(6) 0.027(7) 0.013(5) -0.001(5) -0.010(5)
O(2) 0.040(8) 0.028(7) 0.026(7) 0.011(7) -0.002(6) -0.013(6)
O(3) 0.039(7) 0.021(6) 0.014(6) 0.020(6) -0.001(5) -0.006(5)
O(4) 0.021(9) 0.024(9) 0.013(8) 0.003(8) 0.0000 0.0000
O(5) 0.023(6) 0.026(7) 0.029(7) 0.007(5) -0.001(5) -0.000(5)
O(6) 0.028(7) 0.016(6) 0.07(1) 0.007(6) -0.004(7) -0.006(7)
O(7) 0.025(7) 0.038(8) 0.019(7) 0.014(6) 0.004(5) -0.000(6)
O(8) 0.03(1) 0.02(1) 0.03(1) 0.015(8) 0.0000 0.0000
O(9) 0.021(6) 0.022(6) 0.05(1) 0.009(5) 0.011(6) 0.010(6)
O(10) 0.026(7) 0.026(7) 0.008(9) 0.013(3) 0.0000 0.0000
O(11) 0.06(1) 0.06(1) 0.041(9) 0.039(9) 0.008(9) -0.000(9)
O(12) 0.036(8) 0.048(8) 0.012(6) 0.022(7) -0.004(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 0.003 0.002
;
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)
;
Cr Cr 0.321 0.624
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
W W -0.849 6.872
;
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)
;
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
O(2) W(1) O(1) 84.8(5) ? . . .
O(3) W(1) O(1) 83.7(6) ? . . .
O(4) W(1) O(1) 88.2(6) ? . . .
O(5) W(1) O(1) 157.4(7) ? . . .
O(6) W(1) O(1) 105.2(7) ? . . .
W(1) O(1) W(2) 153.1(9) ? . . .
O(3) W(1) O(2) 82.0(6) ? . . .
O(4) W(1) O(2) 163.4(8) ? . . .
O(5) W(1) O(2) 88.7(6) ? . . .
O(6) W(1) O(2) 96.4(8) ? . . .
W(1) O(2) W(3) 151.1(7) ? . . .
W(1) O(3) W(2) 89.8(4) ? . . 56505
W(1) O(3) P(1) 128.2(8) ? . . .
W(1) O(3) P(1) 128.1(8) ? . . 66503
W(1) O(3) P(1) 128.1(8) ? . . 56505
O(4) W(1) O(3) 82.3(8) ? . . .
O(5) W(1) O(3) 74.0(5) ? . . .
O(6) W(1) O(3) 170.8(5) ? . . .
O(5) W(1) O(4) 92.0(6) ? . . .
O(6) W(1) O(4) 100.0(9) ? . . .
W(1) O(4) W(1) 164.7(8) ? . . 55510
W(1) O(5) W(2) 122.1(7) ? . . 56505
O(6) W(1) O(5) 97.0(6) ? . . .
O(3) W(2) O(1) 84.2(6) ? 66503 . .
O(5) W(2) O(1) 157.8(7) ? 66503 . .
O(7) W(2) O(1) 85.8(5) ? . . .
O(8) W(2) O(1) 89.3(6) ? . . .
O(9) W(2) O(1) 102.9(7) ? . . .
W(2) O(3) P(1) 127.8(8) ? . 66503 .
W(2) O(3) P(1) 127.8(8) ? . 66503 66503
W(2) O(3) P(1) 127.8(8) ? . 66503 56505
W(2) O(3) W(1) 89.8(4) ? . 66503 66503
O(5) W(2) O(3) 73.8(5) ? 66503 . 66503
O(7) W(2) O(3) 81.4(6) ? . . 66503
O(8) W(2) O(3) 82.6(8) ? . . 66503
O(9) W(2) O(3) 172.6(5) ? . . 66503
W(2) O(5) W(1) 122.1(6) ? . 66503 66503
O(7) W(2) O(5) 87.5(6) ? . . 66503
O(8) W(2) O(5) 91.2(7) ? . . 66503
O(9) W(2) O(5) 98.9(6) ? . . 66503
O(8) W(2) O(7) 163.7(9) ? . . .
O(9) W(2) O(7) 97.1(7) ? . . .
W(2) O(7) W(3) 150.0(7) ? . . .
O(9) W(2) O(8) 99.2(9) ? . . .
W(2) O(8) W(2) 162.8(9) ? . . 55510
O(7) W(3) O(2) 86.7(6) ? . . .
O(10) W(3) O(2) 84.5(6) ? . . .
O(10) W(3) O(2) 84.5(6) ? 66503 . .
O(10) W(3) O(2) 84.5(6) ? 56505 . .
O(11) W(3) O(2) 102.2(8) ? . . .
O(12) W(3) O(2) 88.6(6) ? . . .
O(12) W(3) O(2) 157.4(7) ? 66503 . .
O(10) W(3) O(7) 83.7(6) ? . . .
O(10) W(3) O(7) 83.7(6) ? 66503 . .
O(10) W(3) O(7) 83.6(6) ? 56505 . .
O(11) W(3) O(7) 102.1(8) ? . . .
O(12) W(3) O(7) 156.7(7) ? . . .
O(12) W(3) O(7) 87.4(6) ? 66503 . .
W(3) O(10) P(1) 124.8(4) ? . . .
W(3) O(10) P(1) 124.8(4) ? . . 66503
W(3) O(10) P(1) 124.8(4) ? . . 56505
W(3) O(10) W(3) 90.6(5) ? . . 66503
W(3) O(10) W(3) 90.6(5) ? . . 56505
W(3) O(10) O(10) 45(75) ? . . 66503
O(10) W(3) O(10) 0.0(5) ? 66503 . .
W(3) O(10) O(10) 43(76) ? . . 56505
O(10) W(3) O(10) 0.0(5) ? 56505 . .
O(11) W(3) O(10) 171.3(8) ? . . .
O(12) W(3) O(10) 73.2(5) ? . . .
O(12) W(3) O(10) 73.2(5) ? 66503 . .
W(3) O(10) P(1) 124.9(4) ? . 66503 .
W(3) O(10) P(1) 124.8(4) ? . 66503 66503
W(3) O(10) P(1) 124.8(4) ? . 66503 56505
W(3) O(10) W(3) 90.6(5) ? . 66503 66503
W(3) O(10) W(3) 90.7(5) ? . 66503 56505
W(3) O(10) O(10) 134(75) ? . 66503 .
W(3) O(10) O(10) 89(49) ? . 66503 56505
O(10) W(3) O(10) 0.0(5) ? 56505 . 66503
O(11) W(3) O(10) 171.3(8) ? . . 66503
O(12) W(3) O(10) 73.2(5) ? . . 66503
O(12) W(3) O(10) 73.2(5) ? 66503 . 66503
W(3) O(10) P(1) 124.9(4) ? . 56505 .
W(3) O(10) P(1) 124.8(4) ? . 56505 66503
W(3) O(10) P(1) 124.8(4) ? . 56505 56505
W(3) O(10) W(3) 90.7(5) ? . 56505 66503
W(3) O(10) W(3) 90.6(5) ? . 56505 56505
W(3) O(10) O(10) 135(77) ? . 56505 .
W(3) O(10) O(10) 90(49) ? . 56505 66503
O(11) W(3) O(10) 171.3(8) ? . . 56505
O(12) W(3) O(10) 73.2(5) ? . . 56505
O(12) W(3) O(10) 73.2(5) ? 66503 . 56505
O(12) W(3) O(11) 101.2(7) ? . . .
O(12) W(3) O(11) 100.3(8) ? 66503 . .
W(3) O(12) W(3) 123.0(7) ? . . 56505
O(12) W(3) O(12) 88.3(6) ? 66503 . .
W(3) O(12) W(3) 123.0(7) ? . 66503 66503
Cr(1) O(13) Cr(1) 120.0(2) ? . . 65503
Cr(1) O(13) Cr(1) 120.0(3) ? . . 66505
Cr(1) O(13) O(13) 80.7(2) ? . . 65503
O(13) Cr(1) O(13) 0.0481(1) ? 65503 . .
Cr(1) O(13) O(13) 20.7(2) ? . . 66505
O(13) Cr(1) O(13) 0.0173(2) ? 66505 . .
O(14) Cr(1) O(13) 95.6(7) ? . . .
O(14) Cr(1) O(13) 95.6(7) ? 55510 . .
O(15) Cr(1) O(13) 179.2(9) ? . . .
O(16) Cr(1) O(13) 94.3(6) ? . . .
O(16) Cr(1) O(13) 94.3(6) ? 55510 . .
Cr(1) O(13) O(13) 80.7(2) ? . . 65503
O(13) Cr(1) O(13) 0.0481(1) ? 65503 . .
Cr(1) O(13) O(13) 20.7(2) ? . . 66505
O(13) Cr(1) O(13) 0.0173(2) ? 66505 . .
Cr(1) O(13) Cr(1) 120.0(2) ? . 65503 65503
Cr(1) O(13) Cr(1) 120.0(3) ? . 65503 66505
Cr(1) O(13) O(13) 99.2(2) ? . 65503 .
Cr(1) O(13) O(13) 39.2(2) ? . 65503 66505
O(13) Cr(1) O(13) 0.0309(1) ? 66505 . 65503
O(14) Cr(1) O(13) 95.6(7) ? . . 65503
O(14) Cr(1) O(13) 95.6(7) ? 55510 . 65503
O(15) Cr(1) O(13) 179.1(9) ? . . 65503
O(16) Cr(1) O(13) 94.3(6) ? . . 65503
O(16) Cr(1) O(13) 94.3(6) ? 55510 . 65503
Cr(1) O(13) O(13) 99.2(2) ? . 65503 .
O(13) Cr(1) O(13) 0.0481(1) ? . . 65503
Cr(1) O(13) O(13) 39.2(2) ? . 65503 66505
O(13) Cr(1) O(13) 0.0309(1) ? 66505 . 65503
Cr(1) O(13) Cr(1) 120.0(2) ? . 66505 65503
Cr(1) O(13) Cr(1) 120.0(3) ? . 66505 66505
Cr(1) O(13) O(13) 159.3(2) ? . 66505 .
Cr(1) O(13) O(13) 140.7(2) ? . 66505 65503
O(14) Cr(1) O(13) 95.6(7) ? . . 66505
O(14) Cr(1) O(13) 95.6(7) ? 55510 . 66505
O(15) Cr(1) O(13) 179.2(9) ? . . 66505
O(16) Cr(1) O(13) 94.3(6) ? . . 66505
O(16) Cr(1) O(13) 94.3(6) ? 55510 . 66505
Cr(1) O(13) O(13) 159.3(2) ? . 66505 .
O(13) Cr(1) O(13) 0.0173(2) ? . . 66505
Cr(1) O(13) O(13) 140.7(2) ? . 66505 65503
O(13) Cr(1) O(13) 0.0309(1) ? 65503 . 66505
O(14) Cr(1) O(14) 89.3(8) ? 55510 . .
O(15) Cr(1) O(14) 85.0(9) ? . . .
O(16) Cr(1) O(14) 88.1(8) ? . . .
O(16) Cr(1) O(14) 170.0(8) ? 55510 . .
Cr(1) O(14) C(1) 134(1) ? . . 65503
O(13) Cr(1) O(14) 95.6(7) ? . . .
O(13) Cr(1) O(14) 95.6(7) ? 65503 . .
O(13) Cr(1) O(14) 95.6(7) ? 66505 . .
O(15) Cr(1) O(14) 85.0(9) ? . . 55510
O(16) Cr(1) O(14) 170.0(8) ? . . 55510
O(16) Cr(1) O(14) 88.1(8) ? 55510 . 55510
Cr(1) O(14) C(1) 134(1) ? . 55510 65512
O(13) Cr(1) O(14) 95.6(7) ? . . 55510
O(13) Cr(1) O(14) 95.6(7) ? 65503 . 55510
O(13) Cr(1) O(14) 95.6(7) ? 66505 . 55510
O(16) Cr(1) O(15) 85.1(8) ? . . .
O(16) Cr(1) O(15) 85.1(8) ? 55510 . .
O(13) Cr(1) O(15) 179.2(9) ? . . .
O(13) Cr(1) O(15) 179.1(9) ? 65503 . .
O(13) Cr(1) O(15) 179.2(9) ? 66505 . .
O(16) Cr(1) O(16) 92.8(9) ? 55510 . .
Cr(1) O(16) C(1) 134(1) ? . . .
O(13) Cr(1) O(16) 94.3(6) ? . . .
O(13) Cr(1) O(16) 94.3(6) ? 65503 . .
O(13) Cr(1) O(16) 94.3(6) ? 66505 . .
Cr(1) O(16) C(1) 134(1) ? . 55510 55510
O(13) Cr(1) O(16) 94.3(6) ? . . 55510
O(13) Cr(1) O(16) 94.3(6) ? 65503 . 55510
O(13) Cr(1) O(16) 94.3(6) ? 66505 . 55510
O(18) Cr(2) O(17) 87(1) ? . . .
O(19) Cr(2) O(17) 85(1) ? . . .
O(20) Cr(2) O(17) 86(1) ? . . .
O(21) Cr(2) O(17) 83(1) ? . . .
O(22) Cr(2) O(17) 178(1) ? . . .
O(19) Cr(2) O(18) 91(1) ? . . .
O(20) Cr(2) O(18) 89(1) ? . . .
O(21) Cr(2) O(18) 170(1) ? . . .
O(22) Cr(2) O(18) 93(1) ? . . .
Cr(2) O(19) O(19) 136(2) ? . . 55510
O(20) Cr(2) O(19) 172(1) ? . . .
O(21) Cr(2) O(19) 86(1) ? . . .
O(22) Cr(2) O(19) 94(1) ? . . .
Cr(2) O(19) C(2) 141(2) ? . . .
O(21) Cr(2) O(20) 91(1) ? . . .
O(22) Cr(2) O(20) 92(1) ? . . .
Cr(2) O(20) C(3) 131(2) ? . . .
Cr(2) O(21) O(21) 136(2) ? . . 55510
O(22) Cr(2) O(21) 95(1) ? . . .
P(1) P(1) P(1) 60(58) ? . 66503 56505
P(1) P(1) P(1) 59(58) ? 56505 . 66503
P(1) P(1) O(3) 146(69) ? . 66503 .
O(3) P(1) P(1) 33(69) ? . . 66503
P(1) P(1) O(3) 88(24) ? . 66503 66503
O(3) P(1) P(1) 91(24) ? 66503 . 66503
P(1) P(1) O(10) 89(110) ? . 66503 .
O(10) P(1) P(1) 90(110) ? . . 66503
P(1) P(1) O(10) 89(110) ? . 66503 66503
O(10) P(1) P(1) 89(110) ? 66503 . 66503
P(1) P(1) O(10) 89(110) ? . 66503 56505
O(10) P(1) P(1) 89(110) ? 56505 . 66503
P(1) P(1) O(3) 35(66) ? . 66503 56505
O(3) P(1) P(1) 144(67) ? 56505 . 66503
P(1) P(1) P(1) 60(58) ? . 56505 66503
P(1) P(1) O(3) 91(24) ? . 56505 .
O(3) P(1) P(1) 88(24) ? . . 56505
P(1) P(1) O(3) 144(67) ? . 56505 66503
O(3) P(1) P(1) 35(66) ? 66503 . 56505
P(1) P(1) O(10) 89(110) ? . 56505 .
O(10) P(1) P(1) 89(110) ? . . 56505
P(1) P(1) O(10) 89(110) ? . 56505 66503
O(10) P(1) P(1) 89(110) ? 66503 . 56505
P(1) P(1) O(10) 90(110) ? . 56505 56505
O(10) P(1) P(1) 89(110) ? 56505 . 56505
P(1) P(1) O(3) 33(69) ? . 56505 56505
O(3) P(1) P(1) 146(69) ? 56505 . 56505
P(1) O(3) W(2) 127.8(9) ? . . 56505
P(1) O(3) P(1) 0.0(3) ? . . 66503
P(1) O(3) P(1) 0.1(3) ? . . 56505
O(3) P(1) O(3) 111.1(8) ? 66503 . .
O(10) P(1) O(3) 107.7(5) ? . . .
O(10) P(1) O(3) 107.6(5) ? 66503 . .
O(10) P(1) O(3) 107.7(5) ? 56505 . .
O(3) P(1) O(3) 111.2(8) ? 56505 . .
P(1) O(3) P(1) 0.1(3) ? . 66503 66503
P(1) O(3) P(1) 0.0(3) ? . 66503 56505
P(1) O(3) W(1) 128.1(9) ? . 66503 66503
O(10) P(1) O(3) 107.7(5) ? . . 66503
O(10) P(1) O(3) 107.7(5) ? 66503 . 66503
O(10) P(1) O(3) 107.6(5) ? 56505 . 66503
O(3) P(1) O(3) 111.2(8) ? 56505 . 66503
P(1) O(3) P(1) 0.0(3) ? . 56505 66503
P(1) O(3) P(1) 0.0(3) ? . 56505 56505
O(10) P(1) O(3) 107.7(5) ? . . 56505
O(10) P(1) O(3) 107.8(5) ? 66503 . 56505
O(10) P(1) O(3) 107.8(5) ? 56505 . 56505
P(1) O(3) W(1) 128.1(6) ? . 56505 56505
P(1) O(3) W(2) 127.8(6) ? . 56505 66503
P(1) O(10) P(1) 0.0586(7) ? . . 66503
P(1) O(10) P(1) 0.0586(7) ? . . 56505
P(1) O(10) W(3) 124.8(4) ? . . 66503
P(1) O(10) W(3) 124.8(4) ? . . 56505
P(1) O(10) O(10) 89(120) ? . . 66503
O(10) P(1) O(10) 0.0586(7) ? 66503 . .
P(1) O(10) O(10) 90(120) ? . . 56505
O(10) P(1) O(10) 0.0586(7) ? 56505 . .
P(1) O(10) P(1) 0.0586(7) ? . 66503 66503
P(1) O(10) P(1) 0.0586(7) ? . 66503 56505
P(1) O(10) W(3) 124.8(4) ? . 66503 66503
P(1) O(10) W(3) 124.8(4) ? . 66503 56505
P(1) O(10) O(10) 89(120) ? . 66503 .
P(1) O(10) O(10) 89(120) ? . 66503 56505
O(10) P(1) O(10) 0.0586(6) ? 56505 . 66503
P(1) O(10) P(1) 0.0586(7) ? . 56505 66503
P(1) O(10) P(1) 0.0586(7) ? . 56505 56505
P(1) O(10) W(3) 124.8(4) ? . 56505 66503
P(1) O(10) W(3) 124.8(4) ? . 56505 56505
P(1) O(10) O(10) 89(120) ? . 56505 .
P(1) O(10) O(10) 89(120) ? . 56505 66503
P(1) O(3) W(2) 127.8(9) ? 66503 . 56505
P(1) O(3) W(2) 127.8(9) ? 56505 . 56505
O(3) W(2) O(5) 73.8(5) ? . 56505 .
O(3) W(2) O(1) 84.2(5) ? . 56505 56505
O(3) W(2) O(7) 81.4(4) ? . 56505 56505
O(3) W(2) O(8) 82.6(5) ? . 56505 56505
O(3) W(2) O(9) 172.6(7) ? . 56505 56505
O(3) P(1) P(1) 144(67) ? . 66503 56505
P(1) O(3) P(1) 0.0(3) ? 56505 . 66503
O(3) P(1) O(3) 111.2(8) ? . 66503 66503
O(3) P(1) O(10) 107.8(5) ? . 66503 .
O(3) P(1) O(10) 107.7(5) ? . 66503 66503
O(3) P(1) O(10) 107.8(5) ? . 66503 56505
O(3) P(1) O(3) 111.2(8) ? . 66503 56505
O(3) P(1) P(1) 35(66) ? . 56505 66503
O(3) P(1) O(3) 111.2(8) ? . 56505 66503
O(3) P(1) O(10) 107.7(5) ? . 56505 .
O(3) P(1) O(10) 107.6(5) ? . 56505 66503
O(3) P(1) O(10) 107.7(5) ? . 56505 56505
O(3) P(1) O(3) 111.1(8) ? . 56505 56505
O(4) W(1) O(1) 88.2(6) ? . 55510 55510
O(4) W(1) O(3) 82.3(8) ? . 55510 55510
O(4) W(1) O(5) 92.0(6) ? . 55510 55510
O(4) W(1) O(6) 100.0(9) ? . 55510 55510
O(5) W(2) O(1) 157.8(4) ? . 56505 56505
O(5) W(2) O(7) 87.5(7) ? . 56505 56505
O(5) W(2) O(8) 91.2(9) ? . 56505 56505
O(5) W(2) O(9) 98.9(7) ? . 56505 56505
O(8) W(2) O(1) 89.3(6) ? . 55510 55510
O(8) W(2) O(3) 82.6(8) ? . 55510 66512
O(8) W(2) O(5) 91.2(7) ? . 55510 66512
O(8) W(2) O(9) 99.2(9) ? . 55510 55510
P(1) O(10) W(3) 124.9(4) ? 66503 . 66503
P(1) O(10) W(3) 124.8(4) ? 56505 . 66503
W(3) O(10) W(3) 90.7(5) ? 56505 . 66503
O(10) W(3) O(10) 0.0(5) ? . 66503 66503
O(10) O(10) W(3) 135(77) ? 66503 . 66503
O(10) W(3) O(10) 0.0(5) ? . 66503 56505
O(10) O(10) W(3) 90(49) ? 56505 . 66503
O(10) W(3) O(12) 73.2(4) ? . 66503 66503
O(10) W(3) O(12) 73.2(5) ? . 66503 56505
O(10) W(3) O(2) 84.5(5) ? . 66503 66503
O(10) W(3) O(7) 83.6(5) ? . 66503 66503
P(1) O(10) W(3) 124.8(4) ? 66503 . 56505
P(1) O(10) W(3) 124.9(4) ? 56505 . 56505
O(10) W(3) O(10) 0.0(5) ? . 56505 66503
O(10) O(10) W(3) 89(49) ? 66503 . 56505
O(10) W(3) O(10) 0.0(5) ? . 56505 56505
O(10) O(10) W(3) 134(75) ? 56505 . 56505
O(10) W(3) O(12) 73.2(4) ? . 56505 .
O(10) W(3) O(12) 73.2(5) ? . 56505 56505
O(10) W(3) O(2) 84.5(5) ? . 56505 56505
O(10) W(3) O(7) 83.7(4) ? . 56505 56505
O(10) W(3) O(11) 171.3(7) ? . 56505 56505
O(10) P(1) P(1) 89(110) ? . 66503 56505
P(1) O(10) P(1) 0.0586(7) ? 56505 . 66503
O(10) P(1) O(3) 107.7(5) ? . 66503 66503
O(10) P(1) O(10) 0.0586(7) ? . 66503 66503
O(10) O(10) P(1) 89(120) ? 66503 . 66503
O(10) P(1) O(10) 0.0586(6) ? . 66503 56505
O(10) O(10) P(1) 89(120) ? 56505 . 66503
O(10) P(1) O(3) 107.6(5) ? . 66503 56505
O(10) P(1) P(1) 89(110) ? . 56505 66503
O(10) P(1) O(3) 107.8(5) ? . 56505 66503
O(10) P(1) O(10) 0.0586(6) ? . 56505 66503
O(10) O(10) P(1) 89(120) ? 66503 . 56505
O(10) P(1) O(10) 0.0586(7) ? . 56505 56505
O(10) O(10) P(1) 89(120) ? 56505 . 56505
O(10) P(1) O(3) 107.6(5) ? . 56505 56505
O(10) O(10) P(1) 90(120) ? . 66503 66503
O(10) O(10) P(1) 89(120) ? . 66503 56505
O(10) O(10) W(3) 43(76) ? . 66503 66503
O(10) O(10) W(3) 90(49) ? . 66503 56505
O(10) O(10) O(10) 60(67) ? . 66503 56505
O(10) O(10) O(10) 59(67) ? 56505 . 66503
O(10) O(10) P(1) 89(120) ? . 56505 66503
O(10) O(10) P(1) 89(120) ? . 56505 56505
O(10) O(10) W(3) 89(49) ? . 56505 66503
O(10) O(10) W(3) 45(75) ? . 56505 56505
O(10) O(10) O(10) 60(67) ? . 56505 66503
O(12) W(3) O(10) 73.2(4) ? . 56505 66503
O(12) W(3) O(10) 73.2(4) ? . 56505 56505
O(12) W(3) O(12) 88.3(7) ? . 56505 56505
O(12) W(3) O(2) 157.4(6) ? . 56505 56505
O(12) W(3) O(7) 87.4(7) ? . 56505 56505
O(12) W(3) O(11) 100.3(8) ? . 56505 56505
Cr(1) O(13) Cr(1) 120.0(2) ? 66505 . 65503
O(13) Cr(1) O(13) 0.0173(1) ? . 65503 65503
O(13) O(13) Cr(1) 159.3(1) ? 65503 . 65503
O(13) Cr(1) O(13) 0.0309(1) ? . 65503 66505
O(13) O(13) Cr(1) 140.7(1) ? 66505 . 65503
O(13) Cr(1) O(16) 94.3(7) ? . 65503 65503
O(13) Cr(1) O(16) 94.3(7) ? . 65503 65512
O(13) Cr(1) O(13) 0.0173(1) ? . 65503 65503
O(13) O(13) Cr(1) 159.3(1) ? 65503 . 65503
O(13) Cr(1) O(13) 0.0309(1) ? . 65503 66505
O(13) O(13) Cr(1) 140.7(1) ? 66505 . 65503
O(13) Cr(1) O(14) 95.6(8) ? . 65503 65503
O(13) Cr(1) O(14) 95.6(8) ? . 65503 65512
O(13) Cr(1) O(13) 0.0309(2) ? . 66505 65503
O(13) O(13) Cr(1) 39.2(2) ? 65503 . 66505
O(13) Cr(1) O(13) 0.0481(1) ? . 66505 66505
O(13) O(13) Cr(1) 99.2(2) ? 66505 . 66505
O(13) Cr(1) O(14) 95.6(5) ? . 66505 66505
O(13) Cr(1) O(14) 95.6(5) ? . 66505 66508
O(13) Cr(1) O(13) 0.0309(2) ? . 66505 65503
O(13) O(13) Cr(1) 39.2(2) ? 65503 . 66505
O(13) Cr(1) O(13) 0.0481(1) ? . 66505 66505
O(13) O(13) Cr(1) 99.2(2) ? 66505 . 66505
O(13) Cr(1) O(16) 94.3(5) ? . 66505 66505
O(13) Cr(1) O(16) 94.3(5) ? . 66505 66508
O(13) Cr(1) O(15) 179(1) ? . 66505 66505
O(13) O(13) Cr(1) 99.2(2) ? . 65503 .
Cr(1) O(13) O(13) 80.7(2) ? . . 65503
O(13) O(13) Cr(1) 20.7(1) ? . 65503 65503
Cr(1) O(13) O(13) 159.3(1) ? 65503 . 65503
O(13) O(13) Cr(1) 140.7(2) ? . 65503 66505
Cr(1) O(13) O(13) 39.2(2) ? 66505 . 65503
O(13) O(13) O(13) 60(111) ? . 65503 66505
O(13) O(13) O(13) 59(162) ? 66505 . 65503
O(13) O(13) Cr(1) 159.3(2) ? . 66505 .
Cr(1) O(13) O(13) 20.7(2) ? . . 66505
O(13) O(13) Cr(1) 39.2(1) ? . 66505 65503
Cr(1) O(13) O(13) 140.7(1) ? 65503 . 66505
O(13) O(13) Cr(1) 80.7(2) ? . 66505 66505
Cr(1) O(13) O(13) 99.2(2) ? 66505 . 66505
O(13) O(13) O(13) 60(110) ? . 66505 65503
O(14) C(1) O(16) 122(2) ? . 65503 65503
O(16) C(1) O(14) 122(2) ? . . 66505
O(19) O(19) C(2) 61(1) ? . 55510 .
C(2) O(19) O(19) 61(1) ? . . 55510
O(19) O(19) Cr(2) 136(2) ? . 55510 55510
O(19) C(2) O(19) 57(2) ? . . 55510
O(21) O(21) Cr(2) 136(2) ? . 55510 55510
C(1) O(14) Cr(1) 134(1) ? . 66505 66505
C(2) O(19) Cr(2) 141(2) ? . 55510 55510
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
W(1) O(1) 1.89(1) ? . .
W(1) O(2) 1.92(1) ? . .
W(1) O(3) 2.39(2) ? . .
W(1) O(4) 1.891(2) ? . .
W(1) O(5) 1.91(1) ? . .
W(1) O(6) 1.71(2) ? . .
W(2) O(1) 1.89(1) ? . .
W(2) O(3) 2.38(2) ? . 66503
W(2) O(5) 1.93(1) ? . 66503
W(2) O(7) 1.93(1) ? . .
W(2) O(8) 1.891(3) ? . .
W(2) O(9) 1.71(2) ? . .
W(3) O(2) 1.90(1) ? . .
W(3) O(7) 1.90(1) ? . .
W(3) O(10) 2.38(1) ? . .
W(3) O(10) 2.38(1) ? . 66503
W(3) O(10) 2.38(1) ? . 56505
W(3) O(11) 1.70(2) ? . .
W(3) O(12) 1.93(2) ? . .
W(3) O(12) 1.93(2) ? . 66503
Cr(1) O(13) 1.881(5) ? . .
Cr(1) O(13) 1.881(5) ? . 65503
Cr(1) O(13) 1.880(5) ? . 66505
Cr(1) O(14) 1.95(2) ? . .
Cr(1) O(14) 1.95(2) ? . 55510
Cr(1) O(15) 2.08(3) ? . .
Cr(1) O(16) 1.98(2) ? . .
Cr(1) O(16) 1.98(2) ? . 55510
Cr(2) O(17) 2.03(2) ? . .
Cr(2) O(18) 1.95(4) ? . .
Cr(2) O(19) 1.99(3) ? . .
Cr(2) O(20) 1.94(3) ? . .
Cr(2) O(21) 2.01(3) ? . .
Cr(2) O(22) 1.924(5) ? . .
P(1) P(1) 0.002(8) ? . 66503
P(1) P(1) 0.002(8) ? . 56505
P(1) O(3) 1.52(1) ? . .
P(1) O(3) 1.52(1) ? . 66503
P(1) O(3) 1.51(2) ? . 56505
P(1) O(10) 1.57(2) ? . .
P(1) O(10) 1.57(2) ? . 66503
P(1) O(10) 1.57(2) ? . 56505
O(3) W(2) 2.38(1) ? . 56505
O(3) P(1) 1.51(1) ? . 66503
O(3) P(1) 1.52(1) ? . 56505
O(4) W(1) 1.891(2) ? . 55510
O(5) W(2) 1.93(2) ? . 56505
O(8) W(2) 1.891(3) ? . 55510
O(10) W(3) 2.38(1) ? . 66503
O(10) W(3) 2.38(1) ? . 56505
O(10) P(1) 1.57(2) ? . 66503
O(10) P(1) 1.57(2) ? . 56505
O(10) O(10) 0.00(2) ? . 66503
O(10) O(10) 0.00(2) ? . 56505
O(12) W(3) 1.93(2) ? . 56505
O(13) Cr(1) 1.880(6) ? . 65503
O(13) Cr(1) 1.881(4) ? . 66505
O(13) O(13) 0.0(3) ? . 65503
O(13) O(13) 0.0(3) ? . 66505
O(13) O(13) 0.0(3) ? . 66508
O(13) O(13) 0.0(3) ? . 65512
O(14) C(1) 1.25(4) ? . 65503
O(16) C(1) 1.24(2) ? . .
O(19) O(19) 1.32(4) ? . 55510
O(19) C(2) 1.36(5) ? . .
O(20) C(3) 1.18(7) ? . .
O(21) O(21) 1.32(4) ? . 55510
C(1) O(14) 1.25(3) ? . 66505
C(2) O(19) 1.36(5) ? . 55510
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
W(1) W(2) 3.363(1) ? . 56505
W(1) P(1) 3.5298(9) ? . .
W(1) P(1) 3.5282(9) ? . 66503
W(1) P(1) 3.5290(9) ? . 56505
W(2) W(1) 3.363(1) ? . 66503
W(2) P(1) 3.5192(9) ? . .
W(2) P(1) 3.5184(9) ? . 66503
W(2) P(1) 3.5176(9) ? . 56505
W(3) W(3) 3.385(2) ? . 66503
W(3) W(3) 3.385(2) ? . 56505
W(3) P(1) 3.518(6) ? . .
W(3) P(1) 3.517(6) ? . 66503
W(3) P(1) 3.517(6) ? . 56505
W(3) O(12) 3.58(2) ? . 56505
Cr(1) Cr(1) 3.257(9) ? . 65503
Cr(1) Cr(1) 3.257(5) ? . 66505
Cr(1) O(14) 3.32(2) ? . 66505
Cr(1) O(14) 3.32(2) ? . 66508
Cr(1) O(16) 3.31(2) ? . 65503
Cr(1) O(16) 3.31(2) ? . 65512
Cr(1) C(1) 2.98(2) ? . .
Cr(1) C(1) 2.96(3) ? . 65503
Cr(1) C(1) 2.98(2) ? . 55510
Cr(1) C(1) 2.96(3) ? . 65512
Cr(2) O(19) 3.08(3) ? . 55510
Cr(2) O(21) 3.09(3) ? . 55510
Cr(2) C(2) 3.17(4) ? . .
Cr(2) C(3) 2.86(5) ? . .
P(1) W(1) 3.5290(6) ? . 66503
P(1) W(1) 3.5282(9) ? . 56505
P(1) W(2) 3.5176(9) ? . 66503
P(1) W(2) 3.5184(6) ? . 56505
P(1) W(3) 3.517(6) ? . 66503
P(1) W(3) 3.517(6) ? . 56505
P(1) O(1) 3.35(2) ? . .
P(1) O(1) 3.34(1) ? . 66503
P(1) O(1) 3.34(1) ? . 56505
P(1) O(2) 3.35(2) ? . .
P(1) O(2) 3.35(1) ? . 66503
P(1) O(2) 3.35(2) ? . 56505
P(1) O(7) 3.34(2) ? . .
P(1) O(7) 3.33(2) ? . 66503
P(1) O(7) 3.34(1) ? . 56505
O(1) P(1) 3.34(2) ? . 66503
O(1) P(1) 3.34(2) ? . 56505
O(1) O(1) 3.13(2) ? . 55510
O(1) O(2) 2.57(2) ? . .
O(1) O(3) 2.88(2) ? . .
O(1) O(3) 2.88(2) ? . 66503
O(1) O(4) 2.63(2) ? . .
O(1) O(6) 2.86(2) ? . .
O(1) O(7) 2.60(2) ? . .
O(1) O(8) 2.66(2) ? . .
O(1) O(9) 2.81(2) ? . .
O(1) C(1) 3.42(3) ? . .
O(2) P(1) 3.35(2) ? . 66503
O(2) P(1) 3.35(2) ? . 56505
O(2) O(3) 2.85(2) ? . .
O(2) O(5) 2.68(2) ? . .
O(2) O(6) 2.71(2) ? . .
O(2) O(7) 2.61(2) ? . .
O(2) O(7) 3.15(2) ? . 56505
O(2) O(10) 2.90(2) ? . .
O(2) O(10) 2.90(2) ? . 66503
O(2) O(10) 2.90(2) ? . 56505
O(2) O(11) 2.81(2) ? . .
O(2) O(12) 2.67(2) ? . .
O(2) N(1) 3.05(3) ? . .
O(3) O(1) 2.88(2) ? . 56505
O(3) O(3) 2.50(1) ? . 66503
O(3) O(3) 2.50(2) ? . 56505
O(3) O(3) 3.04(2) ? . 55510
O(3) O(4) 2.84(2) ? . .
O(3) O(5) 2.61(2) ? . .
O(3) O(7) 2.83(2) ? . 56505
O(3) O(8) 2.84(2) ? . 56505
O(3) O(10) 2.49(2) ? . .
O(3) O(10) 2.49(2) ? . 66503
O(3) O(10) 2.49(2) ? . 56505
O(4) O(1) 2.63(2) ? . 55510
O(4) O(3) 2.84(2) ? . 55510
O(4) O(5) 2.74(2) ? . .
O(4) O(5) 2.74(2) ? . 55510
O(4) O(6) 2.76(2) ? . .
O(4) O(6) 2.76(2) ? . 55510
O(4) O(8) 3.03(3) ? . 56505
O(5) O(6) 2.71(2) ? . .
O(5) O(7) 2.67(2) ? . 56505
O(5) O(8) 2.73(2) ? . 56505
O(5) O(9) 2.77(2) ? . 56505
O(5) O(18) 3.55(4) ? . 65503
O(5) O(20) 3.45(3) ? . 56505
O(5) O(21) 3.51(3) ? . 56505
O(5) C(2) 3.41(4) ? . 65503
O(5) C(3) 3.13(4) ? . 56505
O(6) O(15) 3.14(3) ? . .
O(6) O(16) 2.98(3) ? . .
O(6) O(17) 3.20(3) ? . 65503
O(6) O(18) 3.36(3) ? . 65503
O(6) O(19) 3.50(3) ? . 65503
O(6) O(23) 3.26(6) ? . 65503
O(6) N(1) 3.33(3) ? . .
O(6) C(1) 3.55(3) ? . .
O(7) P(1) 3.34(2) ? . 66503
O(7) P(1) 3.33(2) ? . 56505
O(7) O(2) 3.15(2) ? . 66503
O(7) O(3) 2.83(2) ? . 66503
O(7) O(5) 2.67(2) ? . 66503
O(7) O(9) 2.73(2) ? . .
O(7) O(10) 2.88(2) ? . .
O(7) O(10) 2.88(2) ? . 66503
O(7) O(10) 2.88(2) ? . 56505
O(7) O(11) 2.80(2) ? . .
O(7) O(12) 2.64(2) ? . 66503
O(7) N(1) 3.13(3) ? . 66507
O(8) O(1) 2.66(2) ? . 55510
O(8) O(3) 2.84(3) ? . 66503
O(8) O(3) 2.84(3) ? . 66512
O(8) O(4) 3.03(3) ? . 66503
O(8) O(5) 2.73(2) ? . 66503
O(8) O(5) 2.73(2) ? . 66512
O(8) O(9) 2.74(2) ? . .
O(8) O(9) 2.74(2) ? . 55510
O(9) O(5) 2.77(2) ? . 66503
O(9) O(14) 3.05(3) ? . 66505
O(9) O(17) 2.69(3) ? . .
O(9) O(20) 3.28(3) ? . .
O(9) O(21) 3.36(3) ? . .
O(9) O(23) 3.54(6) ? . .
O(9) N(1) 3.18(3) ? . 66507
O(9) C(1) 3.06(3) ? . .
O(10) O(2) 2.90(1) ? . 66503
O(10) O(2) 2.90(2) ? . 56505
O(10) O(3) 2.49(2) ? . 66503
O(10) O(3) 2.49(2) ? . 56505
O(10) O(7) 2.88(2) ? . 66503
O(10) O(7) 2.88(1) ? . 56505
O(10) O(12) 2.59(2) ? . .
O(10) O(12) 2.59(2) ? . 66503
O(10) O(12) 2.59(2) ? . 56505
O(11) O(11) 3.14(3) ? . 66507
O(11) O(12) 2.81(3) ? . .
O(11) O(12) 2.79(3) ? . 66503
O(11) O(16) 3.54(2) ? . 66507
O(11) N(1) 3.18(3) ? . .
O(11) N(1) 3.20(3) ? . 66507
O(11) C(1) 3.06(3) ? . 66507
O(12) W(3) 3.58(1) ? . 66503
O(12) O(7) 2.64(2) ? . 56505
O(12) O(10) 2.59(2) ? . 66503
O(12) O(10) 2.59(2) ? . 56505
O(12) O(11) 2.79(3) ? . 56505
O(12) O(12) 2.68(2) ? . 66503
O(12) O(12) 2.68(3) ? . 56505
O(12) O(23) 2.85(4) ? . 66507
O(13) O(14) 2.84(2) ? . .
O(13) O(14) 2.83(2) ? . 65503
O(13) O(14) 2.84(2) ? . 66505
O(13) O(14) 2.84(2) ? . 66508
O(13) O(14) 2.84(2) ? . 55510
O(13) O(14) 2.83(2) ? . 65512
O(13) O(16) 2.83(2) ? . .
O(13) O(16) 2.83(2) ? . 65503
O(13) O(16) 2.83(2) ? . 66505
O(13) O(16) 2.83(2) ? . 66508
O(13) O(16) 2.83(2) ? . 55510
O(13) O(16) 2.83(2) ? . 65512
O(13) C(1) 3.18(3) ? . .
O(13) C(1) 3.18(2) ? . 65503
O(13) C(1) 3.18(2) ? . 66505
O(13) C(1) 3.18(2) ? . 66508
O(13) C(1) 3.18(3) ? . 55510
O(13) C(1) 3.18(2) ? . 65512
O(14) Cr(1) 3.32(2) ? . 65503
O(14) O(9) 3.05(2) ? . 65503
O(14) O(13) 2.84(2) ? . 65503
O(14) O(13) 2.83(2) ? . 66505
O(14) O(14) 2.74(3) ? . 55510
O(14) O(15) 2.72(4) ? . .
O(14) O(16) 2.73(3) ? . .
O(14) O(16) 2.19(3) ? . 65503
O(14) O(16) 3.55(3) ? . 65512
O(14) O(17) 3.20(4) ? . 65503
O(14) O(23) 3.48(5) ? . 65503
O(14) C(1) 3.43(3) ? . 65512
O(15) O(6) 3.14(3) ? . 55510
O(15) O(14) 2.72(4) ? . 55510
O(15) O(16) 2.75(2) ? . .
O(15) O(16) 2.75(2) ? . 55510
O(15) O(17) 2.63(3) ? . 65503
O(15) O(17) 2.63(3) ? . 65512
O(15) O(19) 3.33(4) ? . 65503
O(15) O(19) 3.33(4) ? . 65512
O(16) Cr(1) 3.31(2) ? . 66505
O(16) O(11) 3.54(2) ? . 66507
O(16) O(13) 2.83(2) ? . 65503
O(16) O(13) 2.83(2) ? . 66505
O(16) O(14) 2.19(2) ? . 66505
O(16) O(14) 3.55(2) ? . 66508
O(16) O(16) 2.87(2) ? . 55510
O(16) C(1) 3.50(3) ? . 55510
O(17) O(6) 3.20(4) ? . 66505
O(17) O(14) 3.20(3) ? . 66505
O(17) O(15) 2.63(4) ? . 66505
O(17) O(18) 2.76(4) ? . .
O(17) O(19) 2.73(3) ? . .
O(17) O(19) 3.58(3) ? . 55510
O(17) O(20) 2.73(5) ? . .
O(17) O(21) 2.68(5) ? . .
O(17) O(21) 3.55(4) ? . 55510
O(17) O(23) 2.37(5) ? . .
O(18) O(5) 3.55(4) ? . 66505
O(18) O(6) 3.36(4) ? . 66505
O(18) O(19) 2.83(4) ? . .
O(18) O(20) 2.74(6) ? . .
O(18) O(22) 2.83(4) ? . .
O(18) O(23) 3.23(4) ? . .
O(18) N(1) 3.43(5) ? . 66505
O(19) Cr(2) 3.08(3) ? . 55510
O(19) O(6) 3.50(4) ? . 66505
O(19) O(15) 3.33(3) ? . 66505
O(19) O(17) 3.58(3) ? . 55510
O(19) O(21) 2.74(5) ? . .
O(19) O(21) 3.04(5) ? . 55510
O(19) O(22) 2.88(4) ? . .
O(20) O(5) 3.45(4) ? . 66503
O(20) O(21) 2.81(4) ? . .
O(20) O(22) 2.80(3) ? . .
O(20) O(23) 3.58(7) ? . .
O(20) N(1) 3.39(4) ? . 66507
O(21) Cr(2) 3.09(3) ? . 55510
O(21) O(5) 3.51(4) ? . 66503
O(21) O(17) 3.55(4) ? . 55510
O(21) O(19) 3.04(5) ? . 55510
O(21) O(22) 2.91(3) ? . .
O(21) C(3) 3.32(5) ? . .
O(22) C(2) 3.40(6) ? . .
O(22) C(3) 3.06(4) ? . .
O(23) O(6) 3.26(5) ? . 66505
O(23) O(12) 2.85(4) ? . 66507
O(23) O(14) 3.48(4) ? . 66505
O(23) N(1) 3.05(6) ? . 66505
O(23) N(1) 2.99(7) ? . 66507
N(1) O(7) 3.13(3) ? . 66507
N(1) O(9) 3.18(3) ? . 66507
N(1) O(11) 3.20(3) ? . 66507
N(1) O(18) 3.43(4) ? . 65503
N(1) O(20) 3.39(4) ? . 66507
N(1) O(23) 3.05(7) ? . 65503
N(1) O(23) 2.99(7) ? . 66507
N(1) C(3) 3.58(4) ? . 56505
C(1) Cr(1) 2.96(2) ? . 66505
C(1) O(11) 3.06(3) ? . 66507
C(1) O(13) 3.18(3) ? . 65503
C(1) O(13) 3.18(3) ? . 66505
C(1) O(14) 3.43(3) ? . 66508
C(1) O(16) 3.50(3) ? . 55510
C(2) Cr(2) 3.17(4) ? . 55510
C(2) O(5) 3.41(6) ? . 66505
C(2) O(5) 3.41(6) ? . 66508
C(2) O(22) 3.40(6) ? . 55510
C(3) O(5) 3.13(4) ? . 66503
C(3) N(1) 3.58(6) ? . 66503
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
O(2) W(1) O(1) W(2) 31(1) ? . . . .
O(3) W(1) O(1) W(2) -51(1) ? . . . .
O(4) W(1) O(1) W(2) -133(1) ? . . . .
O(5) W(1) O(1) W(2) -42(2) ? . . . .
O(6) W(1) O(1) W(2) 126(1) ? . . . .
O(1) W(1) O(2) W(3) -28(2) ? . . . .
O(3) W(1) O(2) W(3) 55(2) ? . . . .
O(4) W(1) O(2) W(3) 36(3) ? . . . .
O(5) W(1) O(2) W(3) 129(2) ? . . . .
O(6) W(1) O(2) W(3) -133(2) ? . . . .
O(1) W(1) O(3) P(1) 39(1) ? . . . .
O(2) W(1) O(3) P(1) -46(1) ? . . . .
O(4) W(1) O(3) P(1) 128(1) ? . . . .
O(5) W(1) O(3) P(1) -137(1) ? . . . .
O(7) W(2) O(1) W(1) -30(1) ? . . . .
O(8) W(2) O(1) W(1) 133(1) ? . . . .
O(9) W(2) O(1) W(1) -126(1) ? . . . .
O(1) W(2) O(7) W(3) 24(2) ? . . . .
O(8) W(2) O(7) W(3) -48(3) ? . . . .
O(9) W(2) O(7) W(3) 127(2) ? . . . .
O(7) W(3) O(2) W(1) 28(2) ? . . . .
O(10) W(3) O(2) W(1) -55(2) ? . . . .
O(11) W(3) O(2) W(1) 130(2) ? . . . .
O(12) W(3) O(2) W(1) -128(2) ? . . . .
O(2) W(3) O(7) W(2) -24(2) ? . . . .
O(10) W(3) O(7) W(2) 59(2) ? . . . .
O(11) W(3) O(7) W(2) -126(1) ? . . . .
O(12) W(3) O(7) W(2) 53(2) ? . . . .
O(2) W(3) O(10) P(1) 43(2) ? . . . .
O(7) W(3) O(10) P(1) -44(2) ? . . . .
O(12) W(3) O(10) P(1) 133(2) ? . . . .
O(13) Cr(1) O(16) C(1) -22(9) ? . . . .
O(14) Cr(1) O(16) C(1) -118(3) ? . . . .
O(15) Cr(1) O(16) C(1) 156(4) ? . . . .
O(17) Cr(2) O(19) C(2) 166(10) ? . . . .
O(18) Cr(2) O(19) C(2) 78(10) ? . . . .
O(21) Cr(2) O(19) C(2) -110(10) ? . . . .
O(22) Cr(2) O(19) C(2) -15(10) ? . . . .
O(17) Cr(2) O(20) C(3) 151(3) ? . . . .
O(18) Cr(2) O(20) C(3) -120(3) ? . . . .
O(21) Cr(2) O(20) C(3) 68(3) ? . . . .
O(22) Cr(2) O(20) C(3) -27(3) ? . . . .
O(10) P(1) O(3) W(1) 63(4) ? . . . .
O(3) P(1) O(10) W(3) -59(5) ? . . . .
|
1100930.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-17 15:49:45 +0200 (Thu, 17 Mar 2016) $
#$Revision: 178240 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100930.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_1100930
loop_
_publ_author_name
'Tang, Liqiu'
'Dadachov, Mike S.'
'Zou, Xiaodong'
_publ_section_title
;
SU-12: A Silicon-Substituted ASU-16 with Circular 24-Rings and Templated
by a Monoamine
;
_journal_coden_ASTM CMATEX
_journal_issue 10
_journal_name_full 'Chemistry of Materials'
_journal_page_first 2530
_journal_page_last 2536
_journal_paper_doi 10.1021/cm049373f
_journal_volume 17
_journal_year 2005
_chemical_formula_sum 'C4.5 H15 F2 Ge6.44 N1.5 O17 Si0.56'
_chemical_formula_weight 883.28
_space_group_IT_number 121
_symmetry_cell_setting tetragonal
_symmetry_space_group_name_Hall 'I -4 2'
_symmetry_space_group_name_H-M 'I -4 2 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 90.00
_cell_formula_units_Z 16
_cell_length_a 27.646(2)
_cell_length_b 27.646(2)
_cell_length_c 17.0885(14)
_cell_measurement_temperature 293(2)
_cell_volume 13060.8(18)
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 293(2)
_diffrn_measured_fraction_theta_full 0.998
_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 0.1026
_diffrn_reflns_av_sigmaI/netI 0.0503
_diffrn_reflns_limit_h_max 32
_diffrn_reflns_limit_h_min -32
_diffrn_reflns_limit_k_max 32
_diffrn_reflns_limit_k_min -31
_diffrn_reflns_limit_l_max 20
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 47555
_diffrn_reflns_theta_full 25.02
_diffrn_reflns_theta_max 25.02
_diffrn_reflns_theta_min 2.03
_exptl_absorpt_coefficient_mu 5.933
_exptl_crystal_density_diffrn 1.797
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 6726
_refine_diff_density_max 1.580
_refine_diff_density_min -0.849
_refine_diff_density_rms 0.210
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack 0.01(3)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.078
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 327
_refine_ls_number_reflns 5977
_refine_ls_number_restraints 12
_refine_ls_restrained_S_all 1.077
_refine_ls_R_factor_all 0.0570
_refine_ls_R_factor_gt 0.0512
_refine_ls_shift/su_max 0.171
_refine_ls_shift/su_mean 0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0975P)^2^+100.2118P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1430
_refine_ls_wR_factor_ref 0.1487
_reflns_number_gt 5471
_reflns_number_total 5977
_reflns_threshold_expression >2sigma(I)
_cod_duplicate_entry 4000498
_cod_data_source_file cm049373fsi20040418_051707.cif
_cod_data_source_block SU-12
_cod_original_formula_sum 'C4.50 H15 F2 Ge6.44 N1.50 O17 Si0.56'
_cod_database_code 1100930
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x, y, -z'
'x, -y, -z'
'-y, -x, z'
'y, x, z'
'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+1/2, 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'
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
Ge1 Ge 0.35377(4) 0.19211(4) 0.25829(6) 0.0166(3) Uani 1 1 d . . .
Ge2 Ge 0.36200(4) 0.05832(4) 0.28091(6) 0.0163(3) Uani 1 1 d . . .
Ge3 Ge 0.29027(4) 0.09192(4) 0.17012(6) 0.0192(3) Uani 1 1 d . . .
Ge4 Ge 0.32048(4) 0.13247(4) 0.39945(6) 0.0170(5) Uani 0.864(7) 1 d P . .
Si4 Si 0.32048(4) 0.13247(4) 0.39945(6) 0.0170(5) Uani 0.14 1 d P . .
Ge5 Ge 0.43849(4) 0.12649(4) 0.20203(6) 0.0166(4) Uani 0.892(7) 1 d P . .
Si5 Si 0.43849(4) 0.12649(4) 0.20203(6) 0.0166(4) Uani 0.11 1 d P . .
Ge6 Ge 0.36095(4) 0.15980(5) 0.08770(6) 0.0183(5) Uani 0.841(7) 1 d P . .
Si6 Si 0.36095(4) 0.15980(5) 0.08770(6) 0.0183(5) Uani 0.16 1 d P . .
Ge7 Ge 0.24548(4) 0.16457(4) 0.28281(7) 0.0193(5) Uani 0.841(6) 1 d P . .
Si7 Si 0.24548(4) 0.16457(4) 0.28281(7) 0.0193(5) Uani 0.16 1 d P . .
F1 F 0.3693(3) 0.2552(2) 0.2766(4) 0.0349(17) Uani 1 1 d . . .
F2 F 0.2502(3) 0.0530(3) 0.1124(4) 0.0404(18) Uani 1 1 d . . .
O1 O 0.4206(3) 0.1767(3) 0.2551(4) 0.0204(15) Uani 1 1 d . . .
O2 O 0.3371(3) 0.1242(2) 0.2372(4) 0.0180(15) Uani 1 1 d . . .
O3 O 0.2876(3) 0.2098(3) 0.2627(4) 0.0228(16) Uani 1 1 d . . .
O4 O 0.3512(3) 0.2061(3) 0.1512(4) 0.0218(16) Uani 1 1 d . . .
O5 O 0.3545(3) 0.1805(3) 0.3662(4) 0.0241(17) Uani 1 1 d . . .
O6 O 0.3464(3) 0.0767(3) 0.3775(4) 0.0230(16) Uani 1 1 d . . .
O7 O 0.3157(3) 0.0393(3) 0.2145(4) 0.0233(16) Uani 1 1 d . . .
O8 O 0.4212(3) 0.0722(3) 0.2454(4) 0.0237(16) Uani 1 1 d . . .
O9 O 0.3790(3) -0.0015(3) 0.3146(5) 0.035(2) Uani 1 1 d . . .
O10 O 0.2390(3) 0.1215(3) 0.2098(4) 0.0261(17) Uani 1 1 d . . .
O11 O 0.3138(3) 0.1169(3) 0.0845(4) 0.0227(16) Uani 1 1 d . . .
O12 O 0.2604(3) 0.1343(3) 0.3687(4) 0.0234(16) Uani 1 1 d . . .
O13 O 0.3136(3) 0.1339(3) 0.4992(4) 0.034(2) Uani 1 1 d . . .
O14 O 0.4151(3) 0.1286(3) 0.1070(4) 0.0218(16) Uani 1 1 d . . .
O15 O 0.1876(3) 0.1876(3) 0.2960(6) 0.030(3) Uani 1 2 d S . .
OW1 O 0.5000 0.0000 -0.2500 0.18(2) Uani 1 4 d S . .
OW2 O 0.4224(5) 0.2859(5) 0.2433(13) 0.115(7) Uani 1 1 d . . .
OW3 O 0.4686(6) 0.2664(8) 0.286(2) 0.211(17) Uani 1 1 d . . .
OW4 O 0.4454(10) 0.5002(9) 0.4095(16) 0.018(10) Uani 0.25(3) 1 d P . .
N1 N 0.3432(5) 0.0000 0.5000 0.033(3) Uani 1 2 d S . .
H1A H 0.3539 -0.0109 0.4542 0.050 Uiso 0.50 1 calc PR . .
H1B H 0.3539 -0.0191 0.5382 0.050 Uiso 0.50 1 calc PR . .
H1C H 0.3539 0.0300 0.5076 0.050 Uiso 0.50 1 calc PR . .
C1 C 0.2917(7) 0.0000 0.5000 0.070(8) Uani 1 2 d SD . .
H1D H 0.2827 0.0188 0.4543 0.084 Uiso 0.50 1 calc PR . .
H1E H 0.2827 -0.0331 0.4881 0.084 Uiso 0.50 1 calc PR . .
C2 C 0.2599(8) 0.0141(13) 0.5569(17) 0.053(8) Uani 0.50 1 d PD . .
H2A H 0.2629 0.0488 0.5639 0.064 Uiso 0.50 1 calc PR . .
H2B H 0.2693 -0.0011 0.6058 0.064 Uiso 0.50 1 calc PR . .
C3 C 0.2084(7) 0.002(2) 0.541(3) 0.12(2) Uani 0.50 1 d PD . .
H3D H 0.1890 0.0128 0.5849 0.187 Uiso 0.50 1 calc PR . .
H3E H 0.2049 -0.0318 0.5343 0.187 Uiso 0.50 1 calc PR . .
H3F H 0.1980 0.0189 0.4949 0.187 Uiso 0.50 1 calc PR . .
N2 N 0.2216(8) 0.2216(8) 0.6267(19) 0.32(5) Uani 1 2 d SD . .
H2C H 0.2338 0.2371 0.6679 0.475 Uiso 0.50 1 calc PR . .
H2D H 0.2073 0.2427 0.5949 0.475 Uiso 0.50 1 calc PR . .
H2E H 0.2453 0.2066 0.6012 0.475 Uiso 0.50 1 calc PR . .
C4 C 0.1924(10) 0.1924(10) 0.6485(16) 0.20(4) Uani 1 2 d SD . .
H4A H 0.1702 0.2099 0.6821 0.245 Uiso 0.50 1 calc PR . .
H4B H 0.2099 0.1702 0.6821 0.245 Uiso 0.50 1 calc PR . .
C5 C 0.1652(8) 0.1652(8) 0.603(3) 0.82(18) Uani 1 2 d SD . .
H5A H 0.1313 0.1715 0.6130 0.985 Uiso 0.50 1 calc PR . .
H5B H 0.1715 0.1313 0.6130 0.985 Uiso 0.50 1 calc PR . .
C6 C 0.1773(16) 0.1773(16) 0.513(2) 0.41(8) Uani 1 2 d SD . .
H6A H 0.1568 0.1585 0.4790 0.616 Uiso 1 2 calc SR . .
H6B H 0.2106 0.1697 0.5020 0.616 Uiso 0.50 1 calc PR . .
H6C H 0.1718 0.2111 0.5029 0.616 Uiso 0.50 1 calc PR . .
N3 N 0.2902(7) 0.2902(7) 0.3762(13) 0.107(12) Uani 1 2 d SD . .
H3A H 0.2954 0.2674 0.3405 0.161 Uiso 0.50 1 calc PR . .
H3B H 0.3182 0.3040 0.3889 0.161 Uiso 0.50 1 calc PR . .
H3C H 0.2703 0.3125 0.3568 0.161 Uiso 0.50 1 calc PR . .
C7 C 0.2689(10) 0.2689(10) 0.4447(16) 0.24(4) Uani 1 2 d SD . .
H7A H 0.2396 0.2527 0.4279 0.287 Uiso 0.50 1 calc PR . .
H7B H 0.2909 0.2439 0.4625 0.287 Uiso 0.50 1 calc PR . .
C8 C 0.2569(18) 0.2966(16) 0.5102(14) 0.44(12) Uani 0.50 1 d PD . .
H8A H 0.2223 0.2940 0.5190 0.526 Uiso 0.50 1 calc PR . .
H8B H 0.2639 0.3303 0.4988 0.526 Uiso 0.50 1 calc PR . .
C9 C 0.2828(19) 0.2828(19) 0.585(2) 0.26(5) Uani 1 2 d SD . .
H9A H 0.2735 0.3045 0.6260 0.385 Uiso 0.50 1 calc PR . .
H9B H 0.3171 0.2847 0.5768 0.385 Uiso 0.50 1 calc PR . .
H9C H 0.2742 0.2503 0.5991 0.385 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
Ge1 0.0240(6) 0.0155(5) 0.0102(5) -0.0004(4) 0.0016(4) 0.0021(4)
Ge2 0.0202(6) 0.0148(5) 0.0139(5) -0.0009(4) -0.0008(4) 0.0020(4)
Ge3 0.0204(6) 0.0237(6) 0.0135(5) -0.0003(4) -0.0016(4) 0.0017(4)
Ge4 0.0252(7) 0.0186(7) 0.0072(6) -0.0002(4) -0.0008(4) 0.0048(5)
Si4 0.0252(7) 0.0186(7) 0.0072(6) -0.0002(4) -0.0008(4) 0.0048(5)
Ge5 0.0137(7) 0.0229(7) 0.0133(6) 0.0000(4) -0.0007(4) 0.0000(4)
Si5 0.0137(7) 0.0229(7) 0.0133(6) 0.0000(4) -0.0007(4) 0.0000(4)
Ge6 0.0214(7) 0.0253(8) 0.0082(6) 0.0012(5) -0.0002(4) 0.0032(5)
Si6 0.0214(7) 0.0253(8) 0.0082(6) 0.0012(5) -0.0002(4) 0.0032(5)
Ge7 0.0214(7) 0.0236(8) 0.0129(6) 0.0035(5) 0.0023(5) 0.0093(5)
Si7 0.0214(7) 0.0236(8) 0.0129(6) 0.0035(5) 0.0023(5) 0.0093(5)
F1 0.061(5) 0.017(3) 0.027(3) 0.003(3) 0.006(3) -0.002(3)
F2 0.040(4) 0.046(5) 0.035(4) -0.003(3) -0.015(3) -0.008(4)
O1 0.025(4) 0.023(4) 0.013(3) -0.004(3) 0.001(3) -0.008(3)
O2 0.022(4) 0.019(4) 0.013(3) 0.002(3) -0.003(3) 0.003(3)
O3 0.032(4) 0.018(4) 0.018(4) 0.002(3) 0.006(3) 0.009(3)
O4 0.034(4) 0.022(4) 0.010(3) 0.001(3) 0.005(3) 0.002(3)
O5 0.033(4) 0.029(4) 0.010(3) -0.007(3) 0.002(3) -0.001(3)
O6 0.035(5) 0.022(4) 0.012(3) 0.002(3) 0.001(3) 0.006(3)
O7 0.033(4) 0.016(4) 0.020(3) -0.004(3) -0.004(3) -0.002(3)
O8 0.020(4) 0.030(4) 0.022(4) 0.007(3) 0.000(3) 0.011(3)
O9 0.048(5) 0.011(4) 0.045(5) 0.002(3) -0.020(4) 0.000(3)
O10 0.021(4) 0.039(5) 0.019(4) -0.002(3) 0.006(3) 0.005(3)
O11 0.027(4) 0.027(4) 0.015(3) -0.009(3) -0.006(3) 0.002(3)
O12 0.030(4) 0.024(4) 0.015(3) 0.004(3) 0.000(3) 0.002(3)
O13 0.048(5) 0.047(5) 0.008(3) -0.006(3) -0.009(3) -0.002(4)
O14 0.023(4) 0.028(4) 0.015(3) 0.001(3) 0.001(3) 0.004(3)
O15 0.030(4) 0.030(4) 0.030(6) 0.007(4) 0.007(4) 0.016(5)
OW1 0.022(7) 0.022(7) 0.49(8) 0.000 0.000 0.000
OW2 0.063(9) 0.052(8) 0.23(2) -0.010(10) 0.070(11) -0.024(6)
OW3 0.070(11) 0.131(17) 0.43(5) -0.15(2) -0.105(19) 0.052(11)
OW4 0.021(17) 0.000(14) 0.032(18) -0.007(11) -0.024(13) 0.002(10)
N1 0.039(9) 0.032(8) 0.028(7) 0.006(6) 0.000 0.000
C1 0.052(15) 0.069(17) 0.088(18) 0.051(15) 0.000 0.000
C2 0.026(15) 0.09(3) 0.047(16) -0.021(16) 0.003(12) 0.011(15)
C3 0.04(2) 0.15(5) 0.19(6) -0.08(5) 0.03(3) 0.01(3)
N2 0.36(6) 0.36(6) 0.24(6) -0.24(6) -0.24(6) 0.23(7)
C4 0.21(4) 0.21(4) 0.19(4) 0.17(4) 0.17(4) 0.19(5)
C5 1.0(2) 1.0(2) 0.4(2) -0.27(14) -0.27(14) -0.524
C6 0.43(11) 0.43(11) 0.38(12) 0.22(10) 0.22(10) 0.40(11)
N3 0.096(13) 0.096(13) 0.13(2) -0.071(15) -0.071(15) 0.057(16)
C7 0.35(7) 0.35(7) 0.026(16) 0.00(3) 0.00(3) 0.20(8)
C8 0.9(3) 0.21(8) 0.25(10) 0.18(8) 0.34(15) 0.41(14)
C9 0.16(4) 0.16(4) 0.44(13) -0.10(6) -0.10(6) 0.13(5)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ge Ge 0.1547 1.8001 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
F F 0.0171 0.0103 '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
F1 Ge1 O4 88.8(3) . . ?
F1 Ge1 O5 89.5(3) . . ?
O4 Ge1 O5 177.4(3) . . ?
F1 Ge1 O3 88.5(3) . . ?
O4 Ge1 O3 87.1(3) . . ?
O5 Ge1 O3 90.9(3) . . ?
F1 Ge1 O1 89.4(3) . . ?
O4 Ge1 O1 93.1(3) . . ?
O5 Ge1 O1 88.8(3) . . ?
O3 Ge1 O1 177.9(3) . . ?
F1 Ge1 O2 179.3(3) . . ?
O4 Ge1 O2 90.5(3) . . ?
O5 Ge1 O2 91.1(3) . . ?
O3 Ge1 O2 91.5(3) . . ?
O1 Ge1 O2 90.5(3) . . ?
O6 Ge2 O8 118.3(4) . . ?
O6 Ge2 O7 119.9(4) . . ?
O8 Ge2 O7 120.2(3) . . ?
O6 Ge2 O9 91.6(4) . . ?
O8 Ge2 O9 93.8(4) . . ?
O7 Ge2 O9 96.8(3) . . ?
O6 Ge2 O2 90.2(3) . . ?
O8 Ge2 O2 89.6(3) . . ?
O7 Ge2 O2 78.1(3) . . ?
O9 Ge2 O2 174.8(3) . . ?
O6 Ge2 Ge3 110.5(2) . . ?
O8 Ge2 Ge3 109.7(2) . . ?
O7 Ge2 Ge3 35.9(2) . . ?
O9 Ge2 Ge3 132.7(3) . . ?
O2 Ge2 Ge3 42.22(19) . . ?
O11 Ge3 O10 116.0(3) . . ?
O11 Ge3 O7 122.1(3) . . ?
O10 Ge3 O7 121.9(4) . . ?
O11 Ge3 F2 90.4(3) . . ?
O10 Ge3 F2 89.7(4) . . ?
O7 Ge3 F2 89.3(3) . . ?
O11 Ge3 O2 93.7(3) . . ?
O10 Ge3 O2 95.4(3) . . ?
O7 Ge3 O2 82.1(3) . . ?
F2 Ge3 O2 171.3(3) . . ?
O11 Ge3 Ge2 114.8(2) . . ?
O10 Ge3 Ge2 116.4(2) . . ?
O7 Ge3 Ge2 36.0(2) . . ?
F2 Ge3 Ge2 125.3(2) . . ?
O2 Ge3 Ge2 46.1(2) . . ?
O13 Ge4 O5 111.7(4) . . ?
O13 Ge4 O6 106.2(4) . . ?
O5 Ge4 O6 112.8(4) . . ?
O13 Ge4 O12 101.1(4) . . ?
O5 Ge4 O12 113.5(4) . . ?
O6 Ge4 O12 110.7(4) . . ?
O9 Ge5 O1 116.1(4) 11 . ?
O9 Ge5 O8 105.3(4) 11 . ?
O1 Ge5 O8 113.0(3) . . ?
O9 Ge5 O14 102.1(4) 11 . ?
O1 Ge5 O14 110.7(3) . . ?
O8 Ge5 O14 108.9(4) . . ?
O13 Ge6 O4 104.9(4) 15_554 . ?
O13 Ge6 O14 108.0(4) 15_554 . ?
O4 Ge6 O14 112.6(4) . . ?
O13 Ge6 O11 109.2(4) 15_554 . ?
O4 Ge6 O11 114.2(4) . . ?
O14 Ge6 O11 107.7(3) . . ?
O10 Ge7 O15 104.6(5) . . ?
O10 Ge7 O12 107.5(4) . . ?
O15 Ge7 O12 106.6(4) . . ?
O10 Ge7 O3 114.8(3) . . ?
O15 Ge7 O3 112.2(4) . . ?
O12 Ge7 O3 110.7(4) . . ?
OW2 F1 Ge1 126.4(6) . . ?
Ge5 O1 Ge1 118.3(4) . . ?
Ge3 O2 Ge1 134.6(4) . . ?
Ge3 O2 Ge2 91.7(3) . . ?
Ge1 O2 Ge2 133.7(3) . . ?
Ge7 O3 Ge1 118.0(4) . . ?
Ge6 O4 Ge1 117.6(4) . . ?
Ge4 O5 Ge1 116.8(4) . . ?
Ge4 O6 Ge2 123.5(4) . . ?
Ge3 O7 Ge2 108.1(4) . . ?
Ge5 O8 Ge2 125.5(4) . . ?
Si5 O9 Ge5 0.00(11) 12_545 12_545 ?
Si5 O9 Ge2 145.0(5) 12_545 . ?
Ge5 O9 Ge2 145.0(5) 12_545 . ?
Ge7 O10 Ge3 120.7(4) . . ?
Ge3 O11 Ge6 121.1(4) . . ?
Ge7 O12 Ge4 119.7(4) . . ?
Si6 O13 Ge6 0.00(8) 15 15 ?
Si6 O13 Ge4 147.5(6) 15 . ?
Ge6 O13 Ge4 147.5(6) 15 . ?
Ge5 O14 Ge6 120.3(4) . . ?
Ge7 O15 Si7 131.3(7) . 8 ?
Ge7 O15 Ge7 131.3(7) . 8 ?
Si7 O15 Ge7 0.00(11) 8 8 ?
OW3 OW2 F1 110.8(16) . . ?
C2 C1 N1 129.9(9) . . ?
C1 C2 C3 115.3(17) . . ?
N2 C4 C5 125.6(5) . . ?
C4 C5 C6 109.2(4) . . ?
C8 C7 N3 121.7(5) . . ?
C7 C8 C9 115.1(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
Ge1 F1 1.823(6) . ?
Ge1 O4 1.871(6) . ?
Ge1 O5 1.873(7) . ?
Ge1 O3 1.894(7) . ?
Ge1 O1 1.896(7) . ?
Ge1 O2 1.966(7) . ?
Ge2 O6 1.780(7) . ?
Ge2 O8 1.788(7) . ?
Ge2 O7 1.791(7) . ?
Ge2 O9 1.813(8) . ?
Ge2 O2 2.085(7) . ?
Ge2 Ge3 2.8947(15) . ?
Ge3 O11 1.744(8) . ?
Ge3 O10 1.771(7) . ?
Ge3 O7 1.785(7) . ?
Ge3 F2 1.833(7) . ?
Ge3 O2 1.946(7) . ?
Ge4 O13 1.716(7) . ?
Ge4 O5 1.723(8) . ?
Ge4 O6 1.742(7) . ?
Ge4 O12 1.743(8) . ?
Ge5 O9 1.690(8) 11 ?
Ge5 O1 1.731(7) . ?
Ge5 O8 1.741(8) . ?
Ge5 O14 1.749(7) . ?
Ge6 O13 1.688(7) 15_554 ?
Ge6 O4 1.699(7) . ?
Ge6 O14 1.759(7) . ?
Ge6 O11 1.763(8) . ?
Ge7 O10 1.733(8) . ?
Ge7 O15 1.736(5) . ?
Ge7 O12 1.739(7) . ?
Ge7 O3 1.742(8) . ?
F1 OW2 1.791(13) . ?
O9 Si5 1.690(8) 12_545 ?
O9 Ge5 1.690(8) 12_545 ?
O13 Si6 1.688(7) 15 ?
O13 Ge6 1.688(7) 15 ?
O15 Si7 1.736(5) 8 ?
O15 Ge7 1.736(5) 8 ?
OW2 OW3 1.57(3) . ?
N1 C1 1.42(2) . ?
C1 C2 1.37(3) . ?
C2 C3 1.485(4) . ?
N2 C4 1.199(4) . ?
C4 C5 1.324(4) . ?
C5 C6 1.610(4) . ?
N3 C7 1.437(4) . ?
C7 C8 1.397(4) . ?
C8 C9 1.512(4) . ?
|
1100931.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-17 14:53:33 +0200 (Thu, 17 Mar 2016) $
#$Revision: 178237 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100931.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_1100931
loop_
_publ_author_name
'Mizukami, Shin'
'Houjou, Hirohiko'
'Sugaya, Kenta'
'Koyama, Emiko'
'Tokuhisa, Hideo'
'Sasaki, Takeshi'
'Kanesato, Masatoshi'
_publ_section_title
;
Fluorescence Color Modulation by Intramolecular and Intermolecular
\p--\p Interactions in a Helical Zinc(II) Complex
;
_journal_coden_ASTM CMATEX
_journal_issue 1
_journal_name_full 'Chemistry of Materials'
_journal_page_first 50
_journal_page_last 56
_journal_paper_doi 10.1021/cm049744s
_journal_volume 17
_journal_year 2005
_chemical_formula_moiety 'C52 H68 N4 O5 Zn2 '
_chemical_formula_sum 'C52 H68 N4 O5 Zn2'
_chemical_formula_weight 959.89
_chemical_melting_point ?
_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 99.73(4)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 15.307(6)
_cell_length_b 19.782(6)
_cell_length_c 16.817(7)
_cell_measurement_reflns_used 42111
_cell_measurement_temperature 193.1
_cell_measurement_theta_max 27.4
_cell_measurement_theta_min 3.0
_cell_volume 5019.0(3)
_computing_cell_refinement PROCESS-AUTO
_computing_data_collection PROCESS-AUTO
_computing_data_reduction CrystalStructure
_computing_publication_material 'CrystalStructure Ver. 3.10'
_computing_structure_refinement CRYSTALS
_computing_structure_solution DirectMethod
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.9934
_diffrn_measured_fraction_theta_max 0.9934
_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 0.055
_diffrn_reflns_limit_h_max 19
_diffrn_reflns_limit_h_min -19
_diffrn_reflns_limit_k_max 25
_diffrn_reflns_limit_k_min -25
_diffrn_reflns_limit_l_max 21
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_number 47374
_diffrn_reflns_theta_full 27.41
_diffrn_reflns_theta_max 27.41
_exptl_absorpt_coefficient_mu 1.005
_exptl_absorpt_correction_T_max 0.778
_exptl_absorpt_correction_T_min 0.676
_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 1.270
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 2032.00
_exptl_crystal_size_max 0.40
_exptl_crystal_size_mid 0.35
_exptl_crystal_size_min 0.25
_refine_diff_density_max 0.95
_refine_diff_density_min -0.87
_refine_ls_extinction_coef 71.2(2)
_refine_ls_extinction_method
'Larson (1970) Crystallographic Computing eq. 22'
_refine_ls_goodness_of_fit_ref 0.811
_refine_ls_hydrogen_treatment refall
_refine_ls_number_parameters 637
_refine_ls_number_reflns 7336
_refine_ls_R_factor_gt 0.0490
_refine_ls_shift/su_max 0.0090
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0008Fo^2^ + 2.0000\s^2^(Fo) + 0.2000]/(4Fo^2^)'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_ref 0.1010
_reflns_number_gt 6595
_reflns_number_total 11357
_reflns_threshold_expression F^2^>2.0\s(F^2^)
_cod_data_source_file 1
_cod_data_source_block cm049744ssi20040219_042336.cif
_cod_duplicate_entry 4000537
_cod_depositor_comments
;
The following automatic conversions were performed:
'_chemical_melting_point' value ' not measured ' was changed to '?' -
the value is undefined or not given.
Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana
;
_cod_original_formula_sum 'C52 H68 N4 O5 Zn2 '
_cod_database_code 1100931
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x,y+1/2,-z+1/2
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 -0.16982(3) -0.08365(2) -0.91413(2) 0.0316(1) Uani 1.00 1 d . . .
Zn2 Zn -0.36950(3) -0.12177(2) -1.09342(3) 0.0388(1) Uani 1.00 1 d . . .
O1 O -0.2136(2) -0.0369(1) -0.8307(1) 0.0404(8) Uani 1.00 1 d . . .
O2 O -0.3589(2) -0.0995(1) -1.2013(2) 0.0435(8) Uani 1.00 1 d . . .
O3 O -0.0459(2) -0.1056(1) -0.8937(1) 0.0468(9) Uani 1.00 1 d . . .
O4 O -0.4767(2) -0.1585(1) -1.0689(2) 0.0424(8) Uani 1.00 1 d . . .
C49 C -0.0820(4) -0.1760(3) -0.5520(5) 0.105(3) Uani 1.00 1 d . . .
N1 N -0.2267(3) -0.1717(2) -0.8983(2) 0.050(1) Uani 1.00 1 d . . .
N2 N -0.2742(2) -0.1919(2) -1.0801(2) 0.047(1) Uani 1.00 1 d . . .
N3 N -0.1667(2) -0.0396(1) -1.0203(2) 0.0315(9) Uani 1.00 1 d . . .
N4 N -0.3638(2) -0.0455(1) -1.0137(2) 0.0333(9) Uani 1.00 1 d . . .
C1 C -0.2054(4) -0.2328(2) -0.9468(3) 0.075(2) Uani 1.00 1 d . . .
C2 C -0.2687(4) -0.2459(2) -1.0177(3) 0.068(2) Uani 1.00 1 d . . .
C3 C -0.2360(3) 0.0054(2) -1.0634(2) 0.039(1) Uani 1.00 1 d . . .
C4 C -0.3116(3) 0.0165(2) -1.0176(3) 0.042(1) Uani 1.00 1 d . . .
C5 C -0.2640(3) -0.1803(3) -0.8369(3) 0.059(2) Uani 1.00 1 d . . .
C6 C -0.2818(3) -0.1319(3) -0.7775(3) 0.050(1) Uani 1.00 1 d . . .
C7 C -0.2521(3) -0.0632(2) -0.7740(2) 0.044(1) Uani 1.00 1 d . . .
C8 C -0.2662(4) -0.0225(3) -0.7078(3) 0.067(2) Uani 1.00 1 d . . .
C9 C -0.3140(4) -0.0503(4) -0.6523(3) 0.090(2) Uani 1.00 1 d . . .
C10 C -0.3446(4) -0.1166(4) -0.6576(4) 0.094(2) Uani 1.00 1 d . . .
C11 C -0.3267(3) -0.1569(3) -0.7175(3) 0.079(2) Uani 1.00 1 d . . .
C12 C -0.2356(5) 0.0487(3) -0.7012(3) 0.086(2) Uani 1.00 1 d . . .
C13 C -0.1366(5) 0.0525(3) -0.6999(3) 0.091(2) Uani 1.00 1 d . . .
C14 C -0.2833(5) 0.0925(3) -0.7702(3) 0.105(3) Uani 1.00 1 d . . .
C15 C -0.2509(7) 0.0820(4) -0.6210(4) 0.165(4) Uani 1.00 1 d . . .
C16 C -0.2209(3) -0.1957(2) -1.1318(3) 0.054(1) Uani 1.00 1 d . . .
C17 C -0.2189(3) -0.1535(2) -1.2016(3) 0.044(1) Uani 1.00 1 d . . .
C18 C -0.2893(3) -0.1097(2) -1.2354(2) 0.036(1) Uani 1.00 1 d . . .
C19 C -0.2852(3) -0.0757(2) -1.3099(2) 0.043(1) Uani 1.00 1 d . . .
C20 C -0.2090(4) -0.0838(3) -1.3426(3) 0.061(2) Uani 1.00 1 d . . .
C21 C -0.1388(4) -0.1251(3) -1.3083(3) 0.068(2) Uani 1.00 1 d . . .
C22 C -0.1443(3) -0.1605(3) -1.2399(3) 0.059(2) Uani 1.00 1 d . . .
C23 C -0.3632(3) -0.0325(2) -1.3502(2) 0.054(1) Uani 1.00 1 d . . .
C24 C -0.3763(3) 0.0284(2) -1.2971(3) 0.057(2) Uani 1.00 1 d . . .
C25 C -0.3469(5) -0.0039(3) -1.4320(3) 0.104(3) Uani 1.00 1 d . . .
C26 C -0.4473(4) -0.0746(3) -1.3664(3) 0.084(2) Uani 1.00 1 d . . .
C27 C -0.0993(2) -0.0499(2) -1.0555(2) 0.032(1) Uani 1.00 1 d . . .
C28 C -0.0208(2) -0.0891(2) -1.0280(2) 0.031(1) Uani 1.00 1 d . . .
C29 C 0.0034(2) -0.1150(2) -0.9487(2) 0.034(1) Uani 1.00 1 d . . .
C30 C 0.0853(3) -0.1511(2) -0.9280(3) 0.040(1) Uani 1.00 1 d . . .
C31 C 0.1361(3) -0.1604(2) -0.9876(3) 0.049(1) Uani 1.00 1 d . . .
C32 C 0.1126(3) -0.1346(2) -1.0653(3) 0.052(1) Uani 1.00 1 d . . .
C33 C 0.0365(3) -0.0986(2) -1.0847(2) 0.044(1) Uani 1.00 1 d . . .
C34 C 0.1131(3) -0.1780(3) -0.8416(3) 0.053(1) Uani 1.00 1 d . . .
C35 C 0.0443(3) -0.2296(3) -0.8218(3) 0.077(2) Uani 1.00 1 d . . .
C36 C 0.2035(3) -0.2134(3) -0.8309(3) 0.082(2) Uani 1.00 1 d . . .
C37 C 0.1219(3) -0.1197(3) -0.7807(3) 0.070(2) Uani 1.00 1 d . . .
C38 C -0.4086(2) -0.0504(2) -0.9548(2) 0.034(1) Uani 1.00 1 d . . .
C39 C -0.4678(2) -0.1047(2) -0.9406(2) 0.032(1) Uani 1.00 1 d . . .
C40 C -0.4988(2) -0.1561(2) -0.9974(2) 0.034(1) Uani 1.00 1 d . . .
C41 C -0.5579(3) -0.2067(2) -0.9755(3) 0.040(1) Uani 1.00 1 d . . .
C42 C -0.5787(3) -0.2037(2) -0.8993(3) 0.049(1) Uani 1.00 1 d . . .
C43 C -0.5489(3) -0.1531(3) -0.8440(3) 0.052(1) Uani 1.00 1 d . . .
C44 C -0.4945(3) -0.1035(2) -0.8645(2) 0.043(1) Uani 1.00 1 d . . .
C45 C -0.5944(3) -0.2616(2) -1.0362(3) 0.051(1) Uani 1.00 1 d . . .
C46 C -0.5188(3) -0.3029(2) -1.0630(3) 0.056(2) Uani 1.00 1 d . . .
C47 C -0.6535(3) -0.3123(3) -0.9998(4) 0.075(2) Uani 1.00 1 d . . .
C48 C -0.6512(3) -0.2294(3) -1.1097(3) 0.074(2) Uani 1.00 1 d . . .
C50 C -0.0794(7) -0.1145(5) -0.580(1) 0.284(7) Uani 1.00 1 d . . .
C51 C 0.006(1) -0.0906(6) -0.557(1) 0.35(1) Uani 1.00 1 d . . .
C52 C 0.0574(7) -0.1544(7) -0.5648(7) 0.197(6) Uani 1.00 1 d . . .
O5 O -0.0071(7) -0.1985(6) -0.569(1) 0.400(8) Uani 1.00 1 d . . .
H1 H -0.2005(4) -0.2715(2) -0.9128(3) 0.085(2) Uiso 1.00 1 c . . .
H2 H -0.1503(4) -0.2246(2) -0.9638(3) 0.085(2) Uiso 1.00 1 c . . .
H3 H -0.2557(4) -0.2877(2) -1.0408(3) 0.080(2) Uiso 1.00 1 c . . .
H4 H -0.3250(4) -0.2485(2) -1.0013(3) 0.080(2) Uiso 1.00 1 c . . .
H5 H -0.2595(3) -0.0145(2) -1.1139(2) 0.047(2) Uiso 1.00 1 c . . .
H6 H -0.2098(3) 0.0477(2) -1.0721(2) 0.047(2) Uiso 1.00 1 c . . .
H7 H -0.2874(3) 0.0304(2) -0.9643(3) 0.049(2) Uiso 1.00 1 c . . .
H8 H -0.3496(3) 0.0509(2) -1.0433(3) 0.050(2) Uiso 1.00 1 c . . .
H9 H -0.2826(3) -0.2253(3) -0.8292(3) 0.069(2) Uiso 1.00 1 c . . .
H10 H -0.3258(4) -0.0229(4) -0.6090(3) 0.114(3) Uiso 1.00 1 c . . .
H11 H -0.3786(4) -0.1331(4) -0.6194(4) 0.117(3) Uiso 1.00 1 c . . .
H12 H -0.3448(3) -0.2029(3) -0.7193(3) 0.095(2) Uiso 1.00 1 c . . .
H13 H -0.1236(5) 0.0337(3) -0.7486(3) 0.107(3) Uiso 1.00 1 c . . .
H14 H -0.1070(5) 0.0273(3) -0.6553(3) 0.107(3) Uiso 1.00 1 c . . .
H15 H -0.1172(5) 0.0981(3) -0.6954(3) 0.107(3) Uiso 1.00 1 c . . .
H16 H -0.2628(5) 0.1379(3) -0.7655(3) 0.131(3) Uiso 1.00 1 c . . .
H17 H -0.3447(5) 0.0914(3) -0.7674(3) 0.131(3) Uiso 1.00 1 c . . .
H18 H -0.2740(5) 0.0745(3) -0.8205(3) 0.131(3) Uiso 1.00 1 c . . .
H19 H -0.2304(7) 0.1274(4) -0.6178(4) 0.207(5) Uiso 1.00 1 c . . .
H20 H -0.2204(7) 0.0571(4) -0.5764(4) 0.207(5) Uiso 1.00 1 c . . .
H21 H -0.3127(7) 0.0813(4) -0.6198(4) 0.207(5) Uiso 1.00 1 c . . .
H22 H -0.1776(3) -0.2305(2) -1.1224(3) 0.064(2) Uiso 1.00 1 c . . .
H23 H -0.2043(4) -0.0600(3) -1.3908(3) 0.078(2) Uiso 1.00 1 c . . .
H24 H -0.0876(4) -0.1287(3) -1.3330(3) 0.087(2) Uiso 1.00 1 c . . .
H25 H -0.0973(3) -0.1897(3) -1.2172(3) 0.072(2) Uiso 1.00 1 c . . .
H26 H -0.3244(3) 0.0556(2) -1.2895(3) 0.068(2) Uiso 1.00 1 c . . .
H27 H -0.3875(3) 0.0131(2) -1.2462(3) 0.068(2) Uiso 1.00 1 c . . .
H28 H -0.4252(3) 0.0544(2) -1.3228(3) 0.068(2) Uiso 1.00 1 c . . .
H29 H -0.3386(5) -0.0400(3) -1.4672(3) 0.127(3) Uiso 1.00 1 c . . .
H30 H -0.2952(5) 0.0236(3) -1.4231(3) 0.127(3) Uiso 1.00 1 c . . .
H31 H -0.3963(5) 0.0226(3) -1.4557(3) 0.127(3) Uiso 1.00 1 c . . .
H32 H -0.4951(4) -0.0473(3) -1.3916(3) 0.096(2) Uiso 1.00 1 c . . .
H33 H -0.4600(4) -0.0913(3) -1.3166(3) 0.096(2) Uiso 1.00 1 c . . .
H34 H -0.4394(4) -0.1115(3) -1.4006(3) 0.096(2) Uiso 1.00 1 c . . .
H35 H -0.1018(2) -0.0287(2) -1.1066(2) 0.039(1) Uiso 1.00 1 c . . .
H36 H 0.1894(3) -0.1857(2) -0.9746(3) 0.059(2) Uiso 1.00 1 c . . .
H37 H 0.1497(3) -0.1420(2) -1.1044(3) 0.064(2) Uiso 1.00 1 c . . .
H38 H 0.0212(3) -0.0795(2) -1.1371(2) 0.053(2) Uiso 1.00 1 c . . .
H39 H -0.0126(3) -0.2093(3) -0.8264(3) 0.094(2) Uiso 1.00 1 c . . .
H40 H 0.0617(3) -0.2464(3) -0.7685(3) 0.094(2) Uiso 1.00 1 c . . .
H41 H 0.0419(3) -0.2659(3) -0.8592(3) 0.094(2) Uiso 1.00 1 c . . .
H42 H 0.1989(3) -0.2497(3) -0.8683(3) 0.098(3) Uiso 1.00 1 c . . .
H43 H 0.2191(3) -0.2305(3) -0.7776(3) 0.098(3) Uiso 1.00 1 c . . .
H44 H 0.2478(3) -0.1827(3) -0.8417(3) 0.098(3) Uiso 1.00 1 c . . .
H45 H 0.1665(3) -0.0895(3) -0.7921(3) 0.083(2) Uiso 1.00 1 c . . .
H46 H 0.1378(3) -0.1366(3) -0.7273(3) 0.083(2) Uiso 1.00 1 c . . .
H47 H 0.0670(3) -0.0964(3) -0.7855(3) 0.083(2) Uiso 1.00 1 c . . .
H48 H -0.4020(2) -0.0143(2) -0.9171(2) 0.040(1) Uiso 1.00 1 c . . .
H49 H -0.6151(3) -0.2384(2) -0.8834(3) 0.061(2) Uiso 1.00 1 c . . .
H50 H -0.5664(3) -0.1529(3) -0.7925(3) 0.065(2) Uiso 1.00 1 c . . .
H51 H -0.4747(3) -0.0683(2) -0.8275(2) 0.052(2) Uiso 1.00 1 c . . .
H52 H -0.5433(3) -0.3357(2) -1.1017(3) 0.068(2) Uiso 1.00 1 c . . .
H53 H -0.4855(3) -0.3249(2) -1.0176(3) 0.068(2) Uiso 1.00 1 c . . .
H54 H -0.4812(3) -0.2733(2) -1.0863(3) 0.068(2) Uiso 1.00 1 c . . .
H55 H -0.7013(3) -0.2890(3) -0.9828(4) 0.092(2) Uiso 1.00 1 c . . .
H56 H -0.6191(3) -0.3342(3) -0.9549(4) 0.092(2) Uiso 1.00 1 c . . .
H57 H -0.6761(3) -0.3451(3) -1.0393(4) 0.092(2) Uiso 1.00 1 c . . .
H58 H -0.6164(3) -0.1976(3) -1.1329(3) 0.084(2) Uiso 1.00 1 c . . .
H59 H -0.7003(3) -0.2070(3) -1.0937(3) 0.084(2) Uiso 1.00 1 c . . .
H60 H -0.6719(3) -0.2633(3) -1.1482(3) 0.084(2) Uiso 1.00 1 c . . .
H61 H -0.1206(7) -0.0862(5) -0.559(1) 0.32(1) Uiso 1.00 1 c . . .
H62 H -0.0939(7) -0.1161(5) -0.637(1) 0.32(1) Uiso 1.00 1 c . . .
H63 H 0.015(1) -0.0736(6) -0.503(1) 0.41(1) Uiso 1.00 1 c . . .
H64 H 0.021(1) -0.0568(6) -0.592(1) 0.41(1) Uiso 1.00 1 c . . .
H65 H 0.1034(7) -0.1596(7) -0.5196(7) 0.249(7) Uiso 1.00 1 c . . .
H66 H 0.0820(7) -0.1556(7) -0.6130(7) 0.249(7) Uiso 1.00 1 c . . .
H67 H -0.1304(4) -0.2024(3) -0.5779(5) 0.122(3) Uiso 1.00 1 c . . .
H68 H -0.0834(4) -0.1738(3) -0.4958(5) 0.122(3) 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
Zn1 0.0294(2) 0.0373(3) 0.0286(2) 0.0015(2) 0.0069(2) 0.0033(2)
Zn2 0.0485(3) 0.0331(3) 0.0388(3) 0.0035(2) 0.0193(2) 0.0069(2)
O1 0.053(2) 0.038(2) 0.035(2) 0.002(1) 0.024(1) 0.009(1)
O2 0.047(2) 0.047(2) 0.041(2) 0.009(1) 0.019(1) 0.010(1)
O3 0.038(2) 0.076(2) 0.028(1) 0.011(1) 0.010(1) 0.009(1)
O4 0.046(2) 0.047(2) 0.035(2) -0.008(1) 0.011(1) 0.003(1)
C49 0.035(3) 0.085(5) 0.184(7) -0.015(3) -0.012(4) 0.068(5)
N1 0.067(3) 0.036(2) 0.042(2) -0.005(2) -0.007(2) 0.013(2)
N2 0.062(3) 0.036(2) 0.043(2) 0.010(2) 0.011(2) 0.010(2)
N3 0.028(2) 0.031(2) 0.036(2) -0.004(1) 0.005(1) 0.006(1)
N4 0.029(2) 0.031(2) 0.040(2) 0.003(1) 0.008(1) 0.007(1)
C1 0.094(4) 0.036(3) 0.083(4) -0.001(3) -0.018(3) 0.009(3)
C2 0.093(4) 0.040(3) 0.066(3) 0.009(3) 0.003(3) 0.018(3)
C3 0.036(2) 0.033(2) 0.047(3) -0.001(2) 0.008(2) 0.019(2)
C4 0.038(2) 0.030(2) 0.056(3) 0.002(2) 0.005(2) 0.013(2)
C5 0.059(3) 0.052(3) 0.060(3) -0.022(2) -0.009(3) 0.025(3)
C6 0.026(2) 0.073(3) 0.052(3) 0.001(2) 0.006(2) 0.037(3)
C7 0.042(3) 0.056(3) 0.038(2) 0.015(2) 0.021(2) 0.022(2)
C8 0.097(4) 0.067(4) 0.048(3) 0.036(3) 0.045(3) 0.025(3)
C9 0.106(5) 0.120(6) 0.058(4) 0.059(4) 0.053(3) 0.039(4)
C10 0.058(4) 0.150(7) 0.083(5) 0.019(4) 0.041(3) 0.068(5)
C11 0.055(3) 0.118(5) 0.065(4) -0.014(3) 0.014(3) 0.056(4)
C12 0.149(6) 0.070(4) 0.051(3) 0.019(4) 0.054(4) 0.005(3)
C13 0.171(7) 0.050(3) 0.046(3) -0.030(4) 0.006(4) -0.006(3)
C14 0.185(7) 0.067(4) 0.077(4) 0.055(4) 0.057(4) 0.025(3)
C15 0.36(1) 0.095(6) 0.066(4) 0.044(7) 0.103(6) -0.003(4)
C16 0.058(3) 0.047(3) 0.055(3) 0.020(2) 0.008(2) -0.000(2)
C17 0.042(3) 0.047(3) 0.045(3) 0.000(2) 0.015(2) -0.005(2)
C18 0.040(2) 0.036(2) 0.033(2) -0.004(2) 0.012(2) -0.003(2)
C19 0.057(3) 0.043(3) 0.032(2) -0.011(2) 0.015(2) -0.009(2)
C20 0.084(4) 0.057(3) 0.053(3) -0.011(3) 0.040(3) -0.006(3)
C21 0.063(3) 0.077(4) 0.078(4) -0.014(3) 0.052(3) -0.022(3)
C22 0.045(3) 0.067(3) 0.069(3) 0.004(2) 0.015(3) -0.020(3)
C23 0.076(3) 0.061(3) 0.024(2) -0.003(3) 0.004(2) 0.005(2)
C24 0.079(4) 0.052(3) 0.039(3) 0.008(3) 0.003(2) 0.010(2)
C25 0.173(7) 0.106(5) 0.037(3) 0.022(5) 0.027(4) 0.019(3)
C26 0.083(4) 0.091(4) 0.065(4) -0.006(4) -0.028(3) -0.007(3)
C27 0.033(2) 0.034(2) 0.031(2) -0.009(2) 0.008(2) 0.005(2)
C28 0.029(2) 0.036(2) 0.030(2) -0.006(2) 0.008(2) 0.000(2)
C29 0.029(2) 0.038(2) 0.035(2) -0.005(2) 0.005(2) -0.000(2)
C30 0.033(2) 0.044(2) 0.043(2) -0.000(2) 0.010(2) 0.005(2)
C31 0.033(2) 0.059(3) 0.056(3) 0.007(2) 0.007(2) 0.000(2)
C32 0.040(3) 0.076(3) 0.043(3) 0.005(2) 0.019(2) -0.009(2)
C33 0.037(2) 0.063(3) 0.033(2) -0.006(2) 0.010(2) -0.001(2)
C34 0.029(2) 0.074(3) 0.056(3) 0.011(2) 0.008(2) 0.024(3)
C35 0.056(3) 0.094(4) 0.085(4) 0.011(3) 0.020(3) 0.050(3)
C36 0.046(3) 0.125(5) 0.075(4) 0.027(3) 0.011(3) 0.041(4)
C37 0.045(3) 0.125(5) 0.037(3) 0.002(3) -0.001(2) 0.023(3)
C38 0.030(2) 0.036(2) 0.033(2) 0.007(2) -0.002(2) 0.001(2)
C39 0.021(2) 0.039(2) 0.037(2) 0.005(2) 0.004(2) 0.009(2)
C40 0.028(2) 0.037(2) 0.037(2) 0.007(2) 0.006(2) 0.009(2)
C41 0.029(2) 0.037(2) 0.056(3) 0.005(2) 0.012(2) 0.013(2)
C42 0.034(2) 0.048(3) 0.069(3) 0.004(2) 0.025(2) 0.016(2)
C43 0.043(3) 0.069(3) 0.049(3) 0.010(2) 0.023(2) 0.013(2)
C44 0.036(2) 0.054(3) 0.040(2) 0.007(2) 0.013(2) 0.003(2)
C45 0.034(2) 0.043(3) 0.075(3) -0.006(2) 0.005(2) 0.003(2)
C46 0.053(3) 0.045(3) 0.071(3) -0.006(2) 0.017(3) -0.005(2)
C47 0.047(3) 0.055(3) 0.130(5) -0.016(2) 0.032(3) -0.001(3)
C48 0.050(3) 0.069(4) 0.092(4) -0.007(3) -0.019(3) -0.006(3)
C50 0.110(8) 0.079(6) 0.60(3) -0.032(6) -0.12(1) 0.11(1)
C51 0.23(2) 0.098(9) 0.68(4) 0.01(1) -0.02(2) 0.04(1)
C52 0.133(9) 0.26(1) 0.23(1) 0.06(1) 0.114(9) 0.11(1)
O5 0.154(9) 0.20(1) 0.85(3) -0.045(8) 0.10(1) -0.07(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 6.1.1.4)
;
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)
;
Zn Zn 0.284 1.430
;
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_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 . Zn1 . O3 . 116.10(12) yes
O1 . Zn1 . N1 . 96.37(14) yes
O3 . Zn1 . N1 . 102.73(14) yes
O1 . Zn1 . N3 . 120.96(12) yes
O3 . Zn1 . N3 . 94.99(12) yes
N1 . Zn1 . N3 . 125.49(14) yes
O2 . Zn2 . O4 . 120.76(12) yes
O2 . Zn2 . N2 . 95.12(13) yes
O4 . Zn2 . N2 . 110.51(13) yes
O2 . Zn2 . N4 . 117.52(12) yes
O4 . Zn2 . N4 . 94.82(12) yes
N2 . Zn2 . N4 . 119.84(14) yes
Zn1 . O1 . C7 . 127.1(3) yes
Zn2 . O2 . C18 . 126.2(3) yes
Zn1 . O3 . C29 . 125.4(2) yes
Zn2 . O4 . C40 . 123.7(2) yes
C50 . C49 . O5 . 99.1(9) yes
C50 . C49 . H67 . 114.8(9) no
O5 . C49 . H67 . 110.9(9) no
C50 . C49 . H68 . 108.5(9) no
O5 . C49 . H68 . 113.8(9) no
H67 . C49 . H68 . 109.5(9) no
Zn1 . N1 . C1 . 119.1(3) yes
Zn1 . N1 . C5 . 119.5(3) yes
C1 . N1 . C5 . 119.6(4) yes
Zn2 . N2 . C2 . 122.0(3) yes
Zn2 . N2 . C16 . 119.8(3) yes
C2 . N2 . C16 . 117.8(4) yes
Zn1 . N3 . C3 . 125.3(2) yes
Zn1 . N3 . C27 . 118.9(3) yes
C3 . N3 . C27 . 115.7(3) yes
Zn2 . N4 . C4 . 124.0(2) yes
Zn2 . N4 . C38 . 118.9(3) yes
C4 . N4 . C38 . 117.1(3) yes
N1 . C1 . C2 . 114.5(4) yes
N1 . C1 . H1 . 108.7(5) no
C2 . C1 . H1 . 109.2(6) no
N1 . C1 . H2 . 107.9(5) no
C2 . C1 . H2 . 107.0(6) no
H1 . C1 . H2 . 109.5(7) no
N2 . C2 . C1 . 114.1(4) yes
N2 . C2 . H3 . 109.1(5) no
C1 . C2 . H3 . 109.9(6) no
N2 . C2 . H4 . 107.3(5) no
C1 . C2 . H4 . 106.8(6) no
H3 . C2 . H4 . 109.5(7) no
N3 . C3 . C4 . 112.7(3) yes
N3 . C3 . H5 . 108.7(4) no
C4 . C3 . H5 . 108.0(4) no
N3 . C3 . H6 . 108.7(4) no
C4 . C3 . H6 . 109.2(4) no
H5 . C3 . H6 . 109.5(5) no
N4 . C4 . C3 . 111.7(3) yes
N4 . C4 . H7 . 109.1(4) no
C3 . C4 . H7 . 108.3(4) no
N4 . C4 . H8 . 108.7(4) no
C3 . C4 . H8 . 109.6(4) no
H7 . C4 . H8 . 109.5(5) no
N1 . C5 . C6 . 129.5(4) yes
N1 . C5 . H9 . 114.9(6) no
C6 . C5 . H9 . 115.6(5) no
C5 . C6 . C7 . 124.3(4) yes
C5 . C6 . C11 . 115.9(5) yes
C7 . C6 . C11 . 119.7(5) yes
O1 . C7 . C6 . 121.8(4) yes
O1 . C7 . C8 . 119.5(4) yes
C6 . C7 . C8 . 118.7(4) yes
C7 . C8 . C9 . 118.0(5) yes
C7 . C8 . C12 . 120.6(4) yes
C9 . C8 . C12 . 121.3(5) yes
C8 . C9 . C10 . 122.6(6) yes
C8 . C9 . H10 . 118.5(7) no
C10 . C9 . H10 . 118.8(7) no
C9 . C10 . C11 . 119.8(5) yes
C9 . C10 . H11 . 119.9(8) no
C11 . C10 . H11 . 120.3(8) no
C6 . C11 . C10 . 121.0(6) yes
C6 . C11 . H12 . 119.3(6) no
C10 . C11 . H12 . 119.7(7) no
C8 . C12 . C13 . 110.6(5) yes
C8 . C12 . C14 . 112.1(6) yes
C13 . C12 . C14 . 109.3(5) yes
C8 . C12 . C15 . 112.1(5) yes
C13 . C12 . C15 . 105.3(6) yes
C14 . C12 . C15 . 107.2(5) yes
C12 . C13 . H13 . 108.9(6) no
C12 . C13 . H14 . 109.2(6) no
H13 . C13 . H14 . 109.5(8) no
C12 . C13 . H15 . 110.3(6) no
H13 . C13 . H15 . 109.5(8) no
H14 . C13 . H15 . 109.5(8) no
C12 . C14 . H16 . 111.3(7) no
C12 . C14 . H17 . 107.3(7) no
H16 . C14 . H17 . 109.5(8) no
C12 . C14 . H18 . 109.7(7) no
H16 . C14 . H18 . 109.5(8) no
H17 . C14 . H18 . 109.5(8) no
C12 . C15 . H19 . 110.7(8) no
C12 . C15 . H20 . 109.8(8) no
H19 . C15 . H20 . 109.5(1) no
C12 . C15 . H21 . 108.0(8) no
H19 . C15 . H21 . 109.5(1) no
H20 . C15 . H21 . 109.5(1) no
N2 . C16 . C17 . 128.1(4) yes
N2 . C16 . H22 . 115.6(5) no
C17 . C16 . H22 . 116.3(5) no
C16 . C17 . C18 . 123.8(4) yes
C16 . C17 . C22 . 116.4(4) yes
C18 . C17 . C22 . 119.6(4) yes
O2 . C18 . C17 . 122.4(3) yes
O2 . C18 . C19 . 118.1(4) yes
C17 . C18 . C19 . 119.5(4) yes
C18 . C19 . C20 . 117.3(4) yes
C18 . C19 . C23 . 120.2(4) yes
C20 . C19 . C23 . 122.5(4) yes
C19 . C20 . C21 . 123.2(4) yes
C19 . C20 . H23 . 118.2(6) no
C21 . C20 . H23 . 118.6(6) no
C20 . C21 . C22 . 119.9(4) yes
C20 . C21 . H24 . 119.9(6) no
C22 . C21 . H24 . 120.3(6) no
C17 . C22 . C21 . 120.4(5) yes
C17 . C22 . H25 . 119.5(6) no
C21 . C22 . H25 . 120.2(6) no
C19 . C23 . C24 . 110.5(3) yes
C19 . C23 . C25 . 111.5(4) yes
C24 . C23 . C25 . 106.6(4) yes
C19 . C23 . C26 . 110.4(4) yes
C24 . C23 . C26 . 110.2(4) yes
C25 . C23 . C26 . 107.5(4) yes
C23 . C24 . H26 . 109.5(5) no
C23 . C24 . H27 . 109.6(5) no
H26 . C24 . H27 . 109.5(6) no
C23 . C24 . H28 . 109.3(5) no
H26 . C24 . H28 . 109.5(6) no
H27 . C24 . H28 . 109.5(6) no
C23 . C25 . H29 . 109.7(6) no
C23 . C25 . H30 . 108.9(6) no
H29 . C25 . H30 . 109.5(8) no
C23 . C25 . H31 . 109.7(6) no
H29 . C25 . H31 . 109.5(8) no
H30 . C25 . H31 . 109.5(8) no
C23 . C26 . H32 . 109.6(6) no
C23 . C26 . H33 . 109.1(6) no
H32 . C26 . H33 . 109.5(7) no
C23 . C26 . H34 . 109.8(6) no
H32 . C26 . H34 . 109.5(7) no
H33 . C26 . H34 . 109.5(7) no
N3 . C27 . C28 . 128.8(3) yes
N3 . C27 . H35 . 115.6(4) no
C28 . C27 . H35 . 115.6(4) no
C27 . C28 . C29 . 124.7(3) yes
C27 . C28 . C33 . 115.7(3) yes
C29 . C28 . C33 . 119.6(4) yes
O3 . C29 . C28 . 121.7(3) yes
O3 . C29 . C30 . 119.1(3) yes
C28 . C29 . C30 . 119.1(3) yes
C29 . C30 . C31 . 117.9(4) yes
C29 . C30 . C34 . 119.5(3) yes
C31 . C30 . C34 . 122.6(4) yes
C30 . C31 . C32 . 123.0(4) yes
C30 . C31 . H36 . 118.1(5) no
C32 . C31 . H36 . 118.9(5) no
C31 . C32 . C33 . 119.6(4) yes
C31 . C32 . H37 . 120.2(5) no
C33 . C32 . H37 . 120.2(5) no
C28 . C33 . C32 . 120.8(4) yes
C28 . C33 . H38 . 119.3(5) no
C32 . C33 . H38 . 119.9(5) no
C30 . C34 . C35 . 110.0(4) yes
C30 . C34 . C36 . 111.6(4) yes
C35 . C34 . C36 . 107.9(4) yes
C30 . C34 . C37 . 110.5(4) yes
C35 . C34 . C37 . 109.9(4) yes
C36 . C34 . C37 . 106.8(4) yes
C34 . C35 . H39 . 110.5(6) no
C34 . C35 . H40 . 109.9(6) no
H39 . C35 . H40 . 109.5(7) no
C34 . C35 . H41 . 108.0(6) no
H39 . C35 . H41 . 109.5(7) no
H40 . C35 . H41 . 109.5(7) no
C34 . C36 . H42 . 107.7(6) no
C34 . C36 . H43 . 110.5(6) no
H42 . C36 . H43 . 109.5(7) no
C34 . C36 . H44 . 110.2(6) no
H42 . C36 . H44 . 109.5(7) no
H43 . C36 . H44 . 109.5(7) no
C34 . C37 . H45 . 108.8(5) no
C34 . C37 . H46 . 110.3(5) no
H45 . C37 . H46 . 109.5(6) no
C34 . C37 . H47 . 109.3(5) no
H45 . C37 . H47 . 109.5(6) no
H46 . C37 . H47 . 109.5(6) no
N4 . C38 . C39 . 127.3(4) yes
N4 . C38 . H48 . 116.3(4) no
C39 . C38 . H48 . 116.4(4) no
C38 . C39 . C40 . 124.4(3) yes
C38 . C39 . C44 . 115.1(4) yes
C40 . C39 . C44 . 120.5(4) yes
O4 . C40 . C39 . 122.5(3) yes
O4 . C40 . C41 . 118.9(4) yes
C39 . C40 . C41 . 118.6(4) yes
C40 . C41 . C42 . 117.7(4) yes
C40 . C41 . C45 . 119.8(4) yes
C42 . C41 . C45 . 122.5(4) yes
C41 . C42 . C43 . 123.6(4) yes
C41 . C42 . H49 . 118.1(5) no
C43 . C42 . H49 . 118.4(5) no
C42 . C43 . C44 . 119.6(4) yes
C42 . C43 . H50 . 120.1(5) no
C44 . C43 . H50 . 120.4(5) no
C39 . C44 . C43 . 120.1(4) yes
C39 . C44 . H51 . 119.8(5) no
C43 . C44 . H51 . 120.1(5) no
C41 . C45 . C46 . 111.3(3) yes
C41 . C45 . C47 . 111.6(4) yes
C46 . C45 . C47 . 106.8(4) yes
C41 . C45 . C48 . 109.8(4) yes
C46 . C45 . C48 . 109.7(4) yes
C47 . C45 . C48 . 107.5(4) yes
C45 . C46 . H52 . 109.5(5) no
C45 . C46 . H53 . 109.5(5) no
H52 . C46 . H53 . 109.5(6) no
C45 . C46 . H54 . 109.4(5) no
H52 . C46 . H54 . 109.5(6) no
H53 . C46 . H54 . 109.5(6) no
C45 . C47 . H55 . 109.7(5) no
C45 . C47 . H56 . 109.2(5) no
H55 . C47 . H56 . 109.5(7) no
C45 . C47 . H57 . 109.5(5) no
H55 . C47 . H57 . 109.5(7) no
H56 . C47 . H57 . 109.5(7) no
C45 . C48 . H58 . 109.2(5) no
C45 . C48 . H59 . 109.6(5) no
H58 . C48 . H59 . 109.5(7) no
C45 . C48 . H60 . 109.6(5) no
H58 . C48 . H60 . 109.5(7) no
H59 . C48 . H60 . 109.5(7) no
C49 . C50 . C51 . 107.8(9) yes
C49 . C50 . H61 . 111.0(1) no
C51 . C50 . H61 . 110.8(1) no
C49 . C50 . H62 . 108.1(1) no
C51 . C50 . H62 . 109.7(1) no
H61 . C50 . H62 . 109.5(2) no
C50 . C51 . C52 . 100.1(11) yes
C50 . C51 . H63 . 110.9(2) no
C52 . C51 . H63 . 112.7(2) no
C50 . C51 . H64 . 113.0(2) no
C52 . C51 . H64 . 110.4(2) no
H63 . C51 . H64 . 109.5(2) no
C51 . C52 . O5 . 99.3(10) yes
C51 . C52 . H65 . 110.4(1) no
O5 . C52 . H65 . 115.1(2) no
C51 . C52 . H66 . 112.5(1) no
O5 . C52 . H66 . 109.7(1) no
H65 . C52 . H66 . 109.5(2) no
C49 . O5 . C52 . 116.2(11) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Zn1 . O1 . 1.896(3) yes
Zn1 . O3 . 1.920(3) yes
Zn1 . N1 . 1.985(4) yes
Zn1 . N3 . 1.995(3) yes
Zn2 . O2 . 1.900(3) yes
Zn2 . O4 . 1.902(3) yes
Zn2 . N2 . 1.998(3) yes
Zn2 . N4 . 2.010(3) yes
O1 . C7 . 1.309(4) yes
O2 . C18 . 1.309(4) yes
O3 . C29 . 1.302(4) yes
O4 . C40 . 1.303(4) yes
C49 . C50 . 1.305(9) yes
C49 . O5 . 1.308(12) yes
C49 . H67 . 0.95(2) no
C49 . H68 . 0.95(1) no
N1 . C1 . 1.523(6) yes
N1 . C5 . 1.273(6) yes
N2 . C2 . 1.489(5) yes
N2 . C16 . 1.291(5) yes
N3 . C3 . 1.476(5) yes
N3 . C27 . 1.290(4) yes
N4 . C4 . 1.472(5) yes
N4 . C38 . 1.300(4) yes
C1 . C2 . 1.427(6) yes
C1 . H1 . 0.950(7) no
C1 . H2 . 0.95(1) no
C2 . H3 . 0.950(7) no
C2 . H4 . 0.95(1) no
C3 . C4 . 1.510(5) yes
C3 . H5 . 0.95(1) no
C3 . H6 . 0.950(6) no
C4 . H7 . 0.95(1) no
C4 . H8 . 0.95(1) no
C5 . C6 . 1.442(7) yes
C5 . H9 . 0.950(7) no
C6 . C7 . 1.431(6) yes
C6 . C11 . 1.404(6) yes
C7 . C8 . 1.419(6) yes
C8 . C9 . 1.394(7) yes
C8 . C12 . 1.482(8) yes
C9 . C10 . 1.389(9) yes
C9 . H10 . 0.95(1) no
C10 . C11 . 1.349(8) yes
C10 . H11 . 0.95(2) no
C11 . H12 . 0.950(9) no
C12 . C13 . 1.513(8) yes
C12 . C14 . 1.532(8) yes
C12 . C15 . 1.554(7) yes
C13 . H13 . 0.950(9) no
C13 . H14 . 0.95(2) no
C13 . H15 . 0.950(8) no
C14 . H16 . 0.950(8) no
C14 . H17 . 0.95(1) no
C14 . H18 . 0.950(9) no
C15 . H19 . 0.95(1) no
C15 . H20 . 0.95(2) no
C15 . H21 . 0.95(1) no
C16 . C17 . 1.445(6) yes
C16 . H22 . 0.950(8) no
C17 . C18 . 1.425(6) yes
C17 . C22 . 1.409(6) yes
C18 . C19 . 1.433(5) yes
C19 . C20 . 1.380(6) yes
C19 . C23 . 1.530(6) yes
C20 . C21 . 1.394(7) yes
C20 . H23 . 0.950(7) no
C21 . C22 . 1.362(7) yes
C21 . H24 . 0.95(1) no
C22 . H25 . 0.95(1) no
C23 . C24 . 1.534(6) yes
C23 . C25 . 1.546(6) yes
C23 . C26 . 1.519(7) yes
C24 . H26 . 0.950(8) no
C24 . H27 . 0.950(8) no
C24 . H28 . 0.95(1) no
C25 . H29 . 0.950(9) no
C25 . H30 . 0.95(1) no
C25 . H31 . 0.95(2) no
C26 . H32 . 0.95(1) no
C26 . H33 . 0.95(1) no
C26 . H34 . 0.950(8) no
C27 . C28 . 1.440(5) yes
C27 . H35 . 0.950(5) no
C28 . C29 . 1.418(5) yes
C28 . C33 . 1.414(5) yes
C29 . C30 . 1.433(5) yes
C30 . C31 . 1.381(5) yes
C30 . C34 . 1.539(6) yes
C31 . C32 . 1.392(6) yes
C31 . H36 . 0.950(9) no
C32 . C33 . 1.357(6) yes
C32 . H37 . 0.95(2) no
C33 . H38 . 0.95(1) no
C34 . C35 . 1.544(6) yes
C34 . C36 . 1.534(6) yes
C34 . C37 . 1.533(7) yes
C35 . H39 . 0.950(8) no
C35 . H40 . 0.95(1) no
C35 . H41 . 0.950(8) no
C36 . H42 . 0.950(8) no
C36 . H43 . 0.95(1) no
C36 . H44 . 0.950(9) no
C37 . H45 . 0.950(9) no
C37 . H46 . 0.95(1) no
C37 . H47 . 0.950(8) no
C38 . C39 . 1.450(5) yes
C38 . H48 . 0.950(6) no
C39 . C40 . 1.422(5) yes
C39 . C44 . 1.407(5) yes
C40 . C41 . 1.439(5) yes
C41 . C42 . 1.373(6) yes
C41 . C45 . 1.529(6) yes
C42 . C43 . 1.390(6) yes
C42 . H49 . 0.950(8) no
C43 . C44 . 1.367(6) yes
C43 . H50 . 0.95(1) no
C44 . H51 . 0.95(1) no
C45 . C46 . 1.544(6) yes
C45 . C47 . 1.545(6) yes
C45 . C48 . 1.525(6) yes
C46 . H52 . 0.95(1) no
C46 . H53 . 0.95(2) no
C46 . H54 . 0.95(1) no
C47 . H55 . 0.95(1) no
C47 . H56 . 0.95(2) no
C47 . H57 . 0.95(1) no
C48 . H58 . 0.95(1) no
C48 . H59 . 0.95(1) no
C48 . H60 . 0.95(1) no
C50 . C51 . 1.379(14) yes
C50 . H61 . 0.95(2) no
C50 . H62 . 0.95(2) no
C51 . C52 . 1.505(14) yes
C51 . H63 . 0.95(3) no
C51 . H64 . 0.95(2) no
C52 . O5 . 1.309(13) yes
C52 . H65 . 0.95(3) no
C52 . H66 . 0.95(2) no
loop_
_geom_contact_atom_site_label_1
_geom_contact_site_symmetry_1
_geom_contact_atom_site_label_2
_geom_contact_site_symmetry_2
_geom_contact_distance
_geom_contact_publ_flag
Zn1 . O1 . 1.896(3) yes
Zn1 . O3 . 1.920(3) yes
Zn1 . N1 . 1.985(4) yes
Zn1 . N3 . 1.995(3) yes
Zn1 . N4 . 3.241(3) yes
Zn1 . C1 . 3.033(5) yes
Zn1 . C3 . 3.093(4) yes
Zn1 . C4 . 3.222(4) yes
Zn1 . C5 . 2.837(5) yes
Zn1 . C6 . 3.233(4) yes
Zn1 . C7 . 2.881(4) yes
Zn1 . C27 . 2.852(4) yes
Zn1 . C28 . 3.218(4) yes
Zn1 . C29 . 2.877(4) yes
Zn1 . H2 . 2.940(5) no
Zn1 . H7 . 2.920(4) no
Zn1 . H39 . 3.598(5) no
Zn2 . O2 . 1.900(3) yes
Zn2 . O4 . 1.902(3) yes
Zn2 . N2 . 1.998(3) yes
Zn2 . N3 . 3.535(3) yes
Zn2 . N4 . 2.010(3) yes
Zn2 . C2 . 3.060(5) yes
Zn2 . C3 . 3.226(4) yes
Zn2 . C4 . 3.084(4) yes
Zn2 . C16 . 2.868(5) yes
Zn2 . C17 . 3.231(4) yes
Zn2 . C18 . 2.874(4) yes
Zn2 . C38 . 2.873(4) yes
Zn2 . C39 . 3.209(4) yes
Zn2 . C40 . 2.840(4) yes
Zn2 . H4 . 2.966(4) no
Zn2 . H5 . 2.766(4) no
Zn2 . H8 . 3.519(4) no
Zn2 . H54 . 3.464(5) no
O1 . O3 . 3.237(4) yes
O1 . N1 . 2.893(4) yes
O1 . N3 . 3.386(4) yes
O1 . N4 . 3.521(4) yes
O1 . C4 . 3.413(5) yes
O1 . C5 . 2.937(5) yes
O1 . C6 . 2.394(5) yes
O1 . C7 . 1.309(4) yes
O1 . C8 . 2.357(5) yes
O1 . C12 . 2.822(6) yes
O1 . C13 . 2.910(6) yes
O1 . C14 . 3.015(6) yes
O1 . C38 . 3.352(5) yes
O1 . H7 . 2.691(5) no
O1 . H13 . 2.260(6) no
O1 . H14 . 3.368(6) no
O1 . H17 . 3.510(6) no
O1 . H18 . 2.406(6) no
O1 . H48 . 3.035(5) no
O2 . O4 . 3.305(4) yes
O2 . N2 . 2.878(4) yes
O2 . N4 . 3.343(4) yes
O2 . C3 . 3.428(5) yes
O2 . C16 . 2.935(5) yes
O2 . C17 . 2.396(5) yes
O2 . C18 . 1.309(4) yes
O2 . C19 . 2.352(5) yes
O2 . C20 . 3.585(5) yes
O2 . C23 . 2.824(5) yes
O2 . C24 . 2.988(5) yes
O2 . C26 . 2.917(6) yes
O2 . H5 . 2.559(5) no
O2 . H26 . 3.487(5) no
O2 . H27 . 2.371(5) no
O2 . H33 . 2.273(6) no
O2 . H34 . 3.378(6) no
O3 . N1 . 3.050(5) yes
O3 . N3 . 2.887(4) yes
O3 . C1 . 3.515(6) yes
O3 . C27 . 2.922(5) yes
O3 . C28 . 2.377(4) yes
O3 . C29 . 1.302(4) yes
O3 . C30 . 2.359(5) yes
O3 . C31 . 3.594(5) yes
O3 . C34 . 2.832(5) yes
O3 . C35 . 2.971(6) yes
O3 . C37 . 2.939(5) yes
O3 . H2 . 2.974(6) no
O3 . H35 2_553 3.488(5) no
O3 . H39 . 2.356(6) no
O3 . H41 . 3.454(6) no
O3 . H45 . 3.421(5) no
O3 . H47 . 2.294(5) no
O4 . N2 . 3.205(5) yes
O4 . N4 . 2.881(4) yes
O4 . C2 . 3.597(6) yes
O4 . C38 . 2.943(5) yes
O4 . C39 . 2.390(5) yes
O4 . C40 . 1.303(4) yes
O4 . C41 . 2.363(5) yes
O4 . C42 . 3.590(5) yes
O4 . C45 . 2.836(5) yes
O4 . C46 . 2.933(5) yes
O4 . C48 . 2.992(6) yes
O4 . H4 . 2.994(6) no
O4 . H53 . 3.412(5) no
O4 . H54 . 2.291(5) no
O4 . H58 . 2.356(5) no
O4 . H59 . 3.511(6) no
C49 . C1 4_545 3.331(8) yes
C49 . C2 4_545 3.383(8) yes
C49 . C16 4_545 3.435(8) yes
C49 . C50 . 1.305(9) yes
C49 . C51 . 2.168(15) yes
C49 . C52 . 2.221(11) yes
C49 . O5 . 1.308(12) yes
C49 . H1 4_545 3.359(9) no
C49 . H2 4_545 2.773(8) no
C49 . H3 4_545 2.791(8) no
C49 . H22 4_545 2.526(8) no
C49 . H61 . 1.869(11) no
C49 . H62 . 1.837(13) no
C49 . H63 . 2.558(16) no
C49 . H64 . 2.978(16) no
C49 . H65 . 2.816(12) no
C49 . H66 . 2.90(1) no
C49 . H67 . 0.95(2) no
C49 . H68 . 0.95(1) no
N1 . N2 . 3.047(5) yes
N1 . N3 . 3.538(5) yes
N1 . C1 . 1.523(6) yes
N1 . C2 . 2.482(6) yes
N1 . C5 . 1.273(6) yes
N1 . C6 . 2.457(6) yes
N1 . C7 . 3.066(6) yes
N1 . H1 . 2.038(6) no
N1 . H2 . 2.028(7) no
N1 . H3 . 3.294(6) no
N1 . H4 . 2.587(6) no
N1 . H9 . 1.882(5) no
N1 . H39 . 3.380(6) no
N2 . N3 . 3.499(5) yes
N2 . N4 . 3.468(5) yes
N2 . C1 . 2.448(6) yes
N2 . C2 . 1.489(5) yes
N2 . C16 . 1.291(5) yes
N2 . C17 . 2.461(5) yes
N2 . C18 . 3.053(5) yes
N2 . H1 . 3.254(6) no
N2 . H2 . 2.567(6) no
N2 . H3 . 2.012(5) no
N2 . H4 . 1.991(6) no
N2 . H5 . 3.568(5) no
N2 . H12 4_544 3.182(6) no
N2 . H22 . 1.905(5) no
N2 . H54 . 3.540(6) no
N2 . H67 4_544 3.031(7) no
N3 . N4 . 3.039(4) yes
N3 . C3 . 1.476(5) yes
N3 . C4 . 2.486(5) yes
N3 . C27 . 1.290(4) yes
N3 . C28 . 2.462(5) yes
N3 . C29 . 3.066(5) yes
N3 . H5 . 1.995(5) no
N3 . H6 . 1.995(5) no
N3 . H7 . 2.608(5) no
N3 . H8 . 3.289(5) no
N3 . H35 . 1.904(4) no
N4 . C3 . 2.468(5) yes
N4 . C4 . 1.472(5) yes
N4 . C38 . 1.300(4) yes
N4 . C39 . 2.465(5) yes
N4 . C40 . 3.053(5) yes
N4 . H5 . 2.583(5) no
N4 . H6 . 3.271(5) no
N4 . H7 . 1.996(5) no
N4 . H8 . 1.992(5) no
N4 . H48 . 1.921(5) no
C1 . C2 . 1.427(6) yes
C1 . C5 . 2.419(8) yes
C1 . C16 . 3.166(7) yes
C1 . H1 . 0.950(7) no
C1 . H2 . 0.95(1) no
C1 . H3 . 1.965(7) no
C1 . H4 . 1.929(7) no
C1 . H9 . 2.472(8) no
C1 . H22 . 3.055(7) no
C1 . H39 . 3.318(8) no
C1 . H67 4_544 2.946(9) no
C1 . H68 4_544 2.847(8) no
C2 . C5 . 3.295(8) yes
C2 . C16 . 2.382(7) yes
C2 . H1 . 1.958(6) no
C2 . H2 . 1.931(7) no
C2 . H3 . 0.950(7) no
C2 . H4 . 0.95(1) no
C2 . H9 . 3.238(8) no
C2 . H11 4_544 3.243(8) no
C2 . H12 4_544 3.542(7) no
C2 . H22 . 2.443(7) no
C2 . H54 . 3.308(7) no
C2 . H67 4_544 2.697(8) no
C2 . H68 4_544 3.217(8) no
C3 . C4 . 1.510(5) yes
C3 . C27 . 2.344(5) yes
C3 . C31 2_553 3.470(6) yes
C3 . H5 . 0.95(1) no
C3 . H6 . 0.950(6) no
C3 . H7 . 2.021(6) no
C3 . H8 . 2.036(5) no
C3 . H27 . 3.529(6) no
C3 . H35 . 2.389(5) no
C3 . H45 2_553 3.269(6) no
C4 . C38 . 2.366(5) yes
C4 . H5 . 2.018(6) no
C4 . H6 . 2.032(5) no
C4 . H7 . 0.95(1) no
C4 . H8 . 0.95(1) no
C4 . H18 . 3.462(7) no
C4 . H48 . 2.436(5) no
C5 . C6 . 1.442(7) yes
C5 . C7 . 2.540(7) yes
C5 . C11 . 2.413(8) yes
C5 . H1 . 2.500(8) no
C5 . H2 . 3.099(8) no
C5 . H4 . 3.077(7) no
C5 . H9 . 0.950(7) no
C5 . H12 . 2.543(7) no
C6 . C7 . 1.431(6) yes
C6 . C8 . 2.453(8) yes
C6 . C9 . 2.762(8) yes
C6 . C10 . 2.396(8) yes
C6 . C11 . 1.404(6) yes
C6 . C44 . 3.383(6) yes
C6 . H9 . 2.041(7) no
C6 . H11 . 3.256(7) no
C6 . H12 . 2.044(6) no
C6 . H48 . 3.583(5) no
C6 . H51 . 3.189(6) no
C6 . H62 . 3.418(12) no
C7 . C8 . 1.419(6) yes
C7 . C9 . 2.411(6) yes
C7 . C10 . 2.810(6) yes
C7 . C11 . 2.452(6) yes
C7 . C12 . 2.521(8) yes
C7 . C13 . 3.027(7) yes
C7 . C14 . 3.119(7) yes
C7 . C38 . 3.548(6) yes
C7 . H9 . 3.349(7) no
C7 . H10 . 3.267(6) no
C7 . H12 . 3.307(7) no
C7 . H13 . 2.727(7) no
C7 . H14 . 3.259(7) no
C7 . H17 . 3.380(7) no
C7 . H18 . 2.837(7) no
C7 . H48 . 3.181(5) no
C7 . H51 . 3.377(6) no
C7 . H62 . 3.226(11) no
C8 . C9 . 1.394(7) yes
C8 . C10 . 2.441(8) yes
C8 . C11 . 2.810(8) yes
C8 . C12 . 1.482(8) yes
C8 . C13 . 2.462(8) yes
C8 . C14 . 2.501(7) yes
C8 . C15 . 2.519(9) yes
C8 . H10 . 2.027(6) no
C8 . H11 . 3.289(8) no
C8 . H13 . 2.641(8) no
C8 . H14 . 2.639(8) no
C8 . H15 . 3.283(8) no
C8 . H16 . 3.322(7) no
C8 . H17 . 2.669(7) no
C8 . H18 . 2.685(7) no
C8 . H19 . 3.332(9) no
C8 . H20 . 2.707(9) no
C8 . H21 . 2.696(8) no
C8 . H51 . 3.590(7) no
C8 . H61 . 3.306(12) no
C8 . H62 . 3.28(1) no
C9 . C10 . 1.389(9) yes
C9 . C11 . 2.37(1) yes
C9 . C12 . 2.51(1) yes
C9 . C13 . 3.59(1) yes
C9 . C14 . 3.529(9) yes
C9 . C15 . 2.809(11) yes
C9 . H10 . 0.95(1) no
C9 . H11 . 2.036(8) no
C9 . H12 . 3.23(1) no
C9 . H14 . 3.53(1) no
C9 . H17 . 3.394(8) no
C9 . H20 . 2.753(12) no
C9 . H21 . 2.66(1) no
C9 . H29 1_556 3.205(7) no
C9 . H51 . 3.522(8) no
C9 . H61 . 3.187(11) no
C9 . H62 . 3.581(12) no
C10 . C11 . 1.349(8) yes
C10 . H3 4_545 2.896(8) no
C10 . H10 . 2.03(1) no
C10 . H11 . 0.95(2) no
C10 . H12 . 2.00(1) no
C10 . H29 1_556 3.53(1) no
C10 . H51 . 3.335(7) no
C10 . H52 4_545 3.463(7) no
C10 . H54 4_545 3.376(8) no
C10 . H61 . 3.597(12) no
C11 . C16 4_545 3.525(7) yes
C11 . C44 . 3.418(6) yes
C11 . H3 4_545 3.182(7) no
C11 . H9 . 2.500(9) no
C11 . H10 . 3.22(1) no
C11 . H11 . 2.004(7) no
C11 . H12 . 0.950(9) no
C11 . H22 4_545 3.391(7) no
C11 . H51 . 3.195(6) no
C12 . C13 . 1.513(8) yes
C12 . C14 . 1.532(8) yes
C12 . C15 . 1.554(7) yes
C12 . H10 . 2.653(9) no
C12 . H13 . 2.030(8) no
C12 . H14 . 2.034(8) no
C12 . H15 . 2.047(8) no
C12 . H16 . 2.076(7) no
C12 . H17 . 2.029(9) no
C12 . H18 . 2.058(7) no
C12 . H19 . 2.088(8) no
C12 . H20 . 2.078(7) no
C12 . H21 . 2.056(8) no
C13 . C14 . 2.483(9) yes
C13 . C15 . 2.44(1) yes
C13 . H13 . 0.950(9) no
C13 . H14 . 0.95(2) no
C13 . H15 . 0.950(8) no
C13 . H16 . 2.661(8) no
C13 . H17 . 3.29(1) no
C13 . H18 . 2.698(9) no
C13 . H19 . 2.614(9) no
C13 . H20 . 2.621(9) no
C13 . H21 . 3.260(11) no
C13 . H38 2_553 3.544(7) no
C13 . H62 . 3.53(1) no
C13 . H64 . 3.507(17) no
C14 . C15 . 2.484(8) yes
C14 . C48 2_453 3.424(7) yes
C14 . H7 . 3.478(7) no
C14 . H13 . 2.676(9) no
C14 . H14 . 3.305(9) no
C14 . H15 . 2.64(1) no
C14 . H16 . 0.950(8) no
C14 . H17 . 0.95(1) no
C14 . H18 . 0.950(9) no
C14 . H19 . 2.645(9) no
C14 . H20 . 3.313(9) no
C14 . H21 . 2.653(8) no
C14 . H37 2_553 3.323(8) no
C14 . H48 . 3.514(8) no
C14 . H58 2_453 2.912(7) no
C14 . H59 2_453 3.198(7) no
C15 . C47 3_453 3.413(8) yes
C15 . H10 . 2.395(11) no
C15 . H13 . 3.275(9) no
C15 . H14 . 2.605(11) no
C15 . H15 . 2.59(1) no
C15 . H16 . 2.649(8) no
C15 . H17 . 2.64(1) no
C15 . H18 . 3.317(8) no
C15 . H19 . 0.95(1) no
C15 . H20 . 0.95(2) no
C15 . H21 . 0.95(1) no
C15 . H42 3_553 3.435(9) no
C15 . H55 3_453 3.244(8) no
C15 . H56 3_453 3.032(8) no
C15 . H57 3_453 3.408(8) no
C15 . H65 2_554 3.352(18) no
C16 . C17 . 1.445(6) yes
C16 . C18 . 2.532(6) yes
C16 . C22 . 2.426(7) yes
C16 . C27 . 3.553(6) yes
C16 . H2 . 2.906(7) no
C16 . H3 . 2.494(6) no
C16 . H4 . 3.103(7) no
C16 . H12 4_544 2.975(7) no
C16 . H22 . 0.950(8) no
C16 . H25 . 2.563(7) no
C16 . H67 4_544 2.526(8) no
C17 . C18 . 1.425(6) yes
C17 . C19 . 2.469(6) yes
C17 . C20 . 2.769(7) yes
C17 . C21 . 2.404(6) yes
C17 . C22 . 1.409(6) yes
C17 . C27 . 3.475(6) yes
C17 . H5 . 3.231(6) no
C17 . H9 4_544 3.255(6) no
C17 . H12 4_544 3.417(8) no
C17 . H22 . 2.051(6) no
C17 . H24 . 3.266(6) no
C17 . H25 . 2.050(6) no
C17 . H35 . 3.301(6) no
C18 . C19 . 1.433(5) yes
C18 . C20 . 2.402(6) yes
C18 . C21 . 2.802(6) yes
C18 . C22 . 2.449(6) yes
C18 . C23 . 2.568(6) yes
C18 . C24 . 3.138(6) yes
C18 . C26 . 3.063(6) yes
C18 . H5 . 2.759(6) no
C18 . H22 . 3.338(6) no
C18 . H23 . 3.261(6) no
C18 . H25 . 3.305(6) no
C18 . H26 . 3.411(6) no
C18 . H27 . 2.847(6) no
C18 . H33 . 2.761(6) no
C18 . H34 . 3.293(6) no
C19 . C20 . 1.380(6) yes
C19 . C21 . 2.440(7) yes
C19 . C22 . 2.828(7) yes
C19 . C23 . 1.530(6) yes
C19 . C24 . 2.517(6) yes
C19 . C25 . 2.543(7) yes
C19 . C26 . 2.503(7) yes
C19 . H5 . 3.471(6) no
C19 . H23 . 2.011(6) no
C19 . H24 . 3.285(7) no
C19 . H26 . 2.700(6) no
C19 . H27 . 2.694(6) no
C19 . H28 . 3.333(6) no
C19 . H29 . 2.726(6) no
C19 . H30 . 2.720(7) no
C19 . H31 . 3.357(7) no
C19 . H32 . 3.323(7) no
C19 . H33 . 2.678(7) no
C19 . H34 . 2.681(6) no
C20 . C21 . 1.394(7) yes
C20 . C22 . 2.386(8) yes
C20 . C23 . 2.552(7) yes
C20 . C24 . 3.569(7) yes
C20 . C25 . 2.853(8) yes
C20 . H1 4_544 3.108(7) no
C20 . H23 . 0.950(7) no
C20 . H24 . 2.041(7) no
C20 . H25 . 3.247(8) no
C20 . H26 . 3.472(7) no
C20 . H29 . 2.770(8) no
C20 . H30 . 2.736(8) no
C20 . H34 . 3.539(8) no
C21 . C22 . 1.362(7) yes
C21 . H1 4_544 2.759(7) no
C21 . H23 . 2.029(7) no
C21 . H24 . 0.95(1) no
C21 . H25 . 2.014(7) no
C21 . H38 . 3.566(7) no
C21 . H68 1_554 3.54(1) no
C22 . H1 4_544 3.188(7) no
C22 . H9 4_544 3.282(7) no
C22 . H22 . 2.534(7) no
C22 . H23 . 3.233(7) no
C22 . H24 . 2.015(6) no
C22 . H25 . 0.95(1) no
C22 . H35 . 3.428(6) no
C22 . H38 . 3.239(6) no
C23 . C24 . 1.534(6) yes
C23 . C25 . 1.546(6) yes
C23 . C26 . 1.519(7) yes
C23 . H23 . 2.690(7) no
C23 . H26 . 2.057(6) no
C23 . H27 . 2.057(6) no
C23 . H28 . 2.054(6) no
C23 . H29 . 2.070(6) no
C23 . H30 . 2.061(7) no
C23 . H31 . 2.070(6) no
C23 . H32 . 2.043(7) no
C23 . H33 . 2.037(7) no
C23 . H34 . 2.046(7) no
C24 . C25 . 2.470(7) yes
C24 . C26 . 2.503(7) yes
C24 . H5 . 3.399(6) no
C24 . H26 . 0.950(8) no
C24 . H27 . 0.950(8) no
C24 . H28 . 0.95(1) no
C24 . H29 . 3.302(7) no
C24 . H30 . 2.632(7) no
C24 . H31 . 2.634(6) no
C24 . H32 . 2.665(7) no
C24 . H33 . 2.687(7) no
C24 . H34 . 3.325(7) no
C24 . H45 2_553 3.521(7) no
C24 . H50 2_453 3.090(7) no
C24 . H51 2_453 3.439(6) no
C24 . H52 3_452 3.306(6) no
C25 . C26 . 2.472(9) yes
C25 . H10 1_554 3.071(7) no
C25 . H20 1_554 3.562(9) no
C25 . H23 . 2.443(9) no
C25 . H26 . 2.639(7) no
C25 . H27 . 3.304(7) no
C25 . H28 . 2.623(7) no
C25 . H29 . 0.950(9) no
C25 . H30 . 0.95(1) no
C25 . H31 . 0.95(2) no
C25 . H32 . 2.621(9) no
C25 . H33 . 3.300(8) no
C25 . H34 . 2.659(9) no
C25 . H57 3_452 3.207(8) no
C26 . H26 . 3.320(7) no
C26 . H27 . 2.703(7) no
C26 . H28 . 2.661(7) no
C26 . H29 . 2.658(8) no
C26 . H30 . 3.294(9) no
C26 . H31 . 2.638(8) no
C26 . H32 . 0.95(1) no
C26 . H33 . 0.95(1) no
C26 . H34 . 0.950(8) no
C26 . H53 4_544 3.203(7) no
C26 . H56 4_544 3.325(7) no
C27 . C28 . 1.440(5) yes
C27 . C28 2_553 3.470(5) yes
C27 . C29 . 2.531(5) yes
C27 . C29 2_553 3.572(5) yes
C27 . C33 . 2.416(6) yes
C27 . H5 . 2.579(5) no
C27 . H6 . 2.551(5) no
C27 . H35 . 0.950(5) no
C27 . H38 . 2.546(5) no
C28 . C29 . 1.418(5) yes
C28 . C30 . 2.458(6) yes
C28 . C31 . 2.769(6) yes
C28 . C32 . 2.409(6) yes
C28 . C33 . 1.414(5) yes
C28 . H35 . 2.039(5) no
C28 . H35 2_553 3.556(5) no
C28 . H37 . 3.270(6) no
C28 . H38 . 2.053(5) no
C29 . C30 . 1.433(5) yes
C29 . C31 . 2.410(6) yes
C29 . C32 . 2.810(6) yes
C29 . C33 . 2.447(5) yes
C29 . C34 . 2.567(6) yes
C29 . C35 . 3.104(6) yes
C29 . C37 . 3.090(6) yes
C29 . H2 . 3.177(6) no
C29 . H6 2_553 3.392(5) no
C29 . H35 . 3.334(5) no
C29 . H35 2_553 3.278(5) no
C29 . H36 . 3.266(6) no
C29 . H38 . 3.301(6) no
C29 . H39 . 2.817(6) no
C29 . H41 . 3.350(6) no
C29 . H45 . 3.346(6) no
C29 . H47 . 2.776(6) no
C30 . C31 . 1.381(5) yes
C30 . C32 . 2.436(6) yes
C30 . C33 . 2.813(6) yes
C30 . C34 . 1.539(6) yes
C30 . C35 . 2.526(6) yes
C30 . C36 . 2.542(6) yes
C30 . C37 . 2.524(6) yes
C30 . H6 2_553 2.796(6) no
C30 . H36 . 2.011(5) no
C30 . H37 . 3.284(6) no
C30 . H39 . 2.711(6) no
C30 . H40 . 3.347(6) no
C30 . H41 . 2.683(6) no
C30 . H42 . 2.693(6) no
C30 . H43 . 3.363(6) no
C30 . H44 . 2.733(6) no
C30 . H45 . 2.700(6) no
C30 . H46 . 3.348(6) no
C30 . H47 . 2.686(6) no
C31 . C32 . 1.392(6) yes
C31 . C33 . 2.376(6) yes
C31 . C34 . 2.563(6) yes
C31 . C35 . 3.598(6) yes
C31 . C36 . 2.861(7) yes
C31 . H6 2_553 2.622(6) no
C31 . H36 . 0.950(9) no
C31 . H37 . 2.042(6) no
C31 . H38 . 3.236(6) no
C31 . H41 . 3.485(6) no
C31 . H42 . 2.723(7) no
C31 . H44 . 2.779(7) no
C31 . H45 . 3.532(7) no
C31 . H55 1_655 3.550(7) no
C31 . H59 1_655 3.437(7) no
C32 . C33 . 1.357(6) yes
C32 . H6 2_553 3.057(6) no
C32 . H7 2_553 3.348(6) no
C32 . H18 2_553 3.580(8) no
C32 . H36 . 2.030(6) no
C32 . H37 . 0.95(2) no
C32 . H38 . 2.007(6) no
C32 . H59 1_655 3.308(7) no
C33 . H6 2_553 3.556(6) no
C33 . H13 2_553 3.543(7) no
C33 . H25 . 3.296(6) no
C33 . H35 . 2.503(6) no
C33 . H36 . 3.225(6) no
C33 . H37 . 2.011(5) no
C33 . H38 . 0.95(1) no
C34 . C35 . 1.544(6) yes
C34 . C36 . 1.534(6) yes
C34 . C37 . 1.533(7) yes
C34 . H6 2_553 3.416(6) no
C34 . H36 . 2.697(6) no
C34 . H39 . 2.077(6) no
C34 . H40 . 2.070(6) no
C34 . H41 . 2.047(7) no
C34 . H42 . 2.035(7) no
C34 . H43 . 2.068(6) no
C34 . H44 . 2.064(6) no
C34 . H45 . 2.047(7) no
C34 . H46 . 2.064(6) no
C34 . H47 . 2.052(7) no
C35 . C36 . 2.489(7) yes
C35 . C37 . 2.518(8) yes
C35 . H2 . 3.489(8) no
C35 . H15 3_543 3.581(8) no
C35 . H24 4_545 3.440(8) no
C35 . H25 4_545 3.410(6) no
C35 . H39 . 0.950(8) no
C35 . H40 . 0.95(1) no
C35 . H41 . 0.950(8) no
C35 . H42 . 2.646(7) no
C35 . H43 . 2.654(7) no
C35 . H44 . 3.321(7) no
C35 . H45 . 3.334(8) no
C35 . H46 . 2.683(8) no
C35 . H47 . 2.714(8) no
C36 . C37 . 2.462(8) yes
C36 . H16 3_543 3.408(8) no
C36 . H19 3_543 3.310(9) no
C36 . H36 . 2.451(7) no
C36 . H39 . 3.322(7) no
C36 . H40 . 2.647(7) no
C36 . H41 . 2.651(7) no
C36 . H42 . 0.950(8) no
C36 . H43 . 0.95(1) no
C36 . H44 . 0.950(9) no
C36 . H45 . 2.622(8) no
C36 . H46 . 2.636(8) no
C36 . H47 . 3.292(7) no
C36 . H49 1_655 3.092(6) no
C36 . H55 1_655 3.484(8) no
C36 . H60 4_645 3.363(7) no
C37 . H6 2_553 3.331(6) no
C37 . H26 2_553 3.372(7) no
C37 . H35 2_553 3.480(6) no
C37 . H39 . 2.726(7) no
C37 . H40 . 2.690(8) no
C37 . H41 . 3.325(8) no
C37 . H42 . 3.281(8) no
C37 . H43 . 2.644(8) no
C37 . H44 . 2.642(7) no
C37 . H45 . 0.950(9) no
C37 . H46 . 0.95(1) no
C37 . H47 . 0.950(8) no
C37 . H66 . 3.07(1) no
C38 . C39 . 1.450(5) yes
C38 . C40 . 2.541(6) yes
C38 . C44 . 2.412(6) yes
C38 . H7 . 2.473(5) no
C38 . H8 . 2.738(5) no
C38 . H48 . 0.950(6) no
C38 . H48 2_453 3.546(7) no
C38 . H51 . 2.544(6) no
C39 . C40 . 1.422(5) yes
C39 . C41 . 2.460(6) yes
C39 . C42 . 2.758(6) yes
C39 . C43 . 2.403(6) yes
C39 . C44 . 1.407(5) yes
C39 . H8 2_453 2.961(5) no
C39 . H48 . 2.057(5) no
C39 . H50 . 3.265(6) no
C39 . H51 . 2.052(5) no
C40 . C41 . 1.439(5) yes
C40 . C42 . 2.407(6) yes
C40 . C43 . 2.813(6) yes
C40 . C44 . 2.456(6) yes
C40 . C45 . 2.569(6) yes
C40 . C46 . 3.103(6) yes
C40 . C48 . 3.101(6) yes
C40 . H4 . 3.238(6) no
C40 . H8 2_453 3.275(5) no
C40 . H48 . 3.349(6) no
C40 . H49 . 3.264(6) no
C40 . H51 . 3.312(6) no
C40 . H53 . 3.366(6) no
C40 . H54 . 2.798(6) no
C40 . H58 . 2.778(6) no
C40 . H59 . 3.385(6) no
C41 . C42 . 1.373(6) yes
C41 . C43 . 2.435(6) yes
C41 . C44 . 2.825(6) yes
C41 . C45 . 1.529(6) yes
C41 . C46 . 2.537(6) yes
C41 . C47 . 2.543(6) yes
C41 . C48 . 2.498(6) yes
C41 . H8 2_453 3.430(6) no
C41 . H49 . 2.004(5) no
C41 . H50 . 3.280(6) no
C41 . H52 . 3.350(6) no
C41 . H53 . 2.731(6) no
C41 . H54 . 2.707(6) no
C41 . H55 . 2.719(6) no
C41 . H56 . 2.733(6) no
C41 . H57 . 3.355(6) no
C41 . H58 . 2.654(7) no
C41 . H59 . 2.691(6) no
C41 . H60 . 3.320(7) no
C42 . C43 . 1.390(6) yes
C42 . C44 . 2.383(6) yes
C42 . C45 . 2.546(7) yes
C42 . C47 . 2.851(7) yes
C42 . C48 . 3.561(7) yes
C42 . H8 2_453 3.306(6) no
C42 . H36 1_455 3.580(6) no
C42 . H44 1_455 3.006(6) no
C42 . H49 . 0.950(8) no
C42 . H50 . 2.039(6) no
C42 . H51 . 3.244(7) no
C42 . H53 . 3.563(6) no
C42 . H55 . 2.729(7) no
C42 . H56 . 2.779(7) no
C42 . H59 . 3.479(7) no
C43 . C44 . 1.367(6) yes
C43 . H8 2_453 3.016(6) no
C43 . H12 . 3.594(7) no
C43 . H27 2_453 3.378(7) no
C43 . H28 2_453 3.495(7) no
C43 . H44 1_455 3.174(7) no
C43 . H49 . 2.023(6) no
C43 . H50 . 0.95(1) no
C43 . H51 . 2.018(6) no
C44 . H8 2_453 2.817(6) no
C44 . H27 2_453 3.326(6) no
C44 . H48 . 2.515(6) no
C44 . H49 . 3.230(6) no
C44 . H50 . 2.020(5) no
C44 . H51 . 0.95(1) no
C45 . C46 . 1.544(6) yes
C45 . C47 . 1.545(6) yes
C45 . C48 . 1.525(6) yes
C45 . H49 . 2.681(7) no
C45 . H52 . 2.065(6) no
C45 . H53 . 2.066(6) no
C45 . H54 . 2.064(6) no
C45 . H55 . 2.068(6) no
C45 . H56 . 2.062(7) no
C45 . H57 . 2.067(6) no
C45 . H58 . 2.044(7) no
C45 . H59 . 2.050(6) no
C45 . H60 . 2.050(6) no
C46 . C47 . 2.481(6) yes
C46 . C48 . 2.510(7) yes
C46 . H4 . 3.161(7) no
C46 . H11 4_544 2.793(7) no
C46 . H28 3_442 3.440(6) no
C46 . H34 4_545 3.269(7) no
C46 . H52 . 0.95(1) no
C46 . H53 . 0.95(2) no
C46 . H54 . 0.95(1) no
C46 . H55 . 3.313(6) no
C46 . H56 . 2.644(7) no
C46 . H57 . 2.641(6) no
C46 . H58 . 2.713(7) no
C46 . H59 . 3.332(7) no
C46 . H60 . 2.650(7) no
C47 . C48 . 2.476(7) yes
C47 . H19 3_443 3.112(8) no
C47 . H20 3_443 3.589(8) no
C47 . H21 3_443 3.017(8) no
C47 . H30 3_442 3.534(8) no
C47 . H31 3_442 3.464(8) no
C47 . H36 1_455 3.548(7) no
C47 . H49 . 2.434(7) no
C47 . H52 . 2.640(7) no
C47 . H53 . 2.650(6) no
C47 . H54 . 3.311(6) no
C47 . H55 . 0.95(1) no
C47 . H56 . 0.95(2) no
C47 . H57 . 0.95(1) no
C47 . H58 . 3.304(7) no
C47 . H59 . 2.640(7) no
C47 . H60 . 2.648(8) no
C48 . H16 2_453 2.911(7) no
C48 . H17 2_453 3.417(7) no
C48 . H18 2_453 3.409(7) no
C48 . H37 1_455 3.518(7) no
C48 . H43 4_444 3.265(7) no
C48 . H52 . 2.663(7) no
C48 . H53 . 3.328(7) no
C48 . H54 . 2.708(7) no
C48 . H55 . 2.663(7) no
C48 . H56 . 3.300(8) no
C48 . H57 . 2.634(7) no
C48 . H58 . 0.95(1) no
C48 . H59 . 0.95(1) no
C48 . H60 . 0.95(1) no
C50 . C51 . 1.379(14) yes
C50 . C52 . 2.213(14) yes
C50 . O5 . 1.989(14) yes
C50 . H3 4_545 3.470(12) no
C50 . H14 . 3.08(1) no
C50 . H22 4_545 3.44(1) no
C50 . H61 . 0.95(2) no
C50 . H62 . 0.95(2) no
C50 . H63 . 1.933(18) no
C50 . H64 . 1.956(16) no
C50 . H65 . 2.948(14) no
C50 . H66 . 2.748(15) no
C50 . H67 . 1.91(1) no
C50 . H68 . 1.842(14) no
C51 . C52 . 1.505(14) yes
C51 . O5 . 2.149(16) yes
C51 . H14 . 3.192(16) no
C51 . H61 . 1.932(18) no
C51 . H62 . 1.920(19) no
C51 . H63 . 0.95(3) no
C51 . H63 2_554 3.44(3) no
C51 . H64 . 0.95(2) no
C51 . H65 . 2.041(15) no
C51 . H66 . 2.065(18) no
C51 . H67 . 3.019(16) no
C51 . H68 . 2.471(17) no
C52 . O5 . 1.309(13) yes
C52 . H46 . 3.20(1) no
C52 . H61 . 3.057(15) no
C52 . H62 . 2.540(14) no
C52 . H63 . 2.067(19) no
C52 . H64 . 2.041(14) no
C52 . H65 . 0.95(3) no
C52 . H66 . 0.95(2) no
C52 . H67 . 3.000(12) no
C52 . H68 . 2.64(1) no
O5 . H2 4_545 3.404(16) no
O5 . H22 4_545 2.966(12) no
O5 . H25 4_545 3.438(15) no
O5 . H41 4_545 3.56(2) no
O5 . H61 . 2.843(15) no
O5 . H62 . 2.279(16) no
O5 . H63 . 2.704(19) no
O5 . H64 . 2.872(17) no
O5 . H65 . 1.916(16) no
O5 . H66 . 1.858(13) no
O5 . H67 . 1.87(1) no
O5 . H68 . 1.902(16) no
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_site_symmetry_1
_geom_torsion_atom_site_label_2
_geom_torsion_site_symmetry_2
_geom_torsion_atom_site_label_3
_geom_torsion_site_symmetry_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
O3 . Zn1 . O1 . C7 . -95.4(3) yes
N1 . Zn1 . O1 . C7 . 12.2(4) yes
N3 . Zn1 . O1 . C7 . 150.6(3) yes
O1 . Zn1 . O3 . C29 . -154.5(3) yes
N1 . Zn1 . O3 . C29 . 101.8(3) yes
N3 . Zn1 . O3 . C29 . -26.4(3) yes
O1 . Zn1 . N1 . C1 . -173.9(3) yes
O1 . Zn1 . N1 . C5 . -9.3(4) yes
O3 . Zn1 . N1 . C1 . -55.3(4) yes
O3 . Zn1 . N1 . C5 . 109.3(4) yes
N3 . Zn1 . N1 . C1 . 50.4(4) yes
N3 . Zn1 . N1 . C5 . -145.0(4) yes
O1 . Zn1 . N3 . C3 . -39.1(4) yes
O1 . Zn1 . N3 . C27 . 140.4(3) yes
O3 . Zn1 . N3 . C3 . -163.7(3) yes
O3 . Zn1 . N3 . C27 . 15.8(3) yes
N1 . Zn1 . N3 . C3 . 86.8(4) yes
N1 . Zn1 . N3 . C27 . -93.7(4) yes
O4 . Zn2 . O2 . C18 . -140.0(3) yes
N2 . Zn2 . O2 . C18 . -22.4(4) yes
N4 . Zn2 . O2 . C18 . 105.2(3) yes
O2 . Zn2 . O4 . C40 . -158.6(3) yes
N2 . Zn2 . O4 . C40 . 92.0(3) yes
N4 . Zn2 . O4 . C40 . -32.4(3) yes
O2 . Zn2 . N2 . C2 . -158.9(3) yes
O2 . Zn2 . N2 . C16 . 13.8(4) yes
O4 . Zn2 . N2 . C2 . -33.3(4) yes
O4 . Zn2 . N2 . C16 . 139.4(3) yes
N4 . Zn2 . N2 . C2 . 75.2(4) yes
N4 . Zn2 . N2 . C16 . -112.1(4) yes
O2 . Zn2 . N4 . C4 . -31.4(4) yes
O2 . Zn2 . N4 . C38 . 148.6(3) yes
O4 . Zn2 . N4 . C4 . -159.9(3) yes
O4 . Zn2 . N4 . C38 . 20.0(3) yes
N2 . Zn2 . N4 . C4 . 83.2(4) yes
N2 . Zn2 . N4 . C38 . -96.9(3) yes
Zn1 . O1 . C7 . C6 . -12.5(5) yes
Zn1 . O1 . C7 . C8 . 168.5(3) yes
Zn2 . O2 . C18 . C17 . 15.4(5) yes
Zn2 . O2 . C18 . C19 . -165.4(2) yes
Zn1 . O3 . C29 . C28 . 21.0(4) yes
Zn1 . O3 . C29 . C30 . -160.5(2) yes
Zn2 . O4 . C40 . C39 . 26.7(4) yes
Zn2 . O4 . C40 . C41 . -154.2(3) yes
O5 . C49 . C50 . C51 . -42.2(2) yes
C50 . C49 . O5 . C52 . 33.6(2) yes
Zn1 . N1 . C1 . C2 . -97.0(4) yes
C5 . N1 . C1 . C2 . 98.4(6) yes
Zn1 . N1 . C5 . C6 . 8.2(6) yes
C1 . N1 . C5 . C6 . 172.7(5) yes
Zn2 . N2 . C2 . C1 . -99.7(4) yes
C16 . N2 . C2 . C1 . 87.5(6) yes
Zn2 . N2 . C16 . C17 . 0.9(6) yes
C2 . N2 . C16 . C17 . 173.9(5) yes
Zn1 . N3 . C3 . C4 . 1.0(4) yes
C27 . N3 . C3 . C4 . -178.5(3) yes
Zn1 . N3 . C27 . C28 . -1.5(5) yes
C3 . N3 . C27 . C28 . 178.1(4) yes
Zn2 . N4 . C4 . C3 . -23.8(4) yes
C38 . N4 . C4 . C3 . 156.3(4) yes
Zn2 . N4 . C38 . C39 . -3.1(4) yes
C4 . N4 . C38 . C39 . 176.8(4) yes
N1 . C1 . C2 . N2 . 64.9(5) yes
N3 . C3 . C4 . N4 . -68.4(4) yes
N1 . C5 . C6 . C7 . -5.9(7) yes
N1 . C5 . C6 . C11 . 178.2(4) yes
C5 . C6 . C7 . O1 . 7.4(7) yes
C5 . C6 . C7 . C8 . -173.6(5) yes
C11 . C6 . C7 . O1 . -176.8(5) yes
C11 . C6 . C7 . C8 . 2.2(7) yes
C5 . C6 . C11 . C10 . 178.0(5) yes
C7 . C6 . C11 . C10 . 1.9(8) yes
O1 . C7 . C8 . C9 . 174.6(4) yes
O1 . C7 . C8 . C12 . -1.7(6) yes
C6 . C7 . C8 . C9 . -4.4(7) yes
C6 . C7 . C8 . C12 . 179.3(5) yes
C7 . C8 . C9 . C10 . 2.9(8) yes
C12 . C8 . C9 . C10 . 179.1(6) yes
C7 . C8 . C12 . C13 . -58.2(6) yes
C7 . C8 . C12 . C14 . 64.0(6) yes
C7 . C8 . C12 . C15 . -175.4(5) yes
C9 . C8 . C12 . C13 . 125.6(6) yes
C9 . C8 . C12 . C14 . -112.2(7) yes
C9 . C8 . C12 . C15 . 8.4(9) yes
C8 . C9 . C10 . C11 . 1.2(9) yes
C9 . C10 . C11 . C6 . -3.6(9) yes
N2 . C16 . C17 . C18 . -14.8(7) yes
N2 . C16 . C17 . C22 . 169.0(4) yes
C16 . C17 . C18 . O2 . 6.1(7) yes
C16 . C17 . C18 . C19 . -173.1(4) yes
C22 . C17 . C18 . O2 . -177.8(4) yes
C22 . C17 . C18 . C19 . 2.9(6) yes
C16 . C17 . C22 . C21 . 177.0(5) yes
C18 . C17 . C22 . C21 . 0.7(7) yes
O2 . C18 . C19 . C20 . 176.3(4) yes
O2 . C18 . C19 . C23 . -3.8(5) yes
C17 . C18 . C19 . C20 . -4.4(6) yes
C17 . C18 . C19 . C23 . 175.5(4) yes
C18 . C19 . C20 . C21 . 2.5(7) yes
C23 . C19 . C20 . C21 . -177.4(5) yes
C18 . C19 . C23 . C24 . 64.8(5) yes
C18 . C19 . C23 . C25 . -176.8(4) yes
C18 . C19 . C23 . C26 . -57.3(5) yes
C20 . C19 . C23 . C24 . -115.4(5) yes
C20 . C19 . C23 . C25 . 3.0(7) yes
C20 . C19 . C23 . C26 . 122.5(5) yes
C19 . C20 . C21 . C22 . 1.1(7) yes
C20 . C21 . C22 . C17 . -2.7(7) yes
N3 . C27 . C28 . C29 . -11.5(6) yes
N3 . C27 . C28 . C33 . 171.7(3) yes
C27 . C28 . C29 . O3 . 1.1(6) yes
C27 . C28 . C29 . C30 . -177.5(4) yes
C33 . C28 . C29 . O3 . 177.7(4) yes
C33 . C28 . C29 . C30 . -0.8(6) yes
C27 . C28 . C33 . C32 . 179.8(4) yes
C29 . C28 . C33 . C32 . 2.8(6) yes
O3 . C29 . C30 . C31 . 179.9(3) yes
O3 . C29 . C30 . C34 . 0.1(5) yes
C28 . C29 . C30 . C31 . -1.5(6) yes
C28 . C29 . C30 . C34 . 178.7(4) yes
C29 . C30 . C31 . C32 . 2.1(6) yes
C34 . C30 . C31 . C32 . -178.1(4) yes
C29 . C30 . C34 . C35 . 61.8(5) yes
C29 . C30 . C34 . C36 . -178.5(4) yes
C29 . C30 . C34 . C37 . -59.8(5) yes
C31 . C30 . C34 . C35 . -118.0(5) yes
C31 . C30 . C34 . C36 . 1.8(6) yes
C31 . C30 . C34 . C37 . 120.4(5) yes
C30 . C31 . C32 . C33 . -0.2(7) yes
C31 . C32 . C33 . C28 . -2.3(6) yes
N4 . C38 . C39 . C40 . -11.9(6) yes
N4 . C38 . C39 . C44 . 168.5(3) yes
C38 . C39 . C40 . O4 . -0.5(6) yes
C38 . C39 . C40 . C41 . -179.7(4) yes
C44 . C39 . C40 . O4 . 179.1(4) yes
C44 . C39 . C40 . C41 . -0.1(6) yes
C38 . C39 . C44 . C43 . -178.7(4) yes
C40 . C39 . C44 . C43 . 1.7(6) yes
O4 . C40 . C41 . C42 . 178.7(3) yes
O4 . C40 . C41 . C45 . -0.8(5) yes
C39 . C40 . C41 . C42 . -2.1(6) yes
C39 . C40 . C41 . C45 . 178.3(4) yes
C40 . C41 . C42 . C43 . 2.8(6) yes
C45 . C41 . C42 . C43 . -177.6(4) yes
C40 . C41 . C45 . C46 . 58.6(5) yes
C40 . C41 . C45 . C47 . 177.9(4) yes
C40 . C41 . C45 . C48 . -63.0(5) yes
C42 . C41 . C45 . C46 . -120.9(5) yes
C42 . C41 . C45 . C47 . -1.7(6) yes
C42 . C41 . C45 . C48 . 117.5(5) yes
C41 . C42 . C43 . C44 . -1.3(7) yes
C42 . C43 . C44 . C39 . -1.1(6) yes
C49 . C50 . C51 . C52 . 36.2(1) yes
C50 . C51 . C52 . O5 . -14.4(1) yes
C51 . C52 . O5 . C49 . -11.4(2) yes
|
1100932.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-17 14:53:33 +0200 (Thu, 17 Mar 2016) $
#$Revision: 178237 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100932.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_1100932
loop_
_publ_author_name
'Mizukami, Shin'
'Houjou, Hirohiko'
'Sugaya, Kenta'
'Koyama, Emiko'
'Tokuhisa, Hideo'
'Sasaki, Takeshi'
'Kanesato, Masatoshi'
_publ_section_title
;
Fluorescence Color Modulation by Intramolecular and Intermolecular
\p--\p Interactions in a Helical Zinc(II) Complex
;
_journal_coden_ASTM CMATEX
_journal_issue 1
_journal_name_full 'Chemistry of Materials'
_journal_page_first 50
_journal_page_last 56
_journal_paper_doi 10.1021/cm049744s
_journal_volume 17
_journal_year 2005
_chemical_formula_moiety 'C49 H64 N4 O5 Zn2 '
_chemical_formula_sum 'C49 H64 N4 O5 Zn2'
_chemical_formula_weight 919.83
_chemical_melting_point ?
_chemical_name_common 'A dizinc complex of tBu-salen with methanol'
_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 62.01(9)
_cell_angle_beta 82.3(1)
_cell_angle_gamma 76.7(1)
_cell_formula_units_Z 2
_cell_length_a 12.50(2)
_cell_length_b 14.17(1)
_cell_length_c 15.80(2)
_cell_measurement_reflns_used 14006
_cell_measurement_temperature 193.1
_cell_measurement_theta_max 27.5
_cell_measurement_theta_min 3.0
_cell_volume 2405.1(5)
_computing_data_reduction CrystalStructure
_computing_publication_material 'CrystalStructure Ver. 3.10'
_computing_structure_refinement CRYSTALS
_computing_structure_solution DirectMethod
_diffrn_measured_fraction_theta_full 0.9235
_diffrn_measured_fraction_theta_max 0.9235
_diffrn_measurement_device_type 'Rigaku RAXIS-RAPID'
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.7107
_diffrn_reflns_av_R_equivalents 0.064
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_l_max 20
_diffrn_reflns_limit_l_min -20
_diffrn_reflns_number 20606
_diffrn_reflns_theta_full 27.49
_diffrn_reflns_theta_max 27.49
_exptl_absorpt_coefficient_mu 1.045
_exptl_absorpt_correction_type sphere
_exptl_absorpt_process_details International_Tables
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.270
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 972.00
_exptl_crystal_size_max 0.60
_exptl_crystal_size_mid 0.40
_exptl_crystal_size_min 0.20
_refine_diff_density_max 1.43
_refine_diff_density_min -1.24
_refine_ls_extinction_coef -26.8(2)
_refine_ls_extinction_method
'Larson (1970) Crystallographic Computing eq. 22'
_refine_ls_goodness_of_fit_ref 1.142
_refine_ls_hydrogen_treatment refall
_refine_ls_number_parameters 609
_refine_ls_number_reflns 6406
_refine_ls_R_factor_gt 0.0760
_refine_ls_shift/su_max 0.0100
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0010Fo^2^ + 3.0000\s^2^(Fo) + 0.5000]/(4Fo^2^)'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_ref 0.1850
_reflns_number_gt 5761
_reflns_number_total 10196
_reflns_threshold_expression F^2^>2.0\s(F^2^)
_cod_duplicate_entry 4000531
_cod_data_source_file cm049744ssi20040219_042354.cif
_cod_data_source_block 2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_chemical_melting_point' value ' not measured ' was changed to '?' -
the value is undefined or not given.
Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana
;
_cod_original_sg_symbol_H-M 'P -1 '
_cod_original_formula_sum 'C49 H64 N4 O5 Zn2 '
_cod_database_code 1100932
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
Zn1 Zn 0.16912(8) 0.17936(8) 0.35702(7) 0.0331(3) Uani 1.00 1 d . . .
Zn2 Zn -0.02022(8) 0.48578(8) 0.26543(7) 0.0348(3) Uani 1.00 1 d . . .
O1 O 0.2175(4) 0.0598(5) 0.4759(4) 0.036(2) Uani 1.00 1 d . . .
O2 O 0.0472(6) 0.6034(5) 0.1741(5) 0.052(2) Uani 1.00 1 d . . .
O3 O 0.2301(5) 0.1780(5) 0.2412(4) 0.042(2) Uani 1.00 1 d . . .
O4 O -0.1686(5) 0.5168(5) 0.3090(4) 0.038(2) Uani 1.00 1 d . . .
O5 O 0.1484(9) 0.3131(7) 0.6508(7) 0.098(4) Uani 1.00 1 d . . .
N1 N 0.0085(7) 0.1891(5) 0.3885(6) 0.043(2) Uani 1.00 1 d . . .
N2 N 0.0095(5) 0.3977(5) 0.1939(4) 0.028(2) Uani 1.00 1 d . . .
N3 N 0.2430(5) 0.2964(5) 0.3464(4) 0.027(2) Uani 1.00 1 d . . .
N4 N 0.0422(5) 0.4294(5) 0.3938(5) 0.030(2) Uani 1.00 1 d . . .
C1 C -0.0789(8) 0.2495(8) 0.3184(7) 0.050(3) Uani 1.00 1 d . . .
C2 C -0.0402(9) 0.3016(8) 0.2173(8) 0.056(3) Uani 1.00 1 d . . .
C3 C 0.2346(8) 0.3242(7) 0.4268(7) 0.044(3) Uani 1.00 1 d . . .
C4 C 0.1540(7) 0.4296(7) 0.4095(7) 0.040(3) Uani 1.00 1 d . . .
C5 C -0.0196(8) 0.1388(7) 0.4747(7) 0.036(3) Uani 1.00 1 d . . .
C6 C 0.0410(7) 0.0709(7) 0.5638(6) 0.034(3) Uani 1.00 1 d . . .
C7 C 0.1600(6) 0.0388(6) 0.5568(5) 0.027(2) Uani 1.00 1 d . . .
C8 C 0.2155(8) -0.0235(7) 0.6475(7) 0.040(3) Uani 1.00 1 d . . .
C9 C 0.1524(8) -0.0494(7) 0.7318(7) 0.047(3) Uani 1.00 1 d . . .
C10 C 0.0372(7) -0.0213(7) 0.7359(6) 0.037(2) Uani 1.00 1 d . . .
C11 C -0.0156(8) 0.0389(8) 0.6518(8) 0.050(3) Uani 1.00 1 d . . .
C12 C 0.3422(7) -0.0578(7) 0.6471(6) 0.044(3) Uani 1.00 1 d . . .
C13 C 0.3963(7) 0.0415(8) 0.5914(7) 0.051(3) Uani 1.00 1 d . . .
C14 C 0.3786(9) -0.1351(8) 0.6011(9) 0.070(4) Uani 1.00 1 d . . .
C15 C 0.3844(9) -0.117(1) 0.7511(8) 0.082(4) Uani 1.00 1 d . . .
C16 C 0.0740(6) 0.4300(6) 0.1163(5) 0.028(2) Uani 1.00 1 d . . .
C17 C 0.1266(8) 0.5192(7) 0.0753(6) 0.038(3) Uani 1.00 1 d . . .
C18 C 0.1115(7) 0.6005(7) 0.1064(6) 0.030(2) Uani 1.00 1 d . . .
C19 C 0.1755(6) 0.6874(7) 0.0547(5) 0.028(2) Uani 1.00 1 d . . .
C20 C 0.2480(7) 0.6854(7) -0.0208(5) 0.035(2) Uani 1.00 1 d . . .
C21 C 0.2587(7) 0.6050(7) -0.0487(6) 0.034(2) Uani 1.00 1 d . . .
C22 C 0.1989(7) 0.5227(7) -0.0011(6) 0.037(3) Uani 1.00 1 d . . .
C23 C 0.1635(8) 0.7802(7) 0.0815(6) 0.037(3) Uani 1.00 1 d . . .
C24 C 0.190(1) 0.7346(9) 0.1875(8) 0.076(4) Uani 1.00 1 d . . .
C25 C 0.043(1) 0.8431(9) 0.066(1) 0.086(5) Uani 1.00 1 d . . .
C26 C 0.2382(9) 0.8640(9) 0.0178(8) 0.063(4) Uani 1.00 1 d . . .
C27 C 0.3142(6) 0.3362(7) 0.2754(6) 0.029(2) Uani 1.00 1 d . . .
C28 C 0.3406(7) 0.3120(7) 0.1986(7) 0.041(3) Uani 1.00 1 d . . .
C29 C 0.3031(6) 0.2332(6) 0.1839(6) 0.028(2) Uani 1.00 1 d . . .
C30 C 0.3495(7) 0.2155(7) 0.1005(6) 0.034(2) Uani 1.00 1 d . . .
C31 C 0.4236(7) 0.2764(7) 0.0399(6) 0.039(3) Uani 1.00 1 d . . .
C32 C 0.4597(7) 0.3544(8) 0.0538(7) 0.042(3) Uani 1.00 1 d . . .
C33 C 0.4173(7) 0.3702(7) 0.1336(6) 0.034(2) Uani 1.00 1 d . . .
C34 C 0.3151(8) 0.1268(8) 0.0846(7) 0.047(3) Uani 1.00 1 d . . .
C35 C 0.1915(8) 0.154(1) 0.0699(9) 0.064(4) Uani 1.00 1 d . . .
C36 C 0.346(1) 0.0150(8) 0.1736(8) 0.069(4) Uani 1.00 1 d . . .
C37 C 0.3731(9) 0.118(1) -0.0018(8) 0.066(4) Uani 1.00 1 d . . .
C38 C -0.0197(7) 0.3945(7) 0.4694(6) 0.033(2) Uani 1.00 1 d . . .
C39 C -0.1352(8) 0.3872(7) 0.4749(7) 0.039(3) Uani 1.00 1 d . . .
C40 C -0.2048(7) 0.4506(6) 0.3921(5) 0.029(2) Uani 1.00 1 d . . .
C41 C -0.3207(7) 0.4385(7) 0.4087(6) 0.035(3) Uani 1.00 1 d . . .
C42 C -0.3530(9) 0.3648(8) 0.4978(8) 0.055(3) Uani 1.00 1 d . . .
C43 C -0.2841(8) 0.3055(8) 0.5757(7) 0.048(3) Uani 1.00 1 d . . .
C44 C -0.1769(8) 0.3206(7) 0.5617(6) 0.040(3) Uani 1.00 1 d . . .
C45 C -0.3990(8) 0.5061(8) 0.3238(8) 0.049(3) Uani 1.00 1 d . . .
C46 C -0.3577(8) 0.4813(8) 0.2379(6) 0.044(3) Uani 1.00 1 d . . .
C47 C -0.4075(9) 0.6272(8) 0.2915(7) 0.054(3) Uani 1.00 1 d . . .
C48 C -0.5139(8) 0.4793(9) 0.3525(8) 0.060(4) Uani 1.00 1 d . . .
C49 C 0.176(1) 0.212(1) 0.718(1) 0.108(6) Uani 1.00 1 d . . .
H1 H 0.4524(7) 0.2635(7) -0.0133(6) 0.046(3) Uiso 1.00 1 c . . .
H2 H 0.5101(7) 0.3962(8) 0.0095(7) 0.047(3) Uiso 1.00 1 c . . .
H3 H 0.4413(7) 0.4220(7) 0.1450(6) 0.040(3) Uiso 1.00 1 c . . .
H4 H -0.1301(8) 0.2837(7) 0.6149(6) 0.047(3) Uiso 1.00 1 c . . .
H5 H -0.3099(8) 0.2557(8) 0.6361(7) 0.055(4) Uiso 1.00 1 c . . .
H6 H -0.4267(9) 0.3541(8) 0.5064(8) 0.073(4) Uiso 1.00 1 c . . .
H7 H 0.2071(7) 0.4674(7) -0.0207(6) 0.045(3) Uiso 1.00 1 c . . .
H8 H 0.3073(7) 0.6064(7) -0.1008(6) 0.041(3) Uiso 1.00 1 c . . .
H9 H 0.2906(7) 0.7407(7) -0.0525(5) 0.037(3) Uiso 1.00 1 c . . .
H10 H -0.0935(8) 0.0589(8) 0.6530(8) 0.063(4) Uiso 1.00 1 c . . .
H11 H -0.0026(7) -0.0435(7) 0.7955(6) 0.041(3) Uiso 1.00 1 c . . .
H12 H 0.1896(8) -0.0885(7) 0.7907(7) 0.055(4) Uiso 1.00 1 c . . .
H13 H -0.0971(8) 0.1454(7) 0.4845(7) 0.044(3) Uiso 1.00 1 c . . .
H14 H 0.0872(6) 0.3856(6) 0.0845(5) 0.034(3) Uiso 1.00 1 c . . .
H15 H 0.3510(6) 0.3866(7) 0.2773(6) 0.035(3) Uiso 1.00 1 c . . .
H16 H 0.0134(7) 0.3710(7) 0.5285(6) 0.040(3) Uiso 1.00 1 c . . .
H17 H 0.2095(8) 0.2672(7) 0.4825(7) 0.055(4) Uiso 1.00 1 c . . .
H18 H 0.3054(8) 0.3301(7) 0.4372(7) 0.056(4) Uiso 1.00 1 c . . .
H19 H 0.1792(7) 0.4861(7) 0.3533(7) 0.051(3) Uiso 1.00 1 c . . .
H20 H 0.1535(7) 0.4442(7) 0.4624(7) 0.051(3) Uiso 1.00 1 c . . .
H21 H -0.1007(9) 0.3254(8) 0.1770(8) 0.071(4) Uiso 1.00 1 c . . .
H22 H 0.0132(9) 0.2489(8) 0.2057(8) 0.071(4) Uiso 1.00 1 c . . .
H23 H -0.1240(8) 0.2006(8) 0.3255(7) 0.065(4) Uiso 1.00 1 c . . .
H24 H -0.1213(8) 0.3055(8) 0.3327(7) 0.065(4) Uiso 1.00 1 c . . .
H25 H 0.4502(9) 0.099(1) 0.0069(8) 0.087(6) Uiso 1.00 1 c . . .
H26 H 0.3501(9) 0.065(1) -0.0114(8) 0.087(6) Uiso 1.00 1 c . . .
H27 H 0.3558(9) 0.187(1) -0.0562(8) 0.087(6) Uiso 1.00 1 c . . .
H28 H 0.1748(8) 0.222(1) 0.0150(9) 0.092(6) Uiso 1.00 1 c . . .
H29 H 0.1695(8) 0.100(1) 0.0604(9) 0.092(6) Uiso 1.00 1 c . . .
H30 H 0.1532(8) 0.158(1) 0.1245(9) 0.092(6) Uiso 1.00 1 c . . .
H31 H 0.309(1) 0.0188(8) 0.2287(8) 0.083(5) Uiso 1.00 1 c . . .
H32 H 0.326(1) -0.0407(8) 0.1655(8) 0.083(5) Uiso 1.00 1 c . . .
H33 H 0.423(1) -0.0008(8) 0.1815(8) 0.083(5) Uiso 1.00 1 c . . .
H34 H -0.5422(8) 0.4941(9) 0.4048(8) 0.075(5) Uiso 1.00 1 c . . .
H35 H -0.5611(8) 0.5223(9) 0.2999(8) 0.075(5) Uiso 1.00 1 c . . .
H36 H -0.5096(8) 0.4044(9) 0.3710(8) 0.075(5) Uiso 1.00 1 c . . .
H37 H -0.3552(8) 0.4066(8) 0.2569(6) 0.053(4) Uiso 1.00 1 c . . .
H38 H -0.4062(8) 0.5250(8) 0.1863(6) 0.053(4) Uiso 1.00 1 c . . .
H39 H -0.2861(8) 0.4973(8) 0.2179(6) 0.053(4) Uiso 1.00 1 c . . .
H40 H -0.3367(9) 0.6455(8) 0.2731(7) 0.062(4) Uiso 1.00 1 c . . .
H41 H -0.4545(9) 0.6682(8) 0.2384(7) 0.062(4) Uiso 1.00 1 c . . .
H42 H -0.4372(9) 0.6434(8) 0.3428(7) 0.062(4) Uiso 1.00 1 c . . .
H43 H 0.142(1) 0.6867(9) 0.2271(8) 0.099(6) Uiso 1.00 1 c . . .
H44 H 0.264(1) 0.6958(9) 0.1967(8) 0.099(6) Uiso 1.00 1 c . . .
H45 H 0.182(1) 0.7924(9) 0.2039(8) 0.099(6) Uiso 1.00 1 c . . .
H46 H 0.033(1) 0.9011(9) 0.083(1) 0.110(6) Uiso 1.00 1 c . . .
H47 H 0.025(1) 0.8716(9) 0.001(1) 0.110(6) Uiso 1.00 1 c . . .
H48 H -0.004(1) 0.7939(9) 0.106(1) 0.110(6) Uiso 1.00 1 c . . .
H49 H 0.3131(9) 0.8284(9) 0.0264(8) 0.082(5) Uiso 1.00 1 c . . .
H50 H 0.2210(9) 0.8935(9) -0.0477(8) 0.082(5) Uiso 1.00 1 c . . .
H51 H 0.2261(9) 0.9209(9) 0.0358(8) 0.082(5) Uiso 1.00 1 c . . .
H52 H 0.3518(9) -0.179(1) 0.7873(8) 0.078(4) Uiso 1.00 1 c . . .
H53 H 0.4621(9) -0.139(1) 0.7505(8) 0.078(4) Uiso 1.00 1 c . . .
H54 H 0.3641(9) -0.069(1) 0.7795(8) 0.077(4) Uiso 1.00 1 c . . .
H55 H 0.3457(9) -0.1974(8) 0.6355(9) 0.073(4) Uiso 1.00 1 c . . .
H56 H 0.3560(9) -0.0980(8) 0.5366(9) 0.073(4) Uiso 1.00 1 c . . .
H57 H 0.4564(9) -0.1571(8) 0.6024(9) 0.073(4) Uiso 1.00 1 c . . .
H58 H 0.4740(7) 0.0191(8) 0.5928(7) 0.053(3) Uiso 1.00 1 c . . .
H59 H 0.3738(7) 0.0780(8) 0.5269(7) 0.053(3) Uiso 1.00 1 c . . .
H60 H 0.3745(7) 0.0895(8) 0.6197(7) 0.053(3) Uiso 1.00 1 c . . .
H61 H 0.117(1) 0.175(1) 0.730(1) 0.132(8) Uiso 1.00 1 c . . .
H62 H 0.240(1) 0.177(1) 0.697(1) 0.132(8) Uiso 1.00 1 c . . .
H63 H 0.191(1) 0.212(1) 0.775(1) 0.132(8) Uiso 1.00 1 c . . .
H64 H 0.139(6) 0.348(6) 0.697(5) 0.02(2) 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
Zn1 0.0332(6) 0.0320(6) 0.0326(6) -0.0092(5) -0.0027(5) -0.0118(5)
Zn2 0.0378(7) 0.0355(6) 0.0344(6) -0.0090(5) 0.0003(5) -0.0181(5)
O1 0.025(3) 0.040(3) 0.031(3) -0.007(3) 0.010(3) -0.009(3)
O2 0.067(5) 0.035(4) 0.063(5) -0.005(3) -0.011(4) -0.030(3)
O3 0.045(4) 0.033(3) 0.056(4) -0.013(3) -0.009(3) -0.023(3)
O4 0.043(4) 0.033(3) 0.037(4) 0.002(3) -0.014(3) -0.015(3)
O5 0.17(1) 0.055(5) 0.087(7) -0.025(6) -0.058(6) -0.033(5)
N1 0.060(5) 0.013(3) 0.059(5) 0.002(3) -0.037(4) -0.015(4)
N2 0.026(4) 0.036(4) 0.016(3) -0.018(3) 0.014(3) -0.004(3)
N3 0.021(4) 0.034(4) 0.020(3) -0.006(3) 0.013(3) -0.011(3)
N4 0.028(4) 0.034(4) 0.025(4) -0.006(3) 0.006(3) -0.013(3)
C1 0.053(6) 0.038(5) 0.070(7) 0.010(5) -0.044(5) -0.031(5)
C2 0.069(7) 0.039(6) 0.069(7) 0.009(5) -0.055(6) -0.027(5)
C3 0.048(6) 0.036(5) 0.054(6) 0.007(4) -0.030(5) -0.026(5)
C4 0.041(6) 0.043(5) 0.043(6) -0.004(4) -0.007(4) -0.025(5)
C5 0.035(5) 0.029(5) 0.046(6) -0.004(4) -0.005(4) -0.021(5)
C6 0.042(6) 0.028(5) 0.036(5) -0.007(4) -0.008(4) -0.017(4)
C7 0.024(4) 0.028(4) 0.023(4) -0.013(4) 0.017(3) -0.008(4)
C8 0.045(6) 0.026(4) 0.045(6) -0.008(4) -0.009(5) -0.011(4)
C9 0.061(7) 0.030(5) 0.046(6) -0.013(5) -0.014(5) -0.008(4)
C10 0.040(6) 0.040(5) 0.021(5) -0.009(4) 0.017(4) -0.010(4)
C11 0.044(6) 0.039(5) 0.075(8) -0.002(5) -0.019(6) -0.031(5)
C12 0.033(5) 0.046(5) 0.028(5) 0.000(4) 0.009(4) -0.001(4)
C13 0.029(5) 0.055(6) 0.048(6) -0.016(5) 0.007(4) -0.004(5)
C14 0.061(8) 0.040(6) 0.082(9) 0.016(5) -0.020(6) -0.012(6)
C15 0.049(7) 0.081(9) 0.064(8) 0.007(6) -0.021(6) 0.006(7)
C16 0.033(5) 0.029(4) 0.022(4) -0.002(4) -0.006(4) -0.012(3)
C17 0.047(6) 0.027(5) 0.043(6) 0.008(4) -0.030(5) -0.016(4)
C18 0.024(5) 0.041(5) 0.027(5) 0.003(4) -0.004(4) -0.020(4)
C19 0.023(4) 0.036(4) 0.020(4) -0.014(4) 0.011(3) -0.007(4)
C20 0.034(5) 0.043(5) 0.017(4) -0.016(4) 0.012(4) -0.004(4)
C21 0.031(5) 0.050(5) 0.021(4) -0.013(4) 0.016(4) -0.017(4)
C22 0.046(6) 0.034(5) 0.032(5) 0.002(4) -0.014(4) -0.016(4)
C23 0.059(6) 0.034(5) 0.020(4) -0.027(5) 0.017(4) -0.011(4)
C24 0.13(1) 0.060(7) 0.055(7) -0.032(8) -0.020(7) -0.033(6)
C25 0.09(1) 0.049(7) 0.14(1) 0.012(7) -0.036(9) -0.059(8)
C26 0.081(9) 0.063(7) 0.062(7) -0.047(7) 0.021(6) -0.034(6)
C27 0.020(4) 0.037(5) 0.032(5) -0.006(4) -0.002(3) -0.016(4)
C28 0.034(5) 0.034(5) 0.057(6) 0.010(4) -0.033(5) -0.022(5)
C29 0.017(4) 0.028(4) 0.031(5) -0.007(3) 0.000(3) -0.006(4)
C30 0.030(5) 0.036(5) 0.029(5) -0.009(4) 0.000(4) -0.009(4)
C31 0.039(6) 0.043(5) 0.033(5) -0.004(4) -0.003(4) -0.016(4)
C32 0.030(5) 0.049(6) 0.039(6) -0.014(4) 0.000(4) -0.012(5)
C33 0.032(5) 0.031(5) 0.036(5) -0.021(4) 0.003(4) -0.006(4)
C34 0.047(6) 0.053(6) 0.054(6) -0.008(5) -0.002(5) -0.035(5)
C35 0.051(7) 0.089(9) 0.091(9) -0.032(6) 0.009(6) -0.068(8)
C36 0.10(1) 0.040(6) 0.069(8) -0.031(6) 0.017(7) -0.023(6)
C37 0.069(8) 0.082(8) 0.066(8) -0.034(7) 0.033(6) -0.051(7)
C38 0.040(5) 0.039(5) 0.020(4) -0.005(4) 0.002(4) -0.015(4)
C39 0.048(6) 0.027(5) 0.047(6) -0.002(4) -0.014(5) -0.020(4)
C40 0.042(5) 0.031(4) 0.009(4) -0.013(4) 0.011(4) -0.006(3)
C41 0.033(5) 0.043(5) 0.035(5) -0.012(4) 0.008(4) -0.021(4)
C42 0.047(6) 0.059(7) 0.076(8) -0.011(5) -0.006(6) -0.044(6)
C43 0.047(6) 0.062(6) 0.028(5) -0.029(5) 0.025(5) -0.014(5)
C44 0.058(6) 0.035(5) 0.025(5) -0.010(5) -0.001(4) -0.011(4)
C45 0.047(6) 0.038(5) 0.070(7) 0.001(5) -0.025(5) -0.030(5)
C46 0.046(6) 0.057(6) 0.031(5) -0.017(5) 0.009(4) -0.021(5)
C47 0.055(7) 0.043(6) 0.056(7) -0.003(5) -0.016(5) -0.017(5)
C48 0.044(6) 0.072(8) 0.072(8) -0.011(6) -0.011(5) -0.038(6)
C49 0.16(2) 0.073(9) 0.10(1) -0.05(1) 0.07(1) -0.049(9)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 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)
;
Zn Zn 0.284 1.430
;
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_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 . Zn1 . O3 . 119.4(3) yes
O1 . Zn1 . N1 . 96.8(3) yes
O3 . Zn1 . N1 . 121.8(3) yes
O1 . Zn1 . N3 . 103.4(3) yes
O3 . Zn1 . N3 . 96.1(3) yes
N1 . Zn1 . N3 . 119.4(3) yes
O2 . Zn2 . O4 . 119.1(3) yes
O2 . Zn2 . N2 . 97.2(3) yes
O4 . Zn2 . N2 . 117.5(3) yes
O2 . Zn2 . N4 . 109.2(3) yes
O4 . Zn2 . N4 . 93.8(3) yes
N2 . Zn2 . N4 . 121.6(3) yes
Zn1 . O1 . C7 . 122.7(5) yes
Zn2 . O2 . C18 . 124.7(5) yes
Zn1 . O3 . C29 . 127.0(5) yes
Zn2 . O4 . C40 . 121.1(6) yes
C49 . O5 . H64 . 94.9(5) no
Zn1 . N1 . C1 . 125.1(7) yes
Zn1 . N1 . C5 . 117.1(6) yes
C1 . N1 . C5 . 117.7(9) yes
Zn2 . N2 . C2 . 125.6(6) yes
Zn2 . N2 . C16 . 117.5(5) yes
C2 . N2 . C16 . 116.8(7) yes
Zn1 . N3 . C3 . 120.4(5) yes
Zn1 . N3 . C27 . 120.1(5) yes
C3 . N3 . C27 . 118.5(7) yes
Zn2 . N4 . C4 . 124.7(5) yes
Zn2 . N4 . C38 . 119.7(6) yes
C4 . N4 . C38 . 115.6(7) yes
N1 . C1 . C2 . 115.1(9) yes
N1 . C1 . H23 . 108.2(1) no
C2 . C1 . H23 . 108.7(1) no
N1 . C1 . H24 . 107.9(1) no
C2 . C1 . H24 . 107.4(1) no
H23 . C1 . H24 . 109.5(1) no
N2 . C2 . C1 . 112.6(7) yes
N2 . C2 . H21 . 108.3(1) no
C1 . C2 . H21 . 109.0(1) no
N2 . C2 . H22 . 109.3(1) no
C1 . C2 . H22 . 108.1(1) no
H21 . C2 . H22 . 109.5(2) no
N3 . C3 . C4 . 113.2(7) yes
N3 . C3 . H17 . 108.2(1) no
C4 . C3 . H17 . 107.6(1) no
N3 . C3 . H18 . 109.0(1) no
C4 . C3 . H18 . 109.3(1) no
H17 . C3 . H18 . 109.5(1) no
N4 . C4 . C3 . 114.1(7) yes
N4 . C4 . H19 . 107.6(1) no
C3 . C4 . H19 . 107.2(1) no
N4 . C4 . H20 . 108.9(1) no
C3 . C4 . H20 . 109.5(1) no
H19 . C4 . H20 . 109.5(1) no
N1 . C5 . C6 . 134.0(9) yes
N1 . C5 . H13 . 112.8(1) no
C6 . C5 . H13 . 113.2(1) no
C5 . C6 . C7 . 118.4(8) yes
C5 . C6 . C11 . 119.8(9) yes
C7 . C6 . C11 . 121.8(8) yes
O1 . C7 . C6 . 124.8(8) yes
O1 . C7 . C8 . 119.6(7) yes
C6 . C7 . C8 . 115.6(7) yes
C7 . C8 . C9 . 118.4(8) yes
C7 . C8 . C12 . 119.3(8) yes
C9 . C8 . C12 . 122.3(8) yes
C8 . C9 . C10 . 124.4(9) yes
C8 . C9 . H12 . 117.8(1) no
C10 . C9 . H12 . 117.8(1) no
C9 . C10 . C11 . 117.8(8) yes
C9 . C10 . H11 . 121.2(1) no
C11 . C10 . H11 . 121.0(1) no
C6 . C11 . C10 . 121.9(9) yes
C6 . C11 . H10 . 118.9(1) no
C10 . C11 . H10 . 119.2(1) no
C8 . C12 . C13 . 110.9(8) yes
C8 . C12 . C14 . 110.2(8) yes
C13 . C12 . C14 . 109.0(8) yes
C8 . C12 . C15 . 110.6(8) yes
C13 . C12 . C15 . 107.4(9) yes
C14 . C12 . C15 . 108.8(9) yes
C12 . C13 . H58 . 109.7(1) no
C12 . C13 . H59 . 109.2(1) no
H58 . C13 . H59 . 109.5(1) no
C12 . C13 . H60 . 109.5(1) no
H58 . C13 . H60 . 109.5(1) no
H59 . C13 . H60 . 109.5(1) no
C12 . C14 . H55 . 109.7(1) no
C12 . C14 . H56 . 108.9(1) no
H55 . C14 . H56 . 109.5(2) no
C12 . C14 . H57 . 109.8(1) no
H55 . C14 . H57 . 109.5(2) no
H56 . C14 . H57 . 109.5(2) no
C12 . C15 . H52 . 108.9(1) no
C12 . C15 . H53 . 110.1(1) no
H52 . C15 . H53 . 109.5(2) no
C12 . C15 . H54 . 109.3(1) no
H52 . C15 . H54 . 109.5(2) no
H53 . C15 . H54 . 109.5(2) no
N2 . C16 . C17 . 129.1(8) yes
N2 . C16 . H14 . 115.2(9) no
C17 . C16 . H14 . 115.7(1) no
C16 . C17 . C18 . 125.0(9) yes
C16 . C17 . C22 . 114.0(7) yes
C18 . C17 . C22 . 121.0(8) yes
O2 . C18 . C17 . 124.7(8) yes
O2 . C18 . C19 . 118.4(7) yes
C17 . C18 . C19 . 116.9(8) yes
C18 . C19 . C20 . 119.3(7) yes
C18 . C19 . C23 . 120.9(7) yes
C20 . C19 . C23 . 119.8(7) yes
C19 . C20 . C21 . 121.5(7) yes
C19 . C20 . H9 . 118.7(1) no
C21 . C20 . H9 . 119.8(1) no
C20 . C21 . C22 . 120.0(7) yes
C20 . C21 . H8 . 119.7(1) no
C22 . C21 . H8 . 120.2(1) no
C17 . C22 . C21 . 121.3(8) yes
C17 . C22 . H7 . 119.3(1) no
C21 . C22 . H7 . 119.4(1) no
C19 . C23 . C24 . 110.4(7) yes
C19 . C23 . C25 . 108.5(7) yes
C24 . C23 . C25 . 108.6(9) yes
C19 . C23 . C26 . 112.8(7) yes
C24 . C23 . C26 . 109.2(8) yes
C25 . C23 . C26 . 107.1(9) yes
C23 . C24 . H43 . 109.8(1) no
C23 . C24 . H44 . 108.5(1) no
H43 . C24 . H44 . 109.5(2) no
C23 . C24 . H45 . 110.1(1) no
H43 . C24 . H45 . 109.5(2) no
H44 . C24 . H45 . 109.5(2) no
C23 . C25 . H46 . 110.2(2) no
C23 . C25 . H47 . 109.8(2) no
H46 . C25 . H47 . 109.5(2) no
C23 . C25 . H48 . 108.4(2) no
H46 . C25 . H48 . 109.5(2) no
H47 . C25 . H48 . 109.5(2) no
C23 . C26 . H49 . 109.3(1) no
C23 . C26 . H50 . 109.5(1) no
H49 . C26 . H50 . 109.5(2) no
C23 . C26 . H51 . 109.5(1) no
H49 . C26 . H51 . 109.5(2) no
H50 . C26 . H51 . 109.5(2) no
N3 . C27 . C28 . 126.9(8) yes
N3 . C27 . H15 . 116.1(1) no
C28 . C27 . H15 . 117.0(1) no
C27 . C28 . C29 . 127.3(9) yes
C27 . C28 . C33 . 113.1(8) yes
C29 . C28 . C33 . 119.5(8) yes
O3 . C29 . C28 . 122.2(8) yes
O3 . C29 . C30 . 120.2(7) yes
C28 . C29 . C30 . 117.6(7) yes
C29 . C30 . C31 . 119.2(8) yes
C29 . C30 . C34 . 119.2(7) yes
C31 . C30 . C34 . 121.5(8) yes
C30 . C31 . C32 . 123.2(9) yes
C30 . C31 . H1 . 117.6(1) no
C32 . C31 . H1 . 119.2(1) no
C31 . C32 . C33 . 117.8(8) yes
C31 . C32 . H2 . 120.9(1) no
C33 . C32 . H2 . 121.3(1) no
C28 . C33 . C32 . 122.6(8) yes
C28 . C33 . H3 . 118.0(1) no
C32 . C33 . H3 . 119.3(1) no
C30 . C34 . C35 . 110.0(8) yes
C30 . C34 . C36 . 108.9(8) yes
C35 . C34 . C36 . 110.0(9) yes
C30 . C34 . C37 . 111.7(8) yes
C35 . C34 . C37 . 108.1(9) yes
C36 . C34 . C37 . 108.1(9) yes
C34 . C35 . H28 . 108.3(1) no
C34 . C35 . H29 . 110.6(1) no
H28 . C35 . H29 . 109.5(2) no
C34 . C35 . H30 . 109.4(1) no
H28 . C35 . H30 . 109.5(2) no
H29 . C35 . H30 . 109.5(2) no
C34 . C36 . H31 . 109.1(1) no
C34 . C36 . H32 . 110.4(1) no
H31 . C36 . H32 . 109.5(2) no
C34 . C36 . H33 . 108.9(1) no
H31 . C36 . H33 . 109.5(2) no
H32 . C36 . H33 . 109.5(2) no
C34 . C37 . H25 . 109.3(1) no
C34 . C37 . H26 . 110.7(1) no
H25 . C37 . H26 . 109.5(2) no
C34 . C37 . H27 . 108.4(1) no
H25 . C37 . H27 . 109.5(2) no
H26 . C37 . H27 . 109.5(2) no
N4 . C38 . C39 . 127.4(8) yes
N4 . C38 . H16 . 116.3(1) no
C39 . C38 . H16 . 116.3(1) no
C38 . C39 . C40 . 121.7(8) yes
C38 . C39 . C44 . 117.5(8) yes
C40 . C39 . C44 . 120.8(9) yes
O4 . C40 . C39 . 122.5(8) yes
O4 . C40 . C41 . 121.5(8) yes
C39 . C40 . C41 . 116.0(7) yes
C40 . C41 . C42 . 118.5(8) yes
C40 . C41 . C45 . 118.2(8) yes
C42 . C41 . C45 . 123.3(8) yes
C41 . C42 . C43 . 123.9(9) yes
C41 . C42 . H6 . 117.8(1) no
C43 . C42 . H6 . 118.3(1) no
C42 . C43 . C44 . 117.7(8) yes
C42 . C43 . H5 . 121.1(1) no
C44 . C43 . H5 . 121.2(1) no
C39 . C44 . C43 . 123.0(9) yes
C39 . C44 . H4 . 118.4(1) no
C43 . C44 . H4 . 118.6(1) no
C41 . C45 . C46 . 111.2(8) yes
C41 . C45 . C47 . 109.9(7) yes
C46 . C45 . C47 . 109.1(9) yes
C41 . C45 . C48 . 111.0(8) yes
C46 . C45 . C48 . 107.0(7) yes
C47 . C45 . C48 . 108.6(8) yes
C45 . C46 . H37 . 109.5(1) no
C45 . C46 . H38 . 109.6(1) no
H37 . C46 . H38 . 109.5(1) no
C45 . C46 . H39 . 109.3(1) no
H37 . C46 . H39 . 109.5(1) no
H38 . C46 . H39 . 109.5(1) no
C45 . C47 . H40 . 109.8(1) no
C45 . C47 . H41 . 109.3(1) no
H40 . C47 . H41 . 109.5(1) no
C45 . C47 . H42 . 109.3(1) no
H40 . C47 . H42 . 109.5(1) no
H41 . C47 . H42 . 109.5(1) no
C45 . C48 . H34 . 109.4(1) no
C45 . C48 . H35 . 109.9(1) no
H34 . C48 . H35 . 109.5(2) no
C45 . C48 . H36 . 109.2(1) no
H34 . C48 . H36 . 109.5(2) no
H35 . C48 . H36 . 109.5(2) no
O5 . C49 . H61 . 109.5(2) no
O5 . C49 . H62 . 108.8(2) no
H61 . C49 . H62 . 109.5(2) no
O5 . C49 . H63 . 110.0(2) no
H61 . C49 . H63 . 109.5(2) no
H62 . C49 . H63 . 109.5(2) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Zn1 . O1 . 1.900(6) yes
Zn1 . O3 . 1.893(7) yes
Zn1 . N1 . 1.992(9) yes
Zn1 . N3 . 2.009(7) yes
Zn2 . O2 . 1.907(7) yes
Zn2 . O4 . 1.916(7) yes
Zn2 . N2 . 1.992(7) yes
Zn2 . N4 . 1.995(7) yes
O1 . C7 . 1.317(9) yes
O2 . C18 . 1.26(1) yes
O3 . C29 . 1.307(9) yes
O4 . C40 . 1.301(9) yes
O5 . C49 . 1.318(15) yes
O5 . H64 . 1.0(1) no
N1 . C1 . 1.469(11) yes
N1 . C5 . 1.250(11) yes
N2 . C2 . 1.494(11) yes
N2 . C16 . 1.320(9) yes
N3 . C3 . 1.48(1) yes
N3 . C27 . 1.32(1) yes
N4 . C4 . 1.45(1) yes
N4 . C38 . 1.28(1) yes
C1 . C2 . 1.477(14) yes
C1 . H23 . 0.95(5) no
C1 . H24 . 0.95(6) no
C2 . H21 . 0.95(7) no
C2 . H22 . 0.95(6) no
C3 . C4 . 1.522(12) yes
C3 . H17 . 0.95(8) no
C3 . H18 . 0.95(2) no
C4 . H19 . 0.95(8) no
C4 . H20 . 0.95(2) no
C5 . C6 . 1.471(12) yes
C5 . H13 . 0.95(2) no
C6 . C7 . 1.457(12) yes
C6 . C11 . 1.389(13) yes
C7 . C8 . 1.454(12) yes
C8 . C9 . 1.386(13) yes
C8 . C12 . 1.546(13) yes
C9 . C10 . 1.404(13) yes
C9 . H12 . 0.95(7) no
C10 . C11 . 1.357(13) yes
C10 . H11 . 0.95(6) no
C11 . H10 . 0.95(4) no
C12 . C13 . 1.526(12) yes
C12 . C14 . 1.537(14) yes
C12 . C15 . 1.555(14) yes
C13 . H58 . 0.95(4) no
C13 . H59 . 0.95(6) no
C13 . H60 . 0.95(4) no
C14 . H55 . 0.95(7) no
C14 . H56 . 0.95(7) no
C14 . H57 . 0.95(4) no
C15 . H52 . 0.95(7) no
C15 . H53 . 0.95(4) no
C15 . H54 . 0.95(4) no
C16 . C17 . 1.396(11) yes
C16 . H14 . 0.95(3) no
C17 . C18 . 1.418(11) yes
C17 . C22 . 1.396(13) yes
C18 . C19 . 1.470(11) yes
C19 . C20 . 1.40(1) yes
C19 . C23 . 1.533(11) yes
C20 . C21 . 1.377(12) yes
C20 . H9 . 0.95(7) no
C21 . C22 . 1.384(11) yes
C21 . H8 . 0.95(6) no
C22 . H7 . 0.95(3) no
C23 . C24 . 1.538(13) yes
C23 . C25 . 1.552(15) yes
C23 . C26 . 1.559(12) yes
C24 . H43 . 0.95(8) no
C24 . H44 . 0.95(7) no
C24 . H45 . 0.95(3) no
C25 . H46 . 0.95(3) no
C25 . H47 . 0.95(6) no
C25 . H48 . 0.95(8) no
C26 . H49 . 0.95(6) no
C26 . H50 . 0.95(5) no
C26 . H51 . 0.95(3) no
C27 . C28 . 1.387(12) yes
C27 . H15 . 0.95(4) no
C28 . C29 . 1.428(11) yes
C28 . C33 . 1.400(12) yes
C29 . C30 . 1.474(12) yes
C30 . C31 . 1.369(11) yes
C30 . C34 . 1.551(12) yes
C31 . C32 . 1.399(12) yes
C31 . H1 . 0.95(4) no
C32 . C33 . 1.397(12) yes
C32 . H2 . 0.95(8) no
C33 . H3 . 0.95(3) no
C34 . C35 . 1.527(13) yes
C34 . C36 . 1.551(14) yes
C34 . C37 . 1.500(13) yes
C35 . H28 . 0.95(9) no
C35 . H29 . 0.95(3) no
C35 . H30 . 0.95(5) no
C36 . H31 . 0.95(5) no
C36 . H32 . 0.95(3) no
C36 . H33 . 0.95(4) no
C37 . H25 . 0.95(4) no
C37 . H26 . 0.95(3) no
C37 . H27 . 0.95(8) no
C38 . C39 . 1.460(12) yes
C38 . H16 . 0.95(5) no
C39 . C40 . 1.456(12) yes
C39 . C44 . 1.365(12) yes
C40 . C41 . 1.473(11) yes
C41 . C42 . 1.377(13) yes
C41 . C45 . 1.546(13) yes
C42 . C43 . 1.395(14) yes
C42 . H6 . 0.95(3) no
C43 . C44 . 1.377(12) yes
C43 . H5 . 0.95(8) no
C44 . H4 . 0.95(8) no
C45 . C46 . 1.553(13) yes
C45 . C47 . 1.524(13) yes
C45 . C48 . 1.525(13) yes
C46 . H37 . 0.95(4) no
C46 . H38 . 0.95(8) no
C46 . H39 . 0.95(4) no
C47 . H40 . 0.95(4) no
C47 . H41 . 0.95(8) no
C47 . H42 . 0.95(4) no
C48 . H34 . 0.95(4) no
C48 . H35 . 0.95(8) no
C48 . H36 . 0.95(4) no
C49 . H61 . 0.95(6) no
C49 . H62 . 0.95(7) no
C49 . H63 . 0.95(3) no
loop_
_geom_contact_atom_site_label_1
_geom_contact_site_symmetry_1
_geom_contact_atom_site_label_2
_geom_contact_site_symmetry_2
_geom_contact_distance
_geom_contact_publ_flag
Zn1 . O1 . 1.900(6) yes
Zn1 . O3 . 1.893(7) yes
Zn1 . N1 . 1.992(9) yes
Zn1 . N2 . 3.355(9) yes
Zn1 . N3 . 2.009(7) yes
Zn1 . C1 . 3.08(1) yes
Zn1 . C2 . 3.26(1) yes
Zn1 . C3 . 3.041(8) yes
Zn1 . C5 . 2.79(1) yes
Zn1 . C6 . 3.26(1) yes
Zn1 . C7 . 2.838(9) yes
Zn1 . C27 . 2.904(9) yes
Zn1 . C28 . 3.224(11) yes
Zn1 . C29 . 2.876(9) yes
Zn1 . H17 . 2.936(8) no
Zn1 . H22 . 2.94(1) no
Zn1 . H59 . 3.514(11) no
Zn2 . O2 . 1.907(7) yes
Zn2 . O4 . 1.916(7) yes
Zn2 . N2 . 1.992(7) yes
Zn2 . N4 . 1.995(7) yes
Zn2 . C1 . 3.28(1) yes
Zn2 . C2 . 3.109(9) yes
Zn2 . C4 . 3.07(1) yes
Zn2 . C16 . 2.853(8) yes
Zn2 . C17 . 3.194(11) yes
Zn2 . C18 . 2.821(9) yes
Zn2 . C38 . 2.856(9) yes
Zn2 . C39 . 3.207(11) yes
Zn2 . C40 . 2.817(9) yes
Zn2 . H19 . 3.015(9) no
Zn2 . H21 . 3.542(9) no
Zn2 . H24 . 2.80(1) no
Zn2 . H39 . 3.46(1) no
Zn2 . H64 2_566 2.75(7) no
O1 . O3 . 3.27(1) yes
O1 . N1 . 2.91(1) yes
O1 . N3 . 3.068(9) yes
O1 . C3 . 3.506(11) yes
O1 . C5 . 2.916(12) yes
O1 . C6 . 2.459(11) yes
O1 . C7 . 1.317(9) yes
O1 . C8 . 2.396(11) yes
O1 . C12 . 2.870(12) yes
O1 . C13 . 2.964(12) yes
O1 . C14 . 2.996(13) yes
O1 . H13 2_556 3.342(11) no
O1 . H17 . 2.97(1) no
O1 . H55 . 3.461(13) no
O1 . H56 . 2.359(12) no
O1 . H59 . 2.321(11) no
O1 . H60 . 3.417(12) no
O2 . O4 . 3.294(11) yes
O2 . N2 . 2.925(9) yes
O2 . N4 . 3.181(11) yes
O2 . C4 . 3.592(13) yes
O2 . C16 . 2.94(1) yes
O2 . C17 . 2.373(11) yes
O2 . C18 . 1.26(1) yes
O2 . C19 . 2.35(1) yes
O2 . C23 . 2.864(11) yes
O2 . C24 . 2.950(13) yes
O2 . C25 . 2.992(14) yes
O2 . H19 . 3.013(12) no
O2 . H43 . 2.311(12) no
O2 . H44 . 3.395(14) no
O2 . H47 . 3.458(15) no
O2 . H48 . 2.349(13) no
O2 . H64 2_566 3.06(7) no
O3 . N1 . 3.395(12) yes
O3 . N2 . 3.503(11) yes
O3 . N3 . 2.902(9) yes
O3 . C2 . 3.409(13) yes
O3 . C16 . 3.415(11) yes
O3 . C27 . 2.97(1) yes
O3 . C28 . 2.395(11) yes
O3 . C29 . 1.307(9) yes
O3 . C30 . 2.412(11) yes
O3 . C34 . 2.899(12) yes
O3 . C35 . 2.996(12) yes
O3 . C36 . 2.988(13) yes
O3 . H14 . 3.147(11) no
O3 . H22 . 2.702(12) no
O3 . H28 . 3.465(13) no
O3 . H30 . 2.344(12) no
O3 . H31 . 2.332(12) no
O3 . H33 . 3.455(14) no
O4 . O5 2_566 2.84(1) yes
O4 . N2 . 3.34(1) yes
O4 . N4 . 2.86(1) yes
O4 . C38 . 2.925(11) yes
O4 . C39 . 2.418(11) yes
O4 . C40 . 1.301(9) yes
O4 . C41 . 2.421(11) yes
O4 . C45 . 2.893(12) yes
O4 . C46 . 2.983(11) yes
O4 . C47 . 3.019(13) yes
O4 . H24 . 2.766(11) no
O4 . H37 . 3.460(11) no
O4 . H39 . 2.331(11) no
O4 . H40 . 2.377(12) no
O4 . H42 . 3.525(13) no
O4 . H63 2_566 3.375(15) no
O4 . H64 2_566 1.99(7) no
O5 . C3 . 3.500(14) yes
O5 . C4 . 3.368(14) yes
O5 . C38 . 3.370(13) yes
O5 . C40 2_566 3.317(11) yes
O5 . C49 . 1.318(15) yes
O5 . H16 . 2.451(12) no
O5 . H17 . 2.987(13) no
O5 . H20 . 2.671(14) no
O5 . H40 2_566 3.065(13) no
O5 . H61 . 1.865(14) no
O5 . H62 . 1.857(17) no
O5 . H63 . 1.870(18) no
O5 . H64 . 1.03(7) no
N1 . N2 . 3.110(11) yes
N1 . N3 . 3.454(11) yes
N1 . N4 . 3.567(9) yes
N1 . C1 . 1.469(11) yes
N1 . C2 . 2.486(13) yes
N1 . C5 . 1.250(11) yes
N1 . C6 . 2.506(12) yes
N1 . C6 2_556 3.585(11) yes
N1 . C7 . 3.062(12) yes
N1 . C11 2_556 3.555(11) yes
N1 . H13 . 1.840(12) no
N1 . H21 . 3.274(13) no
N1 . H22 . 2.598(13) no
N1 . H23 . 1.983(11) no
N1 . H24 . 1.979(11) no
N2 . N4 . 3.48(1) yes
N2 . C1 . 2.472(12) yes
N2 . C2 . 1.494(11) yes
N2 . C16 . 1.320(9) yes
N2 . C17 . 2.452(12) yes
N2 . C18 . 3.047(11) yes
N2 . H14 . 1.93(1) no
N2 . H21 . 2.007(11) no
N2 . H22 . 2.019(11) no
N2 . H23 . 3.268(13) no
N2 . H24 . 2.554(13) no
N3 . N4 . 3.01(1) yes
N3 . C3 . 1.48(1) yes
N3 . C4 . 2.508(11) yes
N3 . C27 . 1.32(1) yes
N3 . C28 . 2.422(12) yes
N3 . C29 . 3.048(11) yes
N3 . C33 . 3.596(11) yes
N3 . H15 . 1.93(1) no
N3 . H17 . 1.994(11) no
N3 . H18 . 2.00(1) no
N3 . H19 . 2.672(11) no
N3 . H20 . 3.312(11) no
N3 . H59 . 3.320(13) no
N4 . C3 . 2.497(12) yes
N4 . C4 . 1.45(1) yes
N4 . C38 . 1.28(1) yes
N4 . C39 . 2.459(12) yes
N4 . C40 . 3.035(12) yes
N4 . H16 . 1.90(1) no
N4 . H16 2_566 3.480(11) no
N4 . H17 . 2.678(12) no
N4 . H18 . 3.293(12) no
N4 . H19 . 1.962(11) no
N4 . H20 . 1.977(11) no
N4 . H24 . 3.461(11) no
N4 . H64 2_566 3.24(7) no
C1 . C2 . 1.477(14) yes
C1 . C5 . 2.330(14) yes
C1 . C40 . 3.537(13) yes
C1 . H13 . 2.340(14) no
C1 . H21 . 2.000(13) no
C1 . H22 . 1.989(15) no
C1 . H23 . 0.95(5) no
C1 . H24 . 0.95(6) no
C1 . H55 2_556 3.491(16) no
C2 . C16 . 2.399(14) yes
C2 . H14 . 2.448(14) no
C2 . H21 . 0.95(7) no
C2 . H22 . 0.95(6) no
C2 . H23 . 1.996(15) no
C2 . H24 . 1.981(15) no
C2 . H30 . 3.422(16) no
C3 . C4 . 1.522(12) yes
C3 . C27 . 2.408(13) yes
C3 . C38 . 3.185(13) yes
C3 . H15 . 2.487(13) no
C3 . H16 . 3.104(13) no
C3 . H17 . 0.95(8) no
C3 . H18 . 0.95(2) no
C3 . H19 . 2.019(13) no
C3 . H20 . 2.045(12) no
C3 . H36 1_655 3.504(14) no
C3 . H59 . 3.235(14) no
C3 . H60 . 3.557(14) no
C4 . C27 . 3.244(12) yes
C4 . C38 . 2.316(12) yes
C4 . H15 . 3.149(12) no
C4 . H16 . 2.375(13) no
C4 . H16 2_566 3.556(13) no
C4 . H17 . 2.024(13) no
C4 . H18 . 2.043(13) no
C4 . H19 . 0.95(8) no
C4 . H20 . 0.95(2) no
C4 . H43 . 3.407(15) no
C5 . C6 . 1.471(12) yes
C5 . C6 2_556 3.374(11) yes
C5 . C7 . 2.514(13) yes
C5 . C11 . 2.475(15) yes
C5 . C38 . 3.586(12) yes
C5 . C39 . 3.485(12) yes
C5 . C44 . 3.557(13) yes
C5 . H10 . 2.619(15) no
C5 . H13 . 0.95(2) no
C5 . H23 . 2.528(13) no
C5 . H24 . 2.577(14) no
C6 . C7 . 1.457(12) yes
C6 . C8 . 2.463(13) yes
C6 . C9 . 2.746(14) yes
C6 . C10 . 2.400(12) yes
C6 . C11 . 1.389(13) yes
C6 . H10 . 2.027(14) no
C6 . H11 . 3.260(13) no
C6 . H13 . 2.041(13) no
C6 . H13 2_556 3.396(12) no
C6 . H17 . 3.528(13) no
C6 . H23 2_556 3.357(13) no
C7 . C8 . 1.454(12) yes
C7 . C9 . 2.441(13) yes
C7 . C10 . 2.874(11) yes
C7 . C11 . 2.487(13) yes
C7 . C12 . 2.590(13) yes
C7 . C13 . 3.089(12) yes
C7 . C14 . 3.134(14) yes
C7 . H10 . 3.336(13) no
C7 . H12 . 3.294(13) no
C7 . H13 . 3.323(13) no
C7 . H13 2_556 3.246(11) no
C7 . H17 . 3.067(12) no
C7 . H23 2_556 3.119(13) no
C7 . H55 . 3.380(14) no
C7 . H56 . 2.837(14) no
C7 . H59 . 2.789(12) no
C7 . H60 . 3.313(13) no
C8 . C9 . 1.386(13) yes
C8 . C10 . 2.468(13) yes
C8 . C11 . 2.821(14) yes
C8 . C12 . 1.546(13) yes
C8 . C13 . 2.530(12) yes
C8 . C14 . 2.529(15) yes
C8 . C15 . 2.549(14) yes
C8 . H11 . 3.317(13) no
C8 . H12 . 2.013(13) no
C8 . H23 2_556 2.825(12) no
C8 . H52 . 2.712(14) no
C8 . H53 . 3.370(15) no
C8 . H54 . 2.729(15) no
C8 . H55 . 2.695(14) no
C8 . H56 . 2.707(15) no
C8 . H57 . 3.350(15) no
C8 . H58 . 3.350(13) no
C8 . H59 . 2.710(13) no
C8 . H60 . 2.699(12) no
C8 . H61 . 3.539(16) no
C8 . H62 . 3.363(16) no
C9 . C10 . 1.404(13) yes
C9 . C11 . 2.364(14) yes
C9 . C12 . 2.569(14) yes
C9 . C14 . 3.596(16) yes
C9 . C15 . 2.847(16) yes
C9 . H10 . 3.227(15) no
C9 . H11 . 2.063(13) no
C9 . H12 . 0.95(7) no
C9 . H22 2_556 3.575(14) no
C9 . H23 2_556 2.791(12) no
C9 . H50 1_546 3.373(16) no
C9 . H52 . 2.707(15) no
C9 . H54 . 2.767(15) no
C9 . H55 . 3.496(16) no
C9 . H60 . 3.557(13) no
C9 . H61 . 3.094(16) no
C9 . H62 . 3.403(16) no
C10 . C11 . 1.357(13) yes
C10 . H10 . 2.000(13) no
C10 . H11 . 0.95(6) no
C10 . H12 . 2.030(13) no
C10 . H22 2_556 3.105(13) no
C10 . H23 2_556 3.055(13) no
C10 . H30 2_556 3.315(14) no
C10 . H61 . 3.124(16) no
C11 . H4 . 3.234(14) no
C11 . H10 . 0.95(4) no
C11 . H11 . 2.017(13) no
C11 . H12 . 3.211(15) no
C11 . H13 . 2.565(14) no
C11 . H23 2_556 3.314(14) no
C11 . H61 . 3.504(18) no
C12 . C13 . 1.526(12) yes
C12 . C14 . 1.537(14) yes
C12 . C15 . 1.555(14) yes
C12 . H12 . 2.696(14) no
C12 . H52 . 2.069(14) no
C12 . H53 . 2.083(14) no
C12 . H54 . 2.073(16) no
C12 . H55 . 2.062(14) no
C12 . H56 . 2.053(15) no
C12 . H57 . 2.063(14) no
C12 . H58 . 2.052(12) no
C12 . H59 . 2.046(12) no
C12 . H60 . 2.049(13) no
C13 . C14 . 2.494(15) yes
C13 . C15 . 2.484(14) yes
C13 . H17 . 3.334(14) no
C13 . H52 . 3.306(15) no
C13 . H53 . 2.661(15) no
C13 . H54 . 2.655(15) no
C13 . H55 . 3.318(15) no
C13 . H56 . 2.664(16) no
C13 . H56 2_656 3.502(15) no
C13 . H57 . 2.667(15) no
C13 . H57 2_656 3.258(16) no
C13 . H58 . 0.95(4) no
C13 . H58 2_656 3.50(2) no
C13 . H59 . 0.95(6) no
C13 . H60 . 0.95(4) no
C13 . H62 . 3.269(17) no
C14 . C15 . 2.514(18) yes
C14 . H23 2_556 3.422(17) no
C14 . H37 2_556 3.488(15) no
C14 . H52 . 2.695(18) no
C14 . H53 . 2.680(18) no
C14 . H54 . 3.334(19) no
C14 . H55 . 0.95(7) no
C14 . H56 . 0.95(7) no
C14 . H57 . 0.95(4) no
C14 . H58 . 2.665(15) no
C14 . H58 2_656 3.262(16) no
C14 . H59 . 2.666(14) no
C14 . H59 2_656 3.502(15) no
C14 . H60 . 3.318(15) no
C15 . H9 1_546 3.051(14) no
C15 . H12 . 2.420(16) no
C15 . H50 1_546 3.586(17) no
C15 . H52 . 0.95(7) no
C15 . H53 . 0.95(4) no
C15 . H54 . 0.95(4) no
C15 . H55 . 2.707(19) no
C15 . H56 . 3.335(18) no
C15 . H57 . 2.667(18) no
C15 . H58 . 2.636(15) no
C15 . H59 . 3.313(15) no
C15 . H60 . 2.661(15) no
C16 . C17 . 1.396(11) yes
C16 . C18 . 2.496(11) yes
C16 . C22 . 2.341(12) yes
C16 . C28 . 3.486(12) yes
C16 . C29 . 3.385(13) yes
C16 . H7 . 2.468(12) no
C16 . H14 . 0.95(3) no
C16 . H14 2_565 3.531(16) no
C16 . H21 . 2.736(13) no
C16 . H22 . 2.524(13) no
C17 . C18 . 1.418(11) yes
C17 . C19 . 2.460(12) yes
C17 . C20 . 2.799(13) yes
C17 . C21 . 2.423(13) yes
C17 . C22 . 1.396(13) yes
C17 . C28 . 3.462(13) yes
C17 . H7 . 2.037(12) no
C17 . H8 . 3.279(13) no
C17 . H14 . 2.000(11) no
C17 . H14 2_565 3.507(12) no
C17 . H21 2_565 3.554(14) no
C18 . C19 . 1.470(11) yes
C18 . C20 . 2.480(12) yes
C18 . C21 . 2.845(12) yes
C18 . C22 . 2.448(12) yes
C18 . C23 . 2.612(12) yes
C18 . C24 . 3.116(13) yes
C18 . C25 . 3.115(14) yes
C18 . H7 . 3.299(12) no
C18 . H9 . 3.336(12) no
C18 . H14 . 3.306(11) no
C18 . H19 . 3.590(13) no
C18 . H43 . 2.807(12) no
C18 . H44 . 3.351(13) no
C18 . H47 . 3.357(15) no
C18 . H48 . 2.788(14) no
C19 . C20 . 1.40(1) yes
C19 . C21 . 2.426(11) yes
C19 . C22 . 2.803(12) yes
C19 . C23 . 1.533(11) yes
C19 . C24 . 2.523(13) yes
C19 . C25 . 2.504(14) yes
C19 . C26 . 2.575(12) yes
C19 . H8 . 3.279(12) no
C19 . H9 . 2.04(1) no
C19 . H43 . 2.696(13) no
C19 . H44 . 2.694(13) no
C19 . H45 . 3.344(13) no
C19 . H46 . 3.332(14) no
C19 . H47 . 2.678(14) no
C19 . H48 . 2.662(15) no
C19 . H49 . 2.774(12) no
C19 . H50 . 2.750(12) no
C19 . H51 . 3.381(12) no
C20 . C21 . 1.377(12) yes
C20 . C22 . 2.392(12) yes
C20 . C23 . 2.542(12) yes
C20 . C25 . 3.574(15) yes
C20 . C26 . 2.841(14) yes
C20 . C32 2_665 3.573(13) yes
C20 . H2 2_665 2.976(13) no
C20 . H7 . 3.245(13) no
C20 . H8 . 2.024(11) no
C20 . H9 . 0.95(7) no
C20 . H12 1_564 3.198(13) no
C20 . H21 2_565 3.350(12) no
C20 . H44 . 3.542(13) no
C20 . H47 . 3.476(15) no
C20 . H49 . 2.769(13) no
C20 . H50 . 2.720(14) no
C20 . H52 1_564 3.032(15) no
C21 . C22 . 1.384(11) yes
C21 . C33 . 3.578(14) yes
C21 . H2 2_665 3.032(13) no
C21 . H7 . 2.028(12) no
C21 . H8 . 0.95(6) no
C21 . H9 . 2.024(12) no
C21 . H21 2_565 2.700(13) no
C21 . H37 2_565 3.413(12) no
C21 . H38 2_565 3.554(12) no
C21 . H39 2_565 3.541(12) no
C21 . H52 1_564 3.288(15) no
C22 . C28 . 3.497(13) yes
C22 . C32 . 3.507(14) yes
C22 . C33 . 3.343(13) yes
C22 . H7 . 0.95(3) no
C22 . H8 . 2.035(12) no
C22 . H9 . 3.249(13) no
C22 . H14 . 2.414(12) no
C22 . H21 2_565 2.820(13) no
C22 . H39 2_565 3.575(13) no
C23 . C24 . 1.538(13) yes
C23 . C25 . 1.552(15) yes
C23 . C26 . 1.559(12) yes
C23 . H9 . 2.669(12) no
C23 . H43 . 2.064(13) no
C23 . H44 . 2.049(15) no
C23 . H45 . 2.067(12) no
C23 . H46 . 2.081(14) no
C23 . H47 . 2.077(15) no
C23 . H48 . 2.060(15) no
C23 . H49 . 2.077(13) no
C23 . H50 . 2.080(12) no
C23 . H51 . 2.079(12) no
C24 . C25 . 2.511(18) yes
C24 . C26 . 2.525(16) yes
C24 . H4 2_566 3.013(14) no
C24 . H5 2_566 3.408(15) no
C24 . H19 . 3.279(15) no
C24 . H43 . 0.95(8) no
C24 . H44 . 0.95(7) no
C24 . H45 . 0.95(3) no
C24 . H46 . 2.689(18) no
C24 . H47 . 3.336(18) no
C24 . H48 . 2.669(18) no
C24 . H49 . 2.707(16) no
C24 . H50 . 3.345(16) no
C24 . H51 . 2.691(16) no
C25 . C26 . 2.503(17) yes
C25 . H29 2_565 3.260(16) no
C25 . H43 . 2.684(18) no
C25 . H44 . 3.329(18) no
C25 . H45 . 2.691(17) no
C25 . H46 . 0.95(3) no
C25 . H46 2_575 3.26(2) no
C25 . H47 . 0.95(6) no
C25 . H47 2_575 3.58(2) no
C25 . H48 . 0.95(8) no
C25 . H49 . 3.331(17) no
C25 . H50 . 2.679(18) no
C25 . H51 . 2.659(16) no
C25 . H61 2_566 3.48(2) no
C25 . H63 2_566 3.56(2) no
C26 . H9 . 2.411(14) no
C26 . H12 1_564 3.440(15) no
C26 . H26 1_565 3.270(14) no
C26 . H32 1_565 3.577(16) no
C26 . H43 . 3.350(16) no
C26 . H44 . 2.710(16) no
C26 . H45 . 2.674(15) no
C26 . H46 . 2.662(17) no
C26 . H47 . 2.689(17) no
C26 . H48 . 3.326(17) no
C26 . H49 . 0.95(6) no
C26 . H50 . 0.95(5) no
C26 . H51 . 0.95(3) no
C27 . C28 . 1.387(12) yes
C27 . C29 . 2.523(12) yes
C27 . C33 . 2.326(12) yes
C27 . H3 . 2.431(11) no
C27 . H15 . 0.95(4) no
C27 . H17 . 3.134(13) no
C27 . H18 . 2.507(12) no
C27 . H19 . 3.021(12) no
C27 . H35 1_655 3.545(13) no
C27 . H36 1_655 3.366(13) no
C27 . H57 2_656 3.455(14) no
C28 . C29 . 1.428(11) yes
C28 . C30 . 2.483(12) yes
C28 . C31 . 2.805(14) yes
C28 . C32 . 2.454(14) yes
C28 . C33 . 1.400(12) yes
C28 . H2 . 3.311(14) no
C28 . H3 . 2.028(11) no
C28 . H7 . 3.514(13) no
C28 . H14 . 3.553(12) no
C28 . H15 . 2.006(11) no
C28 . H53 2_656 2.941(15) no
C29 . C30 . 1.474(12) yes
C29 . C31 . 2.453(12) yes
C29 . C32 . 2.857(12) yes
C29 . C33 . 2.443(11) yes
C29 . C34 . 2.610(12) yes
C29 . C35 . 3.124(13) yes
C29 . C36 . 3.092(13) yes
C29 . H1 . 3.305(13) no
C29 . H3 . 3.291(11) no
C29 . H7 . 3.470(13) no
C29 . H14 . 3.111(12) no
C29 . H15 . 3.335(12) no
C29 . H22 . 3.560(14) no
C29 . H28 . 3.373(13) no
C29 . H30 . 2.803(12) no
C29 . H31 . 2.764(13) no
C29 . H33 . 3.325(14) no
C29 . H53 2_656 3.032(14) no
C30 . C31 . 1.369(11) yes
C30 . C32 . 2.435(12) yes
C30 . C33 . 2.802(12) yes
C30 . C34 . 1.551(12) yes
C30 . C35 . 2.522(12) yes
C30 . C36 . 2.525(13) yes
C30 . C37 . 2.525(13) yes
C30 . H1 . 1.995(12) no
C30 . H2 . 3.285(13) no
C30 . H7 . 3.339(14) no
C30 . H14 . 3.554(13) no
C30 . H25 . 2.703(13) no
C30 . H26 . 3.352(13) no
C30 . H27 . 2.678(13) no
C30 . H28 . 2.681(13) no
C30 . H29 . 3.351(12) no
C30 . H30 . 2.686(13) no
C30 . H31 . 2.687(13) no
C30 . H32 . 3.354(13) no
C30 . H33 . 2.686(14) no
C30 . H53 2_656 3.191(14) no
C31 . C32 . 1.399(12) yes
C31 . C33 . 2.394(13) yes
C31 . C34 . 2.550(13) yes
C31 . C35 . 3.585(13) yes
C31 . C36 . 3.590(13) yes
C31 . C37 . 2.830(14) yes
C31 . H1 . 0.95(4) no
C31 . H2 . 2.055(12) no
C31 . H3 . 3.254(13) no
C31 . H7 . 3.234(13) no
C31 . H9 2_665 3.552(13) no
C31 . H25 . 2.734(14) no
C31 . H27 . 2.697(14) no
C31 . H28 . 3.484(13) no
C31 . H33 . 3.492(14) no
C31 . H38 2_565 3.351(14) no
C31 . H49 2_665 3.524(15) no
C31 . H53 2_656 3.278(15) no
C32 . C33 . 1.397(12) yes
C32 . H1 . 2.038(13) no
C32 . H2 . 0.95(8) no
C32 . H2 2_665 3.292(19) no
C32 . H3 . 2.038(13) no
C32 . H3 2_665 3.586(13) no
C32 . H7 . 3.290(14) no
C32 . H8 . 3.504(14) no
C32 . H8 2_665 3.327(13) no
C32 . H9 2_665 3.104(13) no
C32 . H38 2_565 3.440(14) no
C32 . H52 2_656 3.327(15) no
C32 . H53 2_656 3.229(15) no
C33 . H1 . 3.253(13) no
C33 . H2 . 2.057(12) no
C33 . H2 2_665 3.272(13) no
C33 . H3 . 0.95(3) no
C33 . H7 . 3.413(13) no
C33 . H8 2_665 3.482(12) no
C33 . H15 . 2.408(12) no
C33 . H52 2_656 3.379(15) no
C33 . H53 2_656 3.035(15) no
C34 . C35 . 1.527(13) yes
C34 . C36 . 1.551(14) yes
C34 . C37 . 1.500(13) yes
C34 . H1 . 2.664(14) no
C34 . H25 . 2.024(13) no
C34 . H26 . 2.040(13) no
C34 . H27 . 2.013(14) no
C34 . H28 . 2.037(15) no
C34 . H29 . 2.063(13) no
C34 . H30 . 2.049(14) no
C34 . H31 . 2.067(14) no
C34 . H32 . 2.083(13) no
C34 . H33 . 2.065(16) no
C35 . C36 . 2.521(17) yes
C35 . C37 . 2.451(14) yes
C35 . H11 2_556 3.127(14) no
C35 . H14 . 3.346(14) no
C35 . H22 . 3.381(16) no
C35 . H25 . 3.279(15) no
C35 . H26 . 2.620(14) no
C35 . H27 . 2.623(14) no
C35 . H28 . 0.95(9) no
C35 . H29 . 0.95(3) no
C35 . H30 . 0.95(5) no
C35 . H31 . 2.701(18) no
C35 . H32 . 2.708(17) no
C35 . H33 . 3.334(18) no
C35 . H47 2_565 3.217(15) no
C35 . H48 2_565 3.582(17) no
C35 . H51 1_545 3.510(15) no
C36 . C37 . 2.471(15) yes
C36 . H25 . 2.628(15) no
C36 . H26 . 2.662(16) no
C36 . H27 . 3.294(16) no
C36 . H28 . 3.335(18) no
C36 . H29 . 2.708(17) no
C36 . H30 . 2.700(17) no
C36 . H31 . 0.95(5) no
C36 . H32 . 0.95(3) no
C36 . H33 . 0.95(4) no
C37 . H1 . 2.407(14) no
C37 . H25 . 0.95(4) no
C37 . H25 2_655 3.38(2) no
C37 . H26 . 0.95(3) no
C37 . H27 . 0.95(8) no
C37 . H28 . 2.626(16) no
C37 . H29 . 2.628(14) no
C37 . H30 . 3.275(14) no
C37 . H31 . 3.289(15) no
C37 . H32 . 2.649(15) no
C37 . H33 . 2.653(17) no
C37 . H51 1_545 3.475(14) no
C38 . C39 . 1.460(12) yes
C38 . C40 . 2.546(13) yes
C38 . C44 . 2.416(13) yes
C38 . H4 . 2.533(12) no
C38 . H16 . 0.95(5) no
C38 . H16 2_566 3.358(16) no
C38 . H17 . 2.988(13) no
C38 . H19 . 3.043(13) no
C38 . H20 . 2.401(12) no
C38 . H20 2_566 3.042(12) no
C38 . H24 . 3.452(12) no
C38 . H64 2_566 3.46(7) no
C39 . C40 . 1.456(12) yes
C39 . C41 . 2.484(13) yes
C39 . C42 . 2.770(14) yes
C39 . C43 . 2.410(13) yes
C39 . C44 . 1.365(12) yes
C39 . H4 . 2.000(12) no
C39 . H5 . 3.264(13) no
C39 . H13 . 3.283(12) no
C39 . H16 . 2.065(12) no
C39 . H20 2_566 2.942(12) no
C39 . H24 . 2.945(13) no
C39 . H64 2_566 3.44(7) no
C40 . C41 . 1.473(11) yes
C40 . C42 . 2.450(14) yes
C40 . C43 . 2.862(12) yes
C40 . C44 . 2.453(12) yes
C40 . C45 . 2.590(13) yes
C40 . C46 . 3.108(13) yes
C40 . C47 . 3.105(14) yes
C40 . H4 . 3.303(13) no
C40 . H6 . 3.304(14) no
C40 . H16 . 3.353(13) no
C40 . H20 2_566 3.461(12) no
C40 . H24 . 2.601(12) no
C40 . H37 . 3.372(13) no
C40 . H39 . 2.790(12) no
C40 . H40 . 2.783(13) no
C40 . H42 . 3.386(14) no
C40 . H64 2_566 2.79(7) no
C41 . C42 . 1.377(13) yes
C41 . C43 . 2.447(13) yes
C41 . C44 . 2.804(14) yes
C41 . C45 . 1.546(13) yes
C41 . C46 . 2.556(12) yes
C41 . C47 . 2.513(14) yes
C41 . C48 . 2.531(13) yes
C41 . H5 . 3.297(13) no
C41 . H6 . 2.005(13) no
C41 . H24 . 3.219(14) no
C41 . H34 . 2.699(14) no
C41 . H35 . 3.351(14) no
C41 . H36 . 2.709(13) no
C41 . H37 . 2.744(12) no
C41 . H38 . 3.370(13) no
C41 . H39 . 2.725(12) no
C41 . H40 . 2.680(13) no
C41 . H41 . 3.333(14) no
C41 . H42 . 2.694(14) no
C42 . C43 . 1.395(14) yes
C42 . C44 . 2.372(15) yes
C42 . C45 . 2.574(15) yes
C42 . C48 . 2.862(16) yes
C42 . H4 . 3.230(15) no
C42 . H5 . 2.054(14) no
C42 . H6 . 0.95(3) no
C42 . H34 . 2.742(16) no
C42 . H34 2_466 3.038(15) no
C42 . H36 . 2.766(15) no
C42 . H37 . 3.570(14) no
C42 . H42 . 3.521(15) no
C42 . H42 2_466 3.366(16) no
C43 . C44 . 1.377(12) yes
C43 . H4 . 2.013(14) no
C43 . H5 . 0.95(8) no
C43 . H6 . 2.026(14) no
C43 . H10 . 3.510(15) no
C43 . H13 . 3.523(14) no
C43 . H34 2_466 3.267(15) no
C43 . H42 2_466 3.582(15) no
C43 . H45 2_566 3.396(15) no
C44 . H4 . 0.95(8) no
C44 . H5 . 2.038(12) no
C44 . H6 . 3.226(15) no
C44 . H10 . 3.244(14) no
C44 . H13 . 3.166(12) no
C44 . H16 . 2.558(13) no
C44 . H19 2_566 3.567(12) no
C44 . H20 2_566 3.252(12) no
C44 . H43 2_566 3.375(14) no
C44 . H45 2_566 3.272(14) no
C45 . C46 . 1.553(13) yes
C45 . C47 . 1.524(13) yes
C45 . C48 . 1.525(13) yes
C45 . H6 . 2.707(16) no
C45 . H34 . 2.047(14) no
C45 . H35 . 2.053(13) no
C45 . H36 . 2.044(13) no
C45 . H37 . 2.073(12) no
C45 . H38 . 2.074(13) no
C45 . H39 . 2.071(13) no
C45 . H40 . 2.052(13) no
C45 . H41 . 2.046(13) no
C45 . H42 . 2.045(13) no
C46 . C47 . 2.507(13) yes
C46 . C48 . 2.474(14) yes
C46 . H3 1_455 3.508(13) no
C46 . H7 2_565 3.522(13) no
C46 . H8 2_565 2.904(12) no
C46 . H24 . 3.389(14) no
C46 . H34 . 3.306(14) no
C46 . H35 . 2.636(14) no
C46 . H36 . 2.637(14) no
C46 . H37 . 0.95(4) no
C46 . H38 . 0.95(8) no
C46 . H39 . 0.95(4) no
C46 . H40 . 2.707(13) no
C46 . H41 . 2.649(14) no
C46 . H42 . 3.330(14) no
C46 . H55 2_556 3.531(15) no
C47 . C48 . 2.477(14) yes
C47 . H27 2_565 3.482(16) no
C47 . H34 . 2.662(15) no
C47 . H35 . 2.641(14) no
C47 . H36 . 3.299(14) no
C47 . H37 . 3.327(14) no
C47 . H38 . 2.666(13) no
C47 . H39 . 2.699(14) no
C47 . H40 . 0.95(4) no
C47 . H41 . 0.95(8) no
C47 . H42 . 0.95(4) no
C47 . H64 2_566 3.49(7) no
C48 . H6 . 2.454(16) no
C48 . H15 1_455 3.003(13) no
C48 . H18 1_455 3.180(15) no
C48 . H34 . 0.95(4) no
C48 . H35 . 0.95(8) no
C48 . H36 . 0.95(4) no
C48 . H37 . 2.644(14) no
C48 . H38 . 2.643(14) no
C48 . H39 . 3.301(14) no
C48 . H40 . 3.304(14) no
C48 . H41 . 2.645(15) no
C48 . H42 . 2.646(14) no
C49 . H16 . 3.37(2) no
C49 . H17 . 3.414(18) no
C49 . H40 2_566 3.213(18) no
C49 . H48 2_566 3.25(2) no
C49 . H60 . 3.336(17) no
C49 . H61 . 0.95(6) no
C49 . H62 . 0.95(7) no
C49 . H63 . 0.95(3) no
C49 . H64 . 1.74(7) no
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_site_symmetry_1
_geom_torsion_atom_site_label_2
_geom_torsion_site_symmetry_2
_geom_torsion_atom_site_label_3
_geom_torsion_site_symmetry_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
O3 . Zn1 . O1 . C7 . -160.1(6) yes
N1 . Zn1 . O1 . C7 . -27.5(8) yes
N3 . Zn1 . O1 . C7 . 94.9(7) yes
O1 . Zn1 . O3 . C29 . -104.1(8) yes
N1 . Zn1 . O3 . C29 . 135.2(8) yes
N3 . Zn1 . O3 . C29 . 4.9(8) yes
O1 . Zn1 . N1 . C1 . -164.6(8) yes
O1 . Zn1 . N1 . C5 . 14.6(8) yes
O3 . Zn1 . N1 . C1 . -33.7(1) yes
O3 . Zn1 . N1 . C5 . 145.6(8) yes
N3 . Zn1 . N1 . C1 . 85.8(9) yes
N3 . Zn1 . N1 . C5 . -94.9(9) yes
O1 . Zn1 . N3 . C3 . -50.8(7) yes
O1 . Zn1 . N3 . C27 . 117.7(7) yes
O3 . Zn1 . N3 . C3 . -172.9(6) yes
O3 . Zn1 . N3 . C27 . -4.4(7) yes
N1 . Zn1 . N3 . C3 . 55.1(9) yes
N1 . Zn1 . N3 . C27 . -136.4(7) yes
O4 . Zn2 . O2 . C18 . -142.2(7) yes
N2 . Zn2 . O2 . C18 . -15.2(9) yes
N4 . Zn2 . O2 . C18 . 111.9(8) yes
O2 . Zn2 . O4 . C40 . -154.6(7) yes
N2 . Zn2 . O4 . C40 . 88.7(8) yes
N4 . Zn2 . O4 . C40 . -40.1(7) yes
O2 . Zn2 . N2 . C2 . -168.1(7) yes
O2 . Zn2 . N2 . C16 . 8.2(7) yes
O4 . Zn2 . N2 . C2 . -40.0(9) yes
O4 . Zn2 . N2 . C16 . 136.3(6) yes
N4 . Zn2 . N2 . C2 . 74.1(9) yes
N4 . Zn2 . N2 . C16 . -109.6(7) yes
O2 . Zn2 . N4 . C4 . -31.6(9) yes
O2 . Zn2 . N4 . C38 . 144.9(7) yes
O4 . Zn2 . N4 . C4 . -154.2(7) yes
O4 . Zn2 . N4 . C38 . 22.3(8) yes
N2 . Zn2 . N4 . C4 . 80.0(8) yes
N2 . Zn2 . N4 . C38 . -103.4(8) yes
Zn1 . O1 . C7 . C6 . 25.6(1) yes
Zn1 . O1 . C7 . C8 . -156.3(6) yes
Zn2 . O2 . C18 . C17 . 13.4(1) yes
Zn2 . O2 . C18 . C19 . -167.0(5) yes
Zn1 . O3 . C29 . C28 . -5.6(1) yes
Zn1 . O3 . C29 . C30 . 174.5(5) yes
Zn2 . O4 . C40 . C39 . 33.6(1) yes
Zn2 . O4 . C40 . C41 . -148.5(6) yes
Zn1 . N1 . C1 . C2 . 2.8(1) yes
C5 . N1 . C1 . C2 . -176.4(1) yes
Zn1 . N1 . C5 . C6 . 0.8(1) yes
C1 . N1 . C5 . C6 . -179.9(1) yes
Zn2 . N2 . C2 . C1 . -22.9(1) yes
C16 . N2 . C2 . C1 . 160.8(9) yes
Zn2 . N2 . C16 . C17 . 0.1(1) yes
C2 . N2 . C16 . C17 . 176.7(1) yes
Zn1 . N3 . C3 . C4 . -103.7(7) yes
C27 . N3 . C3 . C4 . 87.7(1) yes
Zn1 . N3 . C27 . C28 . 5.3(1) yes
C3 . N3 . C27 . C28 . 174.0(9) yes
Zn2 . N4 . C4 . C3 . -93.9(8) yes
C38 . N4 . C4 . C3 . 89.5(1) yes
Zn2 . N4 . C38 . C39 . 1.9(1) yes
C4 . N4 . C38 . C39 . 178.8(9) yes
N1 . C1 . C2 . N2 . -71.7(1) yes
N3 . C3 . C4 . N4 . 59.1(9) yes
N1 . C5 . C6 . C7 . -9.9(2) yes
N1 . C5 . C6 . C11 . 170.3(1) yes
C5 . C6 . C7 . O1 . -4.8(1) yes
C5 . C6 . C7 . C8 . 177.0(8) yes
C11 . C6 . C7 . O1 . 174.9(9) yes
C11 . C6 . C7 . C8 . -3.3(1) yes
C5 . C6 . C11 . C10 . -178.2(1) yes
C7 . C6 . C11 . C10 . 2.1(2) yes
O1 . C7 . C8 . C9 . -176.6(8) yes
O1 . C7 . C8 . C12 . 3.8(1) yes
C6 . C7 . C8 . C9 . 1.7(1) yes
C6 . C7 . C8 . C12 . -177.9(8) yes
C7 . C8 . C9 . C10 . 1.2(1) yes
C12 . C8 . C9 . C10 . -179.2(9) yes
C7 . C8 . C12 . C13 . 57.4(1) yes
C7 . C8 . C12 . C14 . -63.3(1) yes
C7 . C8 . C12 . C15 . 176.4(8) yes
C9 . C8 . C12 . C13 . -122.1(1) yes
C9 . C8 . C12 . C14 . 117.1(1) yes
C9 . C8 . C12 . C15 . -3.1(1) yes
C8 . C9 . C10 . C11 . -2.6(2) yes
C9 . C10 . C11 . C6 . 0.9(2) yes
N2 . C16 . C17 . C18 . -6.2(2) yes
N2 . C16 . C17 . C22 . 173.2(8) yes
C16 . C17 . C18 . O2 . -1.2(2) yes
C16 . C17 . C18 . C19 . 179.2(8) yes
C22 . C17 . C18 . O2 . 179.4(9) yes
C22 . C17 . C18 . C19 . -0.2(1) yes
C16 . C17 . C22 . C21 . -179.1(9) yes
C18 . C17 . C22 . C21 . 0.3(1) yes
O2 . C18 . C19 . C20 . 179.7(8) yes
O2 . C18 . C19 . C23 . -0.8(1) yes
C17 . C18 . C19 . C20 . -0.7(1) yes
C17 . C18 . C19 . C23 . 178.9(8) yes
C18 . C19 . C20 . C21 . 1.4(1) yes
C23 . C19 . C20 . C21 . -178.2(9) yes
C18 . C19 . C23 . C24 . 57.8(1) yes
C18 . C19 . C23 . C25 . -61.2(1) yes
C18 . C19 . C23 . C26 . -179.7(8) yes
C20 . C19 . C23 . C24 . -122.7(1) yes
C20 . C19 . C23 . C25 . 118.3(1) yes
C20 . C19 . C23 . C26 . -0.2(1) yes
C19 . C20 . C21 . C22 . -1.2(1) yes
C20 . C21 . C22 . C17 . 0.4(1) yes
N3 . C27 . C28 . C29 . -5.3(2) yes
N3 . C27 . C28 . C33 . 178.3(8) yes
C27 . C28 . C29 . O3 . 5.1(1) yes
C27 . C28 . C29 . C30 . -175.1(9) yes
C33 . C28 . C29 . O3 . -178.7(8) yes
C33 . C28 . C29 . C30 . 1.2(1) yes
C27 . C28 . C33 . C32 . 176.6(9) yes
C29 . C28 . C33 . C32 . -0.2(1) yes
O3 . C29 . C30 . C31 . 178.2(8) yes
O3 . C29 . C30 . C34 . -3.0(1) yes
C28 . C29 . C30 . C31 . -1.7(1) yes
C28 . C29 . C30 . C34 . 177.1(9) yes
C29 . C30 . C31 . C32 . 1.1(1) yes
C34 . C30 . C31 . C32 . -177.6(9) yes
C29 . C30 . C34 . C35 . 61.6(1) yes
C29 . C30 . C34 . C36 . -59.0(1) yes
C29 . C30 . C34 . C37 . -178.3(9) yes
C31 . C30 . C34 . C35 . -119.6(1) yes
C31 . C30 . C34 . C36 . 119.8(1) yes
C31 . C30 . C34 . C37 . 0.4(1) yes
C30 . C31 . C32 . C33 . -0.1(2) yes
C31 . C32 . C33 . C28 . -0.4(1) yes
N4 . C38 . C39 . C40 . -19.9(1) yes
N4 . C38 . C39 . C44 . 161.8(9) yes
C38 . C39 . C40 . O4 . 0.2(1) yes
C38 . C39 . C40 . C41 . -177.8(8) yes
C44 . C39 . C40 . O4 . 178.4(9) yes
C44 . C39 . C40 . C41 . 0.4(1) yes
C38 . C39 . C44 . C43 . -179.0(9) yes
C40 . C39 . C44 . C43 . 2.8(2) yes
O4 . C40 . C41 . C42 . 178.3(8) yes
O4 . C40 . C41 . C45 . 0.5(1) yes
C39 . C40 . C41 . C42 . -3.7(1) yes
C39 . C40 . C41 . C45 . 178.5(9) yes
C40 . C41 . C42 . C43 . 4.3(2) yes
C45 . C41 . C42 . C43 . -178.0(1) yes
C40 . C41 . C45 . C46 . 58.3(1) yes
C40 . C41 . C45 . C47 . -62.6(1) yes
C40 . C41 . C45 . C48 . 177.3(8) yes
C42 . C41 . C45 . C46 . -119.3(1) yes
C42 . C41 . C45 . C47 . 119.8(1) yes
C42 . C41 . C45 . C48 . -0.4(2) yes
C41 . C42 . C43 . C44 . -1.3(2) yes
C42 . C43 . C44 . C39 . -2.4(2) yes
|
1100933.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-17 15:24:33 +0200 (Thu, 17 Mar 2016) $
#$Revision: 178239 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100933.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_1100933
loop_
_publ_author_name
'Ye, Ning'
'Stone-Sundberg, Jennifer L.'
'Hruschka, Michael A.'
'Aka, Gerard'
'Kong, Wei'
'Keszler, Douglas A.'
_publ_section_title
;
Nonlinear Optical Crystal Y~x~La~y~Sc~z~(BO~3~)~4~ (x + y + z = 4)
;
_journal_coden_ASTM CMATEX
_journal_issue 10
_journal_name_full 'Chemistry of Materials'
_journal_page_first 2687
_journal_page_last 2692
_journal_paper_doi 10.1021/cm050090c
_journal_volume 17
_journal_year 2005
_chemical_absolute_configuration unk
_chemical_formula_sum 'B4 La0.72 O12 Sc2.71 Y0.57'
_chemical_formula_weight 507.78
_space_group_IT_number 155
_symmetry_cell_setting trigonal
_symmetry_space_group_name_Hall 'R 3 2"'
_symmetry_space_group_name_H-M 'R 3 2 :H'
_audit_creation_date 2004-07-05T21:04:02-00:00
_audit_creation_method 'WinGX routine CIF_UPDATE'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 3
_cell_length_a 9.7739(10)
_cell_length_b 9.7739(10)
_cell_length_c 7.9456(14)
_cell_measurement_temperature 298(2)
_cell_volume 657.34(15)
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71069
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 11
_diffrn_reflns_limit_l_min -11
_diffrn_reflns_number 2574
_diffrn_reflns_theta_full 30.04
_diffrn_reflns_theta_max 30.04
_diffrn_reflns_theta_min 3.52
_exptl_absorpt_coefficient_mu 9.257
_exptl_absorpt_correction_type none
_exptl_crystal_density_diffrn 3.848
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 708.6
_exptl_crystal_size_max 0.1
_exptl_crystal_size_mid 0.07
_exptl_crystal_size_min 0.07
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
_refine_diff_density_max 0.889
_refine_diff_density_min -1.353
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack 0.052(5)
_refine_ls_extinction_coef 0.0104(18)
_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 1.081
_refine_ls_hydrogen_treatment none
_refine_ls_matrix_type full
_refine_ls_number_parameters 35
_refine_ls_number_reflns 437
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.081
_refine_ls_R_factor_gt 0.0296
_refine_ls_shift/su_max 0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+7.3707P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_ref 0.0815
_reflns_number_gt 437
_reflns_number_total 437
_reflns_threshold_expression >2sigma(I)
_cod_duplicate_entry 4000502
_cod_data_source_file cm050090csi20050114_020153.cif
_cod_data_source_block xl
_cod_original_sg_symbol_H-M 'R 3 2'
_cod_database_code 1100933
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'y, x, -z'
'-x+y, -x, z'
'-x, -x+y, -z'
'x-y, -y, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'y+2/3, x+1/3, -z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, -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'
'y+1/3, x+2/3, -z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, -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_group
_atom_site_disorder_assembly
La La 0 0 0 0.0109(3) Uani 0.72 d SP . .
Y1 Y 0 0 0 0.0109(3) Uani 0.28 d SP . .
Sc Sc -0.11989(18) -0.3333 -0.3333 0.0111(3) Uani 0.9033 d SP . .
Y2 Y -0.11989(18) -0.3333 -0.3333 0.0111(3) Uani 0.0967 d SP . .
B1 B -0.2168(10) -0.3333 0.1667 0.0125(13) Uani 1 d S . .
B2 B 0 0 0.5 0.010(2) Uani 1 d S . .
O1 O 0 -0.4086(8) 0.5 0.0221(17) Uani 1 d S . .
O2 O -0.0188(6) 0.1927(6) -0.1809(5) 0.0161(8) Uani 1 d . . .
O3 O 0 -0.1402(6) 0.5 0.0124(10) 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
La 0.0113(3) 0.0113(3) 0.0101(4) 0 0 0.00563(15)
Y1 0.0113(3) 0.0113(3) 0.0101(4) 0 0 0.00563(15)
Sc 0.0093(5) 0.0094(5) 0.0144(7) 0.0004(4) 0.00022(18) 0.0047(3)
Y2 0.0093(5) 0.0094(5) 0.0144(7) 0.0004(4) 0.00022(18) 0.0047(3)
B1 0.011(3) 0.012(4) 0.015(3) -0.005(4) -0.0025(18) 0.006(2)
B2 0.010(3) 0.010(3) 0.012(5) 0 0 0.0048(15)
O1 0.030(4) 0.015(3) 0.026(3) 0.0064(16) 0.013(3) 0.015(2)
O2 0.0120(19) 0.0173(19) 0.0150(16) 0.0009(15) -0.0011(14) 0.0044(18)
O3 0.015(3) 0.0100(16) 0.014(2) 0.0013(10) 0.003(2) 0.0076(14)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B 0.0013 0.0007 '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'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sc Sc 0.2519 0.3716 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y -2.7962 3.5667 '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 La O2 125.3(2) 2 3 ?
O2 La O2 139.4(2) 2 5 ?
O2 La O2 89.01(15) 3 5 ?
O2 La O2 72.4(2) 2 6 ?
O2 La O2 89.01(15) 3 6 ?
O2 La O2 89.01(15) 5 6 ?
O2 La O2 89.01(15) 2 4 ?
O2 La O2 72.4(2) 3 4 ?
O2 La O2 125.3(2) 5 4 ?
O2 La O2 139.4(2) 6 4 ?
O2 La O2 89.01(15) 2 . ?
O2 La O2 139.4(2) 3 . ?
O2 La O2 72.4(2) 5 . ?
O2 La O2 125.3(2) 6 . ?
O2 La O2 89.01(15) 4 . ?
O2 Sc O2 101.2(3) 2 11_444 ?
O2 Sc O3 95.01(13) 2 8_444 ?
O2 Sc O3 92.83(18) 11_444 8_444 ?
O2 Sc O3 92.83(18) 2 1_554 ?
O2 Sc O3 95.01(13) 11_444 1_554 ?
O3 Sc O3 167.6(2) 8_444 1_554 ?
O2 Sc O1 86.74(14) 2 8_444 ?
O2 Sc O1 167.2(2) 11_444 8_444 ?
O3 Sc O1 76.3(2) 8_444 8_444 ?
O3 Sc O1 94.60(17) 1_554 8_444 ?
O2 Sc O1 167.2(2) 2 1_554 ?
O2 Sc O1 86.74(14) 11_444 1_554 ?
O3 Sc O1 94.60(16) 8_444 1_554 ?
O3 Sc O1 76.3(2) 1_554 1_554 ?
O1 Sc O1 87.33(7) 8_444 1_554 ?
O2 B1 O2 124.1(8) 6 7_445 ?
O2 B1 O1 118.0(4) 6 15_545 ?
O2 B1 O1 118.0(4) 7_445 15_545 ?
O3 B2 O3 120.0000(10) 2 . ?
O3 B2 O3 120.0000(10) 2 3_556 ?
O3 B2 O3 120.000(2) . 3_556 ?
B1 O1 Y2 128.38(17) 8_445 16_545 ?
B1 O1 Sc 128.38(17) 8_445 16_545 ?
B1 O1 Sc 128.38(17) 8_445 1_556 ?
Y2 O1 Sc 103.2(3) 16_545 1_556 ?
Sc O1 Sc 103.2(3) 16_545 1_556 ?
B1 O1 Y2 128.38(17) 8_445 1_556 ?
Y2 O1 Y2 103.2(3) 16_545 1_556 ?
Sc O1 Y2 103.2(3) 16_545 1_556 ?
B1 O2 Y2 131.6(4) 13_554 4 ?
B1 O2 Sc 131.6(4) 13_554 4 ?
B1 O2 La 108.7(4) 13_554 . ?
Y2 O2 La 119.4(2) 4 . ?
Sc O2 La 119.4(2) 4 . ?
B2 O3 Y2 127.96(14) . 1_556 ?
B2 O3 Sc 127.96(14) . 1_556 ?
B2 O3 Y2 127.96(14) . 16_545 ?
Y2 O3 Y2 104.1(3) 1_556 16_545 ?
Sc O3 Y2 104.1(3) 1_556 16_545 ?
B2 O3 Sc 127.96(14) . 16_545 ?
Y2 O3 Sc 104.1(3) 1_556 16_545 ?
Sc O3 Sc 104.1(3) 1_556 16_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
La O2 2.448(5) 2 ?
La O2 2.448(5) 3 ?
La O2 2.448(5) 5 ?
La O2 2.448(5) 6 ?
La O2 2.448(5) 4 ?
La O2 2.448(5) . ?
La B1 3.1550(15) 13_554 ?
La B1 3.1551(15) 14_444 ?
La B1 3.1551(15) 2 ?
La B1 3.1551(15) . ?
La B1 3.1551(15) 4 ?
La B1 3.1551(15) 16_544 ?
Sc O2 2.059(5) 2 ?
Sc O2 2.059(5) 11_444 ?
Sc O3 2.116(4) 8_444 ?
Sc O3 2.116(4) 1_554 ?
Sc O1 2.128(5) 8_444 ?
Sc O1 2.128(5) 1_554 ?
Sc Sc 3.3368(19) 8_445 ?
Sc Y2 3.3368(19) 8_445 ?
Sc Y2 3.3368(19) 16_544 ?
Sc Sc 3.3368(19) 16_544 ?
Sc La 3.8967(4) 7_444 ?
B1 O2 1.354(7) 6 ?
B1 O2 1.354(7) 7_445 ?
B1 O1 1.383(13) 15_545 ?
B1 La 3.1550(15) 7_445 ?
B2 O3 1.370(6) 2 ?
B2 O3 1.370(6) . ?
B2 O3 1.370(6) 3_556 ?
O1 B1 1.383(13) 8_445 ?
O1 Y2 2.128(5) 16_545 ?
O1 Sc 2.128(5) 16_545 ?
O1 Sc 2.128(5) 1_556 ?
O1 Y2 2.128(5) 1_556 ?
O2 B1 1.354(7) 13_554 ?
O2 Y2 2.059(5) 4 ?
O2 Sc 2.059(5) 4 ?
O3 Y2 2.116(4) 1_556 ?
O3 Sc 2.116(4) 1_556 ?
O3 Y2 2.116(4) 16_545 ?
O3 Sc 2.116(4) 16_545 ?
|
1100934.cif | #------------------------------------------------------------------------------
#$Date: 2022-09-14 17:31:13 +0300 (Wed, 14 Sep 2022) $
#$Revision: 277831 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/09/1100934.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_1100934
loop_
_publ_author_name
'Crerar, Shane J.'
'Deakin, Laura'
'Mar, Arthur'
_publ_section_title
;
Structure and Physical Properties of Ternary Antimonide YbCr~3~Sb~3~
;
_journal_coden_ASTM CMATEX
_journal_issue 10
_journal_name_full 'Chemistry of Materials'
_journal_page_first 2780
_journal_page_last 2784
_journal_paper_doi 10.1021/cm0506151
_journal_volume 17
_journal_year 2005
_chemical_formula_structural 'Yb Cr Sb3'
_chemical_formula_sum 'Cr Sb3 Yb'
_chemical_formula_weight 590.29
_chemical_name_common 'ytterbium chromium antimonide'
_chemical_name_systematic 'ytterbium chromium triantimonide'
_space_group_IT_number 57
_space_group_name_Hall '-P 2c 2b'
_space_group_name_H-M_alt 'P b c m'
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall '-P 2c 2b'
_symmetry_space_group_name_H-M 'P b c m'
_atom_sites_solution_hydrogens none
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 12.981(3)
_cell_length_b 6.1396(12)
_cell_length_c 5.9926(12)
_cell_measurement_reflns_used 2892
_cell_measurement_temperature 295(2)
_cell_measurement_theta_max 33.05
_cell_measurement_theta_min 5.01
_cell_volume 477.60(16)
_computing_cell_refinement 'Bruker SAINT 6.45 (Bruker, 2003)'
_computing_data_collection 'Bruker SMART 5.015 (Bruker, 1997)'
_computing_data_reduction 'Bruker SAINT 6.45'
_computing_molecular_graphics 'ATOMS 5.1 (Dowty, 1999)'
_computing_publication_material 'Bruker SHELXTL 6.12'
_computing_structure_refinement 'Bruker SHELXTL 6.12'
_computing_structure_solution 'Bruker SHELXTL 6.12'
_diffrn_ambient_temperature 295(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type 'Bruker Platform/SMART 1000 CCD'
_diffrn_measurement_method '\w scans (0.2\%)'
_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 0.0592
_diffrn_reflns_av_sigmaI/netI 0.0387
_diffrn_reflns_limit_h_max 19
_diffrn_reflns_limit_h_min -19
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_k_min -9
_diffrn_reflns_limit_l_max 9
_diffrn_reflns_limit_l_min -9
_diffrn_reflns_number 6074
_diffrn_reflns_theta_full 33.16
_diffrn_reflns_theta_max 33.16
_diffrn_reflns_theta_min 1.57
_exptl_absorpt_coefficient_mu 38.140
_exptl_absorpt_correction_T_max 0.654
_exptl_absorpt_correction_T_min 0.087
_exptl_absorpt_correction_type numerical
_exptl_absorpt_process_details 'Bruker SHELXTL 6.12 (Sheldrick, 2001)'
_exptl_crystal_colour black
_exptl_crystal_density_diffrn 8.209
_exptl_crystal_description needle
_exptl_crystal_F_000 988
_exptl_crystal_size_max 0.20
_exptl_crystal_size_mid 0.04
_exptl_crystal_size_min 0.01
_refine_diff_density_max 7.799
_refine_diff_density_min -3.192
_refine_diff_density_rms 0.982
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.173
_refine_ls_hydrogen_treatment none
_refine_ls_matrix_type full
_refine_ls_number_parameters 29
_refine_ls_number_reflns 974
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.173
_refine_ls_R_factor_all 0.0710
_refine_ls_R_factor_gt 0.0590
_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^)+(0.0920P)^2^+10.3941P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1550
_refine_ls_wR_factor_ref 0.1613
_reflns_number_gt 825
_reflns_number_total 974
_reflns_threshold_expression I>2\s(I)
_cod_duplicate_entry 4000575
_cod_data_source_file cm0506151si20050321_044701.cif
_cod_data_source_block pbcm
_cod_database_code 1100934
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z-1/2'
'x, -y-1/2, z-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
Yb Yb 0.31066(6) 0.00136(11) 0.2500 0.0134(2) Uani 1 4 d S . .
Cr Cr 0.9018(2) 0.2500 0.0000 0.0120(5) Uani 1 4 d S . .
Sb1 Sb 0.06561(9) 0.11454(17) 0.2500 0.0127(3) Uani 1 4 d S . .
Sb2 Sb 0.22056(10) 0.48975(17) 0.2500 0.0131(3) Uani 1 4 d S . .
Sb3 Sb 0.50211(8) 0.2500 0.0000 0.0132(3) Uani 1 4 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
Yb 0.0141(4) 0.0105(4) 0.0156(4) 0.000 0.000 0.0006(2)
Cr 0.0142(13) 0.0071(11) 0.0147(13) -0.0009(9) 0.000 0.000
Sb1 0.0130(5) 0.0075(5) 0.0175(5) 0.000 0.000 0.0010(4)
Sb2 0.0151(6) 0.0088(5) 0.0155(6) 0.000 0.000 0.0013(4)
Sb3 0.0151(6) 0.0111(6) 0.0136(6) -0.0003(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
Cr Cr 0.3209 0.6236 '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'
Yb Yb -0.3850 5.5486 '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
Sb2 Yb Sb2 137.31(5) 7_565 7_566 ?
Sb2 Yb Sb2 81.49(3) 7_565 . ?
Sb2 Yb Sb2 81.49(3) 7_566 . ?
Sb2 Yb Sb3 135.26(3) 7_565 2_655 ?
Sb2 Yb Sb3 81.40(3) 7_566 2_655 ?
Sb2 Yb Sb3 135.65(3) . 2_655 ?
Sb2 Yb Sb3 81.40(3) 7_565 5_655 ?
Sb2 Yb Sb3 135.26(3) 7_566 5_655 ?
Sb2 Yb Sb3 135.65(3) . 5_655 ?
Sb3 Yb Sb3 54.98(2) 2_655 5_655 ?
Sb2 Yb Sb1 68.97(2) 7_565 . ?
Sb2 Yb Sb1 68.97(2) 7_566 . ?
Sb2 Yb Sb1 56.37(3) . . ?
Sb3 Yb Sb1 146.42(2) 2_655 . ?
Sb3 Yb Sb1 146.42(2) 5_655 . ?
Sb2 Yb Sb3 133.89(3) 7_565 6_556 ?
Sb2 Yb Sb3 80.91(3) 7_566 6_556 ?
Sb2 Yb Sb3 80.89(3) . 6_556 ?
Sb3 Yb Sb3 56.143(17) 2_655 6_556 ?
Sb3 Yb Sb3 82.22(2) 5_655 6_556 ?
Sb1 Yb Sb3 129.87(3) . 6_556 ?
Sb2 Yb Sb3 80.91(3) 7_565 . ?
Sb2 Yb Sb3 133.89(3) 7_566 . ?
Sb2 Yb Sb3 80.89(3) . . ?
Sb3 Yb Sb3 82.22(2) 2_655 . ?
Sb3 Yb Sb3 56.143(17) 5_655 . ?
Sb1 Yb Sb3 129.87(3) . . ?
Sb3 Yb Sb3 54.38(2) 6_556 . ?
Sb2 Yb Sb2 83.63(3) 7_565 1_545 ?
Sb2 Yb Sb2 83.63(3) 7_566 1_545 ?
Sb2 Yb Sb2 138.27(5) . 1_545 ?
Sb3 Yb Sb2 79.38(3) 2_655 1_545 ?
Sb3 Yb Sb2 79.38(3) 5_655 1_545 ?
Sb1 Yb Sb2 81.90(3) . 1_545 ?
Sb3 Yb Sb2 134.49(2) 6_556 1_545 ?
Sb3 Yb Sb2 134.49(2) . 1_545 ?
Sb2 Yb Cr 47.30(2) 7_565 5_655 ?
Sb2 Yb Cr 96.88(4) 7_566 5_655 ?
Sb2 Yb Cr 97.15(3) . 5_655 ?
Sb3 Yb Cr 125.34(3) 2_655 5_655 ?
Sb3 Yb Cr 100.55(4) 5_655 5_655 ?
Sb1 Yb Cr 47.45(3) . 5_655 ?
Sb3 Yb Cr 177.22(4) 6_556 5_655 ?
Sb3 Yb Cr 127.40(2) . 5_655 ?
Sb2 Yb Cr 46.48(2) 1_545 5_655 ?
Sb2 Yb Cr 96.88(4) 7_565 2_655 ?
Sb2 Yb Cr 47.30(2) 7_566 2_655 ?
Sb2 Yb Cr 97.15(3) . 2_655 ?
Sb3 Yb Cr 100.55(4) 2_655 2_655 ?
Sb3 Yb Cr 125.34(3) 5_655 2_655 ?
Sb1 Yb Cr 47.45(3) . 2_655 ?
Sb3 Yb Cr 127.40(2) 6_556 2_655 ?
Sb3 Yb Cr 177.22(4) . 2_655 ?
Sb2 Yb Cr 46.48(2) 1_545 2_655 ?
Cr Yb Cr 50.72(4) 5_655 2_655 ?
Sb2 Yb Yb 129.81(3) 7_565 7_566 ?
Sb2 Yb Yb 48.36(2) 7_566 7_566 ?
Sb2 Yb Yb 48.324(17) . 7_566 ?
Sb3 Yb Yb 90.919(11) 2_655 7_566 ?
Sb3 Yb Yb 131.507(18) 5_655 7_566 ?
Sb1 Yb Yb 81.239(17) . 7_566 ?
Sb3 Yb Yb 49.282(18) 6_556 7_566 ?
Sb3 Yb Yb 89.30(2) . 7_566 ?
Sb2 Yb Yb 131.978(15) 1_545 7_566 ?
Cr Yb Yb 127.95(3) 5_655 7_566 ?
Cr Yb Yb 90.853(10) 2_655 7_566 ?
Sb2 Cr Sb2 108.10(11) 3_645 5_665 ?
Sb2 Cr Sb1 105.76(4) 3_645 3_655 ?
Sb2 Cr Sb1 84.87(4) 5_665 3_655 ?
Sb2 Cr Sb1 84.87(4) 3_645 5_655 ?
Sb2 Cr Sb1 105.76(4) 5_665 5_655 ?
Sb1 Cr Sb1 162.16(13) 3_655 5_655 ?
Sb2 Cr Sb1 88.48(4) 3_645 1_655 ?
Sb2 Cr Sb1 160.18(7) 5_665 1_655 ?
Sb1 Cr Sb1 80.08(5) 3_655 1_655 ?
Sb1 Cr Sb1 86.03(6) 5_655 1_655 ?
Sb2 Cr Sb1 160.18(7) 3_645 7_665 ?
Sb2 Cr Sb1 88.48(4) 5_665 7_665 ?
Sb1 Cr Sb1 86.03(6) 3_655 7_665 ?
Sb1 Cr Sb1 80.08(5) 5_655 7_665 ?
Sb1 Cr Sb1 77.73(8) 1_655 7_665 ?
Sb2 Cr Yb 60.90(5) 3_645 5_655 ?
Sb2 Cr Yb 63.92(5) 5_665 5_655 ?
Sb1 Cr Yb 136.05(9) 3_655 5_655 ?
Sb1 Cr Yb 61.62(4) 5_655 5_655 ?
Sb1 Cr Yb 135.61(3) 1_655 5_655 ?
Sb1 Cr Yb 120.89(2) 7_665 5_655 ?
Sb2 Cr Yb 63.92(5) 3_645 3_655 ?
Sb2 Cr Yb 60.90(5) 5_665 3_655 ?
Sb1 Cr Yb 61.62(4) 3_655 3_655 ?
Sb1 Cr Yb 136.05(9) 5_655 3_655 ?
Sb1 Cr Yb 120.89(2) 1_655 3_655 ?
Sb1 Cr Yb 135.61(3) 7_665 3_655 ?
Yb Cr Yb 75.89(6) 5_655 3_655 ?
Cr Sb1 Cr 66.67(3) 5_655 2_655 ?
Cr Sb1 Cr 93.97(6) 5_655 1_455 ?
Cr Sb1 Cr 132.24(5) 2_655 1_455 ?
Cr Sb1 Cr 132.24(5) 5_655 6_456 ?
Cr Sb1 Cr 93.97(6) 2_655 6_456 ?
Cr Sb1 Cr 66.54(7) 1_455 6_456 ?
Cr Sb1 Sb2 121.09(7) 5_655 . ?
Cr Sb1 Sb2 121.09(7) 2_655 . ?
Cr Sb1 Sb2 106.42(5) 1_455 . ?
Cr Sb1 Sb2 106.42(5) 6_456 . ?
Cr Sb1 Yb 70.93(6) 5_655 . ?
Cr Sb1 Yb 70.93(6) 2_655 . ?
Cr Sb1 Yb 145.66(4) 1_455 . ?
Cr Sb1 Yb 145.66(4) 6_456 . ?
Sb2 Sb1 Yb 61.20(4) . . ?
Cr Sb2 Cr 67.24(5) 2_665 5_665 ?
Cr Sb2 Sb1 93.36(6) 2_665 . ?
Cr Sb2 Sb1 93.36(6) 5_665 . ?
Cr Sb2 Yb 71.80(4) 2_665 7_566 ?
Cr Sb2 Yb 135.99(3) 5_665 7_566 ?
Sb1 Sb2 Yb 104.59(2) . 7_566 ?
Cr Sb2 Yb 135.99(3) 2_665 7_565 ?
Cr Sb2 Yb 71.80(4) 5_665 7_565 ?
Sb1 Sb2 Yb 104.59(2) . 7_565 ?
Yb Sb2 Yb 137.31(5) 7_566 7_565 ?
Cr Sb2 Yb 139.77(3) 2_665 . ?
Cr Sb2 Yb 139.77(3) 5_665 . ?
Sb1 Sb2 Yb 62.43(4) . . ?
Yb Sb2 Yb 83.32(3) 7_566 . ?
Yb Sb2 Yb 83.32(3) 7_565 . ?
Cr Sb2 Yb 69.60(4) 2_665 1_565 ?
Cr Sb2 Yb 69.60(4) 5_665 1_565 ?
Sb1 Sb2 Yb 159.30(5) . 1_565 ?
Yb Sb2 Yb 81.79(3) 7_566 1_565 ?
Yb Sb2 Yb 81.79(3) 7_565 1_565 ?
Yb Sb2 Yb 138.27(5) . 1_565 ?
Sb3 Sb3 Sb3 180.00(8) 6_556 6 ?
Sb3 Sb3 Sb3 90.0 6_556 5_655 ?
Sb3 Sb3 Sb3 90.0 6 5_655 ?
Sb3 Sb3 Sb3 90.0 6_556 5_665 ?
Sb3 Sb3 Sb3 90.0 6 5_665 ?
Sb3 Sb3 Sb3 177.96(8) 5_655 5_665 ?
Sb3 Sb3 Yb 62.509(12) 6_556 3_655 ?
Sb3 Sb3 Yb 117.491(11) 6 3_655 ?
Sb3 Sb3 Yb 119.26(4) 5_655 3_655 ?
Sb3 Sb3 Yb 62.48(3) 5_665 3_655 ?
Sb3 Sb3 Yb 117.491(11) 6_556 5_655 ?
Sb3 Sb3 Yb 62.509(12) 6 5_655 ?
Sb3 Sb3 Yb 62.48(3) 5_655 5_655 ?
Sb3 Sb3 Yb 119.26(4) 5_665 5_655 ?
Yb Sb3 Yb 83.01(4) 3_655 5_655 ?
Sb3 Sb3 Yb 62.812(11) 6_556 . ?
Sb3 Sb3 Yb 117.188(11) 6 . ?
Sb3 Sb3 Yb 61.38(3) 5_655 . ?
Sb3 Sb3 Yb 116.87(4) 5_665 . ?
Yb Sb3 Yb 125.314(16) 3_655 . ?
Yb Sb3 Yb 123.857(17) 5_655 . ?
Sb3 Sb3 Yb 117.188(11) 6_556 7_565 ?
Sb3 Sb3 Yb 62.812(11) 6 7_565 ?
Sb3 Sb3 Yb 116.87(4) 5_655 7_565 ?
Sb3 Sb3 Yb 61.38(3) 5_665 7_565 ?
Yb Sb3 Yb 123.857(17) 3_655 7_565 ?
Yb Sb3 Yb 125.314(16) 5_655 7_565 ?
Yb Sb3 Yb 81.44(4) . 7_565 ?
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
Yb Sb2 3.2170(8) 7_565 ?
Yb Sb2 3.2170(8) 7_566 ?
Yb Sb2 3.2186(14) . ?
Yb Sb3 3.2455(11) 2_655 ?
Yb Sb3 3.2455(12) 5_655 ?
Yb Sb1 3.2560(16) . ?
Yb Sb3 3.2788(12) 6_556 ?
Yb Sb3 3.2788(12) . ?
Yb Sb2 3.3518(14) 1_545 ?
Yb Cr 3.498(2) 5_655 ?
Yb Cr 3.498(2) 2_655 ?
Yb Yb 4.2778(11) 7_566 ?
Cr Sb2 2.7057(19) 3_645 ?
Cr Sb2 2.7057(19) 5_665 ?
Cr Sb1 2.7262(11) 3_655 ?
Cr Sb1 2.7262(11) 5_655 ?
Cr Sb1 2.731(2) 1_655 ?
Cr Sb1 2.731(2) 7_665 ?
Cr Yb 3.498(2) 5_655 ?
Cr Yb 3.498(2) 3_655 ?
Sb1 Cr 2.7262(11) 5_655 ?
Sb1 Cr 2.7262(11) 2_655 ?
Sb1 Cr 2.731(2) 1_455 ?
Sb1 Cr 2.731(2) 6_456 ?
Sb1 Sb2 3.0582(17) . ?
Sb2 Cr 2.7057(19) 2_665 ?
Sb2 Cr 2.7057(19) 5_665 ?
Sb2 Yb 3.2170(8) 7_566 ?
Sb2 Yb 3.2170(8) 7_565 ?
Sb2 Yb 3.3518(14) 1_565 ?
Sb3 Sb3 2.9963(6) 6_556 ?
Sb3 Sb3 2.9963(6) 6 ?
Sb3 Sb3 3.0703(6) 5_655 ?
Sb3 Sb3 3.0703(6) 5_665 ?
Sb3 Yb 3.2455(12) 3_655 ?
Sb3 Yb 3.2455(11) 5_655 ?
Sb3 Yb 3.2788(12) 7_565 ?
|
1100935.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100935.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_1100935
loop_
_publ_author_name
'Joseph M. Collins'
'Ritika Uppal'
'Christopher D. Incarvito'
'Ann M. Valentine'
_publ_contact_author
;
Prof. Ann M. Valentine
Department of Chemistry
Yale University
225 Prospect St
PO Box 208107
New Haven, CT 06520-8107
USA
;
_publ_contact_author_email ann.valentine@yale.edu
_publ_contact_author_fax '+203 432 6144'
_publ_contact_author_phone '+203 432 5162'
_publ_section_title
;
Titanium(IV) Citrate Speciation and Structure under Environmentally and
Biologically Relevant Conditions
;
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3431
_journal_page_last 3440
_journal_paper_doi 10.1021/ic048158y
_journal_volume 44
_journal_year 2005
_chemical_formula_sum 'C18 H46 Na8 O38 Ti'
_chemical_formula_weight 1102.37
_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 99.27(3)
_cell_angle_beta 92.21(3)
_cell_angle_gamma 99.95(3)
_cell_formula_units_Z 2
_cell_length_a 11.634(2)
_cell_length_b 13.223(3)
_cell_length_c 13.291(3)
_cell_measurement_temperature 293(2)
_cell_volume 1982.9(8)
_computing_cell_refinement Denzo
_computing_data_collection 'Nonius Collect'
_computing_data_reduction Denzo
_computing_molecular_graphics XP
_computing_publication_material XCIF
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 293(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type 'Nonius KappaCCD'
_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 0.0249
_diffrn_reflns_av_sigmaI/netI 0.0493
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_number 16679
_diffrn_reflns_theta_full 28.66
_diffrn_reflns_theta_max 28.66
_diffrn_reflns_theta_min 2.16
_exptl_absorpt_coefficient_mu 0.430
_exptl_absorpt_correction_type none
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.846
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 1136
_exptl_crystal_size_max 0.25
_exptl_crystal_size_mid 0.25
_exptl_crystal_size_min 0.10
_refine_diff_density_max 1.376
_refine_diff_density_min -0.810
_refine_diff_density_rms 0.102
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.342
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 701
_refine_ls_number_reflns 9836
_refine_ls_number_restraints 24
_refine_ls_restrained_S_all 1.341
_refine_ls_R_factor_all 0.0737
_refine_ls_R_factor_gt 0.0575
_refine_ls_shift/su_max 1.258
_refine_ls_shift/su_mean 0.055
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1748
_refine_ls_wR_factor_ref 0.1858
_reflns_number_gt 7889
_reflns_number_total 9836
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file ic048158ysi20041230_010156.cif
_cod_data_source_block ru02
_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 1982.9(7)
_cod_database_code 1100935
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
Ti1 Ti 0.64581(4) 0.19287(3) 0.66419(3) 0.01312(13) Uani 1 1 d . . .
O1 O 0.61682(15) 0.16471(13) 0.51165(13) 0.0167(4) Uani 1 1 d . . .
O2 O 0.69536(15) 0.32515(14) 0.63458(13) 0.0168(4) Uani 1 1 d . . .
O3 O 0.63402(17) 0.23328(15) 0.37234(14) 0.0226(4) Uani 1 1 d . . .
O4 O 0.9103(2) 0.50630(19) 0.6478(2) 0.0508(8) Uani 1 1 d . . .
O5 O 0.8564(2) 0.57073(16) 0.51652(17) 0.0321(5) Uani 1 1 d . . .
O6 O 0.46190(17) 0.41610(16) 0.64284(15) 0.0259(4) Uani 1 1 d . . .
O7 O 0.42277(16) 0.31810(14) 0.49177(14) 0.0208(4) Uani 1 1 d . . .
O8 O 0.46476(15) 0.17245(13) 0.65512(13) 0.0148(4) Uani 1 1 d . . .
O9 O 0.61669(15) 0.23188(14) 0.79811(13) 0.0161(4) Uani 1 1 d . . .
O10 O 0.31277(15) 0.21222(14) 0.73794(14) 0.0184(4) Uani 1 1 d . . .
O11 O 0.39159(16) 0.00328(14) 0.79334(14) 0.0201(4) Uani 1 1 d . . .
O12 O 0.55594(18) 0.01049(15) 0.88735(15) 0.0259(4) Uani 1 1 d . . .
O13 O 0.4790(2) 0.36268(17) 1.05472(15) 0.0309(5) Uani 1 1 d . . .
O14 O 0.6571(2) 0.40940(18) 1.00478(16) 0.0338(5) Uani 1 1 d . . .
O15 O 0.60765(15) 0.03122(13) 0.64114(14) 0.0172(4) Uani 1 1 d . . .
O16 O 0.79369(15) 0.15954(13) 0.68038(13) 0.0150(4) Uani 1 1 d . . .
O17 O 0.68628(17) -0.11198(14) 0.63425(15) 0.0220(4) Uani 1 1 d . . .
O18 O 0.9240(2) 0.1936(2) 0.9073(2) 0.0335(6) Uani 0.80 1 d P A 1
O18' O 0.9774(10) 0.0708(13) 0.9150(9) 0.052(4) Uani 0.20 1 d P B 2
O19 O 1.04682(17) 0.14690(18) 0.79047(17) 0.0298(5) Uani 1 1 d . . .
O20 O 0.90643(17) 0.13674(15) 0.46379(15) 0.0228(4) Uani 1 1 d . . .
O21 O 0.77351(16) -0.00872(15) 0.43987(15) 0.0211(4) Uani 1 1 d . . .
C1 C 0.6452(2) 0.2420(2) 0.46503(19) 0.0174(5) Uani 1 1 d . . .
C2 C 0.6933(2) 0.3461(2) 0.53483(19) 0.0173(5) Uani 1 1 d . . .
C3 C 0.8173(2) 0.3859(2) 0.5043(2) 0.0214(5) Uani 1 1 d . . .
H3A H 0.8687 0.3394 0.5203 0.026 Uiso 1 1 calc R . .
H3B H 0.8150 0.3848 0.4311 0.026 Uiso 1 1 calc R . .
C4 C 0.8667(2) 0.4962(2) 0.5593(2) 0.0235(6) Uani 1 1 d . . .
C5 C 0.6117(2) 0.42426(19) 0.5259(2) 0.0167(5) Uani 1 1 d . . .
H5A H 0.6432 0.4896 0.5704 0.020 Uiso 1 1 calc R . .
H5B H 0.6078 0.4375 0.4563 0.020 Uiso 1 1 calc R . .
C6 C 0.4890(2) 0.3836(2) 0.5549(2) 0.0186(5) Uani 1 1 d . . .
C7 C 0.4175(2) 0.20788(18) 0.73524(18) 0.0140(5) Uani 1 1 d . . .
C8 C 0.5036(2) 0.23979(19) 0.82960(18) 0.0151(5) Uani 1 1 d . . .
C9 C 0.4709(2) 0.1627(2) 0.90293(19) 0.0183(5) Uani 1 1 d . . .
H9A H 0.5248 0.1828 0.9632 0.022 Uiso 1 1 calc R . .
H9B H 0.3931 0.1677 0.9245 0.022 Uiso 1 1 calc R . .
C10 C 0.4731(2) 0.0499(2) 0.85718(19) 0.0182(5) Uani 1 1 d . . .
C11 C 0.4973(2) 0.3522(2) 0.87878(19) 0.0189(5) Uani 1 1 d . . .
H11A H 0.5398 0.4002 0.8393 0.023 Uiso 1 1 calc R . .
H11B H 0.4164 0.3613 0.8769 0.023 Uiso 1 1 calc R . .
C12 C 0.5477(3) 0.3780(2) 0.9872(2) 0.0219(6) Uani 1 1 d . . .
C13 C 0.6933(2) -0.0165(2) 0.64711(19) 0.0163(5) Uani 1 1 d . . .
C14 C 0.8126(2) 0.05617(19) 0.67509(19) 0.0157(5) Uani 1 1 d . . .
C15 C 0.8567(2) 0.0405(2) 0.7795(2) 0.0235(6) Uani 1 1 d . . .
H15A H 0.8900 -0.0224 0.7724 0.028 Uiso 1 1 calc R C 1
H15B H 0.7918 0.0321 0.8229 0.028 Uiso 1 1 calc R C 1
C16 C 0.9518(3) 0.1360(4) 0.8309(3) 0.0222(7) Uani 0.80 1 d P A 1
C16' C 0.9646(13) 0.0797(14) 0.8225(10) 0.020(3) Uani 0.20 1 d P B 2
C17 C 0.8975(2) 0.0333(2) 0.59300(19) 0.0163(5) Uani 1 1 d . . .
H17A H 0.9738 0.0760 0.6140 0.020 Uiso 1 1 calc R A .
H17B H 0.9058 -0.0392 0.5860 0.020 Uiso 1 1 calc R . .
C18 C 0.8556(2) 0.05501(19) 0.49130(19) 0.0162(5) Uani 1 1 d . A .
Na1 Na 0.59341(9) 0.02602(8) 0.37963(8) 0.0187(2) Uani 1 1 d . . .
Na2 Na 0.68444(11) 0.18367(9) 0.20307(8) 0.0257(3) Uani 1 1 d . . .
O201 O 0.8648(2) 0.13845(18) 0.26630(16) 0.0321(5) Uani 1 1 d D . .
H201 H 0.885(3) 0.142(3) 0.3369(7) 0.048 Uiso 1 1 d D . .
H202 H 0.924(2) 0.190(2) 0.247(3) 0.048 Uiso 1 1 d D . .
O202 O 0.7263(2) 0.12346(19) 0.02529(17) 0.0358(5) Uani 1 1 d D . .
H203 H 0.791(2) 0.162(3) -0.002(3) 0.054 Uiso 1 1 d D . .
H204 H 0.670(3) 0.109(3) -0.031(2) 0.054 Uiso 1 1 d D . .
O203 O 0.7424(2) 0.36145(17) 0.18465(17) 0.0332(5) Uani 1 1 d D . .
H205 H 0.709(3) 0.375(3) 0.1227(17) 0.050 Uiso 1 1 d D . .
H206 H 0.727(3) 0.417(2) 0.234(2) 0.050 Uiso 1 1 d D . .
O204 O 0.4820(2) 0.19418(16) 0.17002(15) 0.0279(5) Uani 1 1 d D . .
H207 H 0.449(3) 0.1225(8) 0.150(3) 0.042 Uiso 1 1 d D . .
H208 H 0.433(3) 0.235(2) 0.143(3) 0.042 Uiso 1 1 d D . .
Na3 Na 0.42911(11) 0.26374(9) 0.32372(8) 0.0271(3) Uani 1 1 d . . .
O301 O 0.4190(2) 0.41153(18) 0.24796(17) 0.0389(6) Uani 1 1 d D . .
H301 H 0.471(3) 0.467(2) 0.289(3) 0.058 Uiso 1 1 d D . .
H302 H 0.443(4) 0.387(3) 0.1822(14) 0.058 Uiso 1 1 d D . .
O302 O 0.1827(4) 0.2678(3) 0.3180(2) 0.0669(10) Uani 1 1 d D . .
H303 H 0.179(5) 0.320(3) 0.375(3) 0.100 Uiso 1 1 d D . .
H304 H 0.1029(15) 0.269(5) 0.301(5) 0.100 Uiso 1 1 d D . .
Na4 Na 0.29758(9) 0.18417(8) 0.54334(8) 0.0186(2) Uani 1 1 d . . .
O401 O 0.11750(17) 0.23970(15) 0.55092(16) 0.0232(4) Uani 1 1 d D . .
H401 H 0.0417(14) 0.204(2) 0.525(3) 0.035 Uiso 1 1 d D . .
H402 H 0.121(3) 0.3043(13) 0.527(3) 0.035 Uiso 1 1 d D . .
Na5 Na 0.14807(9) 0.30208(8) 0.74140(8) 0.0219(2) Uani 1 1 d . . .
O501 O 0.1839(2) 0.40121(19) 0.90673(18) 0.0366(5) Uani 1 1 d D . .
H501 H 0.241(3) 0.459(2) 0.940(3) 0.055 Uiso 1 1 d D . .
H502 H 0.214(3) 0.362(3) 0.952(3) 0.055 Uiso 1 1 d D . .
O502 O -0.03771(18) 0.34410(17) 0.72872(17) 0.0300(5) Uani 1 1 d D . .
H503 H -0.090(3) 0.2812(16) 0.701(3) 0.045 Uiso 1 1 d D . .
H504 H -0.061(3) 0.394(2) 0.692(3) 0.045 Uiso 1 1 d D . .
O503 O 0.24577(17) 0.45325(16) 0.67910(15) 0.0245(4) Uani 1 1 d D . .
H505 H 0.3273(7) 0.454(3) 0.676(3) 0.037 Uiso 1 1 d D . .
H506 H 0.202(3) 0.456(3) 0.6183(15) 0.037 Uiso 1 1 d D . .
Na6 Na 0.19551(10) 0.04728(9) 0.76925(10) 0.0292(3) Uani 1 1 d . . .
O601 O 0.1887(3) 0.0550(3) 0.9487(2) 0.0627(9) Uani 1 1 d D . .
H601 H 0.227(4) 0.001(3) 0.965(4) 0.094 Uiso 1 1 d D . .
H602 H 0.117(3) 0.050(4) 0.982(4) 0.094 Uiso 1 1 d D . .
Na7 Na 0.82373(15) 0.36216(15) 0.88873(14) 0.0288(4) Uani 0.65 1 d P D 1
Na7' Na 0.7881(4) 0.4489(4) 0.8500(4) 0.0518(11) Uani 0.35 1 d P E 2
O70A O 0.9652(3) 0.3858(3) 0.8987(2) 0.0277(7) Uani 0.65 1 d P F 1
O70B O 1.0138(5) 0.5151(5) 0.9428(5) 0.0307(13) Uani 0.35 1 d P . 2
O702 O 0.7739(4) 0.5225(5) 0.8013(4) 0.1088(15) Uani 1 1 d . . .
O703 O 0.945(3) 0.297(3) 1.011(3) 0.77(2) Uiso 1 1 d . . .
Na8 Na 0.8650(2) 0.7031(2) 0.8353(2) 0.0411(6) Uani 0.50 1 d P G 1
Na8' Na 0.8072(3) 0.6172(3) 0.7965(2) 0.0526(8) Uani 0.50 1 d P H 2
O801 O 1.0324(3) 0.6531(3) 0.7881(3) 0.0858(12) Uani 1 1 d . . .
O802 O 0.9720(5) 0.8570(4) 0.9273(4) 0.1235(18) Uani 1 1 d . . .
O803 O 0.7523(3) 0.7185(3) 0.9581(2) 0.0548(7) Uani 1 1 d D . .
H805 H 0.770(5) 0.7907(9) 0.954(4) 0.082 Uiso 1 1 d D . .
H806 H 0.6729(14) 0.702(4) 0.974(4) 0.082 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
Ti1 0.0124(2) 0.0126(2) 0.0143(2) 0.00173(16) 0.00027(15) 0.00268(16)
O1 0.0203(9) 0.0140(8) 0.0152(8) 0.0014(7) 0.0010(7) 0.0025(7)
O2 0.0181(9) 0.0159(9) 0.0158(8) 0.0032(7) 0.0007(6) 0.0013(7)
O3 0.0284(10) 0.0240(10) 0.0157(9) 0.0031(8) 0.0032(7) 0.0054(8)
O4 0.0637(17) 0.0295(13) 0.0499(16) 0.0162(11) -0.0356(13) -0.0177(12)
O5 0.0422(13) 0.0207(10) 0.0331(12) 0.0099(9) -0.0031(9) 0.0014(9)
O6 0.0264(10) 0.0309(11) 0.0206(10) 0.0010(8) 0.0062(8) 0.0080(8)
O7 0.0216(9) 0.0184(9) 0.0209(9) 0.0027(7) 0.0000(7) 0.0001(7)
O8 0.0147(8) 0.0177(9) 0.0122(8) 0.0007(7) 0.0013(6) 0.0047(7)
O9 0.0160(9) 0.0198(9) 0.0127(8) 0.0015(7) 0.0011(6) 0.0049(7)
O10 0.0152(9) 0.0204(9) 0.0207(9) 0.0022(7) 0.0034(7) 0.0070(7)
O11 0.0243(10) 0.0187(9) 0.0163(9) 0.0014(7) -0.0002(7) 0.0029(7)
O12 0.0292(11) 0.0194(10) 0.0287(11) 0.0010(8) -0.0082(8) 0.0080(8)
O13 0.0441(13) 0.0319(11) 0.0163(10) 0.0011(8) 0.0062(9) 0.0079(10)
O14 0.0369(12) 0.0330(12) 0.0250(11) -0.0002(9) -0.0073(9) -0.0053(10)
O15 0.0135(8) 0.0129(8) 0.0245(9) 0.0029(7) 0.0006(7) 0.0012(7)
O16 0.0139(8) 0.0123(8) 0.0187(9) 0.0012(7) 0.0001(6) 0.0037(7)
O17 0.0238(10) 0.0142(9) 0.0285(10) 0.0050(8) 0.0049(8) 0.0028(7)
O18 0.0314(15) 0.0386(16) 0.0270(14) -0.0035(12) 0.0017(11) 0.0050(12)
O18' 0.025(6) 0.103(12) 0.021(6) 0.017(6) -0.001(4) -0.010(7)
O19 0.0178(10) 0.0396(12) 0.0351(11) 0.0167(10) 0.0003(8) 0.0044(9)
O20 0.0226(10) 0.0217(10) 0.0216(9) 0.0058(8) -0.0038(7) -0.0038(8)
O21 0.0186(9) 0.0173(9) 0.0266(10) 0.0042(8) -0.0041(7) 0.0019(7)
C1 0.0173(12) 0.0181(12) 0.0174(12) 0.0031(10) 0.0015(9) 0.0051(10)
C2 0.0195(12) 0.0152(12) 0.0175(12) 0.0059(10) 0.0009(9) 0.0017(10)
C3 0.0190(13) 0.0212(13) 0.0260(14) 0.0066(11) 0.0060(10) 0.0053(10)
C4 0.0189(13) 0.0225(14) 0.0293(14) 0.0089(11) 0.0026(11) -0.0002(11)
C5 0.0174(12) 0.0148(12) 0.0185(12) 0.0044(10) 0.0019(9) 0.0027(9)
C6 0.0212(13) 0.0168(12) 0.0212(13) 0.0064(10) 0.0023(10) 0.0094(10)
C7 0.0158(11) 0.0114(11) 0.0152(11) 0.0024(9) 0.0008(9) 0.0034(9)
C8 0.0152(11) 0.0163(12) 0.0137(11) 0.0008(9) 0.0020(9) 0.0041(9)
C9 0.0232(13) 0.0181(12) 0.0135(11) 0.0032(9) 0.0024(9) 0.0027(10)
C10 0.0220(13) 0.0176(12) 0.0152(11) 0.0035(9) 0.0037(9) 0.0031(10)
C11 0.0252(13) 0.0156(12) 0.0162(12) 0.0020(10) 0.0006(10) 0.0057(10)
C12 0.0358(16) 0.0125(12) 0.0165(12) -0.0019(10) -0.0002(11) 0.0065(11)
C13 0.0166(12) 0.0184(12) 0.0158(12) 0.0047(10) 0.0053(9) 0.0053(10)
C14 0.0148(11) 0.0145(11) 0.0198(12) 0.0059(9) 0.0014(9) 0.0054(9)
C15 0.0211(13) 0.0302(15) 0.0220(13) 0.0108(11) 0.0045(10) 0.0058(11)
C16 0.0196(17) 0.027(2) 0.0205(18) 0.0048(17) -0.0039(13) 0.0057(16)
C16' 0.023(7) 0.025(8) 0.011(6) 0.001(6) -0.002(5) 0.003(6)
C17 0.0131(11) 0.0171(12) 0.0206(12) 0.0065(10) 0.0028(9) 0.0047(9)
C18 0.0140(11) 0.0160(12) 0.0194(12) 0.0032(10) 0.0029(9) 0.0041(9)
Na1 0.0165(5) 0.0194(5) 0.0180(5) -0.0025(4) -0.0009(4) 0.0029(4)
Na2 0.0340(6) 0.0215(6) 0.0214(6) 0.0047(4) 0.0003(5) 0.0044(5)
O201 0.0323(12) 0.0383(13) 0.0247(11) 0.0092(10) -0.0004(9) 0.0006(10)
O202 0.0359(13) 0.0412(13) 0.0254(11) 0.0029(10) -0.0050(9) -0.0024(10)
O203 0.0503(14) 0.0241(11) 0.0234(11) 0.0044(9) -0.0080(9) 0.0037(10)
O204 0.0449(13) 0.0201(10) 0.0198(10) 0.0031(8) -0.0009(9) 0.0101(9)
Na3 0.0396(7) 0.0227(6) 0.0174(5) 0.0048(4) 0.0027(5) 0.0001(5)
O301 0.0698(17) 0.0258(12) 0.0214(11) 0.0000(9) 0.0055(11) 0.0135(11)
O302 0.127(3) 0.0534(18) 0.0379(16) 0.0209(14) 0.0224(18) 0.048(2)
Na4 0.0188(5) 0.0192(5) 0.0173(5) 0.0037(4) -0.0011(4) 0.0019(4)
O401 0.0204(10) 0.0187(9) 0.0298(11) 0.0053(8) -0.0033(8) 0.0017(8)
Na5 0.0197(5) 0.0206(5) 0.0255(6) 0.0029(4) -0.0001(4) 0.0054(4)
O501 0.0448(14) 0.0330(13) 0.0303(12) 0.0022(10) 0.0040(10) 0.0052(10)
O502 0.0241(10) 0.0255(11) 0.0390(12) 0.0030(9) -0.0099(9) 0.0054(8)
O503 0.0233(10) 0.0266(10) 0.0218(10) 0.0027(8) 0.0017(8) 0.0012(8)
Na6 0.0284(6) 0.0248(6) 0.0368(7) 0.0063(5) 0.0032(5) 0.0099(5)
O601 0.0619(19) 0.096(2) 0.0492(17) 0.0270(17) 0.0162(14) 0.0504(18)
Na7 0.0213(8) 0.0359(10) 0.0262(9) -0.0004(8) 0.0070(7) 0.0015(7)
Na7' 0.049(3) 0.056(3) 0.048(3) 0.006(2) 0.003(2) 0.007(2)
O70A 0.0221(15) 0.046(2) 0.0139(14) -0.0055(13) 0.0005(11) 0.0136(14)
O70B 0.030(3) 0.037(3) 0.027(3) -0.002(3) -0.003(2) 0.016(3)
O702 0.101(3) 0.139(5) 0.095(3) 0.022(3) 0.025(3) 0.041(3)
Na8 0.0367(15) 0.0514(18) 0.0377(15) 0.0126(13) 0.0048(11) 0.0102(13)
Na8' 0.086(3) 0.0424(18) 0.0370(16) 0.0139(14) 0.0183(16) 0.0221(18)
O801 0.055(2) 0.107(3) 0.086(3) 0.002(2) -0.0044(18) 0.007(2)
O802 0.142(5) 0.133(4) 0.099(4) 0.018(3) -0.012(3) 0.040(4)
O803 0.0436(16) 0.0642(19) 0.0577(17) 0.0193(15) -0.0061(13) 0.0071(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'
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'
Ti Ti 0.2776 0.4457 '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 Ti1 O2 97.71(9) . . ?
O9 Ti1 O16 100.35(8) . . ?
O2 Ti1 O16 96.78(8) . . ?
O9 Ti1 O1 157.88(8) . . ?
O2 Ti1 O1 79.49(8) . . ?
O16 Ti1 O1 101.77(8) . . ?
O9 Ti1 O8 78.43(8) . . ?
O2 Ti1 O8 104.89(8) . . ?
O16 Ti1 O8 158.28(8) . . ?
O1 Ti1 O8 81.11(8) . . ?
O9 Ti1 O15 103.96(8) . . ?
O2 Ti1 O15 158.29(8) . . ?
O16 Ti1 O15 78.20(8) . . ?
O1 Ti1 O15 80.90(8) . . ?
O8 Ti1 O15 81.06(8) . . ?
C1 O1 Ti1 116.83(16) . . ?
C2 O2 Ti1 122.49(16) . . ?
C7 O8 Ti1 116.66(15) . . ?
C8 O9 Ti1 122.71(15) . . ?
C13 O15 Ti1 117.21(16) . . ?
C14 O16 Ti1 123.07(15) . . ?
C16 O18 O703 156.2(12) . . ?
C16 O19 C16' 35.0(7) . . ?
O3 C1 O1 122.4(2) . . ?
O3 C1 C2 122.7(2) . . ?
O1 C1 C2 114.9(2) . . ?
O2 C2 C1 106.3(2) . . ?
O2 C2 C5 108.8(2) . . ?
C1 C2 C5 110.3(2) . . ?
O2 C2 C3 111.4(2) . . ?
C1 C2 C3 108.0(2) . . ?
C5 C2 C3 111.8(2) . . ?
C4 C3 C2 112.2(2) . . ?
O5 C4 O4 123.3(3) . . ?
O5 C4 C3 119.2(3) . . ?
O4 C4 C3 117.4(3) . . ?
C6 C5 C2 111.5(2) . . ?
O7 C6 O6 123.5(3) . . ?
O7 C6 C5 118.6(2) . . ?
O6 C6 C5 117.8(2) . . ?
O10 C7 O8 123.9(2) . . ?
O10 C7 C8 123.1(2) . . ?
O8 C7 C8 112.9(2) . . ?
O9 C8 C7 108.16(19) . . ?
O9 C8 C9 108.4(2) . . ?
C7 C8 C9 108.3(2) . . ?
O9 C8 C11 111.2(2) . . ?
C7 C8 C11 108.7(2) . . ?
C9 C8 C11 111.9(2) . . ?
C10 C9 C8 114.0(2) . . ?
O11 C10 O12 125.0(2) . . ?
O11 C10 C9 117.7(2) . . ?
O12 C10 C9 117.3(2) . . ?
C12 C11 C8 112.1(2) . . ?
O13 C12 O14 123.9(3) . . ?
O13 C12 C11 117.0(3) . . ?
O14 C12 C11 119.0(3) . . ?
O17 C13 O15 125.5(2) . . ?
O17 C13 C14 120.4(2) . . ?
O15 C13 C14 114.0(2) . . ?
O16 C14 C15 109.6(2) . . ?
O16 C14 C17 109.5(2) . . ?
C15 C14 C17 112.3(2) . . ?
O16 C14 C13 107.35(19) . . ?
C15 C14 C13 107.7(2) . . ?
C17 C14 C13 110.2(2) . . ?
C16' C15 C14 124.5(7) . . ?
C16' C15 C16 29.5(7) . . ?
C14 C15 C16 110.9(2) . . ?
O19 C16 O18 126.9(4) . . ?
O19 C16 C15 116.0(3) . . ?
O18 C16 C15 117.0(3) . . ?
O18' C16' O19 115.5(12) . . ?
O18' C16' C15 114.0(12) . . ?
O19 C16' C15 128.2(11) . . ?
C18 C17 C14 111.6(2) . . ?
O20 C18 O21 124.4(2) . . ?
O20 C18 C17 116.9(2) . . ?
O21 C18 C17 118.7(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
Ti1 O9 1.8330(18) . ?
Ti1 O2 1.8542(18) . ?
Ti1 O16 1.8613(18) . ?
Ti1 O1 2.0058(18) . ?
Ti1 O8 2.0730(18) . ?
Ti1 O15 2.0762(18) . ?
O1 C1 1.281(3) . ?
O2 C2 1.397(3) . ?
O3 C1 1.218(3) . ?
O4 C4 1.240(4) . ?
O5 C4 1.235(3) . ?
O6 C6 1.250(3) . ?
O7 C6 1.238(3) . ?
O8 C7 1.276(3) . ?
O9 C8 1.412(3) . ?
O10 C7 1.231(3) . ?
O11 C10 1.252(3) . ?
O12 C10 1.254(3) . ?
O13 C12 1.241(4) . ?
O14 C12 1.269(4) . ?
O15 C13 1.275(3) . ?
O16 C14 1.413(3) . ?
O17 C13 1.234(3) . ?
O18 C16 1.256(5) . ?
O18 O703 1.75(3) . ?
O18' C16' 1.260(18) . ?
O19 C16 1.244(4) . ?
O19 C16' 1.321(15) . ?
O20 C18 1.255(3) . ?
O21 C18 1.256(3) . ?
C1 C2 1.533(4) . ?
C2 C5 1.535(4) . ?
C2 C3 1.540(4) . ?
C3 C4 1.526(4) . ?
C5 C6 1.523(4) . ?
C7 C8 1.530(3) . ?
C8 C9 1.532(3) . ?
C8 C11 1.539(3) . ?
C9 C10 1.522(4) . ?
C11 C12 1.498(4) . ?
C13 C14 1.540(4) . ?
C14 C15 1.519(4) . ?
C14 C17 1.529(3) . ?
C15 C16' 1.339(14) . ?
C15 C16 1.570(5) . ?
C17 C18 1.507(3) . ?
O70B O70B 1.664(13) 2_767 ?
|
1100936.cif | #------------------------------------------------------------------------------
#$Date: 2021-10-24 01:03:07 +0300 (Sun, 24 Oct 2021) $
#$Revision: 270073 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/09/1100936.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_1100936
loop_
_publ_author_name
'Becker, Gerd'
'Brombach, Heike'
'Horner, Stephen T.'
'Niecke, Edgar'
'Schwarz, Wolfgang'
'Streubel, Rainer'
'W\"urthwein, Ernst-Ulrich'
_publ_contact_author
;
Gerd Becker
Institut fuer Anorganische Chemie
Universitaet Stuttgart
70569 Stuttgart
Germany
;
_publ_contact_author_email becker@iac.uni-stuttgart.de
_publ_contact_author_fax '(+49 711) 685 4241'
_publ_contact_author_phone '(+49 711) 685 4221'
_publ_section_title
;
Synthesis and Structure of K^+^[^i^PrN\\db C\\db P]^-^,
a 1-Aza-3\l^3^-phospha-3-allenide
;
_journal_coden_ASTM INOCAJ
_journal_issue 9
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3080
_journal_page_last 3086
_journal_paper_doi 10.1021/ic048162+
_journal_volume 44
_journal_year 2005
_chemical_formula_sum 'C7 H16 N P Si'
_chemical_formula_weight 173.27
_space_group_IT_number 11
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2yb'
_symmetry_space_group_name_H-M 'P 1 21/m 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 112.21(2)
_cell_angle_gamma 90.00
_cell_formula_units_Z 2
_cell_length_a 7.285(3)
_cell_length_b 10.067(4)
_cell_length_c 8.103(2)
_cell_measurement_reflns_used 45
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 18
_cell_measurement_theta_min 14
_cell_volume 550.2(3)
_diffrn_ambient_temperature 173(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type 'Siemens P4'
_diffrn_measurement_method Wyckoff-Scan
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'normal-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0263
_diffrn_reflns_av_sigmaI/netI 0.0210
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -1
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 10
_diffrn_reflns_limit_l_min -11
_diffrn_reflns_number 3887
_diffrn_reflns_theta_full 25.00
_diffrn_reflns_theta_max 30.02
_diffrn_reflns_theta_min 2.72
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count 98
_diffrn_standards_interval_time ?
_diffrn_standards_number 2
_exptl_absorpt_coefficient_mu 0.302
_exptl_absorpt_correction_T_max 0.860
_exptl_absorpt_correction_T_min 0.765
_exptl_absorpt_correction_type psi-scan
_exptl_absorpt_process_details '(North et al., 1968)'
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.046
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description cylinder
_exptl_crystal_F_000 188
_exptl_crystal_size_max 0.4
_exptl_crystal_size_mid 0.4
_exptl_crystal_size_min 0.4
_exptl_crystal_size_rad 0.15
_refine_diff_density_max 0.412
_refine_diff_density_min -0.212
_refine_diff_density_rms 0.044
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.080
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 89
_refine_ls_number_reflns 1689
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.080
_refine_ls_R_factor_all 0.0327
_refine_ls_R_factor_gt 0.0296
_refine_ls_shift/su_max 0.061
_refine_ls_shift/su_mean 0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0557P)^2^+0.0442P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0858
_refine_ls_wR_factor_ref 0.0889
_reflns_number_gt 1555
_reflns_number_total 1689
_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.
'_exptl_absorpt_correction_type' value 'PSI-SCAN' changed to
'psi-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 P21/m
_cod_database_code 1100936
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'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
P P 0.19698(5) 0.2500 -0.20981(5) 0.03990(13) Uani 1 2 d S . .
C C 0.39322(18) 0.2500 -0.04174(15) 0.0280(2) Uani 1 2 d S . .
N N 0.56125(15) 0.2500 0.09777(13) 0.0294(2) Uani 1 2 d S . .
C1 C 0.74870(18) 0.2500 0.06212(17) 0.0328(3) Uani 1 2 d S . .
H1A H 0.848(3) 0.2500 0.180(2) 0.034(4) Uiso 1 2 d S . .
Si Si 0.57488(5) 0.2500 0.32101(4) 0.02920(12) Uani 1 2 d S . .
C11 C 0.7631(2) 0.12446(12) -0.0360(2) 0.0488(3) Uani 1 1 d . . .
H11A H 0.886(2) 0.1252(17) -0.0507(19) 0.056(4) Uiso 1 1 d . . .
H11B H 0.657(3) 0.1207(18) -0.144(2) 0.062(5) Uiso 1 1 d . . .
H11C H 0.754(3) 0.0456(19) 0.029(2) 0.070(5) Uiso 1 1 d . . .
C21 C 0.3173(2) 0.2500 0.3126(2) 0.0466(4) Uani 1 2 d S . .
H21A H 0.247(2) 0.329(2) 0.256(2) 0.078(6) Uiso 1 1 d . . .
H21B H 0.310(4) 0.2500 0.424(4) 0.072(8) Uiso 1 2 d S . .
C22 C 0.71175(19) 0.09784(11) 0.43133(14) 0.0430(2) Uani 1 1 d . . .
H22A H 0.842(3) 0.099(2) 0.432(2) 0.064(5) Uiso 1 1 d . . .
H22B H 0.645(2) 0.0191(19) 0.376(2) 0.068(5) Uiso 1 1 d . . .
H22C H 0.722(2) 0.096(2) 0.552(2) 0.068(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
P 0.03051(19) 0.0522(2) 0.02985(19) 0.000 0.00327(14) 0.000
C 0.0288(5) 0.0303(5) 0.0258(5) 0.000 0.0113(4) 0.000
N 0.0249(4) 0.0397(5) 0.0239(4) 0.000 0.0098(4) 0.000
C1 0.0257(5) 0.0425(7) 0.0324(6) 0.000 0.0133(5) 0.000
Si 0.03068(19) 0.03395(19) 0.02281(17) 0.000 0.00993(13) 0.000
C11 0.0492(6) 0.0433(5) 0.0667(8) -0.0030(5) 0.0364(6) 0.0057(5)
C21 0.0394(7) 0.0668(11) 0.0411(8) 0.000 0.0239(6) 0.000
C22 0.0517(6) 0.0379(5) 0.0335(5) 0.0055(4) 0.0094(4) 0.0023(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'
Si Si 0.0817 0.0704 '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'
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 C P 178.68(10) . . ?
C N C1 117.00(10) . . ?
C N Si 123.48(9) . . ?
C1 N Si 119.52(8) . . ?
N C1 C11 110.47(7) . . ?
N C1 C11 110.47(7) . 4_565 ?
C11 C1 C11 112.73(13) . 4_565 ?
N C1 H1A 102.1(11) . . ?
C11 C1 H1A 110.3(5) . . ?
C11 C1 H1A 110.3(5) 4_565 . ?
N Si C21 107.29(7) . . ?
N Si C22 107.64(4) . 4_565 ?
C21 Si C22 111.65(5) . 4_565 ?
N Si C22 107.64(4) . . ?
C21 Si C22 111.65(5) . . ?
C22 Si C22 110.73(8) 4_565 . ?
C1 C11 H11A 108.4(10) . . ?
C1 C11 H11B 109.3(11) . . ?
H11A C11 H11B 112.1(14) . . ?
C1 C11 H11C 111.3(10) . . ?
H11A C11 H11C 109.8(15) . . ?
H11B C11 H11C 106.0(16) . . ?
Si C21 H21A 111.3(11) . . ?
Si C21 H21B 113.3(16) . . ?
H21A C21 H21B 104.4(13) . . ?
Si C22 H22A 110.5(12) . . ?
Si C22 H22B 112.0(10) . . ?
H22A C22 H22B 110.4(16) . . ?
Si C22 H22C 109.4(11) . . ?
H22A C22 H22C 107.5(14) . . ?
H22B C22 H22C 106.9(16) . . ?
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
P C 1.5578(14) . ?
C N 1.3154(15) . ?
N C1 1.4988(16) . ?
N Si 1.7738(11) . ?
C1 C11 1.5180(14) . ?
C1 C11 1.5180(14) 4_565 ?
C1 H1A 0.956(18) . ?
Si C21 1.8521(17) . ?
Si C22 1.8617(12) 4_565 ?
Si C22 1.8617(12) . ?
C11 H11A 0.947(16) . ?
C11 H11B 0.926(17) . ?
C11 H11C 0.970(18) . ?
C21 H21A 0.96(2) . ?
C21 H21B 0.92(3) . ?
C22 H22A 0.945(17) . ?
C22 H22B 0.949(19) . ?
C22 H22C 0.956(17) . ?
loop_
_cod_changelog_entry_id
_cod_changelog_entry_author
_cod_changelog_entry_date
_cod_changelog_entry_text
1 'Vaitkus, Antanas' 2021-10-24T01:00:00+03:00
'Updated bibliographic information.'
|
1100937.cif | #------------------------------------------------------------------------------
#$Date: 2022-09-14 17:31:13 +0300 (Wed, 14 Sep 2022) $
#$Revision: 277831 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/09/1100937.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.
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data_1100937
loop_
_publ_author_name
'Becker, Gerd'
'Brombach, Heike'
'Horner, Stephen T.'
'Niecke, Edgar'
'Schwarz, Wolfgang'
'Streubel, Rainer'
'W\"urthwein, Ernst-Ulrich'
_publ_contact_author
;
Gerd Becker
Institut fuer Anorganische Chemie
Universitaet Stuttgart
70569 Stuttgart
Germany
;
_publ_contact_author_email becker@iac.uni-stuttgart.de
_publ_contact_author_fax '(+49 711) 685 4241'
_publ_contact_author_phone '(+49 711) 685 4221'
_publ_section_title
;
Synthesis and Structure of K^+^[^i^PrN\\db C\\db P]^-^,
a 1-Aza-3\l^3^-phospha-3-allenide
;
_journal_coden_ASTM INOCAJ
_journal_issue 9
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3080
_journal_page_last 3086
_journal_paper_doi 10.1021/ic048162+
_journal_volume 44
_journal_year 2005
_chemical_formula_moiety 'C16 H31 K N O6 P'
_chemical_formula_sum 'C16 H31 K N O6 P'
_chemical_formula_weight 403.48
_chemical_melting_point ?
_space_group_IT_number 31
_space_group_name_Hall 'P 2ac -2'
_space_group_name_H-M_alt 'P m n 21'
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall 'P 2ac -2'
_symmetry_space_group_name_H-M 'P m n 21'
_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 90.00
_cell_formula_units_Z 2
_cell_length_a 14.3655(19)
_cell_length_b 8.8715(12)
_cell_length_c 8.4647(16)
_cell_measurement_reflns_used ?
_cell_measurement_temperature 173(2)
_cell_measurement_theta_max ?
_cell_measurement_theta_min ?
_cell_volume 1078.8(3)
_diffrn_ambient_temperature 173(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type 'Siemens P4'
_diffrn_measurement_method ?
_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 0.0420
_diffrn_reflns_av_sigmaI/netI 0.0439
_diffrn_reflns_limit_h_max 20
_diffrn_reflns_limit_h_min -20
_diffrn_reflns_limit_k_max 2
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_l_max 11
_diffrn_reflns_limit_l_min -11
_diffrn_reflns_number 4133
_diffrn_reflns_theta_full 25.00
_diffrn_reflns_theta_max 29.99
_diffrn_reflns_theta_min 2.30
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 0.348
_exptl_absorpt_correction_T_max ?
_exptl_absorpt_correction_T_min ?
_exptl_absorpt_correction_type none
_exptl_absorpt_process_details ?
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.242
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description tablet
_exptl_crystal_F_000 432
_exptl_crystal_size_max 0.4
_exptl_crystal_size_mid 0.4
_exptl_crystal_size_min 0.4
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
_refine_diff_density_max 0.418
_refine_diff_density_min -0.342
_refine_diff_density_rms 0.048
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack 0.04(6)
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.984
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 124
_refine_ls_number_reflns 2027
_refine_ls_number_restraints 1
_refine_ls_restrained_S_all 0.984
_refine_ls_R_factor_all 0.0533
_refine_ls_R_factor_gt 0.0369
_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^)+(0.0551P)^2^+0.0559P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0904
_refine_ls_wR_factor_ref 0.0994
_reflns_number_gt 1625
_reflns_number_total 2027
_reflns_threshold_expression >2sigma(I)
_cod_database_code 1100937
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -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
K K 0.0000 0.88567(7) 0.43691(9) 0.03461(17) Uani 1 2 d S . .
O1 O 0.0000 0.5612(3) 0.4578(4) 0.0409(6) Uani 1 2 d S . .
C11 C 0.0822(2) 0.5203(3) 0.5436(4) 0.0482(7) Uani 1 1 d . . .
H11A H 0.0830 0.4100 0.5616 0.058 Uiso 1 1 calc R . .
H11B H 0.0824 0.5710 0.6478 0.058 Uiso 1 1 calc R . .
C12 C 0.16631(17) 0.5658(3) 0.4521(5) 0.0471(7) Uani 1 1 d . . .
H12A H 0.2231 0.5263 0.5038 0.056 Uiso 1 1 calc R . .
H12B H 0.1631 0.5240 0.3438 0.056 Uiso 1 1 calc R . .
O2 O 0.16947(11) 0.72595(18) 0.4461(3) 0.0421(4) Uani 1 1 d . . .
C21 C 0.24732(19) 0.7792(3) 0.3592(4) 0.0445(7) Uani 1 1 d . . .
H21A H 0.2423 0.7475 0.2474 0.053 Uiso 1 1 calc R . .
H21B H 0.3055 0.7370 0.4035 0.053 Uiso 1 1 calc R . .
C22 C 0.24868(18) 0.9488(3) 0.3702(4) 0.0455(7) Uani 1 1 d . . .
H22A H 0.2488 0.9807 0.4823 0.055 Uiso 1 1 calc R . .
H22B H 0.3054 0.9891 0.3189 0.055 Uiso 1 1 calc R . .
O3 O 0.16736(12) 1.00496(18) 0.2923(2) 0.0371(4) Uani 1 1 d . . .
C31 C 0.16528(17) 1.1651(3) 0.2921(4) 0.0413(6) Uani 1 1 d . . .
H31A H 0.2226 1.2052 0.2427 0.050 Uiso 1 1 calc R . .
H31B H 0.1617 1.2033 0.4018 0.050 Uiso 1 1 calc R . .
C32 C 0.08152(18) 1.2152(3) 0.2004(4) 0.0393(6) Uani 1 1 d . . .
H32A H 0.0826 1.3260 0.1873 0.047 Uiso 1 1 calc R . .
H32B H 0.0820 1.1685 0.0942 0.047 Uiso 1 1 calc R . .
O4 O 0.0000 1.1714(3) 0.2833(3) 0.0347(5) Uani 1 2 d S . .
P P 0.0000 1.14012(11) 0.73791(13) 0.0425(2) Uani 1 2 d S . .
C C 0.0000 0.9656(4) 0.7863(4) 0.0351(7) Uani 1 2 d S . .
N N 0.0000 0.8270(4) 0.8107(5) 0.0685(13) Uani 1 2 d S . .
C1 C 0.0000 0.7700(5) 0.9772(6) 0.0763(17) Uani 1 2 d S . .
H1A H 0.0000 0.8597 1.0487 0.092 Uiso 1 2 calc SR . .
C2 C 0.0842(3) 0.6863(7) 1.0079(7) 0.131(2) Uani 1 1 d . . .
H2A H 0.0836 0.6495 1.1170 0.196 Uiso 1 1 calc R . .
H2B H 0.1383 0.7521 0.9922 0.196 Uiso 1 1 calc R . .
H2C H 0.0880 0.6005 0.9352 0.196 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
K 0.0350(3) 0.0285(3) 0.0404(4) -0.0018(4) 0.000 0.000
O1 0.0500(13) 0.0309(10) 0.0418(15) 0.0075(12) 0.000 0.000
C11 0.0629(16) 0.0340(12) 0.0478(16) 0.0058(12) -0.0053(14) 0.0097(12)
C12 0.0504(14) 0.0336(10) 0.0572(17) 0.0021(14) -0.0087(15) 0.0109(10)
O2 0.0409(8) 0.0317(7) 0.0537(11) -0.0039(10) -0.0036(11) 0.0032(6)
C21 0.0312(11) 0.0442(12) 0.0582(19) -0.0086(14) -0.0097(11) 0.0043(11)
C22 0.0335(11) 0.0433(12) 0.0597(19) -0.0071(13) -0.0108(13) -0.0034(11)
O3 0.0328(8) 0.0322(8) 0.0464(10) -0.0045(8) -0.0066(7) -0.0030(6)
C31 0.0404(12) 0.0330(10) 0.0505(15) -0.0014(13) -0.0046(12) -0.0104(10)
C32 0.0399(13) 0.0355(12) 0.0426(14) 0.0054(11) 0.0019(11) -0.0108(10)
O4 0.0363(12) 0.0358(11) 0.0321(13) 0.0043(11) 0.000 0.000
P 0.0504(6) 0.0371(4) 0.0400(5) 0.0058(5) 0.000 0.000
C 0.0382(17) 0.0423(17) 0.0249(15) 0.0037(15) 0.000 0.000
N 0.134(4) 0.0357(16) 0.0357(19) 0.0067(17) 0.000 0.000
C1 0.146(5) 0.041(2) 0.043(3) 0.010(2) 0.000 0.000
C2 0.064(2) 0.226(6) 0.101(4) 0.097(5) -0.028(3) -0.025(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'
K K 0.2009 0.2494 '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 K O2 119.53(7) 4 . ?
O2 K O4 117.38(4) 4 . ?
O2 K O4 117.38(4) . . ?
O2 K O1 59.76(4) 4 . ?
O2 K O1 59.76(4) . . ?
O4 K O1 156.35(9) . . ?
O2 K O3 58.57(5) 4 4 ?
O2 K O3 155.78(7) . 4 ?
O4 K O3 58.82(4) . 4 ?
O1 K O3 112.98(4) . 4 ?
O2 K O3 155.78(7) 4 . ?
O2 K O3 58.57(5) . . ?
O4 K O3 58.82(4) . . ?
O1 K O3 112.98(4) . . ?
O3 K O3 112.11(8) 4 . ?
O2 K C 95.18(6) 4 . ?
O2 K C 95.18(6) . . ?
O4 K C 103.69(9) . . ?
O1 K C 99.96(9) . . ?
O3 K C 109.01(5) 4 . ?
O3 K C 109.01(5) . . ?
O2 K N 83.75(6) 4 . ?
O2 K N 83.75(6) . . ?
O4 K N 126.51(9) . . ?
O1 K N 77.14(9) . . ?
O3 K N 118.43(5) 4 . ?
O3 K N 118.43(5) . . ?
C K N 22.82(10) . . ?
O2 K P 108.23(5) 4 . ?
O2 K P 108.23(5) . . ?
O4 K P 75.62(6) . . ?
O1 K P 128.02(7) . . ?
O3 K P 94.25(4) 4 . ?
O3 K P 94.25(4) . . ?
C K P 28.06(7) . . ?
N K P 50.88(7) . . ?
C11 O1 C11 111.0(3) . 4 ?
C11 O1 K 106.50(15) . . ?
C11 O1 K 106.50(15) 4 . ?
O1 C11 C12 109.6(3) . . ?
O1 C11 H11A 109.7 . . ?
C12 C11 H11A 109.7 . . ?
O1 C11 H11B 109.7 . . ?
C12 C11 H11B 109.7 . . ?
H11A C11 H11B 108.2 . . ?
O2 C12 C11 108.4(2) . . ?
O2 C12 H12A 110.0 . . ?
C11 C12 H12A 110.0 . . ?
O2 C12 H12B 110.0 . . ?
C11 C12 H12B 110.0 . . ?
H12A C12 H12B 108.4 . . ?
C21 O2 C12 112.1(2) . . ?
C21 O2 K 119.93(14) . . ?
C12 O2 K 118.40(13) . . ?
O2 C21 C22 108.1(2) . . ?
O2 C21 H21A 110.1 . . ?
C22 C21 H21A 110.1 . . ?
O2 C21 H21B 110.1 . . ?
C22 C21 H21B 110.1 . . ?
H21A C21 H21B 108.4 . . ?
O3 C22 C21 108.0(2) . . ?
O3 C22 H22A 110.1 . . ?
C21 C22 H22A 110.1 . . ?
O3 C22 H22B 110.1 . . ?
C21 C22 H22B 110.1 . . ?
H22A C22 H22B 108.4 . . ?
C31 O3 C22 111.44(19) . . ?
C31 O3 K 110.37(15) . . ?
C22 O3 K 110.82(16) . . ?
O3 C31 C32 108.3(2) . . ?
O3 C31 H31A 110.0 . . ?
C32 C31 H31A 110.0 . . ?
O3 C31 H31B 110.0 . . ?
C32 C31 H31B 110.0 . . ?
H31A C31 H31B 108.4 . . ?
O4 C32 C31 109.0(2) . . ?
O4 C32 H32A 109.9 . . ?
C31 C32 H32A 109.9 . . ?
O4 C32 H32B 109.9 . . ?
C31 C32 H32B 109.9 . . ?
H32A C32 H32B 108.3 . . ?
C32 O4 C32 111.2(3) 4 . ?
C32 O4 K 117.99(14) 4 . ?
C32 O4 K 117.99(14) . . ?
C P K 63.27(13) . . ?
N C P 174.7(4) . . ?
N C K 86.1(3) . . ?
P C K 88.66(14) . . ?
C N C1 119.3(4) . . ?
C N K 71.1(2) . . ?
C1 N K 169.6(3) . . ?
C2 C1 C2 114.0(5) 4 . ?
C2 C1 N 110.1(3) 4 . ?
C2 C1 N 110.1(3) . . ?
C2 C1 H1A 107.5 4 . ?
C2 C1 H1A 107.5 . . ?
N C1 H1A 107.5 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 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
K O2 2.8179(16) 4 ?
K O2 2.8179(16) . ?
K O4 2.849(3) . ?
K O1 2.884(2) . ?
K O3 2.8981(19) 4 ?
K O3 2.8981(19) . ?
K C 3.041(4) . ?
K N 3.207(4) . ?
K P 3.4040(14) . ?
O1 C11 1.434(3) . ?
O1 C11 1.434(3) 4 ?
C11 C12 1.491(5) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 O2 1.423(3) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
O2 C21 1.419(4) . ?
C21 C22 1.508(4) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 O3 1.431(3) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
O3 C31 1.421(3) . ?
C31 C32 1.499(4) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 O4 1.419(3) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
O4 C32 1.419(3) 4 ?
P C 1.602(4) . ?
C N 1.247(5) . ?
N C1 1.498(6) . ?
C1 C2 1.443(6) 4 ?
C1 C2 1.443(6) . ?
C1 H1A 1.0000 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 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
O2 K O1 C11 -149.5(2) 4 . . . ?
O2 K O1 C11 30.97(19) . . . . ?
O4 K O1 C11 120.75(19) . . . . ?
O3 K O1 C11 -174.95(18) 4 . . . ?
O3 K O1 C11 56.5(2) . . . . ?
C K O1 C11 -59.25(19) . . . . ?
N K O1 C11 -59.25(19) . . . . ?
P K O1 C11 -59.25(19) . . . . ?
O2 K O1 C11 -30.97(19) 4 . . 4 ?
O2 K O1 C11 149.5(2) . . . 4 ?
O4 K O1 C11 -120.75(19) . . . 4 ?
O3 K O1 C11 -56.5(2) 4 . . 4 ?
O3 K O1 C11 174.95(18) . . . 4 ?
C K O1 C11 59.25(19) . . . 4 ?
N K O1 C11 59.25(19) . . . 4 ?
P K O1 C11 59.25(19) . . . 4 ?
C11 O1 C11 C12 -179.41(17) 4 . . . ?
K O1 C11 C12 -63.9(2) . . . . ?
O1 C11 C12 O2 66.9(3) . . . . ?
C11 C12 O2 C21 -179.4(2) . . . . ?
C11 C12 O2 K -33.1(4) . . . . ?
O2 K O2 C21 144.84(16) 4 . . . ?
O4 K O2 C21 -7.9(2) . . . . ?
O1 K O2 C21 145.3(2) . . . . ?
O3 K O2 C21 66.5(2) 4 . . . ?
O3 K O2 C21 -7.07(18) . . . . ?
C K O2 C21 -116.2(2) . . . . ?
N K O2 C21 -136.0(2) . . . . ?
P K O2 C21 -90.8(2) . . . . ?
O2 K O2 C12 1.2(3) 4 . . . ?
O4 K O2 C12 -151.5(2) . . . . ?
O1 K O2 C12 1.7(3) . . . . ?
O3 K O2 C12 -77.1(3) 4 . . . ?
O3 K O2 C12 -150.7(3) . . . . ?
C K O2 C12 100.2(3) . . . . ?
N K O2 C12 80.4(3) . . . . ?
P K O2 C12 125.6(2) . . . . ?
C12 O2 C21 C22 -175.7(3) . . . . ?
K O2 C21 C22 38.6(3) . . . . ?
O2 C21 C22 O3 -64.9(3) . . . . ?
C21 C22 O3 C31 -177.7(2) . . . . ?
C21 C22 O3 K 58.9(3) . . . . ?
O2 K O3 C31 115.75(19) 4 . . . ?
O2 K O3 C31 -151.42(18) . . . . ?
O4 K O3 C31 27.75(17) . . . . ?
O1 K O3 C31 -177.24(17) . . . . ?
O3 K O3 C31 53.71(19) 4 . . . ?
C K O3 C31 -67.07(18) . . . . ?
N K O3 C31 -89.84(18) . . . . ?
P K O3 C31 -42.62(17) . . . . ?
O2 K O3 C22 -120.30(19) 4 . . . ?
O2 K O3 C22 -27.47(16) . . . . ?
O4 K O3 C22 151.70(18) . . . . ?
O1 K O3 C22 -53.29(18) . . . . ?
O3 K O3 C22 177.66(13) 4 . . . ?
C K O3 C22 56.88(17) . . . . ?
N K O3 C22 34.11(18) . . . . ?
P K O3 C22 81.33(16) . . . . ?
C22 O3 C31 C32 176.6(2) . . . . ?
K O3 C31 C32 -59.8(3) . . . . ?
O3 C31 C32 O4 66.4(3) . . . . ?
C31 C32 O4 C32 -179.50(16) . . . 4 ?
C31 C32 O4 K -38.6(3) . . . . ?
O2 K O4 C32 -7.5(2) 4 . . 4 ?
O2 K O4 C32 145.78(18) . . . 4 ?
O1 K O4 C32 69.13(19) . . . 4 ?
O3 K O4 C32 -6.72(18) 4 . . 4 ?
O3 K O4 C32 145.0(2) . . . 4 ?
C K O4 C32 -110.87(19) . . . 4 ?
N K O4 C32 -110.87(19) . . . 4 ?
P K O4 C32 -110.87(19) . . . 4 ?
O2 K O4 C32 -145.78(18) 4 . . . ?
O2 K O4 C32 7.5(2) . . . . ?
O1 K O4 C32 -69.13(19) . . . . ?
O3 K O4 C32 -145.0(2) 4 . . . ?
O3 K O4 C32 6.72(18) . . . . ?
C K O4 C32 110.87(19) . . . . ?
N K O4 C32 110.87(19) . . . . ?
P K O4 C32 110.87(19) . . . . ?
O2 K P C 65.45(5) 4 . . . ?
O2 K P C -65.45(5) . . . . ?
O3 K P C 123.71(4) 4 . . . ?
O3 K P C -123.71(4) . . . . ?
O2 K C N 60.17(4) 4 . . . ?
O2 K C N -60.17(4) . . . . ?
O3 K C N 118.67(4) 4 . . . ?
O3 K C N -118.67(4) . . . . ?
O2 K C P -119.83(4) 4 . . . ?
O2 K C P 119.83(4) . . . . ?
O3 K C P -61.33(4) 4 . . . ?
O3 K C P 61.33(4) . . . . ?
O2 K N C -119.64(4) 4 . . . ?
O2 K N C 119.64(4) . . . . ?
O3 K N C -70.62(6) 4 . . . ?
O3 K N C 70.62(6) . . . . ?
O2 K N C1 60.36(4) 4 . . . ?
O2 K N C1 -60.36(4) . . . . ?
O3 K N C1 109.38(6) 4 . . . ?
O3 K N C1 -109.38(6) . . . . ?
C N C1 C2 116.8(4) . . . 4 ?
K N C1 C2 -63.2(4) . . . 4 ?
C N C1 C2 -116.8(4) . . . . ?
K N C1 C2 63.2(4) . . . . ?
loop_
_cod_changelog_entry_id
_cod_changelog_entry_author
_cod_changelog_entry_date
_cod_changelog_entry_text
1 'Vaitkus, Antanas' 2021-10-24T01:00:00+03:00
'Updated bibliographic information.'
|
1100938.cif | #------------------------------------------------------------------------------
#$Date: 2016-12-31 20:31:26 +0200 (Sat, 31 Dec 2016) $
#$Revision: 189516 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/09/1100938.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_1100938
loop_
_publ_author_name
'Nripen Chanda'
'Debamita Paul'
'Sanjib Kar'
'Shaikh M. Mobin'
'Anindya Datta'
'Vedavati G. Puranik'
'K. Krishnamurthy Rao'
'Goutam Kumar Lahiri'
_publ_section_title
;
Effect of 2-(2-Pyridyl)azole-Based Ancillary Ligands (L1-4) on the
Electrophilicity of the Nitrosyl Function in [RuII(trpy)(L1-4)(NO)]3+
[trpy = 2,2':6',2''-Terpyridine]. Synthesis, Structures, and
Spectroscopic, Electrochemical, and Kinetic Aspects
;
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3499
_journal_page_last 3511
_journal_paper_doi 10.1021/ic048184w
_journal_volume 44
_journal_year 2005
_chemical_formula_moiety
'C27 H20 N7 O Ru.2(ClO4).(NO3).(H2O).0.5(C6H6)'
_chemical_formula_sum 'C30 H25 Cl2 N8 O13 Ru'
_chemical_formula_weight 877.55
_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 111.644(13)
_cell_angle_gamma 90.00
_cell_formula_units_Z 8
_cell_length_a 39.07(3)
_cell_length_b 9.625(8)
_cell_length_c 19.353(16)
_cell_measurement_reflns_used 1115
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 17.30
_cell_measurement_theta_min 2.22
_cell_volume 6765(9)
_computing_cell_refinement 'BRUKER SAINT'
_computing_data_collection 'BRUKER SMART'
_computing_data_reduction 'BRUKER SAINT'
_computing_molecular_graphics 'SHELXTL and PLATON'
_computing_publication_material 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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device ' Bruker Smart APEX'
_diffrn_measurement_device_type ' CCD Area Detector'
_diffrn_measurement_method 'Omega Scan'
_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 0.1745
_diffrn_reflns_av_sigmaI/netI 0.1605
_diffrn_reflns_limit_h_max 43
_diffrn_reflns_limit_h_min -43
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_l_max 21
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_number 22233
_diffrn_reflns_theta_full 23.50
_diffrn_reflns_theta_max 23.50
_diffrn_reflns_theta_min 2.12
_exptl_absorpt_coefficient_mu 0.702
_exptl_absorpt_correction_T_max 0.9578
_exptl_absorpt_correction_T_min 0.8654
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Bruker SADABS'
_exptl_crystal_colour Brown
_exptl_crystal_density_diffrn 1.721
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description Needle
_exptl_crystal_F_000 3536
_exptl_crystal_size_max 0.21
_exptl_crystal_size_mid 0.14
_exptl_crystal_size_min 0.06
_refine_diff_density_max 1.203
_refine_diff_density_min -0.497
_refine_diff_density_rms 0.118
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.992
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 487
_refine_ls_number_reflns 5014
_refine_ls_number_restraints 68
_refine_ls_restrained_S_all 1.002
_refine_ls_R_factor_all 0.1679
_refine_ls_R_factor_gt 0.0744
_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^)+(0.0786P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1456
_refine_ls_wR_factor_ref 0.1846
_reflns_number_gt 2526
_reflns_number_total 5014
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file ic048184wsi20041223_112911.cif
_cod_data_source_block C30H25Cl2N8O13Ru
_cod_depositor_comments
;
Marking attached hydrogen atoms.
Antanas Vaitkus,
2016-12-31
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 1100938
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
_atom_site_attached_hydrogens
Ru Ru 0.12471(2) 0.84864(9) 0.17243(4) 0.0412(3) Uani 1 1 d . . . 0
O1 O 0.1400(2) 1.0578(9) 0.0822(4) 0.068(2) Uani 1 1 d . . . 0
N1 N 0.1589(2) 0.9334(8) 0.2711(4) 0.041(2) Uani 1 1 d . . . 0
N2 N 0.1241(2) 0.6962(8) 0.2504(4) 0.041(2) Uani 1 1 d . . . 0
N3 N 0.1601(2) 0.7138(8) 0.1505(4) 0.044(2) Uani 1 1 d . . . 0
N4 N 0.0893(2) 0.7377(9) 0.0904(4) 0.044(2) Uani 1 1 d . . . 0
N5 N 0.0756(2) 0.9324(9) 0.1702(4) 0.044(2) Uani 1 1 d . . . 0
N6 N 0.1322(2) 0.9777(11) 0.1165(4) 0.052(3) Uani 1 1 d . . . 0
N7 N 0.1861(2) 0.9175(9) 0.3931(4) 0.054(3) Uani 1 1 d . . . 0
H7 H 0.1933 0.8820 0.4369 0.065 Uiso 1 1 calc R . . 0
C1 C 0.1941(3) 1.0491(12) 0.3749(6) 0.053(3) Uani 1 1 d . . . 0
C2 C 0.2129(3) 1.1583(14) 0.4190(7) 0.079(4) Uani 1 1 d . . . 0
H2 H 0.2235 1.1511 0.4705 0.095 Uiso 1 1 calc R . . 0
C3 C 0.2151(4) 1.2779(14) 0.3824(7) 0.087(5) Uani 1 1 d . . . 0
H3 H 0.2280 1.3529 0.4102 0.105 Uiso 1 1 calc R . . 0
C4 C 0.1988(3) 1.2926(12) 0.3052(7) 0.076(4) Uani 1 1 d . . . 0
H4 H 0.2011 1.3754 0.2825 0.091 Uiso 1 1 calc R . . 0
C5 C 0.1791(3) 1.1813(11) 0.2626(6) 0.059(3) Uani 1 1 d . . . 0
H5 H 0.1676 1.1896 0.2113 0.070 Uiso 1 1 calc R . . 0
C6 C 0.1771(3) 1.0595(11) 0.2978(6) 0.047(3) Uani 1 1 d . . . 0
C7 C 0.1652(2) 0.8564(11) 0.3306(5) 0.042(3) Uani 1 1 d . . . 0
C8 C 0.1486(3) 0.7208(11) 0.3214(5) 0.042(3) Uani 1 1 d . . . 0
C9 C 0.1555(3) 0.6242(12) 0.3766(6) 0.055(3) Uani 1 1 d . . . 0
H9 H 0.1723 0.6424 0.4241 0.066 Uiso 1 1 calc R . . 0
C10 C 0.1366(3) 0.4970(13) 0.3603(6) 0.067(4) Uani 1 1 d . . . 0
H10 H 0.1404 0.4295 0.3968 0.080 Uiso 1 1 calc R . . 0
C11 C 0.1126(3) 0.4755(12) 0.2894(6) 0.060(3) Uani 1 1 d . . . 0
H11 H 0.0999 0.3918 0.2771 0.072 Uiso 1 1 calc R . . 0
C12 C 0.1070(3) 0.5743(12) 0.2367(6) 0.063(3) Uani 1 1 d . . . 0
H12 H 0.0905 0.5560 0.1888 0.076 Uiso 1 1 calc R . . 0
C13 C 0.1969(3) 0.7019(11) 0.1841(6) 0.054(3) Uani 1 1 d . . . 0
H13 H 0.2091 0.7648 0.2216 0.065 Uiso 1 1 calc R . . 0
C14 C 0.2169(3) 0.6042(13) 0.1668(7) 0.075(4) Uani 1 1 d . . . 0
H14 H 0.2422 0.6000 0.1922 0.090 Uiso 1 1 calc R . . 0
C15 C 0.2000(4) 0.5119(13) 0.1119(8) 0.077(4) Uani 1 1 d . . . 0
H15 H 0.2135 0.4446 0.0988 0.093 Uiso 1 1 calc R . . 0
C16 C 0.1627(3) 0.5193(12) 0.0764(6) 0.062(3) Uani 1 1 d . . . 0
H16 H 0.1507 0.4558 0.0390 0.075 Uiso 1 1 calc R . . 0
C17 C 0.1429(3) 0.6195(11) 0.0953(5) 0.046(3) Uani 1 1 d . . . 0
C18 C 0.1028(3) 0.6368(11) 0.0607(5) 0.043(3) Uani 1 1 d . . . 0
C19 C 0.0780(3) 0.5629(12) 0.0021(6) 0.060(3) Uani 1 1 d . . . 0
H19 H 0.0863 0.4933 -0.0212 0.072 Uiso 1 1 calc R . . 0
C20 C 0.0416(3) 0.5923(13) -0.0211(6) 0.066(4) Uani 1 1 d . . . 0
H20 H 0.0250 0.5422 -0.0602 0.080 Uiso 1 1 calc R . . 0
C21 C 0.0290(3) 0.6954(12) 0.0125(6) 0.056(3) Uani 1 1 d . . . 0
H21 H 0.0039 0.7142 -0.0037 0.067 Uiso 1 1 calc R . . 0
C22 C 0.0528(3) 0.7695(12) 0.0691(5) 0.049(3) Uani 1 1 d . . . 0
C23 C 0.0452(3) 0.8811(11) 0.1133(5) 0.049(3) Uani 1 1 d . . . 0
C24 C 0.0119(3) 0.9361(12) 0.0992(6) 0.058(3) Uani 1 1 d . . . 0
H24 H -0.0081 0.9013 0.0600 0.069 Uiso 1 1 calc R . . 0
C25 C 0.0066(3) 1.0440(13) 0.1417(7) 0.070(4) Uani 1 1 d . . . 0
H25 H -0.0167 1.0813 0.1323 0.084 Uiso 1 1 calc R . . 0
C26 C 0.0369(3) 1.0927(13) 0.1977(7) 0.072(4) Uani 1 1 d . . . 0
H26 H 0.0345 1.1658 0.2270 0.086 Uiso 1 1 calc R . . 0
C27 C 0.0708(3) 1.0362(12) 0.2116(6) 0.055(3) Uani 1 1 d . . . 0
H27 H 0.0910 1.0707 0.2507 0.066 Uiso 1 1 calc R . . 0
Cl1 Cl 0.23176(9) 0.1366(4) 0.09661(18) 0.0746(10) Uani 1 1 d U . . 0
O2 O 0.2004(2) 0.2002(8) 0.0419(4) 0.085(3) Uani 1 1 d U . . 0
O3 O 0.2217(3) 0.0263(12) 0.1322(6) 0.138(4) Uani 1 1 d U . . 0
O4 O 0.2542(3) 0.0922(11) 0.0574(7) 0.132(4) Uani 1 1 d U . . 0
O5 O 0.2515(3) 0.2363(11) 0.1454(6) 0.150(4) Uani 1 1 d U . . 0
Cl2 Cl 0.10266(8) 0.1164(3) 0.41833(15) 0.0599(8) Uani 1 1 d U . . 0
O6 O 0.0828(3) 0.2141(8) 0.3621(4) 0.089(3) Uani 1 1 d U . . 0
O7 O 0.0812(2) 0.0796(8) 0.4603(4) 0.067(2) Uani 1 1 d U . . 0
O8 O 0.1102(2) -0.0030(9) 0.3825(5) 0.085(2) Uani 1 1 d U . . 0
O9 O 0.1359(2) 0.1789(10) 0.4668(5) 0.094(3) Uani 1 1 d U . . 0
N8 N 0.0732(3) 0.2906(10) 0.0988(5) 0.052(3) Uani 1 1 d . . . 0
O10 O 0.0504(2) 0.3701(9) 0.1145(4) 0.081(3) Uani 1 1 d . . . 0
O11 O 0.0603(2) 0.2091(10) 0.0485(5) 0.093(3) Uani 1 1 d . . . 0
O12 O 0.1041(3) 0.2985(10) 0.1356(6) 0.122(4) Uani 1 1 d . . . 0
C28 C 0.0173(5) 0.7346(19) 0.2768(10) 0.134(7) Uani 1 1 d . . . 0
H28 H 0.0295 0.8181 0.2936 0.161 Uiso 1 1 calc R . . 0
C29 C 0.0336(5) 0.613(2) 0.3054(10) 0.125(7) Uani 1 1 d . . . 0
H29 H 0.0564 0.6127 0.3443 0.150 Uiso 1 1 calc R . . 0
C30 C 0.0163(5) 0.490(2) 0.2762(9) 0.129(7) Uani 1 1 d . . . 0
H30 H 0.0279 0.4065 0.2941 0.155 Uiso 1 1 calc R . . 0
O13 O 0.1014(3) 0.7384(9) 0.4566(5) 0.107(3) Uani 1 1 d . . . 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
Ru 0.0369(5) 0.0400(5) 0.0353(5) -0.0032(5) -0.0001(3) -0.0024(5)
O1 0.069(6) 0.079(7) 0.048(5) 0.014(5) 0.014(4) -0.011(5)
N1 0.042(5) 0.034(5) 0.037(5) -0.002(4) 0.003(4) -0.007(4)
N2 0.038(5) 0.040(6) 0.035(5) 0.002(4) 0.003(4) -0.006(4)
N3 0.032(5) 0.047(6) 0.039(5) 0.000(4) -0.003(4) -0.003(4)
N4 0.046(6) 0.044(6) 0.029(5) -0.011(4) -0.001(4) -0.007(5)
N5 0.052(6) 0.040(6) 0.035(5) -0.004(4) 0.010(4) 0.002(4)
N6 0.036(5) 0.085(8) 0.029(5) -0.005(5) 0.006(4) -0.008(5)
N7 0.058(6) 0.048(6) 0.034(5) -0.003(4) -0.009(4) -0.013(5)
C1 0.048(7) 0.046(8) 0.045(7) -0.002(6) -0.007(5) -0.011(6)
C2 0.089(9) 0.061(9) 0.061(8) -0.010(8) -0.005(7) -0.023(8)
C3 0.101(11) 0.049(9) 0.071(9) -0.015(8) -0.016(8) -0.011(8)
C4 0.066(8) 0.042(8) 0.093(10) -0.001(7) -0.003(7) -0.021(7)
C5 0.056(7) 0.036(8) 0.066(8) -0.003(6) 0.002(6) -0.008(6)
C6 0.035(6) 0.036(7) 0.051(7) -0.009(6) -0.006(5) -0.009(5)
C7 0.033(6) 0.044(7) 0.040(6) -0.008(6) 0.002(5) -0.011(6)
C8 0.048(7) 0.032(7) 0.037(6) -0.003(5) 0.007(5) 0.001(5)
C9 0.054(7) 0.060(9) 0.042(6) -0.010(6) 0.008(5) 0.000(7)
C10 0.077(9) 0.056(9) 0.056(8) 0.001(7) 0.011(7) -0.002(7)
C11 0.075(9) 0.043(8) 0.055(7) -0.007(6) 0.015(7) -0.021(6)
C12 0.074(9) 0.050(8) 0.054(7) -0.004(7) 0.010(6) -0.033(7)
C13 0.058(8) 0.037(7) 0.059(7) -0.008(6) 0.011(6) 0.002(6)
C14 0.057(8) 0.073(10) 0.079(9) -0.008(8) 0.006(7) 0.027(7)
C15 0.069(10) 0.054(9) 0.101(10) -0.021(8) 0.022(8) 0.012(7)
C16 0.064(9) 0.059(9) 0.052(7) -0.017(6) 0.007(6) -0.001(7)
C17 0.054(7) 0.039(8) 0.044(6) -0.007(5) 0.016(6) 0.007(6)
C18 0.058(7) 0.033(7) 0.033(5) -0.011(5) 0.011(5) -0.008(6)
C19 0.077(10) 0.049(8) 0.050(7) -0.011(6) 0.020(7) -0.007(7)
C20 0.053(9) 0.066(9) 0.054(7) -0.006(7) -0.010(6) -0.014(7)
C21 0.041(7) 0.066(9) 0.049(7) -0.009(6) 0.003(6) -0.007(6)
C22 0.045(7) 0.053(8) 0.036(6) -0.006(6) 0.000(5) -0.010(6)
C23 0.037(7) 0.052(8) 0.041(6) 0.007(6) -0.004(5) 0.002(6)
C24 0.035(7) 0.064(9) 0.064(8) -0.007(7) 0.006(6) -0.004(6)
C25 0.056(8) 0.072(10) 0.079(9) -0.003(8) 0.021(7) 0.012(7)
C26 0.052(8) 0.079(10) 0.078(9) -0.011(7) 0.017(7) 0.003(7)
C27 0.044(7) 0.058(8) 0.053(7) -0.007(6) 0.005(6) -0.009(6)
Cl1 0.073(2) 0.061(2) 0.068(2) 0.0003(19) 0.0007(17) 0.013(2)
O2 0.082(5) 0.067(6) 0.072(5) -0.003(4) -0.012(4) 0.013(4)
O3 0.119(8) 0.136(8) 0.136(8) 0.067(7) 0.022(6) 0.006(6)
O4 0.131(8) 0.112(8) 0.167(9) 0.027(6) 0.070(7) 0.046(6)
O5 0.139(8) 0.116(7) 0.105(7) -0.022(6) -0.060(6) -0.004(6)
Cl2 0.0633(19) 0.059(2) 0.0507(17) 0.0015(15) 0.0137(15) -0.0005(16)
O6 0.126(7) 0.063(5) 0.061(5) 0.016(4) 0.013(4) 0.014(5)
O7 0.063(5) 0.080(6) 0.059(5) -0.002(4) 0.022(4) -0.004(4)
O8 0.103(7) 0.077(6) 0.078(5) 0.000(4) 0.037(5) 0.018(5)
O9 0.055(5) 0.116(7) 0.093(6) -0.014(5) 0.007(4) -0.020(5)
N8 0.035(6) 0.037(6) 0.061(6) -0.007(5) -0.010(5) -0.001(5)
O10 0.068(6) 0.067(7) 0.084(6) -0.010(5) 0.002(5) -0.003(5)
O11 0.077(6) 0.097(8) 0.090(7) -0.047(6) 0.013(5) -0.010(5)
O12 0.064(7) 0.120(9) 0.130(8) -0.059(7) -0.026(6) 0.025(6)
C28 0.16(2) 0.093(13) 0.13(2) -0.013(12) 0.033(14) -0.013(13)
C29 0.102(14) 0.16(2) 0.096(13) -0.007(14) 0.013(10) 0.006(14)
C30 0.15(2) 0.112(14) 0.107(17) 0.014(12) 0.025(12) 0.028(13)
O13 0.134(8) 0.069(7) 0.115(7) -0.003(6) 0.043(7) -0.004(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'
Cl Cl 0.1484 0.1585 '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'
Ru Ru -1.2594 0.8363 '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'
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
N6 Ru N4 96.5(4) . . ?
N6 Ru N3 92.3(4) . . ?
N4 Ru N3 79.6(3) . . ?
N6 Ru N1 95.4(4) . . ?
N4 Ru N1 168.0(3) . . ?
N3 Ru N1 100.8(3) . . ?
N6 Ru N5 94.4(4) . . ?
N4 Ru N5 80.0(4) . . ?
N3 Ru N5 159.0(3) . . ?
N1 Ru N5 98.3(3) . . ?
N6 Ru N2 171.3(3) . . ?
N4 Ru N2 90.5(3) . . ?
N3 Ru N2 84.0(3) . . ?
N1 Ru N2 77.6(3) . . ?
N5 Ru N2 91.7(3) . . ?
C7 N1 C6 105.0(8) . . ?
C7 N1 Ru 116.0(6) . . ?
C6 N1 Ru 138.8(7) . . ?
C12 N2 C8 117.7(9) . . ?
C12 N2 Ru 127.5(7) . . ?
C8 N2 Ru 114.0(7) . . ?
C13 N3 C17 116.7(9) . . ?
C13 N3 Ru 129.3(7) . . ?
C17 N3 Ru 113.8(7) . . ?
C18 N4 C22 124.7(8) . . ?
C18 N4 Ru 117.7(7) . . ?
C22 N4 Ru 117.6(7) . . ?
C27 N5 C23 118.4(9) . . ?
C27 N5 Ru 127.9(7) . . ?
C23 N5 Ru 113.3(7) . . ?
O1 N6 Ru 174.4(9) . . ?
C7 N7 C1 107.3(9) . . ?
C7 N7 H7 126.4 . . ?
C1 N7 H7 126.4 . . ?
N7 C1 C2 131.3(10) . . ?
N7 C1 C6 106.0(9) . . ?
C2 C1 C6 122.7(11) . . ?
C3 C2 C1 116.1(11) . . ?
C3 C2 H2 121.9 . . ?
C1 C2 H2 121.9 . . ?
C2 C3 C4 123.2(12) . . ?
C2 C3 H3 118.4 . . ?
C4 C3 H3 118.4 . . ?
C5 C4 C3 119.1(12) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
C6 C5 C4 118.8(11) . . ?
C6 C5 H5 120.6 . . ?
C4 C5 H5 120.6 . . ?
C5 C6 C1 120.0(10) . . ?
C5 C6 N1 132.1(9) . . ?
C1 C6 N1 107.9(10) . . ?
N1 C7 N7 113.8(9) . . ?
N1 C7 C8 118.2(8) . . ?
N7 C7 C8 128.0(10) . . ?
C9 C8 N2 121.9(9) . . ?
C9 C8 C7 124.8(9) . . ?
N2 C8 C7 113.3(9) . . ?
C8 C9 C10 118.9(10) . . ?
C8 C9 H9 120.6 . . ?
C10 C9 H9 120.6 . . ?
C11 C10 C9 117.9(11) . . ?
C11 C10 H10 121.0 . . ?
C9 C10 H10 121.0 . . ?
C12 C11 C10 120.8(11) . . ?
C12 C11 H11 119.6 . . ?
C10 C11 H11 119.6 . . ?
N2 C12 C11 122.8(10) . . ?
N2 C12 H12 118.6 . . ?
C11 C12 H12 118.6 . . ?
C14 C13 N3 123.7(10) . . ?
C14 C13 H13 118.2 . . ?
N3 C13 H13 118.2 . . ?
C13 C14 C15 119.6(12) . . ?
C13 C14 H14 120.2 . . ?
C15 C14 H14 120.2 . . ?
C14 C15 C16 118.9(12) . . ?
C14 C15 H15 120.6 . . ?
C16 C15 H15 120.6 . . ?
C15 C16 C17 120.3(11) . . ?
C15 C16 H16 119.8 . . ?
C17 C16 H16 119.8 . . ?
C16 C17 N3 120.7(10) . . ?
C16 C17 C18 124.8(10) . . ?
N3 C17 C18 114.4(9) . . ?
N4 C18 C19 117.2(10) . . ?
N4 C18 C17 114.4(9) . . ?
C19 C18 C17 128.4(11) . . ?
C20 C19 C18 119.7(11) . . ?
C20 C19 H19 120.1 . . ?
C18 C19 H19 120.1 . . ?
C19 C20 C21 120.7(11) . . ?
C19 C20 H20 119.6 . . ?
C21 C20 H20 119.6 . . ?
C22 C21 C20 120.3(11) . . ?
C22 C21 H21 119.8 . . ?
C20 C21 H21 119.8 . . ?
C21 C22 N4 117.3(11) . . ?
C21 C22 C23 129.1(11) . . ?
N4 C22 C23 113.6(9) . . ?
C24 C23 N5 120.5(10) . . ?
C24 C23 C22 124.2(10) . . ?
N5 C23 C22 115.3(9) . . ?
C23 C24 C25 121.6(11) . . ?
C23 C24 H24 119.2 . . ?
C25 C24 H24 119.2 . . ?
C26 C25 C24 116.8(12) . . ?
C26 C25 H25 121.6 . . ?
C24 C25 H25 121.6 . . ?
C25 C26 C27 121.2(12) . . ?
C25 C26 H26 119.4 . . ?
C27 C26 H26 119.4 . . ?
N5 C27 C26 121.4(10) . . ?
N5 C27 H27 119.3 . . ?
C26 C27 H27 119.3 . . ?
O5 Cl1 O3 112.4(7) . . ?
O5 Cl1 O4 106.1(8) . . ?
O3 Cl1 O4 112.0(7) . . ?
O5 Cl1 O2 108.8(6) . . ?
O3 Cl1 O2 111.8(6) . . ?
O4 Cl1 O2 105.2(6) . . ?
O7 Cl2 O9 108.6(5) . . ?
O7 Cl2 O8 110.5(5) . . ?
O9 Cl2 O8 110.9(6) . . ?
O7 Cl2 O6 109.3(5) . . ?
O9 Cl2 O6 109.3(6) . . ?
O8 Cl2 O6 108.1(5) . . ?
O12 N8 O11 124.8(12) . . ?
O12 N8 O10 118.1(10) . . ?
O11 N8 O10 117.0(9) . . ?
C29 C28 C28 119.8(12) . 2 ?
C29 C28 H28 120.1 . . ?
C28 C28 H28 120.1 2 . ?
C28 C29 C30 119.3(18) . . ?
C28 C29 H29 120.4 . . ?
C30 C29 H29 120.4 . . ?
C30 C30 C29 120.8(11) 2 . ?
C30 C30 H30 119.6 2 . ?
C29 C30 H30 119.6 . . ?
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
Ru N6 1.742(10) . ?
Ru N4 1.989(7) . ?
Ru N3 2.053(8) . ?
Ru N1 2.053(7) . ?
Ru N5 2.066(8) . ?
Ru N2 2.112(8) . ?
O1 N6 1.130(10) . ?
N1 C7 1.314(11) . ?
N1 C6 1.405(12) . ?
N2 C12 1.327(12) . ?
N2 C8 1.374(11) . ?
N3 C13 1.344(12) . ?
N3 C17 1.373(12) . ?
N4 C18 1.333(12) . ?
N4 C22 1.363(12) . ?
N5 C27 1.337(12) . ?
N5 C23 1.380(11) . ?
N7 C7 1.321(11) . ?
N7 C1 1.380(12) . ?
N7 H7 0.8600 . ?
C1 C2 1.383(14) . ?
C1 C6 1.396(13) . ?
C2 C3 1.370(16) . ?
C2 H2 0.9300 . ?
C3 C4 1.398(16) . ?
C3 H3 0.9300 . ?
C4 C5 1.397(14) . ?
C4 H4 0.9300 . ?
C5 C6 1.373(14) . ?
C5 H5 0.9300 . ?
C7 C8 1.440(13) . ?
C8 C9 1.366(13) . ?
C9 C10 1.404(14) . ?
C9 H9 0.9300 . ?
C10 C11 1.362(14) . ?
C10 H10 0.9300 . ?
C11 C12 1.352(14) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C14 1.343(14) . ?
C13 H13 0.9300 . ?
C14 C15 1.355(15) . ?
C14 H14 0.9300 . ?
C15 C16 1.364(15) . ?
C15 H15 0.9300 . ?
C16 C17 1.368(14) . ?
C16 H16 0.9300 . ?
C17 C18 1.468(14) . ?
C18 C19 1.387(13) . ?
C19 C20 1.354(15) . ?
C19 H19 0.9300 . ?
C20 C21 1.373(15) . ?
C20 H20 0.9300 . ?
C21 C22 1.350(13) . ?
C21 H21 0.9300 . ?
C22 C23 1.470(14) . ?
C23 C24 1.337(14) . ?
C24 C25 1.387(15) . ?
C24 H24 0.9300 . ?
C25 C26 1.362(15) . ?
C25 H25 0.9300 . ?
C26 C27 1.363(14) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
Cl1 O5 1.368(9) . ?
Cl1 O3 1.398(11) . ?
Cl1 O4 1.420(11) . ?
Cl1 O2 1.427(8) . ?
Cl2 O7 1.411(8) . ?
Cl2 O9 1.425(8) . ?
Cl2 O8 1.428(9) . ?
Cl2 O6 1.431(8) . ?
N8 O12 1.155(10) . ?
N8 O11 1.207(10) . ?
N8 O10 1.292(11) . ?
C28 C29 1.35(2) . ?
C28 C28 1.37(3) 2 ?
C28 H28 0.9300 . ?
C29 C30 1.38(2) . ?
C29 H29 0.9300 . ?
C30 C30 1.30(3) 2 ?
C30 H30 0.9300 . ?
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
N6 Ru N1 C7 -171.6(7) . . . . ?
N4 Ru N1 C7 12(2) . . . . ?
N3 Ru N1 C7 -78.2(7) . . . . ?
N5 Ru N1 C7 93.1(7) . . . . ?
N2 Ru N1 C7 3.1(7) . . . . ?
N6 Ru N1 C6 13.9(11) . . . . ?
N4 Ru N1 C6 -162.0(15) . . . . ?
N3 Ru N1 C6 107.3(10) . . . . ?
N5 Ru N1 C6 -81.4(11) . . . . ?
N2 Ru N1 C6 -171.4(11) . . . . ?
N6 Ru N2 C12 -140(2) . . . . ?
N4 Ru N2 C12 4.9(10) . . . . ?
N3 Ru N2 C12 -74.6(9) . . . . ?
N1 Ru N2 C12 -177.1(10) . . . . ?
N5 Ru N2 C12 84.8(9) . . . . ?
N6 Ru N2 C8 30(3) . . . . ?
N4 Ru N2 C8 174.8(7) . . . . ?
N3 Ru N2 C8 95.3(7) . . . . ?
N1 Ru N2 C8 -7.2(7) . . . . ?
N5 Ru N2 C8 -105.3(7) . . . . ?
N6 Ru N3 C13 85.7(9) . . . . ?
N4 Ru N3 C13 -178.1(9) . . . . ?
N1 Ru N3 C13 -10.3(9) . . . . ?
N5 Ru N3 C13 -165.5(8) . . . . ?
N2 Ru N3 C13 -86.4(9) . . . . ?
N6 Ru N3 C17 -97.4(7) . . . . ?
N4 Ru N3 C17 -1.2(7) . . . . ?
N1 Ru N3 C17 166.7(7) . . . . ?
N5 Ru N3 C17 11.4(13) . . . . ?
N2 Ru N3 C17 90.5(7) . . . . ?
N6 Ru N4 C18 90.9(8) . . . . ?
N3 Ru N4 C18 -0.3(7) . . . . ?
N1 Ru N4 C18 -93.2(18) . . . . ?
N5 Ru N4 C18 -175.8(8) . . . . ?
N2 Ru N4 C18 -84.1(7) . . . . ?
N6 Ru N4 C22 -89.7(8) . . . . ?
N3 Ru N4 C22 179.1(8) . . . . ?
N1 Ru N4 C22 86.2(19) . . . . ?
N5 Ru N4 C22 3.6(7) . . . . ?
N2 Ru N4 C22 95.3(8) . . . . ?
N6 Ru N5 C27 -81.6(9) . . . . ?
N4 Ru N5 C27 -177.5(9) . . . . ?
N3 Ru N5 C27 169.9(8) . . . . ?
N1 Ru N5 C27 14.5(9) . . . . ?
N2 Ru N5 C27 92.3(9) . . . . ?
N6 Ru N5 C23 91.3(7) . . . . ?
N4 Ru N5 C23 -4.6(7) . . . . ?
N3 Ru N5 C23 -17.2(13) . . . . ?
N1 Ru N5 C23 -172.6(7) . . . . ?
N2 Ru N5 C23 -94.8(7) . . . . ?
N4 Ru N6 O1 -117(9) . . . . ?
N3 Ru N6 O1 -37(9) . . . . ?
N1 Ru N6 O1 64(9) . . . . ?
N5 Ru N6 O1 163(9) . . . . ?
N2 Ru N6 O1 28(11) . . . . ?
C7 N7 C1 C2 175.8(13) . . . . ?
C7 N7 C1 C6 -1.1(12) . . . . ?
N7 C1 C2 C3 -178.3(12) . . . . ?
C6 C1 C2 C3 -2(2) . . . . ?
C1 C2 C3 C4 1(2) . . . . ?
C2 C3 C4 C5 0(2) . . . . ?
C3 C4 C5 C6 -1.6(19) . . . . ?
C4 C5 C6 C1 0.9(17) . . . . ?
C4 C5 C6 N1 177.9(11) . . . . ?
N7 C1 C6 C5 178.1(10) . . . . ?
C2 C1 C6 C5 0.9(18) . . . . ?
N7 C1 C6 N1 0.5(12) . . . . ?
C2 C1 C6 N1 -176.7(11) . . . . ?
C7 N1 C6 C5 -176.9(12) . . . . ?
Ru N1 C6 C5 -2(2) . . . . ?
C7 N1 C6 C1 0.3(12) . . . . ?
Ru N1 C6 C1 175.2(8) . . . . ?
C6 N1 C7 N7 -1.1(12) . . . . ?
Ru N1 C7 N7 -177.3(7) . . . . ?
C6 N1 C7 C8 177.5(9) . . . . ?
Ru N1 C7 C8 1.2(12) . . . . ?
C1 N7 C7 N1 1.4(12) . . . . ?
C1 N7 C7 C8 -177.0(10) . . . . ?
C12 N2 C8 C9 0.0(15) . . . . ?
Ru N2 C8 C9 -171.0(8) . . . . ?
C12 N2 C8 C7 -179.3(10) . . . . ?
Ru N2 C8 C7 9.8(11) . . . . ?
N1 C7 C8 C9 173.3(10) . . . . ?
N7 C7 C8 C9 -8.3(18) . . . . ?
N1 C7 C8 N2 -7.5(13) . . . . ?
N7 C7 C8 N2 170.9(10) . . . . ?
N2 C8 C9 C10 -0.7(16) . . . . ?
C7 C8 C9 C10 178.4(10) . . . . ?
C8 C9 C10 C11 0.9(17) . . . . ?
C9 C10 C11 C12 -0.4(19) . . . . ?
C8 N2 C12 C11 0.6(17) . . . . ?
Ru N2 C12 C11 170.2(9) . . . . ?
C10 C11 C12 N2 0(2) . . . . ?
C17 N3 C13 C14 -0.2(16) . . . . ?
Ru N3 C13 C14 176.7(9) . . . . ?
N3 C13 C14 C15 0.7(19) . . . . ?
C13 C14 C15 C16 -1(2) . . . . ?
C14 C15 C16 C17 1(2) . . . . ?
C15 C16 C17 N3 -0.3(17) . . . . ?
C15 C16 C17 C18 -180.0(11) . . . . ?
C13 N3 C17 C16 0.0(15) . . . . ?
Ru N3 C17 C16 -177.4(8) . . . . ?
C13 N3 C17 C18 179.7(9) . . . . ?
Ru N3 C17 C18 2.3(11) . . . . ?
C22 N4 C18 C19 2.5(15) . . . . ?
Ru N4 C18 C19 -178.1(7) . . . . ?
C22 N4 C18 C17 -177.7(9) . . . . ?
Ru N4 C18 C17 1.6(12) . . . . ?
C16 C17 C18 N4 177.1(10) . . . . ?
N3 C17 C18 N4 -2.6(13) . . . . ?
C16 C17 C18 C19 -3.2(18) . . . . ?
N3 C17 C18 C19 177.1(10) . . . . ?
N4 C18 C19 C20 -1.8(16) . . . . ?
C17 C18 C19 C20 178.5(11) . . . . ?
C18 C19 C20 C21 0.4(18) . . . . ?
C19 C20 C21 C22 0.4(18) . . . . ?
C20 C21 C22 N4 0.2(16) . . . . ?
C20 C21 C22 C23 -178.7(11) . . . . ?
C18 N4 C22 C21 -1.8(16) . . . . ?
Ru N4 C22 C21 178.9(7) . . . . ?
C18 N4 C22 C23 177.3(9) . . . . ?
Ru N4 C22 C23 -2.0(12) . . . . ?
C27 N5 C23 C24 1.2(15) . . . . ?
Ru N5 C23 C24 -172.4(8) . . . . ?
C27 N5 C23 C22 178.5(9) . . . . ?
Ru N5 C23 C22 4.9(11) . . . . ?
C21 C22 C23 C24 -5.9(19) . . . . ?
N4 C22 C23 C24 175.1(10) . . . . ?
C21 C22 C23 N5 176.9(10) . . . . ?
N4 C22 C23 N5 -2.0(13) . . . . ?
N5 C23 C24 C25 -1.2(17) . . . . ?
C22 C23 C24 C25 -178.3(10) . . . . ?
C23 C24 C25 C26 1.0(18) . . . . ?
C24 C25 C26 C27 -0.9(19) . . . . ?
C23 N5 C27 C26 -1.1(16) . . . . ?
Ru N5 C27 C26 171.5(8) . . . . ?
C25 C26 C27 N5 0.9(19) . . . . ?
C28 C28 C29 C30 5(4) 2 . . . ?
C28 C29 C30 C30 -3(4) . . . 2 ?
|
1100939.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100939.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_1100939
loop_
_publ_author_name
'Nripen Chanda'
'Debamita Paul'
'Sanjib Kar'
'Shaikh M. Mobin'
'Anindya Datta'
'Vedavati G. Puranik'
'K. Krishnamurthy Rao'
'Goutam Kumar Lahiri'
_publ_section_title
;
Effect of 2-(2-Pyridyl)azole-Based Ancillary Ligands (L1-4) on the
Electrophilicity of the Nitrosyl Function in [RuII(trpy)(L1-4)(NO)]3+ [trpy
= 2,2':6',2''-Terpyridine]. Synthesis, Structures, and
Spectroscopic, Electrochemical, and Kinetic Aspects
;
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3499
_journal_page_last 3511
_journal_paper_doi 10.1021/ic048184w
_journal_volume 44
_journal_year 2005
_chemical_formula_sum 'C28 H22 Cl2 N6 O4 Ru'
_chemical_formula_weight 678.49
_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 92.644(6)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 14.3980(8)
_cell_length_b 12.1620(9)
_cell_length_c 15.4770(14)
_cell_measurement_reflns_used 25
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 12.4500
_cell_measurement_theta_min 6.5900
_cell_volume 2707.3(4)
_computing_cell_refinement 'Argus (Nonius, MACH3 software)'
_computing_data_collection 'Argus (Nonius, MACH3 software)'
_computing_data_reduction 'Maxus (Nonius software)'
_computing_molecular_graphics Ortep3
_computing_publication_material Maxus
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 293(2)
_diffrn_measured_fraction_theta_full 0.874
_diffrn_measured_fraction_theta_max 0.874
_diffrn_measurement_device_type 'Enraf-Nonius CAD-4'
_diffrn_measurement_method \w/q-scan
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type ' MoK\a'
_diffrn_radiation_wavelength 0.70930
_diffrn_reflns_av_R_equivalents 0.0000
_diffrn_reflns_av_sigmaI/netI 0.0229
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_h_min 0
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_number 4396
_diffrn_reflns_theta_full 24.94
_diffrn_reflns_theta_max 24.94
_diffrn_reflns_theta_min 1.89
_diffrn_standards_decay_% <3%
_diffrn_standards_interval_time 3600
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 0.824
_exptl_absorpt_correction_T_max 1.000
_exptl_absorpt_correction_T_min 0.966
_exptl_absorpt_correction_type psi-scan
_exptl_absorpt_process_details
;
psi-scan (North, Philips & Mathews, 1968)
;
_exptl_crystal_colour Brown
_exptl_crystal_density_diffrn 1.665
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description Square
_exptl_crystal_F_000 1368
_exptl_crystal_size_max 0.30
_exptl_crystal_size_mid 0.20
_exptl_crystal_size_min 0.20
_refine_diff_density_max 0.737
_refine_diff_density_min -0.541
_refine_diff_density_rms 0.072
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.080
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 458
_refine_ls_number_reflns 4396
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.080
_refine_ls_R_factor_all 0.0410
_refine_ls_R_factor_gt 0.0339
_refine_ls_shift/su_max 0.081
_refine_ls_shift/su_mean 0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0454P)^2^+3.9339P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0860
_refine_ls_wR_factor_ref 0.0934
_reflns_number_gt 3960
_reflns_number_total 4396
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file ic048184wsi20041223_112952.cif
_cod_data_source_block max
_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:
'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0454P)^2^+3.9339P] 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^)+(0.0454P)^2^+3.9339P] 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 'P 21/n'
_cod_database_code 1100939
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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru Ru 0.137754(19) 0.26465(2) 0.137761(18) 0.03327(11) Uani 1 d . . .
Cl1 Cl 0.16385(7) 0.45547(8) 0.17676(6) 0.0449(2) Uani 1 d . . .
Cl2 Cl 0.75961(8) 0.00094(11) 0.13424(8) 0.0642(3) Uani 1 d . . .
N1 N 0.3816(2) 0.0852(3) 0.1201(2) 0.0469(8) Uani 1 d . . .
N2 N 0.2777(2) 0.2158(3) 0.1449(2) 0.0384(7) Uani 1 d . . .
N3 N 0.1281(2) 0.0981(3) 0.11455(19) 0.0384(7) Uani 1 d . . .
N4 N 0.0924(2) 0.2298(2) 0.25946(19) 0.0379(7) Uani 1 d . . .
N5 N 0.0065(2) 0.3006(2) 0.1212(2) 0.0361(7) Uani 1 d . . .
N6 N 0.1335(2) 0.3100(3) 0.00955(19) 0.0389(7) Uani 1 d . . .
C1 C 0.4228(4) -0.0212(5) 0.1009(4) 0.0693(15) Uani 1 d . . .
C2 C 0.3658(3) 0.2636(3) 0.1493(2) 0.0433(9) Uani 1 d . . .
C3 C 0.3937(3) 0.3706(4) 0.1668(3) 0.0559(11) Uani 1 d . . .
C4 C 0.4882(4) 0.3912(5) 0.1683(4) 0.0691(14) Uani 1 d . . .
C5 C 0.5527(3) 0.3086(5) 0.1542(3) 0.0693(14) Uani 1 d . . .
C6 C 0.5262(3) 0.2042(5) 0.1360(3) 0.0614(13) Uani 1 d . . .
C7 C 0.4305(3) 0.1815(4) 0.1340(3) 0.0475(10) Uani 1 d . . .
C8 C 0.2904(3) 0.1099(3) 0.1277(2) 0.0393(8) Uani 1 d . . .
C9 C 0.2090(3) 0.0397(3) 0.1186(2) 0.0417(9) Uani 1 d . . .
C10 C 0.2079(4) -0.0739(4) 0.1170(3) 0.0553(11) Uani 1 d . . .
C11 C 0.1251(4) -0.1289(4) 0.1107(3) 0.0647(14) Uani 1 d . . .
C12 C 0.0438(3) -0.0706(4) 0.1048(3) 0.0562(11) Uani 1 d . . .
C13 C 0.0483(3) 0.0424(3) 0.1066(3) 0.0472(10) Uani 1 d . . .
C14 C 0.1407(3) 0.1872(4) 0.3277(3) 0.0497(10) Uani 1 d . . .
C15 C 0.1009(4) 0.1669(4) 0.4055(3) 0.0643(13) Uani 1 d . . .
C16 C 0.0078(4) 0.1920(5) 0.4147(3) 0.0671(14) Uani 1 d . . .
C17 C -0.0425(4) 0.2343(4) 0.3449(3) 0.0557(11) Uani 1 d . . .
C18 C 0.0000(3) 0.2515(3) 0.2673(3) 0.0417(9) Uani 1 d . . .
C19 C -0.0495(3) 0.2936(3) 0.1888(3) 0.0413(9) Uani 1 d . . .
C20 C -0.1418(3) 0.3237(4) 0.1783(3) 0.0543(11) Uani 1 d . . .
C21 C -0.1749(3) 0.3626(4) 0.0990(4) 0.0608(13) Uani 1 d . . .
C22 C -0.1169(3) 0.3715(3) 0.0312(3) 0.0498(10) Uani 1 d . . .
C23 C -0.0251(3) 0.3392(3) 0.0434(2) 0.0395(8) Uani 1 d . . .
C24 C 0.0472(3) 0.3439(3) -0.0206(2) 0.0379(8) Uani 1 d . . .
C25 C 0.0321(3) 0.3800(3) -0.1047(3) 0.0496(10) Uani 1 d . . .
C26 C 0.1051(4) 0.3835(4) -0.1590(3) 0.0594(12) Uani 1 d . . .
C27 C 0.1920(4) 0.3495(4) -0.1292(3) 0.0651(13) Uani 1 d . . .
C28 C 0.2031(3) 0.3125(4) -0.0454(3) 0.0545(11) Uani 1 d . . .
O1 O 0.7408(6) 0.1074(6) 0.1143(8) 0.260(5) Uani 1 d . . .
O2 O 0.8239(4) -0.0301(8) 0.0809(4) 0.190(4) Uani 1 d . . .
O3 O 0.7932(6) -0.0124(10) 0.2163(4) 0.244(5) Uani 1 d . . .
O4 O 0.6758(4) -0.0487(6) 0.1201(6) 0.197(4) Uani 1 d . . .
H13 H -0.005(3) 0.082(3) 0.102(2) 0.041(11) Uiso 1 d . . .
H22 H -0.138(3) 0.402(3) -0.022(3) 0.047(11) Uiso 1 d . . .
H28 H 0.260(4) 0.291(5) -0.024(4) 0.085(18) Uiso 1 d . . .
H25 H -0.026(3) 0.400(4) -0.127(3) 0.059(13) Uiso 1 d . . .
H14 H 0.200(3) 0.169(4) 0.321(3) 0.049(12) Uiso 1 d . . .
H9 H 0.353(3) 0.421(4) 0.174(3) 0.052(13) Uiso 1 d . . .
H10 H 0.265(3) -0.108(4) 0.125(3) 0.059(13) Uiso 1 d . . .
H26 H 0.099(3) 0.408(4) -0.213(3) 0.053(12) Uiso 1 d . . .
H12 H -0.018(3) -0.104(4) 0.100(3) 0.067(14) Uiso 1 d . . .
H20 H -0.177(3) 0.322(4) 0.220(3) 0.055(13) Uiso 1 d . . .
H1 H 0.416(3) -0.077(5) 0.153(3) 0.079(16) Uiso 1 d . . .
H6 H 0.572(4) 0.147(4) 0.128(3) 0.067(14) Uiso 1 d . . .
H27 H 0.245(4) 0.352(5) -0.173(4) 0.10(2) Uiso 1 d . . .
H4 H 0.505(3) 0.458(4) 0.182(3) 0.059(14) Uiso 1 d . . .
H21 H -0.237(4) 0.382(4) 0.092(3) 0.078(16) Uiso 1 d . . .
H15 H 0.141(4) 0.135(5) 0.450(4) 0.091(18) Uiso 1 d . . .
H17 H -0.109(4) 0.258(4) 0.350(4) 0.078(16) Uiso 1 d . . .
H5 H 0.621(4) 0.327(5) 0.155(4) 0.091(17) Uiso 1 d . . .
H11 H 0.124(4) -0.203(6) 0.113(4) 0.10(2) Uiso 1 d . . .
H16 H -0.020(4) 0.168(6) 0.473(4) 0.12(2) Uiso 1 d . . .
H1B H 0.484(4) -0.005(4) 0.099(3) 0.060(14) Uiso 1 d . . .
H1A H 0.395(4) -0.048(5) 0.040(4) 0.10(2) Uiso 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
Ru 0.03010(16) 0.03443(17) 0.03493(17) 0.00055(12) -0.00239(11) 0.00441(12)
Cl1 0.0439(5) 0.0380(5) 0.0520(6) -0.0010(4) -0.0070(4) 0.0032(4)
Cl2 0.0531(6) 0.0683(8) 0.0728(8) -0.0064(6) 0.0190(6) 0.0017(6)
N1 0.0430(19) 0.050(2) 0.0483(19) 0.0103(16) 0.0060(15) 0.0178(16)
N2 0.0343(16) 0.0401(18) 0.0404(17) 0.0041(14) -0.0014(13) 0.0042(13)
N3 0.0405(18) 0.0389(17) 0.0355(17) -0.0027(13) -0.0020(13) 0.0033(13)
N4 0.0441(17) 0.0343(16) 0.0351(16) -0.0009(13) -0.0009(13) -0.0019(13)
N5 0.0324(15) 0.0334(16) 0.0423(17) -0.0026(13) -0.0018(13) 0.0010(12)
N6 0.0384(17) 0.0396(17) 0.0386(17) -0.0013(14) 0.0011(14) 0.0079(14)
C1 0.065(3) 0.063(3) 0.082(4) 0.009(3) 0.024(3) 0.033(3)
C2 0.034(2) 0.056(2) 0.040(2) 0.0121(18) -0.0020(16) 0.0017(17)
C3 0.043(2) 0.057(3) 0.067(3) 0.007(2) -0.003(2) -0.003(2)
C4 0.049(3) 0.080(4) 0.077(4) 0.009(3) -0.003(2) -0.019(3)
C5 0.037(2) 0.104(4) 0.067(3) 0.021(3) 0.003(2) -0.003(3)
C6 0.036(2) 0.091(4) 0.058(3) 0.027(3) 0.007(2) 0.010(2)
C7 0.040(2) 0.062(3) 0.041(2) 0.0176(19) 0.0030(17) 0.012(2)
C8 0.040(2) 0.040(2) 0.038(2) 0.0059(16) -0.0004(16) 0.0097(16)
C9 0.048(2) 0.041(2) 0.036(2) -0.0009(16) -0.0027(16) 0.0090(17)
C10 0.061(3) 0.043(2) 0.062(3) -0.003(2) -0.008(2) 0.012(2)
C11 0.082(4) 0.037(3) 0.074(3) -0.006(2) -0.013(3) -0.003(2)
C12 0.057(3) 0.047(3) 0.064(3) -0.007(2) -0.008(2) -0.010(2)
C13 0.047(2) 0.042(2) 0.051(2) -0.0066(19) -0.0100(19) 0.0008(19)
C14 0.057(3) 0.047(2) 0.044(2) 0.0030(19) -0.005(2) -0.003(2)
C15 0.079(4) 0.068(3) 0.045(3) 0.013(2) -0.009(2) -0.007(3)
C16 0.084(4) 0.071(3) 0.048(3) 0.002(2) 0.012(3) -0.017(3)
C17 0.060(3) 0.055(3) 0.054(3) -0.001(2) 0.011(2) -0.013(2)
C18 0.042(2) 0.036(2) 0.047(2) -0.0051(16) 0.0037(17) -0.0073(16)
C19 0.037(2) 0.037(2) 0.051(2) -0.0037(17) 0.0040(17) -0.0048(16)
C20 0.035(2) 0.058(3) 0.071(3) -0.002(2) 0.012(2) 0.0003(19)
C21 0.030(2) 0.064(3) 0.089(4) 0.001(3) 0.000(2) 0.005(2)
C22 0.038(2) 0.046(2) 0.064(3) 0.001(2) -0.014(2) 0.0032(18)
C23 0.040(2) 0.0309(19) 0.046(2) -0.0040(16) -0.0107(17) 0.0005(15)
C24 0.038(2) 0.0338(19) 0.041(2) -0.0027(16) -0.0053(16) 0.0041(15)
C25 0.059(3) 0.041(2) 0.047(2) -0.0003(18) -0.017(2) 0.004(2)
C26 0.079(3) 0.065(3) 0.034(2) 0.003(2) 0.000(2) 0.012(3)
C27 0.071(3) 0.075(3) 0.051(3) 0.008(2) 0.016(2) 0.022(3)
C28 0.053(3) 0.065(3) 0.046(2) 0.006(2) 0.005(2) 0.017(2)
O1 0.166(7) 0.098(5) 0.518(18) 0.002(8) 0.025(9) 0.011(5)
O2 0.114(4) 0.363(11) 0.094(4) -0.025(5) 0.029(3) 0.089(6)
O3 0.193(7) 0.457(16) 0.080(4) 0.004(6) -0.005(4) -0.008(9)
O4 0.090(4) 0.186(7) 0.311(10) 0.096(6) -0.043(5) -0.050(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'
O O 0.0106 0.0060 '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'
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
N5 Ru N6 80.08(12) . . ?
N5 Ru N3 98.09(12) . . ?
N6 Ru N3 95.55(12) . . ?
N5 Ru N4 79.64(12) . . ?
N6 Ru N4 159.69(12) . . ?
N3 Ru N4 86.32(12) . . ?
N5 Ru N2 174.37(12) . . ?
N6 Ru N2 96.45(12) . . ?
N3 Ru N2 77.74(12) . . ?
N4 Ru N2 103.69(12) . . ?
N5 Ru Cl1 87.49(9) . . ?
N6 Ru Cl1 88.89(9) . . ?
N3 Ru Cl1 173.38(9) . . ?
N4 Ru Cl1 91.21(9) . . ?
N2 Ru Cl1 96.92(9) . . ?
O2 Cl2 O3 108.8(5) . . ?
O2 Cl2 O1 105.6(6) . . ?
O3 Cl2 O1 112.9(7) . . ?
O2 Cl2 O4 114.5(6) . . ?
O3 Cl2 O4 112.1(5) . . ?
O1 Cl2 O4 102.8(5) . . ?
C8 N1 C7 106.8(3) . . ?
C8 N1 C1 128.1(4) . . ?
C7 N1 C1 125.2(4) . . ?
C8 N2 C2 106.3(3) . . ?
C8 N2 Ru 113.8(2) . . ?
C2 N2 Ru 138.9(3) . . ?
C13 N3 C9 118.0(3) . . ?
C13 N3 Ru 124.5(3) . . ?
C9 N3 Ru 117.0(3) . . ?
C14 N4 C18 118.4(3) . . ?
C14 N4 Ru 128.6(3) . . ?
C18 N4 Ru 113.0(2) . . ?
C23 N5 C19 121.5(3) . . ?
C23 N5 Ru 118.7(3) . . ?
C19 N5 Ru 119.6(3) . . ?
C28 N6 C24 117.9(3) . . ?
C28 N6 Ru 128.8(3) . . ?
C24 N6 Ru 113.3(2) . . ?
N1 C1 H1 111(3) . . ?
N1 C1 H1B 102(3) . . ?
H1 C1 H1B 107(4) . . ?
N1 C1 H1A 108(3) . . ?
H1 C1 H1A 116(4) . . ?
H1B C1 H1A 112(4) . . ?
C3 C2 C7 121.1(4) . . ?
C3 C2 N2 131.0(4) . . ?
C7 C2 N2 107.9(4) . . ?
C4 C3 C2 116.7(5) . . ?
C4 C3 H9 123(3) . . ?
C2 C3 H9 120(3) . . ?
C3 C4 C5 122.0(6) . . ?
C3 C4 H4 115(3) . . ?
C5 C4 H4 122(3) . . ?
C6 C5 C4 121.7(5) . . ?
C6 C5 H5 119(3) . . ?
C4 C5 H5 119(3) . . ?
C5 C6 C7 117.2(5) . . ?
C5 C6 H6 121(3) . . ?
C7 C6 H6 122(3) . . ?
N1 C7 C2 107.1(3) . . ?
N1 C7 C6 131.6(4) . . ?
C2 C7 C6 121.2(5) . . ?
N2 C8 N1 112.0(3) . . ?
N2 C8 C9 118.1(3) . . ?
N1 C8 C9 129.9(4) . . ?
N3 C9 C10 120.7(4) . . ?
N3 C9 C8 112.5(3) . . ?
C10 C9 C8 126.7(4) . . ?
C11 C10 C9 120.0(4) . . ?
C11 C10 H10 124(3) . . ?
C9 C10 H10 116(3) . . ?
C10 C11 C12 119.5(4) . . ?
C10 C11 H11 120(4) . . ?
C12 C11 H11 120(4) . . ?
C11 C12 C13 118.4(4) . . ?
C11 C12 H12 124(3) . . ?
C13 C12 H12 117(3) . . ?
N3 C13 C12 123.3(4) . . ?
N3 C13 H13 117(3) . . ?
C12 C13 H13 120(3) . . ?
N4 C14 C15 122.4(5) . . ?
N4 C14 H14 118(3) . . ?
C15 C14 H14 120(3) . . ?
C14 C15 C16 119.5(5) . . ?
C14 C15 H15 116(3) . . ?
C16 C15 H15 125(3) . . ?
C17 C16 C15 118.6(5) . . ?
C17 C16 H16 125(4) . . ?
C15 C16 H16 116(4) . . ?
C16 C17 C18 119.9(5) . . ?
C16 C17 H17 121(3) . . ?
C18 C17 H17 119(3) . . ?
N4 C18 C17 121.2(4) . . ?
N4 C18 C19 115.5(3) . . ?
C17 C18 C19 123.4(4) . . ?
N5 C19 C20 119.8(4) . . ?
N5 C19 C18 112.1(3) . . ?
C20 C19 C18 128.0(4) . . ?
C21 C20 C19 119.1(4) . . ?
C21 C20 H20 119(3) . . ?
C19 C20 H20 121(3) . . ?
C22 C21 C20 120.6(4) . . ?
C22 C21 H21 120(3) . . ?
C20 C21 H21 119(3) . . ?
C21 C22 C23 118.9(4) . . ?
C21 C22 H22 121(2) . . ?
C23 C22 H22 120(2) . . ?
N5 C23 C22 120.1(4) . . ?
N5 C23 C24 113.2(3) . . ?
C22 C23 C24 126.7(4) . . ?
N6 C24 C25 121.2(4) . . ?
N6 C24 C23 114.7(3) . . ?
C25 C24 C23 124.1(4) . . ?
C26 C25 C24 119.6(4) . . ?
C26 C25 H25 118(3) . . ?
C24 C25 H25 122(3) . . ?
C25 C26 C27 119.6(4) . . ?
C25 C26 H26 122(3) . . ?
C27 C26 H26 118(3) . . ?
C28 C27 C26 118.5(5) . . ?
C28 C27 H27 124(3) . . ?
C26 C27 H27 117(3) . . ?
N6 C28 C27 123.2(4) . . ?
N6 C28 H28 116(4) . . ?
C27 C28 H28 120(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
Ru N5 1.945(3) . ?
Ru N6 2.058(3) . ?
Ru N3 2.060(3) . ?
Ru N4 2.066(3) . ?
Ru N2 2.099(3) . ?
Ru Cl1 2.4229(10) . ?
Cl2 O2 1.323(5) . ?
Cl2 O3 1.347(7) . ?
Cl2 O1 1.355(8) . ?
Cl2 O4 1.358(5) . ?
N1 C8 1.358(5) . ?
N1 C7 1.378(6) . ?
N1 C1 1.460(6) . ?
N2 C8 1.330(5) . ?
N2 C2 1.395(5) . ?
N3 C13 1.335(5) . ?
N3 C9 1.363(5) . ?
N4 C14 1.341(5) . ?
N4 C18 1.368(5) . ?
N5 C23 1.352(5) . ?
N5 C19 1.353(5) . ?
N6 C28 1.343(5) . ?
N6 C24 1.371(5) . ?
C1 H1 1.06(5) . ?
C1 H1B 0.91(5) . ?
C1 H1A 1.06(6) . ?
C2 C3 1.385(6) . ?
C2 C7 1.393(6) . ?
C3 C4 1.383(7) . ?
C3 H9 0.86(4) . ?
C4 C5 1.391(8) . ?
C4 H4 0.87(5) . ?
C5 C6 1.352(8) . ?
C5 H5 1.01(6) . ?
C6 C7 1.404(6) . ?
C6 H6 0.96(5) . ?
C8 C9 1.451(5) . ?
C9 C10 1.382(6) . ?
C10 C11 1.367(7) . ?
C10 H10 0.92(5) . ?
C11 C12 1.368(7) . ?
C11 H11 0.90(7) . ?
C12 C13 1.377(6) . ?
C12 H12 0.98(5) . ?
C13 H13 0.90(4) . ?
C14 C15 1.379(6) . ?
C14 H14 0.89(4) . ?
C15 C16 1.388(8) . ?
C15 H15 0.96(6) . ?
C16 C17 1.373(7) . ?
C16 H16 1.05(7) . ?
C17 C18 1.389(6) . ?
C17 H17 1.01(5) . ?
C18 C19 1.471(6) . ?
C19 C20 1.382(6) . ?
C20 C21 1.380(7) . ?
C20 H20 0.84(4) . ?
C21 C22 1.376(7) . ?
C21 H21 0.93(5) . ?
C22 C23 1.383(5) . ?
C22 H22 0.94(4) . ?
C23 C24 1.471(5) . ?
C24 C25 1.380(5) . ?
C25 C26 1.377(7) . ?
C25 H25 0.92(5) . ?
C26 C27 1.377(7) . ?
C26 H26 0.89(4) . ?
C27 C28 1.375(6) . ?
C27 H27 1.04(6) . ?
C28 H28 0.90(6) . ?
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 Ru N2 C8 -39.5(13) . . . . ?
N6 Ru N2 C8 -91.2(3) . . . . ?
N3 Ru N2 C8 3.1(3) . . . . ?
N4 Ru N2 C8 86.2(3) . . . . ?
Cl1 Ru N2 C8 179.1(2) . . . . ?
N5 Ru N2 C2 127.2(12) . . . . ?
N6 Ru N2 C2 75.5(4) . . . . ?
N3 Ru N2 C2 169.8(4) . . . . ?
N4 Ru N2 C2 -107.1(4) . . . . ?
Cl1 Ru N2 C2 -14.2(4) . . . . ?
N5 Ru N3 C13 -9.7(3) . . . . ?
N6 Ru N3 C13 -90.4(3) . . . . ?
N4 Ru N3 C13 69.3(3) . . . . ?
N2 Ru N3 C13 174.2(3) . . . . ?
Cl1 Ru N3 C13 137.6(7) . . . . ?
N5 Ru N3 C9 179.0(3) . . . . ?
N6 Ru N3 C9 98.3(3) . . . . ?
N4 Ru N3 C9 -102.0(3) . . . . ?
N2 Ru N3 C9 2.9(3) . . . . ?
Cl1 Ru N3 C9 -33.7(9) . . . . ?
N5 Ru N4 C14 176.0(4) . . . . ?
N6 Ru N4 C14 173.2(3) . . . . ?
N3 Ru N4 C14 77.1(3) . . . . ?
N2 Ru N4 C14 0.7(4) . . . . ?
Cl1 Ru N4 C14 -96.7(3) . . . . ?
N5 Ru N4 C18 -1.9(2) . . . . ?
N6 Ru N4 C18 -4.7(5) . . . . ?
N3 Ru N4 C18 -100.8(3) . . . . ?
N2 Ru N4 C18 -177.2(2) . . . . ?
Cl1 Ru N4 C18 85.3(2) . . . . ?
N6 Ru N5 C23 -2.4(3) . . . . ?
N3 Ru N5 C23 -96.7(3) . . . . ?
N4 Ru N5 C23 178.6(3) . . . . ?
N2 Ru N5 C23 -54.8(13) . . . . ?
Cl1 Ru N5 C23 86.9(3) . . . . ?
N6 Ru N5 C19 -178.0(3) . . . . ?
N3 Ru N5 C19 87.7(3) . . . . ?
N4 Ru N5 C19 3.0(3) . . . . ?
N2 Ru N5 C19 129.6(12) . . . . ?
Cl1 Ru N5 C19 -88.7(3) . . . . ?
N5 Ru N6 C28 -179.7(4) . . . . ?
N3 Ru N6 C28 -82.4(4) . . . . ?
N4 Ru N6 C28 -176.8(4) . . . . ?
N2 Ru N6 C28 -4.1(4) . . . . ?
Cl1 Ru N6 C28 92.7(4) . . . . ?
N5 Ru N6 C24 1.9(2) . . . . ?
N3 Ru N6 C24 99.1(3) . . . . ?
N4 Ru N6 C24 4.7(5) . . . . ?
N2 Ru N6 C24 177.4(3) . . . . ?
Cl1 Ru N6 C24 -85.8(2) . . . . ?
C8 N2 C2 C3 -178.7(4) . . . . ?
Ru N2 C2 C3 14.0(7) . . . . ?
C8 N2 C2 C7 -0.1(4) . . . . ?
Ru N2 C2 C7 -167.4(3) . . . . ?
C7 C2 C3 C4 -0.1(7) . . . . ?
N2 C2 C3 C4 178.4(4) . . . . ?
C2 C3 C4 C5 -0.9(8) . . . . ?
C3 C4 C5 C6 1.8(8) . . . . ?
C4 C5 C6 C7 -1.6(7) . . . . ?
C8 N1 C7 C2 -0.5(4) . . . . ?
C1 N1 C7 C2 179.4(4) . . . . ?
C8 N1 C7 C6 178.4(4) . . . . ?
C1 N1 C7 C6 -1.7(7) . . . . ?
C3 C2 C7 N1 179.2(4) . . . . ?
N2 C2 C7 N1 0.3(4) . . . . ?
C3 C2 C7 C6 0.2(6) . . . . ?
N2 C2 C7 C6 -178.7(4) . . . . ?
C5 C6 C7 N1 -178.0(4) . . . . ?
C5 C6 C7 C2 0.7(6) . . . . ?
C2 N2 C8 N1 -0.3(4) . . . . ?
Ru N2 C8 N1 170.7(2) . . . . ?
C2 N2 C8 C9 -179.4(3) . . . . ?
Ru N2 C8 C9 -8.4(4) . . . . ?
C7 N1 C8 N2 0.5(4) . . . . ?
C1 N1 C8 N2 -179.4(4) . . . . ?
C7 N1 C8 C9 179.5(4) . . . . ?
C1 N1 C8 C9 -0.5(7) . . . . ?
C13 N3 C9 C10 -1.7(6) . . . . ?
Ru N3 C9 C10 170.1(3) . . . . ?
C13 N3 C9 C8 -179.6(3) . . . . ?
Ru N3 C9 C8 -7.8(4) . . . . ?
N2 C8 C9 N3 10.8(5) . . . . ?
N1 C8 C9 N3 -168.2(4) . . . . ?
N2 C8 C9 C10 -167.0(4) . . . . ?
N1 C8 C9 C10 14.1(7) . . . . ?
N3 C9 C10 C11 0.4(7) . . . . ?
C8 C9 C10 C11 178.0(4) . . . . ?
C9 C10 C11 C12 0.9(8) . . . . ?
C10 C11 C12 C13 -0.9(8) . . . . ?
C9 N3 C13 C12 1.8(6) . . . . ?
Ru N3 C13 C12 -169.4(3) . . . . ?
C11 C12 C13 N3 -0.5(7) . . . . ?
C18 N4 C14 C15 -1.4(6) . . . . ?
Ru N4 C14 C15 -179.2(3) . . . . ?
N4 C14 C15 C16 -0.6(7) . . . . ?
C14 C15 C16 C17 1.4(8) . . . . ?
C15 C16 C17 C18 -0.2(7) . . . . ?
C14 N4 C18 C17 2.6(5) . . . . ?
Ru N4 C18 C17 -179.3(3) . . . . ?
C14 N4 C18 C19 -177.5(3) . . . . ?
Ru N4 C18 C19 0.7(4) . . . . ?
C16 C17 C18 N4 -1.8(6) . . . . ?
C16 C17 C18 C19 178.3(4) . . . . ?
C23 N5 C19 C20 1.8(6) . . . . ?
Ru N5 C19 C20 177.2(3) . . . . ?
C23 N5 C19 C18 -178.8(3) . . . . ?
Ru N5 C19 C18 -3.4(4) . . . . ?
N4 C18 C19 N5 1.6(5) . . . . ?
C17 C18 C19 N5 -178.4(4) . . . . ?
N4 C18 C19 C20 -179.0(4) . . . . ?
C17 C18 C19 C20 0.9(6) . . . . ?
N5 C19 C20 C21 -1.3(6) . . . . ?
C18 C19 C20 C21 179.4(4) . . . . ?
C19 C20 C21 C22 0.0(7) . . . . ?
C20 C21 C22 C23 1.0(7) . . . . ?
C19 N5 C23 C22 -0.8(5) . . . . ?
Ru N5 C23 C22 -176.2(3) . . . . ?
C19 N5 C23 C24 177.9(3) . . . . ?
Ru N5 C23 C24 2.5(4) . . . . ?
C21 C22 C23 N5 -0.6(6) . . . . ?
C21 C22 C23 C24 -179.1(4) . . . . ?
C28 N6 C24 C25 -0.3(6) . . . . ?
Ru N6 C24 C25 178.4(3) . . . . ?
C28 N6 C24 C23 -179.8(4) . . . . ?
Ru N6 C24 C23 -1.1(4) . . . . ?
N5 C23 C24 N6 -0.7(5) . . . . ?
C22 C23 C24 N6 177.8(4) . . . . ?
N5 C23 C24 C25 179.7(3) . . . . ?
C22 C23 C24 C25 -1.7(6) . . . . ?
N6 C24 C25 C26 -0.9(6) . . . . ?
C23 C24 C25 C26 178.5(4) . . . . ?
C24 C25 C26 C27 0.9(7) . . . . ?
C25 C26 C27 C28 0.2(8) . . . . ?
C24 N6 C28 C27 1.5(7) . . . . ?
Ru N6 C28 C27 -176.9(4) . . . . ?
C26 C27 C28 N6 -1.5(8) . . . . ?
|
1100940.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100940.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_1100940
loop_
_publ_author_name
'Nripen Chanda'
'Debamita Paul'
'Sanjib Kar'
'Shaikh M. Mobin'
'Anindya Datta'
'Vedavati G. Puranik'
'K. Krishnamurthy Rao'
'Goutam Kumar Lahiri'
_publ_section_title
;
Effect of 2-(2-Pyridyl)azole-Based Ancillary Ligands (L1-4) on the
Electrophilicity of the Nitrosyl Function in [RuII(trpy)(L1-4)(NO)]3+ [trpy
= 2,2':6',2''-Terpyridine]. Synthesis, Structures, and
Spectroscopic, Electrochemical, and Kinetic Aspects
;
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3499
_journal_page_last 3511
_journal_paper_doi 10.1021/ic048184w
_journal_volume 44
_journal_year 2005
_chemical_formula_sum 'C28 H22 Cl N7 O6 Ru'
_chemical_formula_weight 689.05
_chemical_name_systematic
;
?
;
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2yab'
_symmetry_space_group_name_H-M 'P 1 21/a 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.000(6)
_cell_angle_beta 101.520(6)
_cell_angle_gamma 90.000(6)
_cell_formula_units_Z 4
_cell_length_a 13.7020(8)
_cell_length_b 13.8050(11)
_cell_length_c 15.1960(12)
_cell_measurement_reflns_used 25
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 12.5600
_cell_measurement_theta_min 5.2000
_cell_volume 2816.5(4)
_computing_cell_refinement 'Argus (Nonius, MACH3 software)'
_computing_data_collection 'Argus (Nonius, MACH3 software)'
_computing_data_reduction 'Maxus (Nonius software)'
_computing_molecular_graphics Ortep
_computing_publication_material Shelx97
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 293(2)
_diffrn_measured_fraction_theta_full 0.835
_diffrn_measured_fraction_theta_max 0.835
_diffrn_measurement_device_type 'Enraf-Nonius CAD-4'
_diffrn_measurement_method \w/q-scan
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type ' MoK\a'
_diffrn_radiation_wavelength 0.70930
_diffrn_reflns_av_R_equivalents 0.0000
_diffrn_reflns_av_sigmaI/netI 0.0317
_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 17
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_number 4345
_diffrn_reflns_theta_full 24.96
_diffrn_reflns_theta_max 24.96
_diffrn_reflns_theta_min 1.36
_diffrn_standards_decay_% <3%
_diffrn_standards_interval_time 3600
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 0.708
_exptl_absorpt_correction_T_max 1.000
_exptl_absorpt_correction_T_min 0.974
_exptl_absorpt_correction_type psi-scan
_exptl_absorpt_process_details
;
psi-scan (North, Philips & Mathews, 1968)
;
_exptl_crystal_colour Dark_Black
_exptl_crystal_density_diffrn 1.625
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description Block
_exptl_crystal_F_000 1392
_exptl_crystal_size_max 0.275
_exptl_crystal_size_mid 0.20
_exptl_crystal_size_min 0.15
_refine_diff_density_max 0.534
_refine_diff_density_min -0.390
_refine_diff_density_rms 0.071
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.065
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 476
_refine_ls_number_reflns 4345
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.065
_refine_ls_R_factor_all 0.0428
_refine_ls_R_factor_gt 0.0330
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0376P)^2^+3.2775P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0757
_refine_ls_wR_factor_ref 0.0817
_reflns_number_gt 3799
_reflns_number_total 4345
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file ic048184wsi20041223_113133.cif
_cod_data_source_block max
_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:
'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0376P)^2^+3.2775P] 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^)+(0.0376P)^2^+3.2775P] 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 'P 21/a'
_cod_database_code 1100940
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru Ru 0.63636(2) 0.03744(2) 0.294154(18) 0.02487(10) Uani 1 d . . .
Cl Cl 0.69023(10) 0.58814(10) 0.04929(12) 0.0747(4) Uani 1 d . . .
N1 N 0.8535(2) -0.0967(2) 0.1792(2) 0.0392(8) Uani 1 d . . .
N2 N 0.7722(2) -0.0114(2) 0.26628(19) 0.0277(6) Uani 1 d . . .
N3 N 0.5916(2) -0.0406(2) 0.17493(19) 0.0289(6) Uani 1 d . . .
N4 N 0.6204(2) 0.1672(2) 0.22528(19) 0.0292(6) Uani 1 d . . .
N5 N 0.5048(2) 0.0776(2) 0.31262(19) 0.0277(6) Uani 1 d . . .
N6 N 0.5980(2) -0.0813(2) 0.36488(19) 0.0314(7) Uani 1 d . . .
N7 N 0.6912(2) 0.1081(2) 0.4111(2) 0.0331(7) Uani 1 d . . .
O1 O 0.6724(2) 0.1952(2) 0.42173(19) 0.0501(7) Uani 1 d . . .
O2 O 0.7410(2) 0.0636(2) 0.47684(17) 0.0454(7) Uani 1 d . . .
O3 O 0.7453(4) 0.5022(3) 0.0599(4) 0.131(2) Uani 1 d . . .
O4 O 0.7263(6) 0.6399(5) 0.1353(4) 0.177(3) Uani 1 d . . .
O5 O 0.7148(3) 0.6508(3) -0.0135(3) 0.1039(15) Uani 1 d . . .
O6 O 0.5920(3) 0.5761(4) 0.0470(4) 0.137(2) Uani 1 d . . .
C1 C 0.8784(4) -0.1575(6) 0.1077(5) 0.0733(19) Uani 1 d . . .
C2 C 0.9248(3) -0.0574(3) 0.2467(3) 0.0346(9) Uani 1 d . . .
C3 C 1.0287(3) -0.0640(3) 0.2643(3) 0.0442(10) Uani 1 d . . .
C4 C 1.0783(3) -0.0146(3) 0.3381(3) 0.0474(11) Uani 1 d . . .
C5 C 1.0283(3) 0.0386(4) 0.3936(3) 0.0503(11) Uani 1 d . . .
C6 C 0.9260(3) 0.0446(3) 0.3766(3) 0.0415(9) Uani 1 d . . .
C7 C 0.8739(3) -0.0044(3) 0.3016(2) 0.0303(8) Uani 1 d . . .
C8 C 0.7637(3) -0.0668(3) 0.1935(2) 0.0323(8) Uani 1 d . . .
C9 C 0.6641(3) -0.0857(3) 0.1401(2) 0.0331(8) Uani 1 d . . .
C10 C 0.6413(3) -0.1419(3) 0.0640(3) 0.0478(11) Uani 1 d . . .
C11 C 0.5432(3) -0.1524(3) 0.0209(3) 0.0512(12) Uani 1 d . . .
C12 C 0.4702(3) -0.1069(3) 0.0547(3) 0.0440(10) Uani 1 d . . .
C13 C 0.4970(3) -0.0517(3) 0.1314(3) 0.0373(9) Uani 1 d . . .
C14 C 0.6795(3) 0.2059(3) 0.1745(3) 0.0376(9) Uani 1 d . . .
C15 C 0.6629(4) 0.2960(3) 0.1351(3) 0.0487(11) Uani 1 d . . .
C16 C 0.5803(4) 0.3477(3) 0.1458(3) 0.0526(12) Uani 1 d . . .
C17 C 0.5170(4) 0.3077(3) 0.1953(3) 0.0453(10) Uani 1 d . . .
C18 C 0.5374(3) 0.2178(3) 0.2351(2) 0.0317(8) Uani 1 d . . .
C19 C 0.4724(3) 0.1673(3) 0.2866(2) 0.0315(8) Uani 1 d . . .
C20 C 0.3846(3) 0.2009(3) 0.3076(3) 0.0426(10) Uani 1 d . . .
C21 C 0.3305(3) 0.1414(3) 0.3530(3) 0.0479(11) Uani 1 d . . .
C22 C 0.3650(3) 0.0500(3) 0.3786(3) 0.0427(10) Uani 1 d . . .
C23 C 0.4539(3) 0.0188(3) 0.3581(2) 0.0309(8) Uani 1 d . . .
C24 C 0.5047(3) -0.0741(3) 0.3833(2) 0.0319(8) Uani 1 d . . .
C25 C 0.4635(3) -0.1501(3) 0.4236(3) 0.0457(10) Uani 1 d . . .
C26 C 0.5176(4) -0.2337(4) 0.4445(3) 0.0591(13) Uani 1 d . . .
C27 C 0.6117(4) -0.2395(3) 0.4288(3) 0.0536(12) Uani 1 d . . .
C28 C 0.6502(3) -0.1629(3) 0.3889(3) 0.0423(10) Uani 1 d . . .
H13 H 0.450(3) -0.024(3) 0.156(2) 0.027(10) Uiso 1 d . . .
H28 H 0.721(3) -0.165(3) 0.378(3) 0.041(11) Uiso 1 d . . .
H21 H 0.270(3) 0.162(3) 0.366(3) 0.050(12) Uiso 1 d . . .
H20 H 0.364(3) 0.261(3) 0.289(3) 0.045(12) Uiso 1 d . . .
H11 H 0.528(3) -0.188(3) -0.029(3) 0.051(13) Uiso 1 d . . .
H25 H 0.398(3) -0.146(3) 0.433(3) 0.046(12) Uiso 1 d . . .
H6 H 0.898(3) 0.078(3) 0.414(3) 0.050(13) Uiso 1 d . . .
H16 H 0.571(3) 0.409(3) 0.121(3) 0.057(13) Uiso 1 d . . .
H12 H 0.400(3) -0.115(3) 0.029(3) 0.060(13) Uiso 1 d . . .
H5 H 1.062(3) 0.068(3) 0.440(3) 0.051(13) Uiso 1 d . . .
H10 H 0.686(3) -0.169(3) 0.041(3) 0.045(12) Uiso 1 d . . .
H3 H 1.062(3) -0.097(3) 0.219(3) 0.056(13) Uiso 1 d . . .
H14 H 0.727(3) 0.171(3) 0.169(3) 0.041(13) Uiso 1 d . . .
H1 H 0.846(4) -0.213(4) 0.100(4) 0.09(2) Uiso 1 d . . .
H4 H 1.148(3) -0.018(3) 0.353(3) 0.060(13) Uiso 1 d . . .
H17 H 0.465(3) 0.335(3) 0.202(3) 0.045(13) Uiso 1 d . . .
H22 H 0.331(3) 0.016(3) 0.410(3) 0.061(15) Uiso 1 d . . .
H27 H 0.652(4) -0.293(4) 0.444(3) 0.068(15) Uiso 1 d . . .
H1A H 0.944(5) -0.160(5) 0.108(4) 0.12(2) Uiso 1 d . . .
H26 H 0.492(4) -0.287(4) 0.467(4) 0.087(18) Uiso 1 d . . .
H15 H 0.710(4) 0.316(4) 0.102(4) 0.084(18) Uiso 1 d . . .
H1B H 0.851(6) -0.128(6) 0.050(6) 0.15(4) Uiso 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
Ru 0.02347(15) 0.02607(15) 0.02635(15) -0.00023(13) 0.00807(10) -0.00064(12)
Cl 0.0578(8) 0.0541(8) 0.1240(13) 0.0174(8) 0.0463(8) -0.0023(6)
N1 0.0299(17) 0.044(2) 0.0461(19) -0.0160(15) 0.0136(15) 0.0011(15)
N2 0.0269(15) 0.0283(16) 0.0283(15) -0.0017(12) 0.0068(12) -0.0026(12)
N3 0.0265(15) 0.0290(15) 0.0308(15) -0.0006(13) 0.0052(12) -0.0032(13)
N4 0.0337(16) 0.0288(16) 0.0261(15) -0.0033(12) 0.0083(13) -0.0063(13)
N5 0.0254(15) 0.0304(15) 0.0278(15) -0.0006(12) 0.0069(12) -0.0003(12)
N6 0.0332(17) 0.0306(16) 0.0302(16) 0.0014(13) 0.0060(13) 0.0001(13)
N7 0.0282(16) 0.0423(19) 0.0317(16) -0.0013(15) 0.0130(13) -0.0090(14)
O1 0.066(2) 0.0370(17) 0.0474(17) -0.0125(13) 0.0124(15) -0.0053(15)
O2 0.0466(16) 0.0583(19) 0.0294(14) 0.0060(13) 0.0027(13) -0.0048(14)
O3 0.093(3) 0.069(3) 0.240(7) 0.036(4) 0.057(4) 0.020(3)
O4 0.232(8) 0.163(6) 0.131(5) -0.013(5) 0.029(5) -0.031(6)
O5 0.119(4) 0.094(3) 0.121(4) 0.029(3) 0.078(3) 0.003(3)
O6 0.060(3) 0.158(5) 0.206(6) 0.079(4) 0.059(3) 0.009(3)
C1 0.041(3) 0.091(5) 0.093(5) -0.055(4) 0.025(3) -0.004(3)
C2 0.0284(19) 0.033(2) 0.044(2) 0.0014(16) 0.0115(16) 0.0009(15)
C3 0.033(2) 0.046(3) 0.057(3) 0.005(2) 0.015(2) 0.0054(18)
C4 0.027(2) 0.059(3) 0.055(3) 0.008(2) 0.0046(19) -0.002(2)
C5 0.035(2) 0.071(3) 0.042(2) -0.004(2) 0.0005(19) -0.009(2)
C6 0.033(2) 0.057(3) 0.034(2) -0.008(2) 0.0070(17) -0.006(2)
C7 0.0251(18) 0.0353(19) 0.0310(18) 0.0034(16) 0.0067(15) -0.0001(15)
C8 0.0274(19) 0.033(2) 0.037(2) -0.0060(16) 0.0098(16) -0.0007(15)
C9 0.0305(19) 0.033(2) 0.036(2) -0.0031(16) 0.0083(16) -0.0016(16)
C10 0.041(2) 0.055(3) 0.049(3) -0.021(2) 0.013(2) -0.003(2)
C11 0.050(3) 0.057(3) 0.044(3) -0.020(2) 0.004(2) -0.012(2)
C12 0.037(2) 0.052(3) 0.041(2) -0.007(2) 0.0025(18) -0.010(2)
C13 0.033(2) 0.040(2) 0.040(2) -0.0017(18) 0.0097(17) -0.0012(18)
C14 0.042(2) 0.042(2) 0.031(2) -0.0035(17) 0.0122(18) -0.008(2)
C15 0.065(3) 0.048(3) 0.034(2) 0.0069(19) 0.010(2) -0.015(2)
C16 0.086(4) 0.033(2) 0.038(2) 0.0061(19) 0.011(2) -0.007(2)
C17 0.060(3) 0.033(2) 0.043(2) 0.0001(19) 0.011(2) 0.008(2)
C18 0.039(2) 0.0272(19) 0.0284(18) 0.0025(15) 0.0052(16) 0.0001(16)
C19 0.0331(19) 0.0299(19) 0.0315(19) -0.0014(16) 0.0065(16) 0.0036(16)
C20 0.037(2) 0.041(2) 0.049(2) 0.002(2) 0.0081(19) 0.0127(19)
C21 0.031(2) 0.060(3) 0.056(3) 0.000(2) 0.017(2) 0.012(2)
C22 0.029(2) 0.057(3) 0.046(2) 0.004(2) 0.0151(18) -0.0015(19)
C23 0.0280(18) 0.033(2) 0.0309(19) 0.0021(15) 0.0046(15) -0.0045(15)
C24 0.031(2) 0.035(2) 0.0298(19) 0.0009(16) 0.0059(15) -0.0055(16)
C25 0.045(3) 0.044(3) 0.050(3) 0.012(2) 0.015(2) -0.009(2)
C26 0.072(3) 0.044(3) 0.062(3) 0.018(2) 0.015(3) -0.014(3)
C27 0.066(3) 0.034(2) 0.058(3) 0.012(2) 0.007(2) 0.003(2)
C28 0.044(2) 0.036(2) 0.046(2) 0.0014(19) 0.007(2) 0.0055(19)
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'
O O 0.0106 0.0060 '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'
Ru Ru -1.2594 0.8363 '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
N5 Ru N7 85.94(12) . . ?
N5 Ru N4 79.60(12) . . ?
N7 Ru N4 90.58(12) . . ?
N5 Ru N6 79.32(12) . . ?
N7 Ru N6 90.79(12) . . ?
N4 Ru N6 158.73(11) . . ?
N5 Ru N3 98.68(11) . . ?
N7 Ru N3 175.23(11) . . ?
N4 Ru N3 91.42(11) . . ?
N6 Ru N3 88.91(11) . . ?
N5 Ru N2 175.85(11) . . ?
N7 Ru N2 98.19(11) . . ?
N4 Ru N2 100.67(11) . . ?
N6 Ru N2 100.14(11) . . ?
N3 Ru N2 77.18(11) . . ?
O6 Cl O5 116.1(3) . . ?
O6 Cl O3 114.3(3) . . ?
O5 Cl O3 114.3(3) . . ?
O6 Cl O4 103.7(4) . . ?
O5 Cl O4 102.8(3) . . ?
O3 Cl O4 103.2(4) . . ?
C8 N1 C2 107.0(3) . . ?
C8 N1 C1 130.2(4) . . ?
C2 N1 C1 122.7(4) . . ?
C8 N2 C7 106.0(3) . . ?
C8 N2 Ru 114.7(2) . . ?
C7 N2 Ru 139.3(2) . . ?
C13 N3 C9 117.6(3) . . ?
C13 N3 Ru 125.0(3) . . ?
C9 N3 Ru 117.4(2) . . ?
C14 N4 C18 118.2(3) . . ?
C14 N4 Ru 128.6(3) . . ?
C18 N4 Ru 113.2(2) . . ?
C19 N5 C23 122.0(3) . . ?
C19 N5 Ru 118.5(2) . . ?
C23 N5 Ru 119.2(2) . . ?
C28 N6 C24 118.3(3) . . ?
C28 N6 Ru 128.5(3) . . ?
C24 N6 Ru 113.0(2) . . ?
O1 N7 O2 117.6(3) . . ?
O1 N7 Ru 121.7(2) . . ?
O2 N7 Ru 120.6(3) . . ?
N1 C1 H1 114(4) . . ?
N1 C1 H1A 114(4) . . ?
H1 C1 H1A 116(6) . . ?
N1 C1 H1B 108(5) . . ?
H1 C1 H1B 99(6) . . ?
H1A C1 H1B 104(6) . . ?
N1 C2 C7 106.6(3) . . ?
N1 C2 C3 131.3(4) . . ?
C7 C2 C3 122.1(4) . . ?
C4 C3 C2 116.4(4) . . ?
C4 C3 H3 124(3) . . ?
C2 C3 H3 119(3) . . ?
C3 C4 C5 122.1(4) . . ?
C3 C4 H4 119(3) . . ?
C5 C4 H4 119(3) . . ?
C6 C5 C4 121.6(4) . . ?
C6 C5 H5 118(3) . . ?
C4 C5 H5 120(3) . . ?
C5 C6 C7 117.4(4) . . ?
C5 C6 H6 118(3) . . ?
C7 C6 H6 124(3) . . ?
N2 C7 C6 131.2(3) . . ?
N2 C7 C2 108.3(3) . . ?
C6 C7 C2 120.5(3) . . ?
N2 C8 N1 112.1(3) . . ?
N2 C8 C9 118.7(3) . . ?
N1 C8 C9 129.2(3) . . ?
N3 C9 C10 121.4(3) . . ?
N3 C9 C8 112.0(3) . . ?
C10 C9 C8 126.6(4) . . ?
C9 C10 C11 119.7(4) . . ?
C9 C10 H10 122(3) . . ?
C11 C10 H10 118(3) . . ?
C12 C11 C10 119.3(4) . . ?
C12 C11 H11 121(3) . . ?
C10 C11 H11 120(3) . . ?
C11 C12 C13 118.7(4) . . ?
C11 C12 H12 123(3) . . ?
C13 C12 H12 118(3) . . ?
N3 C13 C12 123.2(4) . . ?
N3 C13 H13 117(2) . . ?
C12 C13 H13 120(2) . . ?
N4 C14 C15 123.0(4) . . ?
N4 C14 H14 114(3) . . ?
C15 C14 H14 123(3) . . ?
C16 C15 C14 119.0(4) . . ?
C16 C15 H15 125(3) . . ?
C14 C15 H15 116(3) . . ?
C17 C16 C15 118.8(4) . . ?
C17 C16 H16 123(3) . . ?
C15 C16 H16 118(3) . . ?
C16 C17 C18 120.3(4) . . ?
C16 C17 H17 122(3) . . ?
C18 C17 H17 117(3) . . ?
N4 C18 C17 120.7(4) . . ?
N4 C18 C19 114.8(3) . . ?
C17 C18 C19 124.4(4) . . ?
N5 C19 C20 119.4(3) . . ?
N5 C19 C18 113.1(3) . . ?
C20 C19 C18 127.5(3) . . ?
C21 C20 C19 119.6(4) . . ?
C21 C20 H20 123(3) . . ?
C19 C20 H20 118(3) . . ?
C22 C21 C20 119.9(4) . . ?
C22 C21 H21 120(3) . . ?
C20 C21 H21 121(3) . . ?
C21 C22 C23 119.3(4) . . ?
C21 C22 H22 117(3) . . ?
C23 C22 H22 124(3) . . ?
N5 C23 C22 119.8(3) . . ?
N5 C23 C24 113.1(3) . . ?
C22 C23 C24 127.2(3) . . ?
N6 C24 C25 121.0(4) . . ?
N6 C24 C23 115.1(3) . . ?
C25 C24 C23 124.0(3) . . ?
C26 C25 C24 119.2(4) . . ?
C26 C25 H25 121(3) . . ?
C24 C25 H25 120(3) . . ?
C27 C26 C25 119.7(4) . . ?
C27 C26 H26 118(3) . . ?
C25 C26 H26 123(4) . . ?
C26 C27 C28 119.5(5) . . ?
C26 C27 H27 123(3) . . ?
C28 C27 H27 117(3) . . ?
N6 C28 C27 122.2(4) . . ?
N6 C28 H28 117(2) . . ?
C27 C28 H28 121(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
Ru N5 1.959(3) . ?
Ru N7 2.035(3) . ?
Ru N4 2.064(3) . ?
Ru N6 2.084(3) . ?
Ru N3 2.092(3) . ?
Ru N2 2.101(3) . ?
Cl O6 1.349(4) . ?
Cl O5 1.379(4) . ?
Cl O3 1.398(5) . ?
Cl O4 1.485(6) . ?
N1 C8 1.356(5) . ?
N1 C2 1.379(5) . ?
N1 C1 1.467(6) . ?
N2 C8 1.331(4) . ?
N2 C7 1.393(4) . ?
N3 C13 1.342(5) . ?
N3 C9 1.365(5) . ?
N4 C14 1.337(5) . ?
N4 C18 1.367(5) . ?
N5 C19 1.347(4) . ?
N5 C23 1.347(4) . ?
N6 C28 1.345(5) . ?
N6 C24 1.365(5) . ?
N7 O1 1.247(4) . ?
N7 O2 1.252(4) . ?
C1 H1 0.88(6) . ?
C1 H1A 0.90(7) . ?
C1 H1B 0.97(8) . ?
C2 C7 1.396(5) . ?
C2 C3 1.397(5) . ?
C3 C4 1.372(6) . ?
C3 H3 1.00(4) . ?
C4 C5 1.396(6) . ?
C4 H4 0.94(5) . ?
C5 C6 1.376(6) . ?
C5 H5 0.86(4) . ?
C6 C7 1.394(5) . ?
C6 H6 0.88(4) . ?
C8 C9 1.464(5) . ?
C9 C10 1.376(5) . ?
C10 C11 1.380(6) . ?
C10 H10 0.84(4) . ?
C11 C12 1.365(6) . ?
C11 H11 0.90(4) . ?
C12 C13 1.379(6) . ?
C12 H12 0.97(4) . ?
C13 H13 0.88(4) . ?
C14 C15 1.379(6) . ?
C14 H14 0.82(4) . ?
C15 C16 1.376(7) . ?
C15 H15 0.93(5) . ?
C16 C17 1.372(6) . ?
C16 H16 0.93(5) . ?
C17 C18 1.385(5) . ?
C17 H17 0.84(4) . ?
C18 C19 1.473(5) . ?
C19 C20 1.385(5) . ?
C20 C21 1.382(6) . ?
C20 H20 0.90(4) . ?
C21 C22 1.376(6) . ?
C21 H21 0.93(4) . ?
C22 C23 1.385(5) . ?
C22 H22 0.86(5) . ?
C23 C24 1.472(5) . ?
C24 C25 1.390(5) . ?
C25 C26 1.375(7) . ?
C25 H25 0.93(4) . ?
C26 C27 1.359(7) . ?
C26 H26 0.91(5) . ?
C27 C28 1.377(6) . ?
C27 H27 0.92(5) . ?
C28 H28 1.01(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
N5 Ru N2 C8 2.3(17) . . . . ?
N7 Ru N2 C8 176.8(3) . . . . ?
N4 Ru N2 C8 -91.1(3) . . . . ?
N6 Ru N2 C8 84.5(3) . . . . ?
N3 Ru N2 C8 -2.0(2) . . . . ?
N5 Ru N2 C7 -177.4(14) . . . . ?
N7 Ru N2 C7 -2.9(4) . . . . ?
N4 Ru N2 C7 89.2(4) . . . . ?
N6 Ru N2 C7 -95.2(4) . . . . ?
N3 Ru N2 C7 178.3(4) . . . . ?
N5 Ru N3 C13 0.9(3) . . . . ?
N7 Ru N3 C13 166.4(13) . . . . ?
N4 Ru N3 C13 -78.8(3) . . . . ?
N6 Ru N3 C13 80.0(3) . . . . ?
N2 Ru N3 C13 -179.4(3) . . . . ?
N5 Ru N3 C9 -177.3(3) . . . . ?
N7 Ru N3 C9 -11.8(15) . . . . ?
N4 Ru N3 C9 103.0(3) . . . . ?
N6 Ru N3 C9 -98.3(3) . . . . ?
N2 Ru N3 C9 2.4(3) . . . . ?
N5 Ru N4 C14 -173.5(3) . . . . ?
N7 Ru N4 C14 100.7(3) . . . . ?
N6 Ru N4 C14 -165.6(3) . . . . ?
N3 Ru N4 C14 -74.9(3) . . . . ?
N2 Ru N4 C14 2.3(3) . . . . ?
N5 Ru N4 C18 6.7(2) . . . . ?
N7 Ru N4 C18 -79.1(2) . . . . ?
N6 Ru N4 C18 14.6(4) . . . . ?
N3 Ru N4 C18 105.2(2) . . . . ?
N2 Ru N4 C18 -177.6(2) . . . . ?
N7 Ru N5 C19 82.9(3) . . . . ?
N4 Ru N5 C19 -8.4(3) . . . . ?
N6 Ru N5 C19 174.5(3) . . . . ?
N3 Ru N5 C19 -98.2(3) . . . . ?
N2 Ru N5 C19 -102.5(16) . . . . ?
N7 Ru N5 C23 -90.9(3) . . . . ?
N4 Ru N5 C23 177.7(3) . . . . ?
N6 Ru N5 C23 0.6(3) . . . . ?
N3 Ru N5 C23 87.9(3) . . . . ?
N2 Ru N5 C23 83.6(16) . . . . ?
N5 Ru N6 C28 179.0(3) . . . . ?
N7 Ru N6 C28 -95.3(3) . . . . ?
N4 Ru N6 C28 171.0(3) . . . . ?
N3 Ru N6 C28 79.9(3) . . . . ?
N2 Ru N6 C28 3.1(3) . . . . ?
N5 Ru N6 C24 3.0(2) . . . . ?
N7 Ru N6 C24 88.7(2) . . . . ?
N4 Ru N6 C24 -4.9(5) . . . . ?
N3 Ru N6 C24 -96.1(2) . . . . ?
N2 Ru N6 C24 -172.9(2) . . . . ?
N5 Ru N7 O1 -56.1(3) . . . . ?
N4 Ru N7 O1 23.5(3) . . . . ?
N6 Ru N7 O1 -135.3(3) . . . . ?
N3 Ru N7 O1 138.3(13) . . . . ?
N2 Ru N7 O1 124.3(3) . . . . ?
N5 Ru N7 O2 120.1(3) . . . . ?
N4 Ru N7 O2 -160.3(3) . . . . ?
N6 Ru N7 O2 40.9(3) . . . . ?
N3 Ru N7 O2 -45.5(15) . . . . ?
N2 Ru N7 O2 -59.5(3) . . . . ?
C8 N1 C2 C7 0.7(4) . . . . ?
C1 N1 C2 C7 179.9(5) . . . . ?
C8 N1 C2 C3 -179.6(4) . . . . ?
C1 N1 C2 C3 -0.4(8) . . . . ?
N1 C2 C3 C4 179.6(4) . . . . ?
C7 C2 C3 C4 -0.7(6) . . . . ?
C2 C3 C4 C5 0.8(7) . . . . ?
C3 C4 C5 C6 -0.4(7) . . . . ?
C4 C5 C6 C7 -0.1(7) . . . . ?
C8 N2 C7 C6 179.5(4) . . . . ?
Ru N2 C7 C6 -0.8(7) . . . . ?
C8 N2 C7 C2 0.2(4) . . . . ?
Ru N2 C7 C2 179.9(3) . . . . ?
C5 C6 C7 N2 -179.1(4) . . . . ?
C5 C6 C7 C2 0.1(6) . . . . ?
N1 C2 C7 N2 -0.6(4) . . . . ?
C3 C2 C7 N2 179.7(3) . . . . ?
N1 C2 C7 C6 -179.9(4) . . . . ?
C3 C2 C7 C6 0.3(6) . . . . ?
C7 N2 C8 N1 0.2(4) . . . . ?
Ru N2 C8 N1 -179.6(2) . . . . ?
C7 N2 C8 C9 -178.6(3) . . . . ?
Ru N2 C8 C9 1.6(4) . . . . ?
C2 N1 C8 N2 -0.6(4) . . . . ?
C1 N1 C8 N2 -179.7(6) . . . . ?
C2 N1 C8 C9 178.1(4) . . . . ?
C1 N1 C8 C9 -1.0(8) . . . . ?
C13 N3 C9 C10 -1.1(6) . . . . ?
Ru N3 C9 C10 177.3(3) . . . . ?
C13 N3 C9 C8 179.4(3) . . . . ?
Ru N3 C9 C8 -2.2(4) . . . . ?
N2 C8 C9 N3 0.4(5) . . . . ?
N1 C8 C9 N3 -178.2(4) . . . . ?
N2 C8 C9 C10 -179.1(4) . . . . ?
N1 C8 C9 C10 2.3(7) . . . . ?
N3 C9 C10 C11 0.7(7) . . . . ?
C8 C9 C10 C11 -179.8(4) . . . . ?
C9 C10 C11 C12 -0.1(7) . . . . ?
C10 C11 C12 C13 -0.2(7) . . . . ?
C9 N3 C13 C12 0.8(6) . . . . ?
Ru N3 C13 C12 -177.4(3) . . . . ?
C11 C12 C13 N3 -0.2(7) . . . . ?
C18 N4 C14 C15 3.0(5) . . . . ?
Ru N4 C14 C15 -176.9(3) . . . . ?
N4 C14 C15 C16 -2.1(6) . . . . ?
C14 C15 C16 C17 -0.1(7) . . . . ?
C15 C16 C17 C18 1.3(7) . . . . ?
C14 N4 C18 C17 -1.7(5) . . . . ?
Ru N4 C18 C17 178.2(3) . . . . ?
C14 N4 C18 C19 175.8(3) . . . . ?
Ru N4 C18 C19 -4.3(4) . . . . ?
C16 C17 C18 N4 -0.4(6) . . . . ?
C16 C17 C18 C19 -177.6(4) . . . . ?
C23 N5 C19 C20 0.5(5) . . . . ?
Ru N5 C19 C20 -173.2(3) . . . . ?
C23 N5 C19 C18 -178.0(3) . . . . ?
Ru N5 C19 C18 8.3(4) . . . . ?
N4 C18 C19 N5 -2.2(4) . . . . ?
C17 C18 C19 N5 175.2(4) . . . . ?
N4 C18 C19 C20 179.4(4) . . . . ?
C17 C18 C19 C20 -3.1(6) . . . . ?
N5 C19 C20 C21 -1.4(6) . . . . ?
C18 C19 C20 C21 176.8(4) . . . . ?
C19 C20 C21 C22 1.2(7) . . . . ?
C20 C21 C22 C23 -0.1(7) . . . . ?
C19 N5 C23 C22 0.6(5) . . . . ?
Ru N5 C23 C22 174.3(3) . . . . ?
C19 N5 C23 C24 -177.5(3) . . . . ?
Ru N5 C23 C24 -3.8(4) . . . . ?
C21 C22 C23 N5 -0.8(6) . . . . ?
C21 C22 C23 C24 177.0(4) . . . . ?
C28 N6 C24 C25 -1.7(5) . . . . ?
Ru N6 C24 C25 174.8(3) . . . . ?
C28 N6 C24 C23 177.8(3) . . . . ?
Ru N6 C24 C23 -5.8(4) . . . . ?
N5 C23 C24 N6 6.3(4) . . . . ?
C22 C23 C24 N6 -171.6(4) . . . . ?
N5 C23 C24 C25 -174.2(4) . . . . ?
C22 C23 C24 C25 7.8(6) . . . . ?
N6 C24 C25 C26 -0.4(6) . . . . ?
C23 C24 C25 C26 -179.8(4) . . . . ?
C24 C25 C26 C27 2.5(7) . . . . ?
C25 C26 C27 C28 -2.4(8) . . . . ?
C24 N6 C28 C27 1.7(6) . . . . ?
Ru N6 C28 C27 -174.1(3) . . . . ?
C26 C27 C28 N6 0.3(7) . . . . ?
|
1100941.cif | #------------------------------------------------------------------------------
#$Date: 2016-12-31 20:31:26 +0200 (Sat, 31 Dec 2016) $
#$Revision: 189516 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/09/1100941.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_1100941
loop_
_publ_author_name
'Nripen Chanda'
'Debamita Paul'
'Sanjib Kar'
'Shaikh M. Mobin'
'Anindya Datta'
'Vedavati G. Puranik'
'K. Krishnamurthy Rao'
'Goutam Kumar Lahiri'
_publ_section_title
;
Effect of 2-(2-Pyridyl)azole-Based Ancillary Ligands (L1-4) on the
Electrophilicity of the Nitrosyl Function in [RuII(trpy)(L1-4)(NO)]3+
[trpy = 2,2':6',2''-Terpyridine]. Synthesis, Structures, and
Spectroscopic, Electrochemical, and Kinetic Aspects
;
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3499
_journal_page_last 3511
_journal_paper_doi 10.1021/ic048184w
_journal_volume 44
_journal_year 2005
_chemical_formula_moiety 'C28 H22 N7 O Ru.3(ClO4).2(H2O) '
_chemical_formula_sum 'C28 H26 Cl3 N7 O15 Ru'
_chemical_formula_weight 907.98
_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 104.955(2)
_cell_angle_beta 92.655(2)
_cell_angle_gamma 95.718(2)
_cell_formula_units_Z 2
_cell_length_a 9.2829(14)
_cell_length_b 10.4319(15)
_cell_length_c 18.729(3)
_cell_measurement_reflns_used 5484
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 27.82
_cell_measurement_theta_min 2.39
_cell_volume 1738.6(5)
_computing_cell_refinement 'BRUKER SAINT'
_computing_data_collection 'BRUKER SMART'
_computing_data_reduction 'BRUKER SAINT'
_computing_molecular_graphics 'SHELXTL and PLATON'
_computing_publication_material 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 ' Bruker Smart APEX'
_diffrn_measurement_device_type ' CCD Area Detector'
_diffrn_measurement_method 'Omega Scan'
_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 0.0428
_diffrn_reflns_av_sigmaI/netI 0.0562
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_number 16270
_diffrn_reflns_theta_full 25.00
_diffrn_reflns_theta_max 25.00
_diffrn_reflns_theta_min 2.03
_exptl_absorpt_coefficient_mu 0.763
_exptl_absorpt_correction_T_max 0.9471
_exptl_absorpt_correction_T_min 0.6833
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Bruker SADABS'
_exptl_crystal_colour 'Deep Brown'
_exptl_crystal_density_diffrn 1.734
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description Plate
_exptl_crystal_F_000 916
_exptl_crystal_size_max 0.54
_exptl_crystal_size_mid 0.21
_exptl_crystal_size_min 0.07
_refine_diff_density_max 1.079
_refine_diff_density_min -0.441
_refine_diff_density_rms 0.107
_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 488
_refine_ls_number_reflns 6093
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.063
_refine_ls_R_factor_all 0.0771
_refine_ls_R_factor_gt 0.0544
_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^)+(0.0768P)^2^+1.4544P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1317
_refine_ls_wR_factor_ref 0.1428
_reflns_number_gt 4668
_reflns_number_total 6093
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file ic048184wsi20041223_113232.cif
_cod_data_source_block C28H26Cl3N7O15Ru
_cod_depositor_comments
;
Marking attached hydrogen atoms.
Antanas Vaitkus,
2016-12-31
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 1100941
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
_atom_site_attached_hydrogens
Ru Ru 0.02173(4) 0.13102(4) 0.25891(2) 0.03238(16) Uani 1 1 d . . . 0
O1 O -0.2326(5) -0.0622(4) 0.2196(2) 0.0629(12) Uani 1 1 d . . . 0
N1 N -0.0360(5) 0.2489(4) 0.1906(2) 0.0371(10) Uani 1 1 d . . . 0
N2 N 0.2047(5) 0.2737(4) 0.2731(2) 0.0369(10) Uani 1 1 d . . . 0
N5 N -0.0476(5) 0.2438(4) 0.3566(2) 0.0366(10) Uani 1 1 d . . . 0
N4 N 0.1154(4) 0.0495(4) 0.3315(2) 0.0344(9) Uani 1 1 d . . . 0
N3 N 0.1481(5) 0.0049(4) 0.1899(2) 0.0401(10) Uani 1 1 d . . . 0
N6 N -0.1332(5) 0.0135(4) 0.2370(2) 0.0414(11) Uani 1 1 d . . . 0
N7 N 0.0195(6) 0.4173(4) 0.1419(2) 0.0465(12) Uani 1 1 d . . . 0
C1 C -0.1236(7) 0.3711(6) 0.1211(3) 0.0491(15) Uani 1 1 d . . . 0
C2 C -0.2295(9) 0.4168(7) 0.0804(3) 0.0650(19) Uani 1 1 d . . . 0
H2 H -0.2067 0.4882 0.0602 0.078 Uiso 1 1 calc R . . 0
C3 C -0.3628(10) 0.3540(8) 0.0722(4) 0.074(2) Uani 1 1 d . . . 0
H3 H -0.4341 0.3826 0.0454 0.089 Uiso 1 1 calc R . . 0
C4 C -0.4010(8) 0.2475(8) 0.1018(4) 0.0689(19) Uani 1 1 d . . . 0
H4 H -0.4962 0.2068 0.0947 0.083 Uiso 1 1 calc R . . 0
C5 C -0.2977(7) 0.2014(6) 0.1421(3) 0.0554(16) Uani 1 1 d . . . 0
H5 H -0.3220 0.1296 0.1618 0.067 Uiso 1 1 calc R . . 0
C6 C -0.1589(6) 0.2652(5) 0.1518(3) 0.0414(13) Uani 1 1 d . . . 0
C7 C 0.0683(6) 0.3409(5) 0.1841(3) 0.0389(12) Uani 1 1 d . . . 0
C8 C 0.2075(6) 0.3543(5) 0.2263(3) 0.0407(13) Uani 1 1 d . . . 0
C9 C 0.3308(7) 0.4368(7) 0.2239(4) 0.0648(18) Uani 1 1 d . . . 0
H9 H 0.3335 0.4890 0.1905 0.078 Uiso 1 1 calc R . . 0
C10 C 0.4501(8) 0.4420(8) 0.2711(4) 0.076(2) Uani 1 1 d . . . 0
H10 H 0.5340 0.4977 0.2697 0.091 Uiso 1 1 calc R . . 0
C11 C 0.4452(7) 0.3651(7) 0.3201(4) 0.0685(19) Uani 1 1 d . . . 0
H11 H 0.5241 0.3699 0.3535 0.082 Uiso 1 1 calc R . . 0
C12 C 0.3231(6) 0.2819(6) 0.3190(3) 0.0518(15) Uani 1 1 d . . . 0
H12 H 0.3209 0.2279 0.3515 0.062 Uiso 1 1 calc R . . 0
C13 C 0.1620(7) -0.0073(6) 0.1176(3) 0.0486(14) Uani 1 1 d . . . 0
H13 H 0.1045 0.0375 0.0924 0.058 Uiso 1 1 calc R . . 0
C14 C 0.2597(7) -0.0850(7) 0.0802(3) 0.0620(17) Uani 1 1 d . . . 0
H14 H 0.2695 -0.0919 0.0302 0.074 Uiso 1 1 calc R . . 0
C15 C 0.3421(8) -0.1517(7) 0.1169(4) 0.0686(19) Uani 1 1 d . . . 0
H15 H 0.4089 -0.2043 0.0920 0.082 Uiso 1 1 calc R . . 0
C16 C 0.3268(7) -0.1413(6) 0.1915(3) 0.0554(16) Uani 1 1 d . . . 0
H16 H 0.3831 -0.1864 0.2170 0.067 Uiso 1 1 calc R . . 0
C17 C 0.2280(6) -0.0639(5) 0.2269(3) 0.0412(13) Uani 1 1 d . . . 0
C18 C 0.2066(6) -0.0412(5) 0.3065(3) 0.0402(12) Uani 1 1 d . . . 0
C19 C 0.2744(6) -0.0974(6) 0.3566(3) 0.0497(14) Uani 1 1 d . . . 0
H19 H 0.3366 -0.1620 0.3409 0.060 Uiso 1 1 calc R . . 0
C20 C 0.2471(6) -0.0550(6) 0.4303(3) 0.0508(15) Uani 1 1 d . . . 0
H20 H 0.2911 -0.0924 0.4644 0.061 Uiso 1 1 calc R . . 0
C21 C 0.1559(6) 0.0419(6) 0.4546(3) 0.0478(14) Uani 1 1 d . . . 0
H21 H 0.1397 0.0708 0.5045 0.057 Uiso 1 1 calc R . . 0
C22 C 0.0892(6) 0.0950(5) 0.4027(3) 0.0362(12) Uani 1 1 d . . . 0
C23 C -0.0032(5) 0.2040(5) 0.4172(3) 0.0372(12) Uani 1 1 d . . . 0
C24 C -0.0407(6) 0.2676(6) 0.4867(3) 0.0447(13) Uani 1 1 d . . . 0
H24 H -0.0079 0.2422 0.5281 0.054 Uiso 1 1 calc R . . 0
C25 C -0.1280(6) 0.3698(6) 0.4940(3) 0.0525(15) Uani 1 1 d . . . 0
H25 H -0.1562 0.4126 0.5404 0.063 Uiso 1 1 calc R . . 0
C26 C -0.1727(6) 0.4074(6) 0.4322(3) 0.0524(15) Uani 1 1 d . . . 0
H26 H -0.2317 0.4756 0.4364 0.063 Uiso 1 1 calc R . . 0
C27 C -0.1300(6) 0.3441(5) 0.3647(3) 0.0412(13) Uani 1 1 d . . . 0
H27 H -0.1588 0.3713 0.3233 0.049 Uiso 1 1 calc R . . 0
C28 C 0.1016(8) 0.5280(6) 0.1199(4) 0.070(2) Uani 1 1 d . . . 0
H28A H 0.1375 0.5975 0.1633 0.104 Uiso 1 1 calc R . . 0
H28B H 0.0389 0.5628 0.0891 0.104 Uiso 1 1 calc R . . 0
H28C H 0.1818 0.4955 0.0928 0.104 Uiso 1 1 calc R . . 0
Cl1 Cl 0.79285(19) 0.79029(16) 0.02695(8) 0.0591(4) Uani 1 1 d . . . 0
O2 O 0.8162(10) 0.9264(6) 0.0585(4) 0.141(3) Uani 1 1 d . . . 0
O3 O 0.9134(7) 0.7318(7) 0.0431(4) 0.136(3) Uani 1 1 d . . . 0
O4 O 0.6761(8) 0.7274(9) 0.0535(4) 0.153(3) Uani 1 1 d . . . 0
O5 O 0.7650(6) 0.7647(5) -0.0505(3) 0.0909(17) Uani 1 1 d . . . 0
Cl2 Cl 0.92110(17) 0.68174(15) 0.29935(8) 0.0527(4) Uani 1 1 d . . . 0
O6 O 0.9498(7) 0.7290(5) 0.2362(3) 0.0933(17) Uani 1 1 d . . . 0
O7 O 0.9008(6) 0.7940(5) 0.3581(2) 0.0791(14) Uani 1 1 d . . . 0
O8 O 1.0389(6) 0.6184(5) 0.3183(3) 0.0888(16) Uani 1 1 d . . . 0
O9 O 0.7972(6) 0.5876(5) 0.2822(3) 0.0960(17) Uani 1 1 d . . . 0
Cl3 Cl 0.46285(18) 0.27672(17) 0.52435(10) 0.0666(5) Uani 1 1 d . . . 0
O10 O 0.5109(7) 0.2087(7) 0.4552(3) 0.109(2) Uani 1 1 d . . . 0
O11 O 0.3291(6) 0.3222(6) 0.5115(4) 0.109(2) Uani 1 1 d . . . 0
O12 O 0.5699(8) 0.3739(9) 0.5612(5) 0.182(4) Uani 1 1 d . . . 0
O13 O 0.4383(7) 0.1778(8) 0.5656(4) 0.141(3) Uani 1 1 d . . . 0
O14 O 0.5712(7) 0.6642(6) 0.1832(4) 0.123(2) Uani 1 1 d . . . 2
O15 O 0.6792(9) 0.0317(6) 0.3656(4) 0.141(3) Uani 1 1 d . . . 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
Ru 0.0364(3) 0.0330(2) 0.0297(2) 0.01251(16) 0.00039(16) 0.00305(17)
O1 0.060(3) 0.062(3) 0.060(3) 0.017(2) -0.005(2) -0.021(2)
N1 0.043(3) 0.038(2) 0.034(2) 0.0150(19) 0.0029(19) 0.007(2)
N2 0.040(3) 0.038(2) 0.035(2) 0.0145(19) 0.0029(19) 0.0021(19)
N5 0.040(3) 0.034(2) 0.036(2) 0.0108(18) 0.0033(19) 0.0019(19)
N4 0.039(3) 0.034(2) 0.031(2) 0.0123(18) -0.0023(18) 0.0010(19)
N3 0.045(3) 0.037(2) 0.039(2) 0.0118(19) 0.007(2) 0.004(2)
N6 0.046(3) 0.041(3) 0.040(3) 0.016(2) 0.007(2) 0.004(2)
N7 0.067(4) 0.039(3) 0.040(3) 0.020(2) 0.009(2) 0.013(2)
C1 0.071(4) 0.046(3) 0.035(3) 0.012(3) 0.007(3) 0.022(3)
C2 0.097(6) 0.064(4) 0.043(4) 0.020(3) 0.000(4) 0.043(4)
C3 0.088(6) 0.091(6) 0.048(4) 0.013(4) -0.012(4) 0.049(5)
C4 0.063(5) 0.085(5) 0.052(4) 0.002(4) -0.011(3) 0.025(4)
C5 0.056(4) 0.059(4) 0.052(4) 0.014(3) -0.002(3) 0.020(3)
C6 0.050(4) 0.044(3) 0.031(3) 0.008(2) -0.003(2) 0.016(3)
C7 0.052(3) 0.036(3) 0.032(3) 0.012(2) 0.007(2) 0.009(2)
C8 0.052(4) 0.031(3) 0.035(3) 0.004(2) 0.008(2) 0.000(2)
C9 0.062(4) 0.064(4) 0.072(5) 0.030(4) 0.012(4) -0.012(3)
C10 0.054(5) 0.086(5) 0.083(5) 0.028(4) -0.005(4) -0.025(4)
C11 0.053(4) 0.083(5) 0.063(4) 0.021(4) -0.013(3) -0.017(4)
C12 0.049(4) 0.054(4) 0.051(4) 0.017(3) -0.006(3) -0.002(3)
C13 0.059(4) 0.053(3) 0.036(3) 0.014(3) 0.007(3) 0.008(3)
C14 0.076(5) 0.070(4) 0.042(3) 0.011(3) 0.018(3) 0.021(4)
C15 0.074(5) 0.067(4) 0.068(5) 0.011(4) 0.025(4) 0.032(4)
C16 0.063(4) 0.053(4) 0.052(4) 0.011(3) 0.006(3) 0.017(3)
C17 0.040(3) 0.038(3) 0.048(3) 0.015(2) 0.004(2) 0.008(2)
C18 0.046(3) 0.039(3) 0.037(3) 0.013(2) 0.000(2) 0.006(3)
C19 0.050(4) 0.045(3) 0.057(4) 0.018(3) -0.005(3) 0.011(3)
C20 0.055(4) 0.058(4) 0.049(4) 0.030(3) -0.007(3) 0.009(3)
C21 0.051(4) 0.058(4) 0.036(3) 0.021(3) -0.001(3) -0.004(3)
C22 0.039(3) 0.039(3) 0.033(3) 0.016(2) 0.000(2) 0.000(2)
C23 0.035(3) 0.041(3) 0.037(3) 0.014(2) 0.000(2) -0.002(2)
C24 0.046(3) 0.052(3) 0.032(3) 0.006(2) 0.003(2) 0.000(3)
C25 0.045(4) 0.061(4) 0.042(3) -0.003(3) 0.010(3) 0.000(3)
C26 0.043(4) 0.045(3) 0.062(4) 0.000(3) 0.003(3) 0.005(3)
C27 0.037(3) 0.039(3) 0.045(3) 0.007(2) -0.002(2) 0.002(2)
C28 0.099(6) 0.052(4) 0.072(5) 0.039(3) 0.016(4) 0.009(4)
Cl1 0.0747(12) 0.0601(10) 0.0459(9) 0.0184(7) 0.0045(8) 0.0127(8)
O2 0.242(9) 0.075(4) 0.098(5) 0.005(4) -0.013(5) 0.046(5)
O3 0.111(5) 0.122(5) 0.185(7) 0.066(5) -0.048(5) 0.024(4)
O4 0.099(5) 0.246(10) 0.138(6) 0.104(7) 0.020(4) -0.014(6)
O5 0.123(5) 0.102(4) 0.048(3) 0.016(3) 0.010(3) 0.026(4)
Cl2 0.0645(10) 0.0508(8) 0.0407(8) 0.0108(6) -0.0020(7) 0.0027(7)
O6 0.141(5) 0.090(4) 0.061(3) 0.036(3) 0.024(3) 0.017(3)
O7 0.100(4) 0.078(3) 0.049(3) -0.003(2) 0.005(2) 0.016(3)
O8 0.090(4) 0.081(4) 0.094(4) 0.018(3) -0.014(3) 0.028(3)
O9 0.083(4) 0.079(4) 0.117(5) 0.027(3) -0.015(3) -0.021(3)
Cl3 0.0558(11) 0.0658(10) 0.0722(11) 0.0062(9) 0.0048(8) 0.0099(8)
O10 0.102(4) 0.130(5) 0.086(4) 0.002(4) 0.022(3) 0.041(4)
O11 0.090(4) 0.091(4) 0.159(6) 0.039(4) 0.022(4) 0.047(3)
O12 0.114(6) 0.167(7) 0.183(8) -0.069(6) 0.024(5) -0.063(5)
O13 0.116(5) 0.198(8) 0.155(7) 0.124(6) 0.010(5) 0.032(5)
O14 0.099(5) 0.103(5) 0.186(7) 0.070(5) 0.008(4) 0.017(4)
O15 0.195(7) 0.095(4) 0.119(5) 0.004(4) 0.076(5) -0.017(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'
Cl Cl 0.1484 0.1585 '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'
Ru Ru -1.2594 0.8363 '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'
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
N6 Ru N4 95.50(18) . . ?
N6 Ru N5 95.78(18) . . ?
N4 Ru N5 79.85(16) . . ?
N6 Ru N1 97.42(18) . . ?
N4 Ru N1 167.05(16) . . ?
N5 Ru N1 97.89(16) . . ?
N6 Ru N3 93.13(18) . . ?
N4 Ru N3 79.58(17) . . ?
N5 Ru N3 158.26(17) . . ?
N1 Ru N3 100.57(16) . . ?
N6 Ru N2 173.62(17) . . ?
N4 Ru N2 89.96(16) . . ?
N5 Ru N2 88.42(16) . . ?
N1 Ru N2 77.20(16) . . ?
N3 Ru N2 84.58(16) . . ?
C7 N1 C6 107.6(4) . . ?
C7 N1 Ru 114.8(3) . . ?
C6 N1 Ru 137.4(4) . . ?
C12 N2 C8 118.3(5) . . ?
C12 N2 Ru 125.1(4) . . ?
C8 N2 Ru 116.2(3) . . ?
C27 N5 C23 119.6(4) . . ?
C27 N5 Ru 127.5(4) . . ?
C23 N5 Ru 112.9(3) . . ?
C22 N4 C18 124.6(4) . . ?
C22 N4 Ru 117.3(3) . . ?
C18 N4 Ru 117.9(3) . . ?
C13 N3 C17 120.1(5) . . ?
C13 N3 Ru 126.9(4) . . ?
C17 N3 Ru 112.9(3) . . ?
O1 N6 Ru 176.9(4) . . ?
C7 N7 C1 106.8(4) . . ?
C7 N7 C28 128.1(5) . . ?
C1 N7 C28 125.1(5) . . ?
N7 C1 C6 107.5(5) . . ?
N7 C1 C2 131.5(6) . . ?
C6 C1 C2 121.0(6) . . ?
C3 C2 C1 117.3(7) . . ?
C3 C2 H2 121.3 . . ?
C1 C2 H2 121.3 . . ?
C2 C3 C4 123.0(7) . . ?
C2 C3 H3 118.5 . . ?
C4 C3 H3 118.5 . . ?
C3 C4 C5 120.4(7) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
C6 C5 C4 117.8(6) . . ?
C6 C5 H5 121.1 . . ?
C4 C5 H5 121.1 . . ?
C5 C6 N1 132.2(5) . . ?
C5 C6 C1 120.5(5) . . ?
N1 C6 C1 107.2(5) . . ?
N1 C7 N7 111.0(5) . . ?
N1 C7 C8 118.9(4) . . ?
N7 C7 C8 129.9(5) . . ?
N2 C8 C9 120.4(5) . . ?
N2 C8 C7 111.8(4) . . ?
C9 C8 C7 127.7(5) . . ?
C10 C9 C8 119.7(6) . . ?
C10 C9 H9 120.1 . . ?
C8 C9 H9 120.1 . . ?
C11 C10 C9 119.8(6) . . ?
C11 C10 H10 120.1 . . ?
C9 C10 H10 120.1 . . ?
C12 C11 C10 118.6(6) . . ?
C12 C11 H11 120.7 . . ?
C10 C11 H11 120.7 . . ?
N2 C12 C11 123.1(6) . . ?
N2 C12 H12 118.5 . . ?
C11 C12 H12 118.5 . . ?
N3 C13 C14 120.9(6) . . ?
N3 C13 H13 119.5 . . ?
C14 C13 H13 119.5 . . ?
C15 C14 C13 119.4(6) . . ?
C15 C14 H14 120.3 . . ?
C13 C14 H14 120.3 . . ?
C14 C15 C16 120.0(6) . . ?
C14 C15 H15 120.0 . . ?
C16 C15 H15 120.0 . . ?
C17 C16 C15 119.0(6) . . ?
C17 C16 H16 120.5 . . ?
C15 C16 H16 120.5 . . ?
C16 C17 N3 120.4(5) . . ?
C16 C17 C18 123.8(5) . . ?
N3 C17 C18 115.7(4) . . ?
N4 C18 C19 118.6(5) . . ?
N4 C18 C17 113.9(4) . . ?
C19 C18 C17 127.4(5) . . ?
C20 C19 C18 118.3(5) . . ?
C20 C19 H19 120.9 . . ?
C18 C19 H19 120.9 . . ?
C19 C20 C21 121.6(5) . . ?
C19 C20 H20 119.2 . . ?
C21 C20 H20 119.2 . . ?
C20 C21 C22 118.4(5) . . ?
C20 C21 H21 120.8 . . ?
C22 C21 H21 120.8 . . ?
N4 C22 C21 118.4(5) . . ?
N4 C22 C23 114.4(4) . . ?
C21 C22 C23 127.1(5) . . ?
N5 C23 C24 120.5(5) . . ?
N5 C23 C22 115.4(4) . . ?
C24 C23 C22 124.0(5) . . ?
C23 C24 C25 119.1(5) . . ?
C23 C24 H24 120.4 . . ?
C25 C24 H24 120.4 . . ?
C26 C25 C24 119.4(5) . . ?
C26 C25 H25 120.3 . . ?
C24 C25 H25 120.3 . . ?
C27 C26 C25 119.5(5) . . ?
C27 C26 H26 120.2 . . ?
C25 C26 H26 120.2 . . ?
N5 C27 C26 121.8(5) . . ?
N5 C27 H27 119.1 . . ?
C26 C27 H27 119.1 . . ?
N7 C28 H28A 109.5 . . ?
N7 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
N7 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O2 Cl1 O3 109.6(5) . . ?
O2 Cl1 O4 113.4(5) . . ?
O3 Cl1 O4 106.2(5) . . ?
O2 Cl1 O5 109.6(4) . . ?
O3 Cl1 O5 110.4(4) . . ?
O4 Cl1 O5 107.5(4) . . ?
O9 Cl2 O8 108.3(3) . . ?
O9 Cl2 O7 111.8(3) . . ?
O8 Cl2 O7 110.6(3) . . ?
O9 Cl2 O6 108.9(4) . . ?
O8 Cl2 O6 109.9(4) . . ?
O7 Cl2 O6 107.4(3) . . ?
O12 Cl3 O11 115.0(5) . . ?
O12 Cl3 O10 109.0(4) . . ?
O11 Cl3 O10 108.8(4) . . ?
O12 Cl3 O13 109.5(6) . . ?
O11 Cl3 O13 107.9(4) . . ?
O10 Cl3 O13 106.2(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
Ru N6 1.754(5) . ?
Ru N4 1.991(4) . ?
Ru N5 2.072(4) . ?
Ru N1 2.078(4) . ?
Ru N3 2.085(4) . ?
Ru N2 2.103(4) . ?
O1 N6 1.129(5) . ?
N1 C7 1.326(6) . ?
N1 C6 1.373(6) . ?
N2 C12 1.346(7) . ?
N2 C8 1.360(6) . ?
N5 C27 1.338(6) . ?
N5 C23 1.366(6) . ?
N4 C22 1.337(6) . ?
N4 C18 1.341(7) . ?
N3 C13 1.340(6) . ?
N3 C17 1.364(6) . ?
N7 C7 1.353(6) . ?
N7 C1 1.370(8) . ?
N7 C28 1.478(7) . ?
C1 C6 1.390(8) . ?
C1 C2 1.409(8) . ?
C2 C3 1.324(10) . ?
C2 H2 0.9300 . ?
C3 C4 1.388(10) . ?
C3 H3 0.9300 . ?
C4 C5 1.390(8) . ?
C4 H4 0.9300 . ?
C5 C6 1.372(8) . ?
C5 H5 0.9300 . ?
C7 C8 1.458(8) . ?
C8 C9 1.372(8) . ?
C9 C10 1.372(9) . ?
C9 H9 0.9300 . ?
C10 C11 1.366(10) . ?
C10 H10 0.9300 . ?
C11 C12 1.353(8) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C14 1.373(8) . ?
C13 H13 0.9300 . ?
C14 C15 1.357(9) . ?
C14 H14 0.9300 . ?
C15 C16 1.389(9) . ?
C15 H15 0.9300 . ?
C16 C17 1.363(8) . ?
C16 H16 0.9300 . ?
C17 C18 1.474(7) . ?
C18 C19 1.387(7) . ?
C19 C20 1.380(8) . ?
C19 H19 0.9300 . ?
C20 C21 1.384(8) . ?
C20 H20 0.9300 . ?
C21 C22 1.387(7) . ?
C21 H21 0.9300 . ?
C22 C23 1.469(7) . ?
C23 C24 1.377(7) . ?
C24 C25 1.386(8) . ?
C24 H24 0.9300 . ?
C25 C26 1.375(9) . ?
C25 H25 0.9300 . ?
C26 C27 1.363(8) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
Cl1 O2 1.380(6) . ?
Cl1 O3 1.384(6) . ?
Cl1 O4 1.388(7) . ?
Cl1 O5 1.413(5) . ?
Cl2 O9 1.403(5) . ?
Cl2 O8 1.409(5) . ?
Cl2 O7 1.419(5) . ?
Cl2 O6 1.421(5) . ?
Cl3 O12 1.366(6) . ?
Cl3 O11 1.404(5) . ?
Cl3 O10 1.422(5) . ?
Cl3 O13 1.447(6) . ?
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
N6 Ru N1 C7 -170.5(4) . . . . ?
N4 Ru N1 C7 13.6(9) . . . . ?
N5 Ru N1 C7 92.6(4) . . . . ?
N3 Ru N1 C7 -75.9(4) . . . . ?
N2 Ru N1 C7 6.0(3) . . . . ?
N6 Ru N1 C6 14.5(5) . . . . ?
N4 Ru N1 C6 -161.4(7) . . . . ?
N5 Ru N1 C6 -82.4(5) . . . . ?
N3 Ru N1 C6 109.1(5) . . . . ?
N2 Ru N1 C6 -169.0(5) . . . . ?
N6 Ru N2 C12 -149.6(15) . . . . ?
N4 Ru N2 C12 -0.7(5) . . . . ?
N5 Ru N2 C12 79.1(4) . . . . ?
N1 Ru N2 C12 177.6(5) . . . . ?
N3 Ru N2 C12 -80.3(5) . . . . ?
N6 Ru N2 C8 23.6(18) . . . . ?
N4 Ru N2 C8 172.4(4) . . . . ?
N5 Ru N2 C8 -107.8(4) . . . . ?
N1 Ru N2 C8 -9.3(3) . . . . ?
N3 Ru N2 C8 92.9(4) . . . . ?
N6 Ru N5 C27 -86.6(4) . . . . ?
N4 Ru N5 C27 178.8(4) . . . . ?
N1 Ru N5 C27 11.7(4) . . . . ?
N3 Ru N5 C27 159.7(4) . . . . ?
N2 Ru N5 C27 88.6(4) . . . . ?
N6 Ru N5 C23 91.7(4) . . . . ?
N4 Ru N5 C23 -2.8(3) . . . . ?
N1 Ru N5 C23 -169.9(3) . . . . ?
N3 Ru N5 C23 -22.0(6) . . . . ?
N2 Ru N5 C23 -93.1(3) . . . . ?
N6 Ru N4 C22 -92.3(4) . . . . ?
N5 Ru N4 C22 2.6(3) . . . . ?
N1 Ru N4 C22 83.6(8) . . . . ?
N3 Ru N4 C22 175.5(4) . . . . ?
N2 Ru N4 C22 91.0(4) . . . . ?
N6 Ru N4 C18 91.5(4) . . . . ?
N5 Ru N4 C18 -173.6(4) . . . . ?
N1 Ru N4 C18 -92.5(8) . . . . ?
N3 Ru N4 C18 -0.7(4) . . . . ?
N2 Ru N4 C18 -85.2(4) . . . . ?
N6 Ru N3 C13 87.8(5) . . . . ?
N4 Ru N3 C13 -177.2(5) . . . . ?
N5 Ru N3 C13 -158.1(4) . . . . ?
N1 Ru N3 C13 -10.4(5) . . . . ?
N2 Ru N3 C13 -86.3(5) . . . . ?
N6 Ru N3 C17 -96.0(4) . . . . ?
N4 Ru N3 C17 -1.0(3) . . . . ?
N5 Ru N3 C17 18.2(6) . . . . ?
N1 Ru N3 C17 165.9(3) . . . . ?
N2 Ru N3 C17 90.0(4) . . . . ?
N4 Ru N6 O1 -139(8) . . . . ?
N5 Ru N6 O1 141(8) . . . . ?
N1 Ru N6 O1 42(8) . . . . ?
N3 Ru N6 O1 -59(8) . . . . ?
N2 Ru N6 O1 10(9) . . . . ?
C7 N7 C1 C6 -0.1(6) . . . . ?
C28 N7 C1 C6 178.7(5) . . . . ?
C7 N7 C1 C2 176.4(6) . . . . ?
C28 N7 C1 C2 -4.9(10) . . . . ?
N7 C1 C2 C3 -176.7(6) . . . . ?
C6 C1 C2 C3 -0.6(9) . . . . ?
C1 C2 C3 C4 0.2(10) . . . . ?
C2 C3 C4 C5 -0.2(11) . . . . ?
C3 C4 C5 C6 0.5(9) . . . . ?
C4 C5 C6 N1 176.5(6) . . . . ?
C4 C5 C6 C1 -0.9(8) . . . . ?
C7 N1 C6 C5 -177.4(6) . . . . ?
Ru N1 C6 C5 -2.1(9) . . . . ?
C7 N1 C6 C1 0.3(6) . . . . ?
Ru N1 C6 C1 175.6(4) . . . . ?
N7 C1 C6 C5 177.9(5) . . . . ?
C2 C1 C6 C5 1.0(8) . . . . ?
N7 C1 C6 N1 -0.1(6) . . . . ?
C2 C1 C6 N1 -177.1(5) . . . . ?
C6 N1 C7 N7 -0.4(6) . . . . ?
Ru N1 C7 N7 -176.9(3) . . . . ?
C6 N1 C7 C8 174.1(4) . . . . ?
Ru N1 C7 C8 -2.4(6) . . . . ?
C1 N7 C7 N1 0.3(6) . . . . ?
C28 N7 C7 N1 -178.4(5) . . . . ?
C1 N7 C7 C8 -173.4(5) . . . . ?
C28 N7 C7 C8 7.9(9) . . . . ?
C12 N2 C8 C9 3.2(8) . . . . ?
Ru N2 C8 C9 -170.5(4) . . . . ?
C12 N2 C8 C7 -175.9(5) . . . . ?
Ru N2 C8 C7 10.5(5) . . . . ?
N1 C7 C8 N2 -5.4(7) . . . . ?
N7 C7 C8 N2 167.9(5) . . . . ?
N1 C7 C8 C9 175.7(5) . . . . ?
N7 C7 C8 C9 -11.0(9) . . . . ?
N2 C8 C9 C10 -2.7(9) . . . . ?
C7 C8 C9 C10 176.2(6) . . . . ?
C8 C9 C10 C11 -0.1(11) . . . . ?
C9 C10 C11 C12 2.2(11) . . . . ?
C8 N2 C12 C11 -1.0(9) . . . . ?
Ru N2 C12 C11 172.0(5) . . . . ?
C10 C11 C12 N2 -1.7(11) . . . . ?
C17 N3 C13 C14 -2.3(8) . . . . ?
Ru N3 C13 C14 173.7(4) . . . . ?
N3 C13 C14 C15 0.8(10) . . . . ?
C13 C14 C15 C16 0.2(11) . . . . ?
C14 C15 C16 C17 0.2(10) . . . . ?
C15 C16 C17 N3 -1.7(9) . . . . ?
C15 C16 C17 C18 -177.5(6) . . . . ?
C13 N3 C17 C16 2.7(8) . . . . ?
Ru N3 C17 C16 -173.8(4) . . . . ?
C13 N3 C17 C18 178.8(5) . . . . ?
Ru N3 C17 C18 2.3(6) . . . . ?
C22 N4 C18 C19 3.1(8) . . . . ?
Ru N4 C18 C19 179.0(4) . . . . ?
C22 N4 C18 C17 -173.8(4) . . . . ?
Ru N4 C18 C17 2.1(6) . . . . ?
C16 C17 C18 N4 173.1(5) . . . . ?
N3 C17 C18 N4 -2.9(7) . . . . ?
C16 C17 C18 C19 -3.5(9) . . . . ?
N3 C17 C18 C19 -179.5(5) . . . . ?
N4 C18 C19 C20 -1.4(8) . . . . ?
C17 C18 C19 C20 175.1(5) . . . . ?
C18 C19 C20 C21 -0.6(9) . . . . ?
C19 C20 C21 C22 1.1(9) . . . . ?
C18 N4 C22 C21 -2.6(7) . . . . ?
Ru N4 C22 C21 -178.5(4) . . . . ?
C18 N4 C22 C23 174.0(5) . . . . ?
Ru N4 C22 C23 -1.9(5) . . . . ?
C20 C21 C22 N4 0.4(8) . . . . ?
C20 C21 C22 C23 -175.7(5) . . . . ?
C27 N5 C23 C24 -1.0(7) . . . . ?
Ru N5 C23 C24 -179.5(4) . . . . ?
C27 N5 C23 C22 -178.8(4) . . . . ?
Ru N5 C23 C22 2.7(5) . . . . ?
N4 C22 C23 N5 -0.6(6) . . . . ?
C21 C22 C23 N5 175.6(5) . . . . ?
N4 C22 C23 C24 -178.4(5) . . . . ?
C21 C22 C23 C24 -2.1(8) . . . . ?
N5 C23 C24 C25 2.0(8) . . . . ?
C22 C23 C24 C25 179.6(5) . . . . ?
C23 C24 C25 C26 -1.4(8) . . . . ?
C24 C25 C26 C27 -0.3(9) . . . . ?
C23 N5 C27 C26 -0.8(7) . . . . ?
Ru N5 C27 C26 177.5(4) . . . . ?
C25 C26 C27 N5 1.4(8) . . . . ?
|
1100942.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100942.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_1100942
loop_
_publ_author_name
'Nripen Chanda'
'Debamita Paul'
'Sanjib Kar'
'Shaikh M. Mobin'
'Anindya Datta'
'Vedavati G. Puranik'
'K. Krishnamurthy Rao'
'Goutam Kumar Lahiri'
_publ_section_title
;
Effect of 2-(2-Pyridyl)azole-Based Ancillary Ligands (L1-4) on the
Electrophilicity of the Nitrosyl Function in [RuII(trpy)(L1-4)(NO)]3+ [trpy
= 2,2':6',2''-Terpyridine]. Synthesis, Structures, and
Spectroscopic, Electrochemical, and Kinetic Aspects
;
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3499
_journal_page_last 3511
_journal_paper_doi 10.1021/ic048184w
_journal_volume 44
_journal_year 2005
_chemical_formula_moiety '2[(C27 H19 O2 N6 Ru).3(ClO4)].1.5[CH3CN]'
_chemical_formula_sum 'C28.5 H21.25 Cl3 N6.75 O14 Ru'
_chemical_formula_weight 889.69
_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 133.3790(10)
_cell_angle_gamma 90.00
_cell_formula_units_Z 8
_cell_length_a 21.1704(18)
_cell_length_b 30.040(3)
_cell_length_c 14.8373(13)
_cell_measurement_reflns_used 7090
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 25.74
_cell_measurement_theta_min 2.32
_cell_volume 6858.3(11)
_computing_cell_refinement 'BRUKER SAINT'
_computing_data_collection 'BRUKER SMART'
_computing_data_reduction 'BRUKER SAINT'
_computing_molecular_graphics 'SHELXTL and PLATON'
_computing_publication_material 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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device ' Bruker Smart APEX'
_diffrn_measurement_device_type ' CCD Area Detector'
_diffrn_measurement_method 'Omega Scan'
_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 0.0216
_diffrn_reflns_av_sigmaI/netI 0.0291
_diffrn_reflns_limit_h_max 25
_diffrn_reflns_limit_h_min -25
_diffrn_reflns_limit_k_max 35
_diffrn_reflns_limit_k_min -35
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_number 32971
_diffrn_reflns_theta_full 25.00
_diffrn_reflns_theta_max 25.00
_diffrn_reflns_theta_min 1.36
_exptl_absorpt_coefficient_mu 0.770
_exptl_absorpt_correction_T_max 0.9424
_exptl_absorpt_correction_T_min 0.7797
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Bruker SADABS'
_exptl_crystal_colour Red
_exptl_crystal_density_diffrn 1.723
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description 'thin plate'
_exptl_crystal_F_000 3572
_exptl_crystal_size_max 0.34
_exptl_crystal_size_mid 0.20
_exptl_crystal_size_min 0.08
_refine_diff_density_max 0.970
_refine_diff_density_min -0.668
_refine_diff_density_rms 0.088
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack 0.01(3)
_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 975
_refine_ls_number_reflns 11986
_refine_ls_number_restraints 219
_refine_ls_restrained_S_all 1.150
_refine_ls_R_factor_all 0.0475
_refine_ls_R_factor_gt 0.0423
_refine_ls_shift/su_max 4.218
_refine_ls_shift/su_mean 0.025
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0882P)^2^+0.5118P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1127
_refine_ls_wR_factor_ref 0.1170
_reflns_number_gt 10864
_reflns_number_total 11986
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file ic048184wsi20041223_113326.cif
_cod_data_source_block 2[(C27H19O2N6Ru).3(ClO4)].1.5[CH3CN]
_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 'C57 H42.50 Cl6 N13.50 O28 Ru2'
_cod_database_code 1100942
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
Ru Ru 0.35035(3) 0.132938(11) 0.59143(4) 0.04097(11) Uani 1 1 d . . .
O1 O 0.1980(4) 0.18805(19) 0.4272(6) 0.0907(17) Uani 1 1 d . . .
O2 O 0.2928(3) 0.01093(15) 0.6451(4) 0.0623(11) Uani 1 1 d . . .
N1 N 0.2838(3) 0.07747(15) 0.5743(4) 0.0475(10) Uani 1 1 d . . .
N2 N 0.4513(3) 0.08669(16) 0.7152(4) 0.0491(10) Uani 1 1 d . . .
N3 N 0.3541(3) 0.11660(14) 0.4593(4) 0.0462(10) Uani 1 1 d . . .
N4 N 0.4333(3) 0.17815(15) 0.6274(4) 0.0480(10) Uani 1 1 d . . .
N5 N 0.3898(3) 0.16126(16) 0.7513(5) 0.0540(11) Uani 1 1 d . . .
N6 N 0.2583(3) 0.16686(17) 0.4903(5) 0.0542(11) Uani 1 1 d . . .
C1 C 0.2051(4) 0.0205(2) 0.5455(6) 0.0602(15) Uani 1 1 d . . .
C2 C 0.1345(4) -0.0065(3) 0.4983(7) 0.0755(19) Uani 1 1 d . . .
H2 H 0.1405 -0.0341 0.5319 0.091 Uiso 1 1 calc R . .
C3 C 0.0558(5) 0.0112(3) 0.3981(8) 0.083(2) Uani 1 1 d . . .
H3 H 0.0061 -0.0053 0.3615 0.100 Uiso 1 1 calc R . .
C4 C 0.0462(4) 0.0527(3) 0.3480(8) 0.084(2) Uani 1 1 d . . .
H4 H -0.0091 0.0634 0.2808 0.101 Uiso 1 1 calc R . .
C5 C 0.1190(4) 0.0785(2) 0.3979(7) 0.0681(17) Uani 1 1 d . . .
H5 H 0.1142 0.1058 0.3638 0.082 Uiso 1 1 calc R . .
C6 C 0.1975(3) 0.06128(19) 0.4995(5) 0.0498(12) Uani 1 1 d . . .
C7 C 0.3335(4) 0.04674(18) 0.6540(5) 0.0516(13) Uani 1 1 d . . .
C8 C 0.4264(4) 0.04987(18) 0.7383(5) 0.0519(13) Uani 1 1 d . . .
C9 C 0.4845(4) 0.0202(2) 0.8282(6) 0.0631(16) Uani 1 1 d . . .
H9 H 0.4658 -0.0044 0.8427 0.076 Uiso 1 1 calc R . .
C10 C 0.5718(4) 0.0269(3) 0.8980(7) 0.078(2) Uani 1 1 d . . .
H10 H 0.6135 0.0081 0.9636 0.093 Uiso 1 1 calc R . .
C11 C 0.5950(4) 0.0619(3) 0.8678(7) 0.077(2) Uani 1 1 d . . .
H11 H 0.6528 0.0654 0.9076 0.092 Uiso 1 1 calc R . .
C12 C 0.5354(4) 0.0919(2) 0.7808(6) 0.0605(15) Uani 1 1 d . . .
H12 H 0.5537 0.1167 0.7666 0.073 Uiso 1 1 calc R . .
C13 C 0.3144(4) 0.0830(2) 0.3809(5) 0.0560(13) Uani 1 1 d . . .
H13 H 0.2813 0.0634 0.3827 0.067 Uiso 1 1 calc R . .
C14 C 0.3217(5) 0.0766(3) 0.2933(7) 0.079(2) Uani 1 1 d . . .
H14 H 0.2947 0.0524 0.2397 0.095 Uiso 1 1 calc R . .
C15 C 0.3678(5) 0.1056(3) 0.2878(7) 0.0765(19) Uani 1 1 d . . .
H15 H 0.3690 0.1031 0.2264 0.092 Uiso 1 1 calc R . .
C16 C 0.4148(5) 0.1401(2) 0.3786(6) 0.0648(15) Uani 1 1 d . . .
H16 H 0.4519 0.1586 0.3826 0.078 Uiso 1 1 calc R . .
C17 C 0.4049(4) 0.14563(19) 0.4583(5) 0.0471(11) Uani 1 1 d . . .
C18 C 0.4481(3) 0.18055(18) 0.5525(5) 0.0448(11) Uani 1 1 d . . .
C19 C 0.5011(4) 0.2137(2) 0.5720(6) 0.0627(15) Uani 1 1 d . . .
H19 H 0.5136 0.2159 0.5231 0.075 Uiso 1 1 calc R . .
C20 C 0.5353(6) 0.2439(2) 0.6668(8) 0.082(2) Uani 1 1 d . . .
H20 H 0.5668 0.2680 0.6758 0.098 Uiso 1 1 calc R . .
C21 C 0.5247(5) 0.2397(3) 0.7478(7) 0.080(2) Uani 1 1 d . . .
H21 H 0.5528 0.2587 0.8155 0.096 Uiso 1 1 calc R . .
C22 C 0.4702(5) 0.2061(2) 0.7244(6) 0.0623(16) Uani 1 1 d . . .
C23 C 0.4431(5) 0.1966(2) 0.7915(7) 0.075(2) Uani 1 1 d . . .
C24 C 0.4790(8) 0.2191(3) 0.8997(9) 0.112(4) Uani 1 1 d . . .
H24 H 0.5177 0.2425 0.9290 0.135 Uiso 1 1 calc R . .
C25 C 0.4556(9) 0.2057(4) 0.9619(11) 0.130(5) Uani 1 1 d . . .
H25 H 0.4777 0.2206 1.0335 0.156 Uiso 1 1 calc R . .
C26 C 0.3998(7) 0.1704(4) 0.9193(8) 0.100(3) Uani 1 1 d . . .
H26 H 0.3845 0.1614 0.9622 0.120 Uiso 1 1 calc R . .
C27 C 0.3666(5) 0.1487(3) 0.8129(7) 0.0677(17) Uani 1 1 d . . .
H27 H 0.3281 0.1252 0.7830 0.081 Uiso 1 1 calc R . .
Cl1 Cl 0.07581(18) 0.12917(7) 0.0955(3) 0.0865(6) Uani 1 1 d U . .
O3 O 0.1386(7) 0.1481(4) 0.2059(10) 0.187(4) Uani 1 1 d U . .
O4 O 0.0025(9) 0.1254(4) 0.0790(16) 0.202(5) Uani 1 1 d U . .
O5 O 0.0817(10) 0.0901(5) 0.083(2) 0.292(8) Uani 1 1 d U . .
O6 O 0.0439(10) 0.1685(5) 0.0250(12) 0.207(5) Uani 1 1 d U . .
Cl2 Cl 0.33625(11) 0.03869(6) 0.95095(16) 0.0694(4) Uani 1 1 d U . .
O7 O 0.3413(5) 0.0766(3) 1.0103(9) 0.152(3) Uani 1 1 d U . .
O8 O 0.2547(4) 0.0193(2) 0.8652(9) 0.149(4) Uani 1 1 d U . .
O9 O 0.3911(5) 0.0051(3) 1.0386(7) 0.150(3) Uani 1 1 d U . .
O10 O 0.3717(8) 0.0482(4) 0.9037(11) 0.172(4) Uani 1 1 d U . .
Cl3 Cl 0.64428(14) 0.09262(7) 0.6524(2) 0.0880(6) Uani 1 1 d U . .
O11 O 0.6709(8) 0.1007(5) 0.5960(10) 0.186(4) Uani 1 1 d U . .
O12 O 0.6128(6) 0.1318(3) 0.6548(10) 0.142(3) Uani 1 1 d U . .
O13 O 0.5822(7) 0.0590(4) 0.6010(11) 0.176(4) Uani 1 1 d U . .
O14 O 0.7167(5) 0.0805(3) 0.7768(7) 0.134(3) Uani 1 1 d U . .
N N 0.3077(12) 0.2646(4) 0.5734(14) 0.160(5) Uani 1 1 d D . .
C28 C 0.3869(17) 0.3448(5) 0.613(3) 0.243(13) Uani 1 1 d D . .
H28A H 0.4435 0.3430 0.6951 0.365 Uiso 1 1 calc R . .
H28B H 0.3554 0.3692 0.6077 0.365 Uiso 1 1 calc R . .
H28C H 0.3927 0.3493 0.5546 0.365 Uiso 1 1 calc R . .
C29 C 0.3366(14) 0.3006(6) 0.5812(19) 0.190(8) Uani 1 1 d D . .
Ru` Ru 0.35542(2) 0.384002(11) 0.10382(3) 0.04091(11) Uani 1 1 d . . .
O1` O 0.3719(4) 0.42350(19) 0.2953(5) 0.0830(15) Uani 1 1 d . . .
O2` O 0.2633(3) 0.25554(14) 0.0318(4) 0.0681(12) Uani 1 1 d . . .
N1` N 0.3094(3) 0.32348(15) 0.1095(4) 0.0484(10) Uani 1 1 d . . .
N2` N 0.3379(3) 0.34564(15) -0.0303(4) 0.0473(10) Uani 1 1 d . . .
N3` N 0.2379(3) 0.41403(15) -0.0484(4) 0.0500(11) Uani 1 1 d . . .
N4` N 0.3992(3) 0.43609(14) 0.0761(4) 0.0456(10) Uani 1 1 d . . .
N5` N 0.4868(3) 0.36867(14) 0.2249(4) 0.0471(10) Uani 1 1 d . . .
N6` N 0.3656(3) 0.40990(17) 0.2197(5) 0.0554(12) Uani 1 1 d . . .
C1` C 0.2682(4) 0.2590(2) 0.1302(6) 0.0704(19) Uani 1 1 d . . .
C2` C 0.2473(5) 0.2260(3) 0.1719(8) 0.088(3) Uani 1 1 d . . .
H2` H 0.2279 0.1979 0.1363 0.106 Uiso 1 1 calc R . .
C3` C 0.2572(7) 0.2383(4) 0.2667(11) 0.116(4) Uani 1 1 d . . .
H3` H 0.2468 0.2177 0.3019 0.139 Uiso 1 1 calc R . .
C4` C 0.2823(11) 0.2802(5) 0.3140(13) 0.152(5) Uani 1 1 d . . .
H4` H 0.2827 0.2873 0.3754 0.183 Uiso 1 1 calc R . .
C5` C 0.3073(8) 0.3132(3) 0.2787(9) 0.108(3) Uani 1 1 d . . .
H5` H 0.3296 0.3406 0.3184 0.130 Uiso 1 1 calc R . .
C6` C 0.2957(4) 0.3011(2) 0.1775(6) 0.0597(14) Uani 1 1 d . . .
C7` C 0.2898(4) 0.29477(19) 0.0278(5) 0.0561(14) Uani 1 1 d . . .
C8` C 0.3002(4) 0.3052(2) -0.0556(5) 0.0565(14) Uani 1 1 d . . .
C9` C 0.2762(6) 0.2778(3) -0.1471(7) 0.084(2) Uani 1 1 d . . .
H9` H 0.2486 0.2509 -0.1626 0.101 Uiso 1 1 calc R . .
C10` C 0.2945(8) 0.2914(3) -0.2182(9) 0.105(3) Uani 1 1 d . . .
H10` H 0.2786 0.2738 -0.2826 0.126 Uiso 1 1 calc R . .
C11` C 0.3369(8) 0.3316(3) -0.1894(9) 0.102(3) Uani 1 1 d . . .
H11` H 0.3518 0.3407 -0.2327 0.123 Uiso 1 1 calc R . .
C12` C 0.3568(5) 0.3581(2) -0.0974(7) 0.0663(16) Uani 1 1 d . . .
H12` H 0.3840 0.3853 -0.0806 0.080 Uiso 1 1 calc R . .
C13` C 0.1571(4) 0.3990(2) -0.1131(6) 0.0619(15) Uani 1 1 d . . .
H13` H 0.1490 0.3735 -0.0867 0.074 Uiso 1 1 calc R . .
C14` C 0.0849(4) 0.4211(3) -0.2196(8) 0.080(2) Uani 1 1 d . . .
H14` H 0.0292 0.4099 -0.2650 0.096 Uiso 1 1 calc R . .
C15` C 0.0968(5) 0.4589(3) -0.2557(8) 0.085(2) Uani 1 1 d . . .
H15` H 0.0495 0.4737 -0.3267 0.102 Uiso 1 1 calc R . .
C16` C 0.1799(5) 0.4752(2) -0.1864(7) 0.0735(18) Uani 1 1 d . . .
H16` H 0.1887 0.5016 -0.2092 0.088 Uiso 1 1 calc R . .
C17` C 0.2493(4) 0.45231(18) -0.0839(6) 0.0522(13) Uani 1 1 d . . .
C18` C 0.3397(4) 0.4656(2) -0.0098(6) 0.0564(14) Uani 1 1 d . . .
C19` C 0.3706(5) 0.5041(2) -0.0213(7) 0.0693(17) Uani 1 1 d . . .
H19` H 0.3319 0.5261 -0.0775 0.083 Uiso 1 1 calc R . .
C20` C 0.4568(5) 0.5095(3) 0.0494(7) 0.080(2) Uani 1 1 d . . .
H20` H 0.4770 0.5349 0.0402 0.096 Uiso 1 1 calc R . .
C21` C 0.5165(5) 0.4768(3) 0.1371(7) 0.0717(18) Uani 1 1 d . . .
H21` H 0.5759 0.4804 0.1859 0.086 Uiso 1 1 calc R . .
C22` C 0.4846(4) 0.4399(2) 0.1482(5) 0.0563(14) Uani 1 1 d . . .
C23` C 0.5346(4) 0.4010(2) 0.2316(5) 0.0536(13) Uani 1 1 d . . .
C24` C 0.6240(4) 0.3959(3) 0.3070(7) 0.0727(18) Uani 1 1 d . . .
H24` H 0.6572 0.4178 0.3118 0.087 Uiso 1 1 calc R . .
C25` C 0.6609(5) 0.3570(4) 0.3742(8) 0.090(2) Uani 1 1 d . . .
H25` H 0.7204 0.3527 0.4260 0.108 Uiso 1 1 calc R . .
C26` C 0.6131(5) 0.3252(3) 0.3668(7) 0.079(2) Uani 1 1 d . . .
H26` H 0.6391 0.2992 0.4129 0.094 Uiso 1 1 calc R . .
C27` C 0.5243(4) 0.3317(2) 0.2892(6) 0.0629(15) Uani 1 1 d . . .
H27` H 0.4906 0.3096 0.2824 0.076 Uiso 1 1 calc R . .
Cl1` Cl 0.11041(16) 0.17350(7) 0.5675(2) 0.0876(5) Uani 1 1 d U . .
O3` O 0.1658(9) 0.1409(5) 0.6216(11) 0.226(7) Uani 1 1 d U . .
O4' O 0.0464(7) 0.1659(5) 0.5602(11) 0.181(3) Uani 1 1 d U . .
O5` O 0.1064(8) 0.2052(4) 0.6221(10) 0.193(4) Uani 1 1 d U . .
O6` O 0.0606(6) 0.1806(3) 0.4395(7) 0.133(3) Uani 1 1 d U . .
Cl2` Cl 0.31068(11) 0.45650(7) 0.69327(16) 0.0754(5) Uani 1 1 d U . .
O7` O 0.2389(5) 0.4509(5) 0.6742(8) 0.171(4) Uani 1 1 d U . .
O8` O 0.3834(4) 0.4479(3) 0.8166(6) 0.135(3) Uani 1 1 d U . .
O9` O 0.3089(6) 0.4294(4) 0.6161(9) 0.175(4) Uani 1 1 d U . .
O10` O 0.3125(9) 0.4943(4) 0.6489(11) 0.208(5) Uani 1 1 d U . .
Cl3` Cl 0.50411(14) 0.20879(6) 0.26117(17) 0.0744(4) Uani 1 1 d U . .
O11` O 0.5106(8) 0.2263(3) 0.3558(8) 0.152(3) Uani 1 1 d U . .
O12` O 0.4598(5) 0.1675(2) 0.2179(7) 0.124(2) Uani 1 1 d U . .
O13` O 0.5833(5) 0.2058(3) 0.2925(10) 0.142(3) Uani 1 1 d U . .
O14` O 0.4531(5) 0.2400(2) 0.1622(6) 0.0989(17) Uani 1 1 d U . .
N' N 0.6452(15) 0.1714(9) -0.0070(17) 0.143(9) Uani 0.50 1 d PD . .
C28' C 0.612(2) 0.1269(9) 0.108(3) 0.122(9) Uani 0.50 1 d PD . .
H28D H 0.6472 0.1376 0.1917 0.183 Uiso 0.50 1 calc PR . .
H28E H 0.6256 0.0963 0.1101 0.183 Uiso 0.50 1 calc PR . .
H28F H 0.5515 0.1294 0.0655 0.183 Uiso 0.50 1 calc PR . .
C29' C 0.6286(13) 0.1536(8) 0.0436(19) 0.149(14) Uani 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
Ru 0.0491(2) 0.0332(2) 0.0499(2) 0.0013(2) 0.03760(19) -0.0015(2)
O1 0.093(4) 0.078(4) 0.119(4) 0.046(3) 0.079(4) 0.045(3)
O2 0.061(2) 0.051(2) 0.064(2) 0.0134(19) 0.038(2) -0.0083(19)
N1 0.049(2) 0.045(2) 0.054(2) 0.001(2) 0.037(2) -0.002(2)
N2 0.048(2) 0.049(3) 0.049(2) 0.008(2) 0.033(2) 0.007(2)
N3 0.054(3) 0.034(2) 0.053(3) -0.0029(19) 0.038(2) 0.0039(18)
N4 0.068(3) 0.037(2) 0.060(3) -0.010(2) 0.052(2) -0.013(2)
N5 0.078(3) 0.048(3) 0.062(3) -0.006(2) 0.058(3) -0.007(2)
N6 0.065(3) 0.047(3) 0.066(3) 0.008(2) 0.051(3) 0.002(2)
C1 0.060(3) 0.052(3) 0.073(4) 0.004(3) 0.047(3) -0.009(3)
C2 0.066(4) 0.065(4) 0.082(5) 0.008(3) 0.046(4) -0.016(3)
C3 0.064(4) 0.076(5) 0.096(5) -0.010(4) 0.050(4) -0.027(4)
C4 0.045(3) 0.088(5) 0.092(5) 0.010(4) 0.037(4) -0.005(3)
C5 0.065(4) 0.057(4) 0.086(5) 0.006(3) 0.053(4) 0.001(3)
C6 0.044(3) 0.053(3) 0.047(3) -0.002(2) 0.029(2) -0.009(2)
C7 0.053(3) 0.038(3) 0.058(3) 0.010(2) 0.036(3) 0.001(2)
C8 0.059(3) 0.037(3) 0.054(3) 0.007(2) 0.037(3) -0.003(2)
C9 0.058(3) 0.051(4) 0.061(4) 0.012(3) 0.034(3) 0.010(3)
C10 0.060(4) 0.073(5) 0.071(4) 0.012(4) 0.034(3) 0.015(3)
C11 0.047(3) 0.080(5) 0.081(5) 0.008(4) 0.035(3) 0.007(3)
C12 0.054(3) 0.060(4) 0.071(4) -0.002(3) 0.044(3) -0.007(3)
C13 0.060(3) 0.047(3) 0.056(3) -0.012(3) 0.038(3) -0.006(3)
C14 0.081(5) 0.074(5) 0.065(4) -0.030(4) 0.044(4) 0.000(4)
C15 0.091(5) 0.085(5) 0.064(4) -0.007(4) 0.057(4) 0.005(4)
C16 0.077(4) 0.066(4) 0.070(4) -0.007(3) 0.057(4) 0.000(3)
C17 0.056(3) 0.044(3) 0.048(3) 0.007(2) 0.038(3) 0.006(2)
C18 0.055(3) 0.045(3) 0.048(3) 0.000(2) 0.041(3) 0.000(2)
C19 0.087(4) 0.054(4) 0.081(4) -0.004(3) 0.071(4) -0.012(3)
C20 0.124(6) 0.064(4) 0.105(5) -0.034(4) 0.097(6) -0.054(4)
C21 0.104(5) 0.069(5) 0.086(5) -0.032(4) 0.073(5) -0.041(4)
C22 0.093(4) 0.048(3) 0.076(4) -0.022(3) 0.070(4) -0.026(3)
C23 0.119(6) 0.068(4) 0.079(4) -0.032(4) 0.085(5) -0.035(4)
C24 0.176(10) 0.106(7) 0.123(7) -0.061(6) 0.129(8) -0.071(7)
C25 0.227(13) 0.123(9) 0.129(8) -0.054(7) 0.156(10) -0.060(9)
C26 0.152(8) 0.111(7) 0.104(6) -0.013(5) 0.114(7) -0.022(6)
C27 0.090(5) 0.072(4) 0.079(4) 0.002(4) 0.072(4) 0.000(4)
Cl1 0.1019(16) 0.0723(13) 0.0936(14) -0.0179(10) 0.0704(13) -0.0191(10)
O3 0.173(8) 0.137(7) 0.134(6) -0.034(5) 0.060(6) -0.041(7)
O4 0.153(7) 0.214(12) 0.255(12) 0.011(8) 0.146(8) -0.006(6)
O5 0.179(9) 0.137(7) 0.437(16) -0.118(9) 0.164(11) -0.031(7)
O6 0.246(11) 0.184(9) 0.184(8) 0.053(7) 0.145(8) 0.026(8)
Cl2 0.0621(8) 0.0640(9) 0.0751(10) 0.0004(7) 0.0443(8) 0.0030(7)
O7 0.125(6) 0.141(6) 0.170(7) -0.074(6) 0.093(5) -0.031(5)
O8 0.070(3) 0.092(5) 0.182(7) -0.050(5) 0.048(4) -0.004(3)
O9 0.105(5) 0.109(5) 0.125(5) 0.034(4) 0.036(4) -0.015(4)
O10 0.218(9) 0.185(9) 0.183(8) -0.005(6) 0.164(8) -0.039(7)
Cl3 0.0916(13) 0.0816(12) 0.1121(14) 0.0417(11) 0.0781(12) 0.0320(10)
O11 0.191(9) 0.275(12) 0.156(7) 0.023(8) 0.144(7) 0.003(8)
O12 0.135(6) 0.096(5) 0.173(8) 0.028(5) 0.098(6) 0.035(4)
O13 0.125(6) 0.134(6) 0.186(8) 0.017(6) 0.074(6) -0.019(5)
O14 0.130(5) 0.100(5) 0.107(4) 0.034(4) 0.056(4) 0.017(4)
N 0.281(17) 0.118(8) 0.192(12) 0.032(9) 0.205(13) 0.031(10)
C28 0.39(3) 0.094(10) 0.49(4) -0.046(17) 0.39(3) -0.037(15)
C29 0.25(2) 0.23(2) 0.174(14) -0.008(17) 0.178(16) 0.02(2)
Ru` 0.0499(2) 0.03329(19) 0.0475(2) -0.0028(2) 0.03652(19) -0.0046(2)
O1` 0.108(4) 0.085(4) 0.090(3) -0.028(3) 0.081(3) -0.015(3)
O2` 0.076(3) 0.042(2) 0.068(3) -0.0015(19) 0.042(2) -0.021(2)
N1` 0.055(3) 0.043(2) 0.046(2) 0.002(2) 0.034(2) -0.008(2)
N2` 0.058(3) 0.043(2) 0.048(2) -0.0015(19) 0.039(2) 0.002(2)
N3` 0.054(3) 0.040(2) 0.062(3) 0.005(2) 0.042(2) 0.007(2)
N4` 0.054(3) 0.034(2) 0.058(3) 0.000(2) 0.042(2) -0.0044(19)
N5` 0.049(2) 0.045(3) 0.047(2) -0.0052(19) 0.032(2) -0.0056(19)
N6` 0.063(3) 0.048(3) 0.064(3) -0.010(2) 0.047(3) -0.007(2)
C1` 0.059(4) 0.064(4) 0.058(4) 0.009(3) 0.029(3) -0.019(3)
C2` 0.074(4) 0.079(5) 0.091(5) 0.023(4) 0.049(4) -0.017(4)
C3` 0.132(8) 0.123(9) 0.117(8) 0.037(7) 0.095(7) -0.013(7)
C4` 0.253(16) 0.146(11) 0.155(10) 0.013(9) 0.177(12) -0.024(11)
C5` 0.177(10) 0.101(7) 0.099(6) 0.001(5) 0.115(7) -0.025(6)
C6` 0.068(4) 0.055(4) 0.060(3) 0.012(3) 0.045(3) -0.003(3)
C7` 0.061(3) 0.039(3) 0.053(3) -0.006(2) 0.033(3) -0.014(2)
C8` 0.069(4) 0.043(3) 0.055(3) -0.003(2) 0.041(3) -0.003(3)
C9` 0.120(6) 0.063(4) 0.079(5) -0.017(4) 0.072(5) -0.010(4)
C10` 0.166(9) 0.078(6) 0.100(6) -0.032(5) 0.103(7) -0.013(6)
C11` 0.160(9) 0.097(7) 0.111(7) -0.010(5) 0.117(7) -0.013(6)
C12` 0.090(5) 0.059(4) 0.078(4) -0.007(3) 0.068(4) -0.007(3)
C13` 0.050(3) 0.056(4) 0.075(4) -0.001(3) 0.041(3) -0.006(3)
C14` 0.049(3) 0.076(5) 0.092(5) 0.005(4) 0.040(4) 0.000(3)
C15` 0.061(4) 0.083(6) 0.088(5) 0.022(4) 0.043(4) 0.018(4)
C16` 0.077(4) 0.057(4) 0.096(5) 0.016(4) 0.063(4) 0.012(3)
C17` 0.064(3) 0.040(3) 0.070(3) 0.008(3) 0.053(3) 0.006(3)
C18` 0.071(4) 0.045(3) 0.067(4) -0.004(3) 0.052(3) -0.009(3)
C19` 0.090(5) 0.039(3) 0.078(4) 0.003(3) 0.057(4) -0.008(3)
C20` 0.088(5) 0.073(5) 0.083(5) -0.007(4) 0.060(4) -0.035(4)
C21` 0.063(4) 0.068(4) 0.073(4) 0.000(3) 0.043(3) -0.022(3)
C22` 0.061(3) 0.056(4) 0.057(3) -0.008(3) 0.043(3) -0.016(3)
C23` 0.047(3) 0.062(4) 0.047(3) -0.005(3) 0.030(2) -0.005(3)
C24` 0.053(3) 0.090(5) 0.077(4) 0.000(4) 0.045(3) 0.000(3)
C25` 0.048(4) 0.122(7) 0.077(5) -0.001(5) 0.034(4) 0.017(4)
C26` 0.070(4) 0.077(5) 0.072(5) 0.008(4) 0.042(4) 0.011(4)
C27` 0.064(4) 0.050(3) 0.054(3) 0.001(3) 0.033(3) 0.010(3)
Cl1` 0.1068(14) 0.0806(12) 0.0961(13) 0.0168(10) 0.0777(12) 0.0233(11)
O3` 0.160(8) 0.205(10) 0.142(8) 0.017(7) 0.037(7) 0.104(8)
O4' 0.141(5) 0.241(7) 0.164(6) 0.016(6) 0.106(5) -0.006(5)
O5` 0.203(6) 0.159(6) 0.141(5) -0.026(5) 0.089(5) 0.039(5)
O6` 0.163(6) 0.132(6) 0.106(4) 0.029(4) 0.092(5) 0.039(5)
Cl2` 0.0663(9) 0.0851(12) 0.0663(9) -0.0021(8) 0.0423(8) -0.0066(8)
O7` 0.080(4) 0.316(13) 0.122(5) 0.026(7) 0.072(4) 0.000(6)
O8` 0.084(4) 0.218(8) 0.079(3) 0.029(4) 0.047(3) -0.008(5)
O9` 0.117(5) 0.223(9) 0.136(6) -0.073(7) 0.069(5) 0.001(6)
O10` 0.258(11) 0.135(6) 0.192(8) 0.064(6) 0.139(8) -0.017(8)
Cl3` 0.1100(13) 0.0592(9) 0.0797(10) -0.0039(8) 0.0751(10) -0.0104(9)
O11` 0.285(9) 0.115(5) 0.146(5) -0.045(4) 0.183(7) -0.067(6)
O12` 0.177(6) 0.088(4) 0.157(6) -0.032(4) 0.135(6) -0.041(4)
O13` 0.110(5) 0.139(7) 0.184(7) 0.004(6) 0.104(5) 0.007(4)
O14` 0.127(4) 0.090(4) 0.086(3) 0.006(3) 0.075(3) 0.023(3)
N' 0.136(16) 0.17(2) 0.065(10) 0.015(11) 0.046(11) 0.038(15)
C28' 0.14(2) 0.12(2) 0.087(14) -0.005(11) 0.069(15) 0.033(13)
C29' 0.113(18) 0.095(17) 0.062(13) -0.001(11) -0.008(13) 0.009(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'
Cl Cl 0.1484 0.1585 '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'
Ru Ru -1.2594 0.8363 '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
N6 Ru N4 95.2(2) . . ?
N6 Ru N3 94.0(2) . . ?
N4 Ru N3 79.30(18) . . ?
N6 Ru N5 94.5(2) . . ?
N4 Ru N5 79.97(18) . . ?
N3 Ru N5 158.21(19) . . ?
N6 Ru N1 95.7(2) . . ?
N4 Ru N1 169.0(2) . . ?
N3 Ru N1 99.05(18) . . ?
N5 Ru N1 100.02(18) . . ?
N6 Ru N2 172.3(2) . . ?
N4 Ru N2 92.1(2) . . ?
N3 Ru N2 89.65(17) . . ?
N5 Ru N2 84.5(2) . . ?
N1 Ru N2 77.04(18) . . ?
C7 O2 C1 103.9(4) . . ?
C7 N1 C6 105.9(5) . . ?
C7 N1 Ru 113.9(4) . . ?
C6 N1 Ru 140.2(4) . . ?
C12 N2 C8 117.8(5) . . ?
C12 N2 Ru 127.3(4) . . ?
C8 N2 Ru 114.5(4) . . ?
C13 N3 C17 119.9(5) . . ?
C13 N3 Ru 126.9(4) . . ?
C17 N3 Ru 113.2(3) . . ?
C18 N4 C22 123.5(5) . . ?
C18 N4 Ru 118.7(4) . . ?
C22 N4 Ru 117.8(3) . . ?
C27 N5 C23 120.1(5) . . ?
C27 N5 Ru 127.5(5) . . ?
C23 N5 Ru 112.4(4) . . ?
O1 N6 Ru 177.4(5) . . ?
C6 C1 C2 123.9(6) . . ?
C6 C1 O2 109.2(5) . . ?
C2 C1 O2 126.9(6) . . ?
C3 C2 C1 113.9(6) . . ?
C3 C2 H2 123.1 . . ?
C1 C2 H2 123.1 . . ?
C2 C3 C4 123.5(6) . . ?
C2 C3 H3 118.3 . . ?
C4 C3 H3 118.3 . . ?
C3 C4 C5 120.6(7) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 H4 119.7 . . ?
C6 C5 C4 116.0(6) . . ?
C6 C5 H5 122.0 . . ?
C4 C5 H5 122.0 . . ?
C1 C6 C5 122.1(5) . . ?
C1 C6 N1 105.8(5) . . ?
C5 C6 N1 132.1(5) . . ?
N1 C7 O2 115.2(5) . . ?
N1 C7 C8 121.4(5) . . ?
O2 C7 C8 123.2(5) . . ?
C9 C8 N2 122.3(5) . . ?
C9 C8 C7 126.1(5) . . ?
N2 C8 C7 111.6(5) . . ?
C8 C9 C10 119.0(6) . . ?
C8 C9 H9 120.5 . . ?
C10 C9 H9 120.5 . . ?
C11 C10 C9 117.9(7) . . ?
C11 C10 H10 121.1 . . ?
C9 C10 H10 121.1 . . ?
C12 C11 C10 121.1(6) . . ?
C12 C11 H11 119.5 . . ?
C10 C11 H11 119.4 . . ?
N2 C12 C11 121.6(6) . . ?
N2 C12 H12 119.2 . . ?
C11 C12 H12 119.2 . . ?
N3 C13 C14 120.4(6) . . ?
N3 C13 H13 119.8 . . ?
C14 C13 H13 119.8 . . ?
C15 C14 C13 120.3(6) . . ?
C15 C14 H14 119.9 . . ?
C13 C14 H14 119.9 . . ?
C14 C15 C16 118.3(6) . . ?
C14 C15 H15 120.9 . . ?
C16 C15 H15 120.9 . . ?
C17 C16 C15 119.4(7) . . ?
C17 C16 H16 120.3 . . ?
C15 C16 H16 120.3 . . ?
C16 C17 N3 121.3(6) . . ?
C16 C17 C18 123.8(5) . . ?
N3 C17 C18 114.8(4) . . ?
N4 C18 C19 118.9(5) . . ?
N4 C18 C17 113.8(5) . . ?
C19 C18 C17 127.3(5) . . ?
C18 C19 C20 118.0(5) . . ?
C18 C19 H19 121.0 . . ?
C20 C19 H19 121.0 . . ?
C21 C20 C19 122.9(6) . . ?
C21 C20 H20 118.6 . . ?
C19 C20 H20 118.6 . . ?
C20 C21 C22 117.2(6) . . ?
C20 C21 H21 121.4 . . ?
C22 C21 H21 121.4 . . ?
N4 C22 C21 119.3(5) . . ?
N4 C22 C23 112.9(5) . . ?
C21 C22 C23 127.8(6) . . ?
N5 C23 C24 121.2(6) . . ?
N5 C23 C22 116.6(5) . . ?
C24 C23 C22 121.8(7) . . ?
C25 C24 C23 118.0(8) . . ?
C25 C24 H24 121.0 . . ?
C23 C24 H24 121.0 . . ?
C24 C25 C26 120.7(8) . . ?
C24 C25 H25 119.7 . . ?
C26 C25 H25 119.7 . . ?
C27 C26 C25 119.5(7) . . ?
C27 C26 H26 120.2 . . ?
C25 C26 H26 120.2 . . ?
N5 C27 C26 120.5(7) . . ?
N5 C27 H27 119.8 . . ?
C26 C27 H27 119.8 . . ?
O5 Cl1 O3 118.8(11) . . ?
O5 Cl1 O4 96.5(10) . . ?
O3 Cl1 O4 107.5(10) . . ?
O5 Cl1 O6 138.7(14) . . ?
O3 Cl1 O6 96.8(8) . . ?
O4 Cl1 O6 91.6(9) . . ?
O10 Cl2 O8 113.2(7) . . ?
O10 Cl2 O7 108.9(7) . . ?
O8 Cl2 O7 115.3(5) . . ?
O10 Cl2 O9 103.2(7) . . ?
O8 Cl2 O9 105.4(5) . . ?
O7 Cl2 O9 110.1(6) . . ?
O11 Cl3 O12 106.7(9) . . ?
O11 Cl3 O13 116.1(9) . . ?
O12 Cl3 O13 110.1(7) . . ?
O11 Cl3 O14 108.9(7) . . ?
O12 Cl3 O14 107.4(6) . . ?
O13 Cl3 O14 107.2(6) . . ?
C29 C28 H28A 109.4 . . ?
C29 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C29 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N C29 C28 171(3) . . ?
N6` Ru` N4` 95.3(2) . . ?
N6` Ru` N5` 93.5(2) . . ?
N4` Ru` N5` 79.45(18) . . ?
N6` Ru` N1` 95.3(2) . . ?
N4` Ru` N1` 169.36(18) . . ?
N5` Ru` N1` 99.02(18) . . ?
N6` Ru` N3` 96.9(2) . . ?
N4` Ru` N3` 79.41(19) . . ?
N5` Ru` N3` 157.18(19) . . ?
N1` Ru` N3` 100.16(18) . . ?
N6` Ru` N2` 172.5(2) . . ?
N4` Ru` N2` 92.26(18) . . ?
N5` Ru` N2` 87.57(18) . . ?
N1` Ru` N2` 77.14(18) . . ?
N3` Ru` N2` 84.76(18) . . ?
C7` O2` C1` 104.6(5) . . ?
C7` N1` C6` 105.2(5) . . ?
C7` N1` Ru` 113.4(4) . . ?
C6` N1` Ru` 141.2(4) . . ?
C12` N2` C8` 117.3(5) . . ?
C12` N2` Ru` 126.5(4) . . ?
C8` N2` Ru` 116.1(4) . . ?
C13` N3` C17` 119.2(5) . . ?
C13` N3` Ru` 127.9(4) . . ?
C17` N3` Ru` 112.9(4) . . ?
C22` N4` C18` 125.4(5) . . ?
C22` N4` Ru` 117.9(4) . . ?
C18` N4` Ru` 116.6(4) . . ?
C27` N5` C23` 120.2(5) . . ?
C27` N5` Ru` 126.6(4) . . ?
C23` N5` Ru` 113.1(4) . . ?
O1` N6` Ru` 175.3(5) . . ?
C6` C1` C2` 125.7(8) . . ?
C6` C1` O2` 107.8(5) . . ?
C2` C1` O2` 126.6(7) . . ?
C3` C2` C1` 114.1(9) . . ?
C3` C2` H2` 123.0 . . ?
C1` C2` H2` 123.0 . . ?
C2` C3` C4` 121.9(8) . . ?
C2` C3` H3` 119.0 . . ?
C4` C3` H3` 119.1 . . ?
C3` C4` C5` 125.6(10) . . ?
C3` C4` H4` 117.2 . . ?
C5` C4` H4` 117.2 . . ?
C4` C5` C6` 113.0(10) . . ?
C4` C5` H5` 123.5 . . ?
C6` C5` H5` 123.5 . . ?
C1` C6` C5` 119.5(6) . . ?
C1` C6` N1` 107.5(6) . . ?
C5` C6` N1` 133.0(7) . . ?
N1` C7` O2` 114.9(5) . . ?
N1` C7` C8` 121.3(5) . . ?
O2` C7` C8` 123.7(5) . . ?
C9` C8` N2` 124.4(6) . . ?
C9` C8` C7` 124.0(6) . . ?
N2` C8` C7` 111.6(5) . . ?
C8` C9` C10` 117.9(8) . . ?
C8` C9` H9` 121.0 . . ?
C10` C9` H9` 121.0 . . ?
C11` C10` C9` 118.3(7) . . ?
C11` C10` H10` 120.9 . . ?
C9` C10` H10` 120.9 . . ?
C12` C11` C10` 120.2(7) . . ?
C12` C11` H11` 119.9 . . ?
C10` C11` H11` 119.9 . . ?
N2` C12` C11` 121.7(7) . . ?
N2` C12` H12` 119.1 . . ?
C11` C12` H12` 119.1 . . ?
N3` C13` C14` 121.1(6) . . ?
N3` C13` H13` 119.4 . . ?
C14` C13` H13` 119.4 . . ?
C15` C14` C13` 119.3(7) . . ?
C15` C14` H14` 120.3 . . ?
C13` C14` H14` 120.4 . . ?
C14` C15` C16` 119.5(7) . . ?
C14` C15` H15` 120.3 . . ?
C16` C15` H15` 120.3 . . ?
C17` C16` C15` 119.7(7) . . ?
C17` C16` H16` 120.1 . . ?
C15` C16` H16` 120.1 . . ?
N3` C17` C16` 121.1(6) . . ?
N3` C17` C18` 115.5(5) . . ?
C16` C17` C18` 123.4(5) . . ?
N4` C18` C19` 116.9(6) . . ?
N4` C18` C17` 115.1(5) . . ?
C19` C18` C17` 127.9(6) . . ?
C20` C19` C18` 120.0(7) . . ?
C20` C19` H19` 120.0 . . ?
C18` C19` H19` 120.0 . . ?
C19` C20` C21` 120.6(6) . . ?
C19` C20` H20` 119.7 . . ?
C21` C20` H20` 119.7 . . ?
C22` C21` C20` 118.2(6) . . ?
C22` C21` H21` 120.9 . . ?
C20` C21` H21` 120.9 . . ?
N4` C22` C21` 118.9(6) . . ?
N4` C22` C23` 113.4(5) . . ?
C21` C22` C23` 127.6(6) . . ?
N5` C23` C24` 120.8(6) . . ?
N5` C23` C22` 115.7(5) . . ?
C24` C23` C22` 123.3(6) . . ?
C25` C24` C23` 117.0(7) . . ?
C25` C24` H24` 121.5 . . ?
C23` C24` H24` 121.5 . . ?
C26` C25` C24` 121.7(7) . . ?
C26` C25` H25` 119.2 . . ?
C24` C25` H25` 119.2 . . ?
C25` C26` C27` 118.9(8) . . ?
C25` C26` H26` 120.5 . . ?
C27` C26` H26` 120.5 . . ?
N5` C27` C26` 121.3(7) . . ?
N5` C27` H27` 119.4 . . ?
C26` C27` H27` 119.4 . . ?
O5` Cl1` O3` 126.1(8) . . ?
O5` Cl1` O4' 70.6(9) . . ?
O3` Cl1` O4' 111.4(11) . . ?
O5` Cl1` O6` 114.9(6) . . ?
O3` Cl1` O6` 117.8(8) . . ?
O4' Cl1` O6` 98.1(7) . . ?
Cl1` O4' O5` 54.3(7) . . ?
Cl1` O5` O4' 55.1(6) . . ?
O10` Cl2` O7` 114.4(9) . . ?
O10` Cl2` O9` 95.0(9) . . ?
O7` Cl2` O9` 111.5(7) . . ?
O10` Cl2` O8` 115.5(7) . . ?
O7` Cl2` O8` 108.9(5) . . ?
O9` Cl2` O8` 110.9(6) . . ?
O13` Cl3` O12` 111.4(5) . . ?
O13` Cl3` O11` 114.6(6) . . ?
O12` Cl3` O11` 111.0(4) . . ?
O13` Cl3` O14` 105.8(5) . . ?
O12` Cl3` O14` 108.2(5) . . ?
O11` Cl3` O14` 105.5(5) . . ?
C29' C28' H28D 113.2 . . ?
C29' C28' H28E 113.5 . . ?
H28D C28' H28E 105.3 . . ?
C29' C28' H28F 113.4 . . ?
H28D C28' H28F 105.4 . . ?
H28E C28' H28F 105.3 . . ?
N' C29' C28' 174(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
Ru N6 1.753(5) . ?
Ru N4 1.982(4) . ?
Ru N3 2.075(5) . ?
Ru N5 2.081(5) . ?
Ru N1 2.082(4) . ?
Ru N2 2.116(4) . ?
O1 N6 1.126(7) . ?
O2 C7 1.326(7) . ?
O2 C1 1.395(8) . ?
N1 C7 1.284(7) . ?
N1 C6 1.421(7) . ?
N2 C12 1.327(8) . ?
N2 C8 1.366(7) . ?
N3 C13 1.316(7) . ?
N3 C17 1.394(7) . ?
N4 C18 1.348(6) . ?
N4 C22 1.357(7) . ?
N5 C27 1.353(7) . ?
N5 C23 1.354(8) . ?
C1 C6 1.357(8) . ?
C1 C2 1.394(9) . ?
C2 C3 1.366(11) . ?
C2 H2 0.9300 . ?
C3 C4 1.395(12) . ?
C3 H3 0.9300 . ?
C4 C5 1.399(10) . ?
C4 H4 0.9300 . ?
C5 C6 1.364(9) . ?
C5 H5 0.9300 . ?
C7 C8 1.436(8) . ?
C8 C9 1.355(8) . ?
C9 C10 1.379(10) . ?
C9 H9 0.9300 . ?
C10 C11 1.361(11) . ?
C10 H10 0.9300 . ?
C11 C12 1.353(10) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C14 1.423(10) . ?
C13 H13 0.9300 . ?
C14 C15 1.352(12) . ?
C14 H14 0.9300 . ?
C15 C16 1.428(11) . ?
C15 H15 0.9300 . ?
C16 C17 1.344(8) . ?
C16 H16 0.9300 . ?
C17 C18 1.461(8) . ?
C18 C19 1.374(8) . ?
C19 C20 1.388(9) . ?
C19 H19 0.9300 . ?
C20 C21 1.371(10) . ?
C20 H20 0.9300 . ?
C21 C22 1.387(9) . ?
C21 H21 0.9300 . ?
C22 C23 1.477(8) . ?
C23 C24 1.392(10) . ?
C24 C25 1.375(12) . ?
C24 H24 0.9300 . ?
C25 C26 1.374(14) . ?
C25 H25 0.9300 . ?
C26 C27 1.375(11) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
Cl1 O5 1.209(12) . ?
Cl1 O3 1.336(10) . ?
Cl1 O4 1.398(12) . ?
Cl1 O6 1.406(12) . ?
Cl2 O10 1.363(9) . ?
Cl2 O8 1.386(7) . ?
Cl2 O7 1.397(8) . ?
Cl2 O9 1.408(8) . ?
Cl3 O11 1.313(9) . ?
Cl3 O12 1.366(8) . ?
Cl3 O13 1.396(10) . ?
Cl3 O14 1.415(7) . ?
N C29 1.209(15) . ?
C28 C29 1.558(17) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
Ru` N6` 1.760(5) . ?
Ru` N4` 2.000(4) . ?
Ru` N5` 2.077(5) . ?
Ru` N1` 2.092(4) . ?
Ru` N3` 2.094(5) . ?
Ru` N2` 2.101(4) . ?
O1` N6` 1.113(6) . ?
O2` C7` 1.324(7) . ?
O2` C1` 1.394(9) . ?
N1` C7` 1.301(8) . ?
N1` C6` 1.398(7) . ?
N2` C12` 1.355(8) . ?
N2` C8` 1.358(8) . ?
N3` C13` 1.339(8) . ?
N3` C17` 1.353(7) . ?
N4` C22` 1.331(7) . ?
N4` C18` 1.338(8) . ?
N5` C27` 1.316(8) . ?
N5` C23` 1.355(7) . ?
C1` C6` 1.368(10) . ?
C1` C2` 1.392(10) . ?
C2` C3` 1.323(15) . ?
C2` H2` 0.9300 . ?
C3` C4` 1.357(17) . ?
C3` H3` 0.9300 . ?
C4` C5` 1.387(14) . ?
C4` H4` 0.9300 . ?
C5` C6` 1.393(11) . ?
C5` H5` 0.9300 . ?
C7` C8` 1.432(9) . ?
C8` C9` 1.354(9) . ?
C9` C10` 1.410(13) . ?
C9` H9` 0.9300 . ?
C10` C11` 1.387(13) . ?
C10` H10` 0.9300 . ?
C11` C12` 1.373(11) . ?
C11` H11` 0.9300 . ?
C12` H12` 0.9300 . ?
C13` C14` 1.399(10) . ?
C13` H13` 0.9300 . ?
C14` C15` 1.350(12) . ?
C14` H14` 0.9300 . ?
C15` C16` 1.381(11) . ?
C15` H15` 0.9300 . ?
C16` C17` 1.368(9) . ?
C16` H16` 0.9300 . ?
C17` C18` 1.464(9) . ?
C18` C19` 1.396(9) . ?
C19` C20` 1.352(11) . ?
C19` H19` 0.9300 . ?
C20` C21` 1.411(11) . ?
C20` H20` 0.9300 . ?
C21` C22` 1.366(9) . ?
C21` H21` 0.9300 . ?
C22` C23` 1.489(9) . ?
C23` C24` 1.396(9) . ?
C24` C25` 1.380(13) . ?
C24` H24` 0.9300 . ?
C25` C26` 1.338(13) . ?
C25` H25` 0.9300 . ?
C26` C27` 1.389(10) . ?
C26` H26` 0.9300 . ?
C27` H27` 0.9300 . ?
Cl1` O5` 1.290(10) . ?
Cl1` O3` 1.298(10) . ?
Cl1` O4' 1.303(10) . ?
Cl1` O6` 1.419(7) . ?
O4' O5` 1.499(17) . ?
Cl2` O10` 1.326(9) . ?
Cl2` O7` 1.352(7) . ?
Cl2` O9` 1.383(9) . ?
Cl2` O8` 1.384(7) . ?
Cl3` O13` 1.401(8) . ?
Cl3` O12` 1.415(7) . ?
Cl3` O11` 1.415(7) . ?
Cl3` O14` 1.421(6) . ?
N' C29' 1.16(2) . ?
C28' C29' 1.47(2) . ?
C28' H28D 0.9969 . ?
C28' H28E 0.9985 . ?
C28' H28F 0.9978 . ?
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
N6 Ru N1 C7 -168.8(4) . . . . ?
N4 Ru N1 C7 15.7(13) . . . . ?
N3 Ru N1 C7 96.2(4) . . . . ?
N5 Ru N1 C7 -73.2(4) . . . . ?
N2 Ru N1 C7 8.7(4) . . . . ?
N6 Ru N1 C6 12.1(6) . . . . ?
N4 Ru N1 C6 -163.4(8) . . . . ?
N3 Ru N1 C6 -83.0(6) . . . . ?
N5 Ru N1 C6 107.6(6) . . . . ?
N2 Ru N1 C6 -170.5(6) . . . . ?
N6 Ru N2 C12 -164.2(16) . . . . ?
N4 Ru N2 C12 -2.2(5) . . . . ?
N3 Ru N2 C12 77.1(5) . . . . ?
N5 Ru N2 C12 -81.9(5) . . . . ?
N1 Ru N2 C12 176.4(6) . . . . ?
N6 Ru N2 C8 8(2) . . . . ?
N4 Ru N2 C8 170.1(4) . . . . ?
N3 Ru N2 C8 -110.6(4) . . . . ?
N5 Ru N2 C8 90.4(4) . . . . ?
N1 Ru N2 C8 -11.2(4) . . . . ?
N6 Ru N3 C13 -89.1(5) . . . . ?
N4 Ru N3 C13 176.4(5) . . . . ?
N5 Ru N3 C13 158.2(5) . . . . ?
N1 Ru N3 C13 7.4(5) . . . . ?
N2 Ru N3 C13 84.2(5) . . . . ?
N6 Ru N3 C17 90.8(4) . . . . ?
N4 Ru N3 C17 -3.8(4) . . . . ?
N5 Ru N3 C17 -21.9(7) . . . . ?
N1 Ru N3 C17 -172.8(4) . . . . ?
N2 Ru N3 C17 -96.0(4) . . . . ?
N6 Ru N4 C18 -88.1(4) . . . . ?
N3 Ru N4 C18 5.0(4) . . . . ?
N5 Ru N4 C18 178.3(5) . . . . ?
N1 Ru N4 C18 87.4(11) . . . . ?
N2 Ru N4 C18 94.3(4) . . . . ?
N6 Ru N4 C22 89.8(5) . . . . ?
N3 Ru N4 C22 -177.1(5) . . . . ?
N5 Ru N4 C22 -3.8(5) . . . . ?
N1 Ru N4 C22 -94.7(11) . . . . ?
N2 Ru N4 C22 -87.8(5) . . . . ?
N6 Ru N5 C27 89.1(6) . . . . ?
N4 Ru N5 C27 -176.4(6) . . . . ?
N3 Ru N5 C27 -158.3(5) . . . . ?
N1 Ru N5 C27 -7.5(6) . . . . ?
N2 Ru N5 C27 -83.3(6) . . . . ?
N6 Ru N5 C23 -89.6(5) . . . . ?
N4 Ru N5 C23 5.0(5) . . . . ?
N3 Ru N5 C23 23.1(8) . . . . ?
N1 Ru N5 C23 173.8(5) . . . . ?
N2 Ru N5 C23 98.1(5) . . . . ?
N4 Ru N6 O1 -140(14) . . . . ?
N3 Ru N6 O1 141(14) . . . . ?
N5 Ru N6 O1 -59(14) . . . . ?
N1 Ru N6 O1 41(14) . . . . ?
N2 Ru N6 O1 22(15) . . . . ?
C7 O2 C1 C6 0.4(7) . . . . ?
C7 O2 C1 C2 -179.5(7) . . . . ?
C6 C1 C2 C3 1.5(12) . . . . ?
O2 C1 C2 C3 -178.6(7) . . . . ?
C1 C2 C3 C4 -0.7(13) . . . . ?
C2 C3 C4 C5 1.4(14) . . . . ?
C3 C4 C5 C6 -2.7(12) . . . . ?
C2 C1 C6 C5 -3.1(11) . . . . ?
O2 C1 C6 C5 177.0(6) . . . . ?
C2 C1 C6 N1 179.3(7) . . . . ?
O2 C1 C6 N1 -0.6(7) . . . . ?
C4 C5 C6 C1 3.5(10) . . . . ?
C4 C5 C6 N1 -179.7(7) . . . . ?
C7 N1 C6 C1 0.6(6) . . . . ?
Ru N1 C6 C1 179.8(5) . . . . ?
C7 N1 C6 C5 -176.7(7) . . . . ?
Ru N1 C6 C5 2.5(11) . . . . ?
C6 N1 C7 O2 -0.3(7) . . . . ?
Ru N1 C7 O2 -179.8(4) . . . . ?
C6 N1 C7 C8 174.1(5) . . . . ?
Ru N1 C7 C8 -5.4(7) . . . . ?
C1 O2 C7 N1 0.0(7) . . . . ?
C1 O2 C7 C8 -174.3(6) . . . . ?
C12 N2 C8 C9 2.8(9) . . . . ?
Ru N2 C8 C9 -170.3(5) . . . . ?
C12 N2 C8 C7 -175.2(6) . . . . ?
Ru N2 C8 C7 11.6(6) . . . . ?
N1 C7 C8 C9 177.7(6) . . . . ?
O2 C7 C8 C9 -8.3(10) . . . . ?
N1 C7 C8 N2 -4.3(8) . . . . ?
O2 C7 C8 N2 169.7(5) . . . . ?
N2 C8 C9 C10 -0.8(10) . . . . ?
C7 C8 C9 C10 176.9(7) . . . . ?
C8 C9 C10 C11 -3.9(11) . . . . ?
C9 C10 C11 C12 6.7(12) . . . . ?
C8 N2 C12 C11 0.0(10) . . . . ?
Ru N2 C12 C11 172.2(6) . . . . ?
C10 C11 C12 N2 -4.9(12) . . . . ?
C17 N3 C13 C14 -1.2(9) . . . . ?
Ru N3 C13 C14 178.7(5) . . . . ?
N3 C13 C14 C15 -1.6(11) . . . . ?
C13 C14 C15 C16 5.5(12) . . . . ?
C14 C15 C16 C17 -6.7(11) . . . . ?
C15 C16 C17 N3 4.1(10) . . . . ?
C15 C16 C17 C18 -178.4(6) . . . . ?
C13 N3 C17 C16 -0.2(8) . . . . ?
Ru N3 C17 C16 180.0(5) . . . . ?
C13 N3 C17 C18 -177.9(5) . . . . ?
Ru N3 C17 C18 2.3(6) . . . . ?
C22 N4 C18 C19 -2.1(9) . . . . ?
Ru N4 C18 C19 175.7(5) . . . . ?
C22 N4 C18 C17 177.0(6) . . . . ?
Ru N4 C18 C17 -5.2(6) . . . . ?
C16 C17 C18 N4 -176.0(6) . . . . ?
N3 C17 C18 N4 1.7(7) . . . . ?
C16 C17 C18 C19 3.1(10) . . . . ?
N3 C17 C18 C19 -179.3(6) . . . . ?
N4 C18 C19 C20 -1.4(10) . . . . ?
C17 C18 C19 C20 179.6(7) . . . . ?
C18 C19 C20 C21 5.8(13) . . . . ?
C19 C20 C21 C22 -6.4(14) . . . . ?
C18 N4 C22 C21 1.4(10) . . . . ?
Ru N4 C22 C21 -176.3(6) . . . . ?
C18 N4 C22 C23 179.8(6) . . . . ?
Ru N4 C22 C23 2.0(8) . . . . ?
C20 C21 C22 N4 2.7(12) . . . . ?
C20 C21 C22 C23 -175.4(9) . . . . ?
C27 N5 C23 C24 3.5(13) . . . . ?
Ru N5 C23 C24 -177.7(8) . . . . ?
C27 N5 C23 C22 175.8(7) . . . . ?
Ru N5 C23 C22 -5.5(9) . . . . ?
N4 C22 C23 N5 2.5(10) . . . . ?
C21 C22 C23 N5 -179.3(8) . . . . ?
N4 C22 C23 C24 174.7(9) . . . . ?
C21 C22 C23 C24 -7.1(15) . . . . ?
N5 C23 C24 C25 -2.8(17) . . . . ?
C22 C23 C24 C25 -174.7(11) . . . . ?
C23 C24 C25 C26 1(2) . . . . ?
C24 C25 C26 C27 -1(2) . . . . ?
C23 N5 C27 C26 -2.7(11) . . . . ?
Ru N5 C27 C26 178.8(6) . . . . ?
C25 C26 C27 N5 1.2(15) . . . . ?
N6` Ru` N1` C7` 177.1(4) . . . . ?
N4` Ru` N1` C7` -7.7(13) . . . . ?
N5` Ru` N1` C7` -88.5(4) . . . . ?
N3` Ru` N1` C7` 79.0(4) . . . . ?
N2` Ru` N1` C7` -3.1(4) . . . . ?
N6` Ru` N1` C6` -7.6(7) . . . . ?
N4` Ru` N1` C6` 167.6(9) . . . . ?
N5` Ru` N1` C6` 86.8(6) . . . . ?
N3` Ru` N1` C6` -105.7(6) . . . . ?
N2` Ru` N1` C6` 172.2(7) . . . . ?
N6` Ru` N2` C12` -175.7(16) . . . . ?
N4` Ru` N2` C12` 1.8(5) . . . . ?
N5` Ru` N2` C12` -77.5(5) . . . . ?
N1` Ru` N2` C12` -177.3(6) . . . . ?
N3` Ru` N2` C12` 81.0(5) . . . . ?
N6` Ru` N2` C8` 7.6(19) . . . . ?
N4` Ru` N2` C8` -174.9(4) . . . . ?
N5` Ru` N2` C8` 105.8(4) . . . . ?
N1` Ru` N2` C8` 6.0(4) . . . . ?
N3` Ru` N2` C8` -95.7(4) . . . . ?
N6` Ru` N3` C13` -91.0(5) . . . . ?
N4` Ru` N3` C13` 174.9(5) . . . . ?
N5` Ru` N3` C13` 152.5(5) . . . . ?
N1` Ru` N3` C13` 5.7(5) . . . . ?
N2` Ru` N3` C13` 81.6(5) . . . . ?
N6` Ru` N3` C17` 91.4(4) . . . . ?
N4` Ru` N3` C17` -2.7(4) . . . . ?
N5` Ru` N3` C17` -25.1(7) . . . . ?
N1` Ru` N3` C17` -171.9(4) . . . . ?
N2` Ru` N3` C17` -96.0(4) . . . . ?
N6` Ru` N4` C22` 86.5(4) . . . . ?
N5` Ru` N4` C22` -6.0(4) . . . . ?
N1` Ru` N4` C22` -88.7(11) . . . . ?
N3` Ru` N4` C22` -177.4(4) . . . . ?
N2` Ru` N4` C22` -93.1(4) . . . . ?
N6` Ru` N4` C18` -90.0(4) . . . . ?
N5` Ru` N4` C18` 177.4(4) . . . . ?
N1` Ru` N4` C18` 94.8(11) . . . . ?
N3` Ru` N4` C18` 6.1(4) . . . . ?
N2` Ru` N4` C18` 90.3(4) . . . . ?
N6` Ru` N5` C27` 91.5(5) . . . . ?
N4` Ru` N5` C27` -173.8(5) . . . . ?
N1` Ru` N5` C27` -4.5(5) . . . . ?
N3` Ru` N5` C27` -151.4(5) . . . . ?
N2` Ru` N5` C27` -81.1(5) . . . . ?
N6` Ru` N5` C23` -90.2(4) . . . . ?
N4` Ru` N5` C23` 4.5(4) . . . . ?
N1` Ru` N5` C23` 173.8(4) . . . . ?
N3` Ru` N5` C23` 26.9(7) . . . . ?
N2` Ru` N5` C23` 97.3(4) . . . . ?
N4` Ru` N6` O1` -160(6) . . . . ?
N5` Ru` N6` O1` -80(6) . . . . ?
N1` Ru` N6` O1` 19(6) . . . . ?
N3` Ru` N6` O1` 120(6) . . . . ?
N2` Ru` N6` O1` 17(8) . . . . ?
C7` O2` C1` C6` 1.5(7) . . . . ?
C7` O2` C1` C2` -179.8(7) . . . . ?
C6` C1` C2` C3` -1.0(12) . . . . ?
O2` C1` C2` C3` -179.5(8) . . . . ?
C1` C2` C3` C4` 2.6(17) . . . . ?
C2` C3` C4` C5` -6(2) . . . . ?
C3` C4` C5` C6` 7(2) . . . . ?
C2` C1` C6` C5` 2.2(12) . . . . ?
O2` C1` C6` C5` -179.1(8) . . . . ?
C2` C1` C6` N1` -179.8(7) . . . . ?
O2` C1` C6` N1` -1.1(7) . . . . ?
C4` C5` C6` C1` -4.5(15) . . . . ?
C4` C5` C6` N1` 178.1(10) . . . . ?
C7` N1` C6` C1` 0.2(7) . . . . ?
Ru` N1` C6` C1` -175.3(5) . . . . ?
C7` N1` C6` C5` 177.9(9) . . . . ?
Ru` N1` C6` C5` 2.4(13) . . . . ?
C6` N1` C7` O2` 0.8(7) . . . . ?
Ru` N1` C7` O2` 177.7(4) . . . . ?
C6` N1` C7` C8` -176.8(6) . . . . ?
Ru` N1` C7` C8` 0.1(7) . . . . ?
C1` O2` C7` N1` -1.5(7) . . . . ?
C1` O2` C7` C8` 176.1(6) . . . . ?
C12` N2` C8` C9` -3.6(10) . . . . ?
Ru` N2` C8` C9` 173.4(6) . . . . ?
C12` N2` C8` C7` 175.6(6) . . . . ?
Ru` N2` C8` C7` -7.4(7) . . . . ?
N1` C7` C8` C9` -176.0(7) . . . . ?
O2` C7` C8` C9` 6.6(11) . . . . ?
N1` C7` C8` N2` 4.9(9) . . . . ?
O2` C7` C8` N2` -172.5(5) . . . . ?
N2` C8` C9` C10` 2.4(12) . . . . ?
C7` C8` C9` C10` -176.7(8) . . . . ?
C8` C9` C10` C11` 0.8(15) . . . . ?
C9` C10` C11` C12` -2.6(16) . . . . ?
C8` N2` C12` C11` 1.6(11) . . . . ?
Ru` N2` C12` C11` -175.1(7) . . . . ?
C10` C11` C12` N2` 1.5(15) . . . . ?
C17` N3` C13` C14` 2.9(10) . . . . ?
Ru` N3` C13` C14` -174.5(5) . . . . ?
N3` C13` C14` C15` -1.8(12) . . . . ?
C13` C14` C15` C16` -0.6(13) . . . . ?
C14` C15` C16` C17` 1.8(13) . . . . ?
C13` N3` C17` C16` -1.7(9) . . . . ?
Ru` N3` C17` C16` 176.1(5) . . . . ?
C13` N3` C17` C18` -178.5(5) . . . . ?
Ru` N3` C17` C18` -0.7(6) . . . . ?
C15` C16` C17` N3` -0.6(11) . . . . ?
C15` C16` C17` C18` 175.9(7) . . . . ?
C22` N4` C18` C19` -2.2(9) . . . . ?
Ru` N4` C18` C19` 174.0(5) . . . . ?
C22` N4` C18` C17` 175.5(5) . . . . ?
Ru` N4` C18` C17` -8.2(6) . . . . ?
N3` C17` C18` N4` 5.8(7) . . . . ?
C16` C17` C18` N4` -170.9(6) . . . . ?
N3` C17` C18` C19` -176.8(6) . . . . ?
C16` C17` C18` C19` 6.5(10) . . . . ?
N4` C18` C19` C20` 2.4(10) . . . . ?
C17` C18` C19` C20` -175.0(7) . . . . ?
C18` C19` C20` C21` -1.4(11) . . . . ?
C19` C20` C21` C22` 0.0(12) . . . . ?
C18` N4` C22` C21` 0.9(9) . . . . ?
Ru` N4` C22` C21` -175.4(5) . . . . ?
C18` N4` C22` C23` -177.6(5) . . . . ?
Ru` N4` C22` C23` 6.2(6) . . . . ?
C20` C21` C22` N4` 0.3(10) . . . . ?
C20` C21` C22` C23` 178.5(6) . . . . ?
C27` N5` C23` C24` -0.5(8) . . . . ?
Ru` N5` C23` C24` -178.9(5) . . . . ?
C27` N5` C23` C22` 175.8(5) . . . . ?
Ru` N5` C23` C22` -2.7(6) . . . . ?
N4` C22` C23` N5` -2.1(7) . . . . ?
C21` C22` C23` N5` 179.6(6) . . . . ?
N4` C22` C23` C24` 174.0(6) . . . . ?
C21` C22` C23` C24` -4.2(10) . . . . ?
N5` C23` C24` C25` -0.5(10) . . . . ?
C22` C23` C24` C25` -176.4(7) . . . . ?
C23` C24` C25` C26` 0.6(12) . . . . ?
C24` C25` C26` C27` 0.2(13) . . . . ?
C23` N5` C27` C26` 1.3(9) . . . . ?
Ru` N5` C27` C26` 179.5(5) . . . . ?
C25` C26` C27` N5` -1.2(11) . . . . ?
O3` Cl1` O4' O5` 122.2(9) . . . . ?
O6` Cl1` O4' O5` -113.6(7) . . . . ?
O3` Cl1` O5` O4' -102.9(14) . . . . ?
O6` Cl1` O5` O4' 90.1(9) . . . . ?
|
1100943.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100943.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_1100943
loop_
_publ_author_name
'Nripen Chanda'
'Debamita Paul'
'Sanjib Kar'
'Shaikh M. Mobin'
'Anindya Datta'
'Vedavati G. Puranik'
'K. Krishnamurthy Rao'
'Goutam Kumar Lahiri'
_publ_section_title
;
Effect of 2-(2-Pyridyl)azole-Based Ancillary Ligands (L1-4) on the
Electrophilicity of the Nitrosyl Function in [RuII(trpy)(L1-4)(NO)]3+ [trpy
= 2,2':6',2''-Terpyridine]. Synthesis, Structures, and
Spectroscopic, Electrochemical, and Kinetic Aspects
;
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3499
_journal_page_last 3511
_journal_paper_doi 10.1021/ic048184w
_journal_volume 44
_journal_year 2005
_chemical_formula_sum 'C27 H19 Cl2 N5 O5 Ru'
_chemical_formula_weight 665.44
_chemical_name_systematic
;
?
;
_space_group_IT_number 61
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall '-P 2bc 2ac'
_symmetry_space_group_name_H-M 'P c a b'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.000(4)
_cell_angle_beta 90.000(6)
_cell_angle_gamma 90.000(7)
_cell_formula_units_Z 8
_cell_length_a 11.1910(11)
_cell_length_b 14.1940(10)
_cell_length_c 33.1510(10)
_cell_measurement_reflns_used 25
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 11.4900
_cell_measurement_theta_min 5.2500
_cell_volume 5265.9(7)
_computing_cell_refinement 'Argus (Nonius, MACH3 software)'
_computing_data_collection 'Argus (Nonius, MACH3 software)'
_computing_data_reduction 'Maxus (Nonius software)'
_computing_molecular_graphics Ortep3
_computing_publication_material Maxus
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 293(2)
_diffrn_measured_fraction_theta_full 0.726
_diffrn_measured_fraction_theta_max 0.726
_diffrn_measurement_device_type 'Enraf-Nonius CAD-4'
_diffrn_measurement_method \w/q-scan
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type ' MoK\a'
_diffrn_radiation_wavelength 0.70930
_diffrn_reflns_av_R_equivalents 0.0000
_diffrn_reflns_av_sigmaI/netI 0.0283
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min 0
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_l_max 39
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_number 3762
_diffrn_reflns_theta_full 24.93
_diffrn_reflns_theta_max 24.93
_diffrn_reflns_theta_min 1.23
_diffrn_standards_decay_% <3%
_diffrn_standards_interval_time 3600
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 0.848
_exptl_absorpt_correction_T_max 1.000
_exptl_absorpt_correction_T_min 0.991
_exptl_absorpt_correction_type psi-scan
_exptl_absorpt_process_details
;
psi-scan (North, Philips & Mathews, 1968)
;
_exptl_crystal_colour Black
_exptl_crystal_density_diffrn 1.679
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description Block
_exptl_crystal_F_000 2672
_exptl_crystal_size_max 0.40
_exptl_crystal_size_mid 0.25
_exptl_crystal_size_min 0.25
_refine_diff_density_max 0.993
_refine_diff_density_min -0.588
_refine_diff_density_rms 0.073
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.055
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 437
_refine_ls_number_reflns 3762
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.055
_refine_ls_R_factor_all 0.0475
_refine_ls_R_factor_gt 0.0347
_refine_ls_shift/su_max 0.004
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0408P)^2^+9.2470P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0814
_refine_ls_wR_factor_ref 0.0896
_reflns_number_gt 3143
_reflns_number_total 3762
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file ic048184wsi20041223_113506.cif
_cod_data_source_block max
_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
The following automatic conversions were performed:
'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0408P)^2^+9.2470P] 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^)+(0.0408P)^2^+9.2470P] where P=(Fo^2^+2Fc^2^)/3'.
Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas
;
_cod_database_code 1100943
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y+1/2, z+1/2'
'x+1/2, -y, -z+1/2'
'-x+1/2, 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'
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
Ru Ru 0.20425(3) 0.02081(2) 0.609164(10) 0.02978(12) Uani 1 d . . .
Cl1 Cl 0.33954(12) 0.03038(9) 0.55306(4) 0.0520(3) Uani 1 d . . .
Cl2 Cl 0.21929(11) 0.78348(9) 0.73381(4) 0.0489(3) Uani 1 d . . .
N1 N 0.1571(3) -0.1203(2) 0.60040(10) 0.0323(8) Uani 1 d . . .
N2 N 0.0817(3) -0.0012(2) 0.65447(10) 0.0328(8) Uani 1 d . . .
N3 N 0.3481(3) 0.0038(2) 0.64719(11) 0.0345(8) Uani 1 d . . .
N4 N 0.2374(3) 0.1514(2) 0.62216(11) 0.0345(8) Uani 1 d . . .
N5 N 0.0732(3) 0.0873(3) 0.57515(10) 0.0371(9) Uani 1 d . . .
O1 O 0.0309(3) -0.2359(2) 0.61805(9) 0.0440(8) Uani 1 d . . .
O2 O 0.1360(5) 0.7365(4) 0.75821(14) 0.1091(17) Uani 1 d . . .
O3 O 0.3385(4) 0.7590(3) 0.74464(13) 0.0885(14) Uani 1 d . . .
O4 O 0.2059(4) 0.8825(3) 0.73881(15) 0.0937(15) Uani 1 d . . .
O5 O 0.2014(3) 0.7599(3) 0.69238(11) 0.0678(10) Uani 1 d . . .
C1 C 0.1111(4) -0.2727(3) 0.59005(14) 0.0425(11) Uani 1 d . . .
C2 C 0.1142(6) -0.3627(4) 0.57473(18) 0.0609(16) Uani 1 d . . .
C3 C 0.2062(7) -0.3801(4) 0.54820(18) 0.0689(18) Uani 1 d . . .
C4 C 0.2897(6) -0.3120(4) 0.53774(16) 0.0580(15) Uani 1 d . . .
C5 C 0.2833(5) -0.2212(4) 0.55262(15) 0.0456(12) Uani 1 d . . .
C6 C 0.1901(4) -0.2024(3) 0.57940(12) 0.0354(10) Uani 1 d . . .
C7 C 0.0676(4) -0.1453(3) 0.62321(13) 0.0353(10) Uani 1 d . . .
C8 C 0.0194(4) -0.0838(3) 0.65303(13) 0.0335(10) Uani 1 d . . .
C9 C -0.0708(5) -0.1055(3) 0.67987(16) 0.0463(12) Uani 1 d . . .
C10 C -0.0997(5) -0.0412(4) 0.70957(15) 0.0487(13) Uani 1 d . . .
C11 C -0.0363(5) 0.0413(3) 0.71170(15) 0.0445(12) Uani 1 d . . .
C12 C 0.0524(5) 0.0583(3) 0.68431(14) 0.0392(11) Uani 1 d . . .
C13 C 0.4033(4) -0.0763(4) 0.65777(15) 0.0415(11) Uani 1 d . . .
C14 C 0.5039(5) -0.0777(4) 0.68121(16) 0.0516(13) Uani 1 d . . .
C15 C 0.5488(5) 0.0052(4) 0.69585(16) 0.0549(14) Uani 1 d . . .
C16 C 0.4928(5) 0.0885(4) 0.68620(15) 0.0487(13) Uani 1 d . . .
C17 C 0.3921(4) 0.0869(3) 0.66154(12) 0.0372(10) Uani 1 d . . .
C18 C 0.3283(4) 0.1712(3) 0.64763(13) 0.0373(10) Uani 1 d . . .
C19 C 0.3522(5) 0.2635(4) 0.65785(16) 0.0486(13) Uani 1 d . . .
C20 C 0.2849(6) 0.3347(4) 0.64127(17) 0.0610(15) Uani 1 d . . .
C21 C 0.1933(5) 0.3140(3) 0.61481(17) 0.0543(14) Uani 1 d . . .
C22 C 0.1697(4) 0.2204(3) 0.60513(13) 0.0386(10) Uani 1 d . . .
C23 C 0.0761(4) 0.1830(3) 0.57867(13) 0.0404(11) Uani 1 d . . .
C24 C -0.0047(5) 0.2396(4) 0.55808(17) 0.0557(14) Uani 1 d . . .
C25 C -0.0892(6) 0.1997(5) 0.53408(19) 0.0669(17) Uani 1 d . . .
C26 C -0.0926(5) 0.1038(5) 0.53026(17) 0.0606(16) Uani 1 d . . .
C27 C -0.0105(4) 0.0496(4) 0.55140(15) 0.0468(12) Uani 1 d . . .
H27 H -0.016(4) -0.019(3) 0.5521(13) 0.045(13) Uiso 1 d . . .
H9 H -0.105(4) -0.160(3) 0.6763(13) 0.039(13) Uiso 1 d . . .
H13 H 0.370(4) -0.125(3) 0.6481(12) 0.025(11) Uiso 1 d . . .
H12 H 0.095(4) 0.103(3) 0.6875(14) 0.041(14) Uiso 1 d . . .
H11 H -0.056(4) 0.079(3) 0.7314(13) 0.034(12) Uiso 1 d . . .
H10 H -0.163(4) -0.055(3) 0.7269(13) 0.035(11) Uiso 1 d . . .
H5 H 0.332(4) -0.179(3) 0.5448(12) 0.026(12) Uiso 1 d . . .
H15 H 0.622(5) 0.012(3) 0.7136(16) 0.068(16) Uiso 1 d . . .
H26 H -0.144(5) 0.076(4) 0.5158(15) 0.053(16) Uiso 1 d . . .
H20 H 0.305(4) 0.398(4) 0.6481(15) 0.064(16) Uiso 1 d . . .
H14 H 0.529(5) -0.134(4) 0.6879(15) 0.055(16) Uiso 1 d . . .
H4 H 0.353(4) -0.326(3) 0.5184(14) 0.057(15) Uiso 1 d . . .
H21 H 0.154(5) 0.358(4) 0.6021(16) 0.070(19) Uiso 1 d . . .
H19 H 0.405(4) 0.273(3) 0.6733(14) 0.045(15) Uiso 1 d . . .
H3 H 0.199(6) -0.443(5) 0.534(2) 0.12(2) Uiso 1 d . . .
H2 H 0.065(5) -0.407(4) 0.5825(16) 0.063(17) Uiso 1 d . . .
H16 H 0.516(5) 0.140(4) 0.6956(16) 0.062(17) Uiso 1 d . . .
H24 H 0.004(5) 0.302(4) 0.5614(18) 0.09(2) Uiso 1 d . . .
H25 H -0.141(6) 0.230(4) 0.5199(17) 0.08(2) Uiso 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
Ru 0.03124(19) 0.02602(18) 0.03206(19) 0.00011(15) -0.00159(15) -0.00257(15)
Cl1 0.0583(7) 0.0507(7) 0.0471(7) 0.0055(6) 0.0158(6) -0.0029(6)
Cl2 0.0435(7) 0.0478(7) 0.0554(7) -0.0088(5) -0.0022(6) 0.0027(6)
N1 0.0328(19) 0.0315(19) 0.0327(19) -0.0021(15) -0.0029(15) -0.0014(16)
N2 0.0344(19) 0.0298(19) 0.0342(18) 0.0011(14) -0.0035(15) 0.0017(15)
N3 0.0307(18) 0.035(2) 0.038(2) -0.0004(15) -0.0011(16) -0.0030(15)
N4 0.039(2) 0.0271(18) 0.0370(19) -0.0005(15) 0.0029(16) -0.0046(16)
N5 0.040(2) 0.039(2) 0.0324(19) 0.0010(16) -0.0031(17) 0.0007(17)
O1 0.0492(19) 0.0303(17) 0.0524(19) -0.0035(14) 0.0029(16) -0.0096(15)
O2 0.114(4) 0.114(4) 0.100(4) 0.012(3) 0.032(3) -0.042(3)
O3 0.069(3) 0.105(3) 0.092(3) -0.039(3) -0.031(2) 0.033(3)
O4 0.106(4) 0.052(2) 0.123(4) -0.029(2) 0.009(3) 0.014(2)
O5 0.070(3) 0.072(3) 0.062(2) -0.010(2) -0.014(2) 0.000(2)
C1 0.049(3) 0.034(2) 0.044(3) -0.006(2) -0.008(2) 0.002(2)
C2 0.088(5) 0.030(3) 0.065(4) -0.007(3) 0.002(3) -0.006(3)
C3 0.102(5) 0.044(3) 0.060(3) -0.019(3) -0.010(4) 0.014(4)
C4 0.072(4) 0.056(3) 0.046(3) -0.009(3) 0.001(3) 0.024(3)
C5 0.046(3) 0.049(3) 0.041(3) -0.003(2) -0.001(2) 0.006(3)
C6 0.039(3) 0.034(2) 0.033(2) -0.0052(18) -0.008(2) 0.003(2)
C7 0.039(3) 0.025(2) 0.042(2) 0.0013(18) -0.003(2) -0.0060(19)
C8 0.032(2) 0.033(2) 0.036(2) -0.0011(19) -0.0018(19) -0.0011(19)
C9 0.045(3) 0.035(3) 0.059(3) 0.004(2) 0.008(2) -0.004(2)
C10 0.047(3) 0.055(3) 0.044(3) 0.009(2) 0.017(2) 0.009(3)
C11 0.056(3) 0.042(3) 0.035(3) 0.004(2) 0.008(2) 0.013(2)
C12 0.048(3) 0.030(2) 0.039(3) -0.004(2) -0.005(2) 0.004(2)
C13 0.041(3) 0.038(3) 0.046(3) 0.001(2) -0.007(2) 0.006(2)
C14 0.047(3) 0.055(3) 0.053(3) 0.005(3) -0.009(2) 0.012(3)
C15 0.043(3) 0.070(4) 0.051(3) 0.005(3) -0.013(2) -0.002(3)
C16 0.045(3) 0.059(4) 0.042(3) -0.008(3) -0.007(2) -0.014(3)
C17 0.039(3) 0.040(3) 0.032(2) -0.0039(19) 0.002(2) -0.005(2)
C18 0.041(3) 0.036(2) 0.034(2) -0.0023(19) 0.002(2) -0.011(2)
C19 0.049(3) 0.044(3) 0.053(3) -0.007(2) -0.012(3) -0.012(3)
C20 0.080(4) 0.039(3) 0.065(3) -0.011(3) 0.001(3) -0.019(3)
C21 0.069(4) 0.029(2) 0.065(4) 0.003(2) 0.006(3) 0.003(3)
C22 0.042(3) 0.032(2) 0.042(3) 0.001(2) 0.006(2) 0.002(2)
C23 0.043(3) 0.039(2) 0.039(2) 0.006(2) 0.004(2) 0.004(2)
C24 0.060(3) 0.050(4) 0.056(3) 0.006(3) -0.003(3) 0.015(3)
C25 0.062(4) 0.073(4) 0.066(4) 0.013(3) -0.012(3) 0.023(3)
C26 0.047(3) 0.079(4) 0.056(3) 0.005(3) -0.018(3) -0.002(3)
C27 0.046(3) 0.050(3) 0.045(3) 0.003(2) -0.007(2) -0.002(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'
O O 0.0106 0.0060 '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'
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
N4 Ru N2 96.32(14) . . ?
N4 Ru N3 80.02(14) . . ?
N2 Ru N3 93.24(14) . . ?
N4 Ru N5 79.70(15) . . ?
N2 Ru N5 89.67(14) . . ?
N3 Ru N5 159.71(14) . . ?
N4 Ru N1 174.08(14) . . ?
N2 Ru N1 77.77(13) . . ?
N3 Ru N1 99.79(13) . . ?
N5 Ru N1 100.46(14) . . ?
N4 Ru Cl1 89.86(11) . . ?
N2 Ru Cl1 173.64(10) . . ?
N3 Ru Cl1 89.31(10) . . ?
N5 Ru Cl1 89.95(10) . . ?
N1 Ru Cl1 96.06(10) . . ?
O2 Cl2 O4 109.4(3) . . ?
O2 Cl2 O3 111.2(3) . . ?
O4 Cl2 O3 108.0(3) . . ?
O2 Cl2 O5 110.5(3) . . ?
O4 Cl2 O5 109.2(3) . . ?
O3 Cl2 O5 108.5(2) . . ?
C7 N1 C6 105.2(3) . . ?
C7 N1 Ru 112.0(3) . . ?
C6 N1 Ru 142.7(3) . . ?
C12 N2 C8 116.2(4) . . ?
C12 N2 Ru 127.3(3) . . ?
C8 N2 Ru 116.4(3) . . ?
C13 N3 C17 118.4(4) . . ?
C13 N3 Ru 128.3(3) . . ?
C17 N3 Ru 113.3(3) . . ?
C18 N4 C22 122.0(4) . . ?
C18 N4 Ru 118.7(3) . . ?
C22 N4 Ru 119.3(3) . . ?
C27 N5 C23 117.8(4) . . ?
C27 N5 Ru 129.3(3) . . ?
C23 N5 Ru 112.9(3) . . ?
C7 O1 C1 104.1(3) . . ?
C2 C1 C6 124.2(5) . . ?
C2 C1 O1 127.6(5) . . ?
C6 C1 O1 108.2(4) . . ?
C1 C2 C3 114.9(6) . . ?
C1 C2 H2 123(4) . . ?
C3 C2 H2 122(4) . . ?
C2 C3 C4 122.5(5) . . ?
C2 C3 H3 113(4) . . ?
C4 C3 H3 124(4) . . ?
C5 C4 C3 121.7(5) . . ?
C5 C4 H4 117(3) . . ?
C3 C4 H4 121(3) . . ?
C4 C5 C6 116.3(5) . . ?
C4 C5 H5 121(3) . . ?
C6 C5 H5 122(3) . . ?
C1 C6 C5 120.3(4) . . ?
C1 C6 N1 107.7(4) . . ?
C5 C6 N1 132.0(4) . . ?
N1 C7 O1 114.6(4) . . ?
N1 C7 C8 121.7(4) . . ?
O1 C7 C8 123.5(4) . . ?
N2 C8 C9 122.9(4) . . ?
N2 C8 C7 111.0(4) . . ?
C9 C8 C7 125.9(4) . . ?
C8 C9 C10 118.9(5) . . ?
C8 C9 H9 116(3) . . ?
C10 C9 H9 125(3) . . ?
C11 C10 C9 118.7(5) . . ?
C11 C10 H10 123(3) . . ?
C9 C10 H10 118(3) . . ?
C12 C11 C10 119.5(5) . . ?
C12 C11 H11 125(3) . . ?
C10 C11 H11 116(3) . . ?
N2 C12 C11 123.7(5) . . ?
N2 C12 H12 117(3) . . ?
C11 C12 H12 119(3) . . ?
N3 C13 C14 122.7(5) . . ?
N3 C13 H13 113(3) . . ?
C14 C13 H13 124(3) . . ?
C13 C14 C15 119.4(5) . . ?
C13 C14 H14 115(3) . . ?
C15 C14 H14 125(3) . . ?
C14 C15 C16 119.3(5) . . ?
C14 C15 H15 126(3) . . ?
C16 C15 H15 115(3) . . ?
C15 C16 C17 119.5(5) . . ?
C15 C16 H16 122(4) . . ?
C17 C16 H16 119(4) . . ?
N3 C17 C16 120.8(4) . . ?
N3 C17 C18 114.8(4) . . ?
C16 C17 C18 124.4(4) . . ?
N4 C18 C19 119.7(4) . . ?
N4 C18 C17 113.2(4) . . ?
C19 C18 C17 127.1(4) . . ?
C20 C19 C18 119.6(5) . . ?
C20 C19 H19 123(4) . . ?
C18 C19 H19 117(4) . . ?
C19 C20 C21 120.3(5) . . ?
C19 C20 H20 118(3) . . ?
C21 C20 H20 122(3) . . ?
C20 C21 C22 119.3(5) . . ?
C20 C21 H21 122(4) . . ?
C22 C21 H21 118(4) . . ?
N4 C22 C21 119.0(5) . . ?
N4 C22 C23 112.7(4) . . ?
C21 C22 C23 128.3(5) . . ?
N5 C23 C24 121.2(5) . . ?
N5 C23 C22 115.4(4) . . ?
C24 C23 C22 123.4(5) . . ?
C25 C24 C23 120.0(6) . . ?
C25 C24 H24 124(4) . . ?
C23 C24 H24 116(4) . . ?
C24 C25 C26 119.2(6) . . ?
C24 C25 H25 125(4) . . ?
C26 C25 H25 116(4) . . ?
C25 C26 C27 119.1(6) . . ?
C25 C26 H26 123(4) . . ?
C27 C26 H26 118(4) . . ?
N5 C27 C26 122.7(5) . . ?
N5 C27 H27 115(3) . . ?
C26 C27 H27 122(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
Ru N4 1.939(3) . ?
Ru N2 2.058(3) . ?
Ru N3 2.058(4) . ?
Ru N5 2.077(4) . ?
Ru N1 2.092(3) . ?
Ru Cl1 2.4020(12) . ?
Cl2 O2 1.402(5) . ?
Cl2 O4 1.423(4) . ?
Cl2 O3 1.424(4) . ?
Cl2 O5 1.427(4) . ?
N1 C7 1.304(5) . ?
N1 C6 1.407(5) . ?
N2 C12 1.341(6) . ?
N2 C8 1.365(5) . ?
N3 C13 1.340(6) . ?
N3 C17 1.364(5) . ?
N4 C18 1.352(5) . ?
N4 C22 1.361(6) . ?
N5 C27 1.335(6) . ?
N5 C23 1.364(6) . ?
O1 C7 1.360(5) . ?
O1 C1 1.393(5) . ?
C1 C2 1.376(6) . ?
C1 C6 1.379(6) . ?
C2 C3 1.377(9) . ?
C2 H2 0.87(5) . ?
C3 C4 1.389(9) . ?
C3 H3 1.01(7) . ?
C4 C5 1.382(7) . ?
C4 H4 0.97(5) . ?
C5 C6 1.395(6) . ?
C5 H5 0.85(4) . ?
C7 C8 1.425(6) . ?
C8 C9 1.381(6) . ?
C9 C10 1.381(7) . ?
C9 H9 0.87(4) . ?
C10 C11 1.371(7) . ?
C10 H10 0.94(4) . ?
C11 C12 1.367(7) . ?
C11 H11 0.87(4) . ?
C12 H12 0.80(5) . ?
C13 C14 1.368(7) . ?
C13 H13 0.85(4) . ?
C14 C15 1.368(8) . ?
C14 H14 0.88(5) . ?
C15 C16 1.375(8) . ?
C15 H15 1.02(6) . ?
C16 C17 1.392(7) . ?
C16 H16 0.84(5) . ?
C17 C18 1.467(6) . ?
C18 C19 1.380(6) . ?
C19 C20 1.375(8) . ?
C19 H19 0.79(5) . ?
C20 C21 1.381(8) . ?
C20 H20 0.95(6) . ?
C21 C22 1.391(7) . ?
C21 H21 0.88(6) . ?
C22 C23 1.465(6) . ?
C23 C24 1.389(7) . ?
C24 C25 1.359(8) . ?
C24 H24 0.89(6) . ?
C25 C26 1.367(8) . ?
C25 H25 0.87(6) . ?
C26 C27 1.388(7) . ?
C26 H26 0.85(5) . ?
C27 H27 0.97(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
N4 Ru N1 C7 11.8(15) . . . . ?
N2 Ru N1 C7 8.2(3) . . . . ?
N3 Ru N1 C7 99.4(3) . . . . ?
N5 Ru N1 C7 -79.2(3) . . . . ?
Cl1 Ru N1 C7 -170.2(3) . . . . ?
N4 Ru N1 C6 -164.6(12) . . . . ?
N2 Ru N1 C6 -168.1(5) . . . . ?
N3 Ru N1 C6 -76.9(5) . . . . ?
N5 Ru N1 C6 104.5(5) . . . . ?
Cl1 Ru N1 C6 13.4(5) . . . . ?
N4 Ru N2 C12 -6.4(4) . . . . ?
N3 Ru N2 C12 73.9(4) . . . . ?
N5 Ru N2 C12 -86.0(4) . . . . ?
N1 Ru N2 C12 173.2(4) . . . . ?
Cl1 Ru N2 C12 -172.6(7) . . . . ?
N4 Ru N2 C8 170.5(3) . . . . ?
N3 Ru N2 C8 -109.2(3) . . . . ?
N5 Ru N2 C8 90.9(3) . . . . ?
N1 Ru N2 C8 -9.9(3) . . . . ?
Cl1 Ru N2 C8 4.3(11) . . . . ?
N4 Ru N3 C13 -177.6(4) . . . . ?
N2 Ru N3 C13 86.6(4) . . . . ?
N5 Ru N3 C13 -175.6(4) . . . . ?
N1 Ru N3 C13 8.4(4) . . . . ?
Cl1 Ru N3 C13 -87.6(4) . . . . ?
N4 Ru N3 C17 -0.1(3) . . . . ?
N2 Ru N3 C17 -96.0(3) . . . . ?
N5 Ru N3 C17 1.9(6) . . . . ?
N1 Ru N3 C17 -174.1(3) . . . . ?
Cl1 Ru N3 C17 89.9(3) . . . . ?
N2 Ru N4 C18 91.6(3) . . . . ?
N3 Ru N4 C18 -0.6(3) . . . . ?
N5 Ru N4 C18 -179.9(3) . . . . ?
N1 Ru N4 C18 88.1(14) . . . . ?
Cl1 Ru N4 C18 -89.9(3) . . . . ?
N2 Ru N4 C22 -89.1(3) . . . . ?
N3 Ru N4 C22 178.7(3) . . . . ?
N5 Ru N4 C22 -0.6(3) . . . . ?
N1 Ru N4 C22 -92.6(14) . . . . ?
Cl1 Ru N4 C22 89.4(3) . . . . ?
N4 Ru N5 C27 -179.5(4) . . . . ?
N2 Ru N5 C27 -83.0(4) . . . . ?
N3 Ru N5 C27 178.5(4) . . . . ?
N1 Ru N5 C27 -5.5(4) . . . . ?
Cl1 Ru N5 C27 90.6(4) . . . . ?
N4 Ru N5 C23 0.2(3) . . . . ?
N2 Ru N5 C23 96.7(3) . . . . ?
N3 Ru N5 C23 -1.8(6) . . . . ?
N1 Ru N5 C23 174.2(3) . . . . ?
Cl1 Ru N5 C23 -89.7(3) . . . . ?
C7 O1 C1 C2 179.3(5) . . . . ?
C7 O1 C1 C6 -1.0(5) . . . . ?
C6 C1 C2 C3 2.1(8) . . . . ?
O1 C1 C2 C3 -178.2(5) . . . . ?
C1 C2 C3 C4 0.0(9) . . . . ?
C2 C3 C4 C5 -1.8(9) . . . . ?
C3 C4 C5 C6 1.4(8) . . . . ?
C2 C1 C6 C5 -2.5(7) . . . . ?
O1 C1 C6 C5 177.7(4) . . . . ?
C2 C1 C6 N1 178.5(5) . . . . ?
O1 C1 C6 N1 -1.2(5) . . . . ?
C4 C5 C6 C1 0.6(7) . . . . ?
C4 C5 C6 N1 179.3(5) . . . . ?
C7 N1 C6 C1 3.0(5) . . . . ?
Ru N1 C6 C1 179.5(3) . . . . ?
C7 N1 C6 C5 -175.7(5) . . . . ?
Ru N1 C6 C5 0.7(8) . . . . ?
C6 N1 C7 O1 -3.9(5) . . . . ?
Ru N1 C7 O1 178.4(3) . . . . ?
C6 N1 C7 C8 171.7(4) . . . . ?
Ru N1 C7 C8 -6.0(5) . . . . ?
C1 O1 C7 N1 3.2(5) . . . . ?
C1 O1 C7 C8 -172.4(4) . . . . ?
C12 N2 C8 C9 1.4(6) . . . . ?
Ru N2 C8 C9 -175.8(4) . . . . ?
C12 N2 C8 C7 -173.2(4) . . . . ?
Ru N2 C8 C7 9.5(4) . . . . ?
N1 C7 C8 N2 -2.1(6) . . . . ?
O1 C7 C8 N2 173.1(4) . . . . ?
N1 C7 C8 C9 -176.6(4) . . . . ?
O1 C7 C8 C9 -1.3(7) . . . . ?
N2 C8 C9 C10 -0.1(7) . . . . ?
C7 C8 C9 C10 173.7(5) . . . . ?
C8 C9 C10 C11 -1.0(7) . . . . ?
C9 C10 C11 C12 0.7(7) . . . . ?
C8 N2 C12 C11 -1.8(7) . . . . ?
Ru N2 C12 C11 175.2(3) . . . . ?
C10 C11 C12 N2 0.7(7) . . . . ?
C17 N3 C13 C14 -2.2(7) . . . . ?
Ru N3 C13 C14 175.2(4) . . . . ?
N3 C13 C14 C15 2.3(8) . . . . ?
C13 C14 C15 C16 -1.0(8) . . . . ?
C14 C15 C16 C17 -0.4(8) . . . . ?
C13 N3 C17 C16 0.7(6) . . . . ?
Ru N3 C17 C16 -177.1(3) . . . . ?
C13 N3 C17 C18 178.4(4) . . . . ?
Ru N3 C17 C18 0.7(5) . . . . ?
C15 C16 C17 N3 0.6(7) . . . . ?
C15 C16 C17 C18 -177.0(5) . . . . ?
C22 N4 C18 C19 1.9(7) . . . . ?
Ru N4 C18 C19 -178.9(4) . . . . ?
C22 N4 C18 C17 -178.1(4) . . . . ?
Ru N4 C18 C17 1.1(5) . . . . ?
N3 C17 C18 N4 -1.1(5) . . . . ?
C16 C17 C18 N4 176.5(4) . . . . ?
N3 C17 C18 C19 178.8(5) . . . . ?
C16 C17 C18 C19 -3.5(8) . . . . ?
N4 C18 C19 C20 -1.5(7) . . . . ?
C17 C18 C19 C20 178.5(5) . . . . ?
C18 C19 C20 C21 0.5(8) . . . . ?
C19 C20 C21 C22 0.1(8) . . . . ?
C18 N4 C22 C21 -1.2(6) . . . . ?
Ru N4 C22 C21 179.5(4) . . . . ?
C18 N4 C22 C23 -179.9(4) . . . . ?
Ru N4 C22 C23 0.9(5) . . . . ?
C20 C21 C22 N4 0.2(7) . . . . ?
C20 C21 C22 C23 178.6(5) . . . . ?
C27 N5 C23 C24 -0.3(7) . . . . ?
Ru N5 C23 C24 179.9(4) . . . . ?
C27 N5 C23 C22 179.9(4) . . . . ?
Ru N5 C23 C22 0.2(5) . . . . ?
N4 C22 C23 N5 -0.7(6) . . . . ?
C21 C22 C23 N5 -179.2(5) . . . . ?
N4 C22 C23 C24 179.6(4) . . . . ?
C21 C22 C23 C24 1.1(8) . . . . ?
N5 C23 C24 C25 0.4(8) . . . . ?
C22 C23 C24 C25 -179.9(5) . . . . ?
C23 C24 C25 C26 -0.6(9) . . . . ?
C24 C25 C26 C27 0.8(9) . . . . ?
C23 N5 C27 C26 0.6(7) . . . . ?
Ru N5 C27 C26 -179.8(4) . . . . ?
C25 C26 C27 N5 -0.8(9) . . . . ?
|
1100944.cif | #------------------------------------------------------------------------------
#$Date: 2016-12-31 20:31:26 +0200 (Sat, 31 Dec 2016) $
#$Revision: 189516 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/09/1100944.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_1100944
loop_
_publ_author_name
'Nripen Chanda'
'Debamita Paul'
'Sanjib Kar'
'Shaikh M. Mobin'
'Anindya Datta'
'Vedavati G. Puranik'
'K. Krishnamurthy Rao'
'Goutam Kumar Lahiri'
_publ_section_title
;
Effect of 2-(2-Pyridyl)azole-Based Ancillary Ligands (L1-4) on the
Electrophilicity of the Nitrosyl Function in [RuII(trpy)(L1-4)(NO)]3+
[trpy = 2,2':6',2''-Terpyridine]. Synthesis, Structures, and
Spectroscopic, Electrochemical, and Kinetic Aspects
;
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3499
_journal_page_last 3511
_journal_paper_doi 10.1021/ic048184w
_journal_volume 44
_journal_year 2005
_chemical_formula_moiety 'C27 H19 N6 O3 Ru.(ClO4).0.5(H2O)'
_chemical_formula_sum 'C27 H20 Cl N6 O7.5 Ru'
_chemical_formula_weight 685.01
_chemical_name_systematic ?
_space_group_IT_number 61
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall '-P 2bc 2ac'
_symmetry_space_group_name_H-M 'P c a b'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.000(11)
_cell_angle_beta 90.000(10)
_cell_angle_gamma 90.000(6)
_cell_formula_units_Z 8
_cell_length_a 11.1960(9)
_cell_length_b 14.4280(10)
_cell_length_c 34.039(6)
_cell_measurement_temperature 293(2)
_cell_volume 5498.5(11)
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 293(2)
_diffrn_measured_fraction_theta_full 0.875
_diffrn_measured_fraction_theta_max 0.875
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_wavelength 0.70930
_diffrn_reflns_av_R_equivalents 0.0000
_diffrn_reflns_av_sigmaI/netI 0.0301
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min 0
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_l_max 40
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_number 4227
_diffrn_reflns_theta_full 24.91
_diffrn_reflns_theta_max 24.91
_diffrn_reflns_theta_min 1.19
_exptl_absorpt_coefficient_mu 0.728
_exptl_crystal_density_diffrn 1.655
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 2760
_refine_diff_density_max 0.748
_refine_diff_density_min -0.451
_refine_diff_density_rms 0.071
_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 464
_refine_ls_number_reflns 4227
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.063
_refine_ls_R_factor_all 0.0495
_refine_ls_R_factor_gt 0.0357
_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^)+(0.0447P)^2^+6.7176P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0848
_refine_ls_wR_factor_ref 0.0918
_reflns_number_gt 3514
_reflns_number_total 4227
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file ic048184wsi20041223_113549.cif
_cod_data_source_block C27H19N6O3Ru.(ClO4).0.5(H2O)
_cod_depositor_comments
;
Marking attached hydrogen atoms.
Antanas Vaitkus,
2016-12-31
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 5498.5(12)
_cod_original_sg_symbol_H-M 'P b c a'
_cod_original_formula_sum 'C27 H20 Cl N6 O7.50 Ru'
_cod_database_code 1100944
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y+1/2, z+1/2'
'x+1/2, -y, -z+1/2'
'-x+1/2, 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'
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
_atom_site_attached_hydrogens
Ru Ru 0.19100(3) 0.01815(2) 0.387124(8) 0.02922(11) Uani 1 1 d . . . 0
O1 O 0.2780(4) 0.0113(4) 0.46516(12) 0.1126(19) Uani 1 1 d . . . 0
O2 O 0.4137(3) 0.0473(3) 0.42716(11) 0.0777(11) Uani 1 1 d . . . 0
O3 O 0.0249(3) -0.23849(19) 0.37762(9) 0.0472(8) Uani 1 1 d . . . 0
N1 N 0.1467(3) -0.1220(2) 0.39532(9) 0.0338(8) Uani 1 1 d . . . 0
N2 N 0.0629(3) -0.0048(2) 0.34310(9) 0.0315(7) Uani 1 1 d . . . 0
N3 N 0.0612(3) 0.0811(2) 0.42158(9) 0.0367(8) Uani 1 1 d . . . 0
N4 N 0.2207(3) 0.1484(2) 0.37454(9) 0.0331(8) Uani 1 1 d . . . 0
N5 N 0.3315(3) 0.0042(2) 0.34866(10) 0.0336(8) Uani 1 1 d . . . 0
N6 N 0.3084(3) 0.0280(2) 0.43234(10) 0.0408(8) Uani 1 1 d . . . 0
C1 C 0.1050(4) -0.2723(3) 0.40500(13) 0.0463(11) Uani 1 1 d . . . 0
C2 C 0.1100(6) -0.3614(4) 0.41955(18) 0.0679(16) Uani 1 1 d . . . 0
C3 C 0.2002(7) -0.3762(4) 0.44589(19) 0.0787(19) Uani 1 1 d . . . 0
C4 C 0.2812(6) -0.3079(4) 0.45724(16) 0.0686(16) Uani 1 1 d . . . 0
C5 C 0.2720(5) -0.2187(4) 0.44254(14) 0.0512(12) Uani 1 1 d . . . 0
C6 C 0.1807(4) -0.2021(3) 0.41592(12) 0.0383(10) Uani 1 1 d . . . 0
C7 C 0.0577(4) -0.1484(3) 0.37313(12) 0.0367(9) Uani 1 1 d . . . 0
C8 C 0.0054(3) -0.0880(3) 0.34422(12) 0.0344(9) Uani 1 1 d . . . 0
C9 C -0.0866(4) -0.1101(4) 0.31892(15) 0.0500(12) Uani 1 1 d . . . 0
C10 C -0.1210(5) -0.0464(4) 0.29143(15) 0.0572(14) Uani 1 1 d . . . 0
C11 C -0.0622(5) 0.0369(3) 0.28902(13) 0.0495(12) Uani 1 1 d . . . 0
C12 C 0.0288(4) 0.0548(3) 0.31501(12) 0.0402(10) Uani 1 1 d . . . 0
C13 C -0.0173(5) 0.0423(4) 0.44652(14) 0.0534(13) Uani 1 1 d . . . 0
C14 C -0.0988(5) 0.0933(5) 0.46801(16) 0.0676(16) Uani 1 1 d . . . 0
C15 C -0.0988(6) 0.1876(5) 0.46418(18) 0.0759(18) Uani 1 1 d . . . 0
C16 C -0.0185(5) 0.2292(4) 0.43956(17) 0.0621(14) Uani 1 1 d . . . 0
C17 C 0.0607(4) 0.1762(3) 0.41827(12) 0.0412(10) Uani 1 1 d . . . 0
C18 C 0.1511(4) 0.2145(3) 0.39134(12) 0.0417(10) Uani 1 1 d . . . 0
C19 C 0.1721(5) 0.3066(3) 0.38291(16) 0.0570(14) Uani 1 1 d . . . 0
C20 C 0.2617(6) 0.3287(4) 0.35701(17) 0.0643(16) Uani 1 1 d . . . 0
C21 C 0.3306(5) 0.2613(3) 0.34000(15) 0.0521(13) Uani 1 1 d . . . 0
C22 C 0.3090(4) 0.1693(3) 0.34955(11) 0.0365(9) Uani 1 1 d . . . 0
C23 C 0.3744(4) 0.0871(3) 0.33498(12) 0.0387(10) Uani 1 1 d . . . 0
C24 C 0.4734(4) 0.0901(4) 0.31084(14) 0.0503(12) Uani 1 1 d . . . 0
C25 C 0.5312(5) 0.0100(4) 0.30064(15) 0.0585(14) Uani 1 1 d . . . 0
C26 C 0.4875(5) -0.0732(4) 0.31445(16) 0.0552(13) Uani 1 1 d . . . 0
C27 C 0.3872(4) -0.0733(3) 0.33777(13) 0.0419(11) Uani 1 1 d . . . 0
Cl Cl 0.20450(10) 0.78076(8) 0.26525(3) 0.0508(3) Uani 1 1 d . . . 0
O4 O 0.3255(3) 0.7613(3) 0.25503(11) 0.0858(13) Uani 1 1 d . . . 0
O5 O 0.1249(5) 0.7318(4) 0.24076(13) 0.1134(18) Uani 1 1 d . . . 0
O6 O 0.1864(3) 0.7561(3) 0.30546(10) 0.0681(10) Uani 1 1 d . . . 0
O7 O 0.1874(4) 0.8779(3) 0.26037(14) 0.0957(14) Uani 1 1 d . . . 0
O111 O 0.0869(7) 0.4106(5) 0.4829(2) 0.073(2) Uani 0.50 1 d P . . 2
H11 H -0.081(4) 0.080(3) 0.2714(11) 0.033(11) Uiso 1 1 d . . . 0
H5 H 0.321(4) -0.175(3) 0.4507(12) 0.042(13) Uiso 1 1 d . . . 0
H12 H 0.070(4) 0.109(3) 0.3143(12) 0.040(12) Uiso 1 1 d . . . 0
H13 H -0.019(4) -0.022(3) 0.4472(13) 0.054(14) Uiso 1 1 d . . . 0
H9 H -0.114(5) -0.171(4) 0.3201(14) 0.067(16) Uiso 1 1 d . . . 0
H21 H 0.389(4) 0.273(3) 0.3256(12) 0.041(13) Uiso 1 1 d . . . 0
H10 H -0.182(4) -0.062(3) 0.2746(13) 0.052(13) Uiso 1 1 d . . . 0
H24 H 0.487(4) 0.146(3) 0.2998(14) 0.058(15) Uiso 1 1 d . . . 0
H3 H 0.207(7) -0.440(6) 0.455(2) 0.14(3) Uiso 1 1 d . . . 0
H26 H 0.521(5) -0.124(4) 0.3112(15) 0.068(18) Uiso 1 1 d . . . 0
H27 H 0.355(4) -0.124(3) 0.3464(12) 0.037(12) Uiso 1 1 d . . . 0
H25 H 0.602(4) 0.015(3) 0.2841(14) 0.062(14) Uiso 1 1 d . . . 0
H16 H -0.017(5) 0.293(4) 0.4366(15) 0.067(16) Uiso 1 1 d . . . 0
H19 H 0.132(5) 0.352(4) 0.3924(15) 0.071(18) Uiso 1 1 d . . . 0
H4 H 0.358(5) -0.323(4) 0.4793(16) 0.10(2) Uiso 1 1 d . . . 0
H20 H 0.270(4) 0.384(4) 0.3489(15) 0.063(16) Uiso 1 1 d . . . 0
H15 H -0.152(5) 0.223(4) 0.4773(14) 0.068(16) Uiso 1 1 d . . . 0
H14 H -0.149(5) 0.061(4) 0.4839(14) 0.061(15) Uiso 1 1 d . . . 0
H2 H 0.051(5) -0.410(4) 0.4132(17) 0.10(2) Uiso 1 1 d . . . 0
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
Ru 0.03080(17) 0.02682(17) 0.03005(17) 0.00229(13) -0.00063(14) -0.00337(14)
O1 0.081(3) 0.213(6) 0.044(2) -0.002(3) -0.009(2) -0.010(3)
O2 0.057(2) 0.101(3) 0.075(3) 0.000(2) -0.020(2) -0.015(2)
O3 0.0536(19) 0.0307(16) 0.0571(18) 0.0038(14) -0.0006(15) -0.0115(14)
N1 0.0345(18) 0.0314(18) 0.0356(19) 0.0017(14) 0.0029(15) -0.0015(15)
N2 0.0317(17) 0.0321(19) 0.0308(16) -0.0005(14) 0.0005(14) 0.0026(14)
N3 0.0392(19) 0.0380(19) 0.0330(18) -0.0005(15) 0.0008(16) -0.0020(16)
N4 0.0370(19) 0.0268(17) 0.0354(17) 0.0021(14) -0.0030(14) -0.0027(14)
N5 0.0333(18) 0.0302(19) 0.0373(17) -0.0005(14) 0.0002(14) -0.0022(14)
N6 0.039(2) 0.042(2) 0.041(2) 0.0027(16) -0.0007(17) -0.0073(18)
C1 0.057(3) 0.036(2) 0.046(2) 0.007(2) 0.007(2) 0.000(2)
C2 0.087(4) 0.039(3) 0.078(4) 0.014(3) 0.007(3) -0.007(3)
C3 0.112(5) 0.049(3) 0.075(4) 0.022(3) -0.003(4) 0.014(4)
C4 0.085(4) 0.063(4) 0.058(3) 0.019(3) 0.001(3) 0.022(3)
C5 0.055(3) 0.053(3) 0.046(3) 0.004(2) 0.002(2) 0.002(3)
C6 0.043(2) 0.032(2) 0.039(2) 0.0078(18) 0.007(2) 0.004(2)
C7 0.037(2) 0.032(2) 0.041(2) 0.0005(18) 0.0020(19) -0.0047(19)
C8 0.031(2) 0.033(2) 0.039(2) -0.0010(18) 0.0011(18) -0.0029(17)
C9 0.045(3) 0.044(3) 0.061(3) -0.008(2) -0.012(2) -0.005(2)
C10 0.051(3) 0.063(3) 0.057(3) -0.015(3) -0.021(3) 0.014(3)
C11 0.061(3) 0.050(3) 0.038(2) 0.001(2) -0.007(2) 0.020(3)
C12 0.047(3) 0.035(2) 0.039(2) -0.0016(19) -0.002(2) 0.007(2)
C13 0.053(3) 0.054(3) 0.053(3) 0.001(2) 0.016(2) -0.003(3)
C14 0.060(3) 0.087(5) 0.056(3) -0.003(3) 0.025(3) -0.005(3)
C15 0.072(4) 0.079(5) 0.076(4) -0.011(3) 0.026(3) 0.017(4)
C16 0.067(4) 0.052(3) 0.067(3) -0.006(3) 0.007(3) 0.010(3)
C17 0.049(3) 0.037(2) 0.037(2) -0.0025(18) 0.000(2) 0.005(2)
C18 0.049(2) 0.033(2) 0.044(2) -0.0026(19) -0.004(2) 0.0008(19)
C19 0.079(4) 0.032(3) 0.061(3) 0.000(2) -0.003(3) 0.006(3)
C20 0.086(4) 0.033(3) 0.073(4) 0.014(3) -0.002(3) -0.011(3)
C21 0.061(3) 0.041(3) 0.054(3) 0.008(2) 0.006(3) -0.014(2)
C22 0.043(2) 0.032(2) 0.035(2) 0.0051(17) -0.002(2) -0.011(2)
C23 0.038(2) 0.042(2) 0.036(2) 0.0030(19) -0.0029(19) -0.009(2)
C24 0.047(3) 0.060(3) 0.044(3) 0.008(2) 0.008(2) -0.013(3)
C25 0.044(3) 0.081(4) 0.051(3) 0.003(3) 0.017(2) 0.001(3)
C26 0.052(3) 0.053(3) 0.061(3) 0.000(3) 0.007(3) 0.014(3)
C27 0.048(3) 0.039(3) 0.040(2) 0.001(2) 0.003(2) 0.001(2)
Cl 0.0455(6) 0.0520(7) 0.0549(6) 0.0113(5) 0.0006(5) 0.0020(5)
O4 0.063(2) 0.107(3) 0.088(3) 0.034(3) 0.023(2) 0.025(2)
O5 0.119(4) 0.127(4) 0.095(3) -0.013(3) -0.028(3) -0.046(3)
O6 0.070(2) 0.075(2) 0.060(2) 0.0158(19) 0.0153(19) 0.004(2)
O7 0.100(3) 0.063(3) 0.123(4) 0.036(2) -0.006(3) 0.015(3)
O111 0.069(5) 0.064(5) 0.087(5) -0.014(4) -0.041(4) 0.011(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'
O O 0.0106 0.0060 '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'
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
N4 Ru N6 89.34(13) . . ?
N4 Ru N5 79.90(13) . . ?
N6 Ru N5 89.67(14) . . ?
N4 Ru N3 79.76(13) . . ?
N6 Ru N3 89.68(14) . . ?
N5 Ru N3 159.65(13) . . ?
N4 Ru N1 173.78(13) . . ?
N6 Ru N1 96.87(13) . . ?
N5 Ru N1 99.83(12) . . ?
N3 Ru N1 100.44(13) . . ?
N4 Ru N2 96.38(12) . . ?
N6 Ru N2 174.02(13) . . ?
N5 Ru N2 93.02(13) . . ?
N3 Ru N2 89.65(12) . . ?
N1 Ru N2 77.42(12) . . ?
C7 O3 C1 103.8(3) . . ?
C7 N1 C6 104.8(3) . . ?
C7 N1 Ru 112.5(3) . . ?
C6 N1 Ru 142.6(3) . . ?
C12 N2 C8 116.8(4) . . ?
C12 N2 Ru 127.0(3) . . ?
C8 N2 Ru 116.2(2) . . ?
C13 N3 C17 117.7(4) . . ?
C13 N3 Ru 129.1(3) . . ?
C17 N3 Ru 113.1(3) . . ?
C22 N4 C18 122.2(4) . . ?
C22 N4 Ru 118.7(3) . . ?
C18 N4 Ru 119.0(3) . . ?
C27 N5 C23 118.3(4) . . ?
C27 N5 Ru 128.1(3) . . ?
C23 N5 Ru 113.5(3) . . ?
O1 N6 O2 117.1(4) . . ?
O1 N6 Ru 120.8(3) . . ?
O2 N6 Ru 122.1(3) . . ?
C6 C1 C2 124.5(5) . . ?
C6 C1 O3 108.8(4) . . ?
C2 C1 O3 126.7(5) . . ?
C3 C2 C1 114.3(6) . . ?
C3 C2 H2 122(4) . . ?
C1 C2 H2 124(4) . . ?
C2 C3 C4 123.5(5) . . ?
C2 C3 H3 115(5) . . ?
C4 C3 H3 121(5) . . ?
C5 C4 C3 120.5(6) . . ?
C5 C4 H4 118(3) . . ?
C3 C4 H4 122(3) . . ?
C4 C5 C6 116.9(5) . . ?
C4 C5 H5 121(3) . . ?
C6 C5 H5 123(3) . . ?
C1 C6 C5 120.3(4) . . ?
C1 C6 N1 107.8(4) . . ?
C5 C6 N1 132.0(4) . . ?
N1 C7 O3 114.8(4) . . ?
N1 C7 C8 121.9(4) . . ?
O3 C7 C8 123.1(4) . . ?
N2 C8 C9 122.6(4) . . ?
N2 C8 C7 111.2(3) . . ?
C9 C8 C7 126.2(4) . . ?
C10 C9 C8 118.9(5) . . ?
C10 C9 H9 125(3) . . ?
C8 C9 H9 116(3) . . ?
C9 C10 C11 119.6(5) . . ?
C9 C10 H10 118(3) . . ?
C11 C10 H10 122(3) . . ?
C12 C11 C10 118.8(5) . . ?
C12 C11 H11 119(3) . . ?
C10 C11 H11 123(3) . . ?
N2 C12 C11 123.4(5) . . ?
N2 C12 H12 115(3) . . ?
C11 C12 H12 122(3) . . ?
N3 C13 C14 122.9(5) . . ?
N3 C13 H13 116(3) . . ?
C14 C13 H13 120(3) . . ?
C15 C14 C13 118.7(6) . . ?
C15 C14 H14 125(3) . . ?
C13 C14 H14 117(3) . . ?
C14 C15 C16 119.7(6) . . ?
C14 C15 H15 121(3) . . ?
C16 C15 H15 119(3) . . ?
C15 C16 C17 120.2(5) . . ?
C15 C16 H16 121(3) . . ?
C17 C16 H16 119(3) . . ?
N3 C17 C16 120.9(4) . . ?
N3 C17 C18 115.0(4) . . ?
C16 C17 C18 124.2(4) . . ?
N4 C18 C19 119.4(4) . . ?
N4 C18 C17 113.1(4) . . ?
C19 C18 C17 127.4(4) . . ?
C20 C19 C18 118.8(5) . . ?
C20 C19 H19 117(4) . . ?
C18 C19 H19 124(4) . . ?
C21 C20 C19 121.2(5) . . ?
C21 C20 H20 118(4) . . ?
C19 C20 H20 120(4) . . ?
C20 C21 C22 118.8(5) . . ?
C20 C21 H21 123(3) . . ?
C22 C21 H21 118(3) . . ?
N4 C22 C21 119.5(4) . . ?
N4 C22 C23 113.5(3) . . ?
C21 C22 C23 127.0(4) . . ?
N5 C23 C24 120.8(4) . . ?
N5 C23 C22 114.4(3) . . ?
C24 C23 C22 124.8(4) . . ?
C25 C24 C23 120.2(5) . . ?
C25 C24 H24 124(3) . . ?
C23 C24 H24 115(3) . . ?
C24 C25 C26 118.7(5) . . ?
C24 C25 H25 118(3) . . ?
C26 C25 H25 123(3) . . ?
C27 C26 C25 119.3(5) . . ?
C27 C26 H26 117(4) . . ?
C25 C26 H26 124(4) . . ?
N5 C27 C26 122.7(5) . . ?
N5 C27 H27 115(3) . . ?
C26 C27 H27 122(3) . . ?
O5 Cl O7 109.8(3) . . ?
O5 Cl O4 111.0(3) . . ?
O7 Cl O4 107.1(3) . . ?
O5 Cl O6 110.6(3) . . ?
O7 Cl O6 109.7(3) . . ?
O4 Cl O6 108.6(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
Ru N4 1.956(3) . ?
Ru N6 2.029(3) . ?
Ru N5 2.056(3) . ?
Ru N3 2.077(3) . ?
Ru N1 2.101(3) . ?
Ru N2 2.101(3) . ?
O1 N6 1.193(5) . ?
O2 N6 1.225(5) . ?
O3 C7 1.360(5) . ?
O3 C1 1.383(5) . ?
N1 C7 1.308(5) . ?
N1 C6 1.404(5) . ?
N2 C12 1.341(5) . ?
N2 C8 1.362(5) . ?
N3 C13 1.344(6) . ?
N3 C17 1.376(5) . ?
N4 C22 1.338(5) . ?
N4 C18 1.358(5) . ?
N5 C27 1.333(5) . ?
N5 C23 1.370(5) . ?
C1 C6 1.372(6) . ?
C1 C2 1.379(6) . ?
C2 C3 1.368(9) . ?
C2 H2 0.99(6) . ?
C3 C4 1.393(9) . ?
C3 H3 0.97(8) . ?
C4 C5 1.385(7) . ?
C4 H4 1.16(6) . ?
C5 C6 1.387(6) . ?
C5 H5 0.89(4) . ?
C7 C8 1.438(6) . ?
C8 C9 1.381(6) . ?
C9 C10 1.366(7) . ?
C9 H9 0.93(5) . ?
C10 C11 1.374(7) . ?
C10 H10 0.92(5) . ?
C11 C12 1.374(6) . ?
C11 H11 0.88(4) . ?
C12 H12 0.91(4) . ?
C13 C14 1.383(7) . ?
C13 H13 0.92(5) . ?
C14 C15 1.367(8) . ?
C14 H14 0.91(5) . ?
C15 C16 1.367(8) . ?
C15 H15 0.91(5) . ?
C16 C17 1.377(7) . ?
C16 H16 0.93(5) . ?
C17 C18 1.473(6) . ?
C18 C19 1.380(6) . ?
C19 C20 1.373(8) . ?
C19 H19 0.85(5) . ?
C20 C21 1.370(8) . ?
C20 H20 0.85(5) . ?
C21 C22 1.388(6) . ?
C21 H21 0.83(4) . ?
C22 C23 1.479(6) . ?
C23 C24 1.381(6) . ?
C24 C25 1.370(7) . ?
C24 H24 0.90(5) . ?
C25 C26 1.378(7) . ?
C25 H25 0.97(5) . ?
C26 C27 1.375(7) . ?
C26 H26 0.83(5) . ?
C27 H27 0.87(4) . ?
Cl O5 1.410(4) . ?
Cl O7 1.424(4) . ?
Cl O4 1.427(4) . ?
Cl O6 1.429(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
N4 Ru N1 C7 -10.7(13) . . . . ?
N6 Ru N1 C7 171.5(3) . . . . ?
N5 Ru N1 C7 -97.7(3) . . . . ?
N3 Ru N1 C7 80.5(3) . . . . ?
N2 Ru N1 C7 -6.8(3) . . . . ?
N4 Ru N1 C6 166.8(10) . . . . ?
N6 Ru N1 C6 -11.0(5) . . . . ?
N5 Ru N1 C6 79.8(4) . . . . ?
N3 Ru N1 C6 -102.0(4) . . . . ?
N2 Ru N1 C6 170.8(5) . . . . ?
N4 Ru N2 C12 5.1(3) . . . . ?
N6 Ru N2 C12 168.2(12) . . . . ?
N5 Ru N2 C12 -75.1(3) . . . . ?
N3 Ru N2 C12 84.7(3) . . . . ?
N1 Ru N2 C12 -174.5(4) . . . . ?
N4 Ru N2 C8 -172.3(3) . . . . ?
N6 Ru N2 C8 -9.2(14) . . . . ?
N5 Ru N2 C8 107.5(3) . . . . ?
N3 Ru N2 C8 -92.7(3) . . . . ?
N1 Ru N2 C8 8.1(3) . . . . ?
N4 Ru N3 C13 -177.7(4) . . . . ?
N6 Ru N3 C13 -88.3(4) . . . . ?
N5 Ru N3 C13 -176.5(4) . . . . ?
N1 Ru N3 C13 8.6(4) . . . . ?
N2 Ru N3 C13 85.7(4) . . . . ?
N4 Ru N3 C17 0.4(3) . . . . ?
N6 Ru N3 C17 89.8(3) . . . . ?
N5 Ru N3 C17 1.6(5) . . . . ?
N1 Ru N3 C17 -173.3(3) . . . . ?
N2 Ru N3 C17 -96.1(3) . . . . ?
N6 Ru N4 C22 89.6(3) . . . . ?
N5 Ru N4 C22 -0.2(3) . . . . ?
N3 Ru N4 C22 179.3(3) . . . . ?
N1 Ru N4 C22 -88.3(12) . . . . ?
N2 Ru N4 C22 -92.2(3) . . . . ?
N6 Ru N4 C18 -90.6(3) . . . . ?
N5 Ru N4 C18 179.7(3) . . . . ?
N3 Ru N4 C18 -0.8(3) . . . . ?
N1 Ru N4 C18 91.6(12) . . . . ?
N2 Ru N4 C18 87.7(3) . . . . ?
N4 Ru N5 C27 177.2(4) . . . . ?
N6 Ru N5 C27 87.8(4) . . . . ?
N3 Ru N5 C27 176.0(4) . . . . ?
N1 Ru N5 C27 -9.1(4) . . . . ?
N2 Ru N5 C27 -86.8(4) . . . . ?
N4 Ru N5 C23 1.1(3) . . . . ?
N6 Ru N5 C23 -88.2(3) . . . . ?
N3 Ru N5 C23 -0.1(5) . . . . ?
N1 Ru N5 C23 174.8(3) . . . . ?
N2 Ru N5 C23 97.1(3) . . . . ?
N4 Ru N6 O1 121.8(4) . . . . ?
N5 Ru N6 O1 -158.3(4) . . . . ?
N3 Ru N6 O1 42.1(4) . . . . ?
N1 Ru N6 O1 -58.4(4) . . . . ?
N2 Ru N6 O1 -41.4(15) . . . . ?
N4 Ru N6 O2 -61.2(4) . . . . ?
N5 Ru N6 O2 18.7(4) . . . . ?
N3 Ru N6 O2 -141.0(4) . . . . ?
N1 Ru N6 O2 118.5(4) . . . . ?
N2 Ru N6 O2 135.5(11) . . . . ?
C7 O3 C1 C6 0.5(5) . . . . ?
C7 O3 C1 C2 -179.6(5) . . . . ?
C6 C1 C2 C3 -1.4(8) . . . . ?
O3 C1 C2 C3 178.8(5) . . . . ?
C1 C2 C3 C4 -0.2(9) . . . . ?
C2 C3 C4 C5 1.5(10) . . . . ?
C3 C4 C5 C6 -1.1(8) . . . . ?
C2 C1 C6 C5 1.8(7) . . . . ?
O3 C1 C6 C5 -178.4(4) . . . . ?
C2 C1 C6 N1 -179.2(5) . . . . ?
O3 C1 C6 N1 0.7(5) . . . . ?
C4 C5 C6 C1 -0.5(7) . . . . ?
C4 C5 C6 N1 -179.2(4) . . . . ?
C7 N1 C6 C1 -1.6(5) . . . . ?
Ru N1 C6 C1 -179.3(3) . . . . ?
C7 N1 C6 C5 177.2(5) . . . . ?
Ru N1 C6 C5 -0.4(8) . . . . ?
C6 N1 C7 O3 2.1(5) . . . . ?
Ru N1 C7 O3 -179.5(3) . . . . ?
C6 N1 C7 C8 -173.3(4) . . . . ?
Ru N1 C7 C8 5.1(5) . . . . ?
C1 O3 C7 N1 -1.7(5) . . . . ?
C1 O3 C7 C8 173.7(4) . . . . ?
C12 N2 C8 C9 -2.4(6) . . . . ?
Ru N2 C8 C9 175.3(3) . . . . ?
C12 N2 C8 C7 174.6(4) . . . . ?
Ru N2 C8 C7 -7.7(4) . . . . ?
N1 C7 C8 N2 1.6(6) . . . . ?
O3 C7 C8 N2 -173.4(4) . . . . ?
N1 C7 C8 C9 178.5(4) . . . . ?
O3 C7 C8 C9 3.4(7) . . . . ?
N2 C8 C9 C10 0.6(7) . . . . ?
C7 C8 C9 C10 -175.9(4) . . . . ?
C8 C9 C10 C11 1.3(8) . . . . ?
C9 C10 C11 C12 -1.2(7) . . . . ?
C8 N2 C12 C11 2.4(6) . . . . ?
Ru N2 C12 C11 -175.0(3) . . . . ?
C10 C11 C12 N2 -0.7(7) . . . . ?
C17 N3 C13 C14 1.4(7) . . . . ?
Ru N3 C13 C14 179.4(4) . . . . ?
N3 C13 C14 C15 -0.9(9) . . . . ?
C13 C14 C15 C16 -0.3(10) . . . . ?
C14 C15 C16 C17 1.0(10) . . . . ?
C13 N3 C17 C16 -0.7(7) . . . . ?
Ru N3 C17 C16 -179.0(4) . . . . ?
C13 N3 C17 C18 178.3(4) . . . . ?
Ru N3 C17 C18 0.0(5) . . . . ?
C15 C16 C17 N3 -0.5(8) . . . . ?
C15 C16 C17 C18 -179.4(5) . . . . ?
C22 N4 C18 C19 -0.7(6) . . . . ?
Ru N4 C18 C19 179.4(3) . . . . ?
C22 N4 C18 C17 -179.2(4) . . . . ?
Ru N4 C18 C17 1.0(5) . . . . ?
N3 C17 C18 N4 -0.6(5) . . . . ?
C16 C17 C18 N4 178.4(4) . . . . ?
N3 C17 C18 C19 -178.9(5) . . . . ?
C16 C17 C18 C19 0.1(8) . . . . ?
N4 C18 C19 C20 1.3(7) . . . . ?
C17 C18 C19 C20 179.5(5) . . . . ?
C18 C19 C20 C21 -0.8(8) . . . . ?
C19 C20 C21 C22 -0.4(8) . . . . ?
C18 N4 C22 C21 -0.5(6) . . . . ?
Ru N4 C22 C21 179.4(3) . . . . ?
C18 N4 C22 C23 179.4(4) . . . . ?
Ru N4 C22 C23 -0.7(4) . . . . ?
C20 C21 C22 N4 1.0(7) . . . . ?
C20 C21 C22 C23 -178.9(5) . . . . ?
C27 N5 C23 C24 -0.6(6) . . . . ?
Ru N5 C23 C24 175.9(3) . . . . ?
C27 N5 C23 C22 -178.3(4) . . . . ?
Ru N5 C23 C22 -1.8(4) . . . . ?
N4 C22 C23 N5 1.7(5) . . . . ?
C21 C22 C23 N5 -178.4(4) . . . . ?
N4 C22 C23 C24 -175.9(4) . . . . ?
C21 C22 C23 C24 4.0(7) . . . . ?
N5 C23 C24 C25 -0.9(7) . . . . ?
C22 C23 C24 C25 176.6(4) . . . . ?
C23 C24 C25 C26 1.0(8) . . . . ?
C24 C25 C26 C27 0.3(8) . . . . ?
C23 N5 C27 C26 2.0(6) . . . . ?
Ru N5 C27 C26 -173.9(4) . . . . ?
C25 C26 C27 N5 -1.9(8) . . . . ?
|
1100945.cif | #------------------------------------------------------------------------------
#$Date: 2016-12-31 20:31:26 +0200 (Sat, 31 Dec 2016) $
#$Revision: 189516 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/09/1100945.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_1100945
loop_
_publ_author_name
'Nripen Chanda'
'Debamita Paul'
'Sanjib Kar'
'Shaikh M. Mobin'
'Anindya Datta'
'Vedavati G. Puranik'
'K. Krishnamurthy Rao'
'Goutam Kumar Lahiri'
_publ_section_title
;
Effect of 2-(2-Pyridyl)azole-Based Ancillary Ligands (L1-4) on the
Electrophilicity of the Nitrosyl Function in [RuII(trpy)(L1-4)(NO)]3+
[trpy = 2,2':6',2''-Terpyridine]. Synthesis, Structures, and
Spectroscopic, Electrochemical, and Kinetic Aspects
;
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3499
_journal_page_last 3511
_journal_paper_doi 10.1021/ic048184w
_journal_volume 44
_journal_year 2005
_chemical_formula_moiety '2[C27 H18 N5 S Ru (ClO4)].0.5CH3OH'
_chemical_formula_sum 'C27.25 H20 Cl2 N5 O4.25 Ru S'
_chemical_formula_weight 689.51
_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 113.505(2)
_cell_angle_beta 93.348(2)
_cell_angle_gamma 105.418(2)
_cell_formula_units_Z 4
_cell_length_a 13.6062(16)
_cell_length_b 15.2525(18)
_cell_length_c 15.6016(19)
_cell_measurement_reflns_used 4686
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 21.41
_cell_measurement_theta_min 2.31
_cell_volume 2812.3(6)
_computing_cell_refinement 'BRUKER SAINT'
_computing_data_collection 'BRUKER SMART'
_computing_data_reduction 'BRUKER SAINT'
_computing_molecular_graphics 'SHELXTL and PLATON'
_computing_publication_material 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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device ' Bruker Smart APEX'
_diffrn_measurement_device_type ' CCD Area Detector'
_diffrn_measurement_method 'Omega Scan'
_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 0.0450
_diffrn_reflns_av_sigmaI/netI 0.0610
_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 18
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_number 27237
_diffrn_reflns_theta_full 25.00
_diffrn_reflns_theta_max 25.00
_diffrn_reflns_theta_min 1.45
_exptl_absorpt_coefficient_mu 0.866
_exptl_absorpt_correction_T_max 0.9645
_exptl_absorpt_correction_T_min 0.7787
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Bruker SADABS'
_exptl_crystal_colour brown
_exptl_crystal_density_diffrn 1.628
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 1386
_exptl_crystal_size_max 0.30
_exptl_crystal_size_mid 0.23
_exptl_crystal_size_min 0.04
_refine_diff_density_max 2.212
_refine_diff_density_min -0.590
_refine_diff_density_rms 0.146
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.051
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 739
_refine_ls_number_reflns 9875
_refine_ls_number_restraints 75
_refine_ls_restrained_S_all 1.076
_refine_ls_R_factor_all 0.1044
_refine_ls_R_factor_gt 0.0715
_refine_ls_shift/su_max 0.007
_refine_ls_shift/su_mean 0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1206P)^2^+4.3163P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1933
_refine_ls_wR_factor_ref 0.2138
_reflns_number_gt 6727
_reflns_number_total 9875
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file ic048184wsi20041223_113625.cif
_cod_data_source_block thiacl
_cod_depositor_comments
;
Marking attached hydrogen atoms.
Antanas Vaitkus,
2016-12-31
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_formula_sum 'C54.50 H40 Cl4 N10 O8.50 Ru2 S2'
_cod_database_code 1100945
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
_atom_site_attached_hydrogens
Ru Ru 0.25329(4) 0.01295(4) 0.16648(4) 0.0469(2) Uani 1 1 d . . . 0
Cl Cl 0.19542(14) -0.12004(15) 0.00878(14) 0.0589(5) Uani 1 1 d . . . 0
S S 0.4082(2) 0.1595(2) 0.47349(17) 0.0849(8) Uani 1 1 d . . . 0
N1 N 0.3067(5) 0.1108(5) 0.3086(4) 0.0538(16) Uani 1 1 d . . . 0
N2 N 0.3085(5) -0.0750(5) 0.2207(5) 0.0546(16) Uani 1 1 d . . . 0
N3 N 0.0990(5) -0.0127(5) 0.1830(4) 0.0588(17) Uani 1 1 d . . . 0
N4 N 0.2116(5) 0.0984(5) 0.1156(4) 0.0520(16) Uani 1 1 d . . . 0
N5 N 0.3895(4) 0.0724(4) 0.1298(4) 0.0471(14) Uani 1 1 d . . . 0
C1 C 0.3634(7) 0.2481(7) 0.4573(6) 0.066(2) Uani 1 1 d . . . 0
C2 C 0.3751(9) 0.3455(8) 0.5205(8) 0.092(3) Uani 1 1 d . . . 0
H2 H 0.4131 0.3726 0.5818 0.111 Uiso 1 1 calc R . . 0
C3 C 0.3310(8) 0.4004(8) 0.4925(7) 0.084(3) Uani 1 1 d . . . 0
H3 H 0.3364 0.4654 0.5357 0.101 Uiso 1 1 calc R . . 0
C4 C 0.2786(8) 0.3636(7) 0.4027(7) 0.080(3) Uani 1 1 d . . . 0
H4 H 0.2499 0.4045 0.3855 0.096 Uiso 1 1 calc R . . 0
C5 C 0.2668(6) 0.2680(6) 0.3363(6) 0.061(2) Uani 1 1 d . . . 0
H5 H 0.2316 0.2441 0.2744 0.073 Uiso 1 1 calc R . . 0
C6 C 0.3088(6) 0.2085(6) 0.3642(6) 0.058(2) Uani 1 1 d . . . 0
C7 C 0.3519(6) 0.0746(6) 0.3583(6) 0.057(2) Uani 1 1 d . . . 0
C8 C 0.3514(6) -0.0280(7) 0.3122(6) 0.063(2) Uani 1 1 d . . . 0
C9 C 0.3937(8) -0.0741(8) 0.3597(8) 0.088(3) Uani 1 1 d . . . 0
H9 H 0.4232 -0.0398 0.4240 0.106 Uiso 1 1 calc R . . 0
C10 C 0.3900(9) -0.1736(9) 0.3067(9) 0.096(3) Uani 1 1 d . . . 0
H10 H 0.4164 -0.2075 0.3355 0.115 Uiso 1 1 calc R . . 0
C11 C 0.3474(7) -0.2205(7) 0.2128(7) 0.078(3) Uani 1 1 d . . . 0
H11 H 0.3446 -0.2868 0.1765 0.093 Uiso 1 1 calc R . . 0
C12 C 0.3087(6) -0.1692(6) 0.1723(6) 0.060(2) Uani 1 1 d . . . 0
H12 H 0.2811 -0.2018 0.1075 0.072 Uiso 1 1 calc R . . 0
C13 C 0.0492(7) -0.0705(7) 0.2222(7) 0.079(3) Uani 1 1 d . . . 0
H13 H 0.0836 -0.1050 0.2440 0.095 Uiso 1 1 calc R . . 0
C14 C -0.0549(8) -0.0801(8) 0.2308(8) 0.082(3) Uani 1 1 d . . . 0
H14 H -0.0893 -0.1202 0.2586 0.099 Uiso 1 1 calc R . . 0
C15 C -0.1047(9) -0.0298(9) 0.1980(9) 0.107(4) Uani 1 1 d . . . 0
H15 H -0.1735 -0.0351 0.2037 0.129 Uiso 1 1 calc R . . 0
C16 C -0.0526(7) 0.0295(7) 0.1558(7) 0.083(3) Uani 1 1 d . . . 0
H16 H -0.0868 0.0627 0.1319 0.100 Uiso 1 1 calc R . . 0
C17 C 0.0505(6) 0.0387(7) 0.1498(6) 0.063(2) Uani 1 1 d . . . 0
C18 C 0.1118(6) 0.0993(6) 0.1100(6) 0.058(2) Uani 1 1 d . . . 0
C19 C 0.0841(8) 0.1606(8) 0.0718(7) 0.078(3) Uani 1 1 d . . . 0
H19 H 0.0164 0.1625 0.0669 0.094 Uiso 1 1 calc R . . 0
C20 C 0.1561(9) 0.2167(8) 0.0424(7) 0.086(3) Uani 1 1 d . . . 0
H20 H 0.1378 0.2586 0.0189 0.103 Uiso 1 1 calc R . . 0
C21 C 0.2544(8) 0.2129(7) 0.0466(7) 0.075(2) Uani 1 1 d . . . 0
H21 H 0.3029 0.2515 0.0254 0.090 Uiso 1 1 calc R . . 0
C22 C 0.2827(6) 0.1519(6) 0.0821(6) 0.058(2) Uani 1 1 d . . . 0
C23 C 0.3838(6) 0.1368(5) 0.0908(5) 0.0519(18) Uani 1 1 d . . . 0
C24 C 0.4682(7) 0.1830(6) 0.0621(6) 0.063(2) Uani 1 1 d . . . 0
H24 H 0.4633 0.2277 0.0367 0.076 Uiso 1 1 calc R . . 0
C25 C 0.5586(7) 0.1629(7) 0.0709(6) 0.071(3) Uani 1 1 d . . . 0
H25 H 0.6152 0.1926 0.0502 0.085 Uiso 1 1 calc R . . 0
C26 C 0.5662(6) 0.0983(6) 0.1107(6) 0.067(2) Uani 1 1 d . . . 0
H26 H 0.6278 0.0841 0.1177 0.080 Uiso 1 1 calc R . . 0
C27 C 0.4809(6) 0.0556(6) 0.1396(6) 0.0565(19) Uani 1 1 d . . . 0
H27 H 0.4862 0.0129 0.1674 0.068 Uiso 1 1 calc R . . 0
Ru' Ru 0.22704(4) 0.47666(4) 0.80737(5) 0.0478(2) Uani 1 1 d . . . 0
Cl' Cl 0.30041(15) 0.61272(16) 0.95968(14) 0.0614(5) Uani 1 1 d . . . 0
S' S 0.1817(3) 0.1664(2) 0.5812(2) 0.0948(9) Uani 1 1 d . . . 0
N6 N 0.1827(5) 0.3491(5) 0.6819(5) 0.0590(17) Uani 1 1 d . . . 0
N7 N 0.3138(5) 0.3903(5) 0.8323(5) 0.0598(17) Uani 1 1 d . . . 0
N8 N 0.0971(5) 0.4230(5) 0.8561(4) 0.0510(15) Uani 1 1 d . . . 0
N9 N 0.1402(4) 0.5522(4) 0.7851(4) 0.0472(14) Uani 1 1 d . . . 0
N10 N 0.3246(5) 0.5615(4) 0.7533(4) 0.0496(15) Uani 1 1 d . . . 0
C28 C 0.1063(8) 0.2158(7) 0.5316(7) 0.073(3) Uani 1 1 d . . . 0
C29 C 0.0427(11) 0.1711(10) 0.4448(8) 0.106(4) Uani 1 1 d . . . 0
H29 H 0.0362 0.1053 0.4027 0.127 Uiso 1 1 calc R . . 0
C30 C -0.0103(11) 0.2232(11) 0.4211(9) 0.123(5) Uani 1 1 d . . . 0
H30 H -0.0558 0.1930 0.3630 0.148 Uiso 1 1 calc R . . 0
C31 C 0.0029(10) 0.3231(10) 0.4837(8) 0.113(4) Uani 1 1 d . . . 0
H31 H -0.0307 0.3595 0.4641 0.135 Uiso 1 1 calc R . . 0
C32 C 0.0620(8) 0.3687(8) 0.5707(7) 0.085(3) Uani 1 1 d . . . 0
H32 H 0.0660 0.4339 0.6124 0.102 Uiso 1 1 calc R . . 0
C33 C 0.1172(6) 0.3153(7) 0.5968(6) 0.066(2) Uani 1 1 d . . . 0
C34 C 0.2244(7) 0.2779(6) 0.6808(6) 0.061(2) Uani 1 1 d . . . 0
C35 C 0.2984(7) 0.3007(7) 0.7636(7) 0.068(2) Uani 1 1 d . . . 0
C36 C 0.3446(8) 0.2310(8) 0.7674(9) 0.087(3) Uani 1 1 d . . . 0
H36 H 0.3300 0.1680 0.7165 0.104 Uiso 1 1 calc R . . 0
C37 C 0.4121(9) 0.2583(10) 0.8485(10) 0.097(4) Uani 1 1 d . . . 0
H37 H 0.4471 0.2151 0.8529 0.116 Uiso 1 1 calc R . . 0
C38 C 0.4280(8) 0.3498(9) 0.9233(9) 0.089(3) Uani 1 1 d . . . 0
H38 H 0.4720 0.3685 0.9798 0.107 Uiso 1 1 calc R . . 0
C39 C 0.3781(7) 0.4136(8) 0.9139(8) 0.082(3) Uani 1 1 d . . . 0
H39 H 0.3886 0.4754 0.9654 0.098 Uiso 1 1 calc R . . 0
C40 C 0.0798(7) 0.3569(6) 0.8925(6) 0.066(2) Uani 1 1 d . . . 0
H40 H 0.1308 0.3279 0.8972 0.079 Uiso 1 1 calc R . . 0
C41 C -0.0111(7) 0.3291(7) 0.9240(7) 0.076(3) Uani 1 1 d . . . 0
H41 H -0.0211 0.2819 0.9490 0.092 Uiso 1 1 calc R . . 0
C42 C -0.0866(7) 0.3719(7) 0.9178(7) 0.076(3) Uani 1 1 d . . . 0
H42 H -0.1477 0.3553 0.9399 0.091 Uiso 1 1 calc R . . 0
C43 C -0.0712(6) 0.4380(7) 0.8798(6) 0.066(2) Uani 1 1 d . . . 0
H43 H -0.1223 0.4664 0.8741 0.079 Uiso 1 1 calc R . . 0
C44 C 0.0206(6) 0.4640(6) 0.8490(6) 0.0539(19) Uani 1 1 d . . . 0
C45 C 0.0449(6) 0.5375(6) 0.8083(6) 0.058(2) Uani 1 1 d . . . 0
C46 C -0.0170(7) 0.5909(7) 0.7941(7) 0.072(2) Uani 1 1 d . . . 0
H46 H -0.0835 0.5803 0.8080 0.087 Uiso 1 1 calc R . . 0
C47 C 0.0218(8) 0.6601(8) 0.7589(7) 0.083(3) Uani 1 1 d . . . 0
H47 H -0.0189 0.6968 0.7493 0.100 Uiso 1 1 calc R . . 0
C48 C 0.1195(7) 0.6759(7) 0.7377(7) 0.072(2) Uani 1 1 d . . . 0
H48 H 0.1457 0.7238 0.7153 0.086 Uiso 1 1 calc R . . 0
C49 C 0.1782(6) 0.6198(6) 0.7501(5) 0.0529(19) Uani 1 1 d . . . 0
C50 C 0.2824(6) 0.6239(5) 0.7296(5) 0.0505(18) Uani 1 1 d . . . 0
C51 C 0.3372(7) 0.6829(6) 0.6908(6) 0.065(2) Uani 1 1 d . . . 0
H51 H 0.3073 0.7230 0.6733 0.078 Uiso 1 1 calc R . . 0
C52 C 0.4351(8) 0.6835(7) 0.6775(7) 0.082(3) Uani 1 1 d . . . 0
H52 H 0.4721 0.7237 0.6510 0.098 Uiso 1 1 calc R . . 0
C53 C 0.4785(7) 0.6251(7) 0.7031(7) 0.074(3) Uani 1 1 d . . . 0
H53 H 0.5462 0.6265 0.6961 0.089 Uiso 1 1 calc R . . 0
C54 C 0.4219(6) 0.5643(6) 0.7393(6) 0.059(2) Uani 1 1 d . . . 0
H54 H 0.4517 0.5231 0.7550 0.071 Uiso 1 1 calc R . . 0
Cl1 Cl 0.3181(3) 0.9366(3) 0.6560(4) 0.1275(13) Uani 1 1 d U . . 0
O1 O 0.2473(9) 0.8786(9) 0.6853(11) 0.189(4) Uani 1 1 d U . . 0
O2 O 0.3856(10) 0.8913(10) 0.6191(12) 0.216(5) Uani 1 1 d U . . 0
O3 O 0.3739(11) 1.0207(9) 0.7483(11) 0.198(5) Uani 1 1 d U . . 0
O4 O 0.2689(11) 0.9781(8) 0.6126(10) 0.194(5) Uani 1 1 d U . . 0
Cl2 Cl 0.6561(3) 0.4844(4) 0.7802(5) 0.177(2) Uani 1 1 d U . . 0
O5 O 0.5694(11) 0.4133(12) 0.7527(16) 0.268(6) Uani 1 1 d U . . 0
O6 O 0.7213(11) 0.4274(14) 0.7442(16) 0.270(6) Uani 1 1 d U . . 0
O7 O 0.7211(15) 0.5154(16) 0.8775(16) 0.277(6) Uani 1 1 d U . . 0
O8 O 0.6838(12) 0.5588(12) 0.7622(13) 0.248(6) Uani 1 1 d U . . 0
O O 0.1180(17) 0.868(4) 0.393(2) 0.35(3) Uani 0.50 1 d PDU . . 1
C C 0.157(3) 0.783(4) 0.385(4) 0.38(3) Uani 0.50 1 d PDU . . 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
Ru 0.0341(3) 0.0485(4) 0.0538(4) 0.0185(3) 0.0092(3) 0.0116(3)
Cl 0.0464(10) 0.0544(11) 0.0655(12) 0.0134(9) 0.0072(9) 0.0198(9)
S 0.0888(18) 0.0937(19) 0.0600(14) 0.0163(13) 0.0018(13) 0.0390(15)
N1 0.045(3) 0.051(4) 0.052(4) 0.012(3) 0.012(3) 0.011(3)
N2 0.049(4) 0.050(4) 0.067(4) 0.026(3) 0.014(3) 0.016(3)
N3 0.042(3) 0.056(4) 0.056(4) 0.008(3) 0.014(3) 0.005(3)
N4 0.046(4) 0.051(4) 0.050(4) 0.009(3) 0.002(3) 0.022(3)
N5 0.034(3) 0.042(3) 0.055(4) 0.016(3) 0.008(3) 0.004(3)
C1 0.056(5) 0.065(6) 0.059(5) 0.014(4) 0.011(4) 0.014(4)
C2 0.090(8) 0.087(8) 0.074(7) 0.007(6) 0.016(6) 0.030(6)
C3 0.098(8) 0.070(6) 0.068(7) 0.010(5) 0.022(6) 0.030(6)
C4 0.085(7) 0.056(6) 0.082(7) 0.013(5) 0.028(6) 0.019(5)
C5 0.061(5) 0.056(5) 0.062(5) 0.017(4) 0.019(4) 0.024(4)
C6 0.045(4) 0.054(5) 0.063(5) 0.012(4) 0.024(4) 0.013(4)
C7 0.054(5) 0.060(5) 0.057(5) 0.023(4) 0.006(4) 0.023(4)
C8 0.054(5) 0.073(6) 0.060(5) 0.024(5) 0.006(4) 0.025(4)
C9 0.086(7) 0.080(7) 0.086(7) 0.031(6) -0.014(6) 0.023(6)
C10 0.095(8) 0.092(8) 0.126(10) 0.062(8) 0.012(7) 0.047(7)
C11 0.075(6) 0.064(6) 0.083(7) 0.021(5) 0.003(5) 0.024(5)
C12 0.058(5) 0.045(5) 0.073(5) 0.021(4) 0.008(4) 0.017(4)
C13 0.063(6) 0.064(6) 0.078(6) 0.009(5) 0.027(5) 0.001(4)
C14 0.062(6) 0.074(7) 0.096(8) 0.027(6) 0.033(5) 0.010(5)
C15 0.069(7) 0.093(8) 0.108(9) -0.001(7) 0.048(7) 0.007(6)
C16 0.050(5) 0.079(7) 0.088(7) 0.004(6) 0.009(5) 0.019(5)
C17 0.044(4) 0.070(5) 0.058(5) 0.005(4) 0.008(4) 0.029(4)
C18 0.042(4) 0.057(5) 0.058(5) 0.006(4) 0.004(4) 0.019(4)
C19 0.064(6) 0.088(7) 0.080(6) 0.019(6) 0.006(5) 0.048(5)
C20 0.100(8) 0.094(8) 0.088(7) 0.050(6) 0.019(6) 0.054(7)
C21 0.083(7) 0.072(6) 0.085(7) 0.045(5) 0.019(5) 0.031(5)
C22 0.061(5) 0.049(4) 0.056(5) 0.017(4) 0.017(4) 0.015(4)
C23 0.054(5) 0.043(4) 0.046(4) 0.011(3) 0.008(4) 0.011(3)
C24 0.065(5) 0.058(5) 0.064(5) 0.029(4) 0.018(4) 0.010(4)
C25 0.055(5) 0.066(6) 0.067(6) 0.014(5) 0.026(4) -0.002(4)
C26 0.044(4) 0.057(5) 0.078(6) 0.011(5) 0.017(4) 0.010(4)
C27 0.044(4) 0.059(5) 0.063(5) 0.023(4) 0.013(4) 0.016(4)
Ru' 0.0415(3) 0.0425(4) 0.0620(4) 0.0218(3) 0.0180(3) 0.0165(3)
Cl' 0.0549(11) 0.0644(12) 0.0608(12) 0.0225(10) 0.0112(9) 0.0194(10)
S' 0.133(3) 0.0619(15) 0.0849(18) 0.0207(14) 0.0414(17) 0.0359(16)
N6 0.052(4) 0.049(4) 0.067(4) 0.019(3) 0.020(3) 0.008(3)
N7 0.044(4) 0.053(4) 0.089(5) 0.036(4) 0.019(4) 0.016(3)
N8 0.047(4) 0.050(4) 0.057(4) 0.023(3) 0.016(3) 0.016(3)
N9 0.040(3) 0.049(4) 0.050(3) 0.017(3) 0.009(3) 0.017(3)
N10 0.047(3) 0.043(3) 0.054(4) 0.015(3) 0.017(3) 0.015(3)
C28 0.085(6) 0.057(5) 0.060(6) 0.014(5) 0.019(5) 0.012(5)
C29 0.128(11) 0.089(8) 0.074(8) 0.014(7) 0.013(7) 0.026(8)
C30 0.127(11) 0.120(11) 0.087(9) 0.027(9) -0.010(8) 0.017(9)
C31 0.116(10) 0.117(10) 0.074(7) 0.012(7) -0.008(7) 0.040(8)
C32 0.074(6) 0.095(7) 0.070(6) 0.019(6) -0.008(5) 0.033(6)
C33 0.047(5) 0.077(6) 0.065(6) 0.030(5) 0.014(4) 0.005(4)
C34 0.067(5) 0.049(5) 0.075(6) 0.029(4) 0.028(5) 0.025(4)
C35 0.065(5) 0.064(6) 0.101(7) 0.048(5) 0.049(5) 0.036(5)
C36 0.078(7) 0.091(7) 0.123(9) 0.060(7) 0.049(7) 0.049(6)
C37 0.078(7) 0.107(9) 0.153(12) 0.079(9) 0.051(8) 0.059(7)
C38 0.059(6) 0.098(8) 0.135(10) 0.075(8) 0.008(6) 0.026(6)
C39 0.053(5) 0.085(7) 0.112(8) 0.056(6) -0.004(5) 0.011(5)
C40 0.057(5) 0.060(5) 0.080(6) 0.032(5) 0.024(4) 0.013(4)
C41 0.069(6) 0.066(6) 0.090(7) 0.035(5) 0.028(5) 0.008(5)
C42 0.048(5) 0.080(6) 0.078(6) 0.024(5) 0.019(4) 0.000(5)
C43 0.044(4) 0.073(6) 0.067(5) 0.022(5) 0.007(4) 0.011(4)
C44 0.039(4) 0.050(4) 0.059(5) 0.012(4) 0.013(4) 0.009(3)
C45 0.049(4) 0.057(5) 0.057(5) 0.013(4) 0.013(4) 0.021(4)
C46 0.056(5) 0.088(7) 0.084(6) 0.037(6) 0.014(5) 0.040(5)
C47 0.082(7) 0.091(7) 0.094(7) 0.039(6) 0.016(6) 0.057(6)
C48 0.074(6) 0.066(6) 0.083(6) 0.038(5) 0.009(5) 0.028(5)
C49 0.059(5) 0.043(4) 0.059(5) 0.019(4) 0.014(4) 0.023(4)
C50 0.054(4) 0.039(4) 0.054(4) 0.018(3) 0.011(4) 0.010(3)
C51 0.076(6) 0.053(5) 0.064(5) 0.025(4) 0.019(5) 0.016(4)
C52 0.088(7) 0.066(6) 0.085(7) 0.036(5) 0.038(6) 0.005(5)
C53 0.055(5) 0.071(6) 0.092(7) 0.033(5) 0.034(5) 0.011(5)
C54 0.051(5) 0.057(5) 0.066(5) 0.020(4) 0.016(4) 0.021(4)
Cl1 0.090(2) 0.102(2) 0.223(4) 0.089(3) 0.042(2) 0.0488(18)
O1 0.135(8) 0.164(8) 0.319(13) 0.148(8) 0.076(8) 0.047(6)
O2 0.157(9) 0.175(9) 0.317(13) 0.077(8) 0.101(8) 0.091(7)
O3 0.196(10) 0.133(7) 0.246(10) 0.063(6) -0.018(8) 0.066(6)
O4 0.238(11) 0.124(7) 0.229(10) 0.089(7) -0.019(8) 0.065(7)
Cl2 0.093(2) 0.219(5) 0.342(7) 0.226(5) 0.056(3) 0.071(3)
O5 0.127(7) 0.216(11) 0.502(16) 0.197(12) 0.044(10) 0.056(7)
O6 0.146(8) 0.252(12) 0.401(14) 0.116(12) 0.037(11) 0.090(9)
O7 0.255(12) 0.346(14) 0.329(11) 0.221(10) 0.035(10) 0.131(11)
O8 0.240(12) 0.235(10) 0.347(13) 0.226(11) 0.034(11) 0.043(8)
O 0.085(16) 0.84(8) 0.28(3) 0.43(4) 0.044(16) 0.09(2)
C 0.077(19) 0.86(9) 0.28(3) 0.38(5) 0.08(2) 0.06(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'
Cl Cl 0.1484 0.1585 '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'
S S 0.1246 0.1234 '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'
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'
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 Ru N5 79.5(3) . . ?
N4 Ru N1 101.8(3) . . ?
N5 Ru N1 92.1(2) . . ?
N4 Ru N3 78.7(3) . . ?
N5 Ru N3 158.2(3) . . ?
N1 Ru N3 92.3(2) . . ?
N4 Ru N2 176.2(2) . . ?
N5 Ru N2 96.7(2) . . ?
N1 Ru N2 77.6(3) . . ?
N3 Ru N2 105.1(3) . . ?
N4 Ru Cl 87.03(18) . . ?
N5 Ru Cl 90.40(17) . . ?
N1 Ru Cl 171.1(2) . . ?
N3 Ru Cl 88.48(17) . . ?
N2 Ru Cl 93.56(19) . . ?
C7 S C1 90.0(4) . . ?
C7 N1 C6 111.6(7) . . ?
C7 N1 Ru 114.2(5) . . ?
C6 N1 Ru 134.2(6) . . ?
C8 N2 C12 117.8(7) . . ?
C8 N2 Ru 115.0(5) . . ?
C12 N2 Ru 127.1(6) . . ?
C13 N3 C17 121.2(8) . . ?
C13 N3 Ru 126.1(7) . . ?
C17 N3 Ru 112.7(5) . . ?
C18 N4 C22 121.6(7) . . ?
C18 N4 Ru 119.7(6) . . ?
C22 N4 Ru 118.6(5) . . ?
C27 N5 C23 117.6(6) . . ?
C27 N5 Ru 128.4(5) . . ?
C23 N5 Ru 114.0(5) . . ?
C2 C1 C6 120.4(10) . . ?
C2 C1 S 129.4(8) . . ?
C6 C1 S 110.2(6) . . ?
C3 C2 C1 118.9(10) . . ?
C3 C2 H2 120.5 . . ?
C1 C2 H2 120.5 . . ?
C2 C3 C4 121.5(10) . . ?
C2 C3 H3 119.3 . . ?
C4 C3 H3 119.3 . . ?
C3 C4 C5 122.0(10) . . ?
C3 C4 H4 119.0 . . ?
C5 C4 H4 119.0 . . ?
C4 C5 C6 117.7(9) . . ?
C4 C5 H5 121.1 . . ?
C6 C5 H5 121.1 . . ?
C5 C6 N1 127.1(8) . . ?
C5 C6 C1 119.4(8) . . ?
N1 C6 C1 113.5(8) . . ?
N1 C7 C8 118.5(7) . . ?
N1 C7 S 114.6(6) . . ?
C8 C7 S 126.8(6) . . ?
N2 C8 C9 122.9(8) . . ?
N2 C8 C7 114.4(7) . . ?
C9 C8 C7 122.7(8) . . ?
C10 C9 C8 117.3(9) . . ?
C10 C9 H9 121.3 . . ?
C8 C9 H9 121.3 . . ?
C11 C10 C9 119.4(9) . . ?
C11 C10 H10 120.3 . . ?
C9 C10 H10 120.3 . . ?
C10 C11 C12 119.2(9) . . ?
C10 C11 H11 120.4 . . ?
C12 C11 H11 120.4 . . ?
N2 C12 C11 123.3(8) . . ?
N2 C12 H12 118.3 . . ?
C11 C12 H12 118.3 . . ?
N3 C13 C14 120.6(11) . . ?
N3 C13 H13 119.7 . . ?
C14 C13 H13 119.7 . . ?
C15 C14 C13 119.2(10) . . ?
C15 C14 H14 120.4 . . ?
C13 C14 H14 120.4 . . ?
C14 C15 C16 120.0(10) . . ?
C14 C15 H15 120.0 . . ?
C16 C15 H15 120.0 . . ?
C17 C16 C15 119.3(11) . . ?
C17 C16 H16 120.3 . . ?
C15 C16 H16 120.3 . . ?
N3 C17 C16 119.7(9) . . ?
N3 C17 C18 116.4(7) . . ?
C16 C17 C18 123.9(9) . . ?
N4 C18 C19 118.2(8) . . ?
N4 C18 C17 112.5(7) . . ?
C19 C18 C17 129.3(8) . . ?
C20 C19 C18 119.9(9) . . ?
C20 C19 H19 120.1 . . ?
C18 C19 H19 120.1 . . ?
C19 C20 C21 121.0(9) . . ?
C19 C20 H20 119.5 . . ?
C21 C20 H20 119.5 . . ?
C20 C21 C22 120.1(9) . . ?
C20 C21 H21 120.0 . . ?
C22 C21 H21 120.0 . . ?
N4 C22 C21 119.2(8) . . ?
N4 C22 C23 112.9(7) . . ?
C21 C22 C23 127.9(8) . . ?
N5 C23 C24 121.3(7) . . ?
N5 C23 C22 115.0(7) . . ?
C24 C23 C22 123.7(8) . . ?
C25 C24 C23 119.7(8) . . ?
C25 C24 H24 120.1 . . ?
C23 C24 H24 120.1 . . ?
C24 C25 C26 119.9(8) . . ?
C24 C25 H25 120.1 . . ?
C26 C25 H25 120.1 . . ?
C27 C26 C25 118.3(8) . . ?
C27 C26 H26 120.9 . . ?
C25 C26 H26 120.9 . . ?
N5 C27 C26 123.2(8) . . ?
N5 C27 H27 118.4 . . ?
C26 C27 H27 118.4 . . ?
N9 Ru' N6 101.4(3) . . ?
N9 Ru' N10 79.3(2) . . ?
N6 Ru' N10 94.0(2) . . ?
N9 Ru' N8 79.7(2) . . ?
N6 Ru' N8 91.3(2) . . ?
N10 Ru' N8 159.0(2) . . ?
N9 Ru' N7 177.1(2) . . ?
N6 Ru' N7 77.8(3) . . ?
N10 Ru' N7 103.6(2) . . ?
N8 Ru' N7 97.4(2) . . ?
N9 Ru' Cl' 88.62(18) . . ?
N6 Ru' Cl' 169.9(2) . . ?
N10 Ru' Cl' 86.86(17) . . ?
N8 Ru' Cl' 91.38(18) . . ?
N7 Ru' Cl' 92.2(2) . . ?
C34 S' C28 89.9(4) . . ?
C34 N6 C33 110.2(7) . . ?
C34 N6 Ru' 114.1(6) . . ?
C33 N6 Ru' 135.7(6) . . ?
C35 N7 C39 115.9(8) . . ?
C35 N7 Ru' 116.1(6) . . ?
C39 N7 Ru' 127.7(6) . . ?
C40 N8 C44 117.8(7) . . ?
C40 N8 Ru' 128.9(6) . . ?
C44 N8 Ru' 113.4(5) . . ?
C49 N9 C45 121.9(7) . . ?
C49 N9 Ru' 119.4(5) . . ?
C45 N9 Ru' 118.7(5) . . ?
C54 N10 C50 117.3(7) . . ?
C54 N10 Ru' 128.7(6) . . ?
C50 N10 Ru' 113.9(5) . . ?
C29 C28 C33 121.5(11) . . ?
C29 C28 S' 128.9(9) . . ?
C33 C28 S' 109.6(7) . . ?
C30 C29 C28 119.0(12) . . ?
C30 C29 H29 120.5 . . ?
C28 C29 H29 120.5 . . ?
C29 C30 C31 119.9(12) . . ?
C29 C30 H30 120.1 . . ?
C31 C30 H30 120.1 . . ?
C32 C31 C30 122.9(13) . . ?
C32 C31 H31 118.6 . . ?
C30 C31 H31 118.6 . . ?
C31 C32 C33 117.9(11) . . ?
C31 C32 H32 121.1 . . ?
C33 C32 H32 121.1 . . ?
N6 C33 C32 126.7(9) . . ?
N6 C33 C28 114.5(9) . . ?
C32 C33 C28 118.8(9) . . ?
N6 C34 C35 118.4(7) . . ?
N6 C34 S' 115.7(7) . . ?
C35 C34 S' 125.9(6) . . ?
N7 C35 C36 125.1(10) . . ?
N7 C35 C34 113.4(7) . . ?
C36 C35 C34 121.5(9) . . ?
C37 C36 C35 117.5(11) . . ?
C37 C36 H36 121.2 . . ?
C35 C36 H36 121.2 . . ?
C36 C37 C38 119.4(10) . . ?
C36 C37 H37 120.3 . . ?
C38 C37 H37 120.3 . . ?
C37 C38 C39 119.1(11) . . ?
C37 C38 H38 120.4 . . ?
C39 C38 H38 120.4 . . ?
N7 C39 C38 122.8(11) . . ?
N7 C39 H39 118.6 . . ?
C38 C39 H39 118.6 . . ?
N8 C40 C41 122.5(9) . . ?
N8 C40 H40 118.7 . . ?
C41 C40 H40 118.7 . . ?
C42 C41 C40 119.1(9) . . ?
C42 C41 H41 120.4 . . ?
C40 C41 H41 120.4 . . ?
C43 C42 C41 119.2(8) . . ?
C43 C42 H42 120.4 . . ?
C41 C42 H42 120.4 . . ?
C42 C43 C44 120.1(9) . . ?
C42 C43 H43 119.9 . . ?
C44 C43 H43 119.9 . . ?
N8 C44 C43 121.2(8) . . ?
N8 C44 C45 115.1(6) . . ?
C43 C44 C45 123.7(8) . . ?
N9 C45 C46 119.6(8) . . ?
N9 C45 C44 113.1(7) . . ?
C46 C45 C44 127.3(8) . . ?
C47 C46 C45 118.6(8) . . ?
C47 C46 H46 120.7 . . ?
C45 C46 H46 120.7 . . ?
C48 C47 C46 121.1(9) . . ?
C48 C47 H47 119.5 . . ?
C46 C47 H47 119.5 . . ?
C47 C48 C49 119.0(9) . . ?
C47 C48 H48 120.5 . . ?
C49 C48 H48 120.5 . . ?
N9 C49 C48 119.8(8) . . ?
N9 C49 C50 113.1(6) . . ?
C48 C49 C50 127.1(8) . . ?
C51 C50 N10 120.5(7) . . ?
C51 C50 C49 125.2(7) . . ?
N10 C50 C49 114.3(6) . . ?
C52 C51 C50 120.4(9) . . ?
C52 C51 H51 119.8 . . ?
C50 C51 H51 119.8 . . ?
C53 C52 C51 119.7(9) . . ?
C53 C52 H52 120.2 . . ?
C51 C52 H52 120.2 . . ?
C52 C53 C54 119.4(9) . . ?
C52 C53 H53 120.3 . . ?
C54 C53 H53 120.3 . . ?
N10 C54 C53 122.6(8) . . ?
N10 C54 H54 118.7 . . ?
C53 C54 H54 118.7 . . ?
O2 Cl1 O4 122.9(11) . . ?
O2 Cl1 O1 110.7(9) . . ?
O4 Cl1 O1 109.0(9) . . ?
O2 Cl1 O3 106.5(9) . . ?
O4 Cl1 O3 104.6(7) . . ?
O1 Cl1 O3 100.5(9) . . ?
O8 Cl2 O5 130.1(11) . . ?
O8 Cl2 O6 106.5(12) . . ?
O5 Cl2 O6 99.3(11) . . ?
O8 Cl2 O7 105.8(12) . . ?
O5 Cl2 O7 118.6(12) . . ?
O6 Cl2 O7 84.8(10) . . ?
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
Ru N4 1.953(6) . ?
Ru N5 2.057(5) . ?
Ru N1 2.066(6) . ?
Ru N3 2.082(6) . ?
Ru N2 2.108(6) . ?
Ru Cl 2.394(2) . ?
S C7 1.717(8) . ?
S C1 1.719(10) . ?
N1 C7 1.323(10) . ?
N1 C6 1.385(10) . ?
N2 C8 1.324(10) . ?
N2 C12 1.332(10) . ?
N3 C13 1.331(11) . ?
N3 C17 1.369(10) . ?
N4 C18 1.360(9) . ?
N4 C22 1.362(10) . ?
N5 C27 1.347(9) . ?
N5 C23 1.360(9) . ?
C1 C2 1.375(13) . ?
C1 C6 1.401(12) . ?
C2 C3 1.334(15) . ?
C2 H2 0.9300 . ?
C3 C4 1.353(14) . ?
C3 H3 0.9300 . ?
C4 C5 1.370(11) . ?
C4 H4 0.9300 . ?
C5 C6 1.381(12) . ?
C5 H5 0.9300 . ?
C7 C8 1.437(11) . ?
C8 C9 1.399(12) . ?
C9 C10 1.393(14) . ?
C9 H9 0.9300 . ?
C10 C11 1.355(14) . ?
C10 H10 0.9300 . ?
C11 C12 1.366(12) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C14 1.404(13) . ?
C13 H13 0.9300 . ?
C14 C15 1.364(16) . ?
C14 H14 0.9300 . ?
C15 C16 1.395(15) . ?
C15 H15 0.9300 . ?
C16 C17 1.385(11) . ?
C16 H16 0.9300 . ?
C17 C18 1.431(12) . ?
C18 C19 1.406(13) . ?
C19 C20 1.349(14) . ?
C19 H19 0.9300 . ?
C20 C21 1.353(13) . ?
C20 H20 0.9300 . ?
C21 C22 1.379(12) . ?
C21 H21 0.9300 . ?
C22 C23 1.461(11) . ?
C23 C24 1.378(11) . ?
C24 C25 1.355(12) . ?
C24 H24 0.9300 . ?
C25 C26 1.379(13) . ?
C25 H25 0.9300 . ?
C26 C27 1.367(11) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
Ru' N9 1.960(6) . ?
Ru' N6 2.045(7) . ?
Ru' N10 2.058(6) . ?
Ru' N8 2.063(6) . ?
Ru' N7 2.112(7) . ?
Ru' Cl' 2.374(2) . ?
S' C34 1.704(9) . ?
S' C28 1.732(11) . ?
N6 C34 1.348(10) . ?
N6 C33 1.376(11) . ?
N7 C35 1.309(11) . ?
N7 C39 1.362(11) . ?
N8 C40 1.320(10) . ?
N8 C44 1.369(10) . ?
N9 C49 1.350(9) . ?
N9 C45 1.351(9) . ?
N10 C54 1.347(9) . ?
N10 C50 1.385(9) . ?
C28 C29 1.364(15) . ?
C28 C33 1.411(12) . ?
C29 C30 1.342(17) . ?
C29 H29 0.9300 . ?
C30 C31 1.398(17) . ?
C30 H30 0.9300 . ?
C31 C32 1.340(14) . ?
C31 H31 0.9300 . ?
C32 C33 1.396(13) . ?
C32 H32 0.9300 . ?
C34 C35 1.451(13) . ?
C35 C36 1.390(12) . ?
C36 C37 1.364(15) . ?
C36 H36 0.9300 . ?
C37 C38 1.365(16) . ?
C37 H37 0.9300 . ?
C38 C39 1.373(13) . ?
C38 H38 0.9300 . ?
C39 H39 0.9300 . ?
C40 C41 1.382(12) . ?
C40 H40 0.9300 . ?
C41 C42 1.373(14) . ?
C41 H41 0.9300 . ?
C42 C43 1.338(13) . ?
C42 H42 0.9300 . ?
C43 C44 1.381(11) . ?
C43 H43 0.9300 . ?
C44 C45 1.470(11) . ?
C45 C46 1.383(11) . ?
C46 C47 1.377(13) . ?
C46 H46 0.9300 . ?
C47 C48 1.370(13) . ?
C47 H47 0.9300 . ?
C48 C49 1.372(11) . ?
C48 H48 0.9300 . ?
C49 C50 1.463(10) . ?
C50 C51 1.364(11) . ?
C51 C52 1.357(13) . ?
C51 H51 0.9300 . ?
C52 C53 1.355(14) . ?
C52 H52 0.9300 . ?
C53 C54 1.364(12) . ?
C53 H53 0.9300 . ?
C54 H54 0.9300 . ?
Cl1 O2 1.318(11) . ?
Cl1 O4 1.349(11) . ?
Cl1 O1 1.357(11) . ?
Cl1 O3 1.475(13) . ?
Cl2 O8 1.245(12) . ?
Cl2 O5 1.280(14) . ?
Cl2 O6 1.392(17) . ?
Cl2 O7 1.536(19) . ?
O C 1.49(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
N4 Ru N1 C7 -172.2(5) . . . . ?
N5 Ru N1 C7 -92.5(6) . . . . ?
N3 Ru N1 C7 108.9(6) . . . . ?
N2 Ru N1 C7 3.9(5) . . . . ?
Cl Ru N1 C7 13.8(15) . . . . ?
N4 Ru N1 C6 5.4(7) . . . . ?
N5 Ru N1 C6 85.1(7) . . . . ?
N3 Ru N1 C6 -73.6(7) . . . . ?
N2 Ru N1 C6 -178.5(7) . . . . ?
Cl Ru N1 C6 -168.6(8) . . . . ?
N4 Ru N2 C8 80(4) . . . . ?
N5 Ru N2 C8 88.4(6) . . . . ?
N1 Ru N2 C8 -2.3(6) . . . . ?
N3 Ru N2 C8 -91.4(6) . . . . ?
Cl Ru N2 C8 179.2(5) . . . . ?
N4 Ru N2 C12 -96(4) . . . . ?
N5 Ru N2 C12 -88.3(7) . . . . ?
N1 Ru N2 C12 -179.0(7) . . . . ?
N3 Ru N2 C12 91.9(7) . . . . ?
Cl Ru N2 C12 2.5(6) . . . . ?
N4 Ru N3 C13 -177.8(7) . . . . ?
N5 Ru N3 C13 -177.8(6) . . . . ?
N1 Ru N3 C13 -76.2(7) . . . . ?
N2 Ru N3 C13 1.6(7) . . . . ?
Cl Ru N3 C13 94.9(6) . . . . ?
N4 Ru N3 C17 1.3(5) . . . . ?
N5 Ru N3 C17 1.3(9) . . . . ?
N1 Ru N3 C17 102.9(5) . . . . ?
N2 Ru N3 C17 -179.3(5) . . . . ?
Cl Ru N3 C17 -86.0(5) . . . . ?
N5 Ru N4 C18 177.2(6) . . . . ?
N1 Ru N4 C18 -92.9(6) . . . . ?
N3 Ru N4 C18 -2.8(5) . . . . ?
N2 Ru N4 C18 -175(4) . . . . ?
Cl Ru N4 C18 86.2(5) . . . . ?
N5 Ru N4 C22 0.4(5) . . . . ?
N1 Ru N4 C22 90.4(6) . . . . ?
N3 Ru N4 C22 -179.6(6) . . . . ?
N2 Ru N4 C22 9(4) . . . . ?
Cl Ru N4 C22 -90.6(5) . . . . ?
N4 Ru N5 C27 179.8(7) . . . . ?
N1 Ru N5 C27 78.1(6) . . . . ?
N3 Ru N5 C27 179.8(6) . . . . ?
N2 Ru N5 C27 0.3(7) . . . . ?
Cl Ru N5 C27 -93.3(6) . . . . ?
N4 Ru N5 C23 -0.2(5) . . . . ?
N1 Ru N5 C23 -101.8(5) . . . . ?
N3 Ru N5 C23 -0.2(9) . . . . ?
N2 Ru N5 C23 -179.7(5) . . . . ?
Cl Ru N5 C23 86.7(5) . . . . ?
C7 S C1 C2 179.7(10) . . . . ?
C7 S C1 C6 -0.8(6) . . . . ?
C6 C1 C2 C3 2.0(15) . . . . ?
S C1 C2 C3 -178.5(8) . . . . ?
C1 C2 C3 C4 -2.5(17) . . . . ?
C2 C3 C4 C5 1.0(16) . . . . ?
C3 C4 C5 C6 1.1(14) . . . . ?
C4 C5 C6 N1 -179.3(8) . . . . ?
C4 C5 C6 C1 -1.5(12) . . . . ?
C7 N1 C6 C5 -178.3(8) . . . . ?
Ru N1 C6 C5 4.0(12) . . . . ?
C7 N1 C6 C1 3.8(10) . . . . ?
Ru N1 C6 C1 -173.9(5) . . . . ?
C2 C1 C6 C5 0.0(13) . . . . ?
S C1 C6 C5 -179.6(6) . . . . ?
C2 C1 C6 N1 178.1(8) . . . . ?
S C1 C6 N1 -1.5(9) . . . . ?
C6 N1 C7 C8 176.7(7) . . . . ?
Ru N1 C7 C8 -5.1(9) . . . . ?
C6 N1 C7 S -4.4(9) . . . . ?
Ru N1 C7 S 173.7(4) . . . . ?
C1 S C7 N1 3.0(7) . . . . ?
C1 S C7 C8 -178.2(8) . . . . ?
C12 N2 C8 C9 -1.9(13) . . . . ?
Ru N2 C8 C9 -178.9(7) . . . . ?
C12 N2 C8 C7 177.5(7) . . . . ?
Ru N2 C8 C7 0.4(9) . . . . ?
N1 C7 C8 N2 3.2(11) . . . . ?
S C7 C8 N2 -175.6(6) . . . . ?
N1 C7 C8 C9 -177.5(8) . . . . ?
S C7 C8 C9 3.8(13) . . . . ?
N2 C8 C9 C10 0.3(15) . . . . ?
C7 C8 C9 C10 -179.0(9) . . . . ?
C8 C9 C10 C11 0.8(17) . . . . ?
C9 C10 C11 C12 -0.3(16) . . . . ?
C8 N2 C12 C11 2.4(12) . . . . ?
Ru N2 C12 C11 179.1(7) . . . . ?
C10 C11 C12 N2 -1.4(15) . . . . ?
C17 N3 C13 C14 -0.3(12) . . . . ?
Ru N3 C13 C14 178.7(6) . . . . ?
N3 C13 C14 C15 0.4(15) . . . . ?
C13 C14 C15 C16 0.5(16) . . . . ?
C14 C15 C16 C17 -1.6(15) . . . . ?
C13 N3 C17 C16 -0.8(11) . . . . ?
Ru N3 C17 C16 -180.0(6) . . . . ?
C13 N3 C17 C18 179.4(7) . . . . ?
Ru N3 C17 C18 0.3(8) . . . . ?
C15 C16 C17 N3 1.7(13) . . . . ?
C15 C16 C17 C18 -178.5(8) . . . . ?
C22 N4 C18 C19 -2.5(11) . . . . ?
Ru N4 C18 C19 -179.2(6) . . . . ?
C22 N4 C18 C17 -179.6(7) . . . . ?
Ru N4 C18 C17 3.7(9) . . . . ?
N3 C17 C18 N4 -2.5(10) . . . . ?
C16 C17 C18 N4 177.8(7) . . . . ?
N3 C17 C18 C19 -179.2(8) . . . . ?
C16 C17 C18 C19 1.1(14) . . . . ?
N4 C18 C19 C20 -0.3(13) . . . . ?
C17 C18 C19 C20 176.2(9) . . . . ?
C18 C19 C20 C21 1.8(16) . . . . ?
C19 C20 C21 C22 -0.7(16) . . . . ?
C18 N4 C22 C21 3.7(11) . . . . ?
Ru N4 C22 C21 -179.6(6) . . . . ?
C18 N4 C22 C23 -177.2(6) . . . . ?
Ru N4 C22 C23 -0.5(8) . . . . ?
C20 C21 C22 N4 -2.1(13) . . . . ?
C20 C21 C22 C23 179.0(9) . . . . ?
C27 N5 C23 C24 0.2(10) . . . . ?
Ru N5 C23 C24 -179.8(6) . . . . ?
C27 N5 C23 C22 -180.0(6) . . . . ?
Ru N5 C23 C22 0.0(8) . . . . ?
N4 C22 C23 N5 0.3(9) . . . . ?
C21 C22 C23 N5 179.3(8) . . . . ?
N4 C22 C23 C24 -179.9(7) . . . . ?
C21 C22 C23 C24 -0.8(13) . . . . ?
N5 C23 C24 C25 1.2(12) . . . . ?
C22 C23 C24 C25 -178.6(7) . . . . ?
C23 C24 C25 C26 -1.5(13) . . . . ?
C24 C25 C26 C27 0.5(13) . . . . ?
C23 N5 C27 C26 -1.4(11) . . . . ?
Ru N5 C27 C26 178.7(6) . . . . ?
C25 C26 C27 N5 1.0(12) . . . . ?
N9 Ru' N6 C34 -174.1(5) . . . . ?
N10 Ru' N6 C34 106.0(6) . . . . ?
N8 Ru' N6 C34 -94.3(6) . . . . ?
N7 Ru' N6 C34 3.0(5) . . . . ?
Cl' Ru' N6 C34 11.2(14) . . . . ?
N9 Ru' N6 C33 3.7(8) . . . . ?
N10 Ru' N6 C33 -76.2(7) . . . . ?
N8 Ru' N6 C33 83.5(7) . . . . ?
N7 Ru' N6 C33 -179.2(8) . . . . ?
Cl' Ru' N6 C33 -171.0(7) . . . . ?
N9 Ru' N7 C35 73(5) . . . . ?
N6 Ru' N7 C35 -2.3(6) . . . . ?
N10 Ru' N7 C35 -93.5(6) . . . . ?
N8 Ru' N7 C35 87.5(6) . . . . ?
Cl' Ru' N7 C35 179.2(5) . . . . ?
N9 Ru' N7 C39 -102(5) . . . . ?
N6 Ru' N7 C39 -176.9(7) . . . . ?
N10 Ru' N7 C39 91.9(7) . . . . ?
N8 Ru' N7 C39 -87.1(7) . . . . ?
Cl' Ru' N7 C39 4.6(7) . . . . ?
N9 Ru' N8 C40 -179.5(7) . . . . ?
N6 Ru' N8 C40 79.2(7) . . . . ?
N10 Ru' N8 C40 -175.9(7) . . . . ?
N7 Ru' N8 C40 1.3(7) . . . . ?
Cl' Ru' N8 C40 -91.1(7) . . . . ?
N9 Ru' N8 C44 0.0(5) . . . . ?
N6 Ru' N8 C44 -101.3(5) . . . . ?
N10 Ru' N8 C44 3.5(10) . . . . ?
N7 Ru' N8 C44 -179.2(5) . . . . ?
Cl' Ru' N8 C44 88.4(5) . . . . ?
N6 Ru' N9 C49 -93.1(6) . . . . ?
N10 Ru' N9 C49 -1.1(5) . . . . ?
N8 Ru' N9 C49 177.6(6) . . . . ?
N7 Ru' N9 C49 -168(5) . . . . ?
Cl' Ru' N9 C49 86.0(5) . . . . ?
N6 Ru' N9 C45 89.1(6) . . . . ?
N10 Ru' N9 C45 -178.9(6) . . . . ?
N8 Ru' N9 C45 -0.2(5) . . . . ?
N7 Ru' N9 C45 14(5) . . . . ?
Cl' Ru' N9 C45 -91.8(5) . . . . ?
N9 Ru' N10 C54 179.0(7) . . . . ?
N6 Ru' N10 C54 -80.1(7) . . . . ?
N8 Ru' N10 C54 175.5(7) . . . . ?
N7 Ru' N10 C54 -1.7(7) . . . . ?
Cl' Ru' N10 C54 89.8(6) . . . . ?
N9 Ru' N10 C50 -0.4(5) . . . . ?
N6 Ru' N10 C50 100.4(5) . . . . ?
N8 Ru' N10 C50 -4.0(10) . . . . ?
N7 Ru' N10 C50 178.9(5) . . . . ?
Cl' Ru' N10 C50 -89.6(5) . . . . ?
C34 S' C28 C29 179.7(11) . . . . ?
C34 S' C28 C33 -1.4(7) . . . . ?
C33 C28 C29 C30 0.2(18) . . . . ?
S' C28 C29 C30 179.0(10) . . . . ?
C28 C29 C30 C31 2(2) . . . . ?
C29 C30 C31 C32 -4(2) . . . . ?
C30 C31 C32 C33 4.0(19) . . . . ?
C34 N6 C33 C32 -178.4(9) . . . . ?
Ru' N6 C33 C32 3.7(13) . . . . ?
C34 N6 C33 C28 2.2(10) . . . . ?
Ru' N6 C33 C28 -175.7(6) . . . . ?
C31 C32 C33 N6 179.1(10) . . . . ?
C31 C32 C33 C28 -1.5(15) . . . . ?
C29 C28 C33 N6 178.9(9) . . . . ?
S' C28 C33 N6 -0.1(10) . . . . ?
C29 C28 C33 C32 -0.6(15) . . . . ?
S' C28 C33 C32 -179.6(7) . . . . ?
C33 N6 C34 C35 178.2(7) . . . . ?
Ru' N6 C34 C35 -3.5(9) . . . . ?
C33 N6 C34 S' -3.4(9) . . . . ?
Ru' N6 C34 S' 175.0(4) . . . . ?
C28 S' C34 N6 2.8(7) . . . . ?
C28 S' C34 C35 -178.8(8) . . . . ?
C39 N7 C35 C36 -2.1(12) . . . . ?
Ru' N7 C35 C36 -177.4(7) . . . . ?
C39 N7 C35 C34 176.4(7) . . . . ?
Ru' N7 C35 C34 1.1(9) . . . . ?
N6 C34 C35 N7 1.5(11) . . . . ?
S' C34 C35 N7 -176.8(6) . . . . ?
N6 C34 C35 C36 -179.9(8) . . . . ?
S' C34 C35 C36 1.8(12) . . . . ?
N7 C35 C36 C37 -0.7(14) . . . . ?
C34 C35 C36 C37 -179.1(8) . . . . ?
C35 C36 C37 C38 2.9(15) . . . . ?
C36 C37 C38 C39 -2.2(16) . . . . ?
C35 N7 C39 C38 2.9(13) . . . . ?
Ru' N7 C39 C38 177.5(7) . . . . ?
C37 C38 C39 N7 -0.8(16) . . . . ?
C44 N8 C40 C41 -0.6(12) . . . . ?
Ru' N8 C40 C41 178.8(7) . . . . ?
N8 C40 C41 C42 -0.4(14) . . . . ?
C40 C41 C42 C43 1.4(14) . . . . ?
C41 C42 C43 C44 -1.3(14) . . . . ?
C40 N8 C44 C43 0.7(11) . . . . ?
Ru' N8 C44 C43 -178.9(6) . . . . ?
C40 N8 C44 C45 179.7(7) . . . . ?
Ru' N8 C44 C45 0.1(8) . . . . ?
C42 C43 C44 N8 0.3(12) . . . . ?
C42 C43 C44 C45 -178.6(8) . . . . ?
C49 N9 C45 C46 1.6(11) . . . . ?
Ru' N9 C45 C46 179.3(6) . . . . ?
C49 N9 C45 C44 -177.4(6) . . . . ?
Ru' N9 C45 C44 0.3(8) . . . . ?
N8 C44 C45 N9 -0.3(10) . . . . ?
C43 C44 C45 N9 178.7(7) . . . . ?
N8 C44 C45 C46 -179.2(8) . . . . ?
C43 C44 C45 C46 -0.2(13) . . . . ?
N9 C45 C46 C47 -1.8(13) . . . . ?
C44 C45 C46 C47 177.0(8) . . . . ?
C45 C46 C47 C48 0.3(15) . . . . ?
C46 C47 C48 C49 1.4(15) . . . . ?
C45 N9 C49 C48 0.2(11) . . . . ?
Ru' N9 C49 C48 -177.5(6) . . . . ?
C45 N9 C49 C50 -179.9(6) . . . . ?
Ru' N9 C49 C50 2.4(9) . . . . ?
C47 C48 C49 N9 -1.7(13) . . . . ?
C47 C48 C49 C50 178.5(8) . . . . ?
C54 N10 C50 C51 2.0(10) . . . . ?
Ru' N10 C50 C51 -178.5(6) . . . . ?
C54 N10 C50 C49 -177.7(6) . . . . ?
Ru' N10 C50 C49 1.8(8) . . . . ?
N9 C49 C50 C51 177.6(7) . . . . ?
C48 C49 C50 C51 -2.5(13) . . . . ?
N9 C49 C50 N10 -2.6(9) . . . . ?
C48 C49 C50 N10 177.2(8) . . . . ?
N10 C50 C51 C52 -1.9(12) . . . . ?
C49 C50 C51 C52 177.8(8) . . . . ?
C50 C51 C52 C53 -0.1(14) . . . . ?
C51 C52 C53 C54 1.9(15) . . . . ?
C50 N10 C54 C53 -0.2(12) . . . . ?
Ru' N10 C54 C53 -179.6(6) . . . . ?
C52 C53 C54 N10 -1.8(14) . . . . ?
|
1100946.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100946.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_1100946
loop_
_publ_author_name
'Rajesh Koner'
'Hsin-Huang Lin'
'Ho-Hsiang Wei'
'Sasankasekhar Mohanta'
_publ_section_title
;
Syntheses, Structures, and Magnetic Properties of Diphenoxo-Bridged
MIILnIII Complexes Derived from N,N'-Ethylenebis(3-ethoxysalicylaldiimine)
(M = Cu or Ni; Ln = Ce-Yb): Observation of Surprisingly Strong Exchange
Interactions
;
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3524
_journal_page_last 3536
_journal_paper_doi 10.1021/ic048196h
_journal_volume 44
_journal_year 2005
_chemical_formula_sum 'C20 H22 Ce Cu N5 O13'
_chemical_formula_weight 744.09
_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 8.697(6)
_cell_length_b 13.905(6)
_cell_length_c 21.176(8)
_cell_measurement_temperature 293(2)
_cell_volume 2561(2)
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 293(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 0.0000
_diffrn_reflns_av_sigmaI/netI 0.0570
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -1
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min -1
_diffrn_reflns_limit_l_max 25
_diffrn_reflns_limit_l_min -1
_diffrn_reflns_number 2575
_diffrn_reflns_theta_full 25.00
_diffrn_reflns_theta_max 25.00
_diffrn_reflns_theta_min 1.75
_exptl_absorpt_coefficient_mu 2.662
_exptl_crystal_colour Red
_exptl_crystal_density_diffrn 1.930
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1472
_exptl_crystal_size_max 58
_exptl_crystal_size_mid 36
_exptl_crystal_size_min 20
_refine_diff_density_max 0.568
_refine_diff_density_min -0.801
_refine_diff_density_rms 0.121
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack 0.03(4)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.108
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 361
_refine_ls_number_reflns 2575
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.108
_refine_ls_R_factor_all 0.0568
_refine_ls_R_factor_gt 0.0347
_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^)+(0.0157P)^2^+5.4164P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0731
_refine_ls_wR_factor_ref 0.0889
_reflns_number_gt 2059
_reflns_number_total 2575
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file ic048196hsi20050224_082436_01.cif
_cod_data_source_block cuce
_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 1100946
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
Ce Ce 1.74099(6) 0.49939(5) 0.09408(2) 0.02818(13) Uani 1 1 d . . .
Cu Cu 2.06776(15) 0.44371(9) 0.18283(7) 0.0344(3) Uani 1 1 d . . .
N1 N 2.2012(9) 0.5131(7) 0.2389(4) 0.037(2) Uani 1 1 d . . .
O1 O 1.9626(8) 0.5565(5) 0.1537(3) 0.0331(16) Uani 1 1 d . . .
C15 C 1.7935(12) 0.2427(7) 0.0899(5) 0.033(2) Uani 1 1 d . . .
O2 O 1.9163(9) 0.3747(5) 0.1366(4) 0.0383(18) Uani 1 1 d . . .
C1 C 2.0225(12) 0.6451(7) 0.1550(5) 0.034(2) Uani 1 1 d . . .
O4 O 1.6895(8) 0.3118(5) 0.0688(4) 0.0382(19) Uani 1 1 d . . .
N2 N 2.1801(11) 0.3319(7) 0.2094(5) 0.035(2) Uani 1 1 d . . .
C10 C 2.1522(14) 0.2458(8) 0.1921(6) 0.039(3) Uani 1 1 d . . .
H10A H 2.2177 0.1980 0.2070 0.046 Uiso 1 1 calc R . .
C9 C 2.3158(14) 0.3555(9) 0.2499(6) 0.043(3) Uani 1 1 d . . .
H9B H 2.3351 0.3039 0.2797 0.051 Uiso 1 1 calc R . .
H9A H 2.4068 0.3642 0.2241 0.051 Uiso 1 1 calc R . .
C13 C 1.9008(15) 0.0821(7) 0.0977(6) 0.055(3) Uani 1 1 d . . .
H13A H 1.8972 0.0171 0.0875 0.065 Uiso 1 1 calc R . .
C6 C 2.1437(14) 0.6706(8) 0.1967(6) 0.035(3) Uani 1 1 d . . .
C12 C 2.0153(15) 0.1166(7) 0.1337(6) 0.048(3) Uani 1 1 d . . .
H12A H 2.0905 0.0743 0.1480 0.058 Uiso 1 1 calc R . .
C11 C 2.0260(13) 0.2157(8) 0.1507(6) 0.037(3) Uani 1 1 d . . .
C5 C 2.1996(15) 0.7678(8) 0.1941(6) 0.045(3) Uani 1 1 d . . .
H5A H 2.2785 0.7869 0.2210 0.054 Uiso 1 1 calc R . .
C7 C 2.2206(13) 0.6059(8) 0.2392(5) 0.041(3) Uani 1 1 d . . .
H7A H 2.2882 0.6319 0.2687 0.049 Uiso 1 1 calc R . .
C16 C 1.9138(13) 0.2795(7) 0.1270(5) 0.033(3) Uani 1 1 d . . .
O10 O 1.7326(9) 0.5145(6) -0.0258(3) 0.051(2) Uani 1 1 d . . .
O8 O 1.9289(12) 0.5029(7) -0.0886(4) 0.070(2) Uani 1 1 d . . .
N4 N 1.8730(11) 0.4945(9) -0.0370(4) 0.046(2) Uani 1 1 d . . .
O13 O 1.6338(10) 0.6135(6) 0.1794(4) 0.048(2) Uani 1 1 d . . .
O12 O 1.6759(11) 0.4688(6) 0.2129(4) 0.052(3) Uani 1 1 d . . .
O3 O 1.8467(8) 0.6762(5) 0.0745(3) 0.0345(18) Uani 1 1 d . . .
O9 O 1.9528(9) 0.4687(6) 0.0103(4) 0.053(2) Uani 1 1 d . . .
O7 O 1.4930(10) 0.5831(7) 0.0487(5) 0.067(3) Uani 1 1 d . . .
O5 O 1.2581(10) 0.5403(9) 0.0726(5) 0.090(4) Uani 1 1 d . . .
N5 N 1.6347(12) 0.5553(9) 0.2241(6) 0.055(3) Uani 1 1 d . . .
C19 C 1.5519(13) 0.2799(8) 0.0355(5) 0.042(3) Uani 1 1 d . . .
H19B H 1.5804 0.2315 0.0047 0.051 Uiso 1 1 calc R . .
H19A H 1.5079 0.3339 0.0129 0.051 Uiso 1 1 calc R . .
O6 O 1.4521(10) 0.4626(6) 0.1113(4) 0.054(2) Uani 1 1 d . . .
O11 O 1.5946(12) 0.5752(8) 0.2779(4) 0.083(4) Uani 1 1 d . . .
C14 C 1.7847(14) 0.1462(8) 0.0754(5) 0.040(3) Uani 1 1 d . . .
H14A H 1.7035 0.1230 0.0513 0.048 Uiso 1 1 calc R . .
C8 C 2.2780(13) 0.4464(8) 0.2842(5) 0.044(3) Uani 1 1 d . . .
H8B H 2.2102 0.4328 0.3194 0.052 Uiso 1 1 calc R . .
H8A H 2.3712 0.4756 0.3005 0.052 Uiso 1 1 calc R . .
C17 C 1.7734(15) 0.7405(7) 0.0284(5) 0.047(3) Uani 1 1 d . . .
H17B H 1.7231 0.7022 -0.0039 0.056 Uiso 1 1 calc R . .
H17A H 1.8518 0.7791 0.0079 0.056 Uiso 1 1 calc R . .
N3 N 1.3963(12) 0.5274(8) 0.0767(5) 0.050(3) Uani 1 1 d . . .
C20 C 1.4345(15) 0.2394(10) 0.0783(7) 0.061(4) Uani 1 1 d . . .
H20A H 1.3466 0.2196 0.0542 0.092 Uiso 1 1 calc R . .
H20C H 1.4041 0.2874 0.1084 0.092 Uiso 1 1 calc R . .
H20B H 1.4766 0.1850 0.1002 0.092 Uiso 1 1 calc R . .
C4 C 2.1388(15) 0.8319(8) 0.1529(6) 0.052(3) Uani 1 1 d . . .
H4A H 2.1757 0.8946 0.1518 0.063 Uiso 1 1 calc R . .
C2 C 1.9643(12) 0.7134(7) 0.1135(5) 0.030(3) Uani 1 1 d . . .
C3 C 2.0206(13) 0.8041(8) 0.1120(6) 0.042(3) Uani 1 1 d . . .
H3A H 1.9804 0.8484 0.0835 0.051 Uiso 1 1 calc R . .
C18 C 1.6574(16) 0.8057(8) 0.0585(6) 0.056(4) Uani 1 1 d . . .
H18A H 1.6125 0.8464 0.0269 0.084 Uiso 1 1 calc R . .
H18C H 1.7071 0.8447 0.0899 0.084 Uiso 1 1 calc R . .
H18B H 1.5784 0.7678 0.0781 0.084 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
Ce 0.0272(2) 0.0235(2) 0.0339(2) 0.0023(3) -0.0037(3) 0.0012(4)
Cu 0.0329(7) 0.0253(6) 0.0450(7) 0.0043(6) -0.0096(7) 0.0006(6)
N1 0.029(4) 0.045(6) 0.037(4) 0.005(5) -0.009(3) -0.002(5)
O1 0.032(4) 0.021(3) 0.045(4) 0.002(4) -0.011(4) -0.004(3)
C15 0.037(6) 0.025(5) 0.036(6) 0.000(5) -0.002(5) 0.001(4)
O2 0.034(4) 0.027(3) 0.054(5) -0.005(3) -0.009(4) -0.001(4)
C1 0.033(6) 0.020(5) 0.048(6) 0.004(5) 0.004(6) -0.001(4)
O4 0.034(4) 0.031(4) 0.049(5) 0.001(3) -0.013(4) -0.002(3)
N2 0.023(5) 0.044(6) 0.038(6) 0.015(5) -0.003(4) 0.009(4)
C10 0.037(7) 0.032(6) 0.047(8) 0.011(5) -0.001(6) 0.010(5)
C9 0.038(6) 0.051(7) 0.038(6) 0.011(6) -0.011(6) 0.006(6)
C13 0.069(9) 0.026(6) 0.069(8) 0.004(6) 0.002(8) 0.008(6)
C6 0.030(6) 0.028(5) 0.048(8) -0.007(5) -0.006(6) -0.009(5)
C12 0.064(8) 0.022(5) 0.059(8) 0.004(5) 0.011(7) 0.007(6)
C11 0.035(6) 0.035(6) 0.040(6) 0.009(5) 0.007(6) -0.001(5)
C5 0.047(8) 0.033(6) 0.054(8) -0.003(6) -0.008(6) -0.015(5)
C7 0.034(6) 0.046(6) 0.044(6) -0.003(6) -0.002(6) -0.005(6)
C16 0.033(6) 0.030(5) 0.037(6) 0.001(5) 0.007(6) 0.005(5)
O10 0.053(5) 0.056(6) 0.045(4) 0.003(4) 0.000(4) 0.011(5)
O8 0.093(6) 0.064(5) 0.053(5) 0.001(6) 0.019(5) 0.017(8)
N4 0.063(6) 0.037(5) 0.037(5) -0.002(6) 0.010(5) 0.001(7)
O13 0.054(5) 0.046(5) 0.042(5) -0.001(4) 0.005(4) -0.001(4)
O12 0.052(5) 0.056(6) 0.048(5) 0.012(4) -0.003(4) -0.004(4)
O3 0.038(4) 0.021(3) 0.045(5) 0.003(3) -0.007(4) 0.008(3)
O9 0.042(4) 0.064(6) 0.054(5) -0.002(4) -0.001(4) 0.011(4)
O7 0.045(5) 0.087(7) 0.070(6) 0.036(6) -0.002(5) 0.020(5)
O5 0.030(4) 0.129(10) 0.110(8) 0.003(7) -0.005(6) 0.029(6)
N5 0.044(6) 0.065(8) 0.055(7) -0.020(7) 0.005(6) -0.020(7)
C19 0.035(6) 0.047(6) 0.045(7) -0.005(6) -0.013(6) -0.008(6)
O6 0.046(5) 0.045(4) 0.073(6) 0.008(4) -0.002(5) -0.006(4)
O11 0.082(7) 0.114(9) 0.052(5) -0.035(6) 0.021(6) -0.044(7)
C14 0.045(7) 0.034(6) 0.040(6) -0.005(5) 0.002(5) -0.001(5)
C8 0.041(7) 0.046(6) 0.044(6) 0.008(6) -0.008(6) -0.003(6)
C17 0.066(8) 0.026(5) 0.049(6) 0.016(5) -0.012(7) -0.002(6)
N3 0.040(6) 0.059(7) 0.051(6) -0.006(5) -0.008(5) 0.013(5)
C20 0.041(7) 0.060(8) 0.082(10) -0.010(8) 0.003(8) -0.016(7)
C4 0.058(8) 0.026(5) 0.073(9) 0.009(6) -0.001(7) -0.012(6)
C2 0.030(6) 0.023(5) 0.038(6) -0.001(4) 0.016(5) 0.002(5)
C3 0.038(6) 0.031(6) 0.058(8) 0.006(6) 0.001(6) 0.002(5)
C18 0.061(8) 0.034(6) 0.072(9) -0.005(7) -0.021(8) 0.007(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'
Cu Cu 0.3201 1.2651 '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
O1 Ce O2 63.5(2) . . ?
O1 Ce O10 120.8(3) . . ?
O2 Ce O10 115.9(3) . . ?
O1 Ce O13 73.9(3) . . ?
O2 Ce O13 113.5(2) . . ?
O10 Ce O13 129.5(3) . . ?
O1 Ce O6 139.4(3) . . ?
O2 Ce O6 114.0(3) . . ?
O10 Ce O6 97.4(3) . . ?
O13 Ce O6 70.9(3) . . ?
O1 Ce O9 81.1(3) . . ?
O2 Ce O9 72.3(3) . . ?
O10 Ce O9 49.6(3) . . ?
O13 Ce O9 146.9(3) . . ?
O6 Ce O9 138.9(3) . . ?
O1 Ce O12 74.1(3) . . ?
O2 Ce O12 70.7(3) . . ?
O10 Ce O12 165.0(3) . . ?
O13 Ce O12 49.3(3) . . ?
O6 Ce O12 67.8(3) . . ?
O9 Ce O12 141.8(3) . . ?
O1 Ce O7 133.9(3) . . ?
O2 Ce O7 161.1(3) . . ?
O10 Ce O7 64.9(3) . . ?
O13 Ce O7 71.8(3) . . ?
O6 Ce O7 49.0(3) . . ?
O9 Ce O7 113.9(3) . . ?
O12 Ce O7 104.2(3) . . ?
O1 Ce O3 60.4(2) . . ?
O2 Ce O3 119.4(2) . . ?
O10 Ce O3 77.2(2) . . ?
O13 Ce O3 70.4(2) . . ?
O6 Ce O3 122.7(2) . . ?
O9 Ce O3 78.5(2) . . ?
O12 Ce O3 112.1(2) . . ?
O7 Ce O3 79.5(3) . . ?
O1 Ce O4 123.3(2) . . ?
O2 Ce O4 59.9(2) . . ?
O10 Ce O4 83.0(3) . . ?
O13 Ce O4 132.3(3) . . ?
O6 Ce O4 71.1(2) . . ?
O9 Ce O4 79.8(3) . . ?
O12 Ce O4 89.9(3) . . ?
O7 Ce O4 102.6(3) . . ?
O3 Ce O4 156.9(2) . . ?
O1 Ce N4 100.6(3) . . ?
O2 Ce N4 94.8(3) . . ?
O10 Ce N4 24.8(3) . . ?
O13 Ce N4 143.0(3) . . ?
O6 Ce N4 119.8(3) . . ?
O9 Ce N4 24.9(2) . . ?
O12 Ce N4 165.6(3) . . ?
O7 Ce N4 89.2(3) . . ?
O3 Ce N4 75.2(3) . . ?
O4 Ce N4 81.9(3) . . ?
O1 Ce N5 71.6(3) . . ?
O2 Ce N5 92.1(3) . . ?
O10 Ce N5 151.9(3) . . ?
O13 Ce N5 24.3(3) . . ?
O6 Ce N5 67.9(3) . . ?
O9 Ce N5 152.6(3) . . ?
O12 Ce N5 25.0(3) . . ?
O7 Ce N5 88.2(3) . . ?
O3 Ce N5 90.6(3) . . ?
O4 Ce N5 112.3(3) . . ?
N4 Ce N5 165.8(3) . . ?
O2 Cu O1 85.2(3) . . ?
O2 Cu N2 95.4(4) . . ?
O1 Cu N2 177.5(4) . . ?
O2 Cu N1 172.2(4) . . ?
O1 Cu N1 94.4(3) . . ?
N2 Cu N1 85.3(4) . . ?
O2 Cu Ce 43.2(2) . . ?
O1 Cu Ce 42.07(19) . . ?
N2 Cu Ce 138.6(3) . . ?
N1 Cu Ce 135.5(3) . . ?
C7 N1 C8 123.8(10) . . ?
C7 N1 Cu 125.4(8) . . ?
C8 N1 Cu 110.8(7) . . ?
C1 O1 Cu 124.1(6) . . ?
C1 O1 Ce 128.2(6) . . ?
Cu O1 Ce 106.1(3) . . ?
C14 C15 O4 124.3(10) . . ?
C14 C15 C16 121.3(10) . . ?
O4 C15 C16 114.3(8) . . ?
C16 O2 Cu 126.0(7) . . ?
C16 O2 Ce 128.8(7) . . ?
Cu O2 Ce 105.1(3) . . ?
O1 C1 C2 118.3(10) . . ?
O1 C1 C6 122.1(9) . . ?
C2 C1 C6 119.6(9) . . ?
C15 O4 C19 118.5(8) . . ?
C15 O4 Ce 119.7(6) . . ?
C19 O4 Ce 121.8(6) . . ?
C10 N2 C9 121.4(10) . . ?
C10 N2 Cu 125.4(9) . . ?
C9 N2 Cu 113.1(7) . . ?
N2 C10 C11 125.6(11) . . ?
C8 C9 N2 106.9(9) . . ?
C12 C13 C14 119.2(10) . . ?
C1 C6 C7 125.4(9) . . ?
C1 C6 C5 117.5(11) . . ?
C7 C6 C5 117.1(11) . . ?
C13 C12 C11 122.5(11) . . ?
C16 C11 C12 118.1(11) . . ?
C16 C11 C10 123.5(10) . . ?
C12 C11 C10 118.4(10) . . ?
C4 C5 C6 120.8(12) . . ?
N1 C7 C6 123.8(11) . . ?
O2 C16 C15 117.1(10) . . ?
O2 C16 C11 123.8(11) . . ?
C15 C16 C11 119.1(10) . . ?
N4 O10 Ce 98.0(6) . . ?
O8 N4 O9 121.6(10) . . ?
O8 N4 O10 122.3(10) . . ?
O9 N4 O10 116.1(8) . . ?
O8 N4 Ce 173.0(10) . . ?
O9 N4 Ce 59.1(5) . . ?
O10 N4 Ce 57.2(5) . . ?
N5 O13 Ce 97.5(7) . . ?
N5 O12 Ce 95.0(7) . . ?
C2 O3 C17 118.6(8) . . ?
C2 O3 Ce 119.9(5) . . ?
C17 O3 Ce 121.1(6) . . ?
N4 O9 Ce 96.0(6) . . ?
N3 O7 Ce 95.8(6) . . ?
O11 N5 O13 124.0(13) . . ?
O11 N5 O12 117.9(14) . . ?
O13 N5 O12 118.2(11) . . ?
O11 N5 Ce 177.6(11) . . ?
O13 N5 Ce 58.3(6) . . ?
O12 N5 Ce 60.0(6) . . ?
O4 C19 C20 112.8(10) . . ?
N3 O6 Ce 98.7(7) . . ?
C15 C14 C13 119.7(11) . . ?
N1 C8 C9 108.2(9) . . ?
O3 C17 C18 112.2(10) . . ?
O5 N3 O6 121.9(12) . . ?
O5 N3 O7 121.5(11) . . ?
O6 N3 O7 116.5(9) . . ?
C5 C4 C3 120.3(11) . . ?
C3 C2 C1 121.3(11) . . ?
C3 C2 O3 126.1(10) . . ?
C1 C2 O3 112.5(8) . . ?
C2 C3 C4 120.6(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
Ce O1 2.437(7) . ?
Ce O2 2.478(7) . ?
Ce O10 2.549(7) . ?
Ce O13 2.579(8) . ?
Ce O6 2.590(9) . ?
Ce O9 2.593(8) . ?
Ce O12 2.613(9) . ?
Ce O7 2.632(8) . ?
Ce O3 2.657(7) . ?
Ce O4 2.700(7) . ?
Ce N4 3.005(9) . ?
Ce N5 3.007(11) . ?
Cu O2 1.902(7) . ?
Cu O1 1.918(7) . ?
Cu N2 1.921(9) . ?
Cu N1 1.921(9) . ?
N1 C7 1.301(14) . ?
N1 C8 1.492(13) . ?
O1 C1 1.338(11) . ?
C15 C14 1.378(14) . ?
C15 O4 1.393(12) . ?
C15 C16 1.404(15) . ?
O2 C16 1.340(12) . ?
C1 C2 1.389(14) . ?
C1 C6 1.420(15) . ?
O4 C19 1.458(12) . ?
N2 C10 1.275(14) . ?
N2 C9 1.496(15) . ?
C10 C11 1.465(17) . ?
C9 C8 1.495(16) . ?
C13 C12 1.342(17) . ?
C13 C14 1.428(16) . ?
C6 C7 1.437(16) . ?
C6 C5 1.437(14) . ?
C12 C11 1.428(15) . ?
C11 C16 1.411(15) . ?
C5 C4 1.355(17) . ?
O10 N4 1.275(12) . ?
O8 N4 1.202(11) . ?
N4 O9 1.270(11) . ?
O13 N5 1.247(14) . ?
O12 N5 1.277(14) . ?
O3 C2 1.414(13) . ?
O3 C17 1.470(12) . ?
O7 N3 1.289(13) . ?
O5 N3 1.219(13) . ?
N5 O11 1.222(13) . ?
C19 C20 1.476(17) . ?
O6 N3 1.258(12) . ?
C17 C18 1.498(17) . ?
C4 C3 1.398(17) . ?
C2 C3 1.354(14) . ?
|
1100947.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100947.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_1100947
loop_
_publ_author_name
'Rajesh Koner'
'Hsin-Huang Lin'
'Ho-Hsiang Wei'
'Sasankasekhar Mohanta'
_publ_section_title
;
Syntheses, Structures, and Magnetic Properties of Diphenoxo-Bridged
MIILnIII Complexes Derived from N,N'-Ethylenebis(3-ethoxysalicylaldiimine)
(M = Cu or Ni; Ln = Ce-Yb): Observation of Surprisingly Strong Exchange
Interactions
;
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3524
_journal_page_last 3536
_journal_paper_doi 10.1021/ic048196h
_journal_volume 44
_journal_year 2005
_chemical_formula_sum 'C20 H22 Cu N5 O13 Pr'
_chemical_formula_weight 744.88
_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 8.619(5)
_cell_length_b 13.8698(10)
_cell_length_c 21.1269(15)
_cell_measurement_temperature 293(2)
_cell_volume 2525.6(15)
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 293(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 0.0000
_diffrn_reflns_av_sigmaI/netI 0.0274
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -1
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min -1
_diffrn_reflns_limit_l_max 25
_diffrn_reflns_limit_l_min -1
_diffrn_reflns_number 2542
_diffrn_reflns_theta_full 24.99
_diffrn_reflns_theta_max 24.99
_diffrn_reflns_theta_min 1.76
_exptl_absorpt_coefficient_mu 2.826
_exptl_crystal_colour Red
_exptl_crystal_density_diffrn 1.959
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1476
_exptl_crystal_size_max 55
_exptl_crystal_size_mid 38
_exptl_crystal_size_min 20
_refine_diff_density_max 0.427
_refine_diff_density_min -0.864
_refine_diff_density_rms 0.122
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack -0.02(3)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.182
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 361
_refine_ls_number_reflns 2542
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.182
_refine_ls_R_factor_all 0.0331
_refine_ls_R_factor_gt 0.0273
_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^)+(0.0348P)^2^+4.7780P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0718
_refine_ls_wR_factor_ref 0.0837
_reflns_number_gt 2376
_reflns_number_total 2542
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file ic048196hsi20050224_082436_02.cif
_cod_data_source_block cupr
_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 2525.7(15)
_cod_database_code 1100947
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
Pr Pr 0.75869(4) -0.00028(3) 0.094868(16) 0.02698(13) Uani 1 1 d . . .
Cu Cu 0.43274(11) -0.05607(6) 0.18306(5) 0.0328(2) Uani 1 1 d . . .
N4 N 0.6271(9) -0.0056(5) -0.0349(3) 0.0435(16) Uani 1 1 d . . .
O9 O 0.5480(8) -0.0308(5) 0.0113(3) 0.0550(17) Uani 1 1 d . . .
O1 O 0.5378(6) 0.0561(3) 0.1541(2) 0.0313(12) Uani 1 1 d . . .
O2 O 0.5853(7) -0.1247(3) 0.1363(3) 0.0354(13) Uani 1 1 d . . .
C15 C 0.7087(9) -0.2569(5) 0.0894(4) 0.0325(17) Uani 1 1 d . . .
N1 N 0.2997(8) 0.0138(5) 0.2389(3) 0.0366(15) Uani 1 1 d . . .
C10 C 0.3486(10) -0.2545(6) 0.1927(4) 0.038(2) Uani 1 1 d . . .
H10A H 0.2828 -0.3023 0.2080 0.046 Uiso 1 1 calc R . .
C16 C 0.5866(9) -0.2205(5) 0.1269(3) 0.0261(15) Uani 1 1 d . . .
C9 C 0.1861(10) -0.1450(6) 0.2490(4) 0.042(2) Uani 1 1 d . . .
H9A H 0.1658 -0.1969 0.2786 0.050 Uiso 1 1 calc R . .
H9B H 0.0951 -0.1361 0.2226 0.050 Uiso 1 1 calc R . .
O8 O 0.5721(11) 0.0009(5) -0.0875(3) 0.072(2) Uani 1 1 d . . .
O10 O 0.7680(7) 0.0136(5) -0.0239(3) 0.0510(15) Uani 1 1 d . . .
N2 N 0.3220(8) -0.1681(5) 0.2095(3) 0.0349(16) Uani 1 1 d . . .
C11 C 0.4751(10) -0.2840(6) 0.1511(4) 0.0335(18) Uani 1 1 d . . .
O4 O 0.8121(6) -0.1867(4) 0.0695(3) 0.0349(12) Uani 1 1 d . . .
O3 O 0.6545(6) 0.1758(3) 0.0753(3) 0.0323(12) Uani 1 1 d . . .
C13 C 0.6021(11) -0.4161(5) 0.0961(4) 0.046(2) Uani 1 1 d . . .
H13A H 0.6043 -0.4806 0.0839 0.055 Uiso 1 1 calc R . .
C19 C 0.9463(10) -0.2180(6) 0.0347(4) 0.044(2) Uani 1 1 d . . .
H19A H 0.9894 -0.1637 0.0117 0.053 Uiso 1 1 calc R . .
H19B H 0.9157 -0.2666 0.0042 0.053 Uiso 1 1 calc R . .
C17 C 0.7267(10) 0.2410(5) 0.0284(4) 0.0381(19) Uani 1 1 d . . .
H17A H 0.6466 0.2795 0.0083 0.046 Uiso 1 1 calc R . .
H17B H 0.7768 0.2029 -0.0042 0.046 Uiso 1 1 calc R . .
C2 C 0.5388(9) 0.2125(5) 0.1142(4) 0.0311(17) Uani 1 1 d . . .
C14 C 0.7169(11) -0.3537(5) 0.0753(4) 0.0376(19) Uani 1 1 d . . .
H14A H 0.7999 -0.3772 0.0518 0.045 Uiso 1 1 calc R . .
C1 C 0.4780(9) 0.1450(5) 0.1558(4) 0.0288(17) Uani 1 1 d . . .
C8 C 0.2231(10) -0.0519(6) 0.2847(4) 0.0416(19) Uani 1 1 d . . .
H8A H 0.1287 -0.0229 0.3009 0.050 Uiso 1 1 calc R . .
H8B H 0.2917 -0.0651 0.3201 0.050 Uiso 1 1 calc R . .
O12 O 0.8217(8) -0.0333(5) 0.2122(3) 0.0509(17) Uani 1 1 d . . .
O13 O 0.8652(8) 0.1125(4) 0.1803(3) 0.0476(15) Uani 1 1 d . . .
O6 O 1.0449(7) -0.0375(4) 0.1111(3) 0.0505(16) Uani 1 1 d . . .
N5 N 0.8643(9) 0.0527(7) 0.2246(4) 0.049(2) Uani 1 1 d . . .
O7 O 1.0055(8) 0.0831(5) 0.0496(3) 0.061(2) Uani 1 1 d . . .
C7 C 0.2790(10) 0.1053(6) 0.2389(4) 0.0380(18) Uani 1 1 d . . .
H7A H 0.2102 0.1308 0.2684 0.046 Uiso 1 1 calc R . .
N3 N 1.1011(8) 0.0281(6) 0.0776(4) 0.049(2) Uani 1 1 d . . .
C3 C 0.4809(10) 0.3040(5) 0.1115(4) 0.042(2) Uani 1 1 d . . .
H3A H 0.5203 0.3478 0.0823 0.051 Uiso 1 1 calc R . .
C6 C 0.3549(10) 0.1714(5) 0.1963(4) 0.0338(19) Uani 1 1 d . . .
C5 C 0.3008(11) 0.2675(6) 0.1948(4) 0.043(2) Uani 1 1 d . . .
H5A H 0.2230 0.2869 0.2225 0.051 Uiso 1 1 calc R . .
C20 C 1.0686(12) -0.2592(7) 0.0782(5) 0.058(3) Uani 1 1 d . . .
H20A H 1.1564 -0.2795 0.0536 0.088 Uiso 1 1 calc R . .
H20B H 1.0266 -0.3135 0.1005 0.088 Uiso 1 1 calc R . .
H20C H 1.1004 -0.2108 0.1080 0.088 Uiso 1 1 calc R . .
C12 C 0.4857(11) -0.3832(6) 0.1343(4) 0.044(2) Uani 1 1 d . . .
H12A H 0.4121 -0.4264 0.1496 0.053 Uiso 1 1 calc R . .
C4 C 0.3623(11) 0.3320(6) 0.1527(4) 0.047(2) Uani 1 1 d . . .
H4A H 0.3249 0.3949 0.1515 0.057 Uiso 1 1 calc R . .
C18 C 0.8446(12) 0.3068(6) 0.0585(5) 0.052(2) Uani 1 1 d . . .
H18A H 0.8886 0.3481 0.0268 0.077 Uiso 1 1 calc R . .
H18B H 0.9252 0.2689 0.0776 0.077 Uiso 1 1 calc R . .
H18C H 0.7949 0.3454 0.0904 0.077 Uiso 1 1 calc R . .
O5 O 1.2394(8) 0.0417(7) 0.0730(4) 0.084(3) Uani 1 1 d . . .
O11 O 0.9047(9) 0.0764(6) 0.2777(3) 0.076(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
Pr 0.0272(2) 0.0222(2) 0.0315(2) 0.00241(17) 0.00327(15) -0.0012(2)
Cu 0.0318(5) 0.0238(4) 0.0427(5) 0.0032(4) 0.0099(4) -0.0015(4)
N4 0.063(4) 0.028(3) 0.039(4) -0.007(4) -0.004(3) 0.003(4)
O9 0.048(3) 0.063(4) 0.054(4) -0.002(3) -0.001(3) -0.010(3)
O1 0.029(3) 0.020(2) 0.045(3) 0.005(2) 0.009(2) 0.002(2)
O2 0.036(3) 0.018(2) 0.052(3) 0.002(2) 0.015(3) -0.001(2)
C15 0.037(4) 0.024(3) 0.037(4) 0.003(3) -0.004(4) 0.000(3)
N1 0.032(3) 0.034(3) 0.044(4) 0.005(3) 0.007(3) 0.002(3)
C10 0.037(4) 0.031(4) 0.048(5) 0.015(4) 0.008(4) -0.007(4)
C16 0.032(4) 0.018(3) 0.028(3) 0.003(3) -0.004(3) -0.003(3)
C9 0.037(4) 0.048(5) 0.040(4) 0.006(4) 0.012(4) -0.003(4)
O8 0.106(6) 0.065(4) 0.046(4) 0.003(4) -0.020(4) -0.012(5)
O10 0.052(4) 0.059(4) 0.042(3) -0.002(3) 0.004(3) -0.012(4)
N2 0.036(4) 0.034(3) 0.034(3) 0.006(3) 0.006(3) -0.006(3)
C11 0.038(4) 0.032(4) 0.031(4) 0.006(3) -0.006(4) -0.002(4)
O4 0.032(3) 0.030(3) 0.043(3) -0.001(2) 0.009(2) 0.004(2)
O3 0.033(3) 0.020(2) 0.044(3) 0.006(2) 0.006(3) -0.001(2)
C13 0.065(6) 0.022(4) 0.052(5) -0.001(4) -0.009(5) 0.001(4)
C19 0.038(4) 0.045(5) 0.049(5) -0.006(4) 0.010(4) 0.008(4)
C17 0.054(5) 0.027(3) 0.034(4) 0.007(3) 0.013(4) -0.005(4)
C2 0.025(4) 0.026(3) 0.042(4) -0.001(3) -0.007(3) -0.002(3)
C14 0.047(5) 0.025(4) 0.041(4) -0.006(3) -0.006(4) 0.005(4)
C1 0.029(4) 0.017(3) 0.040(4) -0.004(3) -0.002(3) 0.000(3)
C8 0.042(5) 0.046(4) 0.036(4) 0.009(4) 0.007(4) 0.008(4)
O12 0.048(4) 0.059(4) 0.045(3) 0.014(3) -0.001(3) 0.005(3)
O13 0.057(4) 0.033(3) 0.053(4) -0.003(3) -0.004(3) -0.002(3)
O6 0.037(3) 0.046(3) 0.068(4) 0.009(3) 0.003(3) 0.000(3)
N5 0.038(4) 0.061(5) 0.048(5) -0.014(4) -0.004(4) 0.024(4)
O7 0.041(4) 0.078(5) 0.065(4) 0.028(4) 0.004(3) -0.015(4)
C7 0.031(4) 0.046(4) 0.037(4) 0.002(4) 0.001(4) 0.008(4)
N3 0.025(3) 0.055(5) 0.067(5) -0.016(4) 0.006(4) -0.009(3)
C3 0.042(5) 0.025(4) 0.060(5) 0.008(4) -0.010(4) 0.000(3)
C6 0.033(4) 0.025(3) 0.044(5) -0.002(3) 0.001(4) 0.004(3)
C5 0.038(5) 0.031(4) 0.059(6) -0.005(4) 0.004(4) 0.013(4)
C20 0.046(5) 0.046(5) 0.083(7) -0.009(5) -0.006(6) 0.014(5)
C12 0.058(6) 0.025(4) 0.050(5) 0.009(4) -0.007(5) -0.010(4)
C4 0.046(5) 0.028(4) 0.068(6) -0.002(4) -0.004(5) 0.012(4)
C18 0.054(6) 0.032(4) 0.068(6) -0.008(4) 0.020(5) -0.007(4)
O5 0.034(4) 0.125(7) 0.094(6) -0.001(6) 0.009(4) -0.020(5)
O11 0.080(5) 0.103(6) 0.046(4) -0.027(4) -0.021(4) 0.039(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'
Pr Pr -0.2180 2.8214 '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 Pr O2 63.90(16) . . ?
O1 Pr O10 121.22(19) . . ?
O2 Pr O10 115.5(2) . . ?
O1 Pr O6 139.67(19) . . ?
O2 Pr O6 113.68(19) . . ?
O10 Pr O6 96.8(2) . . ?
O1 Pr O13 73.7(2) . . ?
O2 Pr O13 113.47(19) . . ?
O10 Pr O13 130.2(2) . . ?
O6 Pr O13 71.4(2) . . ?
O1 Pr O9 81.5(2) . . ?
O2 Pr O9 72.4(2) . . ?
O10 Pr O9 49.4(2) . . ?
O6 Pr O9 138.2(2) . . ?
O13 Pr O9 147.1(2) . . ?
O1 Pr O12 74.00(19) . . ?
O2 Pr O12 70.1(2) . . ?
O10 Pr O12 164.8(2) . . ?
O6 Pr O12 68.3(2) . . ?
O13 Pr O12 49.8(2) . . ?
O9 Pr O12 141.3(2) . . ?
O1 Pr O7 133.8(2) . . ?
O2 Pr O7 160.8(2) . . ?
O10 Pr O7 64.8(2) . . ?
O6 Pr O7 49.2(2) . . ?
O13 Pr O7 72.2(2) . . ?
O9 Pr O7 113.5(2) . . ?
O12 Pr O7 105.1(2) . . ?
O1 Pr O3 60.75(16) . . ?
O2 Pr O3 120.14(17) . . ?
O10 Pr O3 77.50(19) . . ?
O6 Pr O3 122.67(18) . . ?
O13 Pr O3 70.53(18) . . ?
O9 Pr O3 78.67(19) . . ?
O12 Pr O3 112.78(19) . . ?
O7 Pr O3 79.0(2) . . ?
O1 Pr O4 123.53(16) . . ?
O2 Pr O4 59.69(16) . . ?
O10 Pr O4 82.50(19) . . ?
O6 Pr O4 70.41(18) . . ?
O13 Pr O4 131.97(18) . . ?
O9 Pr O4 79.9(2) . . ?
O12 Pr O4 89.11(19) . . ?
O7 Pr O4 102.4(2) . . ?
O3 Pr O4 157.13(19) . . ?
O1 Pr N4 100.74(19) . . ?
O2 Pr N4 94.6(2) . . ?
O10 Pr N4 25.0(2) . . ?
O6 Pr N4 119.3(2) . . ?
O13 Pr N4 143.52(19) . . ?
O9 Pr N4 24.56(19) . . ?
O12 Pr N4 164.6(2) . . ?
O7 Pr N4 89.1(2) . . ?
O3 Pr N4 75.39(18) . . ?
O4 Pr N4 81.79(18) . . ?
O1 Pr N5 71.54(19) . . ?
O2 Pr N5 91.8(2) . . ?
O10 Pr N5 152.6(2) . . ?
O6 Pr N5 68.3(2) . . ?
O13 Pr N5 24.6(2) . . ?
O9 Pr N5 152.8(2) . . ?
O12 Pr N5 25.2(2) . . ?
O7 Pr N5 88.8(2) . . ?
O3 Pr N5 91.1(2) . . ?
O4 Pr N5 111.7(2) . . ?
N4 Pr N5 166.5(2) . . ?
O2 Cu O1 85.0(2) . . ?
O2 Cu N2 95.2(3) . . ?
O1 Cu N2 177.9(3) . . ?
O2 Cu N1 172.3(3) . . ?
O1 Cu N1 94.0(3) . . ?
N2 Cu N1 86.1(3) . . ?
O2 Cu Pr 43.11(15) . . ?
O1 Cu Pr 42.00(15) . . ?
N2 Cu Pr 138.3(2) . . ?
N1 Cu Pr 135.0(2) . . ?
O8 N4 O9 121.8(8) . . ?
O8 N4 O10 121.9(8) . . ?
O9 N4 O10 116.2(7) . . ?
O8 N4 Pr 174.3(6) . . ?
O9 N4 Pr 59.4(4) . . ?
O10 N4 Pr 57.2(4) . . ?
N4 O9 Pr 96.1(5) . . ?
C1 O1 Cu 124.3(5) . . ?
C1 O1 Pr 128.1(4) . . ?
Cu O1 Pr 106.1(2) . . ?
C16 O2 Cu 125.3(5) . . ?
C16 O2 Pr 129.8(5) . . ?
Cu O2 Pr 104.8(2) . . ?
C14 C15 O4 125.9(8) . . ?
C14 C15 C16 120.6(7) . . ?
O4 C15 C16 113.5(6) . . ?
C7 N1 C8 123.1(7) . . ?
C7 N1 Cu 125.9(6) . . ?
C8 N1 Cu 111.0(5) . . ?
N2 C10 C11 124.6(7) . . ?
O2 C16 C11 124.2(7) . . ?
O2 C16 C15 116.3(7) . . ?
C11 C16 C15 119.4(6) . . ?
N2 C9 C8 107.3(7) . . ?
N4 O10 Pr 97.9(5) . . ?
C10 N2 C9 120.5(7) . . ?
C10 N2 Cu 126.6(6) . . ?
C9 N2 Cu 112.7(5) . . ?
C16 C11 C12 118.3(8) . . ?
C16 C11 C10 123.8(7) . . ?
C12 C11 C10 117.9(8) . . ?
C15 O4 C19 117.5(6) . . ?
C15 O4 Pr 120.5(4) . . ?
C19 O4 Pr 122.1(5) . . ?
C2 O3 C17 118.3(5) . . ?
C2 O3 Pr 119.5(4) . . ?
C17 O3 Pr 121.9(4) . . ?
C12 C13 C14 120.2(7) . . ?
O4 C19 C20 111.4(7) . . ?
O3 C17 C18 111.8(7) . . ?
C3 C2 C1 121.1(8) . . ?
C3 C2 O3 125.4(7) . . ?
C1 C2 O3 113.5(6) . . ?
C15 C14 C13 120.3(8) . . ?
O1 C1 C2 117.5(7) . . ?
O1 C1 C6 123.0(7) . . ?
C2 C1 C6 119.5(6) . . ?
N1 C8 C9 106.7(6) . . ?
N5 O12 Pr 95.3(5) . . ?
N5 O13 Pr 96.9(5) . . ?
N3 O6 Pr 98.8(5) . . ?
O11 N5 O13 120.5(9) . . ?
O11 N5 O12 121.6(9) . . ?
O13 N5 O12 117.9(7) . . ?
O11 N5 Pr 178.2(6) . . ?
O13 N5 Pr 58.5(4) . . ?
O12 N5 Pr 59.5(4) . . ?
N3 O7 Pr 95.3(5) . . ?
N1 C7 C6 124.5(8) . . ?
O5 N3 O6 122.8(9) . . ?
O5 N3 O7 120.5(9) . . ?
O6 N3 O7 116.7(7) . . ?
O5 N3 Pr 177.3(7) . . ?
O6 N3 Pr 56.9(4) . . ?
O7 N3 Pr 59.8(4) . . ?
C2 C3 C4 120.0(8) . . ?
C1 C6 C5 118.6(7) . . ?
C1 C6 C7 123.7(7) . . ?
C5 C6 C7 117.7(8) . . ?
C4 C5 C6 120.3(8) . . ?
C13 C12 C11 121.1(8) . . ?
C5 C4 C3 120.4(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
Pr O1 2.409(5) . ?
Pr O2 2.445(5) . ?
Pr O10 2.518(6) . ?
Pr O6 2.543(7) . ?
Pr O13 2.559(6) . ?
Pr O9 2.568(7) . ?
Pr O12 2.578(6) . ?
Pr O7 2.603(6) . ?
Pr O3 2.634(5) . ?
Pr O4 2.681(5) . ?
Pr N4 2.968(7) . ?
Pr N5 2.980(8) . ?
Cu O2 1.901(5) . ?
Cu O1 1.901(5) . ?
Cu N2 1.908(7) . ?
Cu N1 1.910(7) . ?
N4 O8 1.211(9) . ?
N4 O9 1.241(9) . ?
N4 O10 1.265(9) . ?
O1 C1 1.337(8) . ?
O2 C16 1.343(8) . ?
C15 C14 1.376(10) . ?
C15 O4 1.385(9) . ?
C15 C16 1.410(11) . ?
N1 C7 1.282(10) . ?
N1 C8 1.484(10) . ?
C10 N2 1.270(10) . ?
C10 C11 1.460(12) . ?
C16 C11 1.400(11) . ?
C9 N2 1.473(11) . ?
C9 C8 1.530(12) . ?
C11 C12 1.424(11) . ?
O4 C19 1.438(9) . ?
O3 C2 1.390(9) . ?
O3 C17 1.480(8) . ?
C13 C12 1.367(13) . ?
C13 C14 1.386(12) . ?
C19 C20 1.510(13) . ?
C17 C18 1.507(12) . ?
C2 C3 1.365(11) . ?
C2 C1 1.386(10) . ?
C1 C6 1.412(11) . ?
O12 N5 1.275(11) . ?
O13 N5 1.250(10) . ?
O6 N3 1.249(10) . ?
N5 O11 1.221(10) . ?
O7 N3 1.269(10) . ?
C7 C6 1.441(11) . ?
N3 O5 1.211(9) . ?
C3 C4 1.397(13) . ?
C6 C5 1.412(11) . ?
C5 C4 1.368(13) . ?
|
1100948.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100948.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_1100948
loop_
_publ_author_name
'Rajesh Koner'
'Hsin-Huang Lin'
'Ho-Hsiang Wei'
'Sasankasekhar Mohanta'
_publ_section_title
;
Syntheses, Structures, and Magnetic Properties of Diphenoxo-Bridged
MIILnIII Complexes Derived from N,N'-Ethylenebis(3-ethoxysalicylaldiimine)
(M = Cu or Ni; Ln = Ce-Yb): Observation of Surprisingly Strong Exchange
Interactions
;
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3524
_journal_page_last 3536
_journal_paper_doi 10.1021/ic048196h
_journal_volume 44
_journal_year 2005
_chemical_formula_sum 'C20 H22 Cu Eu N5 O13'
_chemical_formula_weight 755.93
_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 8.601(3)
_cell_length_b 13.786(2)
_cell_length_c 21.1483(16)
_cell_measurement_temperature 293(2)
_cell_volume 2507.6(10)
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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 0.0399
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -1
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min -1
_diffrn_reflns_limit_l_max 25
_diffrn_reflns_limit_l_min -1
_diffrn_reflns_number 2527
_diffrn_reflns_theta_full 24.99
_diffrn_reflns_theta_max 24.99
_diffrn_reflns_theta_min 1.76
_exptl_absorpt_coefficient_mu 3.405
_exptl_crystal_colour Red
_exptl_crystal_density_diffrn 2.002
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1492
_exptl_crystal_size_max 56
_exptl_crystal_size_mid 32
_exptl_crystal_size_min 25
_refine_diff_density_max 0.519
_refine_diff_density_min -0.877
_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 0.00(3)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.089
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 361
_refine_ls_number_reflns 2527
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.089
_refine_ls_R_factor_all 0.0370
_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^)+(0.0377P)^2^+2.1362P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0775
_refine_ls_wR_factor_ref 0.0817
_reflns_number_gt 2254
_reflns_number_total 2527
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file ic048196hsi20050224_082436_03.cif
_cod_data_source_block cueu
_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 2507.7(9)
_cod_database_code 1100948
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
Eu Eu 0.75954(4) 0.00097(3) 0.097750(16) 0.02812(12) Uani 1 1 d . . .
O1 O 0.5422(6) 0.0569(4) 0.1544(2) 0.0326(12) Uani 1 1 d . . .
Cu Cu 0.43574(11) -0.05621(7) 0.18321(5) 0.0342(2) Uani 1 1 d . . .
O2 O 0.5892(7) -0.1240(4) 0.1369(3) 0.0364(14) Uani 1 1 d . . .
N2 N 0.3238(8) -0.1688(5) 0.2092(4) 0.0376(18) Uani 1 1 d . . .
O10 O 0.7791(7) 0.0104(5) -0.0180(3) 0.0490(15) Uani 1 1 d . . .
N1 N 0.3004(8) 0.0134(5) 0.2385(3) 0.0388(16) Uani 1 1 d . . .
N4 N 0.6352(8) -0.0064(6) -0.0305(3) 0.0427(16) Uani 1 1 d . . .
O9 O 0.5532(7) -0.0269(5) 0.0160(3) 0.0537(17) Uani 1 1 d . . .
O4 O 0.8175(6) -0.1832(4) 0.0698(3) 0.0351(13) Uani 1 1 d . . .
O3 O 0.6600(6) 0.1758(4) 0.0756(3) 0.0346(13) Uani 1 1 d . . .
O8 O 0.5839(10) -0.0012(6) -0.0836(3) 0.071(2) Uani 1 1 d . . .
C2 C 0.5430(9) 0.2125(5) 0.1132(4) 0.0314(18) Uani 1 1 d . . .
O13 O 0.8628(7) 0.1115(4) 0.1816(3) 0.0452(14) Uani 1 1 d . . .
O12 O 0.8211(8) -0.0343(5) 0.2128(3) 0.0494(18) Uani 1 1 d . . .
C15 C 0.7164(10) -0.2543(5) 0.0896(4) 0.0322(18) Uani 1 1 d . . .
C10 C 0.3533(10) -0.2552(6) 0.1915(4) 0.037(2) Uani 1 1 d . . .
H10A H 0.2873 -0.3038 0.2059 0.045 Uiso 1 1 calc R . .
C11 C 0.4820(10) -0.2844(6) 0.1505(4) 0.0353(19) Uani 1 1 d . . .
C16 C 0.5912(10) -0.2205(5) 0.1272(4) 0.0305(18) Uani 1 1 d . . .
C19 C 0.9532(9) -0.2140(7) 0.0342(4) 0.041(2) Uani 1 1 d . . .
H19A H 0.9963 -0.1587 0.0119 0.049 Uiso 1 1 calc R . .
H19B H 0.9222 -0.2619 0.0030 0.049 Uiso 1 1 calc R . .
C1 C 0.4819(9) 0.1453(5) 0.1557(4) 0.0278(17) Uani 1 1 d . . .
N5 N 0.8621(8) 0.0519(7) 0.2259(4) 0.047(2) Uani 1 1 d . . .
C7 C 0.2791(10) 0.1051(6) 0.2379(4) 0.0379(19) Uani 1 1 d . . .
H7A H 0.2088 0.1307 0.2668 0.045 Uiso 1 1 calc R . .
C17 C 0.7311(11) 0.2410(6) 0.0289(4) 0.040(2) Uani 1 1 d . . .
H17A H 0.6501 0.2788 0.0086 0.048 Uiso 1 1 calc R . .
H17B H 0.7821 0.2026 -0.0034 0.048 Uiso 1 1 calc R . .
C14 C 0.7259(12) -0.3528(6) 0.0753(4) 0.043(2) Uani 1 1 d . . .
H14A H 0.8083 -0.3761 0.0512 0.051 Uiso 1 1 calc R . .
C3 C 0.4834(10) 0.3054(5) 0.1096(4) 0.039(2) Uani 1 1 d . . .
H3A H 0.5231 0.3493 0.0804 0.047 Uiso 1 1 calc R . .
C13 C 0.6116(12) -0.4168(6) 0.0972(5) 0.049(2) Uani 1 1 d . . .
H13A H 0.6168 -0.4823 0.0869 0.059 Uiso 1 1 calc R . .
C8 C 0.2238(10) -0.0520(7) 0.2838(4) 0.044(2) Uani 1 1 d . . .
H8A H 0.1287 -0.0228 0.2995 0.052 Uiso 1 1 calc R . .
H8B H 0.2918 -0.0645 0.3195 0.052 Uiso 1 1 calc R . .
C12 C 0.4941(11) -0.3833(6) 0.1331(4) 0.045(2) Uani 1 1 d . . .
H12A H 0.4183 -0.4265 0.1469 0.054 Uiso 1 1 calc R . .
C6 C 0.3560(10) 0.1726(6) 0.1955(4) 0.036(2) Uani 1 1 d . . .
C4 C 0.3631(11) 0.3327(6) 0.1501(4) 0.047(2) Uani 1 1 d . . .
H4A H 0.3242 0.3956 0.1482 0.056 Uiso 1 1 calc R . .
C9 C 0.1880(11) -0.1456(7) 0.2492(5) 0.046(2) Uani 1 1 d . . .
H9A H 0.1694 -0.1975 0.2792 0.055 Uiso 1 1 calc R . .
H9B H 0.0958 -0.1378 0.2233 0.055 Uiso 1 1 calc R . .
C5 C 0.3020(11) 0.2690(6) 0.1923(5) 0.045(2) Uani 1 1 d . . .
H5A H 0.2234 0.2893 0.2194 0.053 Uiso 1 1 calc R . .
C20 C 1.0757(13) -0.2568(7) 0.0766(5) 0.058(3) Uani 1 1 d . . .
H20A H 1.1635 -0.2763 0.0516 0.087 Uiso 1 1 calc R . .
H20B H 1.0339 -0.3122 0.0982 0.087 Uiso 1 1 calc R . .
H20C H 1.1079 -0.2092 0.1070 0.087 Uiso 1 1 calc R . .
C18 C 0.8481(12) 0.3089(7) 0.0583(5) 0.055(3) Uani 1 1 d . . .
H18A H 0.8914 0.3500 0.0261 0.082 Uiso 1 1 calc R . .
H18B H 0.9296 0.2718 0.0777 0.082 Uiso 1 1 calc R . .
H18C H 0.7977 0.3481 0.0897 0.082 Uiso 1 1 calc R . .
O6 O 1.0396(7) -0.0367(4) 0.1131(3) 0.0490(16) Uani 1 1 d . . .
O7 O 1.0003(8) 0.0894(6) 0.0546(4) 0.065(2) Uani 1 1 d . . .
O11 O 0.9023(10) 0.0731(7) 0.2795(3) 0.077(3) Uani 1 1 d . . .
N3 N 1.0969(8) 0.0321(6) 0.0806(4) 0.047(2) Uani 1 1 d . . .
O5 O 1.2352(8) 0.0426(8) 0.0753(4) 0.083(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
Eu 0.02828(18) 0.02349(19) 0.0326(2) 0.00211(18) 0.00362(15) -0.0007(2)
O1 0.033(3) 0.022(2) 0.043(3) 0.004(2) 0.006(3) 0.003(3)
Cu 0.0341(5) 0.0252(4) 0.0433(5) 0.0038(5) 0.0106(5) -0.0014(4)
O2 0.039(3) 0.023(3) 0.047(3) 0.001(2) 0.016(3) -0.005(3)
N2 0.033(4) 0.030(3) 0.051(4) 0.008(3) 0.007(4) -0.004(3)
O10 0.052(3) 0.057(4) 0.038(3) 0.000(3) 0.010(3) -0.005(4)
N1 0.035(3) 0.038(4) 0.044(4) 0.007(4) 0.011(3) -0.001(3)
N4 0.056(4) 0.030(4) 0.043(4) 0.000(4) -0.002(3) -0.002(4)
O9 0.045(3) 0.065(5) 0.051(4) -0.002(3) -0.001(3) -0.008(3)
O4 0.035(3) 0.028(3) 0.043(3) 0.000(3) 0.009(3) 0.002(2)
O3 0.040(3) 0.026(3) 0.038(3) 0.006(3) 0.009(3) 0.000(3)
O8 0.109(6) 0.066(4) 0.039(3) 0.002(4) -0.020(4) -0.011(6)
C2 0.032(4) 0.027(4) 0.035(4) -0.005(3) -0.006(4) -0.004(3)
O13 0.056(4) 0.036(3) 0.043(3) -0.004(3) -0.008(3) 0.002(3)
O12 0.044(4) 0.057(4) 0.047(4) 0.020(3) -0.002(3) 0.009(3)
C15 0.037(4) 0.025(4) 0.035(4) 0.005(3) -0.007(4) -0.001(3)
C10 0.033(4) 0.035(4) 0.044(5) 0.014(4) -0.006(4) -0.008(4)
C11 0.046(5) 0.021(4) 0.039(4) 0.003(3) -0.006(4) 0.001(4)
C16 0.037(5) 0.025(4) 0.030(4) 0.000(3) -0.004(4) 0.001(3)
C19 0.033(4) 0.043(5) 0.045(5) -0.003(4) 0.010(4) 0.009(4)
C1 0.028(4) 0.024(4) 0.032(4) 0.000(3) -0.004(3) 0.003(3)
N5 0.030(4) 0.055(5) 0.057(5) -0.018(5) 0.000(4) 0.007(4)
C7 0.036(4) 0.039(4) 0.039(4) -0.002(4) 0.009(4) 0.010(4)
C17 0.054(5) 0.030(4) 0.037(4) 0.006(3) -0.001(4) 0.004(4)
C14 0.053(5) 0.031(4) 0.045(5) -0.003(4) -0.002(5) 0.006(4)
C3 0.041(4) 0.023(4) 0.054(5) 0.004(4) 0.006(4) -0.001(3)
C13 0.065(6) 0.021(4) 0.062(6) -0.001(4) -0.008(5) -0.002(4)
C8 0.042(5) 0.044(5) 0.044(5) 0.008(4) 0.011(4) 0.004(4)
C12 0.055(5) 0.022(4) 0.058(6) 0.004(4) -0.012(5) -0.013(4)
C6 0.035(4) 0.030(4) 0.042(5) 0.003(4) -0.004(4) 0.000(4)
C4 0.055(6) 0.019(4) 0.067(6) 0.000(4) -0.006(5) 0.015(4)
C9 0.033(4) 0.053(5) 0.052(6) 0.012(5) 0.008(4) -0.002(4)
C5 0.040(5) 0.032(4) 0.062(6) -0.001(4) 0.006(5) 0.013(4)
C20 0.054(6) 0.051(6) 0.070(7) -0.008(5) -0.007(6) 0.016(5)
C18 0.054(6) 0.037(5) 0.073(7) -0.002(5) 0.023(5) -0.010(5)
O6 0.039(3) 0.043(3) 0.066(4) 0.002(3) 0.003(3) -0.002(3)
O7 0.048(4) 0.080(5) 0.065(5) 0.030(4) 0.002(4) -0.016(4)
O11 0.082(5) 0.105(7) 0.045(4) -0.027(4) -0.018(4) 0.041(5)
N3 0.032(4) 0.065(5) 0.045(4) -0.011(4) 0.007(4) -0.012(4)
O5 0.037(4) 0.131(7) 0.081(5) -0.005(6) 0.003(4) -0.020(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'
Eu Eu -0.1578 3.6682 '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 Eu O2 64.89(18) . . ?
O1 Eu O10 123.0(2) . . ?
O2 Eu O10 114.9(2) . . ?
O1 Eu O6 140.6(2) . . ?
O2 Eu O6 113.3(2) . . ?
O10 Eu O6 94.3(2) . . ?
O1 Eu O13 73.8(2) . . ?
O2 Eu O13 114.10(19) . . ?
O10 Eu O13 130.5(2) . . ?
O6 Eu O13 72.0(2) . . ?
O1 Eu O9 80.7(2) . . ?
O2 Eu O9 72.3(2) . . ?
O10 Eu O9 50.9(2) . . ?
O6 Eu O9 138.1(2) . . ?
O13 Eu O9 146.5(2) . . ?
O1 Eu O12 74.9(2) . . ?
O2 Eu O12 70.1(2) . . ?
O10 Eu O12 162.0(2) . . ?
O6 Eu O12 68.4(2) . . ?
O13 Eu O12 50.4(2) . . ?
O9 Eu O12 141.2(2) . . ?
O1 Eu O7 131.8(2) . . ?
O2 Eu O7 162.1(2) . . ?
O10 Eu O7 64.3(2) . . ?
O6 Eu O7 50.6(2) . . ?
O13 Eu O7 71.1(2) . . ?
O9 Eu O7 113.5(2) . . ?
O12 Eu O7 105.3(2) . . ?
O1 Eu O3 61.70(17) . . ?
O2 Eu O3 121.65(17) . . ?
O10 Eu O3 78.1(2) . . ?
O6 Eu O3 122.44(19) . . ?
O13 Eu O3 71.32(19) . . ?
O9 Eu O3 77.6(2) . . ?
O12 Eu O3 114.8(2) . . ?
O7 Eu O3 76.2(2) . . ?
O1 Eu O4 125.22(17) . . ?
O2 Eu O4 60.43(17) . . ?
O10 Eu O4 79.4(2) . . ?
O6 Eu O4 69.34(18) . . ?
O13 Eu O4 132.37(19) . . ?
O9 Eu O4 80.4(2) . . ?
O12 Eu O4 89.5(2) . . ?
O7 Eu O4 102.9(2) . . ?
O3 Eu O4 155.3(2) . . ?
O1 Eu N4 101.18(19) . . ?
O2 Eu N4 94.1(2) . . ?
O10 Eu N4 25.9(2) . . ?
O6 Eu N4 118.0(2) . . ?
O13 Eu N4 144.2(2) . . ?
O9 Eu N4 25.07(19) . . ?
O12 Eu N4 164.0(2) . . ?
O7 Eu N4 89.0(2) . . ?
O3 Eu N4 75.2(2) . . ?
O4 Eu N4 80.1(2) . . ?
O1 Eu N5 71.93(19) . . ?
O2 Eu N5 92.1(2) . . ?
O10 Eu N5 152.5(2) . . ?
O6 Eu N5 68.8(2) . . ?
O13 Eu N5 24.9(2) . . ?
O9 Eu N5 152.4(2) . . ?
O12 Eu N5 25.5(2) . . ?
O7 Eu N5 88.4(2) . . ?
O3 Eu N5 92.5(2) . . ?
O4 Eu N5 112.2(2) . . ?
N4 Eu N5 167.7(2) . . ?
C1 O1 Cu 123.9(5) . . ?
C1 O1 Eu 128.5(5) . . ?
Cu O1 Eu 106.1(2) . . ?
O2 Cu N2 95.7(3) . . ?
O2 Cu O1 84.5(2) . . ?
N2 Cu O1 177.7(3) . . ?
O2 Cu N1 172.6(3) . . ?
N2 Cu N1 85.7(3) . . ?
O1 Cu N1 94.4(3) . . ?
O2 Cu Eu 43.14(16) . . ?
N2 Cu Eu 138.8(2) . . ?
O1 Cu Eu 41.44(16) . . ?
N1 Cu Eu 134.9(2) . . ?
C16 O2 Cu 125.2(5) . . ?
C16 O2 Eu 130.3(5) . . ?
Cu O2 Eu 104.4(2) . . ?
C10 N2 C9 121.8(7) . . ?
C10 N2 Cu 125.2(6) . . ?
C9 N2 Cu 112.8(5) . . ?
N4 O10 Eu 97.5(4) . . ?
C7 N1 C8 123.3(8) . . ?
C7 N1 Cu 125.3(6) . . ?
C8 N1 Cu 111.4(6) . . ?
O8 N4 O9 122.8(8) . . ?
O8 N4 O10 122.1(8) . . ?
O9 N4 O10 115.1(7) . . ?
O8 N4 Eu 174.6(7) . . ?
O9 N4 Eu 58.7(4) . . ?
O10 N4 Eu 56.6(4) . . ?
N4 O9 Eu 96.3(5) . . ?
C15 O4 C19 117.3(6) . . ?
C15 O4 Eu 119.6(4) . . ?
C19 O4 Eu 123.1(5) . . ?
C2 O3 C17 117.8(6) . . ?
C2 O3 Eu 118.5(4) . . ?
C17 O3 Eu 123.5(4) . . ?
O3 C2 C3 125.4(7) . . ?
O3 C2 C1 113.8(7) . . ?
C3 C2 C1 120.8(8) . . ?
N5 O13 Eu 97.5(5) . . ?
N5 O12 Eu 95.0(5) . . ?
O4 C15 C14 126.2(8) . . ?
O4 C15 C16 114.7(6) . . ?
C14 C15 C16 119.2(8) . . ?
N2 C10 C11 125.6(8) . . ?
C16 C11 C12 118.2(8) . . ?
C16 C11 C10 123.5(7) . . ?
C12 C11 C10 118.4(8) . . ?
O2 C16 C11 124.6(8) . . ?
O2 C16 C15 114.8(7) . . ?
C11 C16 C15 120.5(7) . . ?
O4 C19 C20 111.6(7) . . ?
O1 C1 C2 116.8(7) . . ?
O1 C1 C6 123.6(7) . . ?
C2 C1 C6 119.5(7) . . ?
O11 N5 O13 122.6(9) . . ?
O11 N5 O12 120.4(10) . . ?
O13 N5 O12 117.0(8) . . ?
O11 N5 Eu 179.0(6) . . ?
O13 N5 Eu 57.6(4) . . ?
O12 N5 Eu 59.4(4) . . ?
N1 C7 C6 125.1(8) . . ?
O3 C17 C18 112.3(7) . . ?
C15 C14 C13 120.0(9) . . ?
C2 C3 C4 119.4(8) . . ?
C12 C13 C14 119.8(8) . . ?
N1 C8 C9 107.3(7) . . ?
C13 C12 C11 122.2(8) . . ?
C5 C6 C1 118.1(8) . . ?
C5 C6 C7 118.9(8) . . ?
C1 C6 C7 122.9(7) . . ?
C5 C4 C3 121.1(8) . . ?
N2 C9 C8 107.5(7) . . ?
C4 C5 C6 120.9(8) . . ?
N3 O6 Eu 98.6(5) . . ?
N3 O7 Eu 94.5(5) . . ?
O5 N3 O7 122.1(9) . . ?
O5 N3 O6 121.5(10) . . ?
O7 N3 O6 116.4(7) . . ?
O5 N3 Eu 177.7(8) . . ?
O7 N3 Eu 60.1(4) . . ?
O6 N3 Eu 56.3(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
Eu O1 2.350(5) . ?
Eu O2 2.409(5) . ?
Eu O10 2.456(6) . ?
Eu O6 2.485(6) . ?
Eu O13 2.501(6) . ?
Eu O9 2.506(6) . ?
Eu O12 2.538(6) . ?
Eu O7 2.570(6) . ?
Eu O3 2.600(5) . ?
Eu O4 2.655(5) . ?
Eu N4 2.917(7) . ?
Eu N5 2.936(9) . ?
O1 C1 1.325(9) . ?
O1 Cu 1.908(5) . ?
Cu O2 1.891(6) . ?
Cu N2 1.907(7) . ?
Cu N1 1.908(7) . ?
O2 C16 1.345(9) . ?
N2 C10 1.274(11) . ?
N2 C9 1.478(12) . ?
O10 N4 1.286(9) . ?
N1 C7 1.278(10) . ?
N1 C8 1.471(11) . ?
N4 O8 1.209(9) . ?
N4 O9 1.243(9) . ?
O4 C15 1.376(9) . ?
O4 C19 1.451(9) . ?
O3 C2 1.379(10) . ?
O3 C17 1.469(9) . ?
C2 C3 1.382(11) . ?
C2 C1 1.393(11) . ?
O13 N5 1.247(11) . ?
O12 N5 1.270(11) . ?
C15 C14 1.394(11) . ?
C15 C16 1.417(12) . ?
C10 C11 1.463(12) . ?
C11 C16 1.378(11) . ?
C11 C12 1.416(11) . ?
C19 C20 1.504(13) . ?
C1 C6 1.422(12) . ?
N5 O11 1.220(10) . ?
C7 C6 1.451(12) . ?
C17 C18 1.508(13) . ?
C14 C13 1.400(13) . ?
C3 C4 1.395(12) . ?
C13 C12 1.346(13) . ?
C8 C9 1.516(13) . ?
C6 C5 1.410(11) . ?
C4 C5 1.358(13) . ?
O6 N3 1.271(10) . ?
O7 N3 1.271(10) . ?
N3 O5 1.204(9) . ?
|
1100949.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100949.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_1100949
loop_
_publ_author_name
'Rajesh Koner'
'Hsin-Huang Lin'
'Ho-Hsiang Wei'
'Sasankasekhar Mohanta'
_publ_section_title
;
Syntheses, Structures, and Magnetic Properties of Diphenoxo-Bridged
MIILnIII Complexes Derived from N,N'-Ethylenebis(3-ethoxysalicylaldiimine)
(M = Cu or Ni; Ln = Ce-Yb): Observation of Surprisingly Strong Exchange
Interactions
;
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3524
_journal_page_last 3536
_journal_paper_doi 10.1021/ic048196h
_journal_volume 44
_journal_year 2005
_chemical_formula_sum 'C20 H22 Cu N5 O13 Tb'
_chemical_formula_weight 762.89
_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 8.611(3)
_cell_length_b 13.814(5)
_cell_length_c 21.244(6)
_cell_measurement_temperature 293(2)
_cell_volume 2527.0(15)
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 293(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 0.0000
_diffrn_reflns_av_sigmaI/netI 0.0377
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -1
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min -1
_diffrn_reflns_limit_l_max 25
_diffrn_reflns_limit_l_min -1
_diffrn_reflns_number 2543
_diffrn_reflns_theta_full 24.98
_diffrn_reflns_theta_max 24.98
_diffrn_reflns_theta_min 1.92
_exptl_absorpt_coefficient_mu 3.695
_exptl_crystal_colour Red
_exptl_crystal_density_diffrn 2.005
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1500
_exptl_crystal_size_max 55
_exptl_crystal_size_mid 38
_exptl_crystal_size_min 22
_refine_diff_density_max 0.679
_refine_diff_density_min -0.948
_refine_diff_density_rms 0.129
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack -0.01(3)
_refine_ls_extinction_coef 0.00057(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 1.159
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 362
_refine_ls_number_reflns 2543
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.159
_refine_ls_R_factor_all 0.0393
_refine_ls_R_factor_gt 0.0289
_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^)+(0.0234P)^2^+6.0316P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0670
_refine_ls_wR_factor_ref 0.0809
_reflns_number_gt 2260
_reflns_number_total 2543
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file ic048196hsi20050224_082436_04.cif
_cod_data_source_block cutb
_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 2527.1(14)
_cod_database_code 1100949
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
Tb Tb 0.76036(4) 0.00144(3) 0.099217(17) 0.02796(13) Uani 1 1 d . . .
Cu Cu 0.43712(13) -0.05640(8) 0.18330(6) 0.0346(3) Uani 1 1 d . . .
O10 O 0.7837(8) 0.0080(6) -0.0155(3) 0.0488(17) Uani 1 1 d . . .
N4 N 0.6419(10) -0.0074(7) -0.0285(4) 0.045(2) Uani 1 1 d . . .
O12 O 0.8185(10) -0.0358(6) 0.2119(4) 0.050(2) Uani 1 1 d . . .
O8 O 0.5937(11) -0.0039(7) -0.0813(4) 0.070(2) Uani 1 1 d . . .
O1 O 0.5437(7) 0.0564(4) 0.1547(3) 0.0305(14) Uani 1 1 d . . .
O9 O 0.5562(8) -0.0262(6) 0.0183(4) 0.055(2) Uani 1 1 d . . .
N1 N 0.3012(9) 0.0136(6) 0.2382(4) 0.0366(18) Uani 1 1 d . . .
O4 O 0.8190(7) -0.1820(4) 0.0702(3) 0.0375(16) Uani 1 1 d . . .
O3 O 0.6635(7) 0.1759(4) 0.0759(3) 0.0317(14) Uani 1 1 d . . .
O2 O 0.5933(8) -0.1233(4) 0.1367(3) 0.0387(17) Uani 1 1 d . . .
C6 C 0.3563(11) 0.1719(7) 0.1949(5) 0.033(2) Uani 1 1 d . . .
C2 C 0.5447(11) 0.2123(6) 0.1141(5) 0.034(2) Uani 1 1 d . . .
N2 N 0.3258(10) -0.1698(6) 0.2087(4) 0.037(2) Uani 1 1 d . . .
C18 C 0.8497(13) 0.3096(7) 0.0590(5) 0.048(3) Uani 1 1 d . . .
H18A H 0.8940 0.3500 0.0269 0.072 Uiso 1 1 calc R . .
H18B H 0.9308 0.2739 0.0796 0.072 Uiso 1 1 calc R . .
H18C H 0.7968 0.3493 0.0893 0.072 Uiso 1 1 calc R . .
C15 C 0.7181(12) -0.2541(6) 0.0903(4) 0.033(2) Uani 1 1 d . . .
C10 C 0.3556(11) -0.2562(7) 0.1908(5) 0.036(2) Uani 1 1 d . . .
H10A H 0.2896 -0.3049 0.2048 0.044 Uiso 1 1 calc R . .
N3 N 1.0962(10) 0.0313(7) 0.0817(4) 0.045(2) Uani 1 1 d . . .
O6 O 1.0362(8) -0.0370(5) 0.1119(4) 0.0491(18) Uani 1 1 d . . .
C7 C 0.2793(11) 0.1058(7) 0.2374(5) 0.036(2) Uani 1 1 d . . .
H7A H 0.2091 0.1316 0.2661 0.044 Uiso 1 1 calc R . .
O13 O 0.8625(8) 0.1106(5) 0.1824(4) 0.0451(17) Uani 1 1 d . . .
C11 C 0.4854(11) -0.2847(6) 0.1501(5) 0.034(2) Uani 1 1 d . . .
C16 C 0.5952(11) -0.2191(6) 0.1261(5) 0.033(2) Uani 1 1 d . . .
O7 O 0.9999(9) 0.0920(6) 0.0583(4) 0.060(2) Uani 1 1 d . . .
O11 O 0.8993(10) 0.0718(7) 0.2803(4) 0.074(3) Uani 1 1 d . . .
C1 C 0.4838(10) 0.1454(6) 0.1555(5) 0.031(2) Uani 1 1 d . . .
C14 C 0.7296(13) -0.3518(7) 0.0751(5) 0.044(2) Uani 1 1 d . . .
H14A H 0.8125 -0.3739 0.0510 0.053 Uiso 1 1 calc R . .
C17 C 0.7359(12) 0.2400(6) 0.0296(4) 0.040(2) Uani 1 1 d . . .
H17A H 0.6556 0.2765 0.0081 0.048 Uiso 1 1 calc R . .
H17B H 0.7896 0.2011 -0.0016 0.048 Uiso 1 1 calc R . .
C3 C 0.4841(11) 0.3060(6) 0.1094(5) 0.039(2) Uani 1 1 d . . .
H3A H 0.5232 0.3492 0.0798 0.047 Uiso 1 1 calc R . .
C19 C 0.9568(11) -0.2126(8) 0.0340(5) 0.042(2) Uani 1 1 d . . .
H19A H 0.9990 -0.1573 0.0117 0.051 Uiso 1 1 calc R . .
H19B H 0.9261 -0.2605 0.0029 0.051 Uiso 1 1 calc R . .
C13 C 0.6155(13) -0.4170(7) 0.0962(5) 0.047(3) Uani 1 1 d . . .
H13A H 0.6213 -0.4822 0.0856 0.056 Uiso 1 1 calc R . .
C8 C 0.2233(12) -0.0526(7) 0.2832(4) 0.043(2) Uani 1 1 d . . .
H8A H 0.1275 -0.0239 0.2983 0.051 Uiso 1 1 calc R . .
H8B H 0.2902 -0.0650 0.3190 0.051 Uiso 1 1 calc R . .
C9 C 0.1888(12) -0.1475(7) 0.2481(5) 0.043(2) Uani 1 1 d . . .
H9A H 0.1703 -0.1994 0.2779 0.052 Uiso 1 1 calc R . .
H9B H 0.0973 -0.1402 0.2219 0.052 Uiso 1 1 calc R . .
C12 C 0.4984(14) -0.3839(7) 0.1317(5) 0.047(3) Uani 1 1 d . . .
H12A H 0.4225 -0.4272 0.1449 0.056 Uiso 1 1 calc R . .
C20 C 1.0810(14) -0.2552(9) 0.0762(6) 0.060(3) Uani 1 1 d . . .
H20A H 1.1686 -0.2743 0.0511 0.090 Uiso 1 1 calc R . .
H20B H 1.0401 -0.3107 0.0977 0.090 Uiso 1 1 calc R . .
H20C H 1.1130 -0.2076 0.1064 0.090 Uiso 1 1 calc R . .
N5 N 0.8603(10) 0.0494(8) 0.2259(5) 0.046(2) Uani 1 1 d . . .
C4 C 0.3637(13) 0.3339(7) 0.1499(6) 0.050(3) Uani 1 1 d . . .
H4A H 0.3257 0.3969 0.1484 0.060 Uiso 1 1 calc R . .
C5 C 0.3018(12) 0.2691(7) 0.1915(5) 0.041(3) Uani 1 1 d . . .
H5A H 0.2222 0.2889 0.2182 0.049 Uiso 1 1 calc R . .
O5 O 1.2365(8) 0.0407(8) 0.0762(4) 0.080(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
Tb 0.02471(19) 0.0247(2) 0.0344(2) 0.0023(2) 0.00377(16) -0.0010(2)
Cu 0.0297(6) 0.0256(5) 0.0487(6) 0.0034(5) 0.0100(6) -0.0018(5)
O10 0.050(4) 0.053(4) 0.044(4) 0.000(4) 0.003(3) -0.010(5)
N4 0.057(5) 0.033(4) 0.044(5) 0.000(5) -0.001(4) -0.006(5)
O12 0.052(5) 0.051(5) 0.048(4) 0.016(4) 0.001(4) 0.003(4)
O8 0.095(6) 0.061(5) 0.055(5) 0.000(5) -0.023(5) -0.013(6)
O1 0.024(3) 0.023(3) 0.044(3) 0.006(3) 0.007(3) 0.004(3)
O9 0.038(4) 0.065(5) 0.063(4) 0.000(4) 0.001(4) -0.008(4)
N1 0.033(4) 0.036(4) 0.041(4) 0.002(4) 0.006(3) 0.001(4)
O4 0.027(3) 0.029(3) 0.056(4) -0.001(3) 0.010(3) 0.001(3)
O3 0.038(3) 0.025(3) 0.033(3) 0.002(3) 0.004(3) 0.000(3)
O2 0.035(4) 0.021(3) 0.060(4) 0.006(3) 0.008(3) 0.001(3)
C6 0.029(5) 0.034(5) 0.037(6) -0.007(4) -0.015(5) 0.005(4)
C2 0.024(5) 0.024(4) 0.054(6) -0.003(4) -0.006(5) -0.003(4)
N2 0.031(4) 0.037(4) 0.044(5) 0.010(4) 0.008(4) -0.007(4)
C18 0.048(6) 0.038(6) 0.058(7) 0.001(5) 0.005(5) -0.013(5)
C15 0.039(5) 0.028(4) 0.032(5) -0.002(4) -0.006(4) 0.007(4)
C10 0.028(5) 0.029(5) 0.052(7) 0.012(5) -0.003(5) -0.008(4)
N3 0.032(4) 0.055(6) 0.048(5) -0.011(4) 0.005(4) -0.006(4)
O6 0.037(4) 0.042(4) 0.068(5) 0.009(4) 0.005(4) 0.001(3)
C7 0.023(4) 0.044(5) 0.043(5) 0.001(5) 0.000(4) 0.005(4)
O13 0.050(4) 0.036(4) 0.049(4) -0.001(4) -0.005(4) 0.002(3)
C11 0.036(5) 0.024(4) 0.041(5) 0.006(4) -0.010(5) -0.010(4)
C16 0.030(5) 0.024(4) 0.044(5) 0.006(4) -0.006(5) -0.003(4)
O7 0.044(4) 0.064(5) 0.073(6) 0.023(5) -0.002(4) -0.013(4)
O11 0.071(6) 0.108(7) 0.044(4) -0.023(5) -0.016(4) 0.043(6)
C1 0.020(4) 0.023(4) 0.049(6) 0.003(4) -0.006(4) 0.002(4)
C14 0.046(6) 0.029(5) 0.057(6) -0.005(4) -0.008(6) 0.005(5)
C17 0.046(6) 0.030(4) 0.045(5) 0.008(4) 0.008(5) 0.003(5)
C3 0.034(5) 0.020(4) 0.063(7) 0.008(5) -0.012(5) 0.000(4)
C19 0.031(5) 0.043(5) 0.053(7) -0.004(5) 0.011(5) 0.009(5)
C13 0.060(7) 0.032(5) 0.049(6) -0.001(5) -0.004(6) -0.005(5)
C8 0.039(5) 0.043(5) 0.045(5) 0.009(5) 0.013(5) 0.000(5)
C9 0.033(5) 0.046(6) 0.050(6) 0.013(5) -0.003(5) -0.004(5)
C12 0.058(7) 0.026(5) 0.056(7) 0.008(5) -0.008(6) -0.015(5)
C20 0.044(6) 0.054(7) 0.083(9) -0.013(7) 0.000(6) 0.008(6)
N5 0.031(5) 0.059(6) 0.049(6) -0.008(5) 0.000(4) 0.021(5)
C4 0.044(6) 0.025(5) 0.081(8) 0.007(5) -0.003(6) 0.009(5)
C5 0.035(5) 0.037(5) 0.051(6) -0.009(5) 0.001(5) 0.013(4)
O5 0.027(4) 0.123(8) 0.090(6) -0.004(6) 0.011(4) -0.024(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'
Tb Tb -0.1723 4.1537 '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 Tb O2 65.4(2) . . ?
O1 Tb O10 123.8(2) . . ?
O2 Tb O10 114.2(3) . . ?
O1 Tb O6 142.2(2) . . ?
O2 Tb O6 113.1(2) . . ?
O10 Tb O6 92.2(2) . . ?
O1 Tb O13 74.1(2) . . ?
O2 Tb O13 114.6(2) . . ?
O10 Tb O13 131.0(3) . . ?
O6 Tb O13 73.1(2) . . ?
O1 Tb O9 80.5(2) . . ?
O2 Tb O9 72.1(2) . . ?
O10 Tb O9 51.4(2) . . ?
O6 Tb O9 136.7(2) . . ?
O13 Tb O9 146.6(2) . . ?
O1 Tb O12 75.1(2) . . ?
O2 Tb O12 69.6(3) . . ?
O10 Tb O12 160.9(3) . . ?
O6 Tb O12 69.9(3) . . ?
O13 Tb O12 51.1(2) . . ?
O9 Tb O12 140.5(3) . . ?
O1 Tb O7 130.9(3) . . ?
O2 Tb O7 162.2(2) . . ?
O10 Tb O7 65.0(3) . . ?
O6 Tb O7 50.4(2) . . ?
O13 Tb O7 70.1(3) . . ?
O9 Tb O7 114.1(2) . . ?
O12 Tb O7 105.3(3) . . ?
O1 Tb O3 62.5(2) . . ?
O2 Tb O3 122.8(2) . . ?
O10 Tb O3 78.6(2) . . ?
O6 Tb O3 122.3(2) . . ?
O13 Tb O3 71.7(2) . . ?
O9 Tb O3 77.5(2) . . ?
O12 Tb O3 116.0(2) . . ?
O7 Tb O3 75.0(2) . . ?
O1 Tb O4 125.4(2) . . ?
O2 Tb O4 60.2(2) . . ?
O10 Tb O4 77.8(3) . . ?
O6 Tb O4 68.5(2) . . ?
O13 Tb O4 132.6(2) . . ?
O9 Tb O4 80.1(2) . . ?
O12 Tb O4 89.3(2) . . ?
O7 Tb O4 103.5(2) . . ?
O3 Tb O4 154.3(2) . . ?
O1 Tb N4 101.9(2) . . ?
O2 Tb N4 94.0(2) . . ?
O10 Tb N4 25.7(2) . . ?
O6 Tb N4 115.8(3) . . ?
O13 Tb N4 144.6(3) . . ?
O9 Tb N4 25.7(2) . . ?
O12 Tb N4 163.3(3) . . ?
O7 Tb N4 89.2(3) . . ?
O3 Tb N4 75.4(2) . . ?
O4 Tb N4 79.0(3) . . ?
O1 Tb N5 72.2(2) . . ?
O2 Tb N5 92.0(3) . . ?
O10 Tb N5 152.9(3) . . ?
O6 Tb N5 70.1(2) . . ?
O13 Tb N5 25.4(3) . . ?
O9 Tb N5 152.3(2) . . ?
O12 Tb N5 25.7(3) . . ?
O7 Tb N5 88.0(3) . . ?
O3 Tb N5 93.5(2) . . ?
O4 Tb N5 112.1(3) . . ?
N4 Tb N5 168.9(3) . . ?
O1 Cu O2 83.8(3) . . ?
O1 Cu N2 177.7(3) . . ?
O2 Cu N2 95.9(3) . . ?
O1 Cu N1 94.3(3) . . ?
O2 Cu N1 172.4(3) . . ?
N2 Cu N1 86.3(4) . . ?
O1 Cu Tb 41.21(18) . . ?
O2 Cu Tb 42.68(18) . . ?
N2 Cu Tb 138.6(3) . . ?
N1 Cu Tb 134.5(2) . . ?
N4 O10 Tb 97.6(5) . . ?
O8 N4 O9 122.8(9) . . ?
O8 N4 O10 122.1(9) . . ?
O9 N4 O10 115.1(8) . . ?
O8 N4 Tb 175.2(9) . . ?
O9 N4 Tb 58.6(5) . . ?
O10 N4 Tb 56.7(4) . . ?
N5 O12 Tb 95.2(6) . . ?
C1 O1 Cu 124.3(5) . . ?
C1 O1 Tb 128.0(5) . . ?
Cu O1 Tb 106.2(3) . . ?
N4 O9 Tb 95.7(5) . . ?
C7 N1 C8 123.6(9) . . ?
C7 N1 Cu 125.5(7) . . ?
C8 N1 Cu 110.9(6) . . ?
C15 O4 C19 117.3(7) . . ?
C15 O4 Tb 119.5(5) . . ?
C19 O4 Tb 123.2(5) . . ?
C2 O3 C17 118.9(7) . . ?
C2 O3 Tb 117.2(5) . . ?
C17 O3 Tb 123.6(5) . . ?
C16 O2 Cu 124.9(6) . . ?
C16 O2 Tb 130.6(6) . . ?
Cu O2 Tb 104.4(3) . . ?
C5 C6 C1 117.7(9) . . ?
C5 C6 C7 118.5(9) . . ?
C1 C6 C7 123.8(8) . . ?
C1 C2 C3 121.6(9) . . ?
C1 C2 O3 114.0(8) . . ?
C3 C2 O3 124.3(9) . . ?
C10 N2 C9 121.6(9) . . ?
C10 N2 Cu 125.4(7) . . ?
C9 N2 Cu 112.9(6) . . ?
O4 C15 C16 113.3(7) . . ?
O4 C15 C14 125.4(9) . . ?
C16 C15 C14 121.2(10) . . ?
N2 C10 C11 125.4(9) . . ?
O5 N3 O6 122.5(10) . . ?
O5 N3 O7 122.3(10) . . ?
O6 N3 O7 115.2(8) . . ?
O5 N3 Tb 177.3(9) . . ?
O6 N3 Tb 54.9(4) . . ?
O7 N3 Tb 60.3(5) . . ?
N3 O6 Tb 100.4(6) . . ?
N1 C7 C6 124.5(9) . . ?
N5 O13 Tb 96.3(6) . . ?
C16 C11 C12 117.8(10) . . ?
C16 C11 C10 123.5(9) . . ?
C12 C11 C10 118.7(9) . . ?
O2 C16 C15 116.3(9) . . ?
O2 C16 C11 124.6(9) . . ?
C15 C16 C11 119.1(9) . . ?
N3 O7 Tb 94.0(5) . . ?
O1 C1 C2 117.6(8) . . ?
O1 C1 C6 122.8(8) . . ?
C2 C1 C6 119.6(8) . . ?
C15 C14 C13 119.8(10) . . ?
O3 C17 C18 112.7(8) . . ?
C2 C3 C4 119.1(9) . . ?
O4 C19 C20 111.7(9) . . ?
C12 C13 C14 119.1(9) . . ?
N1 C8 C9 107.6(8) . . ?
N2 C9 C8 107.3(8) . . ?
C13 C12 C11 122.7(10) . . ?
O11 N5 O13 120.9(11) . . ?
O11 N5 O12 121.8(11) . . ?
O13 N5 O12 117.3(9) . . ?
O11 N5 Tb 178.1(7) . . ?
O13 N5 Tb 58.3(5) . . ?
O12 N5 Tb 59.0(5) . . ?
C5 C4 C3 120.4(9) . . ?
C4 C5 C6 121.5(10) . . ?
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
Tb O1 2.334(6) . ?
Tb O2 2.381(6) . ?
Tb O10 2.446(6) . ?
Tb O6 2.449(7) . ?
Tb O13 2.484(7) . ?
Tb O9 2.488(7) . ?
Tb O12 2.499(8) . ?
Tb O7 2.565(7) . ?
Tb O3 2.598(6) . ?
Tb O4 2.657(6) . ?
Tb N4 2.901(8) . ?
Tb N5 2.902(10) . ?
Cu O1 1.908(6) . ?
Cu O2 1.909(7) . ?
Cu N2 1.915(8) . ?
Cu N1 1.915(8) . ?
O10 N4 1.270(10) . ?
N4 O8 1.197(10) . ?
N4 O9 1.265(10) . ?
O12 N5 1.266(12) . ?
O1 C1 1.333(10) . ?
N1 C7 1.287(12) . ?
N1 C8 1.483(12) . ?
O4 C15 1.389(11) . ?
O4 C19 1.476(11) . ?
O3 C2 1.400(11) . ?
O3 C17 1.463(10) . ?
O2 C16 1.342(10) . ?
C6 C5 1.424(13) . ?
C6 C1 1.428(14) . ?
C6 C7 1.445(14) . ?
C2 C1 1.380(13) . ?
C2 C3 1.399(12) . ?
N2 C10 1.278(12) . ?
N2 C9 1.478(13) . ?
C18 C17 1.508(14) . ?
C15 C16 1.390(14) . ?
C15 C14 1.391(12) . ?
C10 C11 1.467(14) . ?
N3 O5 1.221(11) . ?
N3 O6 1.253(11) . ?
N3 O7 1.280(11) . ?
O13 N5 1.253(12) . ?
C11 C16 1.406(13) . ?
C11 C12 1.429(13) . ?
O11 N5 1.243(11) . ?
C14 C13 1.406(14) . ?
C3 C4 1.400(15) . ?
C19 C20 1.515(15) . ?
C13 C12 1.340(15) . ?
C8 C9 1.536(14) . ?
C4 C5 1.367(15) . ?
|
1100950.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100950.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_1100950
loop_
_publ_author_name
'Rajesh Koner'
'Hsin-Huang Lin'
'Ho-Hsiang Wei'
'Sasankasekhar Mohanta'
_publ_section_title
;
Syntheses, Structures, and Magnetic Properties of Diphenoxo-Bridged
MIILnIII Complexes Derived from N,N'-Ethylenebis(3-ethoxysalicylaldiimine)
(M = Cu or Ni; Ln = Ce-Yb): Observation of Surprisingly Strong Exchange
Interactions
;
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3524
_journal_page_last 3536
_journal_paper_doi 10.1021/ic048196h
_journal_volume 44
_journal_year 2005
_chemical_formula_sum 'C20 H22 Cu Dy N5 O13'
_chemical_formula_weight 766.47
_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 8.5870(3)
_cell_length_b 13.7580(5)
_cell_length_c 21.1665(7)
_cell_measurement_reflns_used 6084
_cell_measurement_temperature 295(2)
_cell_measurement_theta_max 27.50
_cell_measurement_theta_min 1.77
_cell_volume 2500.61(15)
_computing_cell_refinement 'Bruker SAINT'
_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 295(2)
_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 0.0365
_diffrn_reflns_av_sigmaI/netI 0.0277
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_l_max 27
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_number 22294
_diffrn_reflns_theta_full 27.50
_diffrn_reflns_theta_max 27.50
_diffrn_reflns_theta_min 1.77
_diffrn_standards_decay_% 0
_exptl_absorpt_coefficient_mu 3.894
_exptl_absorpt_correction_T_max 0.4915
_exptl_absorpt_correction_T_min 0.2996
_exptl_absorpt_correction_type multi-scan
_exptl_crystal_colour orange
_exptl_crystal_density_diffrn 2.036
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 1504
_exptl_crystal_size_max 0.55
_exptl_crystal_size_mid 0.35
_exptl_crystal_size_min 0.08
_refine_diff_density_max 0.529
_refine_diff_density_min -0.568
_refine_diff_density_rms 0.066
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack -0.002(8)
_refine_ls_extinction_coef 0.00012(6)
_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 1.025
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 362
_refine_ls_number_reflns 5739
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.025
_refine_ls_R_factor_all 0.0264
_refine_ls_R_factor_gt 0.0205
_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^)+(0.0220P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0441
_refine_ls_wR_factor_ref 0.0452
_reflns_number_gt 5040
_reflns_number_total 5739
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file ic048196hsi20050224_082436_05.cif
_cod_data_source_block CuDy
_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
The following automatic conversions were performed:
'_exptl_crystal_density_meas' value 'not_measured' 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_database_code 1100950
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
Dy Dy 0.260295(13) 0.498402(11) 0.900252(6) 0.02929(4) Uani 1 1 d . . .
Cu Cu -0.06242(4) 0.55644(3) 0.81672(2) 0.03509(10) Uani 1 1 d . . .
O3 O 0.1650(2) 0.32448(14) 0.92353(11) 0.0340(5) Uani 1 1 d . . .
O1 O 0.0447(2) 0.44342(15) 0.84483(10) 0.0332(5) Uani 1 1 d . . .
O2 O 0.0933(3) 0.62358(15) 0.86313(11) 0.0378(6) Uani 1 1 d . . .
O4 O 0.3207(2) 0.68166(15) 0.92990(11) 0.0373(5) Uani 1 1 d . . .
O10 O 0.2860(3) 0.4929(2) 1.01416(11) 0.0491(6) Uani 1 1 d . . .
O9 O 0.0570(3) 0.52516(18) 0.98102(12) 0.0533(7) Uani 1 1 d . . .
O8 O 0.0946(4) 0.5044(2) 1.08132(13) 0.0717(8) Uani 1 1 d . . .
O13 O 0.3617(3) 0.38942(17) 0.81756(13) 0.0457(6) Uani 1 1 d . . .
O12 O 0.3187(3) 0.5357(2) 0.78733(12) 0.0492(7) Uani 1 1 d . . .
O11 O 0.3992(4) 0.4292(3) 0.71906(14) 0.0763(10) Uani 1 1 d . . .
O6 O 0.5358(3) 0.53629(17) 0.88649(13) 0.0488(6) Uani 1 1 d . . .
O7 O 0.5010(3) 0.4078(2) 0.94144(14) 0.0606(8) Uani 1 1 d . . .
O5 O 0.7347(3) 0.4597(3) 0.92359(15) 0.0816(9) Uani 1 1 d . . .
N1 N -0.1992(3) 0.48620(19) 0.76176(13) 0.0366(6) Uani 1 1 d . . .
N2 N -0.1733(3) 0.6703(2) 0.79153(14) 0.0368(7) Uani 1 1 d . . .
N4 N 0.1433(3) 0.5077(2) 1.02757(15) 0.0456(7) Uani 1 1 d . . .
N5 N 0.3607(3) 0.4499(3) 0.77360(17) 0.0468(8) Uani 1 1 d . . .
N3 N 0.5953(3) 0.4677(2) 0.91775(15) 0.0447(8) Uani 1 1 d . . .
C18 C 0.3519(4) 0.1907(3) 0.9410(2) 0.0545(11) Uani 1 1 d . . .
H18A H 0.3954 0.1498 0.9733 0.082 Uiso 1 1 calc R . .
H18B H 0.4337 0.2269 0.9210 0.082 Uiso 1 1 calc R . .
H18C H 0.3002 0.1511 0.9101 0.082 Uiso 1 1 calc R . .
C17 C 0.2361(4) 0.2602(2) 0.97036(15) 0.0412(8) Uani 1 1 d . . .
H17A H 0.1550 0.2232 0.9913 0.049 Uiso 1 1 calc R . .
H17B H 0.2885 0.2992 1.0021 0.049 Uiso 1 1 calc R . .
C2 C 0.0454(4) 0.2872(2) 0.88667(16) 0.0307(7) Uani 1 1 d . . .
C3 C -0.0146(4) 0.1936(2) 0.89059(19) 0.0397(8) Uani 1 1 d . . .
H3A H 0.0258 0.1494 0.9195 0.048 Uiso 1 1 calc R . .
C4 C -0.1368(4) 0.1665(3) 0.85032(19) 0.0492(10) Uani 1 1 d . . .
H4A H -0.1764 0.1036 0.8523 0.059 Uiso 1 1 calc R . .
C5 C -0.1982(4) 0.2308(2) 0.8084(2) 0.0444(9) Uani 1 1 d . . .
H5A H -0.2774 0.2107 0.7814 0.053 Uiso 1 1 calc R . .
C6 C -0.1438(4) 0.3277(2) 0.80505(17) 0.0355(8) Uani 1 1 d . . .
C1 C -0.0176(3) 0.3549(2) 0.84401(15) 0.0288(7) Uani 1 1 d . . .
C7 C -0.2209(3) 0.3949(2) 0.76259(16) 0.0370(7) Uani 1 1 d . . .
H7A H -0.2916 0.3692 0.7338 0.044 Uiso 1 1 calc R . .
C8 C -0.2760(4) 0.5526(3) 0.71713(16) 0.0437(8) Uani 1 1 d . . .
H8A H -0.3717 0.5238 0.7016 0.052 Uiso 1 1 calc R . .
H8B H -0.2083 0.5653 0.6814 0.052 Uiso 1 1 calc R . .
C9 C -0.3113(4) 0.6473(3) 0.75228(19) 0.0438(9) Uani 1 1 d . . .
H9A H -0.3310 0.6993 0.7224 0.053 Uiso 1 1 calc R . .
H9B H -0.4027 0.6394 0.7788 0.053 Uiso 1 1 calc R . .
C10 C -0.1432(4) 0.7570(2) 0.80943(18) 0.0371(8) Uani 1 1 d . . .
H10A H -0.2085 0.8062 0.7951 0.044 Uiso 1 1 calc R . .
C11 C -0.0141(4) 0.7848(2) 0.85063(17) 0.0355(8) Uani 1 1 d . . .
C12 C -0.0012(4) 0.8841(2) 0.86727(18) 0.0445(9) Uani 1 1 d . . .
H12A H -0.0752 0.9282 0.8529 0.053 Uiso 1 1 calc R . .
C13 C 0.1184(4) 0.9156(2) 0.90406(19) 0.0487(9) Uani 1 1 d . . .
H13A H 0.1243 0.9809 0.9152 0.058 Uiso 1 1 calc R . .
C14 C 0.2323(4) 0.8512(2) 0.92534(17) 0.0423(8) Uani 1 1 d . . .
H14A H 0.3152 0.8736 0.9495 0.051 Uiso 1 1 calc R . .
C15 C 0.2210(4) 0.7543(2) 0.91034(15) 0.0327(7) Uani 1 1 d . . .
C16 C 0.0953(4) 0.7190(2) 0.87351(16) 0.0315(8) Uani 1 1 d . . .
C19 C 0.4566(4) 0.7122(3) 0.96567(17) 0.0433(9) Uani 1 1 d . . .
H19A H 0.4986 0.6567 0.9883 0.052 Uiso 1 1 calc R . .
H19B H 0.4255 0.7604 0.9966 0.052 Uiso 1 1 calc R . .
C20 C 0.5809(5) 0.7542(3) 0.9242(2) 0.0571(11) Uani 1 1 d . . .
H20A H 0.6684 0.7731 0.9496 0.086 Uiso 1 1 calc R . .
H20B H 0.5407 0.8101 0.9025 0.086 Uiso 1 1 calc R . .
H20C H 0.6133 0.7064 0.8939 0.086 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
Dy 0.02809(6) 0.02553(6) 0.03426(7) 0.00209(7) -0.00386(6) 0.00071(8)
Cu 0.03439(19) 0.02681(18) 0.0441(2) 0.00394(18) -0.01088(19) 0.00153(15)
O3 0.0383(12) 0.0254(11) 0.0384(14) 0.0069(10) -0.0059(10) 0.0012(9)
O1 0.0309(11) 0.0242(10) 0.0445(13) 0.0062(10) -0.0077(10) -0.0009(9)
O2 0.0386(13) 0.0222(10) 0.0528(16) 0.0005(10) -0.0124(11) 0.0021(9)
O4 0.0346(12) 0.0302(12) 0.0470(15) -0.0007(10) -0.0069(10) -0.0020(9)
O10 0.0486(12) 0.0539(15) 0.0447(14) 0.0001(13) -0.0065(10) 0.0056(15)
O9 0.0444(13) 0.068(2) 0.0476(15) -0.0013(13) -0.0031(12) 0.0053(12)
O8 0.103(2) 0.0682(18) 0.0438(16) 0.0009(17) 0.0208(15) 0.022(2)
O13 0.0490(14) 0.0393(13) 0.0487(16) -0.0033(13) 0.0048(13) -0.0018(10)
O12 0.0501(16) 0.0526(16) 0.0450(16) 0.0133(12) -0.0041(13) -0.0051(12)
O11 0.081(2) 0.108(3) 0.0403(17) -0.0206(17) 0.0165(15) -0.0423(19)
O6 0.0373(13) 0.0429(13) 0.0664(18) 0.0021(12) -0.0084(13) 0.0011(10)
O7 0.0496(16) 0.074(2) 0.0588(19) 0.0246(16) -0.0017(14) 0.0167(14)
O5 0.0332(14) 0.123(3) 0.089(2) -0.006(2) -0.0086(14) 0.0188(15)
N1 0.0343(11) 0.0398(16) 0.0357(15) 0.0050(13) -0.0049(11) -0.0030(11)
N2 0.0322(15) 0.0360(15) 0.0422(19) 0.0102(13) -0.0012(13) 0.0054(12)
N4 0.0647(18) 0.0301(15) 0.0418(18) -0.0008(17) 0.0023(14) 0.0029(17)
N5 0.0332(16) 0.057(2) 0.050(2) -0.0060(19) -0.0017(14) -0.0169(15)
N3 0.0337(15) 0.058(2) 0.0426(18) -0.0089(14) -0.0028(14) 0.0087(13)
C18 0.055(2) 0.036(2) 0.072(3) -0.0025(19) -0.018(2) 0.0106(16)
C17 0.056(2) 0.0328(16) 0.0351(19) 0.0090(13) -0.0096(18) 0.0012(16)
C2 0.0300(16) 0.0274(15) 0.035(2) -0.0014(13) 0.0041(15) 0.0019(12)
C3 0.0385(17) 0.0277(16) 0.053(2) 0.0065(16) 0.0043(18) -0.0006(12)
C4 0.050(2) 0.0263(17) 0.071(3) 0.0023(18) -0.0023(19) -0.0120(15)
C5 0.0394(19) 0.0341(17) 0.060(3) -0.0054(17) -0.0063(19) -0.0102(14)
C6 0.0351(18) 0.0328(17) 0.039(2) 0.0007(15) 0.0003(16) -0.0042(13)
C1 0.0275(15) 0.0261(15) 0.0327(18) 0.0000(12) 0.0041(13) 0.0005(11)
C7 0.0295(16) 0.0436(18) 0.0379(19) -0.0015(15) -0.0001(15) -0.0067(14)
C8 0.0395(18) 0.0467(19) 0.045(2) 0.0138(16) -0.0101(16) -0.0037(16)
C9 0.0351(17) 0.049(2) 0.048(2) 0.0131(17) -0.0103(17) 0.0044(14)
C10 0.0366(19) 0.0346(18) 0.040(2) 0.0114(16) 0.0052(17) 0.0109(14)
C11 0.0387(18) 0.0291(16) 0.039(2) 0.0072(14) 0.0072(15) 0.0055(13)
C12 0.057(2) 0.0250(16) 0.051(2) 0.0031(15) 0.0041(18) 0.0114(15)
C13 0.067(2) 0.0232(16) 0.056(3) -0.0047(16) 0.014(2) -0.0016(14)
C14 0.051(2) 0.0319(16) 0.044(2) -0.0038(14) 0.0038(18) -0.0051(15)
C15 0.0370(16) 0.0274(14) 0.0337(18) 0.0028(12) 0.0050(14) -0.0015(12)
C16 0.0391(19) 0.0235(15) 0.0321(19) 0.0025(13) 0.0032(15) 0.0001(12)
C19 0.0375(18) 0.0443(19) 0.048(2) -0.0055(16) -0.0097(17) -0.0061(15)
C20 0.050(2) 0.049(2) 0.072(3) -0.008(2) 0.002(2) -0.0135(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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 '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 Dy O2 65.61(7) . . ?
O1 Dy O10 124.48(8) . . ?
O2 Dy O10 114.01(9) . . ?
O1 Dy O6 141.58(8) . . ?
O2 Dy O6 113.02(8) . . ?
O10 Dy O6 92.13(9) . . ?
O1 Dy O13 73.99(8) . . ?
O2 Dy O13 114.82(8) . . ?
O10 Dy O13 130.99(9) . . ?
O6 Dy O13 72.69(8) . . ?
O1 Dy O9 80.47(8) . . ?
O2 Dy O9 72.20(8) . . ?
O10 Dy O9 51.71(8) . . ?
O6 Dy O9 137.38(9) . . ?
O13 Dy O9 146.29(8) . . ?
O1 Dy O12 75.10(8) . . ?
O2 Dy O12 69.84(9) . . ?
O10 Dy O12 160.30(9) . . ?
O6 Dy O12 69.32(9) . . ?
O13 Dy O12 51.21(9) . . ?
O9 Dy O12 140.72(9) . . ?
O1 Dy O7 131.04(9) . . ?
O2 Dy O7 161.97(8) . . ?
O10 Dy O7 64.75(9) . . ?
O6 Dy O7 50.45(8) . . ?
O13 Dy O7 70.19(9) . . ?
O9 Dy O7 113.98(8) . . ?
O12 Dy O7 105.26(9) . . ?
O1 Dy O3 62.63(7) . . ?
O2 Dy O3 123.04(7) . . ?
O10 Dy O3 79.02(8) . . ?
O6 Dy O3 121.94(7) . . ?
O13 Dy O3 71.51(8) . . ?
O9 Dy O3 77.39(8) . . ?
O12 Dy O3 115.96(8) . . ?
O7 Dy O3 74.91(8) . . ?
O1 Dy O4 125.91(7) . . ?
O2 Dy O4 60.42(7) . . ?
O10 Dy O4 77.07(9) . . ?
O6 Dy O4 68.61(7) . . ?
O13 Dy O4 132.71(8) . . ?
O9 Dy O4 80.36(8) . . ?
O12 Dy O4 89.54(8) . . ?
O7 Dy O4 102.95(8) . . ?
O3 Dy O4 154.25(8) . . ?
O1 Dy N4 102.10(8) . . ?
O2 Dy N4 93.84(9) . . ?
O11 Dy N5 26.02(8) . . ?
O6 Dy N4 116.14(9) . . ?
O13 Dy N4 144.62(9) . . ?
O9 Dy N4 25.75(8) . . ?
O12 Dy N4 163.26(9) . . ?
O7 Dy N4 89.11(9) . . ?
O3 Dy N4 75.60(9) . . ?
O4 Dy N4 78.72(9) . . ?
O1 Dy N5 72.18(8) . . ?
O2 Dy N5 92.33(9) . . ?
O10 Dy N5 152.58(10) . . ?
O6 Dy N5 69.50(8) . . ?
O13 Dy N5 25.34(9) . . ?
O9 Dy N5 152.34(8) . . ?
O12 Dy N5 25.88(9) . . ?
O7 Dy N5 87.86(10) . . ?
O3 Dy N5 93.30(9) . . ?
O4 Dy N5 112.37(9) . . ?
N3 Dy N5 168.90(10) . . ?
O2 Cu O1 83.99(9) . . ?
O2 Cu N2 95.55(11) . . ?
O1 Cu N2 177.88(12) . . ?
O2 Cu N1 172.57(11) . . ?
O1 Cu N1 94.25(10) . . ?
N2 Cu N1 86.47(12) . . ?
O2 Cu Dy 42.91(6) . . ?
O1 Cu Dy 41.18(6) . . ?
N2 Cu Dy 138.45(9) . . ?
N1 Cu Dy 134.49(8) . . ?
C2 O3 C17 117.8(2) . . ?
C2 O3 Dy 118.08(17) . . ?
C17 O3 Dy 124.01(18) . . ?
C1 O1 Cu 123.35(18) . . ?
C1 O1 Dy 128.78(18) . . ?
Cu O1 Dy 106.12(9) . . ?
C16 O2 Cu 125.0(2) . . ?
C16 O2 Dy 130.8(2) . . ?
Cu O2 Dy 104.10(9) . . ?
C15 O4 C19 116.5(2) . . ?
C15 O4 Dy 119.77(18) . . ?
C19 O4 Dy 123.75(18) . . ?
N4 O10 Dy 97.43(18) . . ?
N4 O9 Dy 95.56(19) . . ?
N5 O13 Dy 97.0(2) . . ?
N5 O12 Dy 94.9(2) . . ?
N3 O6 Dy 99.82(19) . . ?
N3 O7 Dy 93.71(19) . . ?
C7 N1 C8 123.9(3) . . ?
C7 N1 Cu 125.5(2) . . ?
C8 N1 Cu 110.6(2) . . ?
C10 N2 C9 121.9(3) . . ?
C10 N2 Cu 125.6(3) . . ?
C9 N2 Cu 112.3(2) . . ?
O8 N4 O9 122.6(3) . . ?
O8 N4 O10 122.3(3) . . ?
O9 N4 O10 115.1(3) . . ?
O8 N4 Dy 175.3(3) . . ?
O9 N4 Dy 58.69(17) . . ?
O10 N4 Dy 56.55(16) . . ?
O11 N5 O13 122.8(4) . . ?
O11 N5 O12 120.3(4) . . ?
O13 N5 O12 116.8(3) . . ?
O11 N5 Dy 178.2(3) . . ?
O13 N5 Dy 57.68(18) . . ?
O12 N5 Dy 59.22(18) . . ?
O5 N3 O7 122.4(4) . . ?
O5 N3 O6 121.6(4) . . ?
O7 N3 O6 116.0(3) . . ?
O5 N3 Dy 176.7(3) . . ?
O7 N3 Dy 60.89(16) . . ?
O6 N3 Dy 55.11(15) . . ?
O3 C17 C18 112.2(3) . . ?
O3 C2 C3 125.7(3) . . ?
O3 C2 C1 113.7(3) . . ?
C3 C2 C1 120.6(3) . . ?
C2 C3 C4 119.2(3) . . ?
C5 C4 C3 120.9(3) . . ?
C4 C5 C6 121.2(3) . . ?
C1 C6 C5 118.3(3) . . ?
C1 C6 C7 123.0(3) . . ?
C5 C6 C7 118.7(3) . . ?
O1 C1 C2 116.3(3) . . ?
O1 C1 C6 123.9(3) . . ?
C2 C1 C6 119.7(3) . . ?
N1 C7 C6 124.9(3) . . ?
N1 C8 C9 107.8(3) . . ?
N2 C9 C8 107.2(3) . . ?
N2 C10 C11 125.1(3) . . ?
C16 C11 C12 119.3(3) . . ?
C16 C11 C10 123.3(3) . . ?
C12 C11 C10 117.4(3) . . ?
C13 C12 C11 120.6(3) . . ?
C12 C13 C14 120.8(3) . . ?
C15 C14 C13 119.5(3) . . ?
C14 C15 O4 126.1(3) . . ?
C14 C15 C16 120.9(3) . . ?
O4 C15 C16 113.0(2) . . ?
O2 C16 C11 125.1(3) . . ?
O2 C16 C15 116.0(3) . . ?
C11 C16 C15 118.9(3) . . ?
O4 C19 C20 112.2(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
Dy O1 2.318(2) . ?
Dy O2 2.375(2) . ?
Dy O10 2.422(2) . ?
Dy O6 2.440(2) . ?
Dy O13 2.464(2) . ?
Dy O9 2.471(2) . ?
Dy O12 2.496(3) . ?
Dy O7 2.566(2) . ?
Dy O3 2.576(2) . ?
Dy O4 2.649(2) . ?
Dy N4 2.879(3) . ?
Dy N5 2.894(4) . ?
Cu O2 1.899(2) . ?
Cu O1 1.902(2) . ?
Cu N2 1.909(3) . ?
Cu N1 1.915(3) . ?
O3 C2 1.388(4) . ?
O3 C17 1.462(3) . ?
O1 C1 1.331(3) . ?
O2 C16 1.331(3) . ?
O4 C15 1.379(4) . ?
O4 C19 1.454(4) . ?
O10 N4 1.273(4) . ?
O9 N4 1.256(4) . ?
O8 N4 1.213(4) . ?
O13 N5 1.248(4) . ?
O12 N5 1.268(4) . ?
O11 N5 1.234(4) . ?
O6 N3 1.260(4) . ?
O7 N3 1.260(4) . ?
O5 N3 1.208(3) . ?
N1 C7 1.271(4) . ?
N1 C8 1.470(4) . ?
N2 C10 1.278(4) . ?
N2 C9 1.482(4) . ?
C18 C17 1.513(5) . ?
C2 C3 1.390(4) . ?
C2 C1 1.405(4) . ?
C3 C4 1.402(5) . ?
C4 C5 1.360(5) . ?
C5 C6 1.415(4) . ?
C6 C1 1.412(4) . ?
C6 C7 1.449(5) . ?
C8 C9 1.530(5) . ?
C10 C11 1.462(5) . ?
C11 C16 1.392(4) . ?
C11 C12 1.414(4) . ?
C12 C13 1.360(5) . ?
C13 C14 1.394(5) . ?
C14 C15 1.374(4) . ?
C15 C16 1.417(4) . ?
C19 C20 1.498(5) . ?
|
1100951.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100951.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_1100951
loop_
_publ_author_name
'Rajesh Koner'
'Hsin-Huang Lin'
'Ho-Hsiang Wei'
'Sasankasekhar Mohanta'
_publ_section_title
;
Syntheses, Structures, and Magnetic Properties of Diphenoxo-Bridged
MIILnIII Complexes Derived from N,N'-Ethylenebis(3-ethoxysalicylaldiimine)
(M = Cu or Ni; Ln = Ce-Yb): Observation of Surprisingly Strong Exchange
Interactions
;
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3524
_journal_page_last 3536
_journal_paper_doi 10.1021/ic048196h
_journal_volume 44
_journal_year 2005
_chemical_formula_sum 'C20 H22 Cu Ho N5 O13'
_chemical_formula_weight 768.90
_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 8.583(3)
_cell_length_b 13.749(3)
_cell_length_c 21.191(3)
_cell_measurement_temperature 293(2)
_cell_volume 2500.7(11)
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 293(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 0.0000
_diffrn_reflns_av_sigmaI/netI 0.0648
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -1
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min -1
_diffrn_reflns_limit_l_max 25
_diffrn_reflns_limit_l_min -1
_diffrn_reflns_number 2518
_diffrn_reflns_theta_full 25.00
_diffrn_reflns_theta_max 25.00
_diffrn_reflns_theta_min 1.92
_exptl_absorpt_coefficient_mu 4.070
_exptl_crystal_colour Red
_exptl_crystal_density_diffrn 2.042
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1508
_exptl_crystal_size_max 48
_exptl_crystal_size_mid 28
_exptl_crystal_size_min 12
_refine_diff_density_max 2.881
_refine_diff_density_min -0.843
_refine_diff_density_rms 0.165
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack 0.02(4)
_refine_ls_extinction_coef 0.00021(14)
_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 1.079
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 362
_refine_ls_number_reflns 2518
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.079
_refine_ls_R_factor_all 0.0723
_refine_ls_R_factor_gt 0.0456
_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^)+(0.0571P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1003
_refine_ls_wR_factor_ref 0.1152
_reflns_number_gt 1899
_reflns_number_total 2518
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file ic048196hsi20050224_082436_06.cif
_cod_data_source_block cuho
_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 2500.8(10)
_cod_database_code 1100951
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
Ho Ho 0.25990(6) 0.49805(6) 0.10040(3) 0.0310(2) Uani 1 1 d . . .
Cu Cu -0.0624(2) 0.55616(13) 0.18325(9) 0.0377(5) Uani 1 1 d . . .
N1 N -0.2004(14) 0.4870(10) 0.2380(6) 0.043(3) Uani 1 1 d . . .
N2 N -0.1735(16) 0.6681(10) 0.2095(7) 0.043(4) Uani 1 1 d . . .
O2 O 0.0930(13) 0.6239(6) 0.1362(5) 0.041(3) Uani 1 1 d . . .
O10 O 0.2866(11) 0.4948(11) -0.0128(5) 0.052(3) Uani 1 1 d . . .
N4 N 0.1442(16) 0.5042(13) -0.0255(6) 0.052(3) Uani 1 1 d . . .
O8 O 0.1029(16) 0.5068(11) -0.0808(5) 0.073(4) Uani 1 1 d . . .
O9 O 0.0591(14) 0.5242(9) 0.0206(6) 0.065(4) Uani 1 1 d . . .
O4 O 0.3190(11) 0.6810(7) 0.0703(5) 0.037(2) Uani 1 1 d . . .
O12 O 0.3176(16) 0.5375(10) 0.2113(6) 0.056(4) Uani 1 1 d . . .
C15 C 0.2179(17) 0.7545(10) 0.0897(7) 0.037(3) Uani 1 1 d . . .
O13 O 0.3604(11) 0.3904(8) 0.1841(5) 0.046(3) Uani 1 1 d . . .
O11 O 0.3990(16) 0.4294(12) 0.2803(5) 0.082(5) Uani 1 1 d . . .
C16 C 0.0949(18) 0.7193(10) 0.1263(7) 0.032(4) Uani 1 1 d . . .
O6 O 0.5344(13) 0.5376(8) 0.1119(6) 0.055(3) Uani 1 1 d . . .
C10 C -0.143(2) 0.7574(12) 0.1900(10) 0.051(5) Uani 1 1 d . . .
H10A H -0.2091 0.8064 0.2038 0.061 Uiso 1 1 calc R . .
C14 C 0.233(2) 0.8502(10) 0.0744(7) 0.044(4) Uani 1 1 d . . .
H14A H 0.3162 0.8720 0.0503 0.053 Uiso 1 1 calc R . .
C11 C -0.0168(17) 0.7859(10) 0.1498(7) 0.034(3) Uani 1 1 d . . .
N3 N 0.5952(15) 0.4670(11) 0.0825(7) 0.050(4) Uani 1 1 d . . .
C12 C -0.0003(19) 0.8827(10) 0.1324(8) 0.044(4) Uani 1 1 d . . .
H12A H -0.0742 0.9273 0.1463 0.053 Uiso 1 1 calc R . .
C19 C 0.4544(17) 0.7100(11) 0.0331(7) 0.043(4) Uani 1 1 d . . .
H19B H 0.4233 0.7584 0.0022 0.051 Uiso 1 1 calc R . .
H19A H 0.4946 0.6540 0.0105 0.051 Uiso 1 1 calc R . .
O7 O 0.5023(14) 0.4052(9) 0.0598(6) 0.062(4) Uani 1 1 d . . .
C13 C 0.1179(19) 0.9151(11) 0.0962(8) 0.051(4) Uani 1 1 d . . .
H13A H 0.1236 0.9806 0.0855 0.061 Uiso 1 1 calc R . .
O1 O 0.0472(11) 0.4433(7) 0.1545(4) 0.032(2) Uani 1 1 d . . .
O3 O 0.1658(11) 0.3248(7) 0.0772(4) 0.035(2) Uani 1 1 d . . .
C7 C -0.2217(17) 0.3951(11) 0.2370(7) 0.036(3) Uani 1 1 d . . .
H7A H -0.2931 0.3692 0.2654 0.044 Uiso 1 1 calc R . .
O5 O 0.7330(13) 0.4614(13) 0.0761(7) 0.088(5) Uani 1 1 d . . .
C1 C -0.0126(15) 0.3544(9) 0.1550(7) 0.030(3) Uani 1 1 d . . .
C9 C -0.3111(18) 0.6460(12) 0.2486(8) 0.044(4) Uani 1 1 d . . .
H9A H -0.4030 0.6397 0.2223 0.053 Uiso 1 1 calc R . .
H9B H -0.3288 0.6977 0.2789 0.053 Uiso 1 1 calc R . .
C17 C 0.240(2) 0.2604(11) 0.0314(7) 0.050(4) Uani 1 1 d . . .
H17B H 0.2979 0.2995 0.0013 0.059 Uiso 1 1 calc R . .
H17A H 0.1599 0.2257 0.0083 0.059 Uiso 1 1 calc R . .
C8 C -0.2785(18) 0.5531(11) 0.2816(7) 0.045(4) Uani 1 1 d . . .
H8B H -0.2126 0.5650 0.3180 0.054 Uiso 1 1 calc R . .
H8A H -0.3752 0.5243 0.2962 0.054 Uiso 1 1 calc R . .
C20 C 0.580(2) 0.7512(12) 0.0744(9) 0.059(5) Uani 1 1 d . . .
H20A H 0.6672 0.7697 0.0489 0.089 Uiso 1 1 calc R . .
H20C H 0.6117 0.7031 0.1045 0.089 Uiso 1 1 calc R . .
H20B H 0.5404 0.8073 0.0962 0.089 Uiso 1 1 calc R . .
C2 C 0.0434(19) 0.2879(11) 0.1140(8) 0.041(4) Uani 1 1 d . . .
C6 C -0.1438(19) 0.3289(11) 0.1953(8) 0.035(4) Uani 1 1 d . . .
N5 N 0.3584(17) 0.4522(14) 0.2269(7) 0.051(4) Uani 1 1 d . . .
C3 C -0.0142(19) 0.1919(11) 0.1084(9) 0.050(4) Uani 1 1 d . . .
H3A H 0.0269 0.1481 0.0794 0.060 Uiso 1 1 calc R . .
C5 C -0.194(2) 0.2306(11) 0.1915(9) 0.047(4) Uani 1 1 d . . .
H5A H -0.2705 0.2091 0.2195 0.056 Uiso 1 1 calc R . .
C4 C -0.136(2) 0.1668(12) 0.1486(9) 0.057(5) Uani 1 1 d . . .
H4A H -0.1781 0.1046 0.1460 0.068 Uiso 1 1 calc R . .
C18 C 0.3472(19) 0.1888(11) 0.0601(9) 0.052(5) Uani 1 1 d . . .
H18A H 0.3920 0.1489 0.0277 0.078 Uiso 1 1 calc R . .
H18C H 0.2905 0.1486 0.0892 0.078 Uiso 1 1 calc R . .
H18B H 0.4286 0.2224 0.0822 0.078 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
Ho 0.0272(3) 0.0269(3) 0.0387(3) -0.0030(4) 0.0035(3) 0.0005(4)
Cu 0.0327(9) 0.0281(8) 0.0523(11) -0.0037(9) 0.0098(9) 0.0029(8)
N1 0.035(6) 0.051(8) 0.042(7) -0.013(7) 0.007(5) -0.003(7)
N2 0.033(7) 0.041(7) 0.055(10) -0.019(7) 0.003(7) 0.007(6)
O2 0.043(6) 0.013(4) 0.066(8) 0.002(5) 0.018(6) 0.004(5)
O10 0.048(6) 0.049(6) 0.060(6) -0.003(7) 0.012(5) 0.006(8)
N4 0.070(9) 0.039(7) 0.046(8) 0.003(10) 0.004(7) -0.004(11)
O8 0.099(9) 0.073(8) 0.048(6) 0.002(8) -0.010(7) 0.023(10)
O9 0.046(6) 0.083(11) 0.065(7) 0.006(7) 0.007(6) 0.003(7)
O4 0.035(5) 0.030(5) 0.047(6) 0.001(5) 0.003(5) 0.002(5)
O12 0.051(8) 0.052(7) 0.063(9) -0.004(7) 0.004(7) 0.003(6)
C15 0.033(8) 0.030(7) 0.047(9) -0.005(6) -0.003(7) 0.001(6)
O13 0.039(6) 0.055(7) 0.045(7) 0.002(6) -0.008(5) 0.002(5)
O11 0.080(9) 0.125(13) 0.040(7) 0.019(8) -0.016(7) -0.054(10)
C16 0.030(9) 0.028(7) 0.040(8) -0.002(7) -0.003(7) 0.004(7)
O6 0.039(6) 0.045(6) 0.079(8) -0.007(6) 0.008(7) 0.008(5)
C10 0.050(11) 0.031(8) 0.072(14) -0.012(9) -0.013(10) 0.021(8)
C14 0.053(10) 0.029(7) 0.051(9) 0.003(6) -0.006(9) -0.008(8)
C11 0.037(8) 0.026(7) 0.040(8) -0.011(7) -0.002(8) 0.012(7)
N3 0.030(7) 0.058(9) 0.061(9) 0.019(7) 0.005(7) 0.010(7)
C12 0.045(9) 0.025(7) 0.063(11) -0.007(7) -0.005(8) 0.005(7)
C19 0.039(8) 0.038(8) 0.051(10) -0.001(7) 0.012(8) -0.004(7)
O7 0.052(7) 0.066(8) 0.069(8) -0.022(7) -0.008(7) 0.015(7)
C13 0.056(10) 0.034(8) 0.064(11) 0.007(8) -0.001(9) 0.009(8)
O1 0.027(5) 0.027(5) 0.043(5) -0.007(5) 0.012(5) 0.000(5)
O3 0.038(6) 0.034(5) 0.033(5) -0.011(5) 0.003(5) -0.001(5)
C7 0.031(8) 0.042(8) 0.037(8) -0.001(7) 0.000(7) -0.008(7)
O5 0.035(6) 0.129(13) 0.101(10) 0.021(9) 0.006(7) 0.018(8)
C1 0.020(7) 0.023(6) 0.046(8) -0.005(6) -0.005(6) 0.004(6)
C9 0.035(8) 0.053(10) 0.045(10) -0.015(8) 0.006(8) 0.003(8)
C17 0.067(11) 0.039(8) 0.043(9) 0.000(7) 0.005(10) 0.016(10)
C8 0.038(9) 0.042(8) 0.055(9) -0.009(8) 0.015(8) -0.001(8)
C20 0.049(10) 0.045(10) 0.084(13) 0.005(9) -0.006(10) -0.037(9)
C2 0.032(9) 0.038(8) 0.054(11) 0.003(8) -0.011(9) 0.001(7)
C6 0.036(9) 0.040(8) 0.029(8) -0.004(7) 0.003(7) -0.002(7)
N5 0.033(8) 0.079(11) 0.041(9) -0.006(9) 0.013(7) -0.020(8)
C3 0.044(9) 0.036(9) 0.069(12) -0.001(9) -0.006(10) -0.002(7)
C5 0.055(11) 0.033(8) 0.052(11) 0.015(8) 0.004(9) -0.004(8)
C4 0.050(10) 0.029(8) 0.091(14) -0.010(9) 0.002(10) -0.005(8)
C18 0.052(10) 0.031(8) 0.072(12) 0.008(8) 0.028(9) 0.001(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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ho Ho -0.2175 4.6783 '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 Ho O2 66.3(3) . . ?
O1 Ho O10 124.7(3) . . ?
O2 Ho O10 112.9(4) . . ?
O1 Ho O6 143.0(4) . . ?
O2 Ho O6 113.0(4) . . ?
O10 Ho O6 90.7(4) . . ?
O1 Ho O9 80.3(4) . . ?
O2 Ho O9 71.8(4) . . ?
O10 Ho O9 51.7(4) . . ?
O6 Ho O9 136.1(4) . . ?
O1 Ho O12 75.8(4) . . ?
O2 Ho O12 69.8(4) . . ?
O10 Ho O12 159.2(4) . . ?
O6 Ho O12 70.1(4) . . ?
O9 Ho O12 140.4(4) . . ?
O1 Ho O13 73.8(3) . . ?
O2 Ho O13 114.8(3) . . ?
O10 Ho O13 132.2(4) . . ?
O6 Ho O13 73.9(4) . . ?
O9 Ho O13 146.5(4) . . ?
O12 Ho O13 51.4(4) . . ?
O1 Ho O3 62.5(3) . . ?
O2 Ho O3 123.3(3) . . ?
O10 Ho O3 79.7(4) . . ?
O6 Ho O3 122.2(3) . . ?
O9 Ho O3 77.4(4) . . ?
O12 Ho O3 116.8(4) . . ?
O13 Ho O3 72.0(3) . . ?
O1 Ho O7 130.3(4) . . ?
O2 Ho O7 162.2(4) . . ?
O10 Ho O7 65.4(4) . . ?
O6 Ho O7 50.5(4) . . ?
O9 Ho O7 114.2(4) . . ?
O12 Ho O7 105.3(4) . . ?
O13 Ho O7 70.2(4) . . ?
O3 Ho O7 74.4(4) . . ?
O1 Ho O4 126.0(3) . . ?
O2 Ho O4 59.9(3) . . ?
O10 Ho O4 76.1(4) . . ?
O6 Ho O4 68.0(3) . . ?
O9 Ho O4 80.1(4) . . ?
O12 Ho O4 89.0(4) . . ?
O13 Ho O4 132.6(3) . . ?
O3 Ho O4 153.9(3) . . ?
O7 Ho O4 103.6(4) . . ?
O1 Ho N4 101.6(4) . . ?
O2 Ho N4 93.9(4) . . ?
O10 Ho N4 26.0(4) . . ?
O6 Ho N4 115.2(4) . . ?
O9 Ho N4 25.9(4) . . ?
O12 Ho N4 163.3(5) . . ?
O13 Ho N4 144.4(5) . . ?
O3 Ho N4 74.8(4) . . ?
O7 Ho N4 89.1(4) . . ?
O4 Ho N4 79.2(4) . . ?
O1 Ho N5 72.2(4) . . ?
O2 Ho N5 92.2(4) . . ?
O10 Ho N5 153.4(4) . . ?
O6 Ho N5 70.8(4) . . ?
O9 Ho N5 152.1(4) . . ?
O12 Ho N5 26.0(4) . . ?
O13 Ho N5 25.4(4) . . ?
O3 Ho N5 93.9(4) . . ?
O7 Ho N5 88.0(4) . . ?
O4 Ho N5 112.1(4) . . ?
N4 Ho N5 168.7(5) . . ?
N2 Cu O2 96.2(5) . . ?
N2 Cu N1 85.1(6) . . ?
O2 Cu N1 173.3(5) . . ?
N2 Cu O1 178.4(5) . . ?
O2 Cu O1 83.4(4) . . ?
N1 Cu O1 95.4(5) . . ?
N2 Cu Ho 139.3(4) . . ?
O2 Cu Ho 43.1(3) . . ?
N1 Cu Ho 135.0(4) . . ?
O1 Cu Ho 40.5(3) . . ?
C7 N1 C8 124.2(13) . . ?
C7 N1 Cu 124.7(11) . . ?
C8 N1 Cu 111.1(10) . . ?
C10 N2 C9 121.8(15) . . ?
C10 N2 Cu 124.2(13) . . ?
C9 N2 Cu 113.6(10) . . ?
C16 O2 Cu 125.0(10) . . ?
C16 O2 Ho 131.5(10) . . ?
Cu O2 Ho 103.5(4) . . ?
N4 O10 Ho 96.8(8) . . ?
O8 N4 O9 124.9(15) . . ?
O8 N4 O10 119.3(14) . . ?
O9 N4 O10 115.0(13) . . ?
O8 N4 Ho 176.4(11) . . ?
O9 N4 Ho 58.6(8) . . ?
O10 N4 Ho 57.2(7) . . ?
N4 O9 Ho 95.5(9) . . ?
C15 O4 C19 117.2(11) . . ?
C15 O4 Ho 119.9(8) . . ?
C19 O4 Ho 122.9(8) . . ?
N5 O12 Ho 95.8(10) . . ?
C14 C15 O4 124.9(14) . . ?
C14 C15 C16 122.5(15) . . ?
O4 C15 C16 112.6(12) . . ?
N5 O13 Ho 96.3(10) . . ?
O2 C16 C15 116.0(13) . . ?
O2 C16 C11 125.1(14) . . ?
C15 C16 C11 118.9(13) . . ?
N3 O6 Ho 100.3(9) . . ?
N2 C10 C11 126.2(15) . . ?
C15 C14 C13 118.1(16) . . ?
C12 C11 C16 117.2(15) . . ?
C12 C11 C10 119.9(13) . . ?
C16 C11 C10 123.0(14) . . ?
O5 N3 O7 122.7(18) . . ?
O5 N3 O6 120.9(18) . . ?
O7 N3 O6 116.4(12) . . ?
O5 N3 Ho 175.2(15) . . ?
O7 N3 Ho 61.8(7) . . ?
O6 N3 Ho 54.6(7) . . ?
C13 C12 C11 123.0(15) . . ?
O4 C19 C20 111.0(13) . . ?
N3 O7 Ho 92.8(9) . . ?
C12 C13 C14 120.3(14) . . ?
C1 O1 Cu 123.7(8) . . ?
C1 O1 Ho 128.2(8) . . ?
Cu O1 Ho 106.6(4) . . ?
C2 O3 C17 118.5(12) . . ?
C2 O3 Ho 117.7(8) . . ?
C17 O3 Ho 123.6(9) . . ?
N1 C7 C6 124.9(14) . . ?
O1 C1 C2 118.8(14) . . ?
O1 C1 C6 121.7(12) . . ?
C2 C1 C6 119.3(13) . . ?
N2 C9 C8 107.0(13) . . ?
O3 C17 C18 113.7(13) . . ?
N1 C8 C9 108.9(13) . . ?
C1 C2 O3 112.3(13) . . ?
C1 C2 C3 124.2(16) . . ?
O3 C2 C3 123.5(15) . . ?
C5 C6 C7 119.7(15) . . ?
C5 C6 C1 115.6(14) . . ?
C7 C6 C1 124.7(13) . . ?
O11 N5 O13 119.7(19) . . ?
O11 N5 O12 123.9(18) . . ?
O13 N5 O12 116.4(16) . . ?
O11 N5 Ho 177.8(15) . . ?
O13 N5 Ho 58.3(9) . . ?
O12 N5 Ho 58.2(9) . . ?
C4 C3 C2 116.3(16) . . ?
C4 C5 C6 122.5(17) . . ?
C5 C4 C3 121.8(16) . . ?
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
Ho O1 2.283(9) . ?
Ho O2 2.371(9) . ?
Ho O10 2.410(11) . ?
Ho O6 2.430(11) . ?
Ho O9 2.441(12) . ?
Ho O12 2.462(13) . ?
Ho O13 2.465(11) . ?
Ho O3 2.563(9) . ?
Ho O7 2.588(12) . ?
Ho O4 2.644(9) . ?
Ho N4 2.848(14) . ?
Ho N5 2.881(17) . ?
Cu N2 1.894(13) . ?
Cu O2 1.908(10) . ?
Cu N1 1.912(12) . ?
Cu O1 1.915(9) . ?
N1 C7 1.277(18) . ?
N1 C8 1.459(18) . ?
N2 C10 1.32(2) . ?
N2 C9 1.47(2) . ?
O2 C16 1.329(16) . ?
O10 N4 1.258(17) . ?
N4 O8 1.224(15) . ?
N4 O9 1.251(16) . ?
O4 C15 1.393(16) . ?
O4 C19 1.460(17) . ?
O12 N5 1.268(19) . ?
C15 C14 1.361(19) . ?
C15 C16 1.40(2) . ?
O13 N5 1.245(18) . ?
O11 N5 1.224(18) . ?
C16 C11 1.42(2) . ?
O6 N3 1.265(17) . ?
C10 C11 1.43(2) . ?
C14 C13 1.41(2) . ?
C11 C12 1.39(2) . ?
N3 O5 1.193(17) . ?
N3 O7 1.260(17) . ?
C12 C13 1.35(2) . ?
C19 C20 1.50(2) . ?
O1 C1 1.325(16) . ?
O3 C2 1.404(19) . ?
O3 C17 1.461(16) . ?
C7 C6 1.43(2) . ?
C1 C2 1.35(2) . ?
C1 C6 1.46(2) . ?
C9 C8 1.48(2) . ?
C17 C18 1.48(2) . ?
C2 C3 1.41(2) . ?
C6 C5 1.42(2) . ?
C3 C4 1.39(2) . ?
C5 C4 1.36(2) . ?
|
1100952.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100952.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_1100952
loop_
_publ_author_name
'Rajesh Koner'
'Hsin-Huang Lin'
'Ho-Hsiang Wei'
'Sasankasekhar Mohanta'
_publ_section_title
;
Syntheses, Structures, and Magnetic Properties of Diphenoxo-Bridged
MIILnIII Complexes Derived from N,N'-Ethylenebis(3-ethoxysalicylaldiimine)
(M = Cu or Ni; Ln = Ce-Yb): Observation of Surprisingly Strong Exchange
Interactions
;
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3524
_journal_page_last 3536
_journal_paper_doi 10.1021/ic048196h
_journal_volume 44
_journal_year 2005
_chemical_formula_sum 'C20 H22 Cu N5 O13 Tm'
_chemical_formula_weight 772.90
_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 8.566(3)
_cell_length_b 13.735(3)
_cell_length_c 21.1786(19)
_cell_measurement_temperature 293(2)
_cell_volume 2491.7(11)
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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 0.0475
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -1
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min -1
_diffrn_reflns_limit_l_max 25
_diffrn_reflns_limit_l_min -1
_diffrn_reflns_number 2507
_diffrn_reflns_theta_full 24.99
_diffrn_reflns_theta_max 24.99
_diffrn_reflns_theta_min 1.77
_exptl_absorpt_coefficient_mu 4.470
_exptl_crystal_colour Red
_exptl_crystal_density_diffrn 2.060
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1516
_exptl_crystal_size_max 50
_exptl_crystal_size_mid 35
_exptl_crystal_size_min 18
_refine_diff_density_max 0.876
_refine_diff_density_min -0.713
_refine_diff_density_rms 0.129
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack -0.04(2)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.106
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 361
_refine_ls_number_reflns 2507
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.106
_refine_ls_R_factor_all 0.0468
_refine_ls_R_factor_gt 0.0306
_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^)+(0.0326P)^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 0.0803
_reflns_number_gt 2060
_reflns_number_total 2507
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file ic048196hsi20050224_082436_07.cif
_cod_data_source_block cutm
_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 2491.8(10)
_cod_database_code 1100952
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
Tm Tm 0.74061(4) 0.49850(3) 0.101388(16) 0.03013(12) Uani 1 1 d . . .
Cu Cu 1.06180(14) 0.55672(8) 0.18305(6) 0.0360(3) Uani 1 1 d . . .
O10 O 0.7105(8) 0.4910(6) -0.0104(3) 0.0473(17) Uani 1 1 d . . .
N4 N 0.8517(10) 0.5087(7) -0.0251(4) 0.044(2) Uani 1 1 d . . .
O8 O 0.8949(11) 0.5054(7) -0.0792(4) 0.071(2) Uani 1 1 d . . .
O9 O 0.9396(9) 0.5224(6) 0.0210(4) 0.057(2) Uani 1 1 d . . .
O13 O 0.6405(8) 0.3908(5) 0.1834(4) 0.0432(17) Uani 1 1 d . . .
O12 O 0.6855(10) 0.5377(6) 0.2129(4) 0.050(2) Uani 1 1 d . . .
N5 N 0.6407(11) 0.4525(9) 0.2263(5) 0.048(3) Uani 1 1 d . . .
O2 O 0.9048(8) 0.6232(4) 0.1367(3) 0.0390(18) Uani 1 1 d . . .
O1 O 0.9527(8) 0.4439(5) 0.1550(3) 0.0340(15) Uani 1 1 d . . .
N1 N 1.1996(9) 0.4865(6) 0.2379(4) 0.0382(19) Uani 1 1 d . . .
C6 C 1.1424(13) 0.3277(7) 0.1931(5) 0.038(3) Uani 1 1 d . . .
C7 C 1.2207(11) 0.3951(7) 0.2369(5) 0.035(2) Uani 1 1 d . . .
H7A H 1.2906 0.3689 0.2658 0.042 Uiso 1 1 calc R . .
N2 N 1.1705(10) 0.6712(6) 0.2091(4) 0.035(2) Uani 1 1 d . . .
O4 O 0.6798(8) 0.6809(4) 0.0696(3) 0.0365(16) Uani 1 1 d . . .
C15 C 0.7753(12) 0.7531(7) 0.0900(4) 0.035(2) Uani 1 1 d . . .
C16 C 0.9027(12) 0.7194(7) 0.1272(5) 0.035(3) Uani 1 1 d . . .
C11 C 1.0119(11) 0.7848(7) 0.1511(5) 0.033(2) Uani 1 1 d . . .
C10 C 1.1419(12) 0.7565(7) 0.1911(6) 0.041(3) Uani 1 1 d . . .
H10A H 1.2093 0.8054 0.2045 0.050 Uiso 1 1 calc R . .
O3 O 0.8321(8) 0.3254(5) 0.0773(3) 0.0360(16) Uani 1 1 d . . .
C3 C 1.0128(11) 0.1940(6) 0.1086(5) 0.038(2) Uani 1 1 d . . .
H3A H 0.9725 0.1503 0.0793 0.045 Uiso 1 1 calc R . .
C1 C 1.0158(11) 0.3552(6) 0.1558(5) 0.030(2) Uani 1 1 d . . .
O11 O 0.6022(11) 0.4311(8) 0.2806(4) 0.079(3) Uani 1 1 d . . .
C2 C 0.9528(12) 0.2881(6) 0.1136(5) 0.032(2) Uani 1 1 d . . .
C17 C 0.7635(13) 0.2596(7) 0.0299(4) 0.045(3) Uani 1 1 d . . .
H17A H 0.8468 0.2240 0.0091 0.054 Uiso 1 1 calc R . .
H17B H 0.7106 0.2982 -0.0020 0.054 Uiso 1 1 calc R . .
C14 C 0.7642(15) 0.8512(7) 0.0746(5) 0.047(3) Uani 1 1 d . . .
H14A H 0.6811 0.8738 0.0504 0.057 Uiso 1 1 calc R . .
C19 C 0.5394(11) 0.7108(8) 0.0342(5) 0.043(3) Uani 1 1 d . . .
H19A H 0.4984 0.6550 0.0116 0.051 Uiso 1 1 calc R . .
H19B H 0.5688 0.7595 0.0032 0.051 Uiso 1 1 calc R . .
C8 C 1.2767(13) 0.5531(8) 0.2829(5) 0.048(3) Uani 1 1 d . . .
H8A H 1.3735 0.5249 0.2980 0.057 Uiso 1 1 calc R . .
H8B H 1.2093 0.5654 0.3188 0.057 Uiso 1 1 calc R . .
C12 C 0.9973(14) 0.8840(8) 0.1327(5) 0.046(3) Uani 1 1 d . . .
H12A H 1.0717 0.9283 0.1466 0.055 Uiso 1 1 calc R . .
C20 C 0.4152(14) 0.7512(8) 0.0750(6) 0.054(3) Uani 1 1 d . . .
H20A H 0.3273 0.7695 0.0495 0.082 Uiso 1 1 calc R . .
H20B H 0.4541 0.8075 0.0968 0.082 Uiso 1 1 calc R . .
H20C H 0.3836 0.7029 0.1052 0.082 Uiso 1 1 calc R . .
C13 C 0.8803(15) 0.9161(7) 0.0960(6) 0.057(3) Uani 1 1 d . . .
H13A H 0.8758 0.9815 0.0846 0.068 Uiso 1 1 calc R . .
C4 C 1.1348(13) 0.1666(8) 0.1488(5) 0.047(3) Uani 1 1 d . . .
H4A H 1.1752 0.1038 0.1465 0.057 Uiso 1 1 calc R . .
C9 C 1.3088(13) 0.6475(8) 0.2471(6) 0.046(3) Uani 1 1 d . . .
H9A H 1.3302 0.6998 0.2767 0.055 Uiso 1 1 calc R . .
H9B H 1.3991 0.6396 0.2199 0.055 Uiso 1 1 calc R . .
C5 C 1.1951(13) 0.2314(7) 0.1913(5) 0.041(3) Uani 1 1 d . . .
H5A H 1.2720 0.2112 0.2194 0.049 Uiso 1 1 calc R . .
C18 C 0.6500(14) 0.1884(8) 0.0574(7) 0.059(3) Uani 1 1 d . . .
H18A H 0.6085 0.1481 0.0244 0.088 Uiso 1 1 calc R . .
H18B H 0.5665 0.2231 0.0776 0.088 Uiso 1 1 calc R . .
H18C H 0.7024 0.1484 0.0880 0.088 Uiso 1 1 calc R . .
O6 O 0.4713(8) 0.5359(5) 0.1131(4) 0.0470(19) Uani 1 1 d . . .
N3 N 0.4054(10) 0.4668(7) 0.0823(5) 0.046(2) Uani 1 1 d . . .
O7 O 0.4986(11) 0.4031(7) 0.0609(4) 0.070(3) Uani 1 1 d . . .
O5 O 0.2674(9) 0.4606(9) 0.0776(5) 0.091(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
Tm 0.02807(19) 0.02740(18) 0.0349(2) -0.0022(2) -0.00386(18) -0.0002(3)
Cu 0.0341(6) 0.0263(5) 0.0476(7) -0.0039(6) -0.0115(6) -0.0009(5)
O10 0.051(4) 0.041(4) 0.050(4) -0.004(4) -0.007(3) -0.003(4)
N4 0.054(5) 0.025(4) 0.053(5) 0.011(5) 0.003(4) -0.005(5)
O8 0.102(7) 0.062(5) 0.049(4) -0.002(5) 0.027(5) -0.020(6)
O9 0.044(4) 0.071(6) 0.056(5) 0.001(4) 0.000(4) -0.002(4)
O13 0.038(4) 0.040(4) 0.051(5) 0.006(4) 0.005(4) 0.005(3)
O12 0.045(5) 0.049(4) 0.054(5) -0.012(4) 0.002(4) 0.000(4)
N5 0.033(5) 0.061(6) 0.050(6) 0.011(6) 0.004(5) 0.016(5)
O2 0.039(4) 0.020(3) 0.058(5) -0.001(3) -0.011(4) -0.003(3)
O1 0.029(3) 0.030(3) 0.044(4) -0.006(3) -0.005(3) -0.004(3)
N1 0.033(4) 0.038(5) 0.043(5) -0.005(4) -0.006(3) 0.004(4)
C6 0.036(6) 0.038(5) 0.039(6) -0.001(5) -0.010(5) 0.001(5)
C7 0.023(5) 0.039(5) 0.043(6) 0.010(5) -0.005(4) 0.010(5)
N2 0.031(5) 0.038(5) 0.035(5) -0.008(4) -0.009(4) 0.002(4)
O4 0.035(4) 0.028(3) 0.046(4) 0.000(3) -0.002(3) -0.004(3)
C15 0.038(5) 0.034(5) 0.032(5) -0.003(4) 0.003(5) 0.007(5)
C16 0.036(6) 0.030(5) 0.038(6) -0.009(4) 0.009(5) 0.007(5)
C11 0.034(5) 0.031(5) 0.032(5) -0.010(4) 0.002(5) -0.005(4)
C10 0.035(6) 0.032(5) 0.057(7) -0.012(5) 0.006(6) -0.009(5)
O3 0.041(4) 0.030(4) 0.038(4) -0.006(3) -0.004(3) -0.001(3)
C3 0.035(5) 0.022(5) 0.056(7) -0.006(5) 0.007(5) -0.003(4)
C1 0.027(5) 0.022(4) 0.040(6) 0.004(4) 0.005(4) 0.004(4)
O11 0.078(6) 0.105(7) 0.053(5) 0.021(6) 0.019(5) 0.042(6)
C2 0.037(6) 0.025(4) 0.034(6) 0.005(4) 0.007(5) 0.002(4)
C17 0.056(7) 0.040(5) 0.038(5) -0.011(4) -0.007(6) -0.011(6)
C14 0.061(7) 0.030(5) 0.051(6) -0.001(4) -0.005(6) 0.001(6)
C19 0.027(5) 0.054(6) 0.048(7) 0.005(5) -0.014(5) 0.002(5)
C8 0.047(6) 0.050(6) 0.046(6) -0.013(5) -0.014(5) 0.005(6)
C12 0.055(7) 0.034(6) 0.049(7) -0.010(5) 0.010(6) -0.004(5)
C20 0.042(6) 0.045(7) 0.077(9) 0.016(6) 0.000(6) 0.007(6)
C13 0.077(8) 0.028(6) 0.065(8) 0.003(6) 0.006(7) -0.007(6)
C4 0.040(6) 0.032(5) 0.069(8) 0.003(5) -0.001(6) 0.002(5)
C9 0.036(6) 0.046(6) 0.055(7) -0.010(5) -0.001(5) -0.002(5)
C5 0.032(6) 0.039(5) 0.051(7) 0.006(5) -0.007(5) 0.001(5)
C18 0.059(7) 0.033(6) 0.084(9) 0.008(6) -0.018(7) -0.014(6)
O6 0.032(4) 0.048(4) 0.061(5) 0.007(4) -0.005(4) 0.003(3)
N3 0.032(5) 0.060(6) 0.046(5) 0.002(4) -0.003(4) -0.017(4)
O7 0.065(6) 0.068(6) 0.076(6) -0.016(5) 0.009(5) -0.010(5)
O5 0.033(4) 0.151(10) 0.089(6) 0.010(7) -0.009(4) -0.021(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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tm Tm -0.3139 5.2483 '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 Tm O2 66.5(2) . . ?
O1 Tm O6 142.7(2) . . ?
O2 Tm O6 113.1(3) . . ?
O1 Tm O10 124.7(2) . . ?
O2 Tm O10 114.5(3) . . ?
O6 Tm O10 90.5(2) . . ?
O1 Tm O9 80.4(3) . . ?
O2 Tm O9 72.7(3) . . ?
O6 Tm O9 136.4(3) . . ?
O10 Tm O9 52.2(2) . . ?
O1 Tm O13 74.0(2) . . ?
O2 Tm O13 115.3(2) . . ?
O6 Tm O13 73.5(2) . . ?
O10 Tm O13 130.1(3) . . ?
O9 Tm O13 145.8(2) . . ?
O1 Tm O12 75.3(3) . . ?
O2 Tm O12 69.5(3) . . ?
O6 Tm O12 70.6(3) . . ?
O10 Tm O12 159.9(3) . . ?
O9 Tm O12 140.8(3) . . ?
O13 Tm O12 51.9(3) . . ?
O1 Tm O3 63.1(2) . . ?
O2 Tm O3 124.1(2) . . ?
O6 Tm O3 121.3(2) . . ?
O10 Tm O3 78.2(2) . . ?
O9 Tm O3 76.7(2) . . ?
O13 Tm O3 71.7(2) . . ?
O12 Tm O3 116.9(2) . . ?
O1 Tm O7 129.6(3) . . ?
O2 Tm O7 162.7(3) . . ?
O6 Tm O7 50.9(3) . . ?
O10 Tm O7 64.1(3) . . ?
O9 Tm O7 113.3(3) . . ?
O13 Tm O7 69.4(3) . . ?
O12 Tm O7 105.9(3) . . ?
O3 Tm O7 73.1(3) . . ?
O1 Tm O4 126.7(2) . . ?
O2 Tm O4 60.4(2) . . ?
O6 Tm O4 68.3(2) . . ?
O10 Tm O4 76.5(2) . . ?
O9 Tm O4 80.4(2) . . ?
O13 Tm O4 133.4(2) . . ?
O12 Tm O4 89.9(2) . . ?
O3 Tm O4 153.0(2) . . ?
O7 Tm O4 103.7(3) . . ?
O1 Tm N4 102.7(2) . . ?
O2 Tm N4 93.7(3) . . ?
O6 Tm N4 114.3(3) . . ?
O10 Tm N4 26.3(2) . . ?
O9 Tm N4 25.9(2) . . ?
O13 Tm N4 144.9(3) . . ?
O12 Tm N4 162.5(3) . . ?
O3 Tm N4 75.8(3) . . ?
O7 Tm N4 88.9(3) . . ?
O4 Tm N4 77.3(2) . . ?
O1 Tm N5 72.7(2) . . ?
O2 Tm N5 92.6(3) . . ?
O6 Tm N5 70.1(2) . . ?
O10 Tm N5 151.6(3) . . ?
O9 Tm N5 152.9(3) . . ?
O13 Tm N5 25.7(3) . . ?
O12 Tm N5 26.2(3) . . ?
O3 Tm N5 94.1(3) . . ?
O7 Tm N5 87.4(3) . . ?
O4 Tm N5 112.7(3) . . ?
N4 Tm N5 169.9(3) . . ?
O2 Cu O1 83.3(3) . . ?
O2 Cu N2 95.6(3) . . ?
O1 Cu N2 178.5(3) . . ?
O2 Cu N1 172.5(3) . . ?
O1 Cu N1 94.7(3) . . ?
N2 Cu N1 86.6(4) . . ?
O2 Cu Tm 42.74(19) . . ?
O1 Cu Tm 40.6(2) . . ?
N2 Cu Tm 138.3(3) . . ?
N1 Cu Tm 134.4(3) . . ?
N4 O10 Tm 97.6(6) . . ?
O8 N4 O9 124.4(9) . . ?
O8 N4 O10 121.2(9) . . ?
O9 N4 O10 114.2(9) . . ?
O8 N4 Tm 174.8(9) . . ?
O9 N4 Tm 58.1(5) . . ?
O10 N4 Tm 56.1(5) . . ?
N4 O9 Tm 96.0(6) . . ?
N5 O13 Tm 96.1(6) . . ?
N5 O12 Tm 94.1(7) . . ?
O11 N5 O13 121.2(12) . . ?
O11 N5 O12 120.9(12) . . ?
O13 N5 O12 117.9(10) . . ?
O11 N5 Tm 177.9(8) . . ?
O13 N5 Tm 58.2(5) . . ?
O12 N5 Tm 59.7(5) . . ?
C16 O2 Cu 124.2(7) . . ?
C16 O2 Tm 131.9(7) . . ?
Cu O2 Tm 103.8(3) . . ?
C1 O1 Cu 122.7(6) . . ?
C1 O1 Tm 129.2(6) . . ?
Cu O1 Tm 106.3(3) . . ?
C7 N1 C8 124.0(9) . . ?
C7 N1 Cu 125.2(7) . . ?
C8 N1 Cu 110.8(6) . . ?
C1 C6 C5 119.5(10) . . ?
C1 C6 C7 122.8(9) . . ?
C5 C6 C7 117.7(10) . . ?
N1 C7 C6 124.6(9) . . ?
C10 N2 C9 122.0(9) . . ?
C10 N2 Cu 125.9(8) . . ?
C9 N2 Cu 111.6(6) . . ?
C15 O4 C19 116.7(7) . . ?
C15 O4 Tm 119.5(5) . . ?
C19 O4 Tm 123.6(6) . . ?
O4 C15 C14 126.4(10) . . ?
O4 C15 C16 113.6(8) . . ?
C14 C15 C16 119.9(10) . . ?
O2 C16 C11 125.0(10) . . ?
O2 C16 C15 114.6(9) . . ?
C11 C16 C15 120.4(9) . . ?
C16 C11 C12 117.3(10) . . ?
C16 C11 C10 123.7(9) . . ?
C12 C11 C10 118.9(9) . . ?
N2 C10 C11 125.1(10) . . ?
C2 O3 C17 116.6(7) . . ?
C2 O3 Tm 117.6(5) . . ?
C17 O3 Tm 125.8(6) . . ?
C2 C3 C4 118.6(10) . . ?
O1 C1 C2 116.1(9) . . ?
O1 C1 C6 124.7(9) . . ?
C2 C1 C6 119.1(8) . . ?
O3 C2 C1 113.6(8) . . ?
O3 C2 C3 125.2(9) . . ?
C1 C2 C3 121.2(9) . . ?
O3 C17 C18 113.2(9) . . ?
C15 C14 C13 119.3(11) . . ?
O4 C19 C20 113.2(9) . . ?
N1 C8 C9 106.6(8) . . ?
C13 C12 C11 122.6(10) . . ?
C12 C13 C14 120.3(10) . . ?
C5 C4 C3 120.5(10) . . ?
N2 C9 C8 108.4(9) . . ?
C4 C5 C6 120.8(10) . . ?
N3 O6 Tm 102.3(6) . . ?
O5 N3 O7 123.2(12) . . ?
O5 N3 O6 122.2(12) . . ?
O7 N3 O6 114.5(8) . . ?
N3 O7 Tm 92.1(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
Tm O1 2.270(7) . ?
Tm O2 2.339(6) . ?
Tm O6 2.377(7) . ?
Tm O10 2.383(7) . ?
Tm O9 2.431(8) . ?
Tm O13 2.437(7) . ?
Tm O12 2.467(8) . ?
Tm O3 2.554(6) . ?
Tm O7 2.598(9) . ?
Tm O4 2.646(6) . ?
Tm N4 2.847(9) . ?
Tm N5 2.851(10) . ?
Cu O2 1.899(7) . ?
Cu O1 1.904(6) . ?
Cu N2 1.909(9) . ?
Cu N1 1.916(8) . ?
O10 N4 1.273(11) . ?
N4 O8 1.204(11) . ?
N4 O9 1.248(11) . ?
O13 N5 1.242(12) . ?
O12 N5 1.264(12) . ?
N5 O11 1.231(12) . ?
O2 C16 1.337(11) . ?
O1 C1 1.333(10) . ?
N1 C7 1.268(12) . ?
N1 C8 1.477(12) . ?
C6 C1 1.394(14) . ?
C6 C5 1.399(14) . ?
C6 C7 1.472(14) . ?
N2 C10 1.256(13) . ?
N2 C9 1.469(14) . ?
O4 C15 1.357(11) . ?
O4 C19 1.476(11) . ?
C15 C14 1.389(13) . ?
C15 C16 1.423(14) . ?
C16 C11 1.393(14) . ?
C11 C12 1.422(14) . ?
C11 C10 1.453(15) . ?
O3 C2 1.386(12) . ?
O3 C17 1.474(11) . ?
C3 C2 1.396(13) . ?
C3 C4 1.398(14) . ?
C1 C2 1.393(14) . ?
C17 C18 1.498(15) . ?
C14 C13 1.411(15) . ?
C19 C20 1.479(15) . ?
C8 C9 1.528(15) . ?
C12 C13 1.343(15) . ?
C4 C5 1.368(15) . ?
O6 N3 1.284(11) . ?
N3 O5 1.189(11) . ?
N3 O7 1.269(12) . ?
|
1100953.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100953.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_1100953
loop_
_publ_author_name
'Rajesh Koner'
'Hsin-Huang Lin'
'Ho-Hsiang Wei'
'Sasankasekhar Mohanta'
_publ_section_title
;
Syntheses, Structures, and Magnetic Properties of Diphenoxo-Bridged
MIILnIII Complexes Derived from N,N'-Ethylenebis(3-ethoxysalicylaldiimine)
(M = Cu or Ni; Ln = Ce-Yb): Observation of Surprisingly Strong Exchange
Interactions
;
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3524
_journal_page_last 3536
_journal_paper_doi 10.1021/ic048196h
_journal_volume 44
_journal_year 2005
_chemical_formula_sum 'C20 H22 Cu N5 O13 Yb'
_chemical_formula_weight 777.01
_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 8.576(3)
_cell_length_b 13.705(3)
_cell_length_c 21.114(3)
_cell_measurement_temperature 293(2)
_cell_volume 2481.6(11)
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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 0.0239
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -1
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min -1
_diffrn_reflns_limit_l_max 25
_diffrn_reflns_limit_l_min -1
_diffrn_reflns_number 2485
_diffrn_reflns_theta_full 24.98
_diffrn_reflns_theta_max 24.98
_diffrn_reflns_theta_min 1.77
_exptl_absorpt_coefficient_mu 4.682
_exptl_crystal_colour Red
_exptl_crystal_density_diffrn 2.080
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1520
_exptl_crystal_size_max 45
_exptl_crystal_size_mid 30
_exptl_crystal_size_min 15
_refine_diff_density_max 2.102
_refine_diff_density_min -2.526
_refine_diff_density_rms 0.224
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack 0.00(3)
_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 361
_refine_ls_number_reflns 2485
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.159
_refine_ls_R_factor_all 0.0518
_refine_ls_R_factor_gt 0.0447
_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^)+(0.0811P)^2^+10.5328P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1137
_refine_ls_wR_factor_ref 0.1332
_reflns_number_gt 2307
_reflns_number_total 2485
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file ic048196hsi20050224_082436_08.cif
_cod_data_source_block cuyb
_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 2481.6(12)
_cod_database_code 1100953
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
Yb Yb 0.25866(5) 0.00072(3) 0.10166(2) 0.0283(2) Uani 1 1 d . . .
Cu Cu -0.06187(18) -0.05762(10) 0.18298(8) 0.0346(4) Uani 1 1 d . . .
O10 O 0.2911(12) 0.0075(8) -0.0087(5) 0.046(2) Uani 1 1 d . . .
N4 N 0.1507(15) -0.0081(8) -0.0243(6) 0.045(3) Uani 1 1 d . . .
O8 O 0.1059(16) -0.0054(8) -0.0786(5) 0.069(3) Uani 1 1 d . . .
N1 N -0.2003(12) 0.0129(8) 0.2375(5) 0.034(2) Uani 1 1 d . . .
O9 O 0.0596(12) -0.0235(8) 0.0210(5) 0.052(3) Uani 1 1 d . . .
C7 C -0.2219(14) 0.1044(9) 0.2371(6) 0.034(3) Uani 1 1 d . . .
H7A H -0.2917 0.1307 0.2661 0.041 Uiso 1 1 calc R . .
C6 C -0.1423(16) 0.1709(9) 0.1932(6) 0.037(3) Uani 1 1 d . . .
O1 O 0.0451(10) 0.0551(6) 0.1557(4) 0.0297(17) Uani 1 1 d . . .
O4 O 0.3217(11) -0.1813(6) 0.0704(4) 0.037(2) Uani 1 1 d . . .
C2 C 0.0484(15) 0.2115(8) 0.1142(6) 0.034(3) Uani 1 1 d . . .
O2 O 0.0953(11) -0.1235(6) 0.1364(5) 0.043(2) Uani 1 1 d . . .
O3 O 0.1693(10) 0.1746(6) 0.0773(4) 0.0310(18) Uani 1 1 d . . .
C15 C 0.2230(15) -0.2539(8) 0.0908(6) 0.034(3) Uani 1 1 d . . .
C16 C 0.0989(17) -0.2201(8) 0.1257(6) 0.034(3) Uani 1 1 d . . .
C1 C -0.0148(14) 0.1434(8) 0.1564(6) 0.030(3) Uani 1 1 d . . .
O13 O 0.3592(11) 0.1085(6) 0.1847(5) 0.045(2) Uani 1 1 d . . .
O12 O 0.3157(13) -0.0380(7) 0.2117(5) 0.046(3) Uani 1 1 d . . .
N5 N 0.3589(15) 0.0467(10) 0.2252(6) 0.046(3) Uani 1 1 d . . .
O6 O 0.5262(11) -0.0358(7) 0.1106(5) 0.045(2) Uani 1 1 d . . .
C10 C -0.1398(16) -0.2582(9) 0.1911(6) 0.038(3) Uani 1 1 d . . .
H10A H -0.2050 -0.3077 0.2055 0.045 Uiso 1 1 calc R . .
C5 C -0.1951(16) 0.2682(9) 0.1905(7) 0.039(3) Uani 1 1 d . . .
H5A H -0.2741 0.2879 0.2179 0.047 Uiso 1 1 calc R . .
N2 N -0.1705(14) -0.1715(8) 0.2080(5) 0.037(3) Uani 1 1 d . . .
N3 N 0.5932(13) 0.0321(9) 0.0832(6) 0.041(3) Uani 1 1 d . . .
C14 C 0.2338(19) -0.3523(9) 0.0752(7) 0.047(4) Uani 1 1 d . . .
H14A H 0.3169 -0.3743 0.0508 0.056 Uiso 1 1 calc R . .
C17 C 0.2399(17) 0.2382(9) 0.0294(6) 0.041(3) Uani 1 1 d . . .
H17A H 0.1585 0.2744 0.0078 0.049 Uiso 1 1 calc R . .
H17B H 0.2934 0.1985 -0.0018 0.049 Uiso 1 1 calc R . .
C13 C 0.123(2) -0.4167(9) 0.0955(7) 0.048(4) Uani 1 1 d . . .
H13A H 0.1297 -0.4820 0.0839 0.058 Uiso 1 1 calc R . .
C8 C -0.2756(16) -0.0540(11) 0.2822(6) 0.043(3) Uani 1 1 d . . .
H8A H -0.3712 -0.0253 0.2982 0.052 Uiso 1 1 calc R . .
H8B H -0.2069 -0.0667 0.3177 0.052 Uiso 1 1 calc R . .
C19 C 0.4609(17) -0.2104(11) 0.0335(7) 0.048(4) Uani 1 1 d . . .
H19A H 0.5021 -0.1539 0.0115 0.057 Uiso 1 1 calc R . .
H19B H 0.4310 -0.2584 0.0020 0.057 Uiso 1 1 calc R . .
O7 O 0.5027(16) 0.0971(9) 0.0607(6) 0.074(4) Uani 1 1 d . . .
C12 C 0.0033(19) -0.3850(9) 0.1331(7) 0.047(4) Uani 1 1 d . . .
H12A H -0.0709 -0.4293 0.1474 0.056 Uiso 1 1 calc R . .
C3 C -0.0131(15) 0.3042(8) 0.1098(7) 0.039(3) Uani 1 1 d . . .
H3A H 0.0267 0.3478 0.0802 0.047 Uiso 1 1 calc R . .
C11 C -0.0089(16) -0.2853(9) 0.1505(6) 0.034(3) Uani 1 1 d . . .
O5 O 0.7314(14) 0.0360(14) 0.0781(7) 0.089(5) Uani 1 1 d . . .
O11 O 0.3965(15) 0.0680(11) 0.2817(5) 0.075(4) Uani 1 1 d . . .
C9 C -0.3116(16) -0.1495(10) 0.2470(7) 0.044(3) Uani 1 1 d . . .
H9A H -0.3315 -0.2018 0.2768 0.053 Uiso 1 1 calc R . .
H9B H -0.4025 -0.1417 0.2201 0.053 Uiso 1 1 calc R . .
C18 C 0.3555(17) 0.3098(10) 0.0588(8) 0.046(3) Uani 1 1 d . . .
H18A H 0.3996 0.3500 0.0262 0.069 Uiso 1 1 calc R . .
H18B H 0.4372 0.2741 0.0796 0.069 Uiso 1 1 calc R . .
H18C H 0.3025 0.3501 0.0891 0.069 Uiso 1 1 calc R . .
C20 C 0.586(2) -0.2527(12) 0.0753(8) 0.056(4) Uani 1 1 d . . .
H20A H 0.6740 -0.2708 0.0500 0.084 Uiso 1 1 calc R . .
H20B H 0.5458 -0.3094 0.0966 0.084 Uiso 1 1 calc R . .
H20C H 0.6169 -0.2050 0.1061 0.084 Uiso 1 1 calc R . .
C4 C -0.1353(18) 0.3332(9) 0.1499(8) 0.051(4) Uani 1 1 d . . .
H4A H -0.1741 0.3965 0.1482 0.061 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
Yb 0.0277(3) 0.0262(3) 0.0311(3) 0.0015(2) 0.00382(17) 0.0002(3)
Cu 0.0320(8) 0.0224(6) 0.0494(8) 0.0043(7) 0.0111(7) -0.0007(6)
O10 0.050(5) 0.036(5) 0.051(5) 0.006(5) 0.002(5) 0.003(5)
N4 0.061(7) 0.022(5) 0.052(7) -0.017(6) -0.003(6) 0.001(6)
O8 0.103(10) 0.061(7) 0.043(6) -0.006(5) -0.023(6) -0.010(8)
N1 0.026(4) 0.037(6) 0.040(5) 0.006(5) -0.001(4) -0.003(5)
O9 0.048(5) 0.063(6) 0.045(5) 0.001(5) 0.007(5) -0.001(5)
C7 0.023(5) 0.037(6) 0.041(7) 0.004(5) 0.001(5) 0.001(5)
C6 0.042(8) 0.028(6) 0.040(7) -0.001(5) -0.014(7) -0.002(6)
O1 0.030(4) 0.023(4) 0.036(4) 0.005(3) 0.003(4) 0.001(4)
O4 0.032(5) 0.031(4) 0.048(5) -0.004(4) 0.010(4) 0.004(4)
C2 0.031(6) 0.023(5) 0.047(7) -0.001(5) -0.001(6) -0.006(5)
O2 0.037(5) 0.015(4) 0.079(7) -0.002(4) 0.018(5) 0.002(4)
O3 0.035(5) 0.024(4) 0.033(4) 0.004(3) 0.010(4) -0.004(4)
C15 0.033(6) 0.021(5) 0.047(7) 0.001(5) -0.014(6) -0.001(5)
C16 0.043(8) 0.013(5) 0.048(7) 0.000(5) -0.010(6) 0.004(5)
C1 0.023(6) 0.020(5) 0.045(7) -0.002(5) 0.002(5) -0.003(5)
O13 0.046(5) 0.035(5) 0.054(6) 0.000(5) 0.006(5) 0.003(4)
O12 0.041(6) 0.048(6) 0.050(5) 0.012(4) -0.001(5) -0.001(5)
N5 0.042(7) 0.050(7) 0.045(7) -0.004(6) -0.010(6) 0.012(6)
O6 0.037(5) 0.044(5) 0.053(6) 0.004(4) 0.000(5) -0.001(4)
C10 0.039(8) 0.030(6) 0.045(7) 0.014(6) -0.014(6) -0.010(6)
C5 0.030(7) 0.037(6) 0.051(8) -0.008(6) -0.001(7) 0.009(6)
N2 0.035(6) 0.034(5) 0.041(6) 0.013(5) 0.008(5) -0.008(5)
N3 0.027(6) 0.058(7) 0.038(6) 0.001(5) 0.003(5) -0.010(5)
C14 0.054(9) 0.023(6) 0.063(9) -0.009(6) -0.010(8) 0.007(6)
C17 0.054(8) 0.030(6) 0.038(6) 0.009(5) 0.013(7) -0.007(6)
C13 0.069(10) 0.021(6) 0.055(9) -0.004(6) -0.006(8) -0.001(6)
C8 0.036(7) 0.052(8) 0.042(7) 0.006(6) 0.013(6) 0.006(7)
C19 0.044(8) 0.042(7) 0.058(9) -0.002(6) 0.015(7) 0.013(7)
O7 0.074(8) 0.055(6) 0.093(9) 0.027(6) -0.007(8) -0.005(6)
C12 0.060(9) 0.024(6) 0.056(8) 0.005(6) -0.009(8) -0.010(7)
C3 0.037(7) 0.019(5) 0.061(8) 0.007(5) 0.008(7) 0.001(5)
C11 0.037(7) 0.034(6) 0.031(6) 0.005(5) -0.001(6) -0.003(6)
O5 0.041(7) 0.153(14) 0.072(8) -0.005(9) 0.005(6) -0.024(8)
O11 0.077(8) 0.109(10) 0.039(5) -0.027(6) -0.016(6) 0.046(8)
C9 0.032(7) 0.046(8) 0.053(8) 0.015(7) 0.007(7) -0.006(6)
C18 0.037(7) 0.033(7) 0.069(10) 0.002(6) 0.012(7) -0.004(6)
C20 0.047(9) 0.051(9) 0.071(10) -0.005(8) -0.009(8) 0.021(8)
C4 0.044(8) 0.021(6) 0.087(12) 0.006(6) -0.004(8) 0.004(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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Yb Yb -0.3850 5.5486 '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 Yb O2 66.3(3) . . ?
O1 Yb O10 125.3(3) . . ?
O2 Yb O10 114.4(4) . . ?
O1 Yb O6 144.2(3) . . ?
O2 Yb O6 114.0(3) . . ?
O10 Yb O6 88.4(3) . . ?
O1 Yb O12 75.8(3) . . ?
O2 Yb O12 70.1(4) . . ?
O10 Yb O12 158.8(4) . . ?
O6 Yb O12 71.4(3) . . ?
O1 Yb O9 80.3(3) . . ?
O2 Yb O9 72.4(4) . . ?
O10 Yb O9 52.7(3) . . ?
O6 Yb O9 135.2(3) . . ?
O12 Yb O9 141.2(3) . . ?
O1 Yb O13 74.2(3) . . ?
O2 Yb O13 115.4(3) . . ?
O10 Yb O13 130.1(4) . . ?
O6 Yb O13 74.2(3) . . ?
O12 Yb O13 51.5(3) . . ?
O9 Yb O13 146.1(3) . . ?
O1 Yb O3 63.6(3) . . ?
O2 Yb O3 124.5(3) . . ?
O10 Yb O3 78.4(3) . . ?
O6 Yb O3 120.4(3) . . ?
O12 Yb O3 117.1(3) . . ?
O9 Yb O3 77.0(3) . . ?
O13 Yb O3 71.8(3) . . ?
O1 Yb O7 129.9(4) . . ?
O2 Yb O7 162.7(3) . . ?
O10 Yb O7 63.7(4) . . ?
O6 Yb O7 49.9(3) . . ?
O12 Yb O7 105.4(4) . . ?
O9 Yb O7 113.4(4) . . ?
O13 Yb O7 69.6(4) . . ?
O3 Yb O7 72.7(3) . . ?
O1 Yb O4 126.8(3) . . ?
O2 Yb O4 60.6(3) . . ?
O10 Yb O4 76.4(3) . . ?
O6 Yb O4 67.6(3) . . ?
O12 Yb O4 89.5(3) . . ?
O9 Yb O4 80.8(3) . . ?
O13 Yb O4 132.6(3) . . ?
O3 Yb O4 153.3(3) . . ?
O7 Yb O4 103.3(3) . . ?
O1 Yb N5 73.1(3) . . ?
O2 Yb N5 93.2(4) . . ?
O10 Yb N5 150.8(4) . . ?
O6 Yb N5 71.1(3) . . ?
O12 Yb N5 26.3(4) . . ?
O9 Yb N5 153.1(3) . . ?
O13 Yb N5 25.2(3) . . ?
O3 Yb N5 94.0(3) . . ?
O7 Yb N5 87.1(4) . . ?
O4 Yb N5 112.4(3) . . ?
O1 Yb N4 102.8(3) . . ?
O2 Yb N4 93.9(4) . . ?
O10 Yb N4 26.4(4) . . ?
O6 Yb N4 112.7(4) . . ?
O12 Yb N4 163.3(3) . . ?
O9 Yb N4 26.3(3) . . ?
O13 Yb N4 144.8(3) . . ?
O3 Yb N4 75.6(3) . . ?
O7 Yb N4 88.4(4) . . ?
O4 Yb N4 77.9(3) . . ?
N5 Yb N4 169.5(3) . . ?
O1 Cu N2 178.4(4) . . ?
O1 Cu O2 83.4(4) . . ?
N2 Cu O2 95.9(4) . . ?
O1 Cu N1 94.1(4) . . ?
N2 Cu N1 86.7(5) . . ?
O2 Cu N1 172.8(4) . . ?
O1 Cu Yb 41.1(2) . . ?
N2 Cu Yb 138.3(4) . . ?
O2 Cu Yb 42.5(3) . . ?
N1 Cu Yb 134.3(3) . . ?
N4 O10 Yb 98.0(8) . . ?
O8 N4 O9 122.1(13) . . ?
O8 N4 O10 122.9(13) . . ?
O9 N4 O10 115.0(12) . . ?
O8 N4 Yb 175.7(10) . . ?
O9 N4 Yb 59.4(7) . . ?
O10 N4 Yb 55.6(7) . . ?
C7 N1 C8 124.0(12) . . ?
C7 N1 Cu 125.8(10) . . ?
C8 N1 Cu 110.2(8) . . ?
N4 O9 Yb 94.3(8) . . ?
N1 C7 C6 123.4(12) . . ?
C1 C6 C5 119.0(12) . . ?
C1 C6 C7 123.3(11) . . ?
C5 C6 C7 117.7(13) . . ?
C1 O1 Cu 124.1(7) . . ?
C1 O1 Yb 128.3(7) . . ?
Cu O1 Yb 106.0(4) . . ?
C15 O4 C19 117.8(10) . . ?
C15 O4 Yb 118.7(7) . . ?
C19 O4 Yb 123.5(7) . . ?
C3 C2 O3 125.6(11) . . ?
C3 C2 C1 120.6(12) . . ?
O3 C2 C1 113.8(10) . . ?
C16 O2 Cu 124.9(9) . . ?
C16 O2 Yb 131.0(9) . . ?
Cu O2 Yb 104.1(3) . . ?
C2 O3 C17 118.6(9) . . ?
C2 O3 Yb 116.7(6) . . ?
C17 O3 Yb 124.7(7) . . ?
C16 C15 O4 113.6(10) . . ?
C16 C15 C14 120.3(13) . . ?
O4 C15 C14 125.9(13) . . ?
O2 C16 C15 116.0(12) . . ?
O2 C16 C11 123.8(12) . . ?
C15 C16 C11 120.1(10) . . ?
O1 C1 C6 124.2(11) . . ?
O1 C1 C2 117.1(11) . . ?
C6 C1 C2 118.6(11) . . ?
N5 O13 Yb 94.8(8) . . ?
N5 O12 Yb 94.3(7) . . ?
O13 N5 O12 119.3(11) . . ?
O13 N5 O11 120.4(14) . . ?
O12 N5 O11 120.2(13) . . ?
O13 N5 Yb 60.0(7) . . ?
O12 N5 Yb 59.4(6) . . ?
O11 N5 Yb 176.9(10) . . ?
N3 O6 Yb 104.8(8) . . ?
N2 C10 C11 124.3(12) . . ?
C4 C5 C6 122.2(13) . . ?
C10 N2 C9 120.9(11) . . ?
C10 N2 Cu 126.3(10) . . ?
C9 N2 Cu 112.6(8) . . ?
O5 N3 O6 122.6(15) . . ?
O5 N3 O7 122.7(16) . . ?
O6 N3 O7 114.7(11) . . ?
O5 N3 Yb 173.6(13) . . ?
O6 N3 Yb 51.1(6) . . ?
O7 N3 Yb 63.6(7) . . ?
C13 C14 C15 120.5(15) . . ?
O3 C17 C18 111.7(11) . . ?
C14 C13 C12 119.9(12) . . ?
N1 C8 C9 108.0(11) . . ?
O4 C19 C20 111.6(12) . . ?
N3 O7 Yb 90.6(8) . . ?
C13 C12 C11 120.7(13) . . ?
C2 C3 C4 120.4(12) . . ?
C16 C11 C12 118.2(13) . . ?
C16 C11 C10 124.7(11) . . ?
C12 C11 C10 117.0(12) . . ?
N2 C9 C8 106.0(11) . . ?
C5 C4 C3 118.9(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
Yb O1 2.282(8) . ?
Yb O2 2.323(9) . ?
Yb O10 2.348(10) . ?
Yb O6 2.356(10) . ?
Yb O12 2.432(10) . ?
Yb O9 2.433(11) . ?
Yb O13 2.449(10) . ?
Yb O3 2.556(8) . ?
Yb O7 2.622(13) . ?
Yb O4 2.637(8) . ?
Yb N5 2.819(12) . ?
Yb N4 2.819(12) . ?
Cu O1 1.887(8) . ?
Cu N2 1.893(10) . ?
Cu O2 1.897(9) . ?
Cu N1 1.915(11) . ?
O10 N4 1.267(16) . ?
N4 O8 1.210(15) . ?
N4 O9 1.253(15) . ?
N1 C7 1.268(16) . ?
N1 C8 1.465(17) . ?
C7 C6 1.468(18) . ?
C6 C1 1.395(19) . ?
C6 C5 1.409(17) . ?
O1 C1 1.315(14) . ?
O4 C15 1.375(15) . ?
O4 C19 1.480(16) . ?
C2 C3 1.379(17) . ?
C2 O3 1.392(16) . ?
C2 C1 1.399(17) . ?
O2 C16 1.344(13) . ?
O3 C17 1.466(14) . ?
C15 C16 1.375(19) . ?
C15 C14 1.391(17) . ?
C16 C11 1.389(18) . ?
O13 N5 1.204(15) . ?
O12 N5 1.252(16) . ?
N5 O11 1.269(15) . ?
O6 N3 1.236(15) . ?
C10 N2 1.267(17) . ?
C10 C11 1.460(19) . ?
C5 C4 1.34(2) . ?
N2 C9 1.494(18) . ?
N3 O5 1.191(16) . ?
N3 O7 1.274(16) . ?
C14 C13 1.36(2) . ?
C17 C18 1.526(19) . ?
C13 C12 1.37(2) . ?
C8 C9 1.54(2) . ?
C19 C20 1.50(2) . ?
C12 C11 1.418(18) . ?
C3 C4 1.40(2) . ?
|
1100954.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100954.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_1100954
loop_
_publ_author_name
'Rajesh Koner'
'Hsin-Huang Lin'
'Ho-Hsiang Wei'
'Sasankasekhar Mohanta'
_publ_section_title
;
Syntheses, Structures, and Magnetic Properties of Diphenoxo-Bridged
MIILnIII Complexes Derived from N,N'-Ethylenebis(3-ethoxysalicylaldiimine)
(M = Cu or Ni; Ln = Ce-Yb): Observation of Surprisingly Strong Exchange
Interactions
;
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3524
_journal_page_last 3536
_journal_paper_doi 10.1021/ic048196h
_journal_volume 44
_journal_year 2005
_chemical_formula_sum 'C20 H22 Ce N5 Ni O13'
_chemical_formula_weight 739.26
_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 8.6323(12)
_cell_length_b 13.822(2)
_cell_length_c 21.176(3)
_cell_measurement_temperature 293(2)
_cell_volume 2526.6(6)
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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 0.0260
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -1
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min -1
_diffrn_reflns_limit_l_max 25
_diffrn_reflns_limit_l_min -1
_diffrn_reflns_number 2546
_diffrn_reflns_theta_full 25.00
_diffrn_reflns_theta_max 25.00
_diffrn_reflns_theta_min 1.76
_exptl_absorpt_coefficient_mu 2.602
_exptl_crystal_colour Red
_exptl_crystal_density_diffrn 1.943
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1468
_exptl_crystal_size_max 60
_exptl_crystal_size_mid 35
_exptl_crystal_size_min 22
_refine_diff_density_max 0.508
_refine_diff_density_min -0.620
_refine_diff_density_rms 0.082
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack 0.00(2)
_refine_ls_extinction_coef 0.00047(13)
_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 1.156
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 362
_refine_ls_number_reflns 2546
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.156
_refine_ls_R_factor_all 0.0292
_refine_ls_R_factor_gt 0.0250
_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^)+(0.0329P)^2^+1.6091P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0659
_refine_ls_wR_factor_ref 0.0707
_reflns_number_gt 2372
_reflns_number_total 2546
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file ic048196hsi20050224_082436_09.cif
_cod_data_source_block nice
_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 2526.7(6)
_cod_database_code 1100954
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
Ce Ce 0.75152(3) 0.00201(2) 0.093734(13) 0.02851(12) Uani 1 1 d . . .
Ni Ni 0.42830(8) 0.06043(5) 0.18509(4) 0.03038(17) Uani 1 1 d . . .
O6 O 1.0416(6) 0.0340(3) 0.1060(2) 0.0539(13) Uani 1 1 d . . .
O7 O 0.9903(6) -0.0878(4) 0.0484(2) 0.0637(16) Uani 1 1 d . . .
N3 N 1.0920(7) -0.0349(4) 0.0738(3) 0.0470(15) Uani 1 1 d . . .
O10 O 0.7584(6) -0.0112(4) -0.0256(2) 0.0559(12) Uani 1 1 d . . .
O1 O 0.5267(5) -0.0498(3) 0.15480(18) 0.0329(9) Uani 1 1 d . . .
O2 O 0.5736(5) 0.1266(2) 0.13622(19) 0.0343(9) Uani 1 1 d . . .
O12 O 0.8246(6) 0.0390(4) 0.2104(2) 0.0553(13) Uani 1 1 d . . .
N4 N 0.6161(7) 0.0071(4) -0.0362(3) 0.0468(13) Uani 1 1 d . . .
O8 O 0.5607(9) -0.0007(4) -0.0888(2) 0.0763(17) Uani 1 1 d . . .
N5 N 0.8612(7) -0.0468(5) 0.2245(3) 0.0489(15) Uani 1 1 d . . .
O13 O 0.8528(6) -0.1099(3) 0.1815(2) 0.0512(12) Uani 1 1 d . . .
O9 O 0.5394(6) 0.0344(4) 0.0107(2) 0.0565(13) Uani 1 1 d . . .
O3 O 0.6436(5) -0.1724(3) 0.07509(19) 0.0351(9) Uani 1 1 d . . .
O4 O 0.8034(5) 0.1866(3) 0.0693(2) 0.0368(10) Uani 1 1 d . . .
C6 C 0.3470(7) -0.1669(4) 0.1967(3) 0.0367(15) Uani 1 1 d . . .
C10 C 0.3472(7) 0.2564(4) 0.1914(3) 0.0396(15) Uani 1 1 d . . .
H10A H 0.2793 0.3039 0.2056 0.048 Uiso 1 1 calc R . .
N2 N 0.3222(6) 0.1702(4) 0.2098(2) 0.0347(11) Uani 1 1 d . . .
C16 C 0.5790(7) 0.2217(4) 0.1270(2) 0.0280(11) Uani 1 1 d . . .
C1 C 0.4680(7) -0.1389(4) 0.1563(3) 0.0335(14) Uani 1 1 d . . .
O11 O 0.9018(7) -0.0688(5) 0.2779(2) 0.083(2) Uani 1 1 d . . .
C11 C 0.4706(8) 0.2868(4) 0.1508(3) 0.0346(14) Uani 1 1 d . . .
C15 C 0.7029(7) 0.2578(4) 0.0901(3) 0.0337(13) Uani 1 1 d . . .
C19 C 0.9426(8) 0.2181(5) 0.0358(3) 0.0429(15) Uani 1 1 d . . .
H19B H 0.9150 0.2679 0.0055 0.051 Uiso 1 1 calc R . .
H19A H 0.9856 0.1639 0.0126 0.051 Uiso 1 1 calc R . .
C2 C 0.5278(7) -0.2075(4) 0.1143(3) 0.0329(13) Uani 1 1 d . . .
O5 O 1.2276(6) -0.0497(6) 0.0662(3) 0.089(2) Uani 1 1 d . . .
N1 N 0.2994(6) -0.0072(4) 0.2385(2) 0.0340(11) Uani 1 1 d . . .
C8 C 0.2238(7) 0.0571(5) 0.2851(3) 0.0431(14) Uani 1 1 d . . .
H8B H 0.2931 0.0704 0.3201 0.052 Uiso 1 1 calc R . .
H8A H 0.1302 0.0274 0.3015 0.052 Uiso 1 1 calc R . .
C7 C 0.2761(7) -0.0983(5) 0.2398(3) 0.0391(15) Uani 1 1 d . . .
H7A H 0.2091 -0.1223 0.2704 0.047 Uiso 1 1 calc R . .
C13 C 0.6002(8) 0.4183(4) 0.0973(3) 0.0471(17) Uani 1 1 d . . .
H13A H 0.6062 0.4836 0.0870 0.056 Uiso 1 1 calc R . .
C14 C 0.7126(8) 0.3547(4) 0.0752(3) 0.0411(16) Uani 1 1 d . . .
H14A H 0.7938 0.3775 0.0505 0.049 Uiso 1 1 calc R . .
C17 C 0.7148(7) -0.2377(4) 0.0291(3) 0.0394(15) Uani 1 1 d . . .
H17B H 0.7653 -0.1997 -0.0034 0.047 Uiso 1 1 calc R . .
H17A H 0.6346 -0.2761 0.0091 0.047 Uiso 1 1 calc R . .
C12 C 0.4810(9) 0.3857(4) 0.1342(3) 0.0453(17) Uani 1 1 d . . .
H12A H 0.4061 0.4289 0.1484 0.054 Uiso 1 1 calc R . .
C3 C 0.4698(7) -0.2999(4) 0.1125(3) 0.0416(15) Uani 1 1 d . . .
H3A H 0.5089 -0.3442 0.0836 0.050 Uiso 1 1 calc R . .
C5 C 0.2941(8) -0.2629(5) 0.1955(3) 0.0462(17) Uani 1 1 d . . .
H5A H 0.2178 -0.2824 0.2238 0.055 Uiso 1 1 calc R . .
C9 C 0.1861(8) 0.1480(5) 0.2502(3) 0.0444(16) Uani 1 1 d . . .
H9B H 0.0943 0.1391 0.2245 0.053 Uiso 1 1 calc R . .
H9A H 0.1673 0.2005 0.2796 0.053 Uiso 1 1 calc R . .
C4 C 0.3529(9) -0.3275(5) 0.1537(3) 0.0513(18) Uani 1 1 d . . .
H4A H 0.3148 -0.3904 0.1526 0.062 Uiso 1 1 calc R . .
C20 C 1.0609(9) 0.2565(6) 0.0796(4) 0.0596(19) Uani 1 1 d . . .
H20A H 1.1505 0.2764 0.0561 0.089 Uiso 1 1 calc R . .
H20C H 1.0897 0.2071 0.1092 0.089 Uiso 1 1 calc R . .
H20B H 1.0193 0.3110 0.1020 0.089 Uiso 1 1 calc R . .
C18 C 0.8321(9) -0.3045(5) 0.0591(4) 0.055(2) Uani 1 1 d . . .
H18A H 0.8758 -0.3459 0.0273 0.083 Uiso 1 1 calc R . .
H18C H 0.7822 -0.3432 0.0908 0.083 Uiso 1 1 calc R . .
H18B H 0.9129 -0.2668 0.0782 0.083 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
Ce 0.02983(18) 0.02389(17) 0.03181(18) -0.00291(12) 0.00295(12) 0.00054(18)
Ni 0.0290(3) 0.0258(3) 0.0364(3) -0.0049(3) 0.0044(3) -0.0002(3)
O6 0.046(3) 0.046(3) 0.070(3) -0.010(2) 0.001(3) -0.001(2)
O7 0.041(3) 0.083(4) 0.067(3) -0.040(3) 0.002(3) 0.009(3)
N3 0.035(3) 0.063(4) 0.043(3) 0.002(3) 0.002(3) 0.004(3)
O10 0.064(3) 0.061(3) 0.042(2) -0.003(2) 0.006(2) 0.011(4)
O1 0.032(2) 0.0231(19) 0.043(2) -0.0032(17) 0.0092(18) -0.0034(17)
O2 0.037(2) 0.0219(17) 0.044(2) 0.0004(17) 0.011(2) -0.0012(19)
O12 0.060(3) 0.054(3) 0.051(3) -0.016(2) 0.002(3) -0.002(3)
N4 0.064(4) 0.032(3) 0.045(3) 0.008(3) -0.004(3) -0.002(3)
O8 0.117(5) 0.068(3) 0.045(3) 0.001(3) -0.030(3) 0.005(4)
N5 0.040(3) 0.065(4) 0.042(3) 0.006(3) 0.001(3) -0.016(3)
O13 0.061(3) 0.044(3) 0.049(3) 0.005(2) -0.007(3) -0.002(2)
O9 0.052(3) 0.073(3) 0.045(3) 0.002(2) 0.001(2) 0.010(3)
O3 0.041(2) 0.0263(19) 0.038(2) -0.0069(18) 0.003(2) -0.0020(19)
O4 0.036(2) 0.030(2) 0.044(2) 0.0019(18) 0.0104(19) -0.0036(19)
C6 0.034(3) 0.027(3) 0.049(4) 0.000(3) 0.003(3) -0.002(3)
C10 0.039(3) 0.029(3) 0.052(4) -0.012(3) -0.004(3) 0.007(3)
N2 0.030(3) 0.042(3) 0.032(3) -0.009(2) 0.001(2) 0.000(2)
C16 0.033(3) 0.023(2) 0.028(3) -0.001(2) -0.001(3) -0.004(2)
C1 0.037(3) 0.021(3) 0.042(3) -0.001(2) -0.009(3) -0.003(2)
O11 0.090(4) 0.113(5) 0.045(3) 0.030(3) -0.027(3) -0.051(4)
C11 0.039(3) 0.030(3) 0.035(3) -0.003(3) -0.004(3) 0.002(3)
C15 0.039(3) 0.023(3) 0.039(3) -0.002(2) -0.006(3) 0.003(2)
C19 0.036(3) 0.043(3) 0.050(4) 0.006(3) 0.013(3) -0.004(3)
C2 0.033(3) 0.025(3) 0.040(3) 0.001(2) -0.003(3) 0.002(2)
O5 0.029(3) 0.132(6) 0.108(5) -0.026(5) 0.003(3) 0.014(4)
N1 0.032(2) 0.037(3) 0.033(2) -0.003(2) 0.0046(19) 0.000(2)
C8 0.041(3) 0.044(3) 0.044(3) -0.011(3) 0.011(3) -0.001(3)
C7 0.036(4) 0.044(3) 0.037(3) 0.000(3) 0.004(3) -0.008(3)
C13 0.060(4) 0.026(3) 0.056(4) 0.002(3) -0.008(4) -0.001(3)
C14 0.048(4) 0.027(3) 0.049(3) 0.002(3) -0.001(3) -0.006(3)
C17 0.051(4) 0.028(3) 0.039(3) -0.010(2) 0.011(3) -0.001(3)
C12 0.056(4) 0.023(3) 0.057(4) -0.008(3) -0.009(4) 0.010(3)
C3 0.039(3) 0.031(3) 0.054(4) -0.008(3) 0.000(3) 0.003(3)
C5 0.043(4) 0.039(3) 0.056(4) 0.005(3) 0.008(3) -0.014(3)
C9 0.035(3) 0.047(4) 0.052(4) -0.011(3) 0.012(3) 0.001(3)
C4 0.054(4) 0.029(3) 0.071(5) -0.001(3) 0.003(4) -0.012(3)
C20 0.050(4) 0.052(4) 0.077(5) 0.010(4) -0.004(4) -0.008(4)
C18 0.059(5) 0.031(3) 0.077(5) 0.003(3) 0.017(4) 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 0.0033 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'
Ni Ni 0.3393 1.1124 '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
O1 Ce O2 61.19(12) . . ?
O1 Ce O10 121.74(15) . . ?
O2 Ce O10 115.26(15) . . ?
O1 Ce O6 140.92(15) . . ?
O2 Ce O6 116.76(15) . . ?
O10 Ce O6 95.22(17) . . ?
O1 Ce O13 73.19(15) . . ?
O2 Ce O13 111.52(14) . . ?
O10 Ce O13 132.02(16) . . ?
O6 Ce O13 72.40(16) . . ?
O1 Ce O9 81.22(15) . . ?
O2 Ce O9 71.74(15) . . ?
O10 Ce O9 49.38(16) . . ?
O6 Ce O9 137.33(17) . . ?
O13 Ce O9 147.02(16) . . ?
O1 Ce O7 133.54(17) . . ?
O2 Ce O7 163.99(15) . . ?
O10 Ce O7 65.00(17) . . ?
O6 Ce O7 48.79(15) . . ?
O13 Ce O7 73.08(18) . . ?
O9 Ce O7 113.30(15) . . ?
O1 Ce O12 75.35(15) . . ?
O2 Ce O12 70.65(16) . . ?
O10 Ce O12 162.89(17) . . ?
O6 Ce O12 68.39(17) . . ?
O13 Ce O12 49.41(16) . . ?
O9 Ce O12 141.83(16) . . ?
O7 Ce O12 104.67(17) . . ?
O1 Ce O3 61.71(12) . . ?
O2 Ce O3 118.36(13) . . ?
O10 Ce O3 77.96(15) . . ?
O6 Ce O3 121.60(14) . . ?
O13 Ce O3 71.05(14) . . ?
O9 Ce O3 78.69(15) . . ?
O7 Ce O3 77.62(15) . . ?
O12 Ce O3 114.28(15) . . ?
O1 Ce O4 121.48(13) . . ?
O2 Ce O4 60.31(12) . . ?
O10 Ce O4 82.53(15) . . ?
O6 Ce O4 71.74(14) . . ?
O13 Ce O4 131.71(15) . . ?
O9 Ce O4 79.57(16) . . ?
O7 Ce O4 104.79(16) . . ?
O12 Ce O4 87.43(15) . . ?
O3 Ce O4 157.13(15) . . ?
O1 Ce N4 100.58(15) . . ?
O2 Ce N4 94.32(15) . . ?
O10 Ce N4 24.96(16) . . ?
O6 Ce N4 118.19(17) . . ?
O13 Ce N4 144.30(15) . . ?
O9 Ce N4 24.57(15) . . ?
O7 Ce N4 88.93(17) . . ?
O12 Ce N4 164.64(16) . . ?
O3 Ce N4 75.14(14) . . ?
O4 Ce N4 82.13(14) . . ?
O1 Ce N5 72.31(14) . . ?
O2 Ce N5 90.96(16) . . ?
O10 Ce N5 153.63(17) . . ?
O6 Ce N5 68.67(16) . . ?
O13 Ce N5 24.68(16) . . ?
O9 Ce N5 153.10(15) . . ?
O7 Ce N5 89.04(18) . . ?
O12 Ce N5 24.74(16) . . ?
O3 Ce N5 92.55(15) . . ?
O4 Ce N5 110.14(16) . . ?
N4 Ce N5 167.67(15) . . ?
N1 Ni N2 86.7(2) . . ?
N1 Ni O1 94.1(2) . . ?
N2 Ni O1 175.8(2) . . ?
N1 Ni O2 174.7(2) . . ?
N2 Ni O2 95.0(2) . . ?
O1 Ni O2 84.45(17) . . ?
N1 Ni Ce 134.92(16) . . ?
N2 Ni Ce 138.01(17) . . ?
O1 Ni Ce 41.71(12) . . ?
O2 Ni Ce 43.00(11) . . ?
N3 O6 Ce 98.8(4) . . ?
N3 O7 Ce 96.8(4) . . ?
O5 N3 O6 122.9(7) . . ?
O5 N3 O7 121.5(7) . . ?
O6 N3 O7 115.5(5) . . ?
O5 N3 Ce 179.7(6) . . ?
O6 N3 Ce 57.0(3) . . ?
O7 N3 Ce 58.6(3) . . ?
N4 O10 Ce 98.0(4) . . ?
C1 O1 Ni 125.1(4) . . ?
C1 O1 Ce 125.9(4) . . ?
Ni O1 Ce 107.83(17) . . ?
C16 O2 Ni 126.2(4) . . ?
C16 O2 Ce 127.7(4) . . ?
Ni O2 Ce 106.09(15) . . ?
N5 O12 Ce 95.8(4) . . ?
O8 N4 O9 123.1(6) . . ?
O8 N4 O10 121.5(6) . . ?
O9 N4 O10 115.4(5) . . ?
O8 N4 Ce 173.5(5) . . ?
O9 N4 Ce 58.9(3) . . ?
O10 N4 Ce 57.1(3) . . ?
O11 N5 O12 121.6(7) . . ?
O11 N5 O13 120.8(7) . . ?
O12 N5 O13 117.5(6) . . ?
O11 N5 Ce 177.9(5) . . ?
O12 N5 Ce 59.4(3) . . ?
O13 N5 Ce 58.1(3) . . ?
N5 O13 Ce 97.2(4) . . ?
N4 O9 Ce 96.5(4) . . ?
C2 O3 C17 119.1(4) . . ?
C2 O3 Ce 119.3(3) . . ?
C17 O3 Ce 121.3(3) . . ?
C15 O4 C19 117.2(5) . . ?
C15 O4 Ce 121.2(3) . . ?
C19 O4 Ce 121.5(3) . . ?
C5 C6 C1 119.5(6) . . ?
C5 C6 C7 119.5(6) . . ?
C1 C6 C7 121.0(5) . . ?
N2 C10 C11 125.7(6) . . ?
C10 N2 C9 120.2(5) . . ?
C10 N2 Ni 126.8(5) . . ?
C9 N2 Ni 112.7(4) . . ?
O2 C16 C11 124.1(5) . . ?
O2 C16 C15 117.1(5) . . ?
C11 C16 C15 118.7(5) . . ?
O1 C1 C2 118.1(5) . . ?
O1 C1 C6 123.6(5) . . ?
C2 C1 C6 118.3(5) . . ?
C16 C11 C12 119.4(6) . . ?
C16 C11 C10 121.9(5) . . ?
C12 C11 C10 118.7(6) . . ?
C14 C15 O4 125.5(6) . . ?
C14 C15 C16 121.0(6) . . ?
O4 C15 C16 113.5(5) . . ?
O4 C19 C20 111.7(5) . . ?
C3 C2 O3 124.9(6) . . ?
C3 C2 C1 120.9(6) . . ?
O3 C2 C1 114.2(5) . . ?
C7 N1 C8 120.5(5) . . ?
C7 N1 Ni 127.6(5) . . ?
C8 N1 Ni 111.8(4) . . ?
N1 C8 C9 105.7(5) . . ?
N1 C7 C6 124.4(6) . . ?
C12 C13 C14 120.6(6) . . ?
C15 C14 C13 119.7(6) . . ?
O3 C17 C18 112.3(5) . . ?
C13 C12 C11 120.6(6) . . ?
C2 C3 C4 120.2(6) . . ?
C4 C5 C6 120.8(6) . . ?
N2 C9 C8 106.6(5) . . ?
C5 C4 C3 120.2(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
Ce O1 2.439(4) . ?
Ce O2 2.477(4) . ?
Ce O10 2.534(5) . ?
Ce O6 2.556(5) . ?
Ce O13 2.571(5) . ?
Ce O9 2.578(5) . ?
Ce O7 2.590(5) . ?
Ce O12 2.600(5) . ?
Ce O3 2.615(4) . ?
Ce O4 2.641(4) . ?
Ce N4 2.991(5) . ?
Ce N5 3.004(6) . ?
Ni N1 1.841(5) . ?
Ni N2 1.848(5) . ?
Ni O1 1.858(4) . ?
Ni O2 1.866(4) . ?
O6 N3 1.250(7) . ?
O7 N3 1.263(7) . ?
N3 O5 1.199(7) . ?
O10 N4 1.274(7) . ?
O1 C1 1.332(7) . ?
O2 C16 1.329(6) . ?
O12 N5 1.263(8) . ?
N4 O8 1.217(7) . ?
N4 O9 1.252(7) . ?
N5 O11 1.222(7) . ?
N5 O13 1.264(7) . ?
O3 C2 1.387(7) . ?
O3 C17 1.463(7) . ?
O4 C15 1.384(7) . ?
O4 C19 1.462(7) . ?
C6 C5 1.403(8) . ?
C6 C1 1.405(9) . ?
C6 C7 1.451(8) . ?
C10 N2 1.272(8) . ?
C10 C11 1.432(9) . ?
N2 C9 1.485(8) . ?
C16 C11 1.393(8) . ?
C16 C15 1.415(8) . ?
C1 C2 1.399(8) . ?
C11 C12 1.415(8) . ?
C15 C14 1.379(8) . ?
C19 C20 1.479(10) . ?
C2 C3 1.373(8) . ?
N1 C7 1.276(8) . ?
N1 C8 1.480(8) . ?
C8 C9 1.494(10) . ?
C13 C12 1.368(9) . ?
C13 C14 1.390(9) . ?
C17 C18 1.510(10) . ?
C3 C4 1.387(9) . ?
C5 C4 1.357(10) . ?
|
1100955.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100955.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_1100955
loop_
_publ_author_name
'Rajesh Koner'
'Hsin-Huang Lin'
'Ho-Hsiang Wei'
'Sasankasekhar Mohanta'
_publ_section_title
;
Syntheses, Structures, and Magnetic Properties of Diphenoxo-Bridged
MIILnIII Complexes Derived from N,N'-Ethylenebis(3-ethoxysalicylaldiimine)
(M = Cu or Ni; Ln = Ce-Yb): Observation of Surprisingly Strong Exchange
Interactions
;
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3524
_journal_page_last 3536
_journal_paper_doi 10.1021/ic048196h
_journal_volume 44
_journal_year 2005
_chemical_formula_sum 'C20 H22 N5 Nd Ni O13'
_chemical_formula_weight 743.38
_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 8.6215(15)
_cell_length_b 13.776(4)
_cell_length_c 21.179(3)
_cell_measurement_temperature 293(2)
_cell_volume 2515.4(9)
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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 0.0418
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -1
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min -1
_diffrn_reflns_limit_l_max 25
_diffrn_reflns_limit_l_min -1
_diffrn_reflns_number 2534
_diffrn_reflns_theta_full 24.99
_diffrn_reflns_theta_max 24.99
_diffrn_reflns_theta_min 1.76
_exptl_absorpt_coefficient_mu 2.868
_exptl_crystal_colour Red
_exptl_crystal_density_diffrn 1.963
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1476
_exptl_crystal_size_max 50
_exptl_crystal_size_mid 30
_exptl_crystal_size_min 18
_refine_diff_density_max 0.634
_refine_diff_density_min -0.645
_refine_diff_density_rms 0.094
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack -0.03(3)
_refine_ls_extinction_coef 0.00041(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 1.091
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 362
_refine_ls_number_reflns 2534
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.091
_refine_ls_R_factor_all 0.0389
_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^)+(0.0282P)^2^+1.5769P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0689
_refine_ls_wR_factor_ref 0.0762
_reflns_number_gt 2195
_reflns_number_total 2534
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file ic048196hsi20050224_082436_10.cif
_cod_data_source_block nind
_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 1100955
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
Nd Nd 0.74843(5) 0.50129(3) 0.095288(15) 0.02902(12) Uani 1 1 d . . .
Ni Ni 1.06998(11) 0.56018(6) 0.18529(5) 0.0312(2) Uani 1 1 d . . .
O1 O 0.9711(6) 0.4491(3) 0.1549(2) 0.0335(12) Uani 1 1 d . . .
O2 O 0.9238(6) 0.6257(3) 0.1367(2) 0.0358(12) Uani 1 1 d . . .
O12 O 0.6769(8) 0.5392(5) 0.2101(3) 0.0547(18) Uani 1 1 d . . .
O4 O 0.6937(6) 0.6846(4) 0.0696(3) 0.0381(13) Uani 1 1 d . . .
N5 N 0.6421(9) 0.4542(6) 0.2256(4) 0.0475(19) Uani 1 1 d . . .
O13 O 0.6473(7) 0.3906(4) 0.1818(3) 0.0483(14) Uani 1 1 d . . .
C16 C 0.9186(9) 0.7211(5) 0.1270(3) 0.0291(16) Uani 1 1 d . . .
O6 O 0.4608(7) 0.5333(4) 0.1077(3) 0.0505(16) Uani 1 1 d . . .
C15 C 0.7936(9) 0.7558(5) 0.0903(4) 0.0345(18) Uani 1 1 d . . .
N3 N 0.4113(9) 0.4631(5) 0.0751(3) 0.0459(18) Uani 1 1 d . . .
C10 C 1.1492(9) 0.7577(6) 0.1912(4) 0.040(2) Uani 1 1 d . . .
H10A H 1.2168 0.8056 0.2054 0.049 Uiso 1 1 calc R . .
C6 C 1.1529(10) 0.3326(6) 0.1955(4) 0.038(2) Uani 1 1 d . . .
C7 C 1.2230(9) 0.4012(6) 0.2384(4) 0.039(2) Uani 1 1 d . . .
H7A H 1.2902 0.3765 0.2688 0.047 Uiso 1 1 calc R . .
N2 N 1.1749(8) 0.6695(4) 0.2099(3) 0.0335(15) Uani 1 1 d . . .
O7 O 0.5129(7) 0.4091(5) 0.0510(3) 0.063(2) Uani 1 1 d . . .
C19 C 0.5550(9) 0.7152(6) 0.0351(4) 0.0405(19) Uani 1 1 d . . .
H19A H 0.5117 0.6600 0.0127 0.049 Uiso 1 1 calc R . .
H19B H 0.5832 0.7639 0.0041 0.049 Uiso 1 1 calc R . .
C11 C 1.0269(9) 0.7869(5) 0.1510(4) 0.0324(17) Uani 1 1 d . . .
O11 O 0.6007(9) 0.4341(6) 0.2784(3) 0.083(2) Uani 1 1 d . . .
C1 C 1.0299(9) 0.3603(5) 0.1557(3) 0.0303(17) Uani 1 1 d . . .
N1 N 1.2010(7) 0.4919(5) 0.2383(3) 0.0373(15) Uani 1 1 d . . .
O3 O 0.8523(6) 0.3275(3) 0.0753(2) 0.0327(12) Uani 1 1 d . . .
C13 C 0.8955(10) 0.9179(6) 0.0960(4) 0.048(2) Uani 1 1 d . . .
H13A H 0.8895 0.9831 0.0850 0.057 Uiso 1 1 calc R . .
C2 C 0.9704(8) 0.2913(5) 0.1139(4) 0.0327(18) Uani 1 1 d . . .
C3 C 1.0293(9) 0.1991(5) 0.1115(5) 0.044(2) Uani 1 1 d . . .
H3A H 0.9902 0.1545 0.0826 0.052 Uiso 1 1 calc R . .
O5 O 0.2752(7) 0.4476(7) 0.0678(4) 0.087(3) Uani 1 1 d . . .
C14 C 0.7847(9) 0.8540(5) 0.0742(4) 0.0369(19) Uani 1 1 d . . .
H14A H 0.7041 0.8762 0.0488 0.044 Uiso 1 1 calc R . .
C17 C 0.7815(10) 0.2619(6) 0.0290(4) 0.041(2) Uani 1 1 d . . .
H17A H 0.8622 0.2242 0.0086 0.050 Uiso 1 1 calc R . .
H17B H 0.7296 0.3000 -0.0033 0.050 Uiso 1 1 calc R . .
C5 C 1.2070(10) 0.2360(6) 0.1951(4) 0.045(2) Uani 1 1 d . . .
H5A H 1.2823 0.2162 0.2238 0.054 Uiso 1 1 calc R . .
C4 C 1.1482(11) 0.1725(6) 0.1526(4) 0.051(2) Uani 1 1 d . . .
H4A H 1.1880 0.1098 0.1507 0.062 Uiso 1 1 calc R . .
C12 C 1.0134(11) 0.8866(5) 0.1335(4) 0.046(2) Uani 1 1 d . . .
H12A H 1.0865 0.9310 0.1480 0.055 Uiso 1 1 calc R . .
C8 C 1.2769(9) 0.5570(6) 0.2851(4) 0.044(2) Uani 1 1 d . . .
H8A H 1.3714 0.5277 0.3010 0.053 Uiso 1 1 calc R . .
H8B H 1.2080 0.5696 0.3203 0.053 Uiso 1 1 calc R . .
C9 C 1.3126(10) 0.6487(6) 0.2506(4) 0.046(2) Uani 1 1 d . . .
H9B H 1.4049 0.6410 0.2250 0.055 Uiso 1 1 calc R . .
H9A H 1.3296 0.7014 0.2802 0.055 Uiso 1 1 calc R . .
O10 O 0.7368(7) 0.4909(5) -0.0225(3) 0.0536(15) Uani 1 1 d . . .
N4 N 0.8780(10) 0.5081(5) -0.0340(3) 0.0492(18) Uani 1 1 d . . .
O9 O 0.9583(7) 0.5323(5) 0.0125(3) 0.0570(17) Uani 1 1 d . . .
C20 C 0.4351(12) 0.7561(7) 0.0792(5) 0.061(3) Uani 1 1 d . . .
H20A H 0.3454 0.7756 0.0555 0.092 Uiso 1 1 calc R . .
H20B H 0.4773 0.8114 0.1008 0.092 Uiso 1 1 calc R . .
H20C H 0.4059 0.7076 0.1095 0.092 Uiso 1 1 calc R . .
C18 C 0.6665(12) 0.1942(6) 0.0590(5) 0.053(2) Uani 1 1 d . . .
H18A H 0.6229 0.1526 0.0273 0.080 Uiso 1 1 calc R . .
H18B H 0.5853 0.2312 0.0785 0.080 Uiso 1 1 calc R . .
H18C H 0.7179 0.1555 0.0904 0.080 Uiso 1 1 calc R . .
O8 O 0.9314(10) 0.5012(5) -0.0872(3) 0.0727(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
Nd 0.02878(19) 0.02409(18) 0.03421(19) -0.00277(17) -0.00329(17) -0.0006(2)
Ni 0.0282(4) 0.0267(4) 0.0388(5) -0.0048(4) -0.0059(5) -0.0002(4)
O1 0.031(3) 0.022(2) 0.048(3) -0.004(2) -0.010(2) 0.001(2)
O2 0.033(3) 0.023(2) 0.052(3) 0.000(2) -0.012(3) 0.001(2)
O12 0.055(4) 0.055(4) 0.054(4) -0.017(3) -0.004(3) 0.001(3)
O4 0.034(3) 0.032(3) 0.048(3) 0.001(2) -0.009(3) -0.001(2)
N5 0.042(4) 0.060(5) 0.041(4) 0.008(4) -0.005(4) 0.019(4)
O13 0.047(3) 0.046(3) 0.052(3) 0.007(3) 0.002(3) 0.005(3)
C16 0.028(4) 0.026(3) 0.034(4) -0.003(3) 0.004(4) -0.001(3)
O6 0.042(3) 0.039(3) 0.070(4) -0.013(3) -0.002(3) 0.001(3)
C15 0.035(4) 0.029(4) 0.040(4) 0.000(3) 0.009(3) -0.004(3)
N3 0.036(4) 0.053(4) 0.049(4) 0.004(3) -0.003(4) -0.005(4)
C10 0.033(4) 0.033(4) 0.056(5) -0.011(4) 0.002(4) -0.009(3)
C6 0.039(5) 0.035(4) 0.039(5) -0.002(4) 0.000(4) 0.003(4)
C7 0.036(5) 0.040(4) 0.043(4) 0.002(3) -0.005(4) 0.013(4)
N2 0.033(4) 0.034(3) 0.033(3) -0.007(3) -0.007(3) -0.003(3)
O7 0.036(3) 0.072(5) 0.079(4) -0.039(4) 0.002(3) -0.010(3)
C19 0.029(4) 0.041(4) 0.051(5) 0.010(4) -0.015(4) 0.010(4)
C11 0.037(4) 0.029(4) 0.031(4) -0.007(3) 0.002(4) -0.003(3)
O11 0.084(5) 0.116(6) 0.048(4) 0.036(4) 0.022(4) 0.048(5)
C1 0.030(4) 0.023(3) 0.038(4) 0.000(3) 0.002(3) 0.003(3)
N1 0.029(3) 0.040(4) 0.043(4) -0.006(3) -0.005(3) 0.002(3)
O3 0.039(3) 0.025(2) 0.035(3) -0.005(2) -0.004(3) -0.001(2)
C13 0.054(6) 0.030(4) 0.058(5) -0.001(4) 0.007(5) 0.002(4)
C2 0.028(4) 0.029(4) 0.042(4) 0.003(3) 0.006(4) -0.002(3)
C3 0.032(4) 0.029(4) 0.070(6) -0.005(4) 0.007(4) -0.001(3)
O5 0.030(4) 0.127(7) 0.106(6) -0.018(6) -0.006(4) -0.021(4)
C14 0.039(5) 0.027(4) 0.045(4) 0.007(3) 0.002(4) 0.000(3)
C17 0.050(6) 0.033(4) 0.041(4) -0.012(3) -0.008(4) -0.001(4)
C5 0.040(5) 0.036(4) 0.059(6) 0.006(4) -0.011(4) 0.009(4)
C4 0.050(5) 0.023(4) 0.081(7) -0.004(4) 0.003(5) 0.014(4)
C12 0.055(6) 0.024(4) 0.057(5) -0.006(4) 0.008(5) -0.014(4)
C8 0.037(5) 0.047(4) 0.048(4) -0.010(4) -0.014(4) 0.003(4)
C9 0.040(5) 0.050(5) 0.047(5) -0.009(4) -0.012(4) -0.010(4)
O10 0.055(4) 0.060(4) 0.046(3) 0.003(3) -0.003(3) -0.010(4)
N4 0.080(6) 0.033(3) 0.035(4) 0.003(4) 0.001(4) 0.003(4)
O9 0.046(4) 0.072(4) 0.053(4) 0.002(3) 0.000(3) -0.008(3)
C20 0.043(5) 0.054(6) 0.086(7) 0.010(5) 0.010(6) 0.013(5)
C18 0.054(6) 0.036(5) 0.069(6) 0.004(4) -0.015(5) -0.006(5)
O8 0.103(5) 0.062(4) 0.053(4) -0.001(4) 0.023(4) -0.008(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'
Ni Ni 0.3393 1.1124 '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'
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 Nd O2 61.87(16) . . ?
O1 Nd O10 122.56(19) . . ?
O2 Nd O10 114.97(19) . . ?
O1 Nd O6 141.10(18) . . ?
O2 Nd O6 116.46(18) . . ?
O10 Nd O6 94.3(2) . . ?
O1 Nd O13 73.51(18) . . ?
O2 Nd O13 111.98(17) . . ?
O10 Nd O13 132.2(2) . . ?
O6 Nd O13 72.13(19) . . ?
O1 Nd O9 81.09(19) . . ?
O2 Nd O9 72.03(19) . . ?
O10 Nd O9 49.7(2) . . ?
O6 Nd O9 137.4(2) . . ?
O13 Nd O9 147.0(2) . . ?
O1 Nd O12 75.8(2) . . ?
O2 Nd O12 70.5(2) . . ?
O10 Nd O12 161.6(2) . . ?
O6 Nd O12 68.3(2) . . ?
O13 Nd O12 49.8(2) . . ?
O9 Nd O12 142.0(2) . . ?
O1 Nd O7 132.3(2) . . ?
O2 Nd O7 164.56(19) . . ?
O10 Nd O7 64.9(2) . . ?
O6 Nd O7 49.53(19) . . ?
O13 Nd O7 72.3(2) . . ?
O9 Nd O7 113.0(2) . . ?
O12 Nd O7 104.9(2) . . ?
O1 Nd O3 62.23(16) . . ?
O2 Nd O3 119.47(16) . . ?
O10 Nd O3 78.36(18) . . ?
O6 Nd O3 121.09(17) . . ?
O13 Nd O3 71.42(18) . . ?
O9 Nd O3 78.33(19) . . ?
O12 Nd O3 115.22(19) . . ?
O7 Nd O3 75.94(19) . . ?
O1 Nd O4 122.62(16) . . ?
O2 Nd O4 60.79(16) . . ?
O10 Nd O4 80.85(19) . . ?
O6 Nd O4 71.23(18) . . ?
O13 Nd O4 131.73(18) . . ?
O9 Nd O4 79.9(2) . . ?
O12 Nd O4 87.6(2) . . ?
O7 Nd O4 104.9(2) . . ?
O3 Nd O4 156.48(18) . . ?
O1 Nd N4 101.2(2) . . ?
O2 Nd N4 94.4(2) . . ?
O10 Nd N4 25.02(19) . . ?
O6 Nd N4 117.4(2) . . ?
O13 Nd N4 144.8(2) . . ?
O9 Nd N4 24.81(19) . . ?
O12 Nd N4 164.3(2) . . ?
O7 Nd N4 88.6(2) . . ?
O3 Nd N4 75.40(18) . . ?
O4 Nd N4 81.10(19) . . ?
O1 Nd N5 72.23(18) . . ?
O2 Nd N5 90.6(2) . . ?
O10 Nd N5 154.0(2) . . ?
O6 Nd N5 68.9(2) . . ?
O13 Nd N5 25.2(2) . . ?
O9 Nd N5 152.9(2) . . ?
O12 Nd N5 24.7(2) . . ?
O7 Nd N5 89.3(2) . . ?
O3 Nd N5 93.23(19) . . ?
O4 Nd N5 110.2(2) . . ?
N4 Nd N5 168.6(2) . . ?
N2 Ni N1 86.8(3) . . ?
N2 Ni O2 95.4(3) . . ?
N1 Ni O2 174.9(3) . . ?
N2 Ni O1 175.9(3) . . ?
N1 Ni O1 94.1(3) . . ?
O2 Ni O1 84.1(2) . . ?
N2 Ni Nd 138.1(2) . . ?
N1 Ni Nd 134.8(2) . . ?
O2 Ni Nd 42.80(15) . . ?
O1 Ni Nd 41.57(15) . . ?
C1 O1 Ni 125.3(5) . . ?
C1 O1 Nd 126.0(4) . . ?
Ni O1 Nd 107.5(2) . . ?
C16 O2 Ni 125.9(5) . . ?
C16 O2 Nd 128.0(5) . . ?
Ni O2 Nd 106.1(2) . . ?
N5 O12 Nd 96.6(5) . . ?
C15 O4 C19 117.7(6) . . ?
C15 O4 Nd 120.4(5) . . ?
C19 O4 Nd 121.8(4) . . ?
O11 N5 O12 121.9(9) . . ?
O11 N5 O13 121.7(9) . . ?
O12 N5 O13 116.4(7) . . ?
O11 N5 Nd 179.0(6) . . ?
O12 N5 Nd 58.7(4) . . ?
O13 N5 Nd 57.8(4) . . ?
N5 O13 Nd 97.1(5) . . ?
O2 C16 C11 124.2(7) . . ?
O2 C16 C15 116.4(7) . . ?
C11 C16 C15 119.4(6) . . ?
N3 O6 Nd 98.1(5) . . ?
O4 C15 C14 125.2(7) . . ?
O4 C15 C16 114.3(6) . . ?
C14 C15 C16 120.3(7) . . ?
O5 N3 O7 121.5(8) . . ?
O5 N3 O6 122.4(8) . . ?
O7 N3 O6 116.1(7) . . ?
O5 N3 Nd 179.1(7) . . ?
O7 N3 Nd 59.0(4) . . ?
O6 N3 Nd 57.2(4) . . ?
N2 C10 C11 125.3(7) . . ?
C1 C6 C5 120.1(8) . . ?
C1 C6 C7 121.0(7) . . ?
C5 C6 C7 118.9(8) . . ?
N1 C7 C6 125.7(8) . . ?
C10 N2 C9 119.4(7) . . ?
C10 N2 Ni 126.8(6) . . ?
C9 N2 Ni 113.5(5) . . ?
N3 O7 Nd 96.3(5) . . ?
O4 C19 C20 111.1(7) . . ?
C16 C11 C10 122.2(7) . . ?
C16 C11 C12 118.3(8) . . ?
C10 C11 C12 119.5(7) . . ?
O1 C1 C2 118.7(6) . . ?
O1 C1 C6 123.1(7) . . ?
C2 C1 C6 118.2(7) . . ?
C7 N1 C8 122.0(7) . . ?
C7 N1 Ni 126.5(6) . . ?
C8 N1 Ni 111.5(5) . . ?
C2 O3 C17 118.3(5) . . ?
C2 O3 Nd 119.1(4) . . ?
C17 O3 Nd 122.3(4) . . ?
C12 C13 C14 120.8(7) . . ?
C3 C2 C1 121.2(7) . . ?
C3 C2 O3 125.4(7) . . ?
C1 C2 O3 113.3(6) . . ?
C2 C3 C4 119.6(8) . . ?
C13 C14 C15 119.9(8) . . ?
O3 C17 C18 111.9(7) . . ?
C4 C5 C6 119.4(8) . . ?
C5 C4 C3 121.3(7) . . ?
C13 C12 C11 121.2(8) . . ?
N1 C8 C9 106.1(7) . . ?
C8 C9 N2 106.3(6) . . ?
N4 O10 Nd 98.1(4) . . ?
O8 N4 O9 122.6(9) . . ?
O8 N4 O10 121.7(8) . . ?
O9 N4 O10 115.7(7) . . ?
O8 N4 Nd 173.7(6) . . ?
O9 N4 Nd 59.3(4) . . ?
O10 N4 Nd 56.9(4) . . ?
N4 O9 Nd 95.9(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
Nd O1 2.407(5) . ?
Nd O2 2.447(5) . ?
Nd O10 2.502(6) . ?
Nd O6 2.533(6) . ?
Nd O13 2.539(6) . ?
Nd O9 2.556(6) . ?
Nd O12 2.563(6) . ?
Nd O7 2.573(6) . ?
Nd O3 2.591(5) . ?
Nd O4 2.626(5) . ?
Nd N4 2.958(7) . ?
Nd N5 2.979(8) . ?
Ni N2 1.832(6) . ?
Ni N1 1.850(6) . ?
Ni O2 1.861(5) . ?
Ni O1 1.866(5) . ?
O1 C1 1.325(8) . ?
O2 C16 1.332(8) . ?
O12 N5 1.251(9) . ?
O4 C15 1.377(9) . ?
O4 C19 1.463(9) . ?
N5 O11 1.206(9) . ?
N5 O13 1.277(9) . ?
C16 C11 1.397(10) . ?
C16 C15 1.412(11) . ?
O6 N3 1.263(9) . ?
C15 C14 1.397(10) . ?
N3 O5 1.203(9) . ?
N3 O7 1.258(9) . ?
C10 N2 1.297(10) . ?
C10 C11 1.414(11) . ?
C6 C1 1.407(11) . ?
C6 C5 1.410(11) . ?
C6 C7 1.443(11) . ?
C7 N1 1.264(10) . ?
N2 C9 1.495(11) . ?
C19 C20 1.504(12) . ?
C11 C12 1.428(10) . ?
C1 C2 1.396(10) . ?
N1 C8 1.487(10) . ?
O3 C2 1.397(9) . ?
O3 C17 1.468(8) . ?
C13 C12 1.360(12) . ?
C13 C14 1.379(11) . ?
C2 C3 1.369(11) . ?
C3 C4 1.394(12) . ?
C17 C18 1.502(12) . ?
C5 C4 1.355(12) . ?
C8 C9 1.491(12) . ?
O10 N4 1.264(9) . ?
N4 O8 1.222(9) . ?
N4 O9 1.248(9) . ?
|
1100956.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100956.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_1100956
loop_
_publ_author_name
'Rajesh Koner'
'Hsin-Huang Lin'
'Ho-Hsiang Wei'
'Sasankasekhar Mohanta'
_publ_section_title
;
Syntheses, Structures, and Magnetic Properties of Diphenoxo-Bridged
MIILnIII Complexes Derived from N,N'-Ethylenebis(3-ethoxysalicylaldiimine)
(M = Cu or Ni; Ln = Ce-Yb): Observation of Surprisingly Strong Exchange
Interactions
;
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3524
_journal_page_last 3536
_journal_paper_doi 10.1021/ic048196h
_journal_volume 44
_journal_year 2005
_chemical_formula_sum 'C20 H22 Eu N5 Ni O13'
_chemical_formula_weight 751.10
_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 8.617(4)
_cell_length_b 21.215(3)
_cell_length_c 13.754(3)
_cell_measurement_temperature 293(2)
_cell_volume 2514.4(13)
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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 0.0277
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -1
_diffrn_reflns_limit_k_max 1
_diffrn_reflns_limit_k_min -25
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_limit_l_min -1
_diffrn_reflns_number 2534
_diffrn_reflns_theta_full 24.99
_diffrn_reflns_theta_max 24.99
_diffrn_reflns_theta_min 1.76
_exptl_absorpt_coefficient_mu 3.298
_exptl_crystal_colour Red
_exptl_crystal_density_diffrn 1.984
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1488
_exptl_crystal_size_max 52
_exptl_crystal_size_mid 34
_exptl_crystal_size_min 22
_refine_diff_density_max 0.802
_refine_diff_density_min -0.996
_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 -0.02(3)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.139
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 361
_refine_ls_number_reflns 2534
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.139
_refine_ls_R_factor_all 0.0327
_refine_ls_R_factor_gt 0.0277
_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^)+(0.0399P)^2^+2.4203P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0744
_refine_ls_wR_factor_ref 0.0796
_reflns_number_gt 2332
_reflns_number_total 2534
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file ic048196hsi20050224_082436_11.cif
_cod_data_source_block nieu
_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 2514.5(12)
_cod_database_code 1100956
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
Eu Eu 0.00272(4) 0.152695(13) 0.24965(2) 0.02685(12) Uani 1 1 d . . .
Ni Ni -0.31772(10) 0.06454(4) 0.19007(6) 0.02885(19) Uani 1 1 d . . .
O1 O -0.2172(5) 0.0944(2) 0.3009(3) 0.0297(10) Uani 1 1 d . . .
N1 N -0.4496(7) 0.0120(3) 0.2574(4) 0.0341(13) Uani 1 1 d . . .
O2 O -0.1707(6) 0.1131(2) 0.1256(3) 0.0328(11) Uani 1 1 d . . .
N2 N -0.4230(7) 0.0397(3) 0.0798(4) 0.0314(13) Uani 1 1 d . . .
O12 O 0.0703(7) 0.0395(3) 0.2091(4) 0.0495(15) Uani 1 1 d . . .
O13 O 0.1010(6) 0.0672(3) 0.3591(4) 0.0448(12) Uani 1 1 d . . .
N5 N 0.1081(8) 0.0244(3) 0.2948(6) 0.0460(17) Uani 1 1 d . . .
O10 O 0.0209(6) 0.2685(3) 0.2570(4) 0.0467(13) Uani 1 1 d . . .
O3 O -0.0987(6) 0.1742(2) 0.4230(3) 0.0321(11) Uani 1 1 d . . .
O4 O 0.0614(6) 0.1796(2) 0.0685(4) 0.0355(11) Uani 1 1 d . . .
N4 N -0.1215(9) 0.2808(3) 0.2410(5) 0.0433(16) Uani 1 1 d . . .
C11 C -0.2721(9) 0.0995(3) -0.0362(5) 0.0342(16) Uani 1 1 d . . .
O8 O -0.1737(10) 0.3343(3) 0.2473(5) 0.0697(19) Uani 1 1 d . . .
C15 C -0.0394(8) 0.1602(3) -0.0048(5) 0.0330(16) Uani 1 1 d . . .
O9 O -0.2051(7) 0.2343(3) 0.2200(4) 0.0532(15) Uani 1 1 d . . .
C2 C -0.2167(8) 0.1365(3) 0.4588(5) 0.0308(15) Uani 1 1 d . . .
C19 C 0.1981(9) 0.2148(3) 0.0380(6) 0.0413(18) Uani 1 1 d . . .
H19A H 0.2396 0.2377 0.0933 0.050 Uiso 1 1 calc R . .
H19B H 0.1683 0.2454 -0.0110 0.050 Uiso 1 1 calc R . .
C16 C -0.1642(8) 0.1226(3) 0.0301(4) 0.0279(14) Uani 1 1 d . . .
C10 C -0.3966(8) 0.0585(4) -0.0075(5) 0.0376(17) Uani 1 1 d . . .
H10A H -0.4635 0.0444 -0.0559 0.045 Uiso 1 1 calc R . .
C1 C -0.2789(8) 0.0940(3) 0.3904(5) 0.0291(15) Uani 1 1 d . . .
O6 O 0.2853(6) 0.1412(3) 0.2166(4) 0.0455(14) Uani 1 1 d . . .
N3 N 0.3366(7) 0.1720(3) 0.2871(5) 0.0441(16) Uani 1 1 d . . .
O7 O 0.2350(7) 0.1958(3) 0.3440(5) 0.0591(17) Uani 1 1 d . . .
O11 O 0.1478(8) -0.0292(3) 0.3155(6) 0.073(2) Uani 1 1 d . . .
C7 C -0.4732(9) 0.0120(3) 0.3504(5) 0.0370(17) Uani 1 1 d . . .
H7A H -0.5417 -0.0178 0.3753 0.044 Uiso 1 1 calc R . .
C14 C -0.0280(10) 0.1753(4) -0.1025(5) 0.0394(18) Uani 1 1 d . . .
H14A H 0.0543 0.1999 -0.1244 0.047 Uiso 1 1 calc R . .
C13 C -0.1397(10) 0.1537(4) -0.1682(5) 0.045(2) Uani 1 1 d . . .
H13A H -0.1325 0.1649 -0.2334 0.054 Uiso 1 1 calc R . .
C6 C -0.4010(9) 0.0547(4) 0.4182(5) 0.0354(17) Uani 1 1 d . . .
C3 C -0.2765(9) 0.1396(4) 0.5517(5) 0.0401(17) Uani 1 1 d . . .
H3A H -0.2376 0.1688 0.5958 0.048 Uiso 1 1 calc R . .
C9 C -0.5621(9) -0.0003(4) 0.1002(6) 0.0427(19) Uani 1 1 d . . .
H9A H -0.5795 -0.0300 0.0476 0.051 Uiso 1 1 calc R . .
H9B H -0.6540 0.0256 0.1078 0.051 Uiso 1 1 calc R . .
C5 C -0.4553(9) 0.0568(4) 0.5150(5) 0.0413(19) Uani 1 1 d . . .
H5A H -0.5326 0.0291 0.5350 0.050 Uiso 1 1 calc R . .
C8 C -0.5255(9) -0.0345(3) 0.1928(6) 0.0409(17) Uani 1 1 d . . .
H8A H -0.6198 -0.0504 0.2224 0.049 Uiso 1 1 calc R . .
H8B H -0.4566 -0.0697 0.1802 0.049 Uiso 1 1 calc R . .
C12 C -0.2599(10) 0.1161(4) -0.1376(5) 0.044(2) Uani 1 1 d . . .
H12A H -0.3330 0.1015 -0.1820 0.053 Uiso 1 1 calc R . .
C17 C -0.0285(9) 0.2208(3) 0.4880(5) 0.0389(17) Uani 1 1 d . . .
H17A H -0.1098 0.2417 0.5246 0.047 Uiso 1 1 calc R . .
H17B H 0.0244 0.2524 0.4494 0.047 Uiso 1 1 calc R . .
C20 C 0.3216(11) 0.1725(4) -0.0026(6) 0.053(2) Uani 1 1 d . . .
H20A H 0.4094 0.1974 -0.0219 0.079 Uiso 1 1 calc R . .
H20B H 0.2815 0.1504 -0.0581 0.079 Uiso 1 1 calc R . .
H20C H 0.3528 0.1427 0.0461 0.079 Uiso 1 1 calc R . .
C4 C -0.3951(9) 0.0989(4) 0.5791(5) 0.045(2) Uani 1 1 d . . .
H4A H -0.4338 0.1005 0.6422 0.054 Uiso 1 1 calc R . .
C18 C 0.0850(11) 0.1916(4) 0.5577(6) 0.051(2) Uani 1 1 d . . .
H18A H 0.1279 0.2238 0.5987 0.076 Uiso 1 1 calc R . .
H18B H 0.1669 0.1716 0.5219 0.076 Uiso 1 1 calc R . .
H18C H 0.0327 0.1609 0.5970 0.076 Uiso 1 1 calc R . .
O5 O 0.4739(7) 0.1805(4) 0.3007(7) 0.079(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
Eu 0.02788(19) 0.03011(19) 0.02256(19) -0.00240(13) -0.0001(2) -0.00272(12)
Ni 0.0273(4) 0.0356(4) 0.0237(4) -0.0055(4) 0.0006(4) -0.0051(4)
O1 0.031(2) 0.038(2) 0.020(2) -0.0043(19) 0.002(2) -0.005(2)
N1 0.032(3) 0.034(3) 0.036(3) -0.006(3) -0.001(3) -0.002(2)
O2 0.036(3) 0.045(3) 0.017(2) -0.0008(19) 0.003(2) -0.007(2)
N2 0.026(3) 0.034(3) 0.034(3) -0.010(3) -0.003(3) 0.000(3)
O12 0.052(3) 0.051(3) 0.046(3) -0.015(3) -0.004(3) 0.000(3)
O13 0.048(3) 0.047(3) 0.040(3) 0.000(3) 0.005(2) 0.002(3)
N5 0.032(3) 0.049(4) 0.057(4) 0.004(4) 0.009(3) -0.001(3)
O10 0.049(3) 0.042(3) 0.049(3) 0.000(2) -0.002(4) -0.006(2)
O3 0.039(3) 0.035(3) 0.022(2) -0.006(2) 0.002(2) -0.004(2)
O4 0.034(3) 0.043(3) 0.030(2) 0.001(2) 0.005(2) -0.008(2)
N4 0.067(4) 0.036(3) 0.027(3) 0.004(3) 0.002(3) -0.003(3)
C11 0.036(4) 0.041(4) 0.026(3) -0.006(3) -0.001(3) 0.010(3)
O8 0.107(5) 0.039(3) 0.063(4) -0.005(3) -0.016(5) 0.018(4)
C15 0.036(4) 0.038(4) 0.025(3) -0.006(3) 0.001(3) 0.006(3)
O9 0.051(3) 0.050(3) 0.059(3) 0.003(3) -0.004(3) 0.000(3)
C2 0.027(3) 0.037(4) 0.029(3) 0.002(3) -0.004(3) 0.007(3)
C19 0.038(4) 0.046(4) 0.040(4) 0.005(3) 0.006(4) -0.012(4)
C16 0.030(3) 0.028(3) 0.026(3) 0.000(3) -0.001(3) 0.006(3)
C10 0.037(4) 0.048(5) 0.027(3) -0.013(3) -0.006(3) 0.000(4)
C1 0.030(4) 0.036(3) 0.022(3) 0.002(3) 0.002(3) 0.005(3)
O6 0.036(3) 0.060(3) 0.041(3) -0.007(3) -0.002(2) -0.005(3)
N3 0.030(3) 0.043(4) 0.059(4) 0.002(3) -0.011(3) -0.002(3)
O7 0.041(3) 0.067(4) 0.069(4) -0.029(3) -0.011(3) -0.002(3)
O11 0.076(5) 0.044(3) 0.100(5) 0.029(4) 0.041(4) 0.022(3)
C7 0.035(4) 0.033(4) 0.043(4) -0.007(3) 0.008(3) 0.000(3)
C14 0.048(5) 0.041(4) 0.029(4) 0.006(3) 0.000(3) -0.003(4)
C13 0.052(5) 0.059(5) 0.025(4) 0.001(3) 0.006(3) 0.008(4)
C6 0.032(4) 0.042(5) 0.032(3) -0.003(3) 0.003(3) 0.001(4)
C3 0.038(4) 0.057(5) 0.025(3) -0.003(3) -0.002(3) 0.005(4)
C9 0.035(4) 0.047(5) 0.045(4) -0.010(4) -0.007(3) -0.009(4)
C5 0.041(4) 0.054(5) 0.029(3) 0.007(3) 0.010(3) -0.006(4)
C8 0.036(4) 0.043(4) 0.044(4) -0.012(4) 0.004(4) -0.010(3)
C12 0.054(5) 0.053(5) 0.025(3) -0.009(3) -0.015(3) 0.016(4)
C17 0.054(5) 0.031(3) 0.032(3) -0.006(3) -0.001(4) -0.007(4)
C20 0.049(5) 0.065(5) 0.044(4) 0.011(4) 0.007(4) 0.000(5)
C4 0.043(4) 0.068(5) 0.024(4) -0.003(4) 0.013(3) -0.002(4)
C18 0.055(5) 0.070(6) 0.028(4) 0.001(4) -0.002(4) -0.015(5)
O5 0.032(3) 0.099(6) 0.108(6) -0.025(5) -0.014(4) -0.004(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'
Ni Ni 0.3393 1.1124 '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'
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 Eu O2 62.26(15) . . ?
O1 Eu O10 123.99(16) . . ?
O2 Eu O10 114.49(18) . . ?
O1 Eu O6 141.77(17) . . ?
O2 Eu O6 116.22(17) . . ?
O10 Eu O6 92.44(19) . . ?
O1 Eu O13 73.36(17) . . ?
O2 Eu O13 112.42(16) . . ?
O10 Eu O13 132.53(19) . . ?
O6 Eu O13 73.04(18) . . ?
O1 Eu O9 80.70(18) . . ?
O2 Eu O9 71.69(18) . . ?
O10 Eu O9 50.81(19) . . ?
O6 Eu O9 137.04(19) . . ?
O13 Eu O9 146.46(18) . . ?
O1 Eu O12 75.80(18) . . ?
O2 Eu O12 69.97(18) . . ?
O10 Eu O12 159.98(19) . . ?
O6 Eu O12 69.04(19) . . ?
O13 Eu O12 50.82(18) . . ?
O9 Eu O12 141.05(19) . . ?
O1 Eu O7 131.45(19) . . ?
O2 Eu O7 165.20(18) . . ?
O10 Eu O7 64.7(2) . . ?
O6 Eu O7 50.32(18) . . ?
O13 Eu O7 71.9(2) . . ?
O9 Eu O7 113.11(19) . . ?
O12 Eu O7 105.7(2) . . ?
O1 Eu O3 63.04(15) . . ?
O2 Eu O3 120.26(15) . . ?
O10 Eu O3 78.88(17) . . ?
O6 Eu O3 121.17(16) . . ?
O13 Eu O3 71.79(16) . . ?
O9 Eu O3 77.71(18) . . ?
O12 Eu O3 116.70(18) . . ?
O7 Eu O3 74.48(18) . . ?
O1 Eu O4 123.64(15) . . ?
O2 Eu O4 61.42(15) . . ?
O10 Eu O4 78.95(17) . . ?
O6 Eu O4 69.93(17) . . ?
O13 Eu O4 131.90(17) . . ?
O9 Eu O4 80.40(18) . . ?
O12 Eu O4 87.27(18) . . ?
O7 Eu O4 104.80(19) . . ?
O3 Eu O4 155.58(18) . . ?
O1 Eu N4 101.81(18) . . ?
O2 Eu N4 93.91(18) . . ?
O10 Eu N4 25.56(18) . . ?
O6 Eu N4 116.19(19) . . ?
O13 Eu N4 145.23(17) . . ?
O9 Eu N4 25.33(18) . . ?
O12 Eu N4 163.05(18) . . ?
O7 Eu N4 88.5(2) . . ?
O3 Eu N4 75.46(17) . . ?
O4 Eu N4 80.12(17) . . ?
O1 Eu N5 72.58(17) . . ?
O2 Eu N5 91.05(19) . . ?
O10 Eu N5 153.6(2) . . ?
O6 Eu N5 69.24(18) . . ?
O13 Eu N5 25.42(19) . . ?
O9 Eu N5 152.80(19) . . ?
O12 Eu N5 25.40(19) . . ?
O7 Eu N5 89.0(2) . . ?
O3 Eu N5 94.21(19) . . ?
O4 Eu N5 110.21(18) . . ?
N4 Eu N5 169.67(19) . . ?
N1 Ni N2 86.4(3) . . ?
N1 Ni O2 175.1(3) . . ?
N2 Ni O2 95.8(2) . . ?
N1 Ni O1 94.6(2) . . ?
N2 Ni O1 176.5(2) . . ?
O2 Ni O1 83.4(2) . . ?
N1 Ni Eu 134.89(19) . . ?
N2 Ni Eu 138.37(19) . . ?
O2 Ni Eu 42.58(14) . . ?
O1 Ni Eu 41.09(14) . . ?
C1 O1 Ni 124.4(4) . . ?
C1 O1 Eu 126.4(4) . . ?
Ni O1 Eu 107.8(2) . . ?
C7 N1 C8 121.6(6) . . ?
C7 N1 Ni 126.4(6) . . ?
C8 N1 Ni 111.9(5) . . ?
C16 O2 Ni 125.8(5) . . ?
C16 O2 Eu 128.1(4) . . ?
Ni O2 Eu 106.11(18) . . ?
C10 N2 C9 119.5(6) . . ?
C10 N2 Ni 126.3(5) . . ?
C9 N2 Ni 113.8(4) . . ?
N5 O12 Eu 95.4(5) . . ?
N5 O13 Eu 96.6(4) . . ?
O11 N5 O12 121.6(8) . . ?
O11 N5 O13 121.2(8) . . ?
O12 N5 O13 117.2(7) . . ?
O11 N5 Eu 177.9(5) . . ?
O12 N5 Eu 59.3(4) . . ?
O13 N5 Eu 58.0(4) . . ?
N4 O10 Eu 97.8(4) . . ?
C2 O3 C17 118.5(5) . . ?
C2 O3 Eu 118.3(4) . . ?
C17 O3 Eu 123.0(4) . . ?
C15 O4 C19 116.6(5) . . ?
C15 O4 Eu 120.4(4) . . ?
C19 O4 Eu 123.0(4) . . ?
O8 N4 O9 122.3(8) . . ?
O8 N4 O10 122.1(7) . . ?
O9 N4 O10 115.6(6) . . ?
O8 N4 Eu 173.6(5) . . ?
O9 N4 Eu 59.2(4) . . ?
O10 N4 Eu 56.6(3) . . ?
C16 C11 C10 122.2(6) . . ?
C16 C11 C12 119.9(7) . . ?
C10 C11 C12 117.9(7) . . ?
C14 C15 O4 126.1(7) . . ?
C14 C15 C16 120.7(7) . . ?
O4 C15 C16 113.1(6) . . ?
N4 O9 Eu 95.4(5) . . ?
C3 C2 O3 125.2(7) . . ?
C3 C2 C1 120.4(7) . . ?
O3 C2 C1 114.4(6) . . ?
O4 C19 C20 111.9(6) . . ?
O2 C16 C11 124.4(6) . . ?
O2 C16 C15 116.8(6) . . ?
C11 C16 C15 118.8(6) . . ?
N2 C10 C11 125.2(6) . . ?
O1 C1 C6 123.6(6) . . ?
O1 C1 C2 117.2(6) . . ?
C6 C1 C2 119.1(6) . . ?
N3 O6 Eu 98.8(4) . . ?
O5 N3 O6 122.9(8) . . ?
O5 N3 O7 121.0(8) . . ?
O6 N3 O7 116.1(6) . . ?
O5 N3 Eu 178.7(7) . . ?
O6 N3 Eu 56.5(4) . . ?
O7 N3 Eu 59.6(4) . . ?
N3 O7 Eu 94.8(4) . . ?
N1 C7 C6 124.8(7) . . ?
C15 C14 C13 120.2(7) . . ?
C12 C13 C14 120.8(7) . . ?
C1 C6 C5 119.3(7) . . ?
C1 C6 C7 121.6(6) . . ?
C5 C6 C7 119.1(7) . . ?
C2 C3 C4 119.8(7) . . ?
N2 C9 C8 105.4(6) . . ?
C4 C5 C6 120.4(7) . . ?
N1 C8 C9 106.4(6) . . ?
C13 C12 C11 119.5(7) . . ?
O3 C17 C18 112.4(6) . . ?
C5 C4 C3 120.9(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
Eu O1 2.371(4) . ?
Eu O2 2.419(5) . ?
Eu O10 2.465(5) . ?
Eu O6 2.489(5) . ?
Eu O13 2.505(6) . ?
Eu O9 2.524(6) . ?
Eu O12 2.533(6) . ?
Eu O7 2.555(6) . ?
Eu O3 2.580(5) . ?
Eu O4 2.606(5) . ?
Eu N4 2.924(6) . ?
Eu N5 2.935(7) . ?
Ni N1 1.842(6) . ?
Ni N2 1.844(6) . ?
Ni O2 1.858(5) . ?
Ni O1 1.865(5) . ?
O1 C1 1.341(8) . ?
N1 C7 1.295(9) . ?
N1 C8 1.480(9) . ?
O2 C16 1.331(7) . ?
N2 C10 1.286(9) . ?
N2 C9 1.495(10) . ?
O12 N5 1.264(9) . ?
O13 N5 1.268(9) . ?
N5 O11 1.221(9) . ?
O10 N4 1.273(8) . ?
O3 C2 1.385(8) . ?
O3 C17 1.462(8) . ?
O4 C15 1.393(9) . ?
O4 C19 1.457(8) . ?
N4 O8 1.224(8) . ?
N4 O9 1.257(8) . ?
C11 C16 1.392(10) . ?
C11 C10 1.437(11) . ?
C11 C12 1.443(10) . ?
C15 C14 1.385(10) . ?
C15 C16 1.421(10) . ?
C2 C3 1.380(10) . ?
C2 C1 1.408(10) . ?
C19 C20 1.500(11) . ?
C1 C6 1.395(10) . ?
O6 N3 1.249(9) . ?
N3 O5 1.211(9) . ?
N3 O7 1.279(9) . ?
C7 C6 1.442(10) . ?
C14 C13 1.398(11) . ?
C13 C12 1.373(11) . ?
C6 C5 1.412(10) . ?
C3 C4 1.390(11) . ?
C9 C8 1.499(11) . ?
C5 C4 1.359(11) . ?
C17 C18 1.502(11) . ?
|
1100957.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100957.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_1100957
loop_
_publ_author_name
'Rajesh Koner'
'Hsin-Huang Lin'
'Ho-Hsiang Wei'
'Sasankasekhar Mohanta'
_publ_section_title
;
Syntheses, Structures, and Magnetic Properties of Diphenoxo-Bridged
MIILnIII Complexes Derived from N,N'-Ethylenebis(3-ethoxysalicylaldiimine)
(M = Cu or Ni; Ln = Ce-Yb): Observation of Surprisingly Strong Exchange
Interactions
;
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3524
_journal_page_last 3536
_journal_paper_doi 10.1021/ic048196h
_journal_volume 44
_journal_year 2005
_chemical_formula_sum 'C20 H22 N5 Ni O13 Tb'
_chemical_formula_weight 758.06
_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 8.607(3)
_cell_length_b 21.240(4)
_cell_length_c 13.742(3)
_cell_measurement_temperature 293(2)
_cell_volume 2512.2(11)
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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 0.0347
_diffrn_reflns_limit_h_max 1
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 1
_diffrn_reflns_limit_k_min -25
_diffrn_reflns_limit_l_max 1
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_number 2526
_diffrn_reflns_theta_full 24.99
_diffrn_reflns_theta_max 24.99
_diffrn_reflns_theta_min 1.92
_exptl_absorpt_coefficient_mu 3.620
_exptl_crystal_colour Red
_exptl_crystal_density_diffrn 2.004
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1496
_exptl_crystal_size_max 55
_exptl_crystal_size_mid 30
_exptl_crystal_size_min 15
_refine_diff_density_max 0.853
_refine_diff_density_min -0.519
_refine_diff_density_rms 0.092
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack -0.03(2)
_refine_ls_extinction_coef 0.00167(14)
_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 1.059
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 362
_refine_ls_number_reflns 2526
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.059
_refine_ls_R_factor_all 0.0316
_refine_ls_R_factor_gt 0.0265
_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^)+(0.0349P)^2^+0.7501P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0659
_refine_ls_wR_factor_ref 0.0698
_reflns_number_gt 2280
_reflns_number_total 2526
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file ic048196hsi20050224_082436_12.cif
_cod_data_source_block nitb
_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 2512.1(11)
_cod_database_code 1100957
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
Tb Tb 0.49643(3) 0.151345(12) 0.249626(19) 0.02728(12) Uani 1 1 d . . .
Ni Ni 0.81595(9) 0.06452(4) 0.30981(5) 0.02873(19) Uani 1 1 d . . .
O10 O 0.4742(6) 0.2659(2) 0.2439(4) 0.0483(12) Uani 1 1 d . . .
N1 N 0.9495(6) 0.0128(3) 0.2433(4) 0.0346(12) Uani 1 1 d . . .
O1 O 0.7152(5) 0.0946(2) 0.1991(3) 0.0319(10) Uani 1 1 d . . .
O4 O 0.4356(5) 0.1794(2) 0.4304(3) 0.0347(10) Uani 1 1 d . . .
N4 N 0.6172(8) 0.2788(3) 0.2593(4) 0.0422(14) Uani 1 1 d . . .
O12 O 0.4301(6) 0.0398(2) 0.2924(4) 0.0487(14) Uani 1 1 d . . .
C7 C 0.9736(8) 0.0119(3) 0.1501(5) 0.0335(15) Uani 1 1 d . . .
H7A H 1.0422 -0.0180 0.1257 0.040 Uiso 1 1 calc R . .
O8 O 0.6678(9) 0.3327(3) 0.2542(4) 0.0705(17) Uani 1 1 d . . .
C6 C 0.9002(7) 0.0548(3) 0.0810(4) 0.0313(15) Uani 1 1 d . . .
N2 N 0.9223(6) 0.0403(3) 0.4197(4) 0.0310(12) Uani 1 1 d . . .
N5 N 0.3936(7) 0.0237(3) 0.2061(5) 0.0413(15) Uani 1 1 d . . .
O13 O 0.4000(6) 0.0665(3) 0.1413(3) 0.0450(12) Uani 1 1 d . . .
C11 C 0.7689(8) 0.0995(3) 0.5364(5) 0.0336(15) Uani 1 1 d . . .
O9 O 0.7013(7) 0.2325(2) 0.2781(4) 0.0550(14) Uani 1 1 d . . .
C15 C 0.5359(8) 0.1603(3) 0.5032(4) 0.0320(15) Uani 1 1 d . . .
C10 C 0.8939(7) 0.0584(3) 0.5082(4) 0.0347(15) Uani 1 1 d . . .
H10A H 0.9592 0.0436 0.5571 0.042 Uiso 1 1 calc R . .
O2 O 0.6685(6) 0.1129(2) 0.3738(3) 0.0340(10) Uani 1 1 d . . .
C16 C 0.6605(7) 0.1231(3) 0.4710(4) 0.0275(13) Uani 1 1 d . . .
C14 C 0.5224(9) 0.1753(3) 0.6015(4) 0.0404(17) Uani 1 1 d . . .
H14A H 0.4387 0.1991 0.6232 0.048 Uiso 1 1 calc R . .
C12 C 0.7556(10) 0.1165(4) 0.6366(5) 0.0455(19) Uani 1 1 d . . .
H12A H 0.8285 0.1021 0.6813 0.055 Uiso 1 1 calc R . .
C13 C 0.6340(9) 0.1545(3) 0.6672(4) 0.0466(19) Uani 1 1 d . . .
H13A H 0.6271 0.1662 0.7323 0.056 Uiso 1 1 calc R . .
O6 O 0.2181(5) 0.1398(2) 0.2830(3) 0.0448(12) Uani 1 1 d . . .
O3 O 0.5950(6) 0.1735(2) 0.0774(3) 0.0340(10) Uani 1 1 d . . .
N3 N 0.1650(7) 0.1712(3) 0.2109(5) 0.0425(14) Uani 1 1 d . . .
C19 C 0.2985(8) 0.2150(3) 0.4607(5) 0.0391(16) Uani 1 1 d . . .
H19A H 0.2569 0.2377 0.4052 0.047 Uiso 1 1 calc R . .
H19B H 0.3284 0.2457 0.5095 0.047 Uiso 1 1 calc R . .
C2 C 0.7151(7) 0.1358(3) 0.0418(4) 0.0297(14) Uani 1 1 d . . .
O11 O 0.3549(7) -0.0300(2) 0.1852(5) 0.0705(18) Uani 1 1 d . . .
C20 C 0.1757(10) 0.1731(4) 0.5014(6) 0.056(2) Uani 1 1 d . . .
H20A H 0.0876 0.1980 0.5205 0.084 Uiso 1 1 calc R . .
H20B H 0.2159 0.1512 0.5571 0.084 Uiso 1 1 calc R . .
H20C H 0.1445 0.1431 0.4529 0.084 Uiso 1 1 calc R . .
C3 C 0.7755(8) 0.1391(4) -0.0530(4) 0.0410(17) Uani 1 1 d . . .
H3A H 0.7361 0.1682 -0.0971 0.049 Uiso 1 1 calc R . .
C8 C 1.0254(8) -0.0342(3) 0.3075(5) 0.0429(16) Uani 1 1 d . . .
H8A H 1.1205 -0.0498 0.2782 0.051 Uiso 1 1 calc R . .
H8B H 0.9566 -0.0695 0.3197 0.051 Uiso 1 1 calc R . .
C5 C 0.9561(8) 0.0575(4) -0.0156(5) 0.0436(18) Uani 1 1 d . . .
H5A H 1.0361 0.0309 -0.0352 0.052 Uiso 1 1 calc R . .
C17 C 0.5263(8) 0.2210(3) 0.0124(5) 0.0363(15) Uani 1 1 d . . .
H17A H 0.6088 0.2423 -0.0225 0.044 Uiso 1 1 calc R . .
H17B H 0.4720 0.2521 0.0512 0.044 Uiso 1 1 calc R . .
C9 C 1.0594(9) 0.0004(3) 0.3998(5) 0.0449(18) Uani 1 1 d . . .
H9A H 1.0763 -0.0290 0.4528 0.054 Uiso 1 1 calc R . .
H9B H 1.1517 0.0262 0.3924 0.054 Uiso 1 1 calc R . .
C1 C 0.7762(8) 0.0934(3) 0.1091(4) 0.0297(14) Uani 1 1 d . . .
C4 C 0.8927(9) 0.0992(4) -0.0803(5) 0.0455(19) Uani 1 1 d . . .
H4A H 0.9298 0.1004 -0.1438 0.055 Uiso 1 1 calc R . .
O5 O 0.0265(6) 0.1795(3) 0.1996(6) 0.079(2) Uani 1 1 d . . .
O7 O 0.2651(6) 0.1937(3) 0.1535(4) 0.0567(15) Uani 1 1 d . . .
C18 C 0.4143(9) 0.1927(4) -0.0602(5) 0.051(2) Uani 1 1 d . . .
H18A H 0.3727 0.2254 -0.1007 0.076 Uiso 1 1 calc R . .
H18B H 0.3311 0.1723 -0.0260 0.076 Uiso 1 1 calc R . .
H18C H 0.4679 0.1625 -0.0998 0.076 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
Tb 0.02835(17) 0.03133(18) 0.02217(17) 0.00257(12) -0.00056(17) 0.00289(11)
Ni 0.0277(4) 0.0355(4) 0.0230(3) 0.0052(4) -0.0002(3) 0.0051(4)
O10 0.053(3) 0.043(3) 0.048(3) 0.003(2) -0.007(3) 0.008(2)
N1 0.032(3) 0.038(3) 0.034(3) 0.009(3) -0.001(3) 0.002(2)
O1 0.034(2) 0.039(2) 0.022(2) 0.0049(19) 0.001(2) 0.003(2)
O4 0.036(2) 0.043(3) 0.025(2) 0.000(2) 0.003(2) 0.009(2)
N4 0.062(4) 0.031(3) 0.033(3) 0.000(3) -0.005(3) -0.002(3)
O12 0.051(3) 0.046(3) 0.049(3) 0.011(3) 0.008(3) 0.003(3)
C7 0.029(3) 0.037(3) 0.034(3) 0.002(3) 0.006(3) 0.004(3)
O8 0.107(5) 0.042(3) 0.062(3) -0.005(3) -0.012(4) -0.024(3)
C6 0.028(3) 0.036(4) 0.030(3) 0.002(3) 0.007(3) 0.002(3)
N2 0.027(3) 0.035(3) 0.030(3) 0.011(2) -0.002(2) 0.002(2)
N5 0.037(3) 0.038(3) 0.049(4) -0.005(3) 0.014(3) 0.006(3)
O13 0.051(3) 0.050(3) 0.033(2) -0.001(3) 0.002(2) 0.001(3)
C11 0.039(4) 0.033(3) 0.028(3) 0.005(3) 0.001(3) -0.003(3)
O9 0.052(3) 0.050(3) 0.064(3) 0.002(3) -0.003(3) 0.003(3)
C15 0.040(4) 0.033(3) 0.024(3) -0.002(3) 0.001(3) -0.003(3)
C10 0.029(3) 0.048(4) 0.027(3) 0.013(3) -0.008(3) -0.003(3)
O2 0.037(3) 0.047(3) 0.0183(19) 0.0012(19) 0.002(2) 0.010(2)
C16 0.031(3) 0.029(3) 0.022(3) 0.004(2) 0.002(3) -0.005(3)
C14 0.052(5) 0.046(4) 0.023(3) -0.006(3) 0.006(3) 0.003(4)
C12 0.059(5) 0.054(4) 0.024(3) 0.003(3) -0.008(3) -0.007(4)
C13 0.065(5) 0.057(5) 0.018(3) -0.001(3) -0.001(3) -0.010(4)
O6 0.036(3) 0.060(3) 0.039(3) 0.007(2) -0.004(2) 0.005(3)
O3 0.045(3) 0.035(2) 0.021(2) 0.005(2) -0.001(2) 0.007(2)
N3 0.034(3) 0.044(3) 0.050(3) 0.001(3) -0.013(3) 0.001(3)
C19 0.036(4) 0.042(4) 0.039(3) -0.007(3) 0.001(3) 0.009(3)
C2 0.029(3) 0.036(3) 0.024(3) -0.002(3) -0.001(3) -0.003(3)
O11 0.073(4) 0.039(3) 0.099(5) -0.020(3) 0.035(4) -0.015(3)
C20 0.051(5) 0.062(5) 0.055(5) -0.005(4) 0.010(4) -0.002(5)
C3 0.043(4) 0.059(4) 0.021(3) 0.013(3) -0.002(3) -0.001(4)
C8 0.041(4) 0.043(4) 0.046(4) 0.018(3) 0.008(4) 0.012(3)
C5 0.037(4) 0.059(5) 0.036(3) -0.008(4) 0.006(3) 0.003(4)
C17 0.047(4) 0.033(3) 0.029(3) 0.010(3) -0.001(3) 0.005(3)
C9 0.037(4) 0.045(4) 0.052(4) 0.012(4) 0.004(3) 0.015(3)
C1 0.036(4) 0.034(3) 0.020(3) 0.001(3) 0.002(3) -0.012(3)
C4 0.041(4) 0.069(5) 0.027(3) 0.004(3) 0.011(3) 0.001(4)
O5 0.035(3) 0.090(5) 0.113(5) 0.019(5) -0.016(4) 0.005(3)
O7 0.044(3) 0.066(4) 0.060(3) 0.029(3) -0.007(3) -0.001(3)
C18 0.048(4) 0.071(5) 0.033(4) 0.000(4) -0.011(4) 0.010(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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 '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 Tb O2 62.60(14) . . ?
O1 Tb O10 124.50(16) . . ?
O2 Tb O10 114.20(17) . . ?
O1 Tb O6 142.21(16) . . ?
O2 Tb O6 115.83(16) . . ?
O10 Tb O6 91.65(17) . . ?
O1 Tb O13 73.56(16) . . ?
O2 Tb O13 112.69(15) . . ?
O10 Tb O13 132.71(18) . . ?
O6 Tb O13 73.33(17) . . ?
O1 Tb O9 80.42(17) . . ?
O2 Tb O9 71.80(17) . . ?
O10 Tb O9 51.15(17) . . ?
O6 Tb O9 136.87(18) . . ?
O13 Tb O9 146.29(17) . . ?
O1 Tb O12 76.47(17) . . ?
O2 Tb O12 69.68(17) . . ?
O10 Tb O12 158.67(18) . . ?
O6 Tb O12 68.87(17) . . ?
O13 Tb O12 51.53(17) . . ?
O9 Tb O12 140.93(18) . . ?
O1 Tb O7 130.92(17) . . ?
O2 Tb O7 165.47(16) . . ?
O10 Tb O7 64.62(18) . . ?
O6 Tb O7 50.94(16) . . ?
O13 Tb O7 71.59(18) . . ?
O9 Tb O7 112.90(17) . . ?
O12 Tb O7 106.05(18) . . ?
O1 Tb O3 63.48(14) . . ?
O2 Tb O3 121.02(14) . . ?
O10 Tb O3 79.21(16) . . ?
O6 Tb O3 121.04(15) . . ?
O13 Tb O3 71.88(15) . . ?
O9 Tb O3 77.53(17) . . ?
O12 Tb O3 117.78(16) . . ?
O7 Tb O3 73.44(16) . . ?
O1 Tb O4 124.18(14) . . ?
O2 Tb O4 61.64(14) . . ?
O10 Tb O4 77.72(16) . . ?
O6 Tb O4 69.40(15) . . ?
O13 Tb O4 132.12(15) . . ?
O9 Tb O4 80.48(16) . . ?
O12 Tb O4 86.97(16) . . ?
O7 Tb O4 104.83(17) . . ?
O3 Tb O4 154.96(17) . . ?
O1 Tb N4 101.88(17) . . ?
O2 Tb N4 93.65(17) . . ?
O10 Tb N4 25.88(16) . . ?
O6 Tb N4 115.73(18) . . ?
O13 Tb N4 145.58(16) . . ?
O9 Tb N4 25.35(17) . . ?
O12 Tb N4 162.20(17) . . ?
O7 Tb N4 88.55(19) . . ?
O3 Tb N4 75.67(16) . . ?
O4 Tb N4 79.33(16) . . ?
O1 Tb N5 72.81(15) . . ?
O2 Tb N5 90.96(17) . . ?
O10 Tb N5 153.72(18) . . ?
O6 Tb N5 69.44(16) . . ?
O13 Tb N5 25.75(16) . . ?
O9 Tb N5 152.73(17) . . ?
O12 Tb N5 25.78(17) . . ?
O7 Tb N5 89.11(19) . . ?
O3 Tb N5 94.70(16) . . ?
O4 Tb N5 110.31(16) . . ?
N4 Tb N5 170.36(17) . . ?
N1 Ni N2 86.0(3) . . ?
N1 Ni O2 175.6(2) . . ?
N2 Ni O2 96.1(2) . . ?
N1 Ni O1 95.2(2) . . ?
N2 Ni O1 175.9(2) . . ?
O2 Ni O1 83.04(18) . . ?
N1 Ni Tb 135.06(18) . . ?
N2 Ni Tb 138.67(17) . . ?
O2 Ni Tb 42.62(13) . . ?
O1 Ni Tb 40.73(13) . . ?
N4 O10 Tb 97.6(4) . . ?
C7 N1 C8 120.4(6) . . ?
C7 N1 Ni 126.9(5) . . ?
C8 N1 Ni 112.5(4) . . ?
C1 O1 Ni 124.3(4) . . ?
C1 O1 Tb 126.6(4) . . ?
Ni O1 Tb 107.96(19) . . ?
C15 O4 C19 116.7(5) . . ?
C15 O4 Tb 119.8(4) . . ?
C19 O4 Tb 123.5(4) . . ?
O8 N4 O9 122.8(7) . . ?
O8 N4 O10 122.1(6) . . ?
O9 N4 O10 115.1(6) . . ?
O8 N4 Tb 174.0(5) . . ?
O9 N4 Tb 58.8(3) . . ?
O10 N4 Tb 56.5(3) . . ?
N5 O12 Tb 95.3(4) . . ?
N1 C7 C6 124.3(6) . . ?
C1 C6 C5 119.7(6) . . ?
C1 C6 C7 121.0(5) . . ?
C5 C6 C7 119.3(6) . . ?
C10 N2 C9 119.6(6) . . ?
C10 N2 Ni 126.4(5) . . ?
C9 N2 Ni 113.9(4) . . ?
O11 N5 O12 122.5(7) . . ?
O11 N5 O13 120.9(7) . . ?
O12 N5 O13 116.6(6) . . ?
O11 N5 Tb 177.5(5) . . ?
O12 N5 Tb 58.9(3) . . ?
O13 N5 Tb 57.7(3) . . ?
N5 O13 Tb 96.5(4) . . ?
C16 C11 C12 118.6(6) . . ?
C16 C11 C10 123.1(6) . . ?
C12 C11 C10 118.3(6) . . ?
N4 O9 Tb 95.8(4) . . ?
O4 C15 C14 125.7(6) . . ?
O4 C15 C16 114.5(5) . . ?
C14 C15 C16 119.8(6) . . ?
N2 C10 C11 124.9(6) . . ?
C16 O2 Ni 126.2(4) . . ?
C16 O2 Tb 127.9(4) . . ?
Ni O2 Tb 105.87(17) . . ?
O2 C16 C11 123.1(6) . . ?
O2 C16 C15 116.0(6) . . ?
C11 C16 C15 120.8(5) . . ?
C13 C14 C15 120.1(7) . . ?
C13 C12 C11 120.0(7) . . ?
C12 C13 C14 120.6(6) . . ?
N3 O6 Tb 98.8(4) . . ?
C2 O3 C17 118.5(5) . . ?
C2 O3 Tb 117.7(3) . . ?
C17 O3 Tb 123.7(4) . . ?
O5 N3 O7 122.3(7) . . ?
O5 N3 O6 121.7(7) . . ?
O7 N3 O6 115.9(6) . . ?
O5 N3 Tb 176.9(6) . . ?
O7 N3 Tb 60.2(3) . . ?
O6 N3 Tb 55.7(3) . . ?
O4 C19 C20 111.7(6) . . ?
C1 C2 O3 114.6(5) . . ?
C1 C2 C3 120.5(6) . . ?
O3 C2 C3 124.9(6) . . ?
C4 C3 C2 119.7(6) . . ?
N1 C8 C9 105.0(6) . . ?
C4 C5 C6 120.0(7) . . ?
O3 C17 C18 112.6(6) . . ?
N2 C9 C8 106.4(6) . . ?
O1 C1 C2 116.8(6) . . ?
O1 C1 C6 124.3(6) . . ?
C2 C1 C6 118.8(5) . . ?
C5 C4 C3 121.1(6) . . ?
N3 O7 Tb 94.3(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
Tb O1 2.341(4) . ?
Tb O2 2.402(4) . ?
Tb O10 2.443(5) . ?
Tb O6 2.451(5) . ?
Tb O13 2.480(5) . ?
Tb O9 2.496(6) . ?
Tb O12 2.506(5) . ?
Tb O7 2.553(5) . ?
Tb O3 2.558(4) . ?
Tb O4 2.608(4) . ?
Tb N4 2.903(6) . ?
Tb N5 2.914(6) . ?
Ni N1 1.834(6) . ?
Ni N2 1.840(5) . ?
Ni O2 1.855(4) . ?
Ni O1 1.864(4) . ?
O10 N4 1.278(8) . ?
N1 C7 1.298(8) . ?
N1 C8 1.484(8) . ?
O1 C1 1.343(7) . ?
O4 C15 1.382(8) . ?
O4 C19 1.462(8) . ?
N4 O8 1.227(7) . ?
N4 O9 1.249(7) . ?
O12 N5 1.273(8) . ?
C7 C6 1.460(9) . ?
C6 C1 1.400(9) . ?
C6 C5 1.413(9) . ?
N2 C10 1.298(8) . ?
N2 C9 1.479(9) . ?
N5 O11 1.223(8) . ?
N5 O13 1.274(8) . ?
C11 C16 1.389(9) . ?
C11 C12 1.428(9) . ?
C11 C10 1.439(9) . ?
C15 C14 1.392(9) . ?
C15 C16 1.404(9) . ?
O2 C16 1.355(7) . ?
C14 C13 1.390(10) . ?
C12 C13 1.387(11) . ?
O6 N3 1.279(8) . ?
O3 C2 1.396(8) . ?
O3 C17 1.471(7) . ?
N3 O5 1.215(8) . ?
N3 O7 1.262(8) . ?
C19 C20 1.491(10) . ?
C2 C1 1.395(9) . ?
C2 C3 1.404(9) . ?
C3 C4 1.370(10) . ?
C8 C9 1.495(11) . ?
C5 C4 1.368(10) . ?
C17 C18 1.511(10) . ?
|
1100958.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100958.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_1100958
loop_
_publ_author_name
'Rajesh Koner'
'Hsin-Huang Lin'
'Ho-Hsiang Wei'
'Sasankasekhar Mohanta'
_publ_section_title
;
Syntheses, Structures, and Magnetic Properties of Diphenoxo-Bridged
MIILnIII Complexes Derived from N,N'-Ethylenebis(3-ethoxysalicylaldiimine)
(M = Cu or Ni; Ln = Ce-Yb): Observation of Surprisingly Strong Exchange
Interactions
;
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3524
_journal_page_last 3536
_journal_paper_doi 10.1021/ic048196h
_journal_volume 44
_journal_year 2005
_chemical_formula_sum 'C20 H22 Er N5 Ni O13'
_chemical_formula_weight 766.40
_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 8.601(4)
_cell_length_b 13.710(4)
_cell_length_c 21.252(5)
_cell_measurement_temperature 293(2)
_cell_volume 2506.0(15)
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 293(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 0.0000
_diffrn_reflns_av_sigmaI/netI 0.0329
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -1
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min -1
_diffrn_reflns_limit_l_max 25
_diffrn_reflns_limit_l_min -1
_diffrn_reflns_number 2515
_diffrn_reflns_theta_full 24.99
_diffrn_reflns_theta_max 24.99
_diffrn_reflns_theta_min 1.92
_exptl_absorpt_coefficient_mu 4.156
_exptl_crystal_colour Red
_exptl_crystal_density_diffrn 2.031
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1508
_exptl_crystal_size_max 50
_exptl_crystal_size_mid 32
_exptl_crystal_size_min 20
_refine_diff_density_max 0.728
_refine_diff_density_min -0.651
_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 -0.02(2)
_refine_ls_extinction_coef 0.00064(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 1.134
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 362
_refine_ls_number_reflns 2515
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.134
_refine_ls_R_factor_all 0.0331
_refine_ls_R_factor_gt 0.0253
_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^)+(0.0228P)^2^+3.8857P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0607
_refine_ls_wR_factor_ref 0.0705
_reflns_number_gt 2266
_reflns_number_total 2515
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file ic048196hsi20050224_082436_13.cif
_cod_data_source_block nier
_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 2506.0(14)
_cod_database_code 1100958
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
Er Er 0.75352(4) 0.50103(2) 0.100335(13) 0.02767(12) Uani 1 1 d . . .
Ni Ni 0.43543(11) 0.44047(7) 0.18550(5) 0.0296(2) Uani 1 1 d . . .
O1 O 0.5368(6) 0.5511(4) 0.1561(2) 0.0305(11) Uani 1 1 d . . .
N1 N 0.3018(7) 0.5076(5) 0.2371(3) 0.0343(14) Uani 1 1 d . . .
N2 N 0.3293(8) 0.3297(5) 0.2099(3) 0.0337(16) Uani 1 1 d . . .
C16 C 0.5933(9) 0.2811(5) 0.1266(4) 0.0300(17) Uani 1 1 d . . .
C10 C 0.3566(10) 0.2418(6) 0.1899(4) 0.040(2) Uani 1 1 d . . .
H10A H 0.2875 0.1932 0.2020 0.048 Uiso 1 1 calc R . .
O2 O 0.5838(7) 0.3771(3) 0.1375(3) 0.0349(13) Uani 1 1 d . . .
C6 C 0.3503(9) 0.6694(5) 0.1955(4) 0.0318(18) Uani 1 1 d . . .
C7 C 0.2762(9) 0.6005(6) 0.2376(4) 0.0348(18) Uani 1 1 d . . .
H7A H 0.2057 0.6247 0.2669 0.042 Uiso 1 1 calc R . .
O4 O 0.8165(7) 0.3214(4) 0.0708(3) 0.0368(13) Uani 1 1 d . . .
C15 C 0.7182(9) 0.2477(5) 0.0901(4) 0.0324(18) Uani 1 1 d . . .
O6 O 1.0280(7) 0.4674(4) 0.1108(3) 0.0444(15) Uani 1 1 d . . .
N3 N 1.0823(9) 0.5397(5) 0.0802(3) 0.0406(17) Uani 1 1 d . . .
C19 C 0.9546(10) 0.2927(6) 0.0349(4) 0.041(2) Uani 1 1 d . . .
H19A H 0.9961 0.3494 0.0133 0.049 Uiso 1 1 calc R . .
H19B H 0.9250 0.2452 0.0032 0.049 Uiso 1 1 calc R . .
C11 C 0.4845(9) 0.2138(6) 0.1506(4) 0.0320(18) Uani 1 1 d . . .
O3 O 0.6588(6) 0.6722(4) 0.0762(2) 0.0333(12) Uani 1 1 d . . .
C2 C 0.5383(9) 0.7091(5) 0.1148(4) 0.0320(18) Uani 1 1 d . . .
C17 C 0.7282(10) 0.7374(6) 0.0295(4) 0.0393(19) Uani 1 1 d . . .
H17A H 0.6459 0.7719 0.0076 0.047 Uiso 1 1 calc R . .
H17B H 0.7841 0.6987 -0.0013 0.047 Uiso 1 1 calc R . .
O5 O 1.2222(7) 0.5489(7) 0.0716(4) 0.078(2) Uani 1 1 d . . .
C3 C 0.4766(10) 0.8028(5) 0.1107(5) 0.044(2) Uani 1 1 d . . .
H3A H 0.5166 0.8468 0.0816 0.053 Uiso 1 1 calc R . .
O7 O 0.9847(8) 0.5989(5) 0.0593(3) 0.0575(19) Uani 1 1 d . . .
C1 C 0.4753(9) 0.6415(5) 0.1549(4) 0.0293(17) Uani 1 1 d . . .
O10 O 0.7818(7) 0.5061(5) -0.0121(3) 0.0471(14) Uani 1 1 d . . .
N4 N 0.6404(9) 0.4914(6) -0.0261(3) 0.0416(17) Uani 1 1 d . . .
O8 O 0.5921(10) 0.4938(5) -0.0804(3) 0.067(2) Uani 1 1 d . . .
O9 O 0.5518(8) 0.4723(4) 0.0201(3) 0.0528(16) Uani 1 1 d . . .
C8 C 0.2249(10) 0.4429(6) 0.2837(4) 0.042(2) Uani 1 1 d . . .
H8A H 0.1298 0.4725 0.2992 0.051 Uiso 1 1 calc R . .
H8B H 0.2933 0.4305 0.3191 0.051 Uiso 1 1 calc R . .
C14 C 0.7302(12) 0.1492(6) 0.0744(4) 0.043(2) Uani 1 1 d . . .
H14A H 0.8129 0.1279 0.0498 0.052 Uiso 1 1 calc R . .
C13 C 0.6198(12) 0.0827(6) 0.0951(4) 0.048(2) Uani 1 1 d . . .
H13A H 0.6268 0.0175 0.0834 0.058 Uiso 1 1 calc R . .
C5 C 0.2966(10) 0.7653(6) 0.1919(4) 0.043(2) Uani 1 1 d . . .
H5A H 0.2179 0.7852 0.2190 0.051 Uiso 1 1 calc R . .
C20 C 1.0774(11) 0.2500(7) 0.0760(5) 0.059(3) Uani 1 1 d . . .
H20A H 1.1657 0.2322 0.0508 0.089 Uiso 1 1 calc R . .
H20B H 1.0373 0.1932 0.0968 0.089 Uiso 1 1 calc R . .
H20C H 1.1084 0.2973 0.1069 0.089 Uiso 1 1 calc R . .
C12 C 0.4997(11) 0.1137(5) 0.1333(4) 0.043(2) Uani 1 1 d . . .
H12A H 0.4274 0.0686 0.1479 0.051 Uiso 1 1 calc R . .
C18 C 0.8383(12) 0.8109(6) 0.0579(5) 0.051(2) Uani 1 1 d . . .
H18A H 0.8800 0.8516 0.0252 0.077 Uiso 1 1 calc R . .
H18B H 0.9216 0.7774 0.0787 0.077 Uiso 1 1 calc R . .
H18C H 0.7834 0.8506 0.0877 0.077 Uiso 1 1 calc R . .
O12 O 0.8179(8) 0.4569(5) 0.2102(3) 0.0478(17) Uani 1 1 d . . .
N5 N 0.8553(9) 0.5440(6) 0.2265(4) 0.0443(19) Uani 1 1 d . . .
C4 C 0.3557(11) 0.8307(6) 0.1499(5) 0.048(2) Uani 1 1 d . . .
H4A H 0.3153 0.8935 0.1476 0.057 Uiso 1 1 calc R . .
C9 C 0.1895(10) 0.3485(6) 0.2484(4) 0.042(2) Uani 1 1 d . . .
H9A H 0.1714 0.2954 0.2777 0.051 Uiso 1 1 calc R . .
H9B H 0.0984 0.3561 0.2220 0.051 Uiso 1 1 calc R . .
O13 O 0.8487(7) 0.6084(4) 0.1848(3) 0.0436(14) Uani 1 1 d . . .
O11 O 0.8953(8) 0.5632(6) 0.2808(3) 0.068(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
Er 0.02794(18) 0.02314(18) 0.03192(18) 0.00227(14) 0.00302(13) 0.0001(2)
Ni 0.0264(5) 0.0232(4) 0.0392(5) 0.0048(4) 0.0057(5) 0.0007(4)
O1 0.027(3) 0.022(2) 0.042(3) 0.006(2) 0.006(2) 0.000(2)
N1 0.029(3) 0.038(4) 0.036(3) 0.006(4) 0.000(3) -0.003(3)
N2 0.029(3) 0.033(4) 0.039(4) 0.010(3) 0.006(3) -0.002(3)
C16 0.030(4) 0.022(3) 0.038(4) -0.002(3) -0.004(4) 0.004(3)
C10 0.041(5) 0.032(4) 0.047(5) 0.013(4) -0.005(5) -0.012(4)
O2 0.035(3) 0.019(2) 0.051(3) -0.001(2) 0.004(3) 0.000(2)
C6 0.030(4) 0.027(4) 0.039(5) 0.004(4) 0.000(4) 0.002(3)
C7 0.031(4) 0.039(4) 0.035(4) 0.004(3) 0.002(4) 0.004(4)
O4 0.036(3) 0.027(3) 0.048(3) 0.000(2) 0.009(3) 0.005(3)
C15 0.032(4) 0.025(4) 0.041(4) 0.001(3) -0.003(4) 0.001(3)
O6 0.039(3) 0.036(3) 0.058(4) 0.007(3) 0.007(3) 0.000(3)
N3 0.036(4) 0.047(4) 0.039(4) -0.003(3) -0.001(4) -0.011(4)
C19 0.038(5) 0.046(5) 0.039(5) -0.009(4) 0.007(4) 0.001(4)
C11 0.034(4) 0.030(4) 0.032(4) 0.003(3) -0.004(4) -0.002(3)
O3 0.039(3) 0.026(3) 0.035(3) 0.006(2) 0.004(3) 0.001(3)
C2 0.028(4) 0.024(4) 0.044(5) -0.001(3) 0.000(4) 0.003(3)
C17 0.047(5) 0.032(4) 0.039(4) 0.010(3) 0.003(4) 0.000(4)
O5 0.034(4) 0.108(6) 0.091(6) 0.011(5) 0.005(4) -0.020(4)
C3 0.039(5) 0.019(4) 0.075(6) 0.013(4) -0.002(5) -0.002(3)
O7 0.043(4) 0.059(4) 0.070(5) 0.025(4) -0.004(3) -0.004(3)
C1 0.030(4) 0.021(3) 0.038(4) -0.002(3) -0.007(4) 0.001(3)
O10 0.049(4) 0.044(3) 0.048(3) 0.005(3) 0.007(3) -0.005(4)
N4 0.060(5) 0.031(4) 0.034(4) -0.004(4) 0.000(3) -0.004(4)
O8 0.103(6) 0.059(4) 0.039(3) -0.001(4) -0.016(4) -0.012(5)
O9 0.046(3) 0.051(4) 0.062(4) 0.002(3) 0.004(3) -0.002(3)
C8 0.033(4) 0.049(5) 0.045(4) 0.012(4) 0.014(4) 0.004(4)
C14 0.051(6) 0.030(4) 0.049(5) -0.005(4) -0.005(5) 0.005(4)
C13 0.069(6) 0.025(4) 0.050(5) -0.005(4) -0.013(5) 0.002(4)
C5 0.039(5) 0.032(4) 0.057(5) -0.010(4) 0.006(5) 0.008(4)
C20 0.038(5) 0.051(6) 0.088(8) -0.017(6) -0.006(6) 0.013(5)
C12 0.053(5) 0.018(4) 0.056(5) 0.008(4) -0.002(5) -0.012(4)
C18 0.052(6) 0.033(5) 0.068(6) -0.005(4) 0.010(5) -0.001(4)
O12 0.050(4) 0.048(4) 0.046(4) 0.016(3) 0.002(3) 0.001(3)
N5 0.035(4) 0.052(5) 0.047(5) -0.004(4) 0.001(4) 0.009(4)
C4 0.041(5) 0.029(4) 0.073(7) -0.004(4) -0.001(5) 0.011(4)
C9 0.034(4) 0.054(5) 0.040(5) 0.010(4) 0.007(4) -0.005(4)
O13 0.043(3) 0.034(3) 0.053(4) 0.000(3) -0.003(3) 0.002(3)
O11 0.069(5) 0.101(6) 0.035(3) -0.023(4) -0.016(3) 0.031(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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Er Er -0.2586 4.9576 '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 Er O2 63.03(17) . . ?
O1 Er O10 125.63(19) . . ?
O2 Er O10 114.4(2) . . ?
O1 Er O6 142.85(19) . . ?
O2 Er O6 115.69(19) . . ?
O10 Er O6 89.9(2) . . ?
O1 Er O13 73.56(19) . . ?
O2 Er O13 112.93(19) . . ?
O10 Er O13 132.4(2) . . ?
O6 Er O13 73.9(2) . . ?
O1 Er O9 80.5(2) . . ?
O2 Er O9 71.5(2) . . ?
O10 Er O9 52.2(2) . . ?
O6 Er O9 136.2(2) . . ?
O13 Er O9 146.55(19) . . ?
O1 Er O12 76.7(2) . . ?
O2 Er O12 69.5(2) . . ?
O10 Er O12 157.3(2) . . ?
O6 Er O12 69.4(2) . . ?
O13 Er O12 51.9(2) . . ?
O9 Er O12 140.5(2) . . ?
O1 Er O3 64.56(17) . . ?
O2 Er O3 122.11(17) . . ?
O10 Er O3 78.7(2) . . ?
O6 Er O3 120.61(18) . . ?
O13 Er O3 72.63(18) . . ?
O9 Er O3 77.38(19) . . ?
O12 Er O3 119.3(2) . . ?
O1 Er O7 130.3(2) . . ?
O2 Er O7 165.6(2) . . ?
O10 Er O7 64.3(2) . . ?
O6 Er O7 51.00(19) . . ?
O13 Er O7 71.1(2) . . ?
O9 Er O7 113.3(2) . . ?
O12 Er O7 106.1(2) . . ?
O3 Er O7 72.2(2) . . ?
O1 Er O4 124.94(17) . . ?
O2 Er O4 61.99(17) . . ?
O10 Er O4 76.5(2) . . ?
O6 Er O4 68.75(18) . . ?
O13 Er O4 132.33(18) . . ?
O9 Er O4 80.11(19) . . ?
O12 Er O4 87.1(2) . . ?
O3 Er O4 153.49(19) . . ?
O7 Er O4 104.7(2) . . ?
O1 Er N4 102.8(2) . . ?
O2 Er N4 94.0(2) . . ?
O10 Er N4 26.07(19) . . ?
O6 Er N4 114.2(2) . . ?
O13 Er N4 145.7(2) . . ?
O9 Er N4 26.3(2) . . ?
O12 Er N4 162.0(2) . . ?
O3 Er N4 75.1(2) . . ?
O7 Er N4 88.2(2) . . ?
O4 Er N4 78.5(2) . . ?
O1 Er N5 72.98(19) . . ?
O2 Er N5 91.4(2) . . ?
O10 Er N5 152.7(2) . . ?
O6 Er N5 69.9(2) . . ?
O13 Er N5 25.6(2) . . ?
O9 Er N5 152.9(2) . . ?
O12 Er N5 26.4(2) . . ?
O3 Er N5 95.6(2) . . ?
O7 Er N5 88.5(2) . . ?
O4 Er N5 110.8(2) . . ?
N4 Er N5 170.7(2) . . ?
N1 Ni N2 86.3(3) . . ?
N1 Ni O2 175.1(3) . . ?
N2 Ni O2 96.3(3) . . ?
N1 Ni O1 94.9(3) . . ?
N2 Ni O1 176.5(3) . . ?
O2 Ni O1 82.8(2) . . ?
N1 Ni Er 134.6(2) . . ?
N2 Ni Er 138.7(2) . . ?
O2 Ni Er 42.51(16) . . ?
O1 Ni Er 40.56(15) . . ?
C1 O1 Ni 125.0(5) . . ?
C1 O1 Er 125.4(5) . . ?
Ni O1 Er 108.0(2) . . ?
C7 N1 C8 120.5(7) . . ?
C7 N1 Ni 127.3(6) . . ?
C8 N1 Ni 112.2(5) . . ?
C10 N2 C9 119.3(7) . . ?
C10 N2 Ni 125.6(6) . . ?
C9 N2 Ni 114.5(5) . . ?
O2 C16 C15 117.6(7) . . ?
O2 C16 C11 122.7(7) . . ?
C15 C16 C11 119.7(7) . . ?
N2 C10 C11 125.3(7) . . ?
C16 O2 Ni 126.8(5) . . ?
C16 O2 Er 127.5(5) . . ?
Ni O2 Er 105.7(2) . . ?
C5 C6 C1 118.0(7) . . ?
C5 C6 C7 120.1(8) . . ?
C1 C6 C7 121.9(7) . . ?
N1 C7 C6 124.2(8) . . ?
C15 O4 C19 117.1(6) . . ?
C15 O4 Er 119.6(4) . . ?
C19 O4 Er 123.3(5) . . ?
O4 C15 C14 126.3(8) . . ?
O4 C15 C16 113.3(6) . . ?
C14 C15 C16 120.4(8) . . ?
N3 O6 Er 99.4(5) . . ?
O5 N3 O7 122.7(8) . . ?
O5 N3 O6 121.1(8) . . ?
O7 N3 O6 116.2(7) . . ?
O5 N3 Er 175.4(7) . . ?
O7 N3 Er 61.2(4) . . ?
O6 N3 Er 55.0(4) . . ?
O4 C19 C20 111.9(7) . . ?
C16 C11 C12 118.4(8) . . ?
C16 C11 C10 123.0(7) . . ?
C12 C11 C10 118.6(8) . . ?
C2 O3 C17 118.2(6) . . ?
C2 O3 Er 116.7(4) . . ?
C17 O3 Er 124.9(4) . . ?
C1 C2 C3 120.8(8) . . ?
C1 C2 O3 114.1(6) . . ?
C3 C2 O3 125.0(7) . . ?
O3 C17 C18 113.2(7) . . ?
C4 C3 C2 120.2(8) . . ?
N3 O7 Er 93.4(5) . . ?
O1 C1 C2 118.6(7) . . ?
O1 C1 C6 122.0(7) . . ?
C2 C1 C6 119.4(6) . . ?
N4 O10 Er 97.6(4) . . ?
O8 N4 O10 122.8(7) . . ?
O8 N4 O9 122.0(8) . . ?
O10 N4 O9 115.2(7) . . ?
O8 N4 Er 175.8(6) . . ?
O10 N4 Er 56.3(4) . . ?
O9 N4 Er 59.2(4) . . ?
N4 O9 Er 94.5(5) . . ?
N1 C8 C9 105.6(7) . . ?
C13 C14 C15 120.6(9) . . ?
C12 C13 C14 119.8(7) . . ?
C4 C5 C6 122.1(8) . . ?
C13 C12 C11 121.1(8) . . ?
N5 O12 Er 94.8(5) . . ?
O11 N5 O13 121.6(8) . . ?
O11 N5 O12 121.5(9) . . ?
O13 N5 O12 116.9(7) . . ?
O11 N5 Er 178.5(6) . . ?
O13 N5 Er 58.1(4) . . ?
O12 N5 Er 58.8(4) . . ?
C5 C4 C3 119.4(8) . . ?
N2 C9 C8 104.9(7) . . ?
N5 O13 Er 96.3(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
Er O1 2.313(5) . ?
Er O2 2.375(5) . ?
Er O10 2.402(6) . ?
Er O6 2.415(6) . ?
Er O13 2.462(6) . ?
Er O9 2.465(7) . ?
Er O12 2.475(6) . ?
Er O3 2.536(5) . ?
Er O7 2.553(6) . ?
Er O4 2.599(5) . ?
Er N4 2.861(7) . ?
Er N5 2.882(8) . ?
Ni N1 1.837(7) . ?
Ni N2 1.846(6) . ?
Ni O2 1.850(5) . ?
Ni O1 1.857(5) . ?
O1 C1 1.348(9) . ?
N1 C7 1.292(10) . ?
N1 C8 1.484(10) . ?
N2 C10 1.299(10) . ?
N2 C9 1.478(11) . ?
C16 O2 1.338(8) . ?
C16 C15 1.402(11) . ?
C16 C11 1.409(11) . ?
C10 C11 1.433(12) . ?
C6 C5 1.395(10) . ?
C6 C1 1.429(11) . ?
C6 C7 1.450(11) . ?
O4 C15 1.380(9) . ?
O4 C19 1.466(10) . ?
C15 C14 1.396(11) . ?
O6 N3 1.274(9) . ?
N3 O5 1.224(9) . ?
N3 O7 1.249(9) . ?
C19 C20 1.491(13) . ?
C11 C12 1.428(11) . ?
O3 C2 1.415(9) . ?
O3 C17 1.464(9) . ?
C2 C1 1.372(11) . ?
C2 C3 1.392(11) . ?
C17 C18 1.508(12) . ?
C3 C4 1.386(13) . ?
O10 N4 1.268(9) . ?
N4 O8 1.228(9) . ?
N4 O9 1.270(9) . ?
C8 C9 1.527(12) . ?
C14 C13 1.388(12) . ?
C13 C12 1.380(13) . ?
C5 C4 1.363(13) . ?
O12 N5 1.284(10) . ?
N5 O11 1.231(9) . ?
N5 O13 1.252(9) . ?
|
1100959.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100959.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_1100959
loop_
_publ_author_name
'Eric J. Hawrelak'
'Wesley H. Bernskoetter'
'Emil Lobkovsky'
'Gordon T. Yee'
'Eckhard Bill'
'Paul J. Chirik'
_publ_section_title
;
Square Planar vs Tetrahedral Geometry in Four Coordinate Iron(II) Complexes
;
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3103
_journal_page_last 3111
_journal_paper_doi 10.1021/ic048202+
_journal_volume 44
_journal_year 2005
_chemical_formula_sum 'C24 H40 Fe P2'
_chemical_formula_weight 446.35
_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 mixed
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 97.9160(10)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 9.4702(5)
_cell_length_b 13.8619(8)
_cell_length_c 18.8839(11)
_cell_measurement_reflns_used ?
_cell_measurement_temperature 173(2)
_cell_measurement_theta_max ?
_cell_measurement_theta_min ?
_cell_volume 2455.4(2)
_diffrn_ambient_temperature 173(2)
_diffrn_measurement_device_type 'Bruker 1K CCD area detector'
_diffrn_measurement_method '0.3 deg. 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 0.0648
_diffrn_reflns_av_sigmaI/netI 0.0837
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_l_max 25
_diffrn_reflns_limit_l_min -24
_diffrn_reflns_number 17030
_diffrn_reflns_theta_max 28.33
_diffrn_reflns_theta_min 2.29
_diffrn_standards_decay_% ?
_exptl_absorpt_coefficient_mu 0.751
_exptl_absorpt_correction_T_max 0.9634
_exptl_absorpt_correction_T_min 0.8060
_exptl_absorpt_correction_type SADABS
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.207
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 960
_exptl_crystal_size_max 0.30
_exptl_crystal_size_mid 0.20
_exptl_crystal_size_min 0.05
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.983
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 335
_refine_ls_number_reflns 6040
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.983
_refine_ls_R_factor_all 0.1064
_refine_ls_R_factor_gt 0.0543
_refine_ls_shift/su_max 0.317
_refine_ls_shift/su_mean 0.027
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0677P)^2^+0.8638P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1162
_refine_ls_wR_factor_ref 0.1362
_reflns_number_gt 3779
_reflns_number_total 6040
_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 1100959
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
Fe1 Fe 0.01005(5) 0.48443(3) 0.26512(2) 0.01923(13) Uani 1 1 d . . .
P1 P 0.15789(9) 0.44315(6) 0.18616(4) 0.0245(2) Uani 1 1 d . . .
P2 P -0.13198(9) 0.53077(6) 0.34492(4) 0.0243(2) Uani 1 1 d . . .
C1 C 0.1815(5) 0.3142(3) 0.1740(2) 0.0382(9) Uani 1 1 d . . .
C2 C 0.3434(4) 0.4813(4) 0.2087(3) 0.0464(11) Uani 1 1 d . . .
C3 C 0.1172(5) 0.4848(3) 0.0940(2) 0.0402(10) Uani 1 1 d . . .
C4 C -0.2908(4) 0.6020(4) 0.3136(2) 0.0568(12) Uani 1 1 d . . .
H4A H -0.3420 0.6166 0.3540 0.085 Uiso 1 1 calc R . .
H4B H -0.3531 0.5652 0.2776 0.085 Uiso 1 1 calc R . .
H4C H -0.2625 0.6623 0.2925 0.085 Uiso 1 1 calc R . .
C5 C -0.0492(5) 0.6093(4) 0.4157(3) 0.0689(15) Uani 1 1 d . . .
H5A H -0.1188 0.6256 0.4477 0.103 Uiso 1 1 calc R . .
H5B H -0.0163 0.6685 0.3948 0.103 Uiso 1 1 calc R . .
H5C H 0.0323 0.5761 0.4429 0.103 Uiso 1 1 calc R . .
C6 C -0.2080(6) 0.4385(3) 0.3953(3) 0.0691(15) Uani 1 1 d . . .
H6A H -0.2670 0.4686 0.4279 0.104 Uiso 1 1 calc R . .
H6B H -0.1314 0.4014 0.4230 0.104 Uiso 1 1 calc R . .
H6C H -0.2671 0.3953 0.3624 0.104 Uiso 1 1 calc R . .
C7 C 0.1387(3) 0.4137(2) 0.34330(16) 0.0223(7) Uani 1 1 d . . .
C8 C 0.1125(3) 0.3156(2) 0.35719(16) 0.0228(7) Uani 1 1 d . . .
C9 C 0.1969(4) 0.2645(3) 0.41012(17) 0.0274(7) Uani 1 1 d . . .
C10 C 0.3123(4) 0.3061(3) 0.45223(17) 0.0292(8) Uani 1 1 d . . .
C11 C 0.3392(4) 0.4018(3) 0.43982(17) 0.0287(8) Uani 1 1 d . . .
C12 C 0.2568(3) 0.4558(2) 0.38730(17) 0.0258(7) Uani 1 1 d . . .
C13 C -0.0101(4) 0.2644(2) 0.31346(18) 0.0309(8) Uani 1 1 d . . .
H13A H 0.0158(6) 0.2448(5) 0.2741(9) 0.046 Uiso 1 1 calc R . .
H13B H -0.0807(16) 0.3034(8) 0.3044(3) 0.046 Uiso 1 1 calc R . .
H13C H -0.0352(7) 0.2158(11) 0.3370(5) 0.046 Uiso 1 1 calc R . .
C14 C 0.4027(4) 0.2495(3) 0.51021(18) 0.0445(11) Uani 1 1 d . . .
H14A H 0.3473(14) 0.2182(8) 0.5358(6) 0.067 Uiso 1 1 calc R . .
H14B H 0.4573(14) 0.2892(10) 0.5378(7) 0.067 Uiso 1 1 calc R . .
H14C H 0.4559(14) 0.2084(10) 0.4906(5) 0.067 Uiso 1 1 calc R . .
C15 C 0.2937(5) 0.5608(3) 0.3774(2) 0.0355(9) Uani 1 1 d . . .
C16 C -0.1213(3) 0.5470(2) 0.18501(16) 0.0227(7) Uani 1 1 d . . .
C17 C -0.0962(3) 0.6422(2) 0.16418(17) 0.0260(7) Uani 1 1 d . . .
C18 C -0.1765(4) 0.6834(3) 0.10454(18) 0.0301(8) Uani 1 1 d . . .
C19 C -0.2865(4) 0.6346(3) 0.06437(17) 0.0305(8) Uani 1 1 d . . .
C20 C -0.3142(4) 0.5415(3) 0.08521(18) 0.0301(8) Uani 1 1 d . . .
C21 C -0.2344(3) 0.4974(2) 0.14390(17) 0.0253(7) Uani 1 1 d . . .
C22 C 0.0220(4) 0.7000(3) 0.20644(19) 0.0354(9) Uani 1 1 d . . .
H22A H 0.0611(10) 0.7354(8) 0.1784(6) 0.053 Uiso 1 1 calc R . .
H22B H 0.0832(14) 0.6620(8) 0.2280(5) 0.053 Uiso 1 1 calc R . .
H22C H -0.0123(8) 0.7349(8) 0.2366(7) 0.053 Uiso 1 1 calc R . .
C23 C -0.3754(5) 0.6825(4) 0.0018(2) 0.0418(10) Uani 1 1 d . . .
C24 C -0.2674(4) 0.3951(3) 0.1631(2) 0.0355(9) Uani 1 1 d . . .
H20 H -0.381(3) 0.506(2) 0.0600(17) 0.022(9) Uiso 1 1 d . . .
H9 H 0.178(3) 0.199(2) 0.4182(16) 0.019(8) Uiso 1 1 d . . .
H3C H 0.026(5) 0.466(3) 0.074(2) 0.056(14) Uiso 1 1 d . . .
H11 H 0.414(4) 0.432(2) 0.4658(18) 0.030(9) Uiso 1 1 d . . .
H24B H -0.189(4) 0.352(2) 0.1617(17) 0.030(9) Uiso 1 1 d . . .
H18 H -0.150(3) 0.744(2) 0.0930(16) 0.023(9) Uiso 1 1 d . . .
H15C H 0.289(5) 0.596(3) 0.417(3) 0.069(15) Uiso 1 1 d . . .
H24A H -0.340(4) 0.365(3) 0.136(2) 0.055(13) Uiso 1 1 d . . .
H15B H 0.224(5) 0.596(3) 0.341(2) 0.064(13) Uiso 1 1 d . . .
H2A H 0.091(4) 0.289(3) 0.156(2) 0.049(12) Uiso 1 1 d . . .
H1A H 0.215(4) 0.282(3) 0.221(2) 0.039(10) Uiso 1 1 d . . .
H15A H 0.383(5) 0.567(4) 0.362(3) 0.082(17) Uiso 1 1 d . . .
H3B H 0.187(4) 0.461(3) 0.068(2) 0.044(11) Uiso 1 1 d . . .
H2C H 0.398(4) 0.455(3) 0.174(2) 0.044(11) Uiso 1 1 d . . .
H2B H 0.342(4) 0.544(3) 0.212(2) 0.039(12) Uiso 1 1 d . . .
H3A H 0.117(4) 0.562(3) 0.092(2) 0.053(12) Uiso 1 1 d . . .
H2A H 0.387(5) 0.455(3) 0.257(2) 0.060(14) Uiso 1 1 d . . .
H23C H -0.409(4) 0.638(3) -0.035(2) 0.054(13) Uiso 1 1 d . . .
H23B H -0.314(5) 0.725(4) -0.019(2) 0.076(16) Uiso 1 1 d . . .
H24C H -0.302(4) 0.389(3) 0.209(2) 0.049(12) Uiso 1 1 d . . .
H23A H -0.456(5) 0.706(4) 0.019(3) 0.078(16) Uiso 1 1 d . . .
H1C H 0.250(5) 0.303(3) 0.141(2) 0.065(14) 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
Fe1 0.0196(2) 0.0184(2) 0.0190(2) 0.00011(18) 0.00033(16) 0.00045(18)
P1 0.0259(4) 0.0241(5) 0.0238(4) 0.0005(3) 0.0045(3) 0.0037(4)
P2 0.0244(4) 0.0266(5) 0.0219(4) -0.0017(3) 0.0033(3) 0.0005(4)
C1 0.053(3) 0.031(2) 0.032(2) -0.0005(17) 0.0113(19) 0.0119(19)
C2 0.028(2) 0.063(3) 0.050(3) -0.009(2) 0.0130(19) -0.007(2)
C3 0.049(3) 0.049(3) 0.0252(19) 0.0076(18) 0.0134(18) 0.019(2)
C4 0.046(3) 0.077(3) 0.049(3) -0.002(2) 0.012(2) 0.023(2)
C5 0.054(3) 0.086(4) 0.069(3) -0.048(3) 0.017(2) -0.015(3)
C6 0.092(4) 0.049(3) 0.076(3) 0.017(3) 0.048(3) 0.006(3)
C7 0.0224(16) 0.0249(17) 0.0195(15) 0.0012(13) 0.0030(12) 0.0015(13)
C8 0.0229(16) 0.0249(17) 0.0213(15) 0.0001(13) 0.0061(13) -0.0003(13)
C9 0.0334(19) 0.0235(18) 0.0275(17) 0.0044(14) 0.0122(15) 0.0052(15)
C10 0.0293(18) 0.038(2) 0.0210(16) 0.0035(14) 0.0061(14) 0.0129(15)
C11 0.0235(18) 0.039(2) 0.0226(17) -0.0066(15) -0.0007(14) 0.0005(15)
C12 0.0255(17) 0.0257(18) 0.0257(16) -0.0054(13) 0.0016(14) 0.0000(13)
C13 0.0314(19) 0.0260(18) 0.0357(19) 0.0028(15) 0.0064(15) -0.0035(15)
C14 0.052(3) 0.050(3) 0.0293(19) 0.0044(18) -0.0010(18) 0.018(2)
C15 0.035(2) 0.030(2) 0.039(2) -0.0043(18) 0.0002(18) -0.0072(17)
C16 0.0217(16) 0.0262(17) 0.0207(15) 0.0006(13) 0.0051(13) 0.0056(13)
C17 0.0263(17) 0.0262(18) 0.0262(17) -0.0001(14) 0.0059(14) 0.0044(14)
C18 0.036(2) 0.0257(19) 0.0310(19) 0.0063(15) 0.0135(16) 0.0099(16)
C19 0.0305(18) 0.040(2) 0.0207(16) 0.0029(15) 0.0031(14) 0.0141(16)
C20 0.0245(18) 0.040(2) 0.0248(17) -0.0059(15) -0.0022(14) 0.0029(15)
C21 0.0247(17) 0.0285(19) 0.0229(16) -0.0002(13) 0.0040(13) 0.0017(13)
C22 0.040(2) 0.029(2) 0.037(2) 0.0031(16) 0.0062(16) -0.0022(16)
C23 0.044(3) 0.051(3) 0.029(2) 0.0103(19) 0.0020(19) 0.016(2)
C24 0.032(2) 0.032(2) 0.041(2) -0.0025(17) -0.0036(18) -0.0044(17)
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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100960.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100960.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_1100960
loop_
_publ_author_name
'Eric J. Hawrelak'
'Wesley H. Bernskoetter'
'Emil Lobkovsky'
'Gordon T. Yee'
'Eckhard Bill'
'Paul J. Chirik'
_publ_section_title
;
Square Planar vs Tetrahedral Geometry in Four Coordinate Iron(II) Complexes
;
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3103
_journal_page_last 3111
_journal_paper_doi 10.1021/ic048202+
_journal_volume 44
_journal_year 2005
_chemical_formula_sum 'C38 H52 Fe P2'
_chemical_formula_weight 626.59
_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 mixed
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.0000(18)
_cell_angle_beta 106.9498(18)
_cell_angle_gamma 90.0000(19)
_cell_formula_units_Z 2
_cell_length_a 10.6501(7)
_cell_length_b 9.2391(6)
_cell_length_c 18.1650(12)
_cell_measurement_reflns_used ?
_cell_measurement_temperature 173(2)
_cell_measurement_theta_max ?
_cell_measurement_theta_min ?
_cell_volume 1709.74(19)
_diffrn_ambient_temperature 173(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type 'Bruker 1K CCD area detector'
_diffrn_measurement_method '0.3 deg. 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 0.0425
_diffrn_reflns_av_sigmaI/netI 0.0658
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_k_min -9
_diffrn_reflns_limit_l_max 23
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_number 11055
_diffrn_reflns_theta_max 29.12
_diffrn_reflns_theta_min 2.34
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 0.559
_exptl_absorpt_correction_T_max 0.9726
_exptl_absorpt_correction_T_min 0.8073
_exptl_absorpt_correction_type SADABS
_exptl_absorpt_process_details ?
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.217
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 672
_exptl_crystal_size_max 0.40
_exptl_crystal_size_mid 0.15
_exptl_crystal_size_min 0.05
_refine_ls_extinction_coef ?
_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 269
_refine_ls_number_reflns 4056
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.020
_refine_ls_R_factor_all 0.0904
_refine_ls_R_factor_gt 0.0494
_refine_ls_shift/su_max 0.997
_refine_ls_shift/su_mean 0.019
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0517P)^2^+0.5268P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0972
_refine_ls_wR_factor_ref 0.1103
_reflns_number_gt 2775
_reflns_number_total 4056
_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 1100960
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
Fe1 Fe 0.0000 0.0000 0.0000 0.01948(14) Uani 1 2 d S . .
P1 P -0.14830(6) -0.16615(7) 0.01228(3) 0.02273(16) Uani 1 1 d . . .
C1 C 0.1473(2) -0.1408(2) 0.04880(13) 0.0219(5) Uani 1 1 d . . .
C2 C 0.2056(2) -0.1366(3) 0.12915(14) 0.0259(6) Uani 1 1 d . . .
C3 C 0.3152(2) -0.2210(3) 0.16527(15) 0.0304(6) Uani 1 1 d . . .
H3 H 0.349(3) -0.215(3) 0.2202(16) 0.035(7) Uiso 1 1 d . . .
C4 C 0.3725(2) -0.3125(3) 0.12394(15) 0.0309(6) Uani 1 1 d . . .
C5 C 0.3153(2) -0.3193(3) 0.04543(16) 0.0287(6) Uani 1 1 d . . .
H5 H 0.352(2) -0.381(3) 0.0141(15) 0.029(7) Uiso 1 1 d . . .
C6 C 0.2063(2) -0.2363(3) 0.00775(14) 0.0245(5) Uani 1 1 d . . .
C7 C 0.1515(3) -0.0375(3) 0.17894(16) 0.0344(7) Uani 1 1 d . . .
H7C H 0.116(3) -0.086(4) 0.2152(19) 0.059(10) Uiso 1 1 d . . .
H7B H 0.214(3) 0.031(3) 0.2074(18) 0.053(9) Uiso 1 1 d . . .
H7A H 0.081(3) 0.014(3) 0.151(2) 0.060(10) Uiso 1 1 d . . .
C8 C 0.4924(3) -0.4012(3) 0.16377(17) 0.0425(7) Uani 1 1 d . . .
H8A H 0.4665 -0.5020 0.1676 0.064 Uiso 1 1 calc R . .
H8B H 0.5327 -0.3624 0.2155 0.064 Uiso 1 1 calc R . .
H8C H 0.5557 -0.3965 0.1341 0.064 Uiso 1 1 calc R . .
C9 C 0.1559(3) -0.2450(3) -0.07911(14) 0.0316(6) Uani 1 1 d . . .
H9A H 0.2303 -0.2454 -0.1006 0.047 Uiso 1 1 calc R . .
H9B H 0.0998 -0.1612 -0.0989 0.047 Uiso 1 1 calc R . .
H9C H 0.1049 -0.3342 -0.0941 0.047 Uiso 1 1 calc R . .
C10 C -0.1344(2) -0.2195(3) 0.11176(13) 0.0256(6) Uani 1 1 d . . .
C11 C -0.2001(3) -0.1438(3) 0.15524(16) 0.0336(7) Uani 1 1 d . . .
H11 H -0.251(3) -0.075(3) 0.1374(15) 0.035(8) Uiso 1 1 d . . .
C12 C -0.1875(3) -0.1828(4) 0.23064(17) 0.0442(8) Uani 1 1 d . . .
H12 H -0.232(3) -0.128(3) 0.2585(18) 0.048(9) Uiso 1 1 d . . .
C13 C -0.1095(3) -0.2970(4) 0.26372(17) 0.0482(9) Uani 1 1 d . . .
H13 H -0.105(3) -0.325(4) 0.315(2) 0.066(10) Uiso 1 1 d . . .
C14 C -0.0422(3) -0.3722(4) 0.22199(18) 0.0473(9) Uani 1 1 d . . .
H14 H 0.004(3) -0.443(3) 0.2393(17) 0.043(9) Uiso 1 1 d . . .
C15 C -0.0542(3) -0.3343(3) 0.14624(16) 0.0362(7) Uani 1 1 d . . .
H15 H -0.005(3) -0.383(3) 0.1181(17) 0.046(9) Uiso 1 1 d . . .
C16 C -0.3226(3) -0.1185(3) -0.02596(17) 0.0310(6) Uani 1 1 d . . .
H16B H -0.334(2) -0.033(3) 0.0004(15) 0.029(7) Uiso 1 1 d . . .
H16A H -0.335(2) -0.093(3) -0.0785(15) 0.031(7) Uiso 1 1 d . . .
C17 C -0.4214(3) -0.2306(4) -0.01752(19) 0.0418(8) Uani 1 1 d . . .
H17C H -0.509(3) -0.196(3) -0.0345(16) 0.042(8) Uiso 1 1 d . . .
H17B H -0.412(3) -0.256(3) 0.0358(18) 0.044(8) Uiso 1 1 d . . .
H17A H -0.419(3) -0.328(4) -0.0487(19) 0.070(11) Uiso 1 1 d . . .
C18 C -0.1404(3) -0.3449(3) -0.03179(15) 0.0296(6) Uani 1 1 d . . .
H18B H -0.051(3) -0.370(3) -0.0160(16) 0.041(8) Uiso 1 1 d . . .
H18A H -0.190(3) -0.415(3) -0.0092(16) 0.044(8) Uiso 1 1 d . . .
C19 C -0.1943(3) -0.3475(4) -0.11898(16) 0.0393(7) Uani 1 1 d . . .
H19C H -0.281(3) -0.318(3) -0.1363(18) 0.053(10) Uiso 1 1 d . . .
H19B H -0.187(3) -0.442(4) -0.140(2) 0.069(11) Uiso 1 1 d . . .
H19A H -0.146(3) -0.283(3) -0.1440(18) 0.050(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
Fe1 0.0208(2) 0.0194(3) 0.0172(2) 0.00086(19) 0.00404(17) -0.0001(2)
P1 0.0233(3) 0.0221(3) 0.0217(3) 0.0015(2) 0.0047(2) -0.0027(3)
C1 0.0237(12) 0.0182(12) 0.0245(12) 0.0030(9) 0.0081(10) -0.0045(10)
C2 0.0256(12) 0.0239(13) 0.0275(12) 0.0023(10) 0.0067(10) -0.0040(11)
C3 0.0272(13) 0.0323(15) 0.0275(13) 0.0092(11) 0.0014(11) -0.0050(12)
C4 0.0245(13) 0.0254(14) 0.0410(15) 0.0113(11) 0.0067(11) -0.0008(11)
C5 0.0243(13) 0.0243(14) 0.0402(15) 0.0036(11) 0.0134(11) -0.0005(11)
C6 0.0244(12) 0.0208(13) 0.0287(12) 0.0047(10) 0.0084(10) -0.0054(10)
C7 0.0367(16) 0.0391(18) 0.0247(13) -0.0005(12) 0.0046(12) 0.0008(13)
C8 0.0302(15) 0.0396(17) 0.0528(18) 0.0180(14) 0.0045(13) 0.0061(13)
C9 0.0322(14) 0.0342(16) 0.0299(13) -0.0010(11) 0.0114(11) 0.0006(12)
C10 0.0259(13) 0.0260(13) 0.0244(12) -0.0004(10) 0.0066(10) -0.0082(11)
C11 0.0327(15) 0.0376(17) 0.0314(14) -0.0027(12) 0.0107(12) -0.0087(14)
C12 0.0468(18) 0.057(2) 0.0322(15) -0.0133(15) 0.0175(14) -0.0196(17)
C13 0.057(2) 0.063(2) 0.0237(14) 0.0033(15) 0.0102(14) -0.0277(18)
C14 0.052(2) 0.045(2) 0.0363(17) 0.0153(15) -0.0001(15) -0.0089(17)
C15 0.0423(16) 0.0338(16) 0.0316(14) 0.0046(12) 0.0093(13) -0.0030(14)
C16 0.0245(13) 0.0347(16) 0.0329(15) 0.0041(12) 0.0068(11) -0.0024(12)
C17 0.0276(15) 0.057(2) 0.0389(17) 0.0071(15) 0.0069(13) -0.0107(15)
C18 0.0331(15) 0.0268(14) 0.0293(13) -0.0032(11) 0.0096(12) -0.0058(12)
C19 0.0433(18) 0.0434(19) 0.0299(15) -0.0078(13) 0.0089(13) -0.0078(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'
P P 0.1023 0.0942 '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'
|
1100961.cif | #------------------------------------------------------------------------------
#$Date: 2022-09-14 18:21:52 +0300 (Wed, 14 Sep 2022) $
#$Revision: 277833 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/09/1100961.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_1100961
loop_
_publ_author_name
'Eric J. Hawrelak'
'Wesley H. Bernskoetter'
'Emil Lobkovsky'
'Gordon T. Yee'
'Eckhard Bill'
'Paul J. Chirik'
_publ_section_title
;
Square Planar vs Tetrahedral Geometry in Four Coordinate Iron(II) Complexes
;
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3103
_journal_page_last 3111
_journal_paper_doi 10.1021/ic048202+
_journal_volume 44
_journal_year 2005
_chemical_formula_sum 'C28 H46 Fe P2'
_chemical_formula_weight 500.44
_space_group_IT_number 61
_space_group_name_Hall '-P 2ac 2ab'
_space_group_name_H-M_alt 'P b c a'
_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
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 8
_cell_length_a 17.9931(5)
_cell_length_b 15.2837(4)
_cell_length_c 20.2132(6)
_cell_measurement_reflns_used ?
_cell_measurement_temperature 173(2)
_cell_measurement_theta_max ?
_cell_measurement_theta_min ?
_cell_volume 5558.7(3)
_diffrn_ambient_temperature 173(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type 'Bruker 1K CCD area detector'
_diffrn_measurement_method '0.3 deg. 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 0.0731
_diffrn_reflns_av_sigmaI/netI 0.0273
_diffrn_reflns_limit_h_max 25
_diffrn_reflns_limit_h_min -25
_diffrn_reflns_limit_k_max 21
_diffrn_reflns_limit_k_min -21
_diffrn_reflns_limit_l_max 28
_diffrn_reflns_limit_l_min -28
_diffrn_reflns_number 105386
_diffrn_reflns_theta_max 30.51
_diffrn_reflns_theta_min 2.02
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 0.671
_exptl_absorpt_correction_T_max 0.8241
_exptl_absorpt_correction_T_min 0.7303
_exptl_absorpt_correction_type SADABS
_exptl_absorpt_process_details ?
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.196
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 2160
_exptl_crystal_size_max 0.50
_exptl_crystal_size_mid 0.40
_exptl_crystal_size_min 0.30
_refine_ls_extinction_coef ?
_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 442
_refine_ls_number_reflns 8485
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.054
_refine_ls_R_factor_all 0.0536
_refine_ls_R_factor_gt 0.0360
_refine_ls_shift/su_max 0.195
_refine_ls_shift/su_mean 0.015
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0392P)^2^+2.6981P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0799
_refine_ls_wR_factor_ref 0.0881
_reflns_number_gt 6679
_reflns_number_total 8485
_reflns_threshold_expression >2sigma(I)
_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 1100961
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
Fe1 Fe 0.123037(11) 0.453885(13) 0.231183(10) 0.01759(6) Uani 1 1 d . . .
P1 P 0.13545(2) 0.29879(2) 0.263555(18) 0.02007(8) Uani 1 1 d . . .
P2 P 0.03119(2) 0.38725(2) 0.154357(18) 0.01944(8) Uani 1 1 d . . .
C1 C 0.07386(10) 0.23019(10) 0.21223(8) 0.0285(3) Uani 1 1 d . . .
H1A H 0.0592(12) 0.1769(14) 0.2361(11) 0.041(6) Uiso 1 1 d . . .
H1B H 0.1034(12) 0.2112(14) 0.1761(11) 0.038(6) Uiso 1 1 d . . .
C2 C 0.00492(10) 0.28021(10) 0.18872(8) 0.0265(3) Uani 1 1 d . . .
H2A H -0.0221(11) 0.2452(14) 0.1595(10) 0.036(5) Uiso 1 1 d . . .
H2B H -0.0276(11) 0.2922(13) 0.2252(10) 0.034(5) Uiso 1 1 d . . .
C3 C 0.21782(10) 0.22817(10) 0.26800(9) 0.0290(3) Uani 1 1 d . . .
H3B H 0.2380(12) 0.2249(13) 0.2236(11) 0.038(6) Uiso 1 1 d . . .
H3A H 0.1987(11) 0.1676(14) 0.2789(10) 0.035(5) Uiso 1 1 d . . .
C4 C 0.27732(11) 0.26028(13) 0.31596(10) 0.0355(4) Uani 1 1 d . . .
H4C H 0.2570(13) 0.2632(15) 0.3622(12) 0.050(6) Uiso 1 1 d . . .
H4B H 0.3157(13) 0.2227(15) 0.3180(11) 0.046(6) Uiso 1 1 d . . .
H4A H 0.2973(12) 0.3149(15) 0.3027(10) 0.040(6) Uiso 1 1 d . . .
C5 C 0.09300(10) 0.29064(10) 0.34613(8) 0.0248(3) Uani 1 1 d . . .
H5B H 0.1185(12) 0.3328(15) 0.3740(11) 0.040(6) Uiso 1 1 d . . .
H5A H 0.0429(11) 0.3075(12) 0.3403(9) 0.027(5) Uiso 1 1 d . . .
C6 C 0.09449(11) 0.20102(12) 0.37949(9) 0.0319(4) Uani 1 1 d . . .
H6C H 0.1450(13) 0.1844(14) 0.3918(11) 0.040(6) Uiso 1 1 d . . .
H6B H 0.0651(14) 0.2008(16) 0.4212(13) 0.058(7) Uiso 1 1 d . . .
H6A H 0.0755(11) 0.1557(14) 0.3519(10) 0.032(5) Uiso 1 1 d . . .
C7 C 0.08200(10) 0.35527(11) 0.07924(8) 0.0262(3) Uani 1 1 d . . .
H7B H 0.1290(11) 0.3345(14) 0.0924(10) 0.032(5) Uiso 1 1 d . . .
H7A H 0.0558(11) 0.3074(12) 0.0575(9) 0.026(5) Uiso 1 1 d . . .
C8 C 0.09546(11) 0.43124(12) 0.03160(8) 0.0315(4) Uani 1 1 d . . .
H8C H 0.0477(13) 0.4487(14) 0.0093(11) 0.041(6) Uiso 1 1 d . . .
H8B H 0.1310(13) 0.4169(17) -0.0021(12) 0.052(7) Uiso 1 1 d . . .
H8A H 0.1167(11) 0.4803(15) 0.0542(11) 0.039(6) Uiso 1 1 d . . .
C9 C -0.05764(9) 0.42974(11) 0.12232(8) 0.0269(3) Uani 1 1 d . . .
H9B H -0.0474(11) 0.4862(14) 0.1077(10) 0.036(5) Uiso 1 1 d . . .
H9A H -0.0883(13) 0.4350(14) 0.1588(11) 0.041(6) Uiso 1 1 d . . .
C10 C -0.09659(10) 0.37543(13) 0.06911(9) 0.0316(4) Uani 1 1 d . . .
H10C H -0.1449(12) 0.4015(13) 0.0572(10) 0.035(5) Uiso 1 1 d . . .
H10B H -0.0670(11) 0.3715(12) 0.0298(10) 0.029(5) Uiso 1 1 d . . .
H10A H -0.1058(12) 0.3178(15) 0.0828(11) 0.042(6) Uiso 1 1 d . . .
C11 C 0.19053(8) 0.52063(9) 0.16536(7) 0.0195(3) Uani 1 1 d . . .
C12 C 0.25353(8) 0.48588(10) 0.13295(7) 0.0224(3) Uani 1 1 d . . .
C13 C 0.28973(9) 0.53142(11) 0.08246(8) 0.0266(3) Uani 1 1 d . . .
H13 H 0.3318(11) 0.5038(13) 0.0604(10) 0.036(5) Uiso 1 1 d . . .
C14 C 0.26576(9) 0.61354(11) 0.06204(7) 0.0265(3) Uani 1 1 d . . .
C15 C 0.20500(9) 0.64982(10) 0.09405(8) 0.0257(3) Uani 1 1 d . . .
H15 H 0.1879(11) 0.7043(13) 0.0812(10) 0.032(5) Uiso 1 1 d . . .
C16 C 0.16788(8) 0.60503(9) 0.14472(7) 0.0218(3) Uani 1 1 d . . .
C17 C 0.28261(10) 0.39624(12) 0.15121(11) 0.0332(4) Uani 1 1 d . . .
H17B H 0.2488(15) 0.3495(17) 0.1403(12) 0.059(7) Uiso 1 1 d . . .
H17A H 0.3292(16) 0.3828(16) 0.1330(12) 0.060(7) Uiso 1 1 d . . .
H17C H 0.2941(14) 0.3917(16) 0.1974(13) 0.061(7) Uiso 1 1 d . . .
C18 C 0.30410(13) 0.66067(15) 0.00594(10) 0.0394(5) Uani 1 1 d . . .
H18C H 0.3028(18) 0.632(2) -0.0313(16) 0.093(11) Uiso 1 1 d . . .
H18B H 0.3504(18) 0.680(2) 0.0181(15) 0.080(9) Uiso 1 1 d . . .
H18A H 0.2793(19) 0.714(2) -0.0065(17) 0.097(11) Uiso 1 1 d . . .
C19 C 0.10077(10) 0.64826(11) 0.17572(9) 0.0336(4) Uani 1 1 d . . .
H19A H 0.09294(15) 0.7031(7) 0.1559(3) 0.040 Uiso 1 1 calc R . .
H19B H 0.10896(13) 0.65566(15) 0.2212(6) 0.040 Uiso 1 1 calc R . .
H19C H 0.0588(5) 0.6129(4) 0.16920(12) 0.040 Uiso 1 1 calc R . .
C20 C 0.09385(8) 0.51013(9) 0.32090(7) 0.0199(3) Uani 1 1 d . . .
C21 C 0.02021(9) 0.52821(9) 0.34123(7) 0.0213(3) Uani 1 1 d . . .
C22 C 0.00516(10) 0.57047(10) 0.40128(8) 0.0250(3) Uani 1 1 d . . .
H22 H -0.0447(11) 0.5815(13) 0.4117(9) 0.029(5) Uiso 1 1 d . . .
C23 C 0.06205(10) 0.59624(10) 0.44373(7) 0.0267(3) Uani 1 1 d . . .
C24 C 0.13448(10) 0.57794(10) 0.42498(8) 0.0265(3) Uani 1 1 d . . .
H24 H 0.1716(11) 0.5938(12) 0.4533(9) 0.027(5) Uiso 1 1 d . . .
C25 C 0.15058(9) 0.53530(9) 0.36525(7) 0.0224(3) Uani 1 1 d . . .
C26 C -0.04443(9) 0.50054(11) 0.29857(9) 0.0269(3) Uani 1 1 d . . .
H26B H -0.0918(11) 0.5212(13) 0.3141(10) 0.028(5) Uiso 1 1 d . . .
H26A H -0.0389(12) 0.5223(14) 0.2546(12) 0.038(6) Uiso 1 1 d . . .
H26C H -0.0489(12) 0.4338(15) 0.2964(11) 0.041(6) Uiso 1 1 d . . .
C27 C 0.04457(12) 0.64112(12) 0.50881(8) 0.0362(4) Uani 1 1 d . . .
H27A H 0.03945(14) 0.6004(6) 0.5410(5) 0.054 Uiso 1 1 calc R . .
H27B H 0.0018(6) 0.6718(4) 0.50482(9) 0.054 Uiso 1 1 calc R . .
H27C H 0.0821(5) 0.6780(5) 0.51946(17) 0.054 Uiso 1 1 calc R . .
C28 C 0.23091(10) 0.51440(12) 0.34986(9) 0.0294(3) Uani 1 1 d . . .
H28B H 0.2403(13) 0.4555(15) 0.3577(11) 0.045(6) Uiso 1 1 d . . .
H28C H 0.2653(14) 0.5449(16) 0.3753(12) 0.053(7) Uiso 1 1 d . . .
H31A H 0.2435(13) 0.5274(15) 0.3059(12) 0.049(6) 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
Fe1 0.01931(10) 0.01688(9) 0.01657(10) -0.00050(7) 0.00249(7) -0.00124(7)
P1 0.02485(18) 0.01695(16) 0.01840(17) 0.00111(12) -0.00179(14) 0.00059(13)
P2 0.02202(18) 0.01998(16) 0.01632(16) -0.00102(13) -0.00184(14) -0.00056(13)
C1 0.0414(10) 0.0180(7) 0.0261(8) -0.0003(6) -0.0074(7) -0.0028(6)
C2 0.0318(8) 0.0230(7) 0.0247(8) 0.0007(6) -0.0058(7) -0.0079(6)
C3 0.0330(8) 0.0241(7) 0.0298(8) 0.0025(6) 0.0018(7) 0.0079(6)
C4 0.0294(9) 0.0365(9) 0.0406(10) 0.0069(8) -0.0032(8) 0.0069(7)
C5 0.0297(8) 0.0234(7) 0.0213(7) 0.0038(5) 0.0010(6) 0.0005(6)
C6 0.0366(9) 0.0300(8) 0.0292(9) 0.0111(7) 0.0013(7) -0.0002(7)
C7 0.0289(8) 0.0286(7) 0.0211(7) -0.0055(6) -0.0015(6) 0.0018(6)
C8 0.0370(9) 0.0398(9) 0.0178(7) -0.0026(6) 0.0009(7) -0.0053(7)
C9 0.0249(8) 0.0322(8) 0.0236(8) -0.0028(6) -0.0037(6) 0.0024(6)
C10 0.0275(8) 0.0402(10) 0.0271(8) -0.0023(7) -0.0068(7) -0.0032(7)
C11 0.0207(7) 0.0196(6) 0.0182(6) -0.0019(5) -0.0003(5) -0.0019(5)
C12 0.0212(7) 0.0227(7) 0.0233(7) -0.0011(5) 0.0013(6) -0.0027(5)
C13 0.0229(7) 0.0340(8) 0.0228(7) -0.0037(6) 0.0049(6) -0.0059(6)
C14 0.0296(8) 0.0330(8) 0.0168(7) 0.0013(6) -0.0012(6) -0.0121(6)
C15 0.0317(8) 0.0224(7) 0.0231(7) 0.0035(5) -0.0053(6) -0.0054(6)
C16 0.0228(7) 0.0227(6) 0.0199(7) -0.0015(5) -0.0021(5) -0.0020(5)
C17 0.0268(8) 0.0275(8) 0.0453(11) 0.0025(7) 0.0103(8) 0.0041(7)
C18 0.0451(12) 0.0487(11) 0.0243(9) 0.0090(8) 0.0032(8) -0.0191(9)
C19 0.0352(9) 0.0262(8) 0.0395(10) 0.0039(7) 0.0070(7) 0.0062(7)
C20 0.0253(7) 0.0155(6) 0.0191(6) 0.0010(5) 0.0023(5) -0.0009(5)
C21 0.0267(7) 0.0161(6) 0.0211(7) 0.0008(5) 0.0023(6) -0.0004(5)
C22 0.0310(8) 0.0206(6) 0.0235(7) -0.0002(5) 0.0055(6) 0.0035(6)
C23 0.0426(9) 0.0189(7) 0.0187(7) 0.0004(5) 0.0019(6) 0.0034(6)
C24 0.0369(9) 0.0220(7) 0.0206(7) 0.0009(5) -0.0070(6) -0.0019(6)
C25 0.0283(7) 0.0179(6) 0.0210(7) 0.0025(5) -0.0004(6) -0.0022(5)
C26 0.0240(8) 0.0266(8) 0.0302(8) -0.0051(6) 0.0029(6) -0.0001(6)
C27 0.0542(12) 0.0321(8) 0.0223(8) -0.0058(6) -0.0005(8) 0.0090(8)
C28 0.0256(8) 0.0310(8) 0.0314(9) -0.0007(7) -0.0024(7) -0.0042(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'
P P 0.1023 0.0942 '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'
|
1100962.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100962.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_1100962
loop_
_publ_author_name
'Eric J. Hawrelak'
'Wesley H. Bernskoetter'
'Emil Lobkovsky'
'Gordon T. Yee'
'Eckhard Bill'
'Paul J. Chirik'
_publ_section_title
;
Square Planar vs Tetrahedral Geometry in Four Coordinate Iron(II) Complexes
;
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3103
_journal_page_last 3111
_journal_paper_doi 10.1021/ic048202+
_journal_volume 44
_journal_year 2005
_chemical_formula_sum 'C35 H35 Cl Fe P2'
_chemical_formula_weight 608.87
_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 mixed
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 91.1370(10)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 12.1140(5)
_cell_length_b 13.1394(6)
_cell_length_c 19.0367(9)
_cell_measurement_reflns_used ?
_cell_measurement_temperature 173(2)
_cell_measurement_theta_max ?
_cell_measurement_theta_min ?
_cell_volume 3029.5(2)
_diffrn_ambient_temperature 173(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type 'Bruker 1K CCD area detector'
_diffrn_measurement_method '0.3 deg. 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 0.1084
_diffrn_reflns_av_sigmaI/netI 0.1093
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 21
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_number 15456
_diffrn_reflns_theta_max 23.27
_diffrn_reflns_theta_min 2.54
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 0.715
_exptl_absorpt_correction_T_max 0.9824
_exptl_absorpt_correction_T_min 0.8703
_exptl_absorpt_correction_type SADABS
_exptl_absorpt_process_details ?
_exptl_crystal_colour yellowish
_exptl_crystal_density_diffrn 1.335
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 1272
_exptl_crystal_size_max 0.20
_exptl_crystal_size_mid 0.10
_exptl_crystal_size_min 0.03
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.989
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 468
_refine_ls_number_reflns 4347
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.989
_refine_ls_R_factor_all 0.1125
_refine_ls_R_factor_gt 0.0536
_refine_ls_shift/su_max 0.318
_refine_ls_shift/su_mean 0.017
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0526P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1007
_refine_ls_wR_factor_ref 0.1183
_reflns_number_gt 2669
_reflns_number_total 4347
_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 1100962
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 0.81788(6) 0.63456(5) 0.19565(4) 0.0253(2) Uani 1 1 d . . .
Cl1 Cl 0.86002(11) 0.57174(10) 0.30274(7) 0.0346(4) Uani 1 1 d . . .
P1 P 0.97840(11) 0.74701(10) 0.18214(7) 0.0259(4) Uani 1 1 d . . .
P2 P 0.72629(11) 0.79963(10) 0.22772(7) 0.0258(4) Uani 1 1 d . . .
C1 C 0.7667(4) 0.5331(4) 0.1204(2) 0.0274(13) Uani 1 1 d . . .
C2 C 0.8443(4) 0.4678(4) 0.0866(2) 0.0249(13) Uani 1 1 d . . .
C3 C 0.8086(5) 0.3874(4) 0.0436(3) 0.0232(13) Uani 1 1 d . . .
H3 H 0.862(3) 0.350(3) 0.0266(19) 0.000(11) Uiso 1 1 d . . .
C4 C 0.6976(4) 0.3656(4) 0.0330(3) 0.0301(13) Uani 1 1 d . . .
C5 C 0.6209(5) 0.4304(4) 0.0646(3) 0.0296(14) Uani 1 1 d . . .
H5 H 0.544(4) 0.419(3) 0.055(2) 0.012(12) Uiso 1 1 d . . .
C6 C 0.6543(4) 0.5119(4) 0.1072(3) 0.0272(13) Uani 1 1 d . . .
C7 C 0.9651(5) 0.4848(5) 0.0951(3) 0.0335(15) Uani 1 1 d . . .
H7C H 0.982(4) 0.502(4) 0.141(3) 0.035(16) Uiso 1 1 d . . .
H7B H 1.008(5) 0.431(5) 0.079(3) 0.08(2) Uiso 1 1 d . . .
H7A H 0.982(4) 0.558(4) 0.071(3) 0.049(17) Uiso 1 1 d . . .
C8 C 0.6585(4) 0.2764(4) -0.0096(3) 0.0351(14) Uani 1 1 d . . .
H8A H 0.7074 0.2665 -0.0494 0.053 Uiso 1 1 calc R . .
H8B H 0.5831 0.2890 -0.0271 0.053 Uiso 1 1 calc R . .
H8C H 0.6595 0.2152 0.0198 0.053 Uiso 1 1 calc R . .
C9 C 0.5660(4) 0.5758(4) 0.1396(3) 0.0404(15) Uani 1 1 d . . .
H9A H 0.4935 0.5459 0.1289 0.061 Uiso 1 1 calc R . .
H9B H 0.5690 0.6450 0.1204 0.061 Uiso 1 1 calc R . .
H9C H 0.5779 0.5783 0.1906 0.061 Uiso 1 1 calc R . .
C10 C 0.9435(5) 0.8624(4) 0.2314(3) 0.0309(14) Uani 1 1 d . . .
H10B H 0.941(3) 0.839(3) 0.276(2) 0.000(11) Uiso 1 1 d . . .
H10A H 0.999(4) 0.915(3) 0.222(2) 0.028(14) Uiso 1 1 d . . .
C11 C 0.8292(5) 0.8996(4) 0.2109(3) 0.0322(15) Uani 1 1 d . . .
H11B H 0.822(4) 0.908(3) 0.156(3) 0.033(14) Uiso 1 1 d . . .
H11A H 0.813(3) 0.961(4) 0.234(2) 0.019(13) Uiso 1 1 d . . .
C12 C 1.1154(4) 0.7129(4) 0.2164(3) 0.0300(13) Uani 1 1 d . . .
C13 C 1.1469(6) 0.7300(5) 0.2848(3) 0.0528(19) Uani 1 1 d . . .
H13 H 1.100(6) 0.754(5) 0.316(4) 0.10(3) Uiso 1 1 d . . .
C14 C 1.2498(6) 0.7017(6) 0.3105(4) 0.069(2) Uani 1 1 d . . .
H14 H 1.273(6) 0.717(5) 0.355(4) 0.09(3) Uiso 1 1 d . . .
C15 C 1.3222(5) 0.6531(5) 0.2686(4) 0.0474(17) Uani 1 1 d . . .
H15 H 1.392(4) 0.630(4) 0.291(3) 0.034(15) Uiso 1 1 d . . .
C16 C 1.2913(5) 0.6343(5) 0.2003(4) 0.0465(18) Uani 1 1 d . . .
H16 H 1.331(5) 0.605(4) 0.172(3) 0.05(2) Uiso 1 1 d . . .
C17 C 1.1893(5) 0.6625(4) 0.1742(4) 0.0393(16) Uani 1 1 d . . .
H17 H 1.171(4) 0.661(4) 0.132(3) 0.034(17) Uiso 1 1 d . . .
C18 C 1.0019(4) 0.7954(4) 0.0944(3) 0.0250(13) Uani 1 1 d . . .
C19 C 1.0871(4) 0.8624(4) 0.0798(3) 0.0289(13) Uani 1 1 d . . .
H19 H 1.148(4) 0.879(3) 0.112(2) 0.028(14) Uiso 1 1 d . . .
C20 C 1.1001(5) 0.9002(4) 0.0130(3) 0.0331(14) Uani 1 1 d . . .
H20 H 1.169(3) 0.941(3) 0.001(2) 0.011(11) Uiso 1 1 d . . .
C21 C 1.0283(5) 0.8719(4) -0.0402(3) 0.0333(14) Uani 1 1 d . . .
H21 H 1.043(4) 0.898(3) -0.082(2) 0.021(14) Uiso 1 1 d . . .
C22 C 0.9434(5) 0.8068(4) -0.0269(3) 0.0362(15) Uani 1 1 d . . .
H22 H 0.899(3) 0.789(3) -0.063(2) 0.010(12) Uiso 1 1 d . . .
C23 C 0.9305(5) 0.7683(4) 0.0393(3) 0.0310(14) Uani 1 1 d . . .
H23 H 0.874(3) 0.726(3) 0.0491(19) 0.000(11) Uiso 1 1 d . . .
C24 C 0.5990(4) 0.8551(4) 0.1909(3) 0.0276(13) Uani 1 1 d . . .
C25 C 0.5939(6) 0.8793(5) 0.1199(3) 0.0441(16) Uani 1 1 d . . .
H25 H 0.663(4) 0.873(3) 0.093(2) 0.036(15) Uiso 1 1 d . . .
C26 C 0.4971(6) 0.9216(5) 0.0911(4) 0.0495(19) Uani 1 1 d . . .
H26 H 0.507(4) 0.938(4) 0.049(3) 0.035(17) Uiso 1 1 d . . .
C27 C 0.4080(6) 0.9385(5) 0.1303(4) 0.0427(18) Uani 1 1 d . . .
H27 H 0.351(4) 0.963(4) 0.113(3) 0.032(17) Uiso 1 1 d . . .
C28 C 0.4111(5) 0.9124(4) 0.1999(4) 0.0428(16) Uani 1 1 d . . .
H28 H 0.347(4) 0.924(4) 0.228(3) 0.041(17) Uiso 1 1 d . . .
C29 C 0.5057(5) 0.8718(4) 0.2300(3) 0.0341(14) Uani 1 1 d . . .
H29 H 0.511(3) 0.853(3) 0.274(2) 0.004(12) Uiso 1 1 d . . .
C30 C 0.7046(4) 0.8023(4) 0.3216(2) 0.0227(12) Uani 1 1 d . . .
C31 C 0.6452(4) 0.7222(4) 0.3510(3) 0.0278(13) Uani 1 1 d . . .
H31 H 0.624(4) 0.670(3) 0.322(2) 0.028(15) Uiso 1 1 d . . .
C32 C 0.6232(5) 0.7221(5) 0.4215(3) 0.0352(15) Uani 1 1 d . . .
H32 H 0.584(3) 0.672(3) 0.436(2) 0.009(13) Uiso 1 1 d . . .
C33 C 0.6583(5) 0.8003(5) 0.4645(3) 0.0361(15) Uani 1 1 d . . .
H33 H 0.651(4) 0.795(4) 0.510(3) 0.042(17) Uiso 1 1 d . . .
C34 C 0.7175(4) 0.8795(4) 0.4368(3) 0.0298(14) Uani 1 1 d . . .
H34 H 0.729(4) 0.937(4) 0.463(2) 0.032(15) Uiso 1 1 d . . .
C35 C 0.7404(4) 0.8797(4) 0.3662(3) 0.0270(13) Uani 1 1 d . . .
H35 H 0.778(3) 0.927(3) 0.349(2) 0.001(12) 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
Fe1 0.0260(5) 0.0256(4) 0.0242(4) -0.0022(3) 0.0021(3) -0.0010(4)
Cl1 0.0390(9) 0.0374(9) 0.0272(8) 0.0022(6) 0.0002(6) 0.0099(7)
P1 0.0238(9) 0.0293(8) 0.0248(8) -0.0053(6) 0.0060(6) -0.0032(7)
P2 0.0257(9) 0.0260(8) 0.0259(8) -0.0015(6) 0.0059(6) 0.0013(7)
C1 0.031(4) 0.028(3) 0.023(3) 0.004(2) 0.005(2) -0.008(3)
C2 0.022(3) 0.028(3) 0.025(3) 0.001(2) 0.004(2) -0.001(3)
C3 0.019(4) 0.026(3) 0.025(3) 0.000(2) 0.009(3) 0.007(3)
C4 0.025(4) 0.033(3) 0.032(3) 0.002(3) 0.002(3) 0.001(3)
C5 0.013(4) 0.040(4) 0.035(3) -0.002(3) -0.002(3) -0.006(3)
C6 0.020(3) 0.036(3) 0.025(3) 0.004(3) 0.007(2) 0.003(3)
C7 0.025(4) 0.038(4) 0.038(4) -0.009(3) -0.001(3) 0.006(3)
C8 0.031(3) 0.040(4) 0.034(3) -0.013(3) 0.006(3) -0.006(3)
C9 0.029(4) 0.049(4) 0.044(4) -0.007(3) 0.009(3) -0.005(3)
C10 0.036(4) 0.030(3) 0.027(3) -0.004(3) 0.014(3) -0.011(3)
C11 0.037(4) 0.027(4) 0.032(4) -0.008(3) 0.011(3) -0.003(3)
C12 0.024(3) 0.035(3) 0.031(3) 0.000(3) 0.004(3) -0.005(3)
C13 0.040(5) 0.081(5) 0.036(4) -0.015(3) -0.008(3) 0.018(4)
C14 0.058(6) 0.095(6) 0.053(5) -0.029(5) -0.024(4) 0.018(5)
C15 0.029(4) 0.050(4) 0.063(5) 0.001(4) -0.015(4) -0.002(3)
C16 0.022(4) 0.050(4) 0.068(5) -0.004(4) 0.013(4) 0.003(3)
C17 0.030(4) 0.048(4) 0.039(4) 0.003(3) 0.003(3) -0.004(3)
C18 0.021(3) 0.023(3) 0.031(3) -0.009(2) 0.009(3) 0.001(3)
C19 0.023(4) 0.030(3) 0.033(3) -0.001(3) 0.001(3) 0.003(3)
C20 0.031(4) 0.029(3) 0.040(4) 0.001(3) 0.015(3) -0.001(3)
C21 0.037(4) 0.032(4) 0.031(4) 0.008(3) 0.008(3) 0.006(3)
C22 0.041(4) 0.041(4) 0.026(4) -0.006(3) -0.005(3) 0.004(3)
C23 0.027(4) 0.033(4) 0.033(4) -0.005(3) 0.005(3) -0.005(3)
C24 0.034(4) 0.022(3) 0.027(3) 0.002(2) 0.000(3) 0.001(3)
C25 0.051(5) 0.043(4) 0.038(4) 0.001(3) 0.006(3) 0.008(3)
C26 0.065(6) 0.047(4) 0.036(4) 0.008(3) -0.016(4) 0.009(4)
C27 0.035(5) 0.039(4) 0.053(5) -0.010(3) -0.019(4) 0.014(3)
C28 0.030(4) 0.044(4) 0.054(5) 0.001(3) -0.006(4) 0.002(3)
C29 0.024(4) 0.047(4) 0.032(4) -0.003(3) 0.002(3) 0.003(3)
C30 0.013(3) 0.028(3) 0.026(3) -0.001(2) 0.002(2) 0.004(2)
C31 0.026(3) 0.029(4) 0.029(3) -0.003(3) 0.007(3) -0.001(3)
C32 0.039(4) 0.030(4) 0.037(4) 0.009(3) 0.016(3) -0.003(3)
C33 0.041(4) 0.044(4) 0.024(4) 0.006(3) 0.009(3) 0.012(3)
C34 0.031(4) 0.032(4) 0.026(3) -0.010(3) 0.001(3) 0.009(3)
C35 0.026(3) 0.023(3) 0.032(3) 0.003(3) 0.003(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'
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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100963.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100963.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_1100963
loop_
_publ_author_name
'Eric J. Hawrelak'
'Wesley H. Bernskoetter'
'Emil Lobkovsky'
'Gordon T. Yee'
'Eckhard Bill'
'Paul J. Chirik'
_publ_section_title
;
Square Planar vs Tetrahedral Geometry in Four Coordinate Iron(II) Complexes
;
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3103
_journal_page_last 3111
_journal_paper_doi 10.1021/ic048202+
_journal_volume 44
_journal_year 2005
_chemical_formula_sum 'C32 H30 Cl10 Fe P2'
_chemical_formula_weight 886.85
_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 difmap
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 103.629(3)
_cell_angle_gamma 90.00
_cell_formula_units_Z 2
_cell_length_a 10.6719(13)
_cell_length_b 14.4951(17)
_cell_length_c 11.6623(14)
_cell_measurement_reflns_used ?
_cell_measurement_temperature 173(2)
_cell_measurement_theta_max ?
_cell_measurement_theta_min ?
_cell_volume 1753.2(4)
_diffrn_ambient_temperature 173(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type 'Bruker 1K CCD area detector'
_diffrn_measurement_method '0.3 deg. 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 0.0659
_diffrn_reflns_av_sigmaI/netI 0.0753
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_k_max 19
_diffrn_reflns_limit_k_min -19
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_number 15148
_diffrn_reflns_theta_max 28.29
_diffrn_reflns_theta_min 2.72
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 1.309
_exptl_absorpt_correction_T_max 0.9374
_exptl_absorpt_correction_T_min 0.8802
_exptl_absorpt_correction_type SADABS
_exptl_absorpt_process_details ?
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.680
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description 'square piramid'
_exptl_crystal_F_000 896
_exptl_crystal_size_max 0.10
_exptl_crystal_size_mid 0.08
_exptl_crystal_size_min 0.05
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.035
_refine_ls_hydrogen_treatment isotropic
_refine_ls_matrix_type full
_refine_ls_number_parameters 265
_refine_ls_number_reflns 4321
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.035
_refine_ls_R_factor_all 0.0899
_refine_ls_R_factor_gt 0.0491
_refine_ls_shift/su_max 0.153
_refine_ls_shift/su_mean 0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0453P)^2^+0.0686P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0898
_refine_ls_wR_factor_ref 0.1010
_reflns_number_gt 2981
_reflns_number_total 4321
_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 1100963
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
Fe1 Fe 0.5000 0.0000 0.0000 0.01373(15) Uani 1 2 d S . .
Cl2 Cl 0.28325(8) 0.15180(6) 0.02531(7) 0.0263(2) Uani 1 1 d . . .
Cl3 Cl 0.17352(8) 0.17950(6) 0.24920(8) 0.0306(2) Uani 1 1 d . . .
Cl4 Cl 0.24457(9) 0.03960(7) 0.45774(8) 0.0345(2) Uani 1 1 d . . .
Cl5 Cl 0.42400(9) -0.12727(6) 0.44089(7) 0.0332(2) Uani 1 1 d . . .
Cl6 Cl 0.54192(8) -0.14789(6) 0.21904(7) 0.0258(2) Uani 1 1 d . . .
P1 P 0.65673(8) 0.09718(6) 0.10340(7) 0.01586(19) Uani 1 1 d . . .
C1 C 0.4143(3) 0.0063(2) 0.1348(3) 0.0174(7) Uani 1 1 d . . .
C2 C 0.3279(3) 0.0759(2) 0.1447(3) 0.0177(7) Uani 1 1 d . . .
C3 C 0.2743(3) 0.0880(2) 0.2418(3) 0.0197(7) Uani 1 1 d . . .
C4 C 0.3061(3) 0.0254(2) 0.3346(3) 0.0212(7) Uani 1 1 d . . .
C5 C 0.3880(3) -0.0476(2) 0.3282(3) 0.0206(7) Uani 1 1 d . . .
C6 C 0.4392(3) -0.0556(2) 0.2291(3) 0.0174(7) Uani 1 1 d . . .
C7 C 0.5932(3) 0.2016(2) 0.1559(3) 0.0185(7) Uani 1 1 d . . .
C8 C 0.5756(3) 0.2825(2) 0.0896(3) 0.0232(7) Uani 1 1 d . . .
H8 H 0.604(3) 0.285(2) 0.019(3) 0.036(10) Uiso 1 1 d . . .
C9 C 0.5211(4) 0.3589(3) 0.1281(3) 0.0294(8) Uani 1 1 d . . .
H9 H 0.511(3) 0.405(2) 0.086(3) 0.031(11) Uiso 1 1 d . . .
C10 C 0.4814(4) 0.3568(3) 0.2327(3) 0.0312(9) Uani 1 1 d . . .
H10 H 0.440(3) 0.402(2) 0.255(3) 0.026(10) Uiso 1 1 d . . .
C11 C 0.4989(3) 0.2776(3) 0.3000(3) 0.0276(8) Uani 1 1 d . . .
H11 H 0.468(3) 0.276(2) 0.372(3) 0.031(10) Uiso 1 1 d . . .
C12 C 0.5537(3) 0.2014(2) 0.2621(3) 0.0210(7) Uani 1 1 d . . .
H12 H 0.563(3) 0.148(2) 0.302(3) 0.010(8) Uiso 1 1 d . . .
C13 C 0.7818(3) 0.1443(3) 0.0337(3) 0.0217(7) Uani 1 1 d . . .
H13B H 0.816(3) 0.193(2) 0.073(3) 0.027(10) Uiso 1 1 d . . .
H13A H 0.742(3) 0.161(2) -0.041(3) 0.029(10) Uiso 1 1 d . . .
C14 C 0.8864(4) 0.0761(3) 0.0253(4) 0.0268(8) Uani 1 1 d . . .
H14C H 0.852(4) 0.023(3) -0.016(4) 0.066(15) Uiso 1 1 d . . .
H14B H 0.936(4) 0.055(3) 0.107(4) 0.066(14) Uiso 1 1 d . . .
H14A H 0.941(4) 0.102(3) 0.002(4) 0.054(14) Uiso 1 1 d . . .
C15 C 0.7518(3) 0.0448(2) 0.2392(3) 0.0221(7) Uani 1 1 d . . .
H15A H 0.691(3) 0.019(2) 0.284(3) 0.021(9) Uiso 1 1 d . . .
H15B H 0.785(4) -0.007(3) 0.212(3) 0.047(13) Uiso 1 1 d . . .
C16 C 0.8523(4) 0.1066(3) 0.3154(3) 0.0280(8) Uani 1 1 d . . .
H16B H 0.819(4) 0.154(3) 0.344(3) 0.035(12) Uiso 1 1 d . . .
H16C H 0.893(4) 0.074(3) 0.373(4) 0.049(13) Uiso 1 1 d . . .
H16A H 0.909(4) 0.133(2) 0.274(3) 0.036(10) 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
Fe1 0.0165(3) 0.0146(3) 0.0112(3) 0.0005(3) 0.0055(3) 0.0013(3)
Cl2 0.0274(5) 0.0270(5) 0.0244(4) 0.0055(4) 0.0062(4) 0.0032(4)
Cl3 0.0259(5) 0.0305(5) 0.0391(5) -0.0079(4) 0.0150(4) 0.0040(4)
Cl4 0.0396(5) 0.0473(6) 0.0239(4) -0.0077(4) 0.0219(4) -0.0079(4)
Cl5 0.0501(6) 0.0325(5) 0.0187(4) 0.0066(4) 0.0114(4) -0.0054(4)
Cl6 0.0305(5) 0.0192(4) 0.0298(5) 0.0017(3) 0.0116(4) 0.0035(4)
P1 0.0185(4) 0.0169(4) 0.0129(4) 0.0014(3) 0.0050(3) -0.0003(3)
C1 0.0196(16) 0.0163(16) 0.0169(15) -0.0007(13) 0.0058(13) -0.0055(13)
C2 0.0189(16) 0.0185(17) 0.0161(15) 0.0005(13) 0.0050(13) -0.0034(13)
C3 0.0170(16) 0.0184(17) 0.0254(17) -0.0060(14) 0.0087(14) -0.0025(14)
C4 0.0218(17) 0.0284(19) 0.0180(16) -0.0078(14) 0.0136(14) -0.0102(14)
C5 0.0258(18) 0.0210(18) 0.0151(16) 0.0028(13) 0.0052(14) -0.0082(15)
C6 0.0202(17) 0.0140(16) 0.0186(16) -0.0027(13) 0.0059(13) -0.0011(13)
C7 0.0185(16) 0.0199(17) 0.0158(16) -0.0026(13) 0.0018(13) -0.0011(14)
C8 0.0275(19) 0.0202(18) 0.0215(18) -0.0002(15) 0.0046(15) -0.0022(15)
C9 0.036(2) 0.019(2) 0.029(2) 0.0020(17) 0.0010(17) -0.0003(17)
C10 0.034(2) 0.022(2) 0.036(2) -0.0116(17) 0.0039(17) 0.0028(17)
C11 0.031(2) 0.031(2) 0.0226(18) -0.0090(16) 0.0108(16) -0.0018(16)
C12 0.0247(18) 0.0195(18) 0.0187(17) -0.0010(14) 0.0046(14) -0.0012(15)
C13 0.0245(18) 0.0228(19) 0.0192(18) 0.0014(15) 0.0078(15) -0.0070(16)
C14 0.0221(19) 0.028(2) 0.034(2) -0.0033(17) 0.0136(17) -0.0059(16)
C15 0.0246(18) 0.025(2) 0.0149(16) 0.0032(15) 0.0010(14) 0.0014(16)
C16 0.026(2) 0.035(2) 0.0193(19) 0.0019(18) -0.0019(16) -0.0055(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'
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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100964.cif | #------------------------------------------------------------------------------
#$Date: 2019-07-03 13:24:39 +0300 (Wed, 03 Jul 2019) $
#$Revision: 216710 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/09/1100964.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_1100964
loop_
_publ_author_name
'Jae Yoo'
'Wolfgang Wernsdorfer'
'En-Che Yang'
'Motohiro Nakano'
'Arnold L. Rheingold'
'David N. Hendrickson'
_publ_section_title
;
One-Dimensional Chain of Tetranuclear Manganese Single-Molecule Magnets
;
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3377
_journal_page_last 3379
_journal_paper_doi 10.1021/ic048212a
_journal_volume 44
_journal_year 2005
_chemical_formula_moiety '(C36 H36 Cl3 Mn4 N6 O6) 2+, 2 (Cl O4) -'
_chemical_formula_sum 'C36 H36 Cl4 Mn4 N6 O14'
_chemical_formula_weight 1138.27
_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 72.939(11)
_cell_angle_beta 74.285(9)
_cell_angle_gamma 70.911(19)
_cell_formula_units_Z 2
_cell_length_a 11.643(6)
_cell_length_b 11.702(6)
_cell_length_c 17.890(9)
_cell_measurement_reflns_used 2559
_cell_measurement_temperature 112(2)
_cell_measurement_theta_max 24.619
_cell_measurement_theta_min 2.284
_cell_volume 2160.4(19)
_computing_cell_refinement 'Bruker SAINT'
_computing_data_collection 'Bruker SMART'
_computing_data_reduction 'Bruker SAINT and SHELXTL'
_computing_molecular_graphics 'XTEL library'
_computing_publication_material 'XTEL library'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 112(2)
_diffrn_detector_area_resol_mean 22.4
_diffrn_detector_details
' The detector was operated in 4x4 "binning" mode.'
_diffrn_detector_type 'Bruker SMART 6000'
_diffrn_measured_fraction_theta_full 0.882
_diffrn_measured_fraction_theta_max 0.882
_diffrn_measurement_details
' 0.3 degree frames were measured with a counting time of 10.2 seconds each.'
_diffrn_measurement_device
'3-circle diffractometer with fixed chi of 54.74 degrees'
_diffrn_measurement_device_type Bruker
_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 0.0699
_diffrn_reflns_av_sigmaI/netI 0.1181
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 21
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_number 7106
_diffrn_reflns_theta_full 25.50
_diffrn_reflns_theta_max 25.50
_diffrn_reflns_theta_min 2.18
_diffrn_standards_decay_% 5.2
_diffrn_standards_interval_time 218
_diffrn_standards_number 72
_exptl_absorpt_coefficient_mu 1.463
_exptl_absorpt_correction_T_max 0.8679
_exptl_absorpt_correction_T_min 0.6210
_exptl_absorpt_correction_type semi-empirical
_exptl_crystal_colour red
_exptl_crystal_density_diffrn 1.750
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description 'irregular block'
_exptl_crystal_F_000 1148
_exptl_crystal_size_max .12
_exptl_crystal_size_mid .10
_exptl_crystal_size_min .08
_refine_diff_density_max 1.631
_refine_diff_density_min -1.191
_refine_diff_density_rms 0.180
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.586
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 577
_refine_ls_number_reflns 7106
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.586
_refine_ls_R_factor_all 0.1670
_refine_ls_R_factor_gt 0.1055
_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
[\s^2^(Fo^2^)+(0.06Fo^2^)^2^]^-1^
;
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2148
_refine_ls_wR_factor_ref 0.2320
_reflns_number_gt 4162
_reflns_number_total 7106
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file ic048212asi20041217_040439.cif
_cod_data_source_block 99063
_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
2019-06-11
Z value and formula fixed to values more according to usual
chemical conventions. miguel
;
_cod_original_formula_sum 'C72 H72 Cl8 Mn8 N12 O28'
_cod_original_formula_weight 2276.54
_cod_original_formula_moiety '(C72 H72 Cl4 Mn8 N12 O12) 4+, 4 (Cl O4) -'
_cod_original_formula_units_Z 1
_cod_original_cell_volume 2160.4(18)
_cod_database_code 1100964
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
Mn1 Mn 0.54580(14) 0.12057(17) 0.48705(10) 0.0218(4) Uani 1 1 d . . .
Mn2 Mn 0.43949(15) 0.08337(18) 0.34478(10) 0.0243(5) Uani 1 1 d . . .
Mn3 Mn 0.61957(13) 0.04435(17) -0.00564(10) 0.0211(4) Uani 1 1 d . . .
Mn4 Mn 0.41035(14) 0.05166(18) 0.15485(10) 0.0247(5) Uani 1 1 d . . .
Cl5 Cl 0.5024(3) 0.1816(3) 0.20424(17) 0.0322(7) Uani 1 1 d . . .
Cl6 Cl 0.3156(2) -0.0157(3) 0.29411(17) 0.0319(8) Uani 1 1 d . . .
O7 O 0.4893(6) 0.1081(8) 0.5962(5) 0.035(2) Uani 1 1 d . . .
C8 C 0.4242(11) 0.2197(13) 0.6256(9) 0.043(4) Uani 1 1 d . . .
C9 C 0.3984(11) 0.3252(14) 0.5570(9) 0.041(4) Uani 1 1 d . . .
C10 C 0.3236(14) 0.4405(15) 0.5656(11) 0.063(5) Uani 1 1 d . . .
C11 C 0.3086(16) 0.5336(16) 0.4970(13) 0.077(6) Uani 1 1 d . . .
C12 C 0.3691(14) 0.5117(15) 0.4195(12) 0.065(5) Uani 1 1 d . . .
C13 C 0.4387(12) 0.3943(14) 0.4166(10) 0.048(4) Uani 1 1 d . . .
N14 N 0.4527(8) 0.3030(10) 0.4829(7) 0.035(3) Uani 1 1 d . . .
O15 O 0.5814(6) 0.1334(8) 0.3770(5) 0.030(2) Uani 1 1 d . . .
C16 C 0.6980(9) 0.1446(13) 0.3300(7) 0.032(3) Uani 1 1 d . . .
C17 C 0.7814(10) 0.1492(11) 0.3795(7) 0.026(3) Uani 1 1 d . . .
C18 C 0.9035(10) 0.1501(12) 0.3480(7) 0.030(3) Uani 1 1 d . . .
C19 C 0.9746(10) 0.1527(13) 0.3968(7) 0.035(3) Uani 1 1 d . . .
C20 C 0.9252(10) 0.1533(12) 0.4762(8) 0.034(3) Uani 1 1 d . . .
C21 C 0.8012(10) 0.1529(12) 0.5024(8) 0.033(3) Uani 1 1 d . . .
N22 N 0.7319(8) 0.1521(9) 0.4544(6) 0.028(2) Uani 1 1 d . . .
O23 O 0.3855(6) 0.0615(7) 0.4775(4) 0.0200(17) Uani 1 1 d . . .
C24 C 0.2637(8) 0.1289(10) 0.5072(6) 0.017(2) Uani 1 1 d . . .
C25 C 0.2197(9) 0.2414(11) 0.4445(7) 0.024(3) Uani 1 1 d . . .
C26 C 0.1130(10) 0.3373(12) 0.4653(8) 0.034(3) Uani 1 1 d . . .
C27 C 0.0711(12) 0.4342(13) 0.4052(9) 0.045(4) Uani 1 1 d . . .
C28 C 0.1342(13) 0.4380(13) 0.3272(8) 0.047(4) Uani 1 1 d . . .
C29 C 0.2366(14) 0.3426(15) 0.3107(8) 0.053(4) Uani 1 1 d . . .
N30 N 0.2787(8) 0.2445(9) 0.3689(5) 0.026(2) Uani 1 1 d . . .
O31 O 0.6396(6) 0.0834(7) -0.1167(5) 0.0262(19) Uani 1 1 d . . .
C32 C 0.6488(10) 0.2047(12) -0.1629(7) 0.031(3) Uani 1 1 d . . .
C33 C 0.6533(9) 0.2846(13) -0.1114(8) 0.030(3) Uani 1 1 d . . .
C34 C 0.6548(10) 0.4088(12) -0.1437(8) 0.036(3) Uani 1 1 d . . .
C35 C 0.6525(11) 0.4733(14) -0.0917(8) 0.042(4) Uani 1 1 d . . .
C36 C 0.6523(10) 0.4213(12) -0.0120(8) 0.035(3) Uani 1 1 d . . .
C37 C 0.6516(9) 0.2984(11) 0.0145(7) 0.023(3) Uani 1 1 d . . .
N38 N 0.6521(7) 0.2297(9) -0.0341(5) 0.022(2) Uani 1 1 d . . .
O39 O 0.6023(6) -0.0177(8) 0.1046(4) 0.0260(19) Uani 1 1 d . . .
C40 C 0.7095(9) -0.0858(13) 0.1385(7) 0.035(3) Uani 1 1 d . . .
C41 C 0.8185(10) -0.1110(13) 0.0734(9) 0.037(3) Uani 1 1 d . . .
C42 C 0.9328(11) -0.1854(14) 0.0896(9) 0.046(4) Uani 1 1 d . . .
C43 C 1.0299(13) -0.1997(19) 0.0241(12) 0.074(6) Uani 1 1 d . . .
C44 C 1.0131(11) -0.1351(16) -0.0516(11) 0.054(4) Uani 1 1 d . . .
C45 C 0.8950(10) -0.0613(13) -0.0614(8) 0.040(4) Uani 1 1 d . . .
N46 N 0.7994(7) -0.0515(10) 0.0004(6) 0.028(2) Uani 1 1 d . . .
O47 O 0.4392(6) 0.1135(7) 0.0215(4) 0.0204(17) Uani 1 1 d . . .
C48 C 0.3677(9) 0.2352(11) -0.0094(7) 0.024(3) Uani 1 1 d . . .
C49 C 0.2581(9) 0.2770(11) 0.0505(7) 0.022(3) Uani 1 1 d . . .
C50 C 0.1664(9) 0.3864(13) 0.0303(8) 0.034(3) Uani 1 1 d . . .
C51 C 0.0647(11) 0.4252(14) 0.0885(9) 0.045(4) Uani 1 1 d . . .
C52 C 0.0560(10) 0.3555(13) 0.1634(8) 0.038(3) Uani 1 1 d . . .
C53 C 0.1503(10) 0.2498(13) 0.1795(7) 0.036(3) Uani 1 1 d . . .
N54 N 0.2470(7) 0.2124(9) 0.1252(5) 0.024(2) Uani 1 1 d . . .
Cl55 Cl 0.9814(3) 0.8165(4) 0.2897(2) 0.0442(9) Uani 1 1 d . . .
O56 O 1.0755(8) 0.7465(12) 0.2415(7) 0.074(4) Uani 1 1 d . . .
O57 O 1.0166(12) 0.8245(14) 0.3559(7) 0.093(5) Uani 1 1 d . . .
O58 O 0.8855(13) 0.759(2) 0.3170(9) 0.154(9) Uani 1 1 d . . .
O59 O 0.9423(19) 0.9356(14) 0.2423(8) 0.160(9) Uani 1 1 d . . .
Cl60 Cl 0.3089(3) 0.4774(4) 0.7844(2) 0.0461(9) Uani 1 1 d . . .
O61 O 0.2482(8) 0.5730(9) 0.7246(6) 0.057(3) Uani 1 1 d . . .
O62 O 0.3306(14) 0.5184(15) 0.8408(8) 0.111(5) Uani 1 1 d . . .
O63 O 0.2216(13) 0.4067(13) 0.8299(7) 0.097(4) Uani 1 1 d . . .
O64 O 0.4112(13) 0.410(2) 0.7462(8) 0.178(11) Uani 1 1 d . . .
H8A H 0.4755 0.2356 0.6555 0.052 Uiso 1 1 calc R . .
H8B H 0.3456 0.2096 0.6621 0.052 Uiso 1 1 calc R . .
H10 H 0.2833 0.4561 0.6168 0.075 Uiso 1 1 calc R . .
H11 H 0.2569 0.6139 0.5017 0.092 Uiso 1 1 calc R . .
H12 H 0.3610 0.5758 0.3726 0.078 Uiso 1 1 calc R . .
H13 H 0.4791 0.3756 0.3661 0.058 Uiso 1 1 calc R . .
H16A H 0.6861 0.2211 0.2872 0.038 Uiso 1 1 calc R . .
H16B H 0.7376 0.0730 0.3045 0.038 Uiso 1 1 calc R . .
H18 H 0.9374 0.1490 0.2935 0.036 Uiso 1 1 calc R . .
H19 H 1.0585 0.1541 0.3760 0.041 Uiso 1 1 calc R . .
H20 H 0.9734 0.1539 0.5112 0.041 Uiso 1 1 calc R . .
H21 H 0.7646 0.1533 0.5567 0.040 Uiso 1 1 calc R . .
H24A H 0.2633 0.1549 0.5552 0.020 Uiso 1 1 calc R . .
H24B H 0.2069 0.0752 0.5225 0.020 Uiso 1 1 calc R . .
H26 H 0.0719 0.3344 0.5193 0.041 Uiso 1 1 calc R . .
H27 H -0.0012 0.4985 0.4170 0.054 Uiso 1 1 calc R . .
H28 H 0.1071 0.5059 0.2855 0.056 Uiso 1 1 calc R . .
H29 H 0.2792 0.3451 0.2571 0.064 Uiso 1 1 calc R . .
H32A H 0.5765 0.2458 -0.1893 0.038 Uiso 1 1 calc R . .
H32B H 0.7245 0.1961 -0.2049 0.038 Uiso 1 1 calc R . .
H34 H 0.6572 0.4453 -0.1989 0.044 Uiso 1 1 calc R . .
H35 H 0.6510 0.5585 -0.1110 0.051 Uiso 1 1 calc R . .
H36 H 0.6527 0.4681 0.0232 0.042 Uiso 1 1 calc R . .
H37 H 0.6507 0.2607 0.0694 0.028 Uiso 1 1 calc R . .
H40A H 0.6968 -0.1651 0.1741 0.042 Uiso 1 1 calc R . .
H40B H 0.7239 -0.0374 0.1704 0.042 Uiso 1 1 calc R . .
H42 H 0.9446 -0.2248 0.1425 0.056 Uiso 1 1 calc R . .
H43 H 1.1084 -0.2547 0.0320 0.089 Uiso 1 1 calc R . .
H44 H 1.0801 -0.1408 -0.0959 0.065 Uiso 1 1 calc R . .
H45 H 0.8816 -0.0165 -0.1134 0.048 Uiso 1 1 calc R . .
H48A H 0.3408 0.2352 -0.0573 0.028 Uiso 1 1 calc R . .
H48B H 0.4197 0.2938 -0.0254 0.028 Uiso 1 1 calc R . .
H50 H 0.1732 0.4344 -0.0229 0.041 Uiso 1 1 calc R . .
H51 H 0.0024 0.4999 0.0754 0.054 Uiso 1 1 calc R . .
H52 H -0.0131 0.3786 0.2040 0.046 Uiso 1 1 calc R . .
H53 H 0.1456 0.2012 0.2326 0.044 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
Mn1 0.0169(8) 0.0150(11) 0.0382(11) -0.0084(8) -0.0027(7) -0.0105(7)
Mn2 0.0255(9) 0.0202(12) 0.0303(10) -0.0090(8) -0.0045(7) -0.0080(8)
Mn3 0.0145(8) 0.0174(11) 0.0373(11) -0.0093(8) -0.0030(7) -0.0109(7)
Mn4 0.0212(8) 0.0252(12) 0.0301(10) -0.0100(8) -0.0028(7) -0.0077(8)
Cl5 0.0414(16) 0.029(2) 0.0332(17) -0.0115(14) -0.0016(13) -0.0189(14)
Cl6 0.0278(14) 0.045(2) 0.0309(16) -0.0109(15) -0.0040(12) -0.0193(14)
O7 0.027(4) 0.032(6) 0.056(6) -0.030(5) -0.024(4) 0.008(4)
C8 0.037(7) 0.029(9) 0.078(11) -0.029(8) -0.019(7) -0.006(6)
C9 0.037(7) 0.035(10) 0.071(10) -0.027(8) -0.023(7) -0.011(6)
C10 0.068(10) 0.020(10) 0.107(14) -0.025(10) -0.029(10) -0.002(8)
C11 0.084(12) 0.012(10) 0.143(19) -0.026(11) -0.045(13) 0.001(8)
C12 0.065(10) 0.017(10) 0.111(15) -0.002(10) -0.027(10) -0.011(8)
C13 0.051(8) 0.027(10) 0.079(11) -0.013(9) -0.018(8) -0.021(7)
N14 0.026(5) 0.023(7) 0.063(8) -0.008(6) -0.012(5) -0.016(5)
O15 0.026(4) 0.033(6) 0.038(5) -0.013(4) -0.002(3) -0.016(4)
C16 0.019(5) 0.052(10) 0.031(7) -0.013(7) -0.001(5) -0.018(6)
C17 0.030(6) 0.016(7) 0.034(7) -0.005(6) -0.003(5) -0.013(5)
C18 0.029(6) 0.024(8) 0.036(7) 0.000(6) 0.003(5) -0.019(6)
C19 0.021(6) 0.038(9) 0.041(8) -0.004(7) -0.004(5) -0.010(6)
C20 0.036(7) 0.017(8) 0.049(8) 0.000(6) -0.019(6) -0.005(6)
C21 0.033(6) 0.020(8) 0.054(9) -0.007(6) -0.011(6) -0.015(6)
N22 0.028(5) 0.014(6) 0.045(7) -0.007(5) -0.010(5) -0.010(4)
O23 0.016(3) 0.009(5) 0.038(5) -0.010(4) -0.002(3) -0.005(3)
C24 0.015(5) 0.011(6) 0.032(6) -0.011(5) -0.003(4) -0.008(4)
C25 0.023(5) 0.015(7) 0.039(7) -0.015(6) -0.002(5) -0.006(5)
C26 0.036(6) 0.013(8) 0.048(8) -0.008(6) -0.004(6) -0.003(6)
C27 0.044(7) 0.015(8) 0.070(10) -0.010(7) -0.005(7) -0.005(6)
C28 0.066(9) 0.017(9) 0.041(8) -0.006(7) -0.005(7) 0.003(7)
C29 0.073(10) 0.042(11) 0.036(8) -0.010(8) -0.015(7) 0.000(8)
N30 0.036(5) 0.013(6) 0.028(6) -0.002(5) -0.001(4) -0.011(4)
O31 0.028(4) 0.011(5) 0.045(5) -0.009(4) -0.001(4) -0.013(3)
C32 0.030(6) 0.024(8) 0.043(8) -0.011(6) 0.002(5) -0.014(6)
C33 0.014(5) 0.032(9) 0.049(8) -0.015(7) -0.003(5) -0.009(5)
C34 0.037(7) 0.020(8) 0.049(8) -0.005(7) -0.006(6) -0.008(6)
C35 0.048(8) 0.029(9) 0.058(10) -0.020(8) -0.001(7) -0.021(7)
C36 0.034(6) 0.034(9) 0.049(9) -0.025(7) 0.010(6) -0.027(6)
C37 0.022(5) 0.018(7) 0.039(7) -0.017(6) 0.002(5) -0.015(5)
N38 0.017(4) 0.017(6) 0.032(6) -0.008(5) -0.001(4) -0.007(4)
O39 0.019(4) 0.027(5) 0.035(5) -0.006(4) -0.006(3) -0.010(4)
C40 0.028(6) 0.032(9) 0.044(8) -0.013(7) -0.013(6) 0.001(6)
C41 0.031(6) 0.031(9) 0.068(10) -0.021(8) -0.025(7) -0.011(6)
C42 0.030(7) 0.042(10) 0.080(11) -0.031(8) -0.025(7) 0.000(6)
C43 0.038(9) 0.076(16) 0.123(17) -0.034(13) -0.033(10) -0.011(9)
C44 0.027(7) 0.057(12) 0.087(13) -0.030(10) 0.000(7) -0.020(7)
C45 0.021(6) 0.043(10) 0.061(9) -0.020(8) -0.002(6) -0.013(6)
N46 0.020(5) 0.033(7) 0.048(7) -0.019(6) -0.006(5) -0.020(5)
O47 0.019(3) 0.016(5) 0.028(4) -0.005(4) 0.000(3) -0.011(3)
C48 0.026(6) 0.010(7) 0.034(7) 0.002(5) -0.007(5) -0.008(5)
C49 0.013(5) 0.024(8) 0.037(7) -0.006(6) -0.007(5) -0.013(5)
C50 0.021(6) 0.033(9) 0.049(8) -0.010(7) -0.011(6) -0.007(6)
C51 0.031(7) 0.038(10) 0.066(10) -0.022(8) -0.008(7) 0.000(6)
C52 0.027(6) 0.033(9) 0.051(9) -0.008(7) 0.004(6) -0.015(6)
C53 0.029(6) 0.041(10) 0.033(7) 0.001(6) -0.003(6) -0.012(6)
N54 0.023(5) 0.026(7) 0.025(5) -0.005(5) -0.008(4) -0.007(4)
Cl55 0.0429(18) 0.047(3) 0.045(2) -0.0155(18) 0.0003(16) -0.0177(17)
O56 0.043(6) 0.078(10) 0.103(9) -0.046(8) 0.010(6) -0.016(6)
O57 0.127(10) 0.119(13) 0.074(8) 0.002(8) -0.035(7) -0.095(10)
O58 0.117(10) 0.29(3) 0.134(13) -0.132(15) 0.076(9) -0.172(14)
O59 0.30(2) 0.048(12) 0.077(10) -0.035(8) -0.053(12) 0.058(12)
Cl60 0.052(2) 0.041(3) 0.043(2) -0.0049(18) -0.0087(16) -0.0137(18)
O61 0.066(6) 0.024(7) 0.069(7) 0.010(5) -0.031(5) 0.002(5)
O62 0.165(13) 0.111(14) 0.100(10) -0.024(10) -0.067(10) -0.059(11)
O63 0.152(12) 0.060(10) 0.095(9) 0.019(8) -0.031(8) -0.076(9)
O64 0.113(11) 0.24(2) 0.084(11) -0.053(13) -0.017(9) 0.097(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'
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'
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
O7 Mn1 O15 172.4(3) . . ?
O7 Mn1 O23 82.2(3) . 2_656 ?
O15 Mn1 O23 99.0(3) . 2_656 ?
O7 Mn1 N14 82.2(4) . . ?
O15 Mn1 N14 96.2(4) . . ?
O23 Mn1 N14 164.2(4) 2_656 . ?
O7 Mn1 N22 108.7(4) . . ?
O15 Mn1 N22 78.8(3) . . ?
O23 Mn1 N22 92.1(3) 2_656 . ?
N14 Mn1 N22 94.9(4) . . ?
O7 Mn1 O23 91.5(3) . . ?
O15 Mn1 O23 81.2(3) . . ?
O23 Mn1 O23 82.2(3) 2_656 . ?
N14 Mn1 O23 96.2(3) . . ?
N22 Mn1 O23 158.1(3) . . ?
O7 Mn2 O15 89.8(3) 2_656 . ?
O7 Mn2 N30 137.7(3) 2_656 . ?
O15 Mn2 N30 99.3(3) . . ?
O7 Mn2 O23 70.0(3) 2_656 . ?
O15 Mn2 O23 75.2(3) . . ?
N30 Mn2 O23 72.7(3) . . ?
O7 Mn2 Cl5 126.9(2) 2_656 . ?
O15 Mn2 Cl5 90.6(2) . . ?
N30 Mn2 Cl5 94.4(3) . . ?
O23 Mn2 Cl5 158.6(2) . . ?
O7 Mn2 Cl6 81.7(2) 2_656 . ?
O15 Mn2 Cl6 166.4(2) . . ?
N30 Mn2 Cl6 94.1(3) . . ?
O23 Mn2 Cl6 111.3(2) . . ?
Cl5 Mn2 Cl6 86.19(11) . . ?
O31 Mn3 O39 171.9(4) . . ?
O31 Mn3 O47 99.1(3) . . ?
O39 Mn3 O47 82.9(3) . . ?
O31 Mn3 N46 96.9(4) . . ?
O39 Mn3 N46 80.6(4) . . ?
O47 Mn3 N46 163.4(4) . . ?
O31 Mn3 N38 79.6(3) . . ?
O39 Mn3 N38 108.2(4) . . ?
O47 Mn3 N38 92.0(3) . . ?
N46 Mn3 N38 95.0(4) . . ?
O31 Mn3 O47 80.5(3) . 2_655 ?
O39 Mn3 O47 92.1(3) . 2_655 ?
O47 Mn3 O47 81.9(3) . 2_655 ?
N46 Mn3 O47 96.8(3) . 2_655 ?
N38 Mn3 O47 157.9(3) . 2_655 ?
O39 Mn4 O31 91.2(3) . 2_655 ?
O39 Mn4 O47 70.6(3) . . ?
O31 Mn4 O47 75.2(3) 2_655 . ?
O39 Mn4 N54 139.0(3) . . ?
O31 Mn4 N54 96.7(3) 2_655 . ?
O47 Mn4 N54 72.8(3) . . ?
O39 Mn4 Cl6 124.3(2) . . ?
O31 Mn4 Cl6 93.0(2) 2_655 . ?
O47 Mn4 Cl6 161.80(19) . . ?
N54 Mn4 Cl6 95.5(2) . . ?
O39 Mn4 Cl5 81.1(2) . . ?
O31 Mn4 Cl5 170.3(2) 2_655 . ?
O47 Mn4 Cl5 107.3(2) . . ?
N54 Mn4 Cl5 92.9(3) . . ?
Cl6 Mn4 Cl5 86.71(11) . . ?
Mn2 Cl5 Mn4 92.72(12) . . ?
Mn4 Cl6 Mn2 92.75(11) . . ?
C8 O7 Mn1 119.4(9) . . ?
C8 O7 Mn2 132.7(8) . 2_656 ?
Mn1 O7 Mn2 107.4(4) . 2_656 ?
O7 C8 C9 108.8(11) . . ?
N14 C9 C10 120.4(15) . . ?
N14 C9 C8 116.7(12) . . ?
C10 C9 C8 122.9(14) . . ?
C9 C10 C11 117.9(17) . . ?
C10 C11 C12 121.7(15) . . ?
C13 C12 C11 116.3(16) . . ?
N14 C13 C12 122.3(16) . . ?
C13 N14 C9 121.3(12) . . ?
C13 N14 Mn1 126.4(10) . . ?
C9 N14 Mn1 112.3(9) . . ?
C16 O15 Mn1 121.8(7) . . ?
C16 O15 Mn2 127.5(7) . . ?
Mn1 O15 Mn2 109.1(3) . . ?
O15 C16 C17 111.2(9) . . ?
N22 C17 C18 121.8(11) . . ?
N22 C17 C16 116.3(9) . . ?
C18 C17 C16 121.9(11) . . ?
C19 C18 C17 118.8(11) . . ?
C18 C19 C20 120.4(10) . . ?
C19 C20 C21 116.7(12) . . ?
N22 C21 C20 122.6(12) . . ?
C17 N22 C21 119.7(10) . . ?
C17 N22 Mn1 111.1(7) . . ?
C21 N22 Mn1 128.2(8) . . ?
C24 O23 Mn1 124.4(6) . 2_656 ?
C24 O23 Mn2 116.3(6) . . ?
Mn1 O23 Mn2 100.2(3) 2_656 . ?
C24 O23 Mn1 118.0(6) . . ?
Mn1 O23 Mn1 97.8(3) 2_656 . ?
Mn2 O23 Mn1 94.5(2) . . ?
O23 C24 C25 110.0(8) . . ?
N30 C25 C26 121.6(11) . . ?
N30 C25 C24 118.1(9) . . ?
C26 C25 C24 120.1(10) . . ?
C27 C26 C25 118.1(12) . . ?
C26 C27 C28 120.0(12) . . ?
C29 C28 C27 119.3(13) . . ?
N30 C29 C28 121.9(13) . . ?
C25 N30 C29 119.1(10) . . ?
C25 N30 Mn2 117.5(8) . . ?
C29 N30 Mn2 123.4(8) . . ?
C32 O31 Mn3 121.2(7) . . ?
C32 O31 Mn4 126.2(7) . 2_655 ?
Mn3 O31 Mn4 109.9(4) . 2_655 ?
O31 C32 C33 111.5(10) . . ?
N38 C33 C34 123.5(12) . . ?
N38 C33 C32 115.7(12) . . ?
C34 C33 C32 120.8(12) . . ?
C35 C34 C33 115.9(13) . . ?
C34 C35 C36 123.0(14) . . ?
C35 C36 C37 117.2(12) . . ?
N38 C37 C36 122.7(12) . . ?
C33 N38 C37 117.8(11) . . ?
C33 N38 Mn3 111.2(8) . . ?
C37 N38 Mn3 130.2(8) . . ?
C40 O39 Mn3 119.7(6) . . ?
C40 O39 Mn4 133.4(7) . . ?
Mn3 O39 Mn4 106.5(3) . . ?
O39 C40 C41 109.2(10) . . ?
N46 C41 C42 123.3(12) . . ?
N46 C41 C40 115.2(10) . . ?
C42 C41 C40 121.4(13) . . ?
C41 C42 C43 116.7(15) . . ?
C44 C43 C42 120.8(14) . . ?
C43 C44 C45 117.9(13) . . ?
N46 C45 C44 121.9(14) . . ?
C41 N46 C45 119.3(10) . . ?
C41 N46 Mn3 114.5(7) . . ?
C45 N46 Mn3 126.2(9) . . ?
C48 O47 Mn3 127.5(6) . . ?
C48 O47 Mn4 115.9(6) . . ?
Mn3 O47 Mn4 99.8(3) . . ?
C48 O47 Mn3 115.0(6) . 2_655 ?
Mn3 O47 Mn3 98.1(3) . 2_655 ?
Mn4 O47 Mn3 94.4(3) . 2_655 ?
O47 C48 C49 111.1(9) . . ?
N54 C49 C50 118.9(10) . . ?
N54 C49 C48 120.0(10) . . ?
C50 C49 C48 121.1(11) . . ?
C51 C50 C49 119.9(12) . . ?
C52 C51 C50 119.2(13) . . ?
C51 C52 C53 117.9(12) . . ?
N54 C53 C52 123.5(12) . . ?
C53 N54 C49 120.6(10) . . ?
C53 N54 Mn4 123.0(8) . . ?
C49 N54 Mn4 116.1(7) . . ?
O56 Cl55 O57 113.8(8) . . ?
O56 Cl55 O58 107.2(9) . . ?
O57 Cl55 O58 107.9(8) . . ?
O56 Cl55 O59 107.3(8) . . ?
O57 Cl55 O59 110.0(10) . . ?
O58 Cl55 O59 110.6(13) . . ?
O64 Cl60 O62 112.9(11) . . ?
O64 Cl60 O61 107.1(8) . . ?
O62 Cl60 O61 115.1(9) . . ?
O64 Cl60 O63 112.8(13) . . ?
O62 Cl60 O63 102.3(9) . . ?
O61 Cl60 O63 106.5(7) . . ?
O7 C8 H8A 109.9 . . ?
C9 C8 H8A 109.9 . . ?
O7 C8 H8B 109.9 . . ?
C9 C8 H8B 109.9 . . ?
H8A C8 H8B 108.3 . . ?
C9 C10 H10 121.0 . . ?
C11 C10 H10 121.0 . . ?
C10 C11 H11 119.1 . . ?
C12 C11 H11 119.1 . . ?
C13 C12 H12 121.9 . . ?
C11 C12 H12 121.9 . . ?
N14 C13 H13 118.8 . . ?
C12 C13 H13 118.8 . . ?
O15 C16 H16A 109.4 . . ?
C17 C16 H16A 109.4 . . ?
O15 C16 H16B 109.4 . . ?
C17 C16 H16B 109.4 . . ?
H16A C16 H16B 108.0 . . ?
C19 C18 H18 120.6 . . ?
C17 C18 H18 120.6 . . ?
C18 C19 H19 119.8 . . ?
C20 C19 H19 119.8 . . ?
C19 C20 H20 121.6 . . ?
C21 C20 H20 121.6 . . ?
N22 C21 H21 118.7 . . ?
C20 C21 H21 118.7 . . ?
O23 C24 H24A 109.7 . . ?
C25 C24 H24A 109.7 . . ?
O23 C24 H24B 109.7 . . ?
C25 C24 H24B 109.7 . . ?
H24A C24 H24B 108.2 . . ?
C27 C26 H26 121.0 . . ?
C25 C26 H26 121.0 . . ?
C26 C27 H27 120.0 . . ?
C28 C27 H27 120.0 . . ?
C29 C28 H28 120.3 . . ?
C27 C28 H28 120.3 . . ?
N30 C29 H29 119.0 . . ?
C28 C29 H29 119.0 . . ?
O31 C32 H32A 109.3 . . ?
C33 C32 H32A 109.3 . . ?
O31 C32 H32B 109.3 . . ?
C33 C32 H32B 109.3 . . ?
H32A C32 H32B 108.0 . . ?
C35 C34 H34 122.0 . . ?
C33 C34 H34 122.0 . . ?
C34 C35 H35 118.5 . . ?
C36 C35 H35 118.5 . . ?
C35 C36 H36 121.4 . . ?
C37 C36 H36 121.4 . . ?
N38 C37 H37 118.7 . . ?
C36 C37 H37 118.7 . . ?
O39 C40 H40A 109.8 . . ?
C41 C40 H40A 109.8 . . ?
O39 C40 H40B 109.8 . . ?
C41 C40 H40B 109.8 . . ?
H40A C40 H40B 108.3 . . ?
C41 C42 H42 121.7 . . ?
C43 C42 H42 121.7 . . ?
C44 C43 H43 119.6 . . ?
C42 C43 H43 119.6 . . ?
C43 C44 H44 121.0 . . ?
C45 C44 H44 121.0 . . ?
N46 C45 H45 119.0 . . ?
C44 C45 H45 119.0 . . ?
O47 C48 H48A 109.4 . . ?
C49 C48 H48A 109.4 . . ?
O47 C48 H48B 109.4 . . ?
C49 C48 H48B 109.4 . . ?
H48A C48 H48B 108.0 . . ?
C51 C50 H50 120.1 . . ?
C49 C50 H50 120.1 . . ?
C52 C51 H51 120.4 . . ?
C50 C51 H51 120.4 . . ?
C51 C52 H52 121.1 . . ?
C53 C52 H52 121.1 . . ?
N54 C53 H53 118.3 . . ?
C52 C53 H53 118.3 . . ?
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
Mn1 O7 1.861(8) . ?
Mn1 O15 1.869(8) . ?
Mn1 O23 1.988(8) 2_656 ?
Mn1 N14 2.043(11) . ?
Mn1 N22 2.210(9) . ?
Mn1 O23 2.253(7) . ?
Mn2 O7 2.167(9) 2_656 ?
Mn2 O15 2.180(8) . ?
Mn2 N30 2.231(10) . ?
Mn2 O23 2.245(7) . ?
Mn2 Cl5 2.457(4) . ?
Mn2 Cl6 2.582(3) . ?
Mn3 O31 1.870(8) . ?
Mn3 O39 1.870(8) . ?
Mn3 O47 1.966(7) . ?
Mn3 N46 2.042(9) . ?
Mn3 N38 2.212(10) . ?
Mn3 O47 2.280(8) 2_655 ?
Mn4 O39 2.149(7) . ?
Mn4 O31 2.180(8) 2_655 ?
Mn4 O47 2.245(7) . ?
Mn4 N54 2.249(9) . ?
Mn4 Cl6 2.444(3) . ?
Mn4 Cl5 2.571(4) . ?
O7 C8 1.448(14) . ?
C8 C9 1.48(2) . ?
C9 N14 1.365(16) . ?
C9 C10 1.37(2) . ?
C10 C11 1.39(2) . ?
C11 C12 1.43(2) . ?
C12 C13 1.36(2) . ?
C13 N14 1.350(17) . ?
O15 C16 1.415(12) . ?
C16 C17 1.503(15) . ?
C17 N22 1.314(14) . ?
C17 C18 1.383(14) . ?
C18 C19 1.368(16) . ?
C19 C20 1.382(16) . ?
C20 C21 1.393(15) . ?
C21 N22 1.332(15) . ?
O23 C24 1.422(11) . ?
C24 C25 1.502(16) . ?
C25 N30 1.337(13) . ?
C25 C26 1.423(15) . ?
C26 C27 1.375(18) . ?
C27 C28 1.385(17) . ?
C28 C29 1.374(18) . ?
C29 N30 1.359(16) . ?
O31 C32 1.439(15) . ?
C32 C33 1.514(17) . ?
C33 N38 1.341(15) . ?
C33 C34 1.402(18) . ?
C34 C35 1.351(18) . ?
C35 C36 1.376(18) . ?
C36 C37 1.378(17) . ?
C37 N38 1.345(14) . ?
O39 C40 1.426(12) . ?
C40 C41 1.486(16) . ?
C41 N46 1.328(16) . ?
C41 C42 1.384(16) . ?
C42 C43 1.40(2) . ?
C43 C44 1.37(2) . ?
C44 C45 1.390(18) . ?
C45 N46 1.340(14) . ?
O47 C48 1.428(13) . ?
C48 C49 1.474(14) . ?
C49 N54 1.324(14) . ?
C49 C50 1.397(16) . ?
C50 C51 1.397(16) . ?
C51 C52 1.345(18) . ?
C52 C53 1.376(17) . ?
C53 N54 1.318(13) . ?
Cl55 O56 1.389(10) . ?
Cl55 O57 1.390(11) . ?
Cl55 O58 1.396(11) . ?
Cl55 O59 1.404(15) . ?
Cl60 O64 1.330(12) . ?
Cl60 O62 1.346(13) . ?
Cl60 O61 1.445(9) . ?
Cl60 O63 1.445(12) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 H29 0.9500 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C42 H42 0.9500 . ?
C43 H43 0.9500 . ?
C44 H44 0.9500 . ?
C45 H45 0.9500 . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C50 H50 0.9500 . ?
C51 H51 0.9500 . ?
C52 H52 0.9500 . ?
C53 H53 0.9500 . ?
|
1100965.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100965.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_1100965
loop_
_publ_author_name
'Jian-Ping Lang'
'Chang-Mei Jiao'
'Shan-Bao Qiao'
'Wen-Hua Zhang'
'Brendan F. Abrahams'
_publ_contact_author_email jplang@suda.edu.cn
_publ_contact_author_fax 86-512-65213506
_publ_contact_author_name 'Jian-Ping Lang'
_publ_contact_author_phone 86-512-65224783
_publ_section_title
;
Acetic Acid Induced Self-Assembly of Supramolecular Compounds
[Et4N]3[(WS4Cu2)2(\m-CN)3].2MeCN and [PPh4][WS4Cu3(\m-CN)2].MeCN from
Preformed Clusters [A]2[WS4(CuCN)2] (A = Et4N, PPh4)
;
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3664
_journal_page_last 3668
_journal_paper_doi 10.1021/ic048224w
_journal_volume 44
_journal_year 2005
_chemical_formula_moiety 'C50 H40 Cu2 N2 P2 S4 W '
_chemical_formula_sum 'C50 H40 Cu2 N2 P2 S4 W'
_chemical_formula_weight 1170.01
_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 70.926(13)
_cell_angle_beta 65.352(11)
_cell_angle_gamma 88.35(2)
_cell_formula_units_Z 2
_cell_length_a 12.7724(4)
_cell_length_b 14.3104(7)
_cell_length_c 15.4164(6)
_cell_measurement_reflns_used 4286
_cell_measurement_temperature 193.1
_cell_measurement_theta_max 27.5
_cell_measurement_theta_min 3.0
_cell_volume 2401.4(4)
_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 SHELXS97
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.9843
_diffrn_measured_fraction_theta_max 0.9843
_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 0.064
_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 18
_diffrn_reflns_limit_l_min -20
_diffrn_reflns_number 24406
_diffrn_reflns_theta_full 27.48
_diffrn_reflns_theta_max 27.48
_exptl_absorpt_coefficient_mu 3.546
_exptl_absorpt_correction_T_max 0.753
_exptl_absorpt_correction_T_min 0.547
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.618
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 1160.00
_exptl_crystal_size_max 0.25
_exptl_crystal_size_mid 0.17
_exptl_crystal_size_min 0.08
_refine_diff_density_max 0.76
_refine_diff_density_min -1.32
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.054
_refine_ls_hydrogen_treatment refall
_refine_ls_number_parameters 590
_refine_ls_number_reflns 6055
_refine_ls_R_factor_gt 0.0550
_refine_ls_shift/su_max 0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details 'w = 1/[0.0020Fo^2^ + 1.0000\s(Fo^2^)]'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_ref 0.0700
_reflns_number_gt 6055
_reflns_number_total 10846
_reflns_threshold_expression F^2^>2.0\s(F^2^)
_cod_data_source_file ic048224wsi20041217_031201_2.cif
_cod_data_source_block '[PPh4]2[WS4(CuCN)2]'
_cod_original_cell_volume 2401.4(2)
_cod_original_formula_sum 'C50 H40 Cu2 N2 P2 S4 W '
_cod_database_code 1100965
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
W(1) W 0.71876(4) 0.72798(3) 0.55149(3) 0.02777(12) Uani 1.00 1 d . . .
Cu(1) Cu 0.67856(12) 0.73712(11) 0.39346(10) 0.0413(4) Uani 1.00 1 d . . .
Cu(2) Cu 0.77724(12) 0.71538(10) 0.70021(10) 0.0376(4) Uani 1.00 1 d . . .
S(1) S 0.5909(2) 0.8140(2) 0.5064(2) 0.0364(8) Uani 1.00 1 d . . .
S(2) S 0.8017(3) 0.6485(2) 0.4446(2) 0.0437(9) Uani 1.00 1 d . . .
S(3) S 0.8560(2) 0.8264(2) 0.5432(2) 0.0396(8) Uani 1.00 1 d . . .
S(4) S 0.6328(2) 0.6217(2) 0.7107(2) 0.0353(8) Uani 1.00 1 d . . .
P(1) P 0.2381(2) 0.6969(2) 0.2530(2) 0.0285(7) Uani 1.00 1 d . . .
P(2) P 0.7575(2) 0.1871(2) 0.1932(2) 0.0287(7) Uani 1.00 1 d . . .
N(1) N 0.6497(9) 0.7476(10) 0.2059(9) 0.066(4) Uani 1.00 1 d . . .
N(2) N 0.8458(9) 0.7084(8) 0.8677(7) 0.050(3) Uani 1.00 1 d . . .
C(1) C 0.6618(11) 0.7448(10) 0.2750(10) 0.055(4) Uani 1.00 1 d . . .
C(2) C 0.8189(9) 0.7093(8) 0.8067(8) 0.033(3) Uani 1.00 1 d . . .
C(3) C 0.2041(9) 0.8219(7) 0.2225(8) 0.032(3) Uani 1.00 1 d . . .
C(4) C 0.2828(10) 0.8980(8) 0.1333(9) 0.043(4) Uani 1.00 1 d . . .
C(5) C 0.2576(11) 0.9973(9) 0.1183(10) 0.048(4) Uani 1.00 1 d . . .
C(6) C 0.1595(13) 1.0194(9) 0.1858(12) 0.058(5) Uani 1.00 1 d . . .
C(7) C 0.0822(12) 0.9456(9) 0.2712(10) 0.053(4) Uani 1.00 1 d . . .
C(8) C 0.1021(11) 0.8462(8) 0.2899(9) 0.043(4) Uani 1.00 1 d . . .
C(9) C 0.2883(9) 0.6731(7) 0.3501(7) 0.026(3) Uani 1.00 1 d . . .
C(10) C 0.3496(10) 0.5933(9) 0.3656(9) 0.043(4) Uani 1.00 1 d . . .
C(11) C 0.3945(10) 0.5749(8) 0.4361(9) 0.038(3) Uani 1.00 1 d . . .
C(12) C 0.3785(10) 0.6354(8) 0.4925(8) 0.041(4) Uani 1.00 1 d . . .
C(13) C 0.3195(11) 0.7166(8) 0.4756(8) 0.043(4) Uani 1.00 1 d . . .
C(14) C 0.2731(10) 0.7350(8) 0.4050(8) 0.040(4) Uani 1.00 1 d . . .
C(15) C 0.1120(8) 0.6123(7) 0.2903(7) 0.027(3) Uani 1.00 1 d . . .
C(16) C 0.0916(9) 0.5188(8) 0.3638(8) 0.036(3) Uani 1.00 1 d . . .
C(17) C 0.0052(10) 0.4509(8) 0.3784(9) 0.047(4) Uani 1.00 1 d . . .
C(18) C -0.0575(10) 0.4728(10) 0.3220(10) 0.052(4) Uani 1.00 1 d . . .
C(19) C -0.0348(10) 0.5684(9) 0.2485(9) 0.048(4) Uani 1.00 1 d . . .
C(20) C 0.0489(8) 0.6369(8) 0.2346(8) 0.033(3) Uani 1.00 1 d . . .
C(21) C 0.3545(9) 0.6782(7) 0.1455(8) 0.030(3) Uani 1.00 1 d . . .
C(22) C 0.3311(9) 0.6224(7) 0.0937(8) 0.033(3) Uani 1.00 1 d . . .
C(23) C 0.4209(9) 0.6083(9) 0.0110(8) 0.040(3) Uani 1.00 1 d . . .
C(24) C 0.5323(10) 0.6448(9) -0.0158(8) 0.045(4) Uani 1.00 1 d . . .
C(25) C 0.5558(10) 0.6973(8) 0.0358(8) 0.038(3) Uani 1.00 1 d . . .
C(26) C 0.4682(9) 0.7154(8) 0.1156(8) 0.038(3) Uani 1.00 1 d . . .
C(27) C 0.6243(9) 0.1207(7) 0.2173(8) 0.032(3) Uani 1.00 1 d . . .
C(28) C 0.6168(9) 0.0183(8) 0.2436(8) 0.037(3) Uani 1.00 1 d . . .
C(29) C 0.5155(11) -0.0338(9) 0.2595(9) 0.049(4) Uani 1.00 1 d . . .
C(30) C 0.4260(10) 0.0158(9) 0.2486(8) 0.046(4) Uani 1.00 1 d . . .
C(31) C 0.4354(10) 0.1171(9) 0.2225(9) 0.043(4) Uani 1.00 1 d . . .
C(32) C 0.5329(9) 0.1722(9) 0.2064(8) 0.038(3) Uani 1.00 1 d . . .
C(33) C 0.6800(10) 0.3575(8) 0.2336(9) 0.044(4) Uani 1.00 1 d . . .
C(34) C 0.7526(9) 0.3188(8) 0.1603(8) 0.035(3) Uani 1.00 1 d . . .
C(35) C 0.8172(10) 0.3854(8) 0.0647(9) 0.044(4) Uani 1.00 1 d . . .
C(36) C 0.8161(12) 0.4874(9) 0.0405(11) 0.057(4) Uani 1.00 1 d . . .
C(37) C 0.7459(13) 0.5219(10) 0.1182(12) 0.064(5) Uani 1.00 1 d . . .
C(38) C 0.6772(13) 0.4582(9) 0.2145(12) 0.061(5) Uani 1.00 1 d . . .
C(39) C 0.7805(9) 0.1455(8) 0.3057(8) 0.031(3) Uani 1.00 1 d . . .
C(40) C 0.8785(10) 0.1870(11) 0.3062(9) 0.057(4) Uani 1.00 1 d . . .
C(41) C 0.9053(11) 0.1540(11) 0.3878(10) 0.058(5) Uani 1.00 1 d . . .
C(42) C 0.8270(12) 0.0793(9) 0.4757(10) 0.049(4) Uani 1.00 1 d . . .
C(43) C 0.7286(12) 0.0427(9) 0.4795(9) 0.051(4) Uani 1.00 1 d . . .
C(44) C 0.7053(10) 0.0731(8) 0.3953(8) 0.041(3) Uani 1.00 1 d . . .
C(45) C 0.8734(9) 0.1657(8) 0.0886(8) 0.032(3) Uani 1.00 1 d . . .
C(46) C 0.9891(10) 0.2006(10) 0.0586(10) 0.055(4) Uani 1.00 1 d . . .
C(47) C 1.0786(10) 0.1887(10) -0.0234(9) 0.049(4) Uani 1.00 1 d . . .
C(48) C 1.0542(9) 0.1413(9) -0.0791(9) 0.045(4) Uani 1.00 1 d . . .
C(49) C 0.9429(9) 0.1066(9) -0.0527(8) 0.041(3) Uani 1.00 1 d . . .
C(50) C 0.8516(9) 0.1185(8) 0.0310(8) 0.038(3) Uani 1.00 1 d . . .
H(1) H 0.3503 0.8826 0.0853 0.051 Uiso 1.00 1 c R . .
H(2) H 0.3100 1.0495 0.0601 0.056 Uiso 1.00 1 c R . .
H(3) H 0.1445 1.0868 0.1738 0.077 Uiso 1.00 1 c R . .
H(4) H 0.0146 0.9624 0.3177 0.074 Uiso 1.00 1 c R . .
H(5) H 0.0471 0.7953 0.3479 0.051 Uiso 1.00 1 c R . .
H(6) H 0.3609 0.5505 0.3274 0.057 Uiso 1.00 1 c R . .
H(7) H 0.4372 0.5200 0.4455 0.053 Uiso 1.00 1 c R . .
H(8) H 0.4073 0.6216 0.5426 0.052 Uiso 1.00 1 c R . .
H(9) H 0.3103 0.7604 0.5124 0.056 Uiso 1.00 1 c R . .
H(10) H 0.2311 0.7903 0.3950 0.055 Uiso 1.00 1 c R . .
H(11) H 0.1354 0.5018 0.4026 0.040 Uiso 1.00 1 c R . .
H(12) H -0.0114 0.3870 0.4295 0.050 Uiso 1.00 1 c R . .
H(13) H -0.1147 0.4243 0.3322 0.061 Uiso 1.00 1 c R . .
H(14) H -0.0774 0.5855 0.2088 0.056 Uiso 1.00 1 c R . .
H(15) H 0.0631 0.7020 0.1859 0.035 Uiso 1.00 1 c R . .
H(16) H 0.2539 0.5946 0.1155 0.040 Uiso 1.00 1 c R . .
H(17) H 0.4054 0.5742 -0.0267 0.049 Uiso 1.00 1 c R . .
H(18) H 0.5945 0.6331 -0.0709 0.054 Uiso 1.00 1 c R . .
H(19) H 0.6339 0.7215 0.0158 0.045 Uiso 1.00 1 c R . .
H(20) H 0.4849 0.7528 0.1501 0.046 Uiso 1.00 1 c R . .
H(21) H 0.6790 -0.0161 0.2509 0.045 Uiso 1.00 1 c R . .
H(22) H 0.5090 -0.1043 0.2778 0.056 Uiso 1.00 1 c R . .
H(23) H 0.3577 -0.0200 0.2591 0.054 Uiso 1.00 1 c R . .
H(24) H 0.3727 0.1508 0.2154 0.054 Uiso 1.00 1 c R . .
H(25) H 0.5379 0.2426 0.1884 0.047 Uiso 1.00 1 c R . .
H(26) H 0.6303 0.3125 0.2992 0.048 Uiso 1.00 1 c R . .
H(27) H 0.8645 0.3605 0.0128 0.050 Uiso 1.00 1 c R . .
H(28) H 0.8616 0.5322 -0.0265 0.069 Uiso 1.00 1 c R . .
H(29) H 0.7455 0.5916 0.1039 0.078 Uiso 1.00 1 c R . .
H(30) H 0.6295 0.4829 0.2664 0.077 Uiso 1.00 1 c R . .
H(31) H 0.9283 0.2404 0.2475 0.064 Uiso 1.00 1 c R . .
H(32) H 0.9744 0.1809 0.3849 0.077 Uiso 1.00 1 c R . .
H(33) H 0.8437 0.0541 0.5331 0.068 Uiso 1.00 1 c R . .
H(34) H 0.6742 -0.0046 0.5413 0.063 Uiso 1.00 1 c R . .
H(35) H 0.6372 0.0439 0.3988 0.050 Uiso 1.00 1 c R . .
H(36) H 1.0058 0.2336 0.0966 0.072 Uiso 1.00 1 c R . .
H(37) H 1.1563 0.2125 -0.0420 0.058 Uiso 1.00 1 c R . .
H(38) H 1.1159 0.1325 -0.1364 0.050 Uiso 1.00 1 c R . .
H(39) H 0.9275 0.0744 -0.0919 0.051 Uiso 1.00 1 c R . .
H(40) H 0.7743 0.0943 0.0490 0.048 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
W(1) 0.0256(2) 0.0287(2) 0.0288(2) 0.0041(2) -0.0113(2) -0.0103(2)
Cu(1) 0.0399(8) 0.0483(9) 0.0342(8) -0.0021(7) -0.0150(7) -0.0133(7)
Cu(2) 0.0362(8) 0.0440(8) 0.0353(8) 0.0069(6) -0.0174(7) -0.0147(7)
S(1) 0.032(2) 0.038(2) 0.044(2) 0.0058(12) -0.0203(13) -0.0159(13)
S(2) 0.046(2) 0.044(2) 0.039(2) 0.014(1) -0.014(1) -0.018(1)
S(3) 0.033(2) 0.042(2) 0.039(2) -0.0010(13) -0.018(1) -0.0062(13)
S(4) 0.038(2) 0.031(1) 0.032(2) 0.0017(12) -0.0109(13) -0.0111(12)
P(1) 0.029(1) 0.026(1) 0.029(2) 0.0027(11) -0.0118(12) -0.0097(12)
P(2) 0.025(1) 0.031(2) 0.029(2) 0.0011(11) -0.0121(12) -0.0079(12)
N(1) 0.041(7) 0.113(10) 0.047(7) -0.014(6) -0.019(6) -0.029(7)
N(2) 0.056(7) 0.055(7) 0.032(6) -0.006(5) -0.023(5) -0.001(5)
C(1) 0.042(8) 0.073(9) 0.037(8) -0.011(7) -0.004(6) -0.018(7)
C(2) 0.025(6) 0.034(6) 0.034(6) -0.010(5) -0.007(5) -0.010(5)
C(3) 0.043(7) 0.020(5) 0.035(6) -0.001(5) -0.023(5) -0.003(5)
C(4) 0.034(6) 0.036(7) 0.059(8) -0.003(5) -0.024(6) -0.009(6)
C(5) 0.049(8) 0.032(7) 0.060(8) -0.014(6) -0.033(7) 0.000(6)
C(6) 0.077(10) 0.021(6) 0.093(11) 0.009(6) -0.056(9) -0.016(7)
C(7) 0.075(10) 0.043(7) 0.068(9) 0.031(7) -0.044(8) -0.038(7)
C(8) 0.054(8) 0.037(7) 0.036(7) 0.008(6) -0.021(6) -0.009(5)
C(9) 0.035(6) 0.017(5) 0.025(5) 0.000(4) -0.014(5) -0.005(4)
C(10) 0.037(7) 0.053(8) 0.053(8) -0.005(6) -0.023(6) -0.028(6)
C(11) 0.045(7) 0.032(6) 0.055(7) 0.017(5) -0.031(6) -0.025(6)
C(12) 0.050(7) 0.046(7) 0.034(7) 0.001(6) -0.022(6) -0.020(6)
C(13) 0.063(8) 0.042(7) 0.034(7) 0.014(6) -0.021(6) -0.025(6)
C(14) 0.063(8) 0.034(6) 0.040(7) 0.019(6) -0.033(6) -0.019(5)
C(15) 0.018(5) 0.031(6) 0.026(6) 0.003(4) -0.002(4) -0.012(5)
C(16) 0.022(5) 0.035(6) 0.042(7) 0.003(5) -0.008(5) -0.011(5)
C(17) 0.044(7) 0.022(6) 0.058(8) -0.009(5) -0.015(6) -0.001(6)
C(18) 0.024(6) 0.062(9) 0.068(9) -0.006(6) -0.005(6) -0.036(8)
C(19) 0.040(7) 0.057(8) 0.044(7) 0.009(6) -0.010(6) -0.024(7)
C(20) 0.026(5) 0.028(6) 0.033(6) -0.009(4) -0.004(5) -0.006(5)
C(21) 0.040(6) 0.024(5) 0.029(6) 0.004(5) -0.015(5) -0.013(5)
C(22) 0.032(6) 0.032(6) 0.035(6) 0.003(5) -0.015(5) -0.010(5)
C(23) 0.033(6) 0.056(7) 0.034(7) 0.002(5) -0.008(5) -0.025(6)
C(24) 0.036(7) 0.063(8) 0.034(7) 0.022(6) -0.009(6) -0.025(6)
C(25) 0.033(6) 0.053(7) 0.025(6) -0.004(5) -0.012(5) -0.008(5)
C(26) 0.037(6) 0.041(7) 0.037(7) -0.004(5) -0.018(5) -0.008(5)
C(27) 0.025(5) 0.027(6) 0.027(6) -0.010(4) -0.000(5) -0.003(5)
C(28) 0.028(6) 0.037(6) 0.048(7) -0.004(5) -0.018(5) -0.012(6)
C(29) 0.052(8) 0.039(7) 0.049(8) -0.003(6) -0.018(7) -0.008(6)
C(30) 0.042(7) 0.059(8) 0.034(7) -0.013(6) -0.017(6) -0.009(6)
C(31) 0.036(6) 0.057(8) 0.042(7) 0.003(6) -0.027(6) -0.010(6)
C(32) 0.033(6) 0.048(7) 0.038(7) 0.006(5) -0.020(5) -0.015(6)
C(33) 0.041(7) 0.034(7) 0.045(7) 0.004(5) -0.012(6) -0.009(6)
C(34) 0.033(6) 0.028(6) 0.045(7) 0.003(5) -0.024(5) -0.004(5)
C(35) 0.048(7) 0.034(7) 0.042(7) -0.002(5) -0.018(6) -0.003(6)
C(36) 0.063(9) 0.035(7) 0.074(10) 0.001(7) -0.043(8) -0.002(7)
C(37) 0.077(10) 0.029(7) 0.088(11) -0.002(7) -0.046(10) -0.008(8)
C(38) 0.078(10) 0.031(7) 0.083(11) 0.016(7) -0.043(9) -0.023(7)
C(39) 0.031(6) 0.041(6) 0.025(6) 0.018(5) -0.013(5) -0.017(5)
C(40) 0.029(6) 0.102(11) 0.030(7) -0.013(7) -0.003(5) -0.023(7)
C(41) 0.043(8) 0.099(11) 0.049(8) 0.023(8) -0.027(7) -0.039(8)
C(42) 0.068(9) 0.049(8) 0.053(8) 0.033(7) -0.044(7) -0.025(7)
C(43) 0.085(10) 0.034(7) 0.039(7) -0.004(7) -0.035(7) -0.006(6)
C(44) 0.049(7) 0.035(6) 0.041(7) -0.007(5) -0.024(6) -0.007(5)
C(45) 0.032(6) 0.036(6) 0.033(6) 0.003(5) -0.014(5) -0.015(5)
C(46) 0.031(7) 0.084(10) 0.066(9) 0.001(6) -0.022(6) -0.043(8)
C(47) 0.029(6) 0.073(9) 0.042(7) 0.003(6) -0.015(6) -0.019(7)
C(48) 0.026(6) 0.063(8) 0.036(7) 0.007(6) -0.003(5) -0.017(6)
C(49) 0.036(6) 0.058(8) 0.034(6) 0.001(6) -0.013(5) -0.025(6)
C(50) 0.032(6) 0.052(7) 0.035(6) 0.002(5) -0.015(5) -0.021(6)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 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)
;
Cu Cu 0.320 1.265
;
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)
;
P P 0.102 0.094
;
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)
;
W W -0.849 6.872
;
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
Cu(2) W(1) Cu(1) 175.00(5) yes . . .
W(1) Cu(1) S(1) 53.1(1) no . . .
S(1) W(1) Cu(1) 54.0(1) no . . .
W(1) Cu(1) S(2) 52.6(1) no . . .
S(2) W(1) Cu(1) 53.7(1) no . . .
S(3) W(1) Cu(1) 124.11(8) no . . .
S(4) W(1) Cu(1) 128.7(1) no . . .
W(1) Cu(1) C(1) 175.8(4) no . . .
S(1) W(1) Cu(2) 130.5(1) no . . .
S(2) W(1) Cu(2) 121.9(1) no . . .
W(1) Cu(2) S(3) 53.3(1) no . . .
S(3) W(1) Cu(2) 53.55(8) no . . .
W(1) Cu(2) S(4) 53.49(8) no . . .
S(4) W(1) Cu(2) 53.7(1) no . . .
W(1) Cu(2) C(2) 178.8(3) yes . . .
W(1) S(1) Cu(1) 72.9(1) yes . . .
S(2) W(1) S(1) 107.7(1) yes . . .
S(3) W(1) S(1) 111.9(1) yes . . .
S(4) W(1) S(1) 111.0(1) yes . . .
W(1) S(2) Cu(1) 73.7(1) yes . . .
S(3) W(1) S(2) 108.2(1) yes . . .
S(4) W(1) S(2) 110.9(1) yes . . .
W(1) S(3) Cu(2) 73.17(9) yes . . .
S(4) W(1) S(3) 107.2(1) yes . . .
W(1) S(4) Cu(2) 72.80(8) yes . . .
S(2) Cu(1) S(1) 105.7(1) yes . . .
C(1) Cu(1) S(1) 129.8(4) yes . . .
C(1) Cu(1) S(2) 124.4(4) yes . . .
Cu(1) C(1) N(1) 178(1) yes . . .
S(4) Cu(2) S(3) 106.7(1) yes . . .
C(2) Cu(2) S(3) 126.0(3) yes . . .
C(2) Cu(2) S(4) 127.2(3) yes . . .
Cu(2) C(2) N(2) 177.8(8) yes . . .
P(1) C(3) C(4) 120.2(8) no . . .
P(1) C(3) C(8) 119.8(7) no . . .
C(9) P(1) C(3) 108.6(6) no . . .
C(15) P(1) C(3) 109.4(5) no . . .
C(21) P(1) C(3) 111.6(4) no . . .
P(1) C(9) C(10) 118(1) no . . .
P(1) C(9) C(14) 122.0(9) no . . .
C(15) P(1) C(9) 113.1(5) no . . .
C(21) P(1) C(9) 106.5(5) no . . .
P(1) C(15) C(16) 119.6(9) no . . .
P(1) C(15) C(20) 118.4(6) no . . .
C(21) P(1) C(15) 107.7(6) no . . .
P(1) C(21) C(22) 120.0(8) no . . .
P(1) C(21) C(26) 120(1) no . . .
P(2) C(27) C(28) 118.1(9) no . . .
P(2) C(27) C(32) 120.8(8) no . . .
C(34) P(2) C(27) 112.3(5) no . . .
C(39) P(2) C(27) 109.2(5) no . . .
C(45) P(2) C(27) 108.3(6) no . . .
P(2) C(34) C(33) 120.0(7) no . . .
P(2) C(34) C(35) 122.9(9) no . . .
C(39) P(2) C(34) 107.1(6) no . . .
C(45) P(2) C(34) 108.0(5) no . . .
P(2) C(39) C(40) 119.9(7) no . . .
P(2) C(39) C(44) 123(1) no . . .
C(45) P(2) C(39) 112.0(5) no . . .
P(2) C(45) C(46) 120(1) no . . .
P(2) C(45) C(50) 121.2(8) no . . .
C(8) C(3) C(4) 119.9(9) no . . .
C(3) C(4) C(5) 117(1) no . . .
C(3) C(8) C(7) 119.5(9) no . . .
C(4) C(5) C(6) 121.3(9) no . . .
C(5) C(6) C(7) 120(1) no . . .
C(6) C(7) C(8) 120(1) no . . .
C(14) C(9) C(10) 119(1) no . . .
C(9) C(10) C(11) 120(1) no . . .
C(9) C(14) C(13) 119(1) no . . .
C(10) C(11) C(12) 120(1) no . . .
C(11) C(12) C(13) 118(1) no . . .
C(12) C(13) C(14) 120(1) no . . .
C(20) C(15) C(16) 121(1) no . . .
C(15) C(16) C(17) 117(1) no . . .
C(15) C(20) C(19) 120.5(9) no . . .
C(16) C(17) C(18) 122(1) no . . .
C(17) C(18) C(19) 118(1) no . . .
C(18) C(19) C(20) 119(1) no . . .
C(26) C(21) C(22) 119(1) no . . .
C(21) C(22) C(23) 119(1) no . . .
C(21) C(26) C(25) 119(1) no . . .
C(22) C(23) C(24) 118(1) no . . .
C(23) C(24) C(25) 121(1) no . . .
C(24) C(25) C(26) 120(1) no . . .
C(32) C(27) C(28) 121(1) no . . .
C(27) C(28) C(29) 118(1) no . . .
C(27) C(32) C(31) 117(1) no . . .
C(28) C(29) C(30) 120(1) no . . .
C(29) C(30) C(31) 119(1) no . . .
C(30) C(31) C(32) 122(1) no . . .
C(33) C(34) C(35) 117(1) no . . .
C(38) C(33) C(34) 122(1) no . . .
C(33) C(38) C(37) 117(1) no . . .
C(34) C(35) C(36) 122(1) no . . .
C(35) C(36) C(37) 117(1) no . . .
C(36) C(37) C(38) 122(1) no . . .
C(44) C(39) C(40) 116(1) no . . .
C(39) C(40) C(41) 122(1) no . . .
C(39) C(44) C(43) 120(1) no . . .
C(40) C(41) C(42) 117(1) no . . .
C(41) C(42) C(43) 120(1) no . . .
C(42) C(43) C(44) 121(1) no . . .
C(50) C(45) C(46) 117(1) no . . .
C(45) C(46) C(47) 122(1) no . . .
C(45) C(50) C(49) 120(1) no . . .
C(46) C(47) C(48) 118(1) no . . .
C(47) C(48) C(49) 120(1) no . . .
C(48) C(49) C(50) 120(1) no . . .
C(3) C(4) H(1) 121.1 no . . .
C(3) C(8) H(5) 120.3 no . . .
H(1) C(4) C(5) 121.1 no . . .
C(4) C(5) H(2) 119.3 no . . .
H(2) C(5) C(6) 119.4 no . . .
C(5) C(6) H(3) 119.6 no . . .
C(6) C(7) H(4) 119.7 no . . .
H(3) C(6) C(7) 119.6 no . . .
C(7) C(8) H(5) 120.2 no . . .
H(4) C(7) C(8) 119.7 no . . .
C(9) C(10) H(6) 119.6 no . . .
C(9) C(14) H(10) 120.0 no . . .
H(6) C(10) C(11) 119.7 no . . .
C(10) C(11) H(7) 119.7 no . . .
C(11) C(12) H(8) 120.6 no . . .
H(7) C(11) C(12) 119.7 no . . .
H(8) C(12) C(13) 120.5 no . . .
C(12) C(13) H(9) 119.7 no . . .
C(13) C(14) H(10) 120.1 no . . .
H(9) C(13) C(14) 119.6 no . . .
C(15) C(16) H(11) 121.3 no . . .
C(15) C(20) H(15) 119.7 no . . .
H(11) C(16) C(17) 121.3 no . . .
C(16) C(17) H(12) 118.7 no . . .
H(12) C(17) C(18) 118.8 no . . .
C(17) C(18) H(13) 120.7 no . . .
C(18) C(19) H(14) 120.1 no . . .
H(13) C(18) C(19) 120.8 no . . .
C(19) C(20) H(15) 119.8 no . . .
H(14) C(19) C(20) 120.1 no . . .
C(21) C(22) H(16) 120.1 no . . .
C(21) C(26) H(20) 120.4 no . . .
H(16) C(22) C(23) 120.1 no . . .
C(22) C(23) H(17) 120.5 no . . .
H(17) C(23) C(24) 120.5 no . . .
C(23) C(24) H(18) 119.3 no . . .
C(24) C(25) H(19) 119.7 no . . .
H(18) C(24) C(25) 119.3 no . . .
C(25) C(26) H(20) 120.4 no . . .
H(19) C(25) C(26) 119.5 no . . .
C(27) C(28) H(21) 120.6 no . . .
C(27) C(32) H(25) 121.2 no . . .
H(21) C(28) C(29) 120.7 no . . .
C(28) C(29) H(22) 119.7 no . . .
H(22) C(29) C(30) 119.7 no . . .
C(29) C(30) H(23) 120.2 no . . .
C(30) C(31) H(24) 118.9 no . . .
H(23) C(30) C(31) 120.2 no . . .
C(31) C(32) H(25) 121.2 no . . .
H(24) C(31) C(32) 118.9 no . . .
H(26) C(33) C(34) 118.7 no . . .
H(26) C(33) C(38) 118.6 no . . .
C(33) C(38) H(30) 121.2 no . . .
C(34) C(35) H(27) 118.67 no . . .
H(27) C(35) C(36) 118.7 no . . .
C(35) C(36) H(28) 121.3 no . . .
C(36) C(37) H(29) 119.0 no . . .
H(28) C(36) C(37) 121.3 no . . .
H(29) C(37) C(38) 119.0 no . . .
C(37) C(38) H(30) 121.0 no . . .
C(39) C(40) H(31) 118.6 no . . .
C(39) C(44) H(35) 119.7 no . . .
H(31) C(40) C(41) 118.6 no . . .
C(40) C(41) H(32) 121.3 no . . .
H(32) C(41) C(42) 121.2 no . . .
C(41) C(42) H(33) 119.7 no . . .
C(42) C(43) H(34) 119.3 no . . .
H(33) C(42) C(43) 119.7 no . . .
C(43) C(44) H(35) 119.7 no . . .
H(34) C(43) C(44) 119.5 no . . .
C(45) C(46) H(36) 119.0 no . . .
C(45) C(50) H(40) 119.9 no . . .
H(36) C(46) C(47) 118.9 no . . .
C(46) C(47) H(37) 120.6 no . . .
H(37) C(47) C(48) 120.5 no . . .
C(47) C(48) H(38) 119.6 no . . .
C(48) C(49) H(39) 119.9 no . . .
H(38) C(48) C(49) 119.5 no . . .
C(49) C(50) H(40) 120.0 no . . .
H(39) C(49) C(50) 119.7 no . . .
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
W(1) Cu(1) 2.655(2) yes . .
W(1) Cu(2) 2.645(2) yes . .
W(1) S(1) 2.222(3) yes . .
W(1) S(2) 2.198(3) yes . .
W(1) S(3) 2.215(4) yes . .
W(1) S(4) 2.226(2) yes . .
Cu(1) S(1) 2.247(4) yes . .
Cu(1) S(2) 2.229(4) yes . .
Cu(1) C(1) 1.89(2) yes . .
Cu(2) S(3) 2.223(3) yes . .
Cu(2) S(4) 2.232(4) yes . .
Cu(2) C(2) 1.90(1) yes . .
P(1) C(3) 1.79(1) no . .
P(1) C(9) 1.80(1) no . .
P(1) C(15) 1.81(1) no . .
P(1) C(21) 1.80(1) no . .
P(2) C(27) 1.81(1) no . .
P(2) C(34) 1.79(1) no . .
P(2) C(39) 1.79(1) no . .
P(2) C(45) 1.79(1) no . .
N(1) C(1) 1.13(2) no . .
N(2) C(2) 1.12(2) no . .
C(3) C(4) 1.42(1) no . .
C(3) C(8) 1.41(2) no . .
C(4) C(5) 1.41(2) no . .
C(5) C(6) 1.36(2) no . .
C(6) C(7) 1.38(2) no . .
C(7) C(8) 1.39(2) no . .
C(9) C(10) 1.38(2) no . .
C(9) C(14) 1.37(2) no . .
C(10) C(11) 1.38(2) no . .
C(11) C(12) 1.37(2) no . .
C(12) C(13) 1.38(2) no . .
C(13) C(14) 1.39(2) no . .
C(15) C(16) 1.39(1) no . .
C(15) C(20) 1.37(2) no . .
C(16) C(17) 1.39(2) no . .
C(17) C(18) 1.37(2) no . .
C(18) C(19) 1.40(2) no . .
C(19) C(20) 1.37(2) no . .
C(21) C(22) 1.41(2) no . .
C(21) C(26) 1.39(2) no . .
C(22) C(23) 1.38(1) no . .
C(23) C(24) 1.37(2) no . .
C(24) C(25) 1.38(2) no . .
C(25) C(26) 1.37(2) no . .
C(27) C(28) 1.38(2) no . .
C(27) C(32) 1.40(2) no . .
C(28) C(29) 1.40(2) no . .
C(29) C(30) 1.37(2) no . .
C(30) C(31) 1.37(2) no . .
C(31) C(32) 1.38(2) no . .
C(33) C(34) 1.40(2) no . .
C(33) C(38) 1.38(2) no . .
C(34) C(35) 1.37(1) no . .
C(35) C(36) 1.38(2) no . .
C(36) C(37) 1.40(2) no . .
C(37) C(38) 1.37(2) no . .
C(39) C(40) 1.40(2) no . .
C(39) C(44) 1.39(1) no . .
C(40) C(41) 1.37(2) no . .
C(41) C(42) 1.40(1) no . .
C(42) C(43) 1.35(2) no . .
C(43) C(44) 1.38(2) no . .
C(45) C(46) 1.40(2) no . .
C(45) C(50) 1.39(2) no . .
C(46) C(47) 1.36(2) no . .
C(47) C(48) 1.38(2) no . .
C(48) C(49) 1.36(2) no . .
C(49) C(50) 1.39(2) no . .
C(50) C(45) 1.39(2) no . .
C(50) C(49) 1.39(2) no . .
C(4) H(1) 0.95 no . .
C(5) H(2) 0.95 no . .
C(6) H(3) 0.95 no . .
C(7) H(4) 0.95 no . .
C(8) H(5) 0.95 no . .
C(10) H(6) 0.95 no . .
C(11) H(7) 0.95 no . .
C(12) H(8) 0.95 no . .
C(13) H(9) 0.95 no . .
C(14) H(10) 0.95 no . .
C(16) H(11) 0.95 no . .
C(17) H(12) 0.95 no . .
C(18) H(13) 0.95 no . .
C(19) H(14) 0.95 no . .
C(20) H(15) 0.95 no . .
C(22) H(16) 0.95 no . .
C(23) H(17) 0.95 no . .
C(24) H(18) 0.95 no . .
C(25) H(19) 0.95 no . .
C(26) H(20) 0.95 no . .
C(28) H(21) 0.95 no . .
C(29) H(22) 0.95 no . .
C(30) H(23) 0.95 no . .
C(31) H(24) 0.95 no . .
C(32) H(25) 0.95 no . .
C(33) H(26) 0.95 no . .
C(35) H(30) 0.95 no . .
C(36) H(29) 0.95 no . .
C(37) H(28) 0.95 no . .
C(38) H(27) 0.95 no . .
C(40) H(31) 0.95 no . .
C(41) H(32) 0.95 no . .
C(42) H(33) 0.95 no . .
C(43) H(34) 0.95 no . .
C(44) H(35) 0.95 no . .
C(46) H(36) 0.95 no . .
C(47) H(37) 0.95 no . .
C(48) H(38) 0.95 no . .
C(49) H(39) 0.95 no . .
C(50) H(40) 0.95 no . .
H(12) C(17) 0.95 no . .
H(17) C(23) 0.95 no . .
|
1100966.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100966.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_1100966
loop_
_publ_author_name
'Jian-Ping Lang'
'Chang-Mei Jiao'
'Shan-Bao Qiao'
'Wen-Hua Zhang'
'Brendan F. Abrahams'
_publ_contact_author_email jplang@suda.edu.cn
_publ_contact_author_fax 86-512-65213506
_publ_contact_author_name 'Jian-Ping Lang'
_publ_contact_author_phone 86-512-65224783
_publ_section_title
;
Acetic Acid Induced Self-Assembly of Supramolecular Compounds
[Et4N]3[(WS4Cu2)2(\m-CN)3].2MeCN and [PPh4][WS4Cu3(\m-CN)2].MeCN from
Preformed Clusters [A]2[WS4(CuCN)2] (A = Et4N, PPh4)
;
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3664
_journal_page_last 3668
_journal_paper_doi 10.1021/ic048224w
_journal_volume 44
_journal_year 2005
_chemical_formula_moiety 'C31 H66 Cu4 N8 S8 W2 '
_chemical_formula_sum 'C31 H66 Cu4 N8 S8 W2'
_chemical_formula_weight 1429.28
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_Int_Tables_number 14
_symmetry_space_group_name_Hall '-P 2yn'
_symmetry_space_group_name_H-M 'P 1 21/n 1'
_cell_angle_alpha 90
_cell_angle_beta 101.785(4)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 10.078(4)
_cell_length_b 18.958(7)
_cell_length_c 13.535(5)
_cell_measurement_reflns_used 6635
_cell_measurement_temperature 193.1
_cell_measurement_theta_max 27.5
_cell_measurement_theta_min 3.2
_cell_volume 2531.5(17)
_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 SHELXS97
_diffrn_detector_area_resol_mean 14.62
_diffrn_measured_fraction_theta_full 0.9962
_diffrn_measured_fraction_theta_max 0.9962
_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 0.040
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 24
_diffrn_reflns_limit_k_min -22
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_number 25541
_diffrn_reflns_theta_full 27.48
_diffrn_reflns_theta_max 27.48
_exptl_absorpt_coefficient_mu 6.542
_exptl_absorpt_correction_T_max 0.375
_exptl_absorpt_correction_T_min 0.264
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour orange
_exptl_crystal_density_diffrn 1.875
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 1400.00
_exptl_crystal_size_max 0.35
_exptl_crystal_size_mid 0.25
_exptl_crystal_size_min 0.15
_refine_diff_density_max 1.63
_refine_diff_density_min -1.25
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.019
_refine_ls_hydrogen_treatment refall
_refine_ls_number_parameters 239
_refine_ls_number_reflns 4715
_refine_ls_R_factor_gt 0.0380
_refine_ls_shift/su_max 0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
'w = 1/[0.0008Fo^2^ + 1.0000\s(Fo^2^) + 0.5000]'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_ref 0.0500
_reflns_number_gt 4715
_reflns_number_total 5781
_reflns_threshold_expression F^2^>2.0\s(F^2^)
_cod_data_source_file ic048224wsi20041217_031201_3.cif
_cod_data_source_block '[Et4N]3[{WS4Cu2(m-CN)}2(m'-CN)].2MeCN'
_cod_original_cell_volume 2531.4(17)
_cod_original_formula_sum 'C31 H66 Cu4 N8 S8 W2 '
_cod_database_code 1100966
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,-Y,-Z
4 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
W(1) W 0.56225(2) 0.18717(10) 0.78849(2) 0.0207(7) Uani 1.00 1 d . . .
Cu(1) Cu 0.67694(9) 0.24783(5) 0.65121(6) 0.0306(2) Uani 1.00 1 d . . .
Cu(2) Cu 0.45556(8) 0.12537(4) 0.93730(6) 0.0268(2) Uani 1.00 1 d . . .
S(1) S 0.5376(2) 0.29912(10) 0.7385(2) 0.0396(5) Uani 1.00 1 d . . .
S(2) S 0.6945(2) 0.13471(10) 0.69766(13) 0.0322(4) Uani 1.00 1 d . . .
S(3) S 0.6590(2) 0.18431(9) 0.94908(12) 0.0287(4) Uani 1.00 1 d . . .
S(4) S 0.3660(2) 0.13219(11) 0.76660(13) 0.0343(5) Uani 1.00 1 d . . .
N(1) N 0.3391(2) 0.1795(2) 1.0146(2) 0.0246(12) Uiso 0.50 1 d P . .
N(1a) N 0.2748(3) 0.2082(3) 1.0633(3) 0.038(2) Uiso 0.50 1 d P . .
N(2) N 0.4781(3) 0.0309(3) 0.9853(3) 0.0306(13) Uiso 0.50 1 d P . .
N(3) N 0.0983(6) 0.3770(3) 0.8289(4) 0.031(2) Uani 1.00 1 d . . .
N(4) N -0.0073(12) 0.0289(6) 0.6290(9) 0.092(4) Uani 1.00 1 d . . .
N(5) N 0.5000 0.5000 0.5000 0.023(2) Uani 1.00 2 d S . .
C(1) C 0.2749(3) 0.2082(3) 1.0634(3) 0.038(2) Uiso 0.50 1 d P . .
C(1a) C 0.3391(2) 0.1795(2) 1.0146(2) 0.0246(12) Uiso 0.50 1 d P . .
C(2) C 0.4781(3) 0.0309(3) 0.9853(3) 0.0306(13) Uiso 0.50 1 d P . .
C(3) C 0.0972(7) 0.4199(4) 0.7329(5) 0.036(2) Uani 1.00 1 d . . .
C(4) C 0.2356(8) 0.4274(6) 0.7060(6) 0.051(3) Uani 1.00 1 d . . .
C(5) C 0.1898(8) 0.4124(5) 0.9176(6) 0.044(2) Uani 1.00 1 d . . .
C(6) C 0.1557(11) 0.4884(6) 0.9386(8) 0.065(3) Uani 1.00 1 d . . .
C(7) C -0.0477(7) 0.3743(4) 0.8400(6) 0.036(2) Uani 1.00 1 d . . .
C(8) C -0.0729(10) 0.3346(6) 0.9322(7) 0.057(3) Uani 1.00 1 d . . .
C(9) C 0.1558(9) 0.3048(4) 0.8208(7) 0.048(2) Uani 1.00 1 d . . .
C(10) C 0.0818(12) 0.2589(5) 0.7343(8) 0.067(3) Uani 1.00 1 d . . .
C(11) C 0.0228(10) 0.0766(6) 0.5859(8) 0.061(3) Uani 1.00 1 d . . .
C(12) C 0.0601(12) 0.1364(6) 0.5295(9) 0.068(3) Uani 1.00 1 d . . .
C(13) C 0.433(2) 0.5386(8) 0.5763(11) 0.035(3) Uiso 0.50 1 d P . .
C(14) C 0.479(2) 0.6113(10) 0.607(2) 0.044(5) Uiso 0.50 1 d P . .
C(15) C 0.6570(13) 0.5027(7) 0.5346(10) 0.026(3) Uiso 0.50 1 d P . .
C(16) C 0.713(2) 0.4748(10) 0.639(2) 0.038(5) Uiso 0.50 1 d P . .
C(17) C 0.451(2) 0.4250(9) 0.4955(12) 0.043(4) Uiso 0.50 1 d P . .
C(18) C 0.498(2) 0.3795(9) 0.4195(13) 0.031(3) Uiso 0.50 1 d P . .
C(19) C 0.468(2) 0.5377(9) 0.3984(12) 0.040(4) Uiso 0.50 1 d P . .
C(20) C 0.317(2) 0.5356(10) 0.349(1) 0.033(4) Uiso 0.50 1 d P . .
H(1) H 0.0383 0.3972 0.6784 0.043 Uiso 1.00 1 c R . .
H(2) H 0.0637 0.4657 0.7421 0.043 Uiso 1.00 1 c R . .
H(3) H 0.2705 0.3819 0.6962 0.063 Uiso 1.00 1 c R . .
H(4) H 0.2276 0.4542 0.6458 0.063 Uiso 1.00 1 c R . .
H(5) H 0.2954 0.4507 0.7593 0.063 Uiso 1.00 1 c R . .
H(6) H 0.1864 0.3855 0.9763 0.051 Uiso 1.00 1 c R . .
H(7) H 0.2795 0.4116 0.9057 0.051 Uiso 1.00 1 c R . .
H(8) H 0.2182 0.5061 0.9955 0.080 Uiso 1.00 1 c R . .
H(9) H 0.1613 0.5157 0.8808 0.080 Uiso 1.00 1 c R . .
H(10) H 0.0668 0.4905 0.9520 0.080 Uiso 1.00 1 c R . .
H(11) H -0.0784 0.4214 0.8439 0.045 Uiso 1.00 1 c R . .
H(12) H -0.0991 0.3521 0.7816 0.045 Uiso 1.00 1 c R . .
H(13) H -0.1664 0.3356 0.9347 0.071 Uiso 1.00 1 c R . .
H(14) H -0.0447 0.2871 0.9275 0.071 Uiso 1.00 1 c R . .
H(15) H -0.0226 0.3560 0.9916 0.071 Uiso 1.00 1 c R . .
H(16) H 0.2467 0.3102 0.8128 0.056 Uiso 1.00 1 c R . .
H(17) H 0.1550 0.2806 0.8822 0.056 Uiso 1.00 1 c R . .
H(18) H -0.0099 0.2536 0.7405 0.078 Uiso 1.00 1 c R . .
H(19) H 0.0847 0.2815 0.6721 0.078 Uiso 1.00 1 c R . .
H(20) H 0.1242 0.2139 0.7373 0.078 Uiso 1.00 1 c R . .
H(21) H 0.1317 0.1233 0.4973 0.081 Uiso 1.00 1 c R . .
H(22) H 0.0889 0.1745 0.5745 0.081 Uiso 1.00 1 c R . .
H(23) H -0.0163 0.1506 0.4801 0.081 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
W(1) 0.0216(1) 0.0216(1) 0.02093(13) 0.00305(10) 0.00911(9) 0.00382(9)
Cu(1) 0.0299(4) 0.0375(5) 0.0273(4) -0.0017(4) 0.0129(3) 0.0086(4)
Cu(2) 0.0288(4) 0.0270(4) 0.0273(4) -0.0011(3) 0.0123(3) -0.0000(3)
S(1) 0.0498(12) 0.0276(9) 0.0476(11) 0.0127(8) 0.0242(9) 0.0140(8)
S(2) 0.0381(10) 0.0350(9) 0.0278(8) 0.0120(7) 0.0167(7) 0.0040(7)
S(3) 0.0278(8) 0.0357(9) 0.0231(7) -0.0064(7) 0.0063(6) -0.0001(7)
S(4) 0.0251(8) 0.0472(11) 0.0297(8) -0.0053(8) 0.0034(7) 0.0013(8)
N(3) 0.025(3) 0.036(3) 0.030(3) -0.001(2) 0.004(2) 0.006(3)
N(4) 0.089(8) 0.085(8) 0.098(8) 0.020(6) 0.011(6) 0.030(7)
N(5) 0.015(3) 0.024(4) 0.032(4) -0.001(3) 0.008(3) 0.007(3)
C(3) 0.030(4) 0.047(4) 0.030(4) 0.003(3) 0.004(3) 0.015(3)
C(4) 0.031(4) 0.085(7) 0.041(4) 0.004(4) 0.013(3) 0.020(5)
C(5) 0.041(5) 0.059(5) 0.028(4) -0.012(4) 0.000(3) 0.011(4)
C(6) 0.067(7) 0.070(7) 0.063(6) -0.023(5) 0.024(5) -0.017(5)
C(7) 0.025(4) 0.046(4) 0.041(4) 0.004(3) 0.015(3) 0.009(3)
C(8) 0.045(5) 0.074(6) 0.058(6) -0.012(5) 0.028(4) 0.012(5)
C(9) 0.049(5) 0.045(5) 0.045(5) 0.019(4) -0.002(4) 0.016(4)
C(10) 0.074(7) 0.053(6) 0.067(6) 0.026(5) -0.005(5) -0.001(5)
C(11) 0.050(6) 0.078(8) 0.052(6) 0.009(5) 0.001(4) -0.009(5)
C(12) 0.069(7) 0.062(7) 0.073(7) 0.004(5) 0.010(6) -0.000(6)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 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)
;
Cu Cu 0.320 1.265
;
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)
;
S S 0.125 0.123
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
W W -0.849 6.872
;
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
Cu(2) W(1) Cu(1) 177.13(2) yes . . .
W(1) Cu(1) S(1) 53.51(6) no . . .
S(1) W(1) Cu(1) 53.79(7) no . . .
W(1) Cu(1) S(2) 53.48(6) no . . .
S(2) W(1) Cu(1) 53.74(5) no . . .
S(3) W(1) Cu(1) 122.52(5) no . . .
S(4) W(1) Cu(1) 128.40(5) no . . .
W(1) Cu(1) N(1a) 174.2(1) yes . . 55404
W(1) Cu(1) C(1) 174.2(1) yes . . 55404
S(1) W(1) Cu(2) 126.61(6) no . . .
S(2) W(1) Cu(2) 125.88(5) no . . .
W(1) Cu(2) S(3) 50.71(4) no . . .
S(3) W(1) Cu(2) 54.64(5) no . . .
W(1) Cu(2) S(4) 50.95(5) no . . .
S(4) W(1) Cu(2) 54.44(5) no . . .
W(1) Cu(2) N(1) 121.7(1) no . . .
W(1) Cu(2) N(2) 128.1(1) no . . .
W(1) Cu(2) C(2) 128.1(1) no . . .
W(1) Cu(2) C(1a) 121.7(1) no . . .
W(1) S(1) Cu(1) 72.70(7) yes . . .
S(2) W(1) S(1) 107.49(8) yes . . .
S(3) W(1) S(1) 108.91(7) yes . . .
S(4) W(1) S(1) 111.67(8) yes . . .
W(1) S(2) Cu(1) 72.78(6) yes . . .
S(3) W(1) S(2) 109.96(6) yes . . .
S(4) W(1) S(2) 109.71(7) yes . . .
W(1) S(3) Cu(2) 74.65(5) yes . . .
S(4) W(1) S(3) 109.08(7) yes . . .
W(1) S(4) Cu(2) 74.62(5) yes . . .
S(2) Cu(1) S(1) 106.95(8) yes . . .
N(1a) Cu(1) S(1) 127.4(2) yes 55404 . .
C(1) Cu(1) S(1) 127.4(2) yes 55404 . .
N(1a) Cu(1) S(2) 125.5(2) yes 55404 . .
C(1) Cu(1) S(2) 125.5(2) yes 55404 . .
Cu(1) N(1a) N(1) 176.0(4) no . 55404 55404
Cu(1) N(1a) C(1) 117(107) no . 55404 55404
C(1) Cu(1) N(1a) 0.0(2) no 55404 . 55404
Cu(1) N(1a) C(1a) 176.0(4) yes . 55404 55404
Cu(1) C(1) N(1) 176.0(4) yes . 55404 55404
Cu(1) C(1) N(1a) 62(107) no . 55404 55404
Cu(1) C(1) C(1a) 176.0(4) no . 55404 55404
S(4) Cu(2) S(3) 101.66(7) yes . . .
N(1) Cu(2) S(3) 108.8(1) yes . . .
N(2) Cu(2) S(3) 112.9(1) yes . . .
C(2) Cu(2) S(3) 112.9(1) no . . .
C(1a) Cu(2) S(3) 108.8(1) no . . .
N(1) Cu(2) S(4) 110.1(1) yes . . .
N(2) Cu(2) S(4) 112.9(1) yes . . .
C(2) Cu(2) S(4) 112.9(1) no . . .
C(1a) Cu(2) S(4) 110.0(1) no . . .
N(2) Cu(2) N(1) 110.2(2) yes . . .
Cu(2) N(1) N(1a) 176.3(4) no . . .
Cu(2) N(1) C(1) 176.3(4) yes . . .
C(2) Cu(2) N(1) 110.2(2) no . . .
Cu(2) N(1) C(1a) 90(96) no . . .
C(1a) Cu(2) N(1) 0.0(2) no . . .
Cu(2) N(2) C(2) 122(128) ? . . .
C(2) Cu(2) N(2) 0.0(2) no . . .
C(1a) Cu(2) N(2) 110.2(2) no . . .
Cu(2) C(2) N(2) 57(128) no . . .
C(1a) Cu(2) C(2) 110.2(2) yes . . .
Cu(2) C(1a) N(1) 89(96) no . . .
Cu(2) C(1a) N(1a) 176.3(4) yes . . .
Cu(2) C(1a) C(1) 176.3(4) no . . .
N(1) N(1a) C(1) 59(109) no . . .
C(1) N(1) N(1a) 0.0(4) no . . .
N(1) N(1a) C(1a) 0.0(3) no . . .
C(1a) N(1) N(1a) 92(97) no . . .
N(1) N(1a) Cu(1) 176.0(4) no . . 45504
N(1) C(1) N(1a) 120(110) no . . .
N(1) C(1) C(1a) 0.0(3) no . . .
C(1a) N(1) C(1) 92(97) no . . .
N(1) C(1) Cu(1) 176.0(4) no . . 45504
N(1) C(1a) N(1a) 87(97) no . . .
N(1) C(1a) C(1) 87(97) no . . .
N(3) C(3) C(4) 113.9(6) no . . .
C(5) N(3) C(3) 109.7(6) no . . .
C(7) N(3) C(3) 105.3(5) no . . .
C(9) N(3) C(3) 111.0(6) no . . .
N(3) C(5) C(6) 116.3(7) no . . .
C(7) N(3) C(5) 112.6(6) no . . .
C(9) N(3) C(5) 106.3(6) no . . .
N(3) C(7) C(8) 115.3(6) no . . .
C(9) N(3) C(7) 112.0(6) no . . .
N(3) C(9) C(10) 116.2(7) no . . .
N(4) C(11) C(12) 178(1) no . . .
C(13) N(5) C(13) 179(1) no 66603 . .
N(5) C(13) C(14) 118(1) no . . .
C(15) N(5) C(13) 110.0(7) no . . .
N(5) C(13) C(15) 55.7(7) no . . 66603
C(15) N(5) C(13) 70.0(7) no 66603 . .
C(17) N(5) C(13) 107.0(9) no . . .
N(5) C(13) C(17) 52.8(7) no . . 66603
C(17) N(5) C(13) 73.0(9) no 66603 . .
N(5) C(13) C(18) 103(1) no . . 66603
C(19) N(5) C(13) 110.1(8) no . . .
N(5) C(13) C(19) 54.9(7) no . . 66603
C(19) N(5) C(13) 69.9(8) no 66603 . .
N(5) C(13) C(14) 118(1) no . 66603 66603
N(5) C(13) C(15) 55.7(7) no . 66603 .
C(15) N(5) C(13) 70.0(7) no . . 66603
C(15) N(5) C(13) 110.0(7) no 66603 . 66603
N(5) C(13) C(17) 52.8(7) no . 66603 .
C(17) N(5) C(13) 73.0(9) no . . 66603
C(17) N(5) C(13) 107.0(9) no 66603 . 66603
N(5) C(13) C(18) 103(1) no . 66603 .
N(5) C(13) C(19) 54.9(7) no . 66603 .
C(19) N(5) C(13) 69.9(8) no . . 66603
C(19) N(5) C(13) 110.1(8) no 66603 . 66603
N(5) C(15) C(13) 54.3(6) no . . 66603
N(5) C(15) C(16) 115(1) no . . .
C(17) N(5) C(15) 110.5(8) no . . .
N(5) C(15) C(17) 53.8(7) no . . 66603
C(17) N(5) C(15) 69.5(8) no 66603 . .
C(19) N(5) C(15) 105.6(8) no . . .
C(19) N(5) C(15) 74.4(8) no 66603 . .
N(5) C(15) C(20) 102(1) no . . 66603
N(5) C(15) C(13) 54.3(6) no . 66603 .
N(5) C(15) C(16) 115(1) no . 66603 66603
N(5) C(15) C(17) 53.8(7) no . 66603 .
C(17) N(5) C(15) 69.5(8) no . . 66603
C(17) N(5) C(15) 110.5(8) no 66603 . 66603
C(19) N(5) C(15) 74.4(8) no . . 66603
C(19) N(5) C(15) 105.6(8) no 66603 . 66603
N(5) C(15) C(20) 102(1) no . 66603 .
N(5) C(17) C(13) 54.2(7) no . . 66603
N(5) C(17) C(14) 102(1) no . . 66603
N(5) C(17) C(15) 56.7(7) no . . 66603
C(17) N(5) C(17) 179(1) no 66603 . .
N(5) C(17) C(18) 115(1) no . . .
C(19) N(5) C(17) 113.6(8) no . . .
N(5) C(17) C(19) 57.4(8) no . . 66603
C(19) N(5) C(17) 66.4(8) no 66603 . .
N(5) C(17) C(13) 54.2(7) no . 66603 .
N(5) C(17) C(14) 102(1) no . 66603 .
N(5) C(17) C(15) 56.7(7) no . 66603 .
N(5) C(17) C(18) 115(1) no . 66603 66603
N(5) C(17) C(19) 57.4(8) no . 66603 .
C(19) N(5) C(17) 66.4(8) no . . 66603
C(19) N(5) C(17) 113.6(8) no 66603 . 66603
N(5) C(19) C(13) 55.2(7) no . . 66603
N(5) C(19) C(16) 101(1) no . . 66603
N(5) C(19) C(17) 56.2(8) no . . 66603
C(19) N(5) C(19) 179(1) no 66603 . .
N(5) C(19) C(20) 112(1) no . . .
N(5) C(19) C(13) 55.2(7) no . 66603 .
N(5) C(19) C(16) 101(1) no . 66603 .
N(5) C(19) C(17) 56.2(8) no . 66603 .
N(5) C(19) C(20) 112(1) no . 66603 66603
N(1a) Cu(1) C(1) 0.0(2) no . 45504 .
C(1) N(1a) Cu(1) 117(107) no . . 45504
C(1a) N(1a) Cu(1) 176.0(4) no . . 45504
N(1a) Cu(1) S(2) 125.5(2) no . 45504 45504
N(1a) C(1) C(1a) 120(110) no . . .
C(1a) N(1a) C(1) 59(109) no . . .
N(1a) C(1) Cu(1) 62(107) no . . 45504
N(1a) C(1a) C(1) 0.0(4) no . . .
C(1a) C(1) Cu(1) 176.0(4) no . . 45504
C(1) Cu(1) S(2) 125.5(2) no . 45504 45504
C(15) C(13) C(14) 136(1) no 66603 . .
C(13) C(14) C(17) 65(1) no . . 66603
C(17) C(13) C(14) 66(1) no 66603 . .
C(13) C(14) C(18) 106(3) no . . 66603
C(18) C(13) C(14) 16(1) no 66603 . .
C(19) C(13) C(14) 125(1) no 66603 . .
C(13) C(15) C(16) 131(1) no . 66603 66603
C(13) C(15) C(17) 87.8(9) no . 66603 .
C(17) C(13) C(15) 89(1) no 66603 . 66603
C(18) C(13) C(15) 124(1) no 66603 . 66603
C(19) C(13) C(15) 88.4(9) no 66603 . 66603
C(13) C(15) C(20) 123(1) no . 66603 .
C(13) C(17) C(14) 48.4(9) no . 66603 .
C(13) C(17) C(15) 90(1) no . 66603 .
C(13) C(17) C(18) 61(1) no . 66603 66603
C(18) C(13) C(17) 50.4(9) no 66603 . 66603
C(13) C(17) C(19) 92(1) no . 66603 .
C(19) C(13) C(17) 90(1) no 66603 . 66603
C(13) C(18) C(14) 57(2) no . 66603 .
C(13) C(18) C(17) 68(1) no . 66603 66603
C(19) C(13) C(18) 122(1) no 66603 . 66603
C(13) C(19) C(16) 116(1) no . 66603 .
C(13) C(19) C(17) 91(1) no . 66603 .
C(13) C(19) C(20) 122(1) no . 66603 66603
C(14) C(17) C(15) 116(1) no . 66603 .
C(14) C(17) C(18) 13.2(9) no . 66603 66603
C(18) C(14) C(17) 42(2) no 66603 . 66603
C(14) C(17) C(19) 128(1) no . 66603 .
C(14) C(18) C(17) 124(3) no . 66603 66603
C(15) C(13) C(14) 136(1) no . 66603 66603
C(16) C(15) C(13) 131(1) no . . 66603
C(15) C(13) C(17) 89(1) no . 66603 .
C(17) C(15) C(13) 87.8(9) no 66603 . 66603
C(15) C(13) C(18) 124(1) no . 66603 .
C(15) C(13) C(19) 88.4(9) no . 66603 .
C(20) C(15) C(13) 123(1) no 66603 . 66603
C(17) C(15) C(16) 126(1) no 66603 . .
C(15) C(16) C(19) 67(1) no . . 66603
C(15) C(16) C(20) 112(3) no . . 66603
C(20) C(15) C(16) 12(1) no 66603 . .
C(15) C(17) C(18) 124(1) no . 66603 66603
C(15) C(17) C(19) 92(1) no . 66603 .
C(20) C(15) C(17) 121(1) no 66603 . 66603
C(15) C(20) C(16) 54(3) no . 66603 .
C(15) C(20) C(19) 69(1) no . 66603 66603
C(16) C(19) C(17) 126(1) no . 66603 .
C(16) C(19) C(20) 10(1) no . 66603 66603
C(20) C(16) C(19) 44(3) no 66603 . 66603
C(16) C(20) C(19) 124(3) no . 66603 66603
C(17) C(13) C(14) 66(1) no . 66603 66603
C(14) C(17) C(13) 48.4(9) no 66603 . 66603
C(15) C(17) C(13) 90(1) no 66603 . 66603
C(17) C(13) C(18) 50.4(9) no . 66603 .
C(18) C(17) C(13) 61(1) no . . 66603
C(17) C(13) C(19) 90(1) no . 66603 .
C(19) C(17) C(13) 92(1) no 66603 . 66603
C(17) C(14) C(13) 65(1) no . 66603 66603
C(15) C(17) C(14) 116(1) no 66603 . 66603
C(17) C(14) C(18) 42(2) no . 66603 .
C(18) C(17) C(14) 13.2(9) no . . 66603
C(19) C(17) C(14) 128(1) no 66603 . 66603
C(17) C(15) C(16) 126(1) no . 66603 66603
C(18) C(17) C(15) 124(1) no . . 66603
C(19) C(17) C(15) 92(1) no 66603 . 66603
C(17) C(15) C(20) 121(1) no . 66603 .
C(17) C(18) C(13) 68(1) no . . 66603
C(17) C(18) C(14) 124(3) no . . 66603
C(19) C(17) C(18) 132(1) no 66603 . .
C(17) C(19) C(20) 131(1) no . 66603 66603
C(18) C(13) C(14) 16(1) no . 66603 66603
C(14) C(18) C(13) 57(2) no 66603 . 66603
C(18) C(13) C(19) 122(1) no . 66603 .
C(18) C(14) C(13) 106(3) no . 66603 66603
C(19) C(13) C(14) 125(1) no . 66603 66603
C(16) C(19) C(13) 116(1) no 66603 . 66603
C(17) C(19) C(13) 91(1) no 66603 . 66603
C(20) C(19) C(13) 122(1) no . . 66603
C(19) C(16) C(15) 67(1) no . 66603 66603
C(17) C(19) C(16) 126(1) no 66603 . 66603
C(19) C(16) C(20) 44(3) no . 66603 .
C(20) C(19) C(16) 10(1) no . . 66603
C(19) C(17) C(18) 132(1) no . 66603 66603
C(20) C(19) C(17) 131(1) no . . 66603
C(19) C(20) C(15) 69(1) no . . 66603
C(19) C(20) C(16) 124(3) no . . 66603
C(20) C(15) C(16) 12(1) no . 66603 66603
C(16) C(20) C(15) 54(3) no 66603 . 66603
C(20) C(16) C(15) 112(3) no . 66603 66603
N(3) C(3) H(1) 108.4 no . . .
N(3) C(3) H(2) 108.4 no . . .
N(3) C(5) H(6) 107.8 no . . .
N(3) C(5) H(7) 107.8 no . . .
N(3) C(7) H(11) 108.0 no . . .
N(3) C(7) H(12) 108.0 no . . .
N(3) C(9) H(16) 107.8 no . . .
N(3) C(9) H(17) 107.8 no . . .
C(3) C(4) H(3) 109.5 no . . .
H(1) C(3) C(4) 108.4 no . . .
H(2) C(3) C(4) 108.4 no . . .
C(3) C(4) H(4) 109.6 no . . .
C(3) C(4) H(5) 109.5 no . . .
H(2) C(3) H(1) 109.5 no . . .
H(4) C(4) H(3) 109.5 no . . .
H(5) C(4) H(3) 109.5 no . . .
H(5) C(4) H(4) 109.3 no . . .
H(6) C(5) C(6) 107.7 no . . .
H(7) C(5) C(6) 107.7 no . . .
C(5) C(6) H(8) 110.4 no . . .
C(5) C(6) H(9) 107.9 no . . .
C(5) C(6) H(10) 109.5 no . . .
H(7) C(5) H(6) 109.5 no . . .
H(9) C(6) H(8) 109.5 no . . .
H(10) C(6) H(8) 109.0 no . . .
H(10) C(6) H(9) 110.5 no . . .
H(11) C(7) C(8) 108.0 no . . .
H(12) C(7) C(8) 108.0 no . . .
C(7) C(8) H(13) 110.7 no . . .
C(7) C(8) H(14) 108.1 no . . .
C(7) C(8) H(15) 109.5 no . . .
H(12) C(7) H(11) 109.5 no . . .
H(14) C(8) H(13) 109.5 no . . .
H(15) C(8) H(13) 108.9 no . . .
H(15) C(8) H(14) 110.2 no . . .
H(16) C(9) C(10) 107.8 no . . .
C(9) C(10) H(20) 109.5 no . . .
H(17) C(9) C(10) 107.8 no . . .
C(9) C(10) H(18) 108.9 no . . .
C(9) C(10) H(19) 108.9 no . . .
H(17) C(9) H(16) 109.6 no . . .
H(20) C(10) H(18) 109.8 no . . .
H(19) C(10) H(18) 109.5 no . . .
H(20) C(10) H(19) 110.3 no . . .
C(11) C(12) H(22) 109.5 no . . .
C(11) C(12) H(21) 109.7 no . . .
C(11) C(12) H(23) 109.3 no . . .
H(22) C(12) H(21) 109.4 no . . .
H(23) C(12) H(21) 109.5 no . . .
H(23) C(12) H(22) 109.5 no . . .
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
W(1) Cu(1) 2.643(1) yes . .
W(1) Cu(2) 2.7331(9) yes . .
W(1) S(1) 2.226(2) yes . .
W(1) S(2) 2.224(2) yes . .
W(1) S(3) 2.194(2) yes . .
W(1) S(4) 2.201(2) yes . .
Cu(1) S(1) 2.234(3) yes . .
Cu(1) S(2) 2.232(2) yes . .
Cu(1) N(1a) 1.887(4) yes . 55404
Cu(1) C(1) 1.887(4) yes . 55404
Cu(2) S(3) 2.311(2) yes . .
Cu(2) S(4) 2.306(2) yes . .
Cu(2) N(1) 2.006(4) yes . .
Cu(2) N(2) 1.903(5) yes . .
Cu(2) C(2) 1.903(5) yes . .
Cu(2) C(1a) 2.006(4) yes . .
N(1) N(1a) 1.152(6) no . .
N(1) C(1) 1.151(6) yes . .
N(1) C(1a) 0.001(7) no . .
N(2) C(2) 0.000(9) no . .
N(3) C(3) 1.53(1) no . .
N(3) C(5) 1.513(9) no . .
N(3) C(7) 1.51(1) no . .
N(3) C(9) 1.50(1) no . .
N(4) C(11) 1.15(2) no . .
N(5) C(13) 1.53(2) no . .
N(5) C(13) 1.53(2) no . 66603
N(5) C(15) 1.56(1) no . .
N(5) C(15) 1.56(1) no . 66603
N(5) C(17) 1.50(2) no . .
N(5) C(17) 1.50(2) no . 66603
N(5) C(19) 1.52(2) no . .
N(5) C(19) 1.52(2) no . 66603
N(1a) Cu(1) 1.887(4) yes . 45504
N(1a) C(1) 0.001(9) no . .
N(1a) C(1a) 1.152(6) yes . .
C(1) Cu(1) 1.887(4) yes . 45504
C(1) C(1a) 1.151(6) yes . .
C(3) C(4) 1.52(1) no . .
C(5) C(6) 1.52(1) no . .
C(7) C(8) 1.52(1) no . .
C(9) C(10) 1.53(1) no . .
C(11) C(12) 1.46(2) no . .
C(13) C(14) 1.49(2) no . .
C(13) C(15) 1.77(2) no . 66603
C(13) C(17) 1.80(2) no . 66603
C(13) C(18) 1.70(2) no . 66603
C(13) C(19) 1.75(2) no . 66603
C(14) C(17) 1.82(3) no . 66603
C(14) C(18) 0.50(3) no . 66603
C(15) C(13) 1.77(2) no . 66603
C(15) C(16) 1.51(2) no . .
C(15) C(17) 1.74(2) no . 66603
C(15) C(20) 1.70(2) no . 66603
C(16) C(19) 1.81(3) no . 66603
C(16) C(20) 0.41(3) no . 66603
C(17) C(13) 1.80(2) no . 66603
C(17) C(14) 1.82(3) no . 66603
C(17) C(15) 1.74(2) no . 66603
C(17) C(18) 1.49(2) no . .
C(17) C(19) 1.66(2) no . 66603
C(18) C(13) 1.70(2) no . 66603
C(18) C(14) 0.50(3) no . 66603
C(19) C(13) 1.75(2) no . 66603
C(19) C(16) 1.81(3) no . 66603
C(19) C(17) 1.66(2) no . 66603
C(19) C(20) 1.54(2) no . .
C(20) C(15) 1.70(2) no . 66603
C(20) C(16) 0.41(3) no . 66603
C(3) H(1) 0.95 no . .
C(3) H(2) 0.95 no . .
C(4) H(3) 0.95 no . .
C(4) H(4) 0.95 no . .
C(4) H(5) 0.95 no . .
C(5) H(6) 0.95 no . .
C(5) H(7) 0.95 no . .
C(6) H(8) 0.95 no . .
C(6) H(9) 0.95 no . .
C(6) H(10) 0.95 no . .
C(7) H(11) 0.95 no . .
C(7) H(12) 0.95 no . .
C(8) H(13) 0.95 no . .
C(8) H(14) 0.95 no . .
C(8) H(15) 0.95 no . .
C(9) H(16) 0.95 no . .
C(9) H(17) 0.95 no . .
C(10) H(18) 0.95 no . .
C(10) H(19) 0.95 no . .
C(10) H(20) 0.95 no . .
C(12) H(21) 0.95 no . .
C(12) H(22) 0.95 no . .
C(12) H(23) 0.95 no . .
|
1100967.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100967.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_1100967
loop_
_publ_author_name
'Jian-Ping Lang'
'Chang-Mei Jiao'
'Shan-Bao Qiao'
'Wen-Hua Zhang'
'Brendan F. Abrahams'
_publ_contact_author_email jplang@suda.edu.cn
_publ_contact_author_fax 86-512-65213506
_publ_contact_author_name 'Jian-Ping Lang'
_publ_contact_author_phone 86-512-65224783
_publ_section_title
;
Acetic Acid Induced Self-Assembly of Supramolecular Compounds
[Et4N]3[(WS4Cu2)2(\m-CN)3].2MeCN and [PPh4][WS4Cu3(\m-CN)2].MeCN from
Preformed Clusters [A]2[WS4(CuCN)2] (A = Et4N, PPh4)
;
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3664
_journal_page_last 3668
_journal_paper_doi 10.1021/ic048224w
_journal_volume 44
_journal_year 2005
_chemical_formula_moiety 'C56 H46 Cu6 N6 P2 S8 W2 '
_chemical_formula_sum 'C56 H46 Cu6 N6 P2 S8 W2'
_chemical_formula_weight 1870.42
_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 128.202(3)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 30.344(3)
_cell_length_b 10.3195(7)
_cell_length_c 26.170(3)
_cell_measurement_reflns_used 9349
_cell_measurement_temperature 193.1
_cell_measurement_theta_max 27.5
_cell_measurement_theta_min 3.2
_cell_volume 6439.7(11)
_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 SHELXS97
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.9942
_diffrn_measured_fraction_theta_max 0.9942
_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 0.045
_diffrn_reflns_limit_h_max 37
_diffrn_reflns_limit_h_min -39
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_l_max 33
_diffrn_reflns_limit_l_min -29
_diffrn_reflns_number 25906
_diffrn_reflns_theta_full 27.48
_diffrn_reflns_theta_max 27.48
_exptl_absorpt_coefficient_mu 5.852
_exptl_absorpt_correction_T_max 0.310
_exptl_absorpt_correction_T_min 0.216
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour orange
_exptl_crystal_density_diffrn 1.929
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 3616.00
_exptl_crystal_size_max 0.30
_exptl_crystal_size_mid 0.22
_exptl_crystal_size_min 0.20
_refine_diff_density_max 1.39
_refine_diff_density_min -1.37
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.012
_refine_ls_hydrogen_treatment refall
_refine_ls_number_parameters 258
_refine_ls_number_reflns 5614
_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/[0.0008Fo^2^ + 2.0000\s(Fo^2^) + 0.3000]'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_ref 0.0570
_reflns_number_gt 5614
_reflns_number_total 7352
_reflns_threshold_expression F^2^>2.0\s(F^2^)
_cod_data_source_file ic048224wsi20041217_031201_1.cif
_cod_data_source_block '[PPh4]2[{WS4Cu3(m-CN)}2(m'-CN)2].2MeCN'
_cod_original_cell_volume 6439.6(10)
_cod_original_formula_sum 'C56 H46 Cu6 N6 P2 S8 W2 '
_cod_database_code 1100967
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +X,+Y,+Z
2 -X,+Y,1/2-Z
3 -X,-Y,-Z
4 +X,-Y,1/2+Z
5 1/2+X,1/2+Y,+Z
6 1/2-X,1/2+Y,1/2-Z
7 1/2-X,1/2-Y,-Z
8 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
W(1) W 0.07576(10) 0.31426(3) 0.13739(10) 0.0185(8) Uani 1.00 1 d . . .
Cu(1) Cu 0.17252(4) 0.43535(10) 0.21771(5) 0.0304(3) Uani 1.00 1 d . . .
Cu(2) Cu -0.00860(4) 0.15593(9) 0.05843(5) 0.0270(3) Uani 1.00 1 d . . .
Cu(3) Cu 0.13476(4) 0.11747(9) 0.13516(5) 0.0247(2) Uani 1.00 1 d . . .
S(1) S 0.14155(8) 0.3367(2) 0.12404(10) 0.0275(5) Uani 1.00 1 d . . .
S(2) S 0.07118(8) 0.1046(2) 0.15682(10) 0.0235(5) Uani 1.00 1 d . . .
S(3) S -0.00601(9) 0.3704(2) 0.04670(11) 0.0335(5) Uani 1.00 1 d . . .
S(4) S 0.10169(10) 0.4309(2) 0.22284(11) 0.0344(6) Uani 1.00 1 d . . .
P(1) P 0.84228(11) 0.4593(4) 0.0556(1) 0.0688(10) Uani 1.00 1 d . . .
N(1) N -0.0648(3) 0.0427(3) -0.0054(3) 0.032(2) Uiso 0.50 1 d P . .
N(2) N 0.0952(3) 0.0243(3) 0.0494(3) 0.022(1) Uiso 0.50 1 d P . .
N(3) N 0.6286(6) 0.3140(12) 0.2641(7) 0.095(4) Uiso 1.00 1 d . . .
N(1a) N 0.2452(3) 0.5056(3) 0.2723(3) 0.035(2) Uiso 0.50 1 d P . .
N(2a) N 0.2097(3) 0.0422(3) 0.1961(3) 0.027(2) Uiso 0.50 1 d P . .
C(1) C 0.2452(3) 0.5055(3) 0.2724(3) 0.035(2) Uiso 0.50 1 d P . .
C(2) C 0.2098(3) 0.0422(3) 0.1962(3) 0.027(2) Uiso 0.50 1 d P . .
C(1a) C -0.0648(3) 0.0428(3) -0.0054(3) 0.032(2) Uiso 0.50 1 d P . .
C(2a) C 0.0951(3) 0.0244(3) 0.0493(3) 0.022(1) Uiso 0.50 1 d P . .
C(3) C 0.8138(4) 0.4026(9) -0.0244(5) 0.038(2) Uiso 1.00 1 d . . .
C(4) C 0.7827(4) 0.4874(10) -0.0764(5) 0.042(2) Uiso 1.00 1 d . . .
C(5) C 0.7589(4) 0.4468(10) -0.1389(5) 0.043(2) Uiso 1.00 1 d . . .
C(6) C 0.7672(4) 0.3171(9) -0.1485(5) 0.040(2) Uiso 1.00 1 d . . .
C(7) C 0.7977(4) 0.2341(10) -0.0976(5) 0.039(2) Uiso 1.00 1 d . . .
C(8) C 0.8219(4) 0.2769(10) -0.0351(5) 0.043(2) Uiso 1.00 1 d . . .
C(9) C 0.6249(6) 0.2916(13) 0.2213(7) 0.068(3) Uiso 1.00 1 d . . .
C(10) C 0.6159(7) 0.257(2) 0.1636(8) 0.091(5) Uiso 1.00 1 d . . .
C(11) C 0.7862(4) 0.5243(10) 0.0536(5) 0.043(2) Uiso 1.00 1 d . . .
C(12) C 0.7998(5) 0.5872(10) 0.1085(5) 0.048(3) Uiso 1.00 1 d . . .
C(13) C 0.7574(5) 0.6408(11) 0.1068(6) 0.053(3) Uiso 1.00 1 d . . .
C(14) C 0.7006(5) 0.6351(11) 0.0507(6) 0.052(3) Uiso 1.00 1 d . . .
C(15) C 0.686(2) 0.565(5) -0.005(3) 0.07(2) Uiso 0.33 1 d P . .
C(15a) C 0.6947(11) 0.533(3) 0.0116(13) 0.017(5) Uiso 0.33 1 d P . .
C(15b) C 0.6830(10) 0.617(3) -0.0123(12) 0.016(5) Uiso 0.33 1 d P . .
C(16) C 0.732(2) 0.504(5) -0.002(3) 0.06(2) Uiso 0.33 1 d P . .
C(16a) C 0.7371(13) 0.468(3) 0.012(2) 0.030(7) Uiso 0.33 1 d P . .
C(16b) C 0.7283(9) 0.560(2) -0.0116(11) 0.015(4) Uiso 0.33 1 d P . .
C(17) C 0.8870(7) 0.617(2) 0.0717(9) 0.030(4) Uiso 0.50 1 d P . .
C(17a) C 0.9012(7) 0.539(2) 0.0908(9) 0.030(4) Uiso 0.50 1 d P . .
C(18) C 0.9099(4) 0.6152(10) 0.0452(5) 0.046(2) Uiso 1.00 1 d . . .
C(19) C 0.9492(6) 0.7127(12) 0.0648(7) 0.065(3) Uiso 1.00 1 d . . .
C(20) C 0.9658(9) 0.810(2) 0.1082(11) 0.048(5) Uiso 0.50 1 d P . .
C(20a) C 0.9825(11) 0.730(3) 0.1386(13) 0.062(6) Uiso 0.50 1 d P . .
C(21) C 0.9380(9) 0.809(2) 0.1353(11) 0.049(5) Uiso 0.50 1 d P . .
C(21a) C 0.9806(11) 0.660(2) 0.1823(13) 0.061(6) Uiso 0.50 1 d P . .
C(22) C 0.8989(9) 0.710(2) 0.1182(10) 0.042(5) Uiso 0.50 1 d P . .
C(22a) C 0.9387(9) 0.568(2) 0.1583(11) 0.046(5) Uiso 0.50 1 d P . .
C(23) C 0.8712(7) 0.286(2) 0.1093(8) 0.023(3) Uiso 0.50 1 d P . .
C(23a) C 0.8754(7) 0.360(2) 0.1115(8) 0.025(3) Uiso 0.50 1 d P . .
C(24) C 0.8460(5) 0.2556(12) 0.1288(6) 0.060(3) Uiso 1.00 1 d . . .
C(25) C 0.8664(8) 0.117(2) 0.1710(10) 0.039(5) Uiso 0.50 1 d P . .
C(25a) C 0.8724(8) 0.170(2) 0.1648(9) 0.033(4) Uiso 0.50 1 d P . .
C(26) C 0.9121(9) 0.054(2) 0.1781(10) 0.045(5) Uiso 0.50 1 d P . .
C(26a) C 0.9310(9) 0.155(2) 0.1979(11) 0.048(5) Uiso 0.50 1 d P . .
C(27) C 0.9375(8) 0.110(2) 0.1524(10) 0.038(4) Uiso 0.50 1 d P . .
C(27a) C 0.9597(9) 0.245(2) 0.1855(11) 0.049(5) Uiso 0.50 1 d P . .
C(28) C 0.9201(8) 0.226(2) 0.1215(10) 0.038(4) Uiso 0.50 1 d P . .
C(28a) C 0.9321(7) 0.349(2) 0.1434(8) 0.028(4) Uiso 0.50 1 d P . .
H(1) H 0.7778 0.5742 -0.0688 0.051 Uiso 1.00 1 c R . .
H(2) H 0.7375 0.5048 -0.1746 0.052 Uiso 1.00 1 c R . .
H(3) H 0.7512 0.2874 -0.1911 0.048 Uiso 1.00 1 c R . .
H(4) H 0.8025 0.1468 -0.1048 0.047 Uiso 1.00 1 c R . .
H(5) H 0.8445 0.2197 0.0008 0.051 Uiso 1.00 1 c R . .
H(6) H 0.6318 0.1737 0.1687 0.109 Uiso 1.00 1 c R . .
H(7) H 0.6331 0.3188 0.1542 0.109 Uiso 1.00 1 c R . .
H(8) H 0.5768 0.2540 0.1289 0.109 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
W(1) 0.0156(1) 0.0174(2) 0.0203(2) -0.00249(12) 0.00999(12) -0.00276(13)
Cu(1) 0.0202(5) 0.0284(5) 0.0307(6) -0.0084(4) 0.0097(5) -0.0064(4)
Cu(2) 0.0202(5) 0.0302(5) 0.0246(5) -0.0071(4) 0.0109(4) -0.0072(4)
Cu(3) 0.0174(5) 0.0268(5) 0.0231(5) 0.0013(4) 0.0091(4) -0.0024(4)
S(1) 0.0256(10) 0.0283(11) 0.0318(11) -0.0074(8) 0.0193(9) -0.0027(8)
S(2) 0.0226(9) 0.0208(9) 0.0258(10) -0.0019(7) 0.0144(9) 0.0017(8)
S(3) 0.0242(10) 0.0296(11) 0.0319(12) 0.0039(8) 0.0099(10) 0.0061(9)
S(4) 0.0371(12) 0.0344(11) 0.0344(12) -0.0086(9) 0.0234(11) -0.0147(9)
P(1) 0.0286(13) 0.155(4) 0.030(1) -0.032(2) 0.0213(12) -0.040(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)
;
Cu Cu 0.320 1.265
;
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)
;
P P 0.102 0.094
;
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)
;
W W -0.849 6.872
;
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
Cu(2) W(1) Cu(1) 168.61(4) yes . . .
Cu(3) W(1) Cu(1) 87.02(3) yes . . .
W(1) Cu(1) S(1) 53.83(7) no . . .
S(1) W(1) Cu(1) 54.26(6) no . . .
S(2) W(1) Cu(1) 118.02(5) no . . .
S(3) W(1) Cu(1) 133.73(7) no . . .
W(1) Cu(1) S(4) 53.18(6) no . . .
S(4) W(1) Cu(1) 54.00(9) no . . .
W(1) Cu(1) N(1a) 172.9(2) yes . . .
W(1) Cu(1) C(1) 172.9(2) yes . . .
Cu(3) W(1) Cu(2) 81.60(3) yes . . .
S(1) W(1) Cu(2) 117.95(6) no . . .
W(1) Cu(2) S(2) 54.04(5) no . . .
S(2) W(1) Cu(2) 54.16(4) no . . .
W(1) Cu(2) S(3) 52.87(5) no . . .
S(3) W(1) Cu(2) 54.36(6) no . . .
S(4) W(1) Cu(2) 134.07(9) no . . .
W(1) Cu(2) N(1) 171.2(3) yes . . .
W(1) Cu(2) C(1a) 171.2(3) yes . . .
W(1) Cu(3) S(1) 52.00(8) no . . .
S(1) W(1) Cu(3) 54.19(6) no . . .
W(1) Cu(3) S(2) 51.97(5) no . . .
S(2) W(1) Cu(3) 54.69(8) no . . .
S(3) W(1) Cu(3) 119.31(8) no . . .
S(4) W(1) Cu(3) 126.73(6) no . . .
W(1) Cu(3) N(2) 115.5(2) no . . .
W(1) Cu(3) C(2a) 115.5(2) no . . .
W(1) Cu(3) N(2a) 136.4(2) no . . .
W(1) Cu(3) C(2) 136.4(2) no . . .
W(1) S(1) Cu(1) 71.9(1) yes . . .
W(1) S(1) Cu(3) 73.81(9) yes . . .
S(2) W(1) S(1) 108.71(9) yes . . .
S(3) W(1) S(1) 108.9(1) yes . . .
S(4) W(1) S(1) 107.9(1) yes . . .
W(1) S(2) Cu(2) 71.80(6) yes . . .
W(1) S(2) Cu(3) 73.34(9) yes . . .
S(3) W(1) S(2) 108.15(7) yes . . .
S(4) W(1) S(2) 109.2(1) yes . . .
W(1) S(3) Cu(2) 72.78(7) yes . . .
S(4) W(1) S(3) 114.0(1) yes . . .
W(1) S(4) Cu(1) 72.8(1) yes . . .
Cu(1) S(1) Cu(3) 108.4(1) yes . . .
S(4) Cu(1) S(1) 106.64(9) yes . . .
N(1a) Cu(1) S(1) 120.4(3) yes . . .
C(1) Cu(1) S(1) 120.4(3) yes . . .
N(1a) Cu(1) S(4) 132.9(3) yes . . .
C(1) Cu(1) S(4) 133.0(3) yes . . .
Cu(1) N(1a) N(2a) 175.4(8) no . . 55506
Cu(1) N(1a) C(1) 129(110) no . . .
C(1) Cu(1) N(1a) 0.0(4) no . . .
Cu(1) N(1a) C(2) 175.4(8) yes . . 55506
Cu(1) C(1) N(1a) 50(110) no . . .
Cu(1) C(1) N(2a) 175.5(8) yes . . 55506
Cu(1) C(1) C(2) 175.5(8) yes . . 55506
Cu(2) S(2) Cu(3) 100.1(1) yes . . .
S(3) Cu(2) S(2) 106.55(7) yes . . .
N(1) Cu(2) S(2) 127.8(1) yes . . .
C(1a) Cu(2) S(2) 127.8(1) yes . . .
N(1) Cu(2) S(3) 125.5(1) yes . . .
C(1a) Cu(2) S(3) 125.5(1) yes . . .
Cu(2) N(1) N(2) 168.8(9) no . . 55503
Cu(2) N(1) C(1a) 100(70) no . . .
C(2a) Cu(2) N(1) 0.0(4) no . . .
Cu(2) N(1) C(2a) 168.8(9) yes . . 55503
Cu(2) C(1a) N(1) 79(70) no . . .
Cu(2) C(1a) N(2) 168.7(9) yes . . 55503
Cu(2) C(1a) C(2a) 168.7(9) no . . 55503
S(2) Cu(3) S(1) 103.8(1) yes . . .
N(2) Cu(3) S(1) 111.4(1) yes . . .
C(2a) Cu(3) S(1) 111.4(1) yes . . .
N(2a) Cu(3) S(1) 110.0(1) yes . . .
C(2) Cu(3) S(1) 110.0(1) yes . . .
N(2) Cu(3) S(2) 103.4(2) yes . . .
C(2a) Cu(3) S(2) 103.4(2) yes . . .
N(2a) Cu(3) S(2) 120.0(3) yes . . .
C(2) Cu(3) S(2) 120.0(3) yes . . .
Cu(3) N(2) C(2a) 119(96) yes . . .
C(2a) Cu(3) N(2) 0.0(3) no . . .
Cu(3) N(2) N(1) 161.9(8) no . . 55503
N(2a) Cu(3) N(2) 108.1(2) no . . .
C(2) Cu(3) N(2) 108.1(2) yes . . .
Cu(3) N(2) C(1a) 161.9(8) yes . . 55503
C(2a) Cu(3) N(2a) 108.1(2) no . . .
Cu(3) N(2a) N(1a) 172.2(8) no . . 54506
Cu(3) N(2a) C(1) 172.2(8) yes . . 54506
Cu(3) N(2a) C(2) 161(160) yes . . .
C(2) Cu(3) N(2a) 0.0(4) no . . .
C(2a) Cu(3) C(2) 108.1(2) no . . .
Cu(3) C(2) N(1a) 172.2(8) yes . . 54506
Cu(3) C(2) N(2a) 18(159) no . . .
Cu(3) C(2) C(1) 172.3(8) no . . 54506
Cu(3) C(2a) N(2) 60(96) no . . .
Cu(3) C(2a) N(1) 161.9(8) yes . . 55503
Cu(3) C(2a) C(1a) 161.9(8) no . . 55503
P(1) C(3) C(4) 118.9(8) no . . .
P(1) C(3) C(8) 121.6(8) no . . .
C(11) P(1) C(3) 108.8(5) no . . .
C(17) P(1) C(3) 106.7(8) no . . .
C(23) P(1) C(3) 101.6(6) no . . .
C(17a) P(1) C(3) 112(1) no . . .
C(23a) P(1) C(3) 116.7(8) no . . .
P(1) C(11) C(12) 118.2(7) no . . .
P(1) C(11) C(16) 118(3) no . . .
C(17) P(1) C(11) 102.1(8) no . . .
C(23) P(1) C(11) 109.4(8) no . . .
P(1) C(11) C(16a) 115(2) no . . .
P(1) C(11) C(16b) 121(1) no . . .
C(17a) P(1) C(11) 120.9(9) no . . .
C(23a) P(1) C(11) 109(1) no . . .
P(1) C(17) C(18) 114(1) no . . .
P(1) C(17) C(22) 121(2) no . . .
C(23) P(1) C(17) 127.4(6) no . . .
P(1) C(17) C(17a) 54(1) no . . .
C(17a) P(1) C(17) 26.7(7) no . . .
C(23a) P(1) C(17) 112.6(8) no . . .
P(1) C(23) C(24) 113(1) no . . .
P(1) C(23) C(28) 117(1) no . . .
C(17a) P(1) C(23) 101.2(7) no . . .
P(1) C(23) C(23a) 35(1) no . . .
C(23a) P(1) C(23) 17.0(7) no . . .
P(1) C(23) C(28a) 83(1) no . . .
P(1) C(17a) C(17) 98(1) no . . .
P(1) C(17a) C(18) 117(1) no . . .
P(1) C(17a) C(22a) 124(2) no . . .
C(23a) P(1) C(17a) 87.5(9) no . . .
P(1) C(23a) C(23) 127(1) no . . .
P(1) C(23a) C(24) 123(1) no . . .
P(1) C(23a) C(28) 128(1) no . . .
P(1) C(23a) C(28a) 118(1) no . . .
N(1) N(2) C(1a) 0.0(7) no . 55503 .
C(1a) N(1) N(2) 86(69) no . . 55503
N(1) N(2) C(2a) 57(91) no . 55503 55503
C(2a) N(1) N(2) 0.0(6) no 55503 . 55503
N(1) N(2) Cu(3) 161.9(8) no . 55503 55503
N(1) C(1a) N(2) 93(69) no . . 55503
N(1) C(1a) C(2a) 93(69) no . . 55503
C(2a) N(1) C(1a) 86(69) no 55503 . .
N(1) C(2a) N(2) 122(92) no . 55503 55503
N(1) C(2a) C(1a) 0.0(7) no . 55503 .
N(1) C(2a) Cu(3) 161.9(8) yes . 55503 55503
N(2) N(1) C(2a) 0.0(6) no . 55503 .
C(2a) N(2) N(1) 57(92) no . . 55503
N(2) N(1) C(1a) 86(68) no . 55503 55503
C(1a) N(2) N(1) 0.0(7) no 55503 . 55503
N(2) N(1) Cu(2) 168.8(9) no . 55503 55503
N(2) C(1a) C(2a) 0.0(6) no . 55503 .
C(2a) N(2) C(1a) 57(92) no . . 55503
N(2) C(1a) N(1) 93(68) no . 55503 55503
N(2) C(1a) Cu(2) 168.7(9) yes . 55503 55503
N(2) C(2a) N(1) 122(92) no . . 55503
N(2) C(2a) C(1a) 122(92) no . . 55503
N(3) C(9) C(10) 175(1) no . . .
N(1a) N(2a) C(1) 0.0(7) no . 55506 .
C(1) N(1a) N(2a) 46(119) no . . 55506
N(1a) N(2a) C(2) 15(168) no . 55506 55506
C(2) N(1a) N(2a) 0.0(6) no 55506 . 55506
N(1a) N(2a) Cu(3) 172.2(8) ? . 55506 55506
N(1a) C(1) N(2a) 133(120) no . . 55506
N(1a) C(1) C(2) 133(120) no . . 55506
C(2) N(1a) C(1) 46(119) no 55506 . .
N(1a) C(2) N(2a) 164(169) no . 55506 55506
N(1a) C(2) C(1) 0.0(7) no . 55506 .
N(1a) C(2) Cu(3) 172.2(8) yes . 55506 55506
N(2a) N(1a) C(1) 46(119) no . 54506 54506
C(1) N(2a) N(1a) 0.0(7) no 54506 . 54506
N(2a) N(1a) C(2) 0.0(6) no . 54506 .
C(2) N(2a) N(1a) 15(168) no . . 54506
N(2a) N(1a) Cu(1) 175.4(7) no . 54506 54506
N(2a) C(1) N(1a) 133(120) no . 54506 54506
N(2a) C(1) C(2) 0.0(6) no . 54506 .
C(2) N(2a) C(1) 15(168) no . . 54506
N(2a) C(1) Cu(1) 175.5(7) yes . 54506 54506
N(2a) C(2) N(1a) 164(169) no . . 54506
N(2a) C(2) C(1) 164(169) no . . 54506
C(1) N(2a) C(2) 15(168) no . 55506 55506
C(2) C(1) N(2a) 0.0(6) no 55506 . 55506
C(1) N(2a) Cu(3) 172.2(8) yes . 55506 55506
C(1) C(2) N(2a) 164(169) no . 55506 55506
C(1) C(2) Cu(3) 172.3(8) yes . 55506 55506
C(2) N(1a) C(1) 46(119) no . 54506 54506
C(1) C(2) N(1a) 0.0(7) no 54506 . 54506
C(2) N(1a) Cu(1) 175.4(7) yes . 54506 54506
C(2) C(1) N(1a) 133(120) no . 54506 54506
C(2) C(1) Cu(1) 175.5(7) no . 54506 54506
C(8) C(3) C(4) 119(1) no . . .
C(3) C(4) C(5) 120(1) no . . .
C(3) C(8) C(7) 120.5(9) no . . .
C(4) C(5) C(6) 118.4(9) no . . .
C(5) C(6) C(7) 120(1) no . . .
C(6) C(7) C(8) 120(1) no . . .
C(16) C(11) C(12) 123(3) no . . .
C(16a) C(11) C(12) 121(2) no . . .
C(16b) C(11) C(12) 115(1) no . . .
C(11) C(12) C(13) 118.7(9) no . . .
C(11) C(16) C(16a) 72(5) no . . .
C(16a) C(11) C(16) 19(2) no . . .
C(11) C(16) C(16b) 94(5) no . . .
C(16b) C(11) C(16) 23(2) no . . .
C(11) C(16) C(15) 118(4) no . . .
C(11) C(16) C(15a) 109(4) no . . .
C(11) C(16) C(15b) 114(3) no . . .
C(11) C(16a) C(16) 88(7) no . . .
C(11) C(16a) C(16b) 80(2) no . . .
C(16b) C(11) C(16a) 42(1) no . . .
C(11) C(16a) C(15) 110(2) no . . .
C(11) C(16a) C(15a) 110(2) no . . .
C(11) C(16b) C(16) 62(4) no . . .
C(11) C(16b) C(16a) 56(1) no . . .
C(11) C(16b) C(15) 112(2) no . . .
C(11) C(16b) C(15a) 95(1) no . . .
C(11) C(16b) C(15b) 121(2) no . . .
C(12) C(13) C(14) 122(1) no . . .
C(13) C(14) C(15) 119(2) no . . .
C(13) C(14) C(15a) 108(1) no . . .
C(13) C(14) C(15b) 124(1) no . . .
C(14) C(15) C(16) 117(3) no . . .
C(14) C(15) C(16a) 112(2) no . . .
C(14) C(15) C(16b) 114(3) no . . .
C(14) C(15) C(15a) 76(8) no . . .
C(15a) C(14) C(15) 19(2) no . . .
C(14) C(15) C(15b) 74(7) no . . .
C(15b) C(14) C(15) 22(2) no . . .
C(14) C(15a) C(16) 125(2) no . . .
C(14) C(15a) C(16a) 129(2) no . . .
C(14) C(15a) C(16b) 110(2) no . . .
C(14) C(15a) C(15) 84(8) no . . .
C(14) C(15a) C(15b) 68(2) no . . .
C(15b) C(14) C(15a) 41(1) no . . .
C(14) C(15b) C(16) 103(2) no . . .
C(14) C(15b) C(16b) 111(1) no . . .
C(14) C(15b) C(15) 82(7) no . . .
C(14) C(15b) C(15a) 69(2) no . . .
C(15) C(16) C(16a) 106(13) no . . .
C(16a) C(15) C(16) 15(3) no . . .
C(15) C(16) C(16b) 70(7) no . . .
C(16b) C(15) C(16) 24(3) no . . .
C(15) C(16) C(15a) 19(2) no . . .
C(15a) C(15) C(16) 71(9) no . . .
C(15) C(16) C(15b) 16(2) no . . .
C(15b) C(15) C(16) 113(11) no . . .
C(15) C(16a) C(16) 57(11) no . . .
C(15) C(16a) C(16b) 56(3) no . . .
C(16b) C(15) C(16a) 40(2) no . . .
C(15) C(16a) C(15a) 16(2) no . . .
C(15a) C(15) C(16a) 56(9) no . . .
C(15b) C(15) C(16a) 127(10) no . . .
C(15) C(15a) C(16) 88(11) no . . .
C(15) C(15a) C(16a) 107(11) no . . .
C(15) C(15a) C(16b) 67(10) no . . .
C(16b) C(15) C(15a) 93(10) no . . .
C(15) C(15a) C(15b) 16(6) no . . .
C(15b) C(15) C(15a) 148(11) no . . .
C(15) C(16b) C(16) 84(8) no . . .
C(15) C(16b) C(16a) 83(4) no . . .
C(15) C(16b) C(15a) 18(2) no . . .
C(15) C(16b) C(15b) 21(2) no . . .
C(15b) C(15) C(16b) 88(9) no . . .
C(15) C(15b) C(16) 49(9) no . . .
C(15) C(15b) C(16b) 69(8) no . . .
C(15) C(15b) C(15a) 14(5) no . . .
C(16) C(15a) C(16b) 9(5) no . . .
C(16b) C(16) C(16a) 163(10) no . . .
C(16) C(15a) C(15a) 73(11) no . . .
C(15a) C(16) C(16a) 87(12) no . . .
C(15b) C(16) C(16a) 122(13) no . . .
C(16) C(15a) C(16a) 18(2) no . . .
C(16) C(15a) C(16b) 24(2) no . . .
C(16b) C(16) C(15a) 87(7) no . . .
C(16) C(15a) C(15b) 93(4) no . . .
C(15b) C(16) C(15a) 34(2) no . . .
C(16) C(16b) C(16a) 7(4) no . . .
C(16) C(16b) C(15a) 67(8) no . . .
C(16) C(16b) C(15b) 106(8) no . . .
C(15b) C(16) C(16b) 54(6) no . . .
C(16) C(15b) C(16b) 19(2) no . . .
C(16) C(15b) C(15a) 52(3) no . . .
C(22) C(17) C(18) 123(1) no . . .
C(17) C(18) C(17a) 34(1) no . . .
C(17a) C(17) C(18) 92(2) no . . .
C(17) C(18) C(19) 115(1) no . . .
C(17a) C(17) C(22) 110(2) no . . .
C(17) C(22) C(22a) 70(1) no . . .
C(17) C(22) C(21) 118(2) no . . .
C(17) C(17a) C(18) 52(2) no . . .
C(17) C(17a) C(22a) 104(2) no . . .
C(17a) C(18) C(19) 125(1) no . . .
C(18) C(19) C(20) 128(2) no . . .
C(18) C(19) C(20a) 106(1) no . . .
C(18) C(17a) C(22a) 117(1) no . . .
C(19) C(20) C(21) 113(2) no . . .
C(19) C(20) C(20a) 78(2) no . . .
C(20a) C(19) C(20) 41(1) no . . .
C(19) C(20a) C(20) 59(2) no . . .
C(19) C(20a) C(21) 96(1) no . . .
C(19) C(20a) C(21a) 130(2) no . . .
C(20) C(21) C(22) 119(2) no . . .
C(20) C(21) C(20a) 41(1) no . . .
C(20a) C(20) C(21) 76(3) no . . .
C(20) C(20a) C(21) 62(2) no . . .
C(20) C(20a) C(21a) 143(4) no . . .
C(21) C(22) C(22a) 106(1) no . . .
C(20a) C(21) C(22) 99(2) no . . .
C(21) C(20a) C(21a) 80(2) no . . .
C(22) C(22a) C(17a) 73(1) no . . .
C(22) C(22a) C(21a) 78(1) no . . .
C(28) C(23) C(24) 129(1) no . . .
C(23) C(24) C(23a) 26(1) no . . .
C(23a) C(23) C(24) 110(3) no . . .
C(28a) C(23) C(24) 133(1) no . . .
C(23) C(24) C(25) 115(1) no . . .
C(23) C(24) C(25a) 103(2) no . . .
C(23) C(28) C(23a) 23(1) no . . .
C(23a) C(23) C(28) 107(2) no . . .
C(23) C(28) C(28a) 70(1) no . . .
C(28a) C(23) C(28) 51(1) no . . .
C(23) C(28) C(27) 118(2) no . . .
C(23) C(28) C(27a) 102(2) no . . .
C(23) C(23a) C(24) 43(2) no . . .
C(23) C(23a) C(28) 48(2) no . . .
C(23) C(23a) C(28a) 92(2) no . . .
C(28a) C(23) C(23a) 58(1) no . . .
C(23) C(28a) C(28) 57(1) no . . .
C(23) C(28a) C(23a) 28(1) no . . .
C(23) C(28a) C(27a) 93(1) no . . .
C(23a) C(24) C(25) 134(1) no . . .
C(24) C(25) C(26) 114(2) no . . .
C(24) C(25) C(26a) 86(1) no . . .
C(24) C(25) C(25a) 29(2) no . . .
C(25a) C(24) C(25) 15(1) no . . .
C(24) C(23a) C(28) 86(1) no . . .
C(24) C(23a) C(28a) 117(1) no . . .
C(25a) C(24) C(23a) 120(1) no . . .
C(24) C(25a) C(25) 134(3) no . . .
C(24) C(25a) C(26) 142(2) no . . .
C(24) C(25a) C(26a) 122(2) no . . .
C(25) C(26) C(27) 120(1) no . . .
C(25) C(26) C(26a) 79(2) no . . .
C(26a) C(25) C(26) 42(1) no . . .
C(25) C(26) C(25a) 23(1) no . . .
C(25a) C(25) C(26) 91(4) no . . .
C(25) C(26a) C(26) 57(2) no . . .
C(25) C(26a) C(27) 108(1) no . . .
C(25) C(26a) C(27a) 140(1) no . . .
C(25) C(26a) C(25a) 21(1) no . . .
C(25a) C(25) C(26a) 56(2) no . . .
C(25) C(25a) C(26) 65(3) no . . .
C(25) C(25a) C(26a) 101(2) no . . .
C(26) C(27) C(28) 121(2) no . . .
C(26) C(27) C(27a) 106(2) no . . .
C(26) C(27) C(26a) 47(1) no . . .
C(26a) C(26) C(27) 64(2) no . . .
C(25a) C(26) C(27) 98(1) no . . .
C(26) C(26a) C(27) 67(2) no . . .
C(26) C(26a) C(27a) 133(3) no . . .
C(26) C(26a) C(25a) 74(1) no . . .
C(25a) C(26) C(26a) 60(1) no . . .
C(26) C(25a) C(26a) 44(1) no . . .
C(27) C(28) C(23a) 136(2) no . . .
C(27) C(28) C(28a) 132(1) no . . .
C(27) C(28) C(27a) 70(1) no . . .
C(27a) C(27) C(28) 54(1) no . . .
C(26a) C(27) C(28) 90(2) no . . .
C(27) C(27a) C(28) 55(1) no . . .
C(27) C(27a) C(28a) 113(1) no . . .
C(27) C(27a) C(26a) 55(1) no . . .
C(26a) C(27) C(27a) 58(1) no . . .
C(27) C(26a) C(27a) 66(2) no . . .
C(27) C(26a) C(25a) 107(1) no . . .
C(28) C(23a) C(28a) 46(1) no . . .
C(28a) C(28) C(23a) 48(1) no . . .
C(27a) C(28) C(23a) 94(1) no . . .
C(28) C(28a) C(23a) 85(1) no . . .
C(28) C(28a) C(27a) 58(1) no . . .
C(27a) C(28) C(28a) 61(1) no . . .
C(28) C(27a) C(28a) 59(1) no . . .
C(28) C(27a) C(26a) 89(1) no . . .
C(16a) C(15a) C(16b) 42(2) no . . .
C(16b) C(16a) C(15a) 71(3) no . . .
C(16a) C(15a) C(15b) 112(4) no . . .
C(16a) C(16b) C(15a) 66(3) no . . .
C(16a) C(16b) C(15b) 105(3) no . . .
C(15a) C(16b) C(15b) 39(1) no . . .
C(15b) C(15a) C(16b) 69(3) no . . .
C(15a) C(15b) C(16b) 71(3) no . . .
C(17a) C(22a) C(21a) 120(2) no . . .
C(22a) C(21a) C(20a) 118(2) no . . .
C(23a) C(28a) C(27a) 117(2) no . . .
C(28a) C(27a) C(26a) 121(2) no . . .
C(27a) C(26a) C(25a) 119(1) no . . .
C(1a) N(2) C(2a) 57(91) no . 55503 55503
C(2a) C(1a) N(2) 0.0(6) no 55503 . 55503
C(1a) N(2) Cu(3) 161.9(8) no . 55503 55503
C(1a) C(2a) N(2) 122(92) no . 55503 55503
C(1a) C(2a) Cu(3) 161.9(8) no . 55503 55503
C(2a) N(1) C(1a) 86(68) no . 55503 55503
C(1a) C(2a) N(1) 0.0(7) no 55503 . 55503
C(2a) N(1) Cu(2) 168.8(9) no . 55503 55503
C(2a) C(1a) N(1) 93(68) no . 55503 55503
C(2a) C(1a) Cu(2) 168.7(9) no . 55503 55503
C(3) C(4) H(1) 119.3 no . . .
C(3) C(8) H(5) 119.5 no . . .
H(1) C(4) C(5) 119.9 no . . .
C(4) C(5) H(2) 120.9 no . . .
H(2) C(5) C(6) 120.7 no . . .
C(5) C(6) H(3) 119.7 no . . .
C(6) C(7) H(4) 119.9 no . . .
H(3) C(6) C(7) 119.5 no . . .
C(7) C(8) H(5) 120.1 no . . .
H(4) C(7) C(8) 120.1 no . . .
C(9) C(10) H(6) 109.7 no . . .
C(9) C(10) H(7) 109.4 no . . .
C(9) C(10) H(8) 109.3 no . . .
H(7) C(10) H(6) 109.5 no . . .
H(8) C(10) H(6) 109.5 no . . .
H(8) C(10) H(7) 109.5 no . . .
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
W(1) Cu(1) 2.6395(9) yes . .
W(1) Cu(2) 2.6362(9) yes . .
W(1) Cu(3) 2.732(1) yes . .
W(1) S(1) 2.241(3) yes . .
W(1) S(2) 2.246(2) yes . .
W(1) S(3) 2.200(2) yes . .
W(1) S(4) 2.212(3) yes . .
Cu(1) S(1) 2.254(3) yes . .
Cu(1) S(4) 2.235(4) yes . .
Cu(1) N(1a) 1.878(7) yes . .
Cu(1) C(1) 1.879(7) yes . .
Cu(2) S(2) 2.250(2) yes . .
Cu(2) S(3) 2.243(2) yes . .
Cu(2) N(1) 1.881(4) yes . .
Cu(2) C(1a) 1.881(4) yes . .
Cu(3) S(1) 2.307(2) yes . .
Cu(3) S(2) 2.327(3) yes . .
Cu(3) N(2) 2.018(5) yes . .
Cu(3) N(2a) 1.958(6) yes . .
Cu(3) C(2) 1.959(6) yes . .
Cu(3) C(2a) 2.018(5) yes . .
P(1) C(3) 1.80(1) no . .
P(1) C(11) 1.80(2) no . .
P(1) C(17) 1.99(2) no . .
P(1) C(23) 2.11(2) no . .
P(1) C(33) 1.64(2) no . .
P(1) C(37) 1.54(2) no . .
N(1) N(2) 1.158(6) no . 55503
N(1) C(1a) 0.00(2) no . .
N(1) C(2a) 1.158(6) yes . 55503
N(2) N(1) 1.158(6) no . 55503
N(2) C(1a) 1.158(6) yes . 55503
N(2) C(2a) 0.00(1) no . .
N(3) C(9) 1.08(3) yes . .
N(1a) N(2a) 1.141(9) no . 55506
N(1a) C(1) 0.00(2) no . .
N(1a) C(2) 1.139(9) yes . 55506
N(2a) N(1a) 1.141(9) no . 54506
N(2a) C(1) 1.140(9) yes . 54506
N(2a) C(2) 0.00(1) no . .
C(1) N(2a) 1.140(9) yes . 55506
C(1) C(2) 1.139(9) no . 55506
C(2) N(1a) 1.139(9) no . 54506
C(2) C(1) 1.139(9) no . 54506
C(3) C(4) 1.39(1) no . .
C(3) C(8) 1.38(1) no . .
C(4) C(5) 1.38(2) no . .
C(5) C(6) 1.41(1) no . .
C(6) C(7) 1.36(1) no . .
C(7) C(8) 1.39(2) no . .
C(9) C(10) 1.41(3) no . .
C(11) P(1) 1.80(2) no . .
C(11) C(12) 1.39(2) no . .
C(11) C(16) 1.38(4) no . .
C(11) C(16a) 1.32(3) no . .
C(11) C(16b) 1.56(2) no . .
C(12) C(11) 1.39(2) no . .
C(12) C(13) 1.38(2) no . .
C(13) C(14) 1.41(1) no . .
C(14) C(15) 1.44(7) no . .
C(14) C(15a) 1.40(3) no . .
C(14) C(15b) 1.40(3) no . .
C(15) C(16) 1.5(1) no . .
C(15) C(16a) 1.66(7) no . .
C(15) C(15a) 0.48(6) no . .
C(15) C(16b) 1.39(9) no . .
C(15) C(15b) 0.55(6) no . .
C(16) C(11) 1.38(4) no . .
C(16) C(16a) 0.47(7) no . .
C(16) C(15a) 1.39(9) no . .
C(16) C(16b) 0.62(6) no . .
C(16) C(15b) 1.76(7) no . .
C(17) C(18) 1.25(3) no . .
C(17) C(22) 1.41(3) no . .
C(17) C(17a) 0.90(2) no . .
C(18) C(19) 1.39(2) no . .
C(18) C(17a) 1.58(3) no . .
C(19) C(20) 1.36(3) no . .
C(19) C(20a) 1.54(3) no . .
C(20) C(21) 1.40(5) no . .
C(20) C(20a) 1.04(3) no . .
C(21) C(22) 1.41(3) no . .
C(21) C(20a) 1.54(5) no . .
C(22) C(22a) 1.77(3) no . .
C(23) C(24) 1.19(3) no . .
C(23) C(28) 1.45(3) no . .
C(23) C(23a) 0.77(2) no . .
C(23) C(28a) 1.61(3) no . .
C(24) C(25) 1.68(3) no . .
C(24) C(23a) 1.63(3) no . .
C(24) C(25a) 1.18(2) no . .
C(25) C(26) 1.44(4) no . .
C(25) C(26a) 1.67(4) no . .
C(25) C(25a) 0.62(3) no . .
C(26) C(27) 1.42(4) no . .
C(26) C(26a) 1.14(3) no . .
C(26) C(25a) 1.58(3) no . .
C(27) C(28) 1.35(3) no . .
C(27) C(27a) 1.56(3) no . .
C(27) C(26a) 1.40(4) no . .
C(28) C(23a) 1.84(3) no . .
C(28) C(28a) 1.34(2) no . .
C(28) C(27a) 1.34(3) no . .
C(16a) C(11) 1.32(3) no . .
C(16a) C(15a) 1.45(6) no . .
C(16a) C(16b) 1.07(4) no . .
C(15a) C(16b) 1.50(5) no . .
C(15a) C(15b) 1.00(4) no . .
C(16b) C(11) 1.56(2) no . .
C(16b) C(15b) 1.48(5) no . .
C(17a) C(22a) 1.42(3) no . .
C(22a) C(21a) 1.39(3) no . .
C(21a) C(20a) 1.38(5) no . .
C(23a) C(28a) 1.38(3) no . .
C(28a) C(27a) 1.38(3) no . .
C(27a) C(26a) 1.45(4) no . .
C(26a) C(25a) 1.42(3) no . .
C(1a) N(2) 1.158(6) no . 55503
C(1a) C(2a) 1.158(6) no . 55503
C(2a) N(1) 1.158(6) no . 55503
C(2a) C(1a) 1.158(6) no . 55503
C(4) H(1) 0.95 no . .
C(5) H(2) 0.95 no . .
C(6) H(3) 0.95 no . .
C(7) H(4) 0.95 no . .
C(8) H(5) 0.95 no . .
C(10) H(6) 0.95 no . .
C(10) H(7) 0.95 no . .
C(10) H(8) 0.95 no . .
|
1100968.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100968.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_1100968
loop_
_publ_author_name
'Corrado Di Nicola'
'Agustin Galindo'
'John V. Hanna'
'Fabio Marchetti'
'Claudio Pettinari'
'Riccardo Pettinari'
'Eleonora Rivarola'
'Brian W. Skelton'
'Allan H. White'
_publ_contact_author_address
;
Department of Chemistry
University of Western Australia
35 Stirling Highway
Crawley
Western Australia 6009
Australia
;
_publ_contact_author_email bws@crystal.uwa.edu.au
_publ_contact_author_fax (+61)_08_9380_1118
_publ_contact_author_name 'Skelton, B. W.'
_publ_contact_author_phone (+61)_08-9380_3481
_publ_section_title
;
Synthesis and Spectroscopic and X-ray Structural Characterization of
R2SnIV-Oxydiacetate and -Iminodiacetate Complexes
;
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3094
_journal_page_last 3102
_journal_paper_doi 10.1021/ic048240t
_journal_volume 44
_journal_year 2005
_chemical_formula_moiety 'C12 H24 O12 Sn2'
_chemical_formula_sum 'C12 H24 O12 Sn2'
_chemical_formula_weight 597.73
_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'
_cell_angle_alpha 90.00000
_cell_angle_beta 125.015(2)
_cell_angle_gamma 90.00000
_cell_formula_units_Z 4
_cell_length_a 22.608(2)
_cell_length_b 6.6669(7)
_cell_length_c 15.527(2)
_cell_measurement_reflns_used 6427
_cell_measurement_temperature 150(2)
_cell_measurement_theta_max 35.5
_cell_measurement_theta_min 2.4
_cell_volume 1916.7(4)
_computing_cell_refinement 'Siemens SAINT (Siemens, 1995)'
_computing_data_collection 'Siemens SMART (Siemens, 1995)'
_computing_data_reduction 'xtal ADDREF SORTRF'
_computing_molecular_graphics xtal
_computing_publication_material 'xtal BONDLA CIFIO'
_computing_structure_refinement 'xtal CRYLSQ'
_computing_structure_solution xtal
_diffrn_ambient_temperature 150(2)
_diffrn_measured_fraction_theta_full 1.0
_diffrn_measured_fraction_theta_max 1.0
_diffrn_measurement_device_type
;
Bruker SMART CCD diffractometer
;
_diffrn_measurement_method '\w scans'
_diffrn_radiation_detector 'CCD area detector'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'sealed tube'
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength .71073
_diffrn_reflns_av_R_equivalents .028
_diffrn_reflns_av_sigmaI/netI .014
_diffrn_reflns_limit_h_max 31
_diffrn_reflns_limit_h_min -38
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 26
_diffrn_reflns_limit_l_min -26
_diffrn_reflns_number 19338
_diffrn_reflns_theta_full 37.49
_diffrn_reflns_theta_max 37.49
_diffrn_reflns_theta_min 2.2
_diffrn_standards_decay_% 0
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 2.663
_exptl_absorpt_correction_T_max .83
_exptl_absorpt_correction_T_min .64
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS; Sheldrick, 1996
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 2.071
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 1168
_exptl_crystal_size_max .4
_exptl_crystal_size_mid .35
_exptl_crystal_size_min .32
_refine_diff_density_max .766
_refine_diff_density_min -2.02
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_all 1.101
_refine_ls_goodness_of_fit_ref 1.105
_refine_ls_hydrogen_treatment noref
_refine_ls_matrix_type full
_refine_ls_number_constraints 0
_refine_ls_number_parameters 118
_refine_ls_number_reflns 4646
_refine_ls_number_restraints 0
_refine_ls_R_factor_all .027
_refine_ls_R_factor_gt .024
_refine_ls_shift/su_max .004
_refine_ls_shift/su_mean .001
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_all .045
_refine_ls_wR_factor_ref .043
_reflns_d_resolution_high .584
_reflns_d_resolution_low 9.241
_reflns_Friedel_coverage 0
_reflns_limit_h_max 38
_reflns_limit_h_min 0
_reflns_limit_k_max 11
_reflns_limit_k_min 0
_reflns_limit_l_max 21
_reflns_limit_l_min -26
_reflns_number_gt 4646
_reflns_number_total 5001
_reflns_threshold_expression 'F > 4.00 sig(F )'
_cod_data_source_file ic048240tsi20041215_025357_1.cif
_cod_data_source_block cp2b
_cod_original_sg_symbol_Hall -c_2yc
_cod_database_code 1100968
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_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn .358670(5) .311521(15) .568428(7) .01136(5) Uani ? ? 1.00000 ? ?
O1 .37361(6) .1362(2) .45030(9) .0167(4) Uani ? ? 1.00000 ? ?
C11 .31596(8) .0461(2) .35473(11) .0140(4) Uani ? ? 1.00000 ? ?
C12 .24862(8) .0373(2) .35375(11) .0136(4) Uani ? ? 1.00000 ? ?
O11 .24780(6) .1359(2) .42363(9) .0151(4) Uani ? ? 1.00000 ? ?
O12 .19784(7) -.0643(2) .28205(11) .0220(5) Uani ? ? 1.00000 ? ?
C21 .43210(9) .2052(2) .44676(13) .0154(5) Uani ? ? 1.00000 ? ?
C22 .49053(9) .2871(2) .55435(13) .0141(5) Uani ? ? 1.00000 ? ?
O21 .47060(7) .3334(2) .61534(10) .0166(4) Uani ? ? 1.00000 ? ?
O22 .55192(7) .3067(2) .57805(12) .0201(5) Uani ? ? 1.00000 ? ?
C01 .32200(9) .5642(3) .46952(13) .0183(5) Uani ? ? 1.00000 ? ?
C02 .37926(10) .0502(3) .65756(14) .0196(5) Uani ? ? 1.00000 ? ?
O03 .41201(6) .5082(2) .70906(9) .0160(4) Uani ? ? 1.00000 ? ?
H11a .32955 -.08563 .34956 .01900 Uiso ? ? 1.00000 ? ?
H12b .30660 .12413 .29689 .01900 Uiso ? ? 1.00000 ? ?
H21a .41580 .30809 .39560 .02100 Uiso ? ? 1.00000 ? ?
H21b .45088 .09702 .42936 .02100 Uiso ? ? 1.00000 ? ?
H01a .36186 .64807 .48870 .02800 Uiso ? ? 1.00000 ? ?
H01b .28880 .63763 .47634 .02800 Uiso ? ? 1.00000 ? ?
H01c .29866 .52261 .39854 .02800 Uiso ? ? 1.00000 ? ?
H02a .35315 -.05872 .61148 .03000 Uiso ? ? 1.00000 ? ?
H02b .36376 .07051 .70246 .03000 Uiso ? ? 1.00000 ? ?
H02c .42956 .02172 .69913 .03000 Uiso ? ? 1.00000 ? ?
H03a .44899 .44762 .76462 .02400 Uiso ? ? 1.00000 ? ?
H03b .38309 .53247 .72230 .02400 Uiso ? ? 1.00000 ? ?
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
Sn .01047(6) .01353(6) .00862(6) -.00043(2) .00463(4) -.00014(2)
O1 .0140(4) .0236(5) .0133(4) -.0049(4) .0084(4) -.0049(4)
C11 .0142(5) .0163(6) .0108(5) -.0013(4) .0068(4) -.0022(4)
C12 .0126(5) .0143(6) .0115(5) .0002(4) .0056(4) -.0020(4)
O11 .0156(4) .0184(5) .0118(4) -.0024(4) .0082(4) -.0045(4)
O12 .0144(5) .0287(6) .0200(5) -.0047(4) .0081(4) -.0133(5)
C21 .0145(6) .0206(7) .0132(6) -.0010(5) .0091(5) -.0012(4)
C22 .0127(5) .0156(6) .0138(6) .0007(4) .0075(5) .0005(4)
O21 .0118(4) .0248(6) .0124(5) -.0019(4) .0065(4) -.0033(4)
O22 .0124(5) .0270(7) .0221(6) -.0033(4) .0106(5) -.0030(4)
C01 .0176(6) .0188(6) .0156(6) .0010(5) .0078(5) .0048(5)
C02 .0199(6) .0192(7) .0172(6) .0012(5) .0091(5) .0041(5)
O03 .0126(4) .0206(5) .0124(4) -.0002(4) .0058(4) -.0027(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C ? 0 48 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1'
H ? 0 96 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1'
O ? 0 48 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1'
Sn ? 0 8 -.873 1.424 'Int Tables Vol IV Tables 2.2B and 2.3.1'
loop_
_diffrn_attenuator_code
_diffrn_attenuator_scale
? ?
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 Sn O11 . . . 65.49(5) ?
O1 Sn O21 . . . 68.86(5) ?
O1 Sn C01 . . . 90.07(7) ?
O1 Sn C02 . . . 91.43(7) ?
O1 Sn O03 . . . 145.03(5) ?
O1 Sn O11 . . '7 556' 132.74(4) ?
O11 Sn O21 . . . 134.31(6) ?
O11 Sn C01 . . . 86.94(5) ?
O11 Sn C02 . . . 86.16(5) ?
O11 Sn O03 . . . 149.43(6) ?
O11 Sn O11 . . '7 556' 67.27(5) ?
O21 Sn C01 . . . 94.89(7) ?
O21 Sn C02 . . . 93.37(7) ?
O21 Sn O03 . . . 76.26(6) ?
O21 Sn O11 . . '7 556' 158.40(5) ?
C01 Sn C02 . . . 171.59(7) ?
C01 Sn O03 . . . 90.53(6) ?
C01 Sn O11 . . '7 556' 86.37(7) ?
C02 Sn O03 . . . 92.97(6) ?
C02 Sn O11 . . '7 556' 86.54(7) ?
O03 Sn O11 . . '7 556' 82.17(5) ?
Sn O1 C11 . . . 124.33(13) ?
Sn O1 C21 . . . 114.77(10) ?
C11 O1 C21 . . . 114.06(16) ?
O1 C11 C12 . . . 109.83(16) ?
O1 C11 H11a . . . 109.28 ?
O1 C11 H12b . . . 109.09 ?
C12 C11 H11a . . . 109.60 ?
C12 C11 H12b . . . 109.51 ?
H11a C11 H12b . . . 109.5 ?
C11 C12 O11 . . . 118.41(12) ?
C11 C12 O12 . . . 115.84(18) ?
O11 C12 O12 . . . 125.7(2) ?
Sn O11 C12 . . . 120.62(12) ?
Sn O11 Sn . . '7 556' 112.73(6) ?
C12 O11 Sn . . '7 556' 126.61(10) ?
O1 C21 C22 . . . 108.27(18) ?
O1 C21 H21a . . . 109.93 ?
O1 C21 H21b . . . 109.90 ?
C22 C21 H21a . . . 109.62 ?
C22 C21 H21b . . . 109.70 ?
H21a C21 H21b . . . 109.4 ?
C21 C22 O21 . . . 116.20(17) ?
C21 C22 O22 . . . 119.4(2) ?
O21 C22 O22 . . . 124.39(15) ?
Sn O21 C22 . . . 123.88(9) ?
Sn C01 H01a . . . 109.67 ?
Sn C01 H01b . . . 109.66 ?
Sn C01 H01c . . . 109.72 ?
H01a C01 H01b . . . 109.17 ?
H01a C01 H01c . . . 109.3 ?
H01b C01 H01c . . . 109.30 ?
Sn C02 H02a . . . 109.28 ?
Sn C02 H02b . . . 109.18 ?
Sn C02 H02c . . . 109.83 ?
H02a C02 H02b . . . 109.2 ?
H02a C02 H02c . . . 110.0 ?
H02b C02 H02c . . . 109.30 ?
Sn O03 H03a . . . 111.51 ?
Sn O03 H03b . . . 107.88 ?
H03a O03 H03b . . . 107.13 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Sn O1 . . 2.3570(17) ?
Sn O11 . . 2.4982(11) ?
Sn O21 . . 2.2000(16) ?
Sn C01 . . 2.1029(18) ?
Sn C02 . . 2.104(2) ?
Sn O03 . . 2.2182(13) ?
Sn O11 . '7 556' 2.5046(17) ?
O1 C11 . . 1.4290(16) ?
O1 C21 . . 1.430(3) ?
C11 C12 . . 1.515(3) ?
C11 H11a . . .9491 ?
C11 H12b . . .9505 ?
C12 O11 . . 1.278(2) ?
C12 O12 . . 1.2449(17) ?
C21 C22 . . 1.517(2) ?
C21 H21a . . .9495 ?
C21 H21b . . .951 ?
C22 O21 . . 1.298(3) ?
C22 O22 . . 1.222(3) ?
C01 H01a . . .952 ?
C01 H01b . . .952 ?
C01 H01c . . .9499 ?
C02 H02a . . .9505 ?
C02 H02b . . .953 ?
C02 H02c . . .9506 ?
O03 H03a . . .8824 ?
O03 H03b . . .8064 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
? ? ? ? ? ? ? ? ? ? ?
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
? ? ? ? ? ? ? ? ? ?
|
1100969.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100969.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_1100969
loop_
_publ_author_name
'Corrado Di Nicola'
'Agustin Galindo'
'John V. Hanna'
'Fabio Marchetti'
'Claudio Pettinari'
'Riccardo Pettinari'
'Eleonora Rivarola'
'Brian W. Skelton'
'Allan H. White'
_publ_contact_author_address
;
Department of Chemistry
University of Western Australia
35 Stirling Highway
Crawley
Western Australia 6009
Australia
;
_publ_contact_author_email bws@crystal.uwa.edu.au
_publ_contact_author_fax (+61)_08_9380_1118
_publ_contact_author_name 'Skelton, B. W.'
_publ_contact_author_phone (+61)_08-9380_3481
_publ_section_title
;
Synthesis and Spectroscopic and X-ray Structural Characterization of
R2SnIV-Oxydiacetate and -Iminodiacetate Complexes
;
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3094
_journal_page_last 3102
_journal_paper_doi 10.1021/ic048240t
_journal_volume 44
_journal_year 2005
_chemical_formula_moiety 'C12 H28 Cl2 O7 Sn2'
_chemical_formula_sum 'C12 H28 Cl2 O7 Sn2'
_chemical_formula_weight 592.68
_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'
_cell_angle_alpha 90.00000
_cell_angle_beta 98.296(4)
_cell_angle_gamma 90.00000
_cell_formula_units_Z 4
_cell_length_a 8.1370(10)
_cell_length_b 17.648(3)
_cell_length_c 14.085(2)
_cell_measurement_reflns_used 8192
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 27.1
_cell_measurement_theta_min 1.9
_cell_volume 2001.5(5)
_computing_cell_refinement 'Siemens SAINT (Siemens, 1995)'
_computing_data_collection 'Siemens SMART (Siemens, 1995)'
_computing_data_reduction 'xtal ADDREF SORTRF'
_computing_molecular_graphics xtal
_computing_publication_material 'xtal BONDLA CIFIO'
_computing_structure_refinement 'xtal CRYLSQ'
_computing_structure_solution xtal
_diffrn_ambient_temperature 293(2)
_diffrn_measured_fraction_theta_full 1.0
_diffrn_measured_fraction_theta_max 1.0
_diffrn_measurement_device_type
;
Bruker SMART CCD diffractometer
;
_diffrn_measurement_method '\w scans'
_diffrn_radiation_detector 'CCD area detector'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'sealed tube'
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength .71073
_diffrn_reflns_av_R_equivalents .068
_diffrn_reflns_av_sigmaI/netI .035
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 22
_diffrn_reflns_limit_k_min -22
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_number 40395
_diffrn_reflns_theta_full 27.5
_diffrn_reflns_theta_max 27.5
_diffrn_reflns_theta_min 1.86
_diffrn_standards_decay_% 0
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 2.79
_exptl_absorpt_correction_T_max .73
_exptl_absorpt_correction_T_min .45
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS; Sheldrick, 1996
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.967
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 1160
_exptl_crystal_size_max .32
_exptl_crystal_size_mid .18
_exptl_crystal_size_min .1
_refine_diff_density_max 5.645
_refine_diff_density_min -2.62
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_all 1.151
_refine_ls_goodness_of_fit_ref 1.16
_refine_ls_hydrogen_treatment noref
_refine_ls_matrix_type atomblock
_refine_ls_number_constraints 0
_refine_ls_number_parameters 204
_refine_ls_number_reflns 3905
_refine_ls_number_restraints 0
_refine_ls_R_factor_all .07
_refine_ls_R_factor_gt .058
_refine_ls_shift/su_max .017
_refine_ls_shift/su_mean .002
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_all .097
_refine_ls_wR_factor_ref .09
_reflns_d_resolution_high .769
_reflns_d_resolution_low 10.914
_reflns_Friedel_coverage 0
_reflns_limit_h_max 10
_reflns_limit_h_min 0
_reflns_limit_k_max 22
_reflns_limit_k_min 0
_reflns_limit_l_max 18
_reflns_limit_l_min -18
_reflns_number_gt 3905
_reflns_number_total 4613
_reflns_threshold_expression 'F > 4.00 sig(F )'
_cod_data_source_file ic048240tsi20041215_025357_2.cif
_cod_data_source_block cpc4am
_cod_original_sg_symbol_Hall -p_2yn
_cod_database_code 1100969
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
1/2-x,1/2+y,1/2-z
-x,-y,-z
1/2+x,1/2-y,1/2+z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn1 .34295(5) .20721(2) .52048(3) .0142(2) Uani ? ? 1.00000 ? ?
Sn2 .14374(5) .44740(2) .69491(3) .0152(3) Uani ? ? 1.00000 ? ?
Cl1 .3051(2) .06631(9) .51978(12) .0222(8) Uani ? ? 1.00000 ? ?
Cl2 .1015(2) .58414(9) .67710(12) .0219(7) Uani ? ? 1.00000 ? ?
O1 .4429(7) .3174(3) .4297(3) .024(2) Uani ? ? 1.00000 ? ?
C11 .3935(9) .3932(4) .4447(5) .020(3) Uani ? ? 1.00000 ? ?
C12 .3205(8) .3944(4) .5379(5) .017(3) Uani ? ? 1.00000 ? ?
O11 .2982(6) .3348(3) .5802(3) .019(2) Uani ? ? 1.00000 ? ?
O12 .2802(6) .4593(3) .5654(3) .017(2) Uani ? ? 1.00000 ? ?
C21 .5186(9) .3042(4) .3470(5) .0214(14) Uiso ? ? 1.00000 ? ?
C22 .5328(8) .2200(4) .3316(5) .020(3) Uani ? ? 1.00000 ? ?
O21 .4690(6) .1763(3) .3869(3) .022(2) Uani ? ? 1.00000 ? ?
O22 .6040(7) .1989(3) .2643(3) .021(2) Uani ? ? 1.00000 ? ?
O01 .2260(7) .1947(3) .6574(4) .025(2) Uani ? ? 1.00000 ? ?
O02 .0026(7) .4645(3) .8212(3) .024(2) Uani ? ? 1.00000 ? ?
C011 .5816(9) .2139(4) .6024(5) .024(3) Uani ? ? 1.00000 ? ?
C012 .6739(11) .1405(5) .6202(7) .040(5) Uani ? ? 1.00000 ? ?
C021 .1152(11) .2243(5) .4316(7) .036(4) Uani ? ? 1.00000 ? ?
C022 -.0425(13) .2063(6) .4726(9) .053(6) Uani ? ? 1.00000 ? ?
C031 .3754(9) .4359(5) .7861(5) .028(4) Uani ? ? 1.00000 ? ?
C032 .4820(9) .5045(4) .7964(5) .026(3) Uani ? ? 1.00000 ? ?
C041 -.0685(9) .4096(4) .6042(5) .024(3) Uani ? ? 1.00000 ? ?
C042 -.2293(10) .4069(5) .6472(7) .035(4) Uani ? ? 1.00000 ? ?
H11a .31269 .41057 .39282 .02500 Uiso ? ? 1.00000 ? ?
H11b .48689 .42710 .44960 .02500 Uiso ? ? 1.00000 ? ?
H21a .62349 .32725 .35301 .03400 Uiso ? ? 1.00000 ? ?
H21b .44896 .32610 .29181 .03400 Uiso ? ? 1.00000 ? ?
H011a .64632 .24751 .56884 .03000 Uiso ? ? 1.00000 ? ?
H011b .56878 .23668 .66229 .03000 Uiso ? ? 1.00000 ? ?
H012a .78000 .14850 .65775 .05900 Uiso ? ? 1.00000 ? ?
H012b .68981 .11697 .56127 .05900 Uiso ? ? 1.00000 ? ?
H012c .61228 .10614 .65472 .05900 Uiso ? ? 1.00000 ? ?
H021a .11496 .19444 .37622 .04400 Uiso ? ? 1.00000 ? ?
H021b .11000 .27686 .41401 .04400 Uiso ? ? 1.00000 ? ?
H022a -.13604 .21429 .42365 .07800 Uiso ? ? 1.00000 ? ?
H022b -.05258 .23993 .52453 .07800 Uiso ? ? 1.00000 ? ?
H022c -.04052 .15603 .49342 .07800 Uiso ? ? 1.00000 ? ?
H031a .35431 .42054 .84789 .03600 Uiso ? ? 1.00000 ? ?
H031b .43711 .39587 .76026 .03600 Uiso ? ? 1.00000 ? ?
H032a .58303 .49342 .83840 .03900 Uiso ? ? 1.00000 ? ?
H032b .42535 .54393 .82359 .03900 Uiso ? ? 1.00000 ? ?
H032c .50816 .51925 .73596 .03900 Uiso ? ? 1.00000 ? ?
H041a -.04666 .35962 .58367 .03000 Uiso ? ? 1.00000 ? ?
H041b -.08563 .44223 .55008 .03000 Uiso ? ? 1.00000 ? ?
H042a -.31900 .39185 .60070 .05300 Uiso ? ? 1.00000 ? ?
H042b -.25264 .45594 .67137 .05300 Uiso ? ? 1.00000 ? ?
H042c -.21879 .37185 .69972 .05300 Uiso ? ? 1.00000 ? ?
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
Sn1 .0158(3) .0174(3) .0113(3) .00079(15) .00868(17) .00056(14)
Sn2 .0180(3) .0176(3) .0114(3) -.00075(15) .00734(17) -.00045(14)
Cl1 .0314(9) .0166(7) .0211(8) -.0012(6) .0127(7) .0010(6)
Cl2 .0312(9) .0178(8) .0193(8) .0007(6) .0126(7) .0000(6)
O1 .042(3) .015(2) .021(3) .005(2) .023(2) .0004(18)
C11 .032(4) .013(3) .018(3) .002(3) .016(3) -.002(2)
C12 .017(3) .021(3) .015(3) -.000(2) .004(2) .002(2)
O11 .022(2) .018(2) .020(2) .0018(18) .014(2) .0013(18)
O12 .020(2) .023(2) .012(2) .0017(18) .0086(17) -.0011(17)
C22 .017(3) .016(3) .030(4) .001(2) .014(3) -.000(3)
O21 .031(3) .025(3) .014(2) .002(2) .017(2) -.0007(18)
O22 .030(3) .025(3) .011(2) -.001(2) .012(2) -.0028(17)
O01 .035(3) .025(3) .019(3) .005(2) .022(2) .0064(19)
O02 .039(3) .020(2) .017(2) -.004(2) .021(2) -.0022(18)
C011 .022(4) .026(4) .022(4) -.002(3) -.004(3) -.007(3)
C012 .027(4) .050(5) .040(5) .005(4) -.000(4) .006(4)
C021 .034(5) .028(4) .045(5) -.001(3) .009(4) -.002(3)
C022 .035(5) .063(7) .062(7) -.006(4) .014(5) -.029(5)
C031 .023(4) .043(5) .016(3) -.008(3) -.005(3) .010(3)
C032 .021(3) .034(4) .023(4) -.003(3) .004(3) -.001(3)
C041 .023(4) .029(4) .021(3) -.002(3) .003(3) -.002(3)
C042 .021(4) .042(5) .041(5) -.001(3) .003(3) .002(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C ? 0 48 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1'
H ? 0 112 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1'
Cl ? 0 8 .132 .159 'Int Tables Vol IV Tables 2.2B and 2.3.1'
O ? 0 28 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1'
Sn ? 0 8 -.873 1.424 'Int Tables Vol IV Tables 2.2B and 2.3.1'
loop_
_diffrn_attenuator_code
_diffrn_attenuator_scale
? ?
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl1 Sn1 O1 . . . 144.14(12) ?
Cl1 Sn1 O11 . . . 152.81(13) ?
Cl1 Sn1 O21 . . . 80.37(13) ?
Cl1 Sn1 O01 . . . 80.88(13) ?
Cl1 Sn1 C011 . . . 99.2(2) ?
Cl1 Sn1 C021 . . . 92.5(2) ?
O1 Sn1 O11 . . . 62.68(16) ?
O1 Sn1 O21 . . . 63.93(17) ?
O1 Sn1 O01 . . . 134.97(17) ?
O1 Sn1 C011 . . . 84.0(2) ?
O1 Sn1 C021 . . . 84.7(3) ?
O11 Sn1 O21 . . . 126.62(17) ?
O11 Sn1 O01 . . . 72.39(17) ?
O11 Sn1 C011 . . . 86.1(2) ?
O11 Sn1 C021 . . . 84.9(3) ?
O21 Sn1 O01 . . . 160.82(17) ?
O21 Sn1 C011 . . . 88.7(2) ?
O21 Sn1 C021 . . . 90.3(3) ?
O01 Sn1 C011 . . . 90.4(3) ?
O01 Sn1 C021 . . . 94.5(3) ?
C011 Sn1 C021 . . . 167.9(3) ?
Cl2 Sn2 C12 . . . 108.16(13) ?
Cl2 Sn2 O11 . . . 132.26(10) ?
Cl2 Sn2 O12 . . . 84.50(12) ?
Cl2 Sn2 O02 . . . 82.52(13) ?
Cl2 Sn2 C031 . . . 104.8(2) ?
Cl2 Sn2 C041 . . . 99.2(2) ?
Cl2 Sn2 O22 . . '4 455' 157.75(12) ?
C12 Sn2 O11 . . . 24.12(16) ?
C12 Sn2 O12 . . . 23.78(17) ?
C12 Sn2 O02 . . . 169.19(18) ?
C12 Sn2 C031 . . . 86.4(2) ?
C12 Sn2 C041 . . . 83.7(2) ?
C12 Sn2 O22 . . '4 455' 93.58(17) ?
O11 Sn2 O12 . . . 47.87(15) ?
O11 Sn2 O02 . . . 145.13(15) ?
O11 Sn2 C031 . . . 81.7(2) ?
O11 Sn2 C041 . . . 80.3(2) ?
O11 Sn2 O22 . . '4 455' 69.49(14) ?
O12 Sn2 O02 . . . 167.00(17) ?
O12 Sn2 C031 . . . 90.0(2) ?
O12 Sn2 C041 . . . 89.7(2) ?
O12 Sn2 O22 . . '4 455' 117.36(16) ?
O02 Sn2 C031 . . . 92.5(2) ?
O02 Sn2 C041 . . . 93.1(2) ?
O02 Sn2 O22 . . '4 455' 75.64(16) ?
C031 Sn2 C041 . . . 155.9(3) ?
C031 Sn2 O22 . . '4 455' 80.7(2) ?
C041 Sn2 O22 . . '4 455' 78.1(2) ?
Sn1 O1 C11 . . . 122.0(4) ?
Sn1 O1 C21 . . . 120.1(4) ?
C11 O1 C21 . . . 116.3(5) ?
O1 C11 C12 . . . 107.3(5) ?
O1 C11 H11a . . . 111.4 ?
O1 C11 H11b . . . 111.1 ?
C12 C11 H11a . . . 110.1 ?
C12 C11 H11b . . . 109.5 ?
H11a C11 H11b . . . 107.6 ?
Sn2 C12 C11 . . . 160.9(4) ?
Sn2 C12 O11 . . . 77.7(4) ?
Sn2 C12 O12 . . . 46.5(3) ?
C11 C12 O11 . . . 120.6(6) ?
C11 C12 O12 . . . 115.3(6) ?
O11 C12 O12 . . . 124.1(6) ?
Sn1 O11 Sn2 . . . 154.5(2) ?
Sn1 O11 C12 . . . 125.3(4) ?
Sn2 O11 C12 . . . 78.2(4) ?
Sn2 O12 C12 . . . 109.8(4) ?
O1 C21 C22 . . . 109.3(6) ?
O1 C21 H21a . . . 110.7 ?
O1 C21 H21b . . . 108.7 ?
C22 C21 H21a . . . 110.6 ?
C22 C21 H21b . . . 108.9 ?
H21a C21 H21b . . . 108.6 ?
C21 C22 O21 . . . 117.9(7) ?
C21 C22 O22 . . . 117.4(6) ?
O21 C22 O22 . . . 124.8(6) ?
Sn1 O21 C22 . . . 128.6(4) ?
C22 O22 Sn2 . . '4 554' 129.5(4) ?
Sn1 C011 C012 . . . 116.2(5) ?
Sn1 C011 H011a . . . 107.0 ?
Sn1 C011 H011b . . . 107.3 ?
C012 C011 H011a . . . 108.5 ?
C012 C011 H011b . . . 109.3 ?
H011a C011 H011b . . . 108.2 ?
C011 C012 H012a . . . 110.8 ?
C011 C012 H012b . . . 110.9 ?
C011 C012 H012c . . . 110.1 ?
H012a C012 H012b . . . 108.8 ?
H012a C012 H012c . . . 108.0 ?
H012b C012 H012c . . . 108.2 ?
Sn1 C021 C022 . . . 117.7(7) ?
Sn1 C021 H021a . . . 108.0 ?
Sn1 C021 H021b . . . 107.2 ?
C022 C021 H021a . . . 107.3 ?
C022 C021 H021b . . . 107.1 ?
H021a C021 H021b . . . 109.4 ?
C021 C022 H022a . . . 108.9 ?
C021 C022 H022b . . . 109.4 ?
C021 C022 H022c . . . 110.1 ?
H022a C022 H022b . . . 108.1 ?
H022a C022 H022c . . . 110.0 ?
H022b C022 H022c . . . 110.4 ?
Sn2 C031 C032 . . . 115.8(5) ?
Sn2 C031 H031a . . . 108.5 ?
Sn2 C031 H031b . . . 107.7 ?
C032 C031 H031a . . . 108.9 ?
C032 C031 H031b . . . 107.7 ?
H031a C031 H031b . . . 108.0 ?
C031 C032 H032a . . . 109.3 ?
C031 C032 H032b . . . 109.2 ?
C031 C032 H032c . . . 110.0 ?
H032a C032 H032b . . . 108.9 ?
H032a C032 H032c . . . 109.1 ?
H032b C032 H032c . . . 110.4 ?
Sn2 C041 C042 . . . 116.5(5) ?
Sn2 C041 H041a . . . 107.7 ?
Sn2 C041 H041b . . . 108.0 ?
C042 C041 H041a . . . 107.5 ?
C042 C041 H041b . . . 107.7 ?
H041a C041 H041b . . . 109.3 ?
C041 C042 H042a . . . 110.8 ?
C041 C042 H042b . . . 109.8 ?
C041 C042 H042c . . . 110.0 ?
H042a C042 H042b . . . 109.0 ?
H042a C042 H042c . . . 109.1 ?
H042b C042 H042c . . . 108.0 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Sn1 Cl1 . . 2.5053(17) ?
Sn1 O1 . . 2.525(5) ?
Sn1 O11 . . 2.450(5) ?
Sn1 O21 . . 2.333(5) ?
Sn1 O01 . . 2.281(6) ?
Sn1 C011 . . 2.114(7) ?
Sn1 C021 . . 2.103(8) ?
Sn2 Cl2 . . 2.4455(17) ?
Sn2 C12 . . 2.958(7) ?
Sn2 O11 . . 2.953(5) ?
Sn2 O12 . . 2.278(5) ?
Sn2 O02 . . 2.272(5) ?
Sn2 C031 . . 2.132(7) ?
Sn2 C041 . . 2.103(7) ?
Sn2 O22 . '4 455' 2.797(5) ?
O1 C11 . . 1.421(8) ?
O1 C21 . . 1.413(9) ?
C11 C12 . . 1.517(10) ?
C11 H11a . . .961 ?
C11 H11b . . .962 ?
C12 O11 . . 1.235(8) ?
C12 O12 . . 1.267(8) ?
C21 C22 . . 1.509(9) ?
C21 H21a . . .938 ?
C21 H21b . . .973 ?
C22 O21 . . 1.260(9) ?
C22 O22 . . 1.237(9) ?
C011 C012 . . 1.502(12) ?
C011 H011a . . .961 ?
C011 H011b . . .954 ?
C012 H012a . . .955 ?
C012 H012b . . .953 ?
C012 H012c . . .962 ?
C021 C022 . . 1.515(15) ?
C021 H021a . . .942 ?
C021 H021b . . .959 ?
C022 H022a . . .961 ?
C022 H022b . . .955 ?
C022 H022c . . .933 ?
C031 C032 . . 1.484(11) ?
C031 H031a . . .951 ?
C031 H031b . . .967 ?
C032 H032a . . .962 ?
C032 H032b . . .946 ?
C032 H032c . . .943 ?
C041 C042 . . 1.520(12) ?
C041 H041a . . .954 ?
C041 H041b . . .949 ?
C042 H042a . . .946 ?
C042 H042b . . .959 ?
C042 H042c . . .958 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
? ? ? ? ? ? ? ? ? ? ?
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
? ? ? ? ? ? ? ? ? ?
loop_
_refln_index_h
_refln_index_k
_refln_index_l
_refln_F_meas
_refln_F_calc
_refln_F_sigma
_refln_F_squared_meas
_refln_F_squared_calc
_refln_F_squared_sigma
_refln_observed_status
_refln_f_meas_friedel
_refln_f_sigma_friedel
_refln_f_squared_meas_friedel
_refln_f_squared_sigma_friedel
? ? ? ? ? ? ? ? ? ? ? ? ? ?
|
1100970.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100970.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_1100970
loop_
_publ_author_name
'Corrado Di Nicola'
'Agustin Galindo'
'John V. Hanna'
'Fabio Marchetti'
'Claudio Pettinari'
'Riccardo Pettinari'
'Eleonora Rivarola'
'Brian W. Skelton'
'Allan H. White'
_publ_contact_author_address
;
Department of Chemistry
University of Western Australia
35 Stirling Highway
Crawley
Western Australia 6009
Australia
;
_publ_contact_author_email bws@crystal.uwa.edu.au
_publ_contact_author_fax (+61)_08_9380_1118
_publ_contact_author_name 'Skelton, B. W.'
_publ_contact_author_phone (+61)_08-9380_3481
_publ_section_title
;
Synthesis and Spectroscopic and X-ray Structural Characterization of
R2SnIV-Oxydiacetate and -Iminodiacetate Complexes
;
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3094
_journal_page_last 3102
_journal_paper_doi 10.1021/ic048240t
_journal_volume 44
_journal_year 2005
_chemical_formula_moiety 'C7 H15 N1 O5 Sn1'
_chemical_formula_sum 'C7 H15 N O5 Sn'
_chemical_formula_weight 311.91
_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'
_cell_angle_alpha 90.00000
_cell_angle_beta 107.2310(10)
_cell_angle_gamma 90.00000
_cell_formula_units_Z 4
_cell_length_a 10.6103(7)
_cell_length_b 6.7816(5)
_cell_length_c 15.5010(10)
_cell_measurement_reflns_used 8352
_cell_measurement_temperature 150
_cell_measurement_theta_max 37.56
_cell_measurement_theta_min 2.25
_cell_volume 1065.31(13)
_computing_cell_refinement 'Siemens SAINT (Siemens, 1995)'
_computing_data_collection 'Siemens SMART (Siemens, 1995)'
_computing_data_reduction xtal
_computing_molecular_graphics xtal
_computing_publication_material 'xtal BONDLA CIFIO'
_computing_structure_refinement xtal
_computing_structure_solution xtal
_diffrn_ambient_temperature 150(2)
_diffrn_measured_fraction_theta_full .95
_diffrn_measured_fraction_theta_max .95
_diffrn_measurement_device_type
;
Bruker SMART CCD diffractometer
;
_diffrn_measurement_method '\w scans'
_diffrn_radiation_detector 'CCD area detector'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'sealed tube'
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength .71073
_diffrn_reflns_av_R_equivalents .032
_diffrn_reflns_av_sigmaI/netI .036
_diffrn_reflns_limit_h_max 16
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_l_max 24
_diffrn_reflns_limit_l_min -24
_diffrn_reflns_number 21952
_diffrn_reflns_theta_full 32.65
_diffrn_reflns_theta_max 34.65
_diffrn_reflns_theta_min 2.01
_diffrn_standards_decay_% 0
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 2.396
_exptl_absorpt_correction_T_max 1
_exptl_absorpt_correction_T_min .89
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS; Sheldrick, 1996
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.945
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description cuboid
_exptl_crystal_F_000 616
_exptl_crystal_size_max .1
_exptl_crystal_size_mid .1
_exptl_crystal_size_min .1
_refine_diff_density_max 3.00
_refine_diff_density_min -.89
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_all 1.1
_refine_ls_goodness_of_fit_ref 1.131
_refine_ls_hydrogen_treatment noref
_refine_ls_matrix_type full
_refine_ls_number_constraints 0
_refine_ls_number_parameters 136
_refine_ls_number_reflns 3887
_refine_ls_number_restraints 0
_refine_ls_R_factor_all .044
_refine_ls_R_factor_gt .034
_refine_ls_shift/su_max .002
_refine_ls_shift/su_mean .0002
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_all .05
_refine_ls_wR_factor_ref .047
_reflns_d_resolution_high .625
_reflns_d_resolution_low 10.114
_reflns_limit_h_max 16
_reflns_limit_h_min 0
_reflns_limit_k_max 10
_reflns_limit_k_min 0
_reflns_limit_l_max 23
_reflns_limit_l_min -24
_reflns_number_gt 3887
_reflns_number_total 4562
_reflns_threshold_expression 'F > 4.00 sig(F )'
_cod_data_source_file ic048240tsi20041215_025357_3.cif
_cod_data_source_block cpsnn2
_cod_original_sg_symbol_Hall -p_2ybc
_cod_original_formula_sum 'C7 H15 N1 O5 Sn1'
_cod_database_code 1100970
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
-x,1/2+y,1/2-z
-x,-y,-z
+x,1/2-y,1/2+z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn .78917(2) .48185(3) .418680(10) .02120(9) Uani ? ? 1.00000 ? ?
C01 .8515(3) .2141(5) .3757(2) .0344(13) Uani ? ? 1.00000 ? ?
C02 .7719(3) .7126(6) .5058(2) .0365(14) Uani ? ? 1.00000 ? ?
N0 .7567(2) .6670(3) .29099(15) .0217(8) Uani ? ? 1.00000 ? ?
C11 .8772(2) .7168(4) .26812(16) .0213(9) Uani ? ? 1.00000 ? ?
C12 .9993(2) .7099(4) .34942(17) .0216(10) Uani ? ? 1.00000 ? ?
O11 .99188(18) .6216(3) .41965(13) .0267(8) Uani ? ? 1.00000 ? ?
O12 1.1004(2) .7914(4) .34091(15) .0355(10) Uani ? ? 1.00000 ? ?
C21 .6532(2) .5698(4) .21871(16) .0221(9) Uani ? ? 1.00000 ? ?
C22 .5485(3) .4851(4) .25759(19) .0208(9) Uani ? ? 1.00000 ? ?
O21 .5835(2) .4540(3) .34346(14) .0263(8) Uani ? ? 1.00000 ? ?
O22 .4379(2) .4503(3) .20527(16) .0302(9) Uani ? ? 1.00000 ? ?
O03 .7075(3) .2579(6) .5086(2) .0281(14) Uani ? ? .809(11) ? ?
C03 .5876(4) .2699(13) .5281(4) .054(3) Uani ? ? .809(11) ? ?
O03' .6993(10) .348(2) .5274(7) .017(2) Uiso ? ? .191(11) ? ?
C03' .605(3) .195(4) .5086(18) .043(6) Uiso ? ? .191(11) ? ?
H01a .91952 .15703 .42362 .05200 Uiso ? ? 1.00000 ? ?
H01b .77906 .12456 .35796 .05200 Uiso ? ? 1.00000 ? ?
H01c .88393 .23684 .32526 .05200 Uiso ? ? 1.00000 ? ?
H02a .73158 .82442 .47126 .05500 Uiso ? ? 1.00000 ? ?
H02b .85644 .74845 .54399 .05500 Uiso ? ? 1.00000 ? ?
H02c .71805 .67083 .54178 .05500 Uiso ? ? 1.00000 ? ?
H0 .72932 .79246 .30093 .02300 Uiso ? ? 1.00000 ? ?
H11a .88749 .62494 .22393 .02700 Uiso ? ? 1.00000 ? ?
H11b .86836 .84592 .24271 .02700 Uiso ? ? 1.00000 ? ?
H21a .61319 .66271 .17288 .02800 Uiso ? ? 1.00000 ? ?
H21b .69109 .46608 .19346 .02800 Uiso ? ? 1.00000 ? ?
H03 .76654 .21923 .55552 .03000 Uiso ? ? 1.00000 ? ?
H03a .56831 .15377 .55624 .05900 Uiso ? ? .809(11) ? ?
H03b .59465 .38094 .57280 .05900 Uiso ? ? .809(11) ? ?
H03c .51762 .30791 .47698 .05900 Uiso ? ? .809(11) ? ?
H03'a .53588 .24457 .45729 .07500 Uiso ? ? .191(11) ? ?
H03'b .62695 .08367 .51470 .07500 Uiso ? ? .191(11) ? ?
H03'c .56056 .23672 .56094 .07500 Uiso ? ? .191(11) ? ?
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
Sn .01188(8) .03246(11) .01799(9) -.00314(6) .00249(6) .00430(6)
C01 .0225(13) .0339(15) .0429(17) -.0004(11) .0035(12) -.0063(12)
C02 .0240(13) .051(2) .0332(15) .0037(13) .0062(11) -.0086(13)
N0 .0171(9) .0258(10) .0210(9) -.0011(7) .0039(7) -.0015(7)
C11 .0152(10) .0303(12) .0180(10) -.0023(8) .0041(8) .0019(8)
C12 .0150(10) .0297(12) .0194(10) -.0015(8) .0039(8) .0029(9)
O11 .0165(8) .0411(11) .0205(8) -.0052(7) .0021(6) .0088(8)
O12 .0167(8) .0574(15) .0299(10) -.0098(9) .0034(8) .0172(10)
C21 .0150(10) .0312(12) .0170(10) -.0015(9) .0001(8) -.0026(9)
C22 .0130(9) .0226(11) .0240(11) .0003(8) .0009(8) .0007(8)
O21 .0142(8) .0371(10) .0244(9) -.0035(7) .0008(7) .0074(8)
O22 .0163(8) .0350(11) .0321(10) -.0063(8) -.0037(7) .0052(8)
O03 .0171(11) .040(2) .0250(13) -.0012(10) .0022(9) .0109(12)
C03 .0149(17) .099(5) .048(3) .002(2) .0070(17) .044(3)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C ? 0 28 .002014 .002014 'Int Tables Vol IV Tables 2.2B and 2.3.1'
H ? 0 60 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1'
N ? 0 4 .004028 .002991 'Int Tables Vol IV Tables 2.2B and 2.3.1'
O ? 0 20 .007996 .005981 'Int Tables Vol IV Tables 2.2B and 2.3.1'
Sn ? 0 4 -.872986 1.424 'Int Tables Vol IV Tables 2.2B and 2.3.1'
loop_
_diffrn_attenuator_code
_diffrn_attenuator_scale
? ?
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C01 Sn C02 . . . 159.46(12) ?
C01 Sn N0 . . . 100.41(12) ?
C01 Sn O11 . . . 88.70(11) ?
C01 Sn O21 . . . 96.63(10) ?
C01 Sn O03 . . . 80.72(14) ?
C01 Sn O03' . . . 97.2(3) ?
C02 Sn N0 . . . 97.33(12) ?
C02 Sn O11 . . . 87.11(11) ?
C02 Sn O21 . . . 98.35(11) ?
C02 Sn O03 . . . 89.02(14) ?
C02 Sn O03' . . . 72.4(3) ?
N0 Sn O11 . . . 71.70(7) ?
N0 Sn O21 . . . 73.18(8) ?
N0 Sn O03 . . . 150.16(8) ?
N0 Sn O03' . . . 147.7(2) ?
O11 Sn O21 . . . 144.86(8) ?
O11 Sn O03 . . . 137.97(7) ?
O11 Sn O03' . . . 135.8(2) ?
O21 Sn O03 . . . 77.06(8) ?
O21 Sn O03' . . . 78.1(2) ?
O03 Sn O03' . . . 16.8(3) ?
Sn C01 H01a . . . 109.9 ?
Sn C01 H01b . . . 109.8 ?
Sn C01 H01c . . . 110.0 ?
H01a C01 H01b . . . 109.0 ?
H01a C01 H01c . . . 109.3 ?
H01b C01 H01c . . . 108.8 ?
Sn C02 H02a . . . 109.9 ?
Sn C02 H02b . . . 110.2 ?
Sn C02 H02c . . . 109.6 ?
H02a C02 H02b . . . 109.3 ?
H02a C02 H02c . . . 108.5 ?
H02b C02 H02c . . . 109.3 ?
Sn N0 C11 . . . 114.76(14) ?
Sn N0 C21 . . . 107.50(17) ?
Sn N0 H0 . . . 109.58 ?
C11 N0 C21 . . . 115.3(2) ?
C11 N0 H0 . . . 99.6 ?
C21 N0 H0 . . . 109.7 ?
N0 C11 C12 . . . 112.6(2) ?
N0 C11 H11a . . . 108.5 ?
N0 C11 H11b . . . 109.1 ?
C12 C11 H11a . . . 108.9 ?
C12 C11 H11b . . . 109.1 ?
H11a C11 H11b . . . 108.7 ?
C11 C12 O11 . . . 118.3(2) ?
C11 C12 O12 . . . 116.6(2) ?
O11 C12 O12 . . . 125.1(2) ?
Sn O11 C12 . . . 118.44(14) ?
N0 C21 C22 . . . 109.5(2) ?
N0 C21 H21a . . . 109.8 ?
N0 C21 H21b . . . 109.5 ?
C22 C21 H21a . . . 109.2 ?
C22 C21 H21b . . . 109.4 ?
H21a C21 H21b . . . 109.4 ?
C21 C22 O21 . . . 116.7(2) ?
C21 C22 O22 . . . 118.3(3) ?
O21 C22 O22 . . . 125.0(3) ?
Sn O21 C22 . . . 118.7(2) ?
Sn O03 C03 . . . 126.9(4) ?
Sn O03 H03 . . . 113.1(3) ?
Sn O03 H03 . . . 113.1(3) ?
C03 O03 H03 . . . 108.8(4) ?
O03 C03 H03a . . . 112.7(6) ?
O03 C03 H03b . . . 107.7(5) ?
O03 C03 H03c . . . 112.0(6) ?
H03a C03 H03b . . . 106.5(6) ?
H03a C03 H03c . . . 112.8(6) ?
H03b C03 H03c . . . 104.5(7) ?
Sn O03' C03' . . . 123.3(13) ?
Sn O03' H03 . . . 103.3(7) ?
C03' O03' H03 . . . 80.8(13) ?
O03' C03' H03'a . . . 103(2) ?
O03' C03' H03'b . . . 121(3) ?
O03' C03' H03'c . . . 95.2(18) ?
H03'a C03' H03'b . . . 124(3) ?
H03'a C03' H03'c . . . 98(3) ?
H03'b C03' H03'c . . . 110(3) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Sn C01 . . 2.107(4) ?
Sn C02 . . 2.109(4) ?
Sn N0 . . 2.282(2) ?
Sn O11 . . 2.346(2) ?
Sn O21 . . 2.156(2) ?
Sn O03 . . 2.391(4) ?
Sn O03' . . 2.351(12) ?
C01 H01a . . .951 ?
C01 H01b . . .954 ?
C01 H01c . . .956 ?
C02 H02a . . .953 ?
C02 H02b . . .949 ?
C02 H02c . . .953 ?
N0 C11 . . 1.463(4) ?
N0 C21 . . 1.472(3) ?
N0 H0 . . .927 ?
C11 C12 . . 1.518(3) ?
C11 H11a . . .956 ?
C11 H11b . . .953 ?
C12 O11 . . 1.265(4) ?
C12 O12 . . 1.248(4) ?
C21 C22 . . 1.524(4) ?
C21 H21a . . .951 ?
C21 H21b . . .950 ?
C22 O21 . . 1.289(4) ?
C22 O22 . . 1.235(3) ?
O03 C03 . . 1.394(6) ?
O03 H03 . . .849 ?
C03 H03a . . .951 ?
C03 H03b . . 1.012 ?
C03 H03c . . .947 ?
O03' C03' . . 1.41(3) ?
C03' H03'a . . .97 ?
C03' H03'b . . .79 ?
C03' H03'c . . 1.09 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
? ? ? ? ? ? ? ? ? ? ?
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
? ? ? ? ? ? ? ? ? ?
loop_
_refln_index_h
_refln_index_k
_refln_index_l
_refln_F_meas
_refln_F_calc
_refln_F_sigma
_refln_F_squared_meas
_refln_F_squared_calc
_refln_F_squared_sigma
_refln_observed_status
_refln_f_meas_friedel
_refln_f_sigma_friedel
_refln_f_squared_meas_friedel
_refln_f_squared_sigma_friedel
? ? ? ? ? ? ? ? ? ? ? ? ? ?
|
1100971.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100971.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_1100971
loop_
_publ_author_name
'Hamdi Ben Yahia'
'Etienne Gaudin'
'Jacques Darriet'
'Michael Banks'
'Reinhard K. Kremer'
'Antoine Villesuzanne'
'Myung-Hwan Whangbo'
_publ_section_title
;
Synthesis, Crystal Structure, Magnetic Properties, and Electronic Structure
of the New Ternary Vanadate CuMnVO4
;
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3087
_journal_page_last 3093
_journal_paper_doi 10.1021/ic048244y
_journal_volume 44
_journal_year 2005
_chemical_formula_moiety 'Cu Mn O4 V'
_chemical_formula_sum 'Cu Mn O4 V'
_chemical_formula_weight 233.4
_chemical_name_systematic ' ?'
_space_group_IT_number 63
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall '-C 2c 2'
_symmetry_space_group_name_H-M 'C m c m'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 5.787(2)
_cell_length_b 8.807(3)
_cell_length_c 6.410(2)
_cell_measurement_temperature 293(1)
_cell_volume 326.69(19)
_computing_publication_material '(Jana2000; Petricek and Dusek, 2000)'
_computing_structure_refinement '(Jana2000; Petricek and Dusek, 2000)'
_diffrn_ambient_temperature 293(1)
_diffrn_measured_fraction_theta_full 1.00
_diffrn_measurement_device_type 'Nonius CCD'
_diffrn_measurement_method '/f scans + /w scans'
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71069
_diffrn_reflns_av_R_equivalents 0.1017
_diffrn_reflns_av_sigmaI/netI 0.0452
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_l_max 11
_diffrn_reflns_limit_l_min -11
_diffrn_reflns_number 6676
_diffrn_reflns_theta_full 39.99
_diffrn_reflns_theta_max 39.99
_diffrn_reflns_theta_min 4.21
_exptl_absorpt_coefficient_mu 12.894
_exptl_absorpt_correction_T_max 0.785
_exptl_absorpt_correction_T_min 0.612
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details '(Jana2000; Petricek and Dusek, 2000)'
_exptl_crystal_colour black
_exptl_crystal_density_diffrn 4.744(3)
_exptl_crystal_description block
_exptl_crystal_F_000 436
_exptl_crystal_size_max 0.050
_exptl_crystal_size_mid 0.031
_exptl_crystal_size_min 0.022
_refine_diff_density_max 2.12
_refine_diff_density_min -1.77
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_gt 1.71
_refine_ls_goodness_of_fit_ref 1.71
_refine_ls_number_parameters 25
_refine_ls_number_reflns 433
_refine_ls_R_factor_all 0.0356
_refine_ls_R_factor_gt 0.0356
_refine_ls_shift/su_max 0.0006
_refine_ls_shift/su_mean 0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details w=1/(\s^2^(I)+0.0016I^2^)
_refine_ls_weighting_scheme sigma
_refine_ls_wR_factor_gt 0.1091
_refine_ls_wR_factor_ref 0.1091
_reflns_number_gt 433
_reflns_number_total 578
_reflns_threshold_expression I>3\s(I)
_cod_data_source_file ic048244ysi20041214_022448.cif
_cod_data_source_block (I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Gaussian' changed to 'gaussian'
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 'Cu1 Mn1 O4 V1'
_cod_database_code 1100971
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 x,y,1/2-z
3 -x,y,z
4 -x,y,1/2-z
5 -x,-y,-z
6 -x,-y,1/2+z
7 x,-y,-z
8 x,-y,1/2+z
9 1/2+x,1/2+y,z
10 1/2+x,1/2+y,1/2-z
11 1/2-x,1/2+y,z
12 1/2-x,1/2+y,1/2-z
13 1/2-x,1/2-y,-z
14 1/2-x,1/2-y,1/2+z
15 1/2+x,1/2-y,-z
16 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_adp_type
_atom_site_U_iso_or_equiv
_atom_site_symmetry_multiplicity
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu Cu 0 0.32230(13) 0.75 Uani 0.0291(3) 4 1 d . . .
Mn Mn 0 0 0.5 Uani 0.0094(2) 4 1 d . . .
V V 0 0.64184(10) 0.75 Uani 0.0075(2) 4 1 d . . .
O1 O 0.2473(5) 0.4748(3) 0.25 Uani 0.0115(7) 8 1 d . . .
O2 O 0 0.2438(3) 0.4625(4) Uani 0.0131(7) 8 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_type_symbol
_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
Cu Cu 0.0472(6) 0.0266(5) 0.0135(4) 0 0 0
Mn Mn 0.0098(4) 0.0114(4) 0.0069(3) 0 0 -0.0001(2)
V V 0.0073(4) 0.0088(4) 0.0063(3) 0 0 0
O1 O 0.0098(12) 0.0155(12) 0.0091(11) -0.0012(9) 0 0
O2 O 0.0143(13) 0.0138(13) 0.0112(10) 0 0 0.0005(10)
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cu 0.320 1.265 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1'
Mn 0.337 0.728 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1'
V 0.301 0.529 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1'
O 0.011 0.006 'International Tables 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_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 Cu O1 5_566 . 13_556 170.51(10) yes
O1 Cu O1 5_566 . 7_566 77.39(11) yes
O1 Cu O1 5_566 . 15_456 112.11(9) yes
O1 Cu O2 5_566 . . 105.92(7) yes
O1 Cu O2 5_566 . 2_556 105.92(7) yes
O1 Cu O1 13_556 . 5_566 170.51(10) yes
O1 Cu O1 13_556 . 7_566 112.11(9) yes
O1 Cu O1 13_556 . 15_456 58.40(8) yes
O1 Cu O2 13_556 . . 72.14(8) yes
O1 Cu O2 13_556 . 2_556 72.14(8) yes
O1 Cu O1 7_566 . 5_566 77.39(11) yes
O1 Cu O1 7_566 . 13_556 112.11(9) yes
O1 Cu O1 7_566 . 15_456 170.51(10) yes
O1 Cu O2 7_566 . . 105.92(7) yes
O1 Cu O2 7_566 . 2_556 105.92(7) yes
O1 Cu O1 15_456 . 5_566 112.11(9) yes
O1 Cu O1 15_456 . 13_556 58.40(8) yes
O1 Cu O1 15_456 . 7_566 170.51(10) yes
O1 Cu O2 15_456 . . 72.14(8) yes
O1 Cu O2 15_456 . 2_556 72.14(8) yes
O2 Cu O2 . . 2_556 138.85(14) yes
O2 Cu O2 2_556 . . 138.85(14) yes
O1 Mn O1 9_445 . 13_556 180 yes
O1 Mn O1 9_445 . 11_545 84.23(8) yes
O1 Mn O1 9_445 . 15_456 95.77(8) yes
O1 Mn O2 9_445 . . 91.10(9) yes
O1 Mn O2 9_445 . 5_556 88.90(9) yes
O1 Mn O1 13_556 . 9_445 180 yes
O1 Mn O1 13_556 . 11_545 95.77(8) yes
O1 Mn O1 13_556 . 15_456 84.23(8) yes
O1 Mn O2 13_556 . . 88.90(9) yes
O1 Mn O2 13_556 . 5_556 91.10(9) yes
O1 Mn O1 11_545 . 9_445 84.23(8) yes
O1 Mn O1 11_545 . 13_556 95.77(8) yes
O1 Mn O1 11_545 . 15_456 180 yes
O1 Mn O2 11_545 . . 91.10(9) yes
O1 Mn O2 11_545 . 5_556 88.90(9) yes
O1 Mn O1 15_456 . 9_445 95.77(8) yes
O1 Mn O1 15_456 . 13_556 84.23(8) yes
O1 Mn O1 15_456 . 11_545 180 yes
O1 Mn O2 15_456 . . 88.90(9) yes
O1 Mn O2 15_456 . 5_556 91.10(9) yes
O2 Mn O2 . . 5_556 180 yes
O2 Mn O2 5_556 . . 180 yes
O1 V O1 5_566 . 7_566 108.63(14) yes
O1 V O2 5_566 . 5_566 110.30(7) yes
O1 V O2 5_566 . 6_565 110.30(7) yes
O1 V O1 7_566 . 5_566 108.63(14) yes
O1 V O2 7_566 . 5_566 110.30(7) yes
O1 V O2 7_566 . 6_565 110.30(7) yes
O2 V O2 5_566 . 6_565 107.02(15) yes
O2 V O2 6_565 . 5_566 107.02(15) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cu O1 . 5_566 2.289(3) yes
Cu O1 . 13_556 2.998(3) yes
Cu O1 . 7_566 2.289(3) yes
Cu O1 . 15_456 2.998(3) yes
Cu O2 . . 1.969(3) yes
Cu O2 . 2_556 1.969(3) yes
Mn O1 . 9_445 2.181(2) yes
Mn O1 . 13_556 2.181(2) yes
Mn O1 . 11_545 2.181(2) yes
Mn O1 . 15_456 2.181(2) yes
Mn O2 . . 2.160(3) yes
Mn O2 . 5_556 2.160(3) yes
V O1 . 5_566 1.762(3) yes
V O1 . 7_566 1.762(3) yes
V O2 . 5_566 1.694(3) yes
V O2 . 6_565 1.694(3) yes
|
1100972.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100972.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_1100972
loop_
_publ_author_name
'David B. Mitzi'
_publ_contact_author_address
;IBM T. J. Watson Research Center
P.O. Box 218
Yorktown Heights, NY 10598
;
_publ_contact_author_email dmitzi@us.ibm.com
_publ_contact_author_fax 914-945-2141
_publ_contact_author_name 'Dr. David B. Mitzi'
_publ_contact_author_phone 914-945-4176
_publ_section_title
;
Synthesis, Structure, and Thermal Properties of Soluble Hydrazinium
Germanium(IV) and Tin(IV) Selenide Salts
;
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3755
_journal_page_last 3761
_journal_paper_doi 10.1021/ic048276l
_journal_volume 44
_journal_year 2005
_chemical_formula_moiety 'N14 H32 Sn2 Se6'
_chemical_formula_sum 'H32 N14 Se6 Sn2'
_chemical_formula_weight 939.53
_chemical_name_common 'hydrazinium/hydrazine tin(IV) selenide'
_chemical_name_systematic 'hydrazinium/hydrazine tin(IV) selenide'
_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 94.110(2)
_cell_angle_beta 99.429(2)
_cell_angle_gamma 104.141(2)
_cell_formula_units_Z 1
_cell_length_a 6.6475(6)
_cell_length_b 9.5474(9)
_cell_length_c 9.883(1)
_cell_measurement_reflns_used 3504
_cell_measurement_temperature 293
_cell_volume 595.91(10)
_computing_data_reduction 'NRCVAX DATRD2'
_computing_molecular_graphics NRCVAX
_computing_publication_material 'NRCVAX TABLES Jan 94 Version'
_computing_structure_refinement 'NRCVAX LSTSQ'
_computing_structure_solution 'NRCVAX SOLVER'
_diffrn_ambient_temperature 293
_diffrn_measurement_device 'SMART 1000'
_diffrn_measurement_method CCD
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Molybdenum K\a'
_diffrn_radiation_wavelength 0.70930
_diffrn_reflns_av_R_equivalents 0.010
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_h_min -8
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_l_max 12
_diffrn_reflns_limit_l_min -12
_diffrn_reflns_number 6514
_diffrn_reflns_theta_max 27.46
_diffrn_reflns_theta_min 0.00
_diffrn_source 'xray tube'
_diffrn_source_type 'Bruker SMART 1000'
_exptl_absorpt_coefficient_mu 11.28
_exptl_absorpt_correction_type empirical
_exptl_absorpt_process_details SADABS
_exptl_crystal_colour 'pale yellow'
_exptl_crystal_density_diffrn 2.618
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 432.70
_exptl_crystal_size_max 0.46
_exptl_crystal_size_mid 0.12
_exptl_crystal_size_min 0.11
_refine_diff_density_max 0.58
_refine_diff_density_min -0.60
_refine_ls_extinction_coef 173(56)
_refine_ls_extinction_method Larson
_refine_ls_goodness_of_fit_obs 1.15
_refine_ls_matrix_type full
_refine_ls_number_parameters 165
_refine_ls_number_reflns 2342
_refine_ls_R_factor_all 0.023
_refine_ls_R_factor_obs 0.023
_refine_ls_shift/esd_max 0.000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details 'calc w=1/(\s^2^(F)+0.0003F^2^)'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_all 0.028
_refine_ls_wR_factor_obs 0.028
_reflns_number_observed 2342
_reflns_number_total 2723
_reflns_observed_criterion 'Inet > 2.5\s(Inet)'
_cod_data_source_file ic048276lsi20050307_015625_1.cif
_cod_data_source_block hydsnse
_cod_original_cell_volume 595.9(1)
_cod_original_formula_sum 'N14 H32 Sn2 Se6'
_cod_database_code 1100972
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_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Sn 0.0210(1) 0.0208(1) 0.0194(1) 0.0037(1) 0.0026(1) 0.0014(1)
Se1 0.0269(2) 0.0212(2) 0.0355(2) 0.0037(1) 0.0073(2) 0.0039(2)
Se2 0.02111(18) 0.03018(20) 0.02798(21) 0.00638(14) 0.00507(15) -0.00459(15)
Se3 0.04371(24) 0.03425(22) 0.02108(20) 0.01107(17) 0.00411(17) 0.00660(15)
N1 0.0343(20) 0.0458(24) 0.0411(23) 0.0027(18) 0.0049(18) -0.0035(19)
N3 0.0300(19) 0.0536(24) 0.0374(22) 0.0107(17) 0.0024(17) 0.0014(17)
N5 0.0523(25) 0.0350(21) 0.0358(22) 0.0168(18) 0.0117(18) 0.0050(17)
N2 0.0464(24) 0.0490(25) 0.044(3) 0.0105(20) 0.0124(20) 0.0034(20)
N4 0.055(3) 0.052(3) 0.039(3) 0.0270(20) 0.0041(21) 0.0036(20)
N7 0.0454(23) 0.0439(23) 0.051(3) 0.0133(18) 0.0010(19) -0.0009(20)
N6 0.073(3) 0.058(3) 0.039(3) 0.028(3) 0.0032(23) 0.0068(21)
loop_
_atom_site_label
_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_calc_flag
_atom_site_refinement_flags
_atom_site_type_symbol
Sn1 0.30370(3) 0.38498(2) 0.37392(2) 0.0209(1) Uani . . Sn
Se1 0.12852(6) 0.13609(4) 0.41146(4) 0.0281(2) Uani . . Se
Se2 0.71084(5) 0.42867(4) 0.42639(4) 0.0268(2) Uani . . Se
Se3 0.18900(7) 0.46138(4) 0.14742(4) 0.0329(2) Uani . . Se
N1 0.2694(6) 0.8114(5) 0.8826(4) 0.0424(22) Uani . . N
N3 0.5585(6) 0.0286(4) 0.3177(4) 0.0410(22) Uani . . N
N5 0.0295(7) 0.7366(4) 0.3068(4) 0.0396(22) Uani . . N
N2 0.4189(7) 0.7489(5) 0.9617(5) 0.0465(24) Uani . . N
N4 0.4578(7) -0.1247(5) 0.2888(5) 0.0472(25) Uani . . N
N7 0.1130(6) 0.0132(5) 0.0270(5) 0.0479(23) Uani . . N
N6 -0.1343(9) 0.7272(5) 0.1910(5) 0.055(3) Uani . . N
HN4b 0.486(8) -0.166(6) 0.214(6) 0.056(16) Uiso . . H
HN7a 0.135(11) 0.041(8) 0.118(8) 0.10(3) Uiso . . H
HN4a 0.504(8) -0.162(5) 0.348(5) 0.038(15) Uiso . . H
HN1a 0.229(8) 0.884(6) 0.939(6) 0.060(16) Uiso . . H
HN5a 0.162(8) 0.793(5) 0.298(5) 0.057(16) Uiso . . H
HN5b -0.001(10) 0.782(6) 0.380(6) 0.077(19) Uiso . . H
HN3a 0.684(8) 0.054(5) 0.369(5) 0.043(13) Uiso . . H
HN3b 0.451(7) 0.059(5) 0.368(4) 0.043(13) Uiso . . H
HN6a -0.107(10) 0.680(7) 0.125(7) 0.080(22) Uiso . . H
HN1b 0.162(7) 0.740(5) 0.836(4) 0.034(12) Uiso . . H
HN2a 0.470(9) 0.706(6) 0.911(6) 0.061(19) Uiso . . H
HN1c 0.326(10) 0.862(7) 0.814(7) 0.085(21) Uiso . . H
HN7b 0.167(12) 0.118(8) -0.001(8) 0.12(3) Uiso . . H
HN5c 0.069(9) 0.653(7) 0.307(6) 0.074(19) Uiso . . H
HN2b 0.340(10) 0.699(7) 1.006(7) 0.077(21) Uiso . . H
HN6b -0.252(10) 0.664(7) 0.202(7) 0.080(23) Uiso . . H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
N N 0.006 0.003 'International Tables Vol. IV Table 2.2B'
H H 0.000 0.000 'International Tables Vol. IV Table 2.2B'
Sn Sn -0.654 1.425 'International Tables Vol. IV Table 2.2B'
Se Se -0.093 2.226 'International Tables Vol. IV Table 2.2B'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
Sn1a Sn1 Se1 121.758(14)
Sn1a Sn1 Se2 47.767(10)
Sn1a Sn1 Se2a 47.825(10)
Sn1a Sn1 Se3 121.879(14)
Se1 Sn1 Se2 110.635(15)
Se1 Sn1 Se2a 110.777(16)
Se1 Sn1 Se3 116.360(16)
Se2 Sn1 Se2a 95.592(13)
Se2 Sn1 Se3 110.403(16)
Se2a Sn1 Se3 111.158(17)
Sn1 Se2 Sn1a 84.409(13)
N2 N1 HN1a 112(3)
N2 N1 HN1b 108(3)
N2 N1 HN1c 111(4)
N2 N1 HN2b 27.4(20)
HN1a N1 HN1b 115(4)
HN1a N1 HN1c 104(5)
HN1a N1 HN2b 101(4)
HN1b N1 HN1c 104(5)
HN1b N1 HN2b 92(3)
HN1c N1 HN2b 138(4)
N4 N3 HN4a 23.6(16)
N4 N3 HN3a 116(3)
N4 N3 HN3b 98.5(24)
HN4a N3 HN3a 95(3)
HN4a N3 HN3b 98(3)
HN3a N3 HN3b 110(4)
N6 N5 HN5a 114(3)
N6 N5 HN5b 108(4)
N6 N5 HN5c 109(4)
HN5a N5 HN5b 104(5)
HN5a N5 HN5c 94(5)
HN5b N5 HN5c 124(5)
N1 N2 HN2a 109(4)
N1 N2 HN2b 99(4)
HN2a N2 HN2b 116(6)
N3 N4 HN4b 113(3)
N3 N4 HN4a 107(4)
HN4b N4 HN4a 104(5)
N7b N7 HN7a 107(4)
N7b N7 HN7b 99(4)
HN7a N7 HN7b 95(6)
N5 N6 HN6a 107(4)
N5 N6 HN6b 109(4)
HN6a N6 HN6b 98(6)
N4 HN4b HN4a 34(3)
N7 HN7a HN7b 46(4)
N3 HN4a N4 48(3)
N3 HN4a HN4b 75(3)
N4 HN4a HN4b 40(3)
N1 HN1a HN1b 30.9(24)
N1 HN1a HN1c 36(3)
HN1b HN1a HN1c 55(3)
N5 HN5a HN5b 36(3)
N5 HN5a HN5c 41(3)
HN5b HN5a HN5c 69(4)
N5 HN5b HN5a 38(3)
N5 HN5b HN5c 27(3)
HN5a HN5b HN5c 52(4)
N3 HN3a HN3b 37(3)
N3 HN3b HN3a 31.5(22)
N6 HN6a HN6b 42(4)
N1 HN1b HN1a 34(3)
N1 HN1b HN1c 38(3)
HN1a HN1b HN1c 59(4)
N2 HN2a HN2b 32(4)
N1 HN1c HN1a 38(3)
N1 HN1c HN1b 36(3)
HN1a HN1c HN1b 64(4)
N7 HN7b HN7a 38(4)
N5 HN5c HN5a 43(3)
N5 HN5c HN5b 27(3)
HN5a HN5c HN5b 58(4)
N1 HN2b N2 53(4)
N1 HN2b HN2a 71(4)
N2 HN2b HN2a 31(3)
N6 HN6b HN6a 39(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Sn1 Sn1a 3.4827(5)
Sn1 Se1 2.4609(5)
Sn1 Se2 2.5933(5)
Sn1 Se2a 2.5909(4)
Sn1 Se3 2.4639(5)
Se2 Sn1a 2.5909(4)
N1 N2 1.434(6)
N1 HN1a 0.97(6)
N1 HN1b 0.89(5)
N1 HN1c 0.93(7)
N3 N4 1.439(6)
N3 HN4a 1.82(5)
N3 HN3a 0.87(5)
N3 HN3b 1.02(5)
N5 N6 1.426(6)
N5 HN5a 0.94(5)
N5 HN5b 0.89(6)
N5 HN5c 0.89(6)
N2 HN2a 0.79(6)
N2 HN2b 0.82(7)
N4 HN4b 0.88(6)
N4 HN4a 0.76(5)
N7 N7b 1.462(8)
N7 HN7a 0.90(7)
N7 HN7b 1.05(8)
N6 HN6a 0.83(7)
N6 HN6b 0.89(7)
HN4b HN4a 1.30(7)
HN7a HN7b 1.45(11)
HN1a HN1b 1.58(7)
HN1a HN1c 1.50(9)
HN5a HN5b 1.44(8)
HN5a HN5c 1.35(8)
HN5b HN5c 1.58(9)
HN3a HN3b 1.56(7)
HN6a HN6b 1.30(9)
HN1b HN1c 1.44(8)
HN2a HN2b 1.37(9)
|
1100973.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100973.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_1100973
loop_
_publ_author_name
'David B. Mitzi'
_publ_contact_author_address
;IBM T. J. Watson Research Center
P.O. Box 218
Yorktown Heights, NY 10598
;
_publ_contact_author_email dmitzi@us.ibm.com
_publ_contact_author_fax 914-945-2141
_publ_contact_author_name 'Dr. David B. Mitzi'
_publ_contact_author_phone 914-945-4176
_publ_section_title
;
Synthesis, Structure, and Thermal Properties of Soluble Hydrazinium
Germanium(IV) and Tin(IV) Selenide Salts
;
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3755
_journal_page_last 3761
_journal_paper_doi 10.1021/ic048276l
_journal_volume 44
_journal_year 2005
_chemical_formula_moiety 'N8 H20 Ge2 Se6'
_chemical_formula_sum 'Ge2 H20 N8 Se6'
_chemical_formula_weight 751.14
_chemical_name_common 'hydrazinium germanium(IV) selenide'
_chemical_name_systematic 'hydrazinium germanium(IV) selenide'
_space_group_IT_number 110
_symmetry_cell_setting tetragonal
_symmetry_Int_Tables_number 110
_symmetry_space_group_name_Hall 'I 4bw -2c'
_symmetry_space_group_name_H-M 'I 41 c d'
_cell_angle_alpha 90.0
_cell_angle_beta 90.0
_cell_angle_gamma 90.0
_cell_formula_units_Z 8
_cell_length_a 12.7080(12)
_cell_length_b 12.7080(12)
_cell_length_c 21.9553(20)
_cell_measurement_reflns_used 24
_cell_measurement_temperature 293
_cell_measurement_theta_max 25.00
_cell_measurement_theta_min 20.00
_cell_volume 3545.6(6)
_computing_data_reduction 'NRCVAX DATRD2'
_computing_molecular_graphics NRCVAX
_computing_publication_material 'NRCVAX TABLES Jan 94 Version'
_computing_structure_refinement 'NRCVAX LSTSQ'
_computing_structure_solution 'NRCVAX SOLVER'
_diffrn_ambient_temperature 293
_diffrn_measurement_device 'SMART 1000'
_diffrn_measurement_method CCD
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Molybdenum K\a'
_diffrn_radiation_wavelength 0.70930
_diffrn_reflns_av_R_equivalents 0.025
_diffrn_reflns_limit_h_max 16
_diffrn_reflns_limit_h_min -3
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -3
_diffrn_reflns_limit_l_max 28
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_number 17454
_diffrn_reflns_theta_max 27.44
_diffrn_reflns_theta_min 0.00
_diffrn_source 'xray tube'
_diffrn_source_type 'Bruker SMART 1000'
_exptl_absorpt_coefficient_mu 15.70
_exptl_absorpt_correction_type empirical
_exptl_absorpt_process_details SADABS
_exptl_crystal_colour 'pale yellow'
_exptl_crystal_density_diffrn 2.814
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description 'irregular block'
_exptl_crystal_F_000 2754.72
_exptl_crystal_size_max 0.18
_exptl_crystal_size_mid 0.05
_exptl_crystal_size_min 0.03
_refine_diff_density_max 0.53
_refine_diff_density_min -0.39
_refine_ls_abs_structure_Flack -.016(83)
_refine_ls_extinction_coef 922(137)
_refine_ls_extinction_method Larson
_refine_ls_goodness_of_fit_obs 0.98
_refine_ls_matrix_type full
_refine_ls_number_parameters 115
_refine_ls_number_reflns 880
_refine_ls_R_factor_all 0.019
_refine_ls_R_factor_obs 0.019
_refine_ls_shift/esd_max 0.000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details 'calc w=1/(\s^2^(F)+0.0003F^2^)'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_all 0.027
_refine_ls_wR_factor_obs 0.027
_reflns_number_observed 1726
_reflns_number_total 2031
_reflns_observed_criterion 'Inet > 2.0\s(Inet)'
_cod_data_source_file ic048276lsi20050307_015625_2.cif
_cod_data_source_block hydgese
_cod_original_cell_volume 3545.6(5)
_cod_original_formula_sum 'N8 H20 Ge2 Se6'
_cod_database_code 1100973
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2+x,1/2+y,1/2+z
-y,1/2+x,1/4+z
1/2-y,x,3/4+z
1/2-x,1/2-y,1/2+z
-x,-y,z
1/2+y,-x,3/4+z
y,1/2-x,1/4+z
-x,y,1/2+z
1/2-x,1/2+y,z
y,1/2+x,3/4+z
1/2+y,x,1/4+z
1/2+x,1/2-y,z
x,-y,1/2+z
1/2-y,-x,1/4+z
-y,1/2-x,3/4+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_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
_atom_site_aniso_type_symbol
Se1 0.02346(23) 0.0315(3) 0.0240(3) 0.00061(19) 0.0011(8) 0.0014(7) Se
Se2 0.0446(6) 0.0294(6) 0.0252(7) -0.0006(3) -0.0020(10) -0.0046(6) Se
Ge1 0.0263(11) 0.0235(11) 0.0212(13) 0.0016(3) 0.00000 0.00000 Ge
Se3 0.0423(7) 0.0323(7) 0.0287(8) 0.0018(3) 0.0003(8) -0.0098(6) Se
Ge2 0.0321(12) 0.0257(11) 0.0139(12) 0.0000(3) 0.00000 0.00000 Ge
N1 0.038(3) 0.036(3) 0.047(4) 0.0018(22) -0.002(5) -0.002(4) N
N3 0.046(3) 0.043(3) 0.053(4) -0.0045(25) 0.011(6) 0.002(4) N
N2 0.044(3) 0.034(3) 0.037(3) -0.0005(23) -0.006(4) 0.004(3) N
N4 0.041(4) 0.032(3) 0.059(4) -0.003(3) 0.003(3) -0.002(3) N
loop_
_atom_site_label
_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_calc_flag
_atom_site_refinement_flags
_atom_site_type_symbol
Se1 0.35986(4) 0.00673(5) 0.13547 0.0263(5) Uani . . Se
Se2 0.49018(8) -0.15314(11) 0.00474(13) 0.0330(6) Uani . . Se
Ge1 0.50000 0.00000 0.20966(22) 0.0236(11) Uani . S Ge
Se3 0.50708(7) 0.15495(13) 0.26500(13) 0.0345(7) Uani . . Se
Ge2 0.50000 0.00000 0.06067(21) 0.0239(12) Uani . S Ge
N1 0.3919(4) 0.7259(4) 0.1332(7) 0.040(3) Uani . . N
N3 0.8493(4) 0.2061(5) 0.1356(7) 0.047(4) Uani . . N
N2 0.4430(5) 0.6242(4) 0.1372(6) 0.038(3) Uani . . N
N4 0.8055(5) 0.2306(6) 0.0772(5) 0.044(4) Uani . . N
H1 0.727(7) 0.269(7) 0.086(4) 0.07(3) Uiso . . H
H2 0.415(8) 0.581(8) 0.167(5) 0.09(3) Uiso . . H
H3 0.804(9) 0.154(9) 0.151(6) 0.16(5) Uiso . . H
H4 0.421(7) 0.587(7) 0.105(4) 0.07(3) Uiso . . H
H5 0.394(8) 0.753(7) 0.166(4) 0.08(4) Uiso . . H
H6 0.856(6) 0.274(7) 0.152(4) 0.07(3) Uiso . . H
H7 0.851(7) 0.272(8) 0.062(4) 0.07(3) Uiso . . H
H8 0.431(6) 0.760(5) 0.099(3) 0.054(22) Uiso . . H
H9 0.800(5) 0.177(6) 0.060(3) 0.040(22) Uiso . . H
H10 0.526(11) 0.646(11) 0.161(7) 0.18(7) Uiso . . H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
N ? 0.006 0.003 'International Tables Vol. IV Table 2.2B'
H ? 0.000 0.000 'International Tables Vol. IV Table 2.2B'
Ge ? 0.155 1.800 'International Tables Vol. IV Table 2.2B'
Se ? -0.093 2.226 'International Tables Vol. IV Table 2.2B'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
Ge1 Se1 Ge2 85.06(12)
Se1 Ge1 Se1a 95.17(17)
Se1 Ge1 Se3 110.64(5)
Se1 Ge1 Se3a 110.82(5)
Se1a Ge1 Se3 110.82(5)
Se1a Ge1 Se3a 110.64(5)
Se3 Ge1 Se3a 116.71(22)
Se1 Ge2 Se1a 94.71(16)
Se1 Ge2 Se2 110.55(5)
Se1 Ge2 Se2a 111.78(5)
Se1a Ge2 Se2 111.78(5)
Se1a Ge2 Se2a 110.55(5)
Se2 Ge2 Se2a 115.60(21)
N2 N1 H5 108(7)
N2 N1 H8 102(4)
H5 N1 H8 118(8)
N4 N3 H3 103(8)
N4 N3 H6 100(5)
H3 N3 H6 124(9)
N1 N2 H2 113(6)
N1 N2 H4 106(6)
N1 N2 H10 102(7)
H2 N2 H4 97(8)
H2 N2 H10 99(9)
H4 N2 H10 137(9)
N3 N4 H1 105(5)
N3 N4 H7 102(6)
N3 N4 H9 106(5)
H1 N4 H7 113(7)
H1 N4 H9 112(7)
H7 N4 H9 114(8)
N2 H2 H4 40(6)
N2 H4 H2 41(6)
N1 H5 H8 34(5)
N4 H7 H9 31(5)
N1 H8 H5 27(4)
N4 H9 H7 34(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Se1 Ge1 2.415(3)
Se1 Ge2 2.424(3)
Se2 Ge2 2.305(3)
Ge1 Se1a 2.415(3)
Ge1 Se3 2.316(3)
Ge1 Se3a 2.316(3)
Ge2 Se1a 2.424(3)
Ge2 Se2a 2.305(3)
N1 N2 1.450(7)
N1 H5 0.80(9)
N1 H8 1.01(8)
N3 N4 1.433(17)
N3 H3 0.94(13)
N3 H6 0.94(9)
N2 H2 0.93(11)
N2 H4 0.90(9)
N2 H10 1.21(13)
N4 H1 1.12(9)
N4 H7 0.85(10)
N4 H9 0.79(7)
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
? ? ? ? ? ?
|
1100974.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100974.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_1100974
loop_
_publ_author_name
'Ruili Sang'
'Li Xu'
_publ_contact_author_address
;
Fujian Institute of Research on the Structure of Matter,
Chinese Academy of Sciences, Fuzhou, Fujian, 350002, China
;
_publ_contact_author_email ' xuli65@hotmail.com '
_publ_contact_author_fax ' (86)591-83705045 '
_publ_contact_author_name ' Li Xu'
_publ_contact_author_phone ' (86)591-83705045 '
_publ_section_title
;
A Series of Single, Double, and Triple Me2biim-Bridged Dinuclear,
Trinuclear, and Polymeric Complexes: Syntheses, Crystal Structures, and
Luminescent Properties
;
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3731
_journal_page_last 3737
_journal_paper_doi 10.1021/ic048280x
_journal_volume 44
_journal_year 2005
_chemical_formula_sum 'C8 H12 Cl4 N4 Zn'
_chemical_formula_weight 371.39
_chemical_name_common '[ZnCl4][H2Me2biim]'
_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 117.899(3)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 15.816(3)
_cell_length_b 8.9899(17)
_cell_length_c 11.474(2)
_cell_measurement_reflns_used 1202
_cell_measurement_temperature 273(2)
_cell_volume 1441.8(5)
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 273(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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 0.0379
_diffrn_reflns_av_sigmaI/netI 0.0486
_diffrn_reflns_limit_h_max 18
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min -5
_diffrn_reflns_limit_l_max 9
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_number 2179
_diffrn_reflns_theta_full 25.04
_diffrn_reflns_theta_max 25.04
_diffrn_reflns_theta_min 2.69
_exptl_absorpt_coefficient_mu 2.428
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_correction_T_min 0.6891
_exptl_absorpt_correction_type SADABS
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.711
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 744
_exptl_crystal_size_max 0.35
_exptl_crystal_size_mid 0.20
_exptl_crystal_size_min 0.10
_refine_diff_density_max 0.458
_refine_diff_density_min -0.569
_refine_diff_density_rms 0.124
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.633
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 78
_refine_ls_number_reflns 1268
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.633
_refine_ls_R_factor_all 0.0813
_refine_ls_R_factor_gt 0.0613
_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^)+(0.0460P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1299
_refine_ls_wR_factor_ref 0.1384
_reflns_number_gt 1030
_reflns_number_total 1268
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file ic048280xsi20041208_095610_1.cif
_cod_data_source_block '[ZnCl4][H2Me2biim]'
_cod_database_code 1100974
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
Zn Zn 0.5000 0.35216(10) 0.7500 0.0296(3) Uani 1 2 d S . .
Cl1 Cl 0.60069(11) 0.49552(17) 0.92496(15) 0.0443(5) Uani 1 1 d . . .
Cl2 Cl 0.41400(11) 0.2104(2) 0.81893(15) 0.0464(5) Uani 1 1 d . . .
N1 N 0.4387(3) 0.7449(6) 0.8450(5) 0.0391(12) Uani 1 1 d . . .
N2 N 0.3729(3) 0.8743(5) 0.6648(4) 0.0274(10) Uani 1 1 d . . .
C1 C 0.4546(3) 0.8119(6) 0.7526(5) 0.0277(12) Uani 1 1 d . . .
C2 C 0.3442(4) 0.7631(7) 0.8139(6) 0.0415(15) Uani 1 1 d . . .
H2 H 0.3139 0.7269 0.8607 0.050 Uiso 1 1 calc R . .
C3 C 0.3039(4) 0.8445(7) 0.7014(6) 0.0378(14) Uani 1 1 d . . .
H3 H 0.2404 0.8747 0.6569 0.045 Uiso 1 1 calc R . .
C4 C 0.3596(4) 0.9653(7) 0.5505(6) 0.0424(16) Uani 1 1 d . . .
H4C H 0.4184 0.9689 0.5455 0.064 Uiso 1 1 calc R . .
H4B H 0.3411 1.0643 0.5605 0.064 Uiso 1 1 calc R . .
H4A H 0.3105 0.9219 0.4712 0.064 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
Zn 0.0271(5) 0.0347(6) 0.0276(5) 0.000 0.0133(4) 0.000
Cl1 0.0374(8) 0.0436(9) 0.0342(8) -0.0039(7) 0.0022(7) -0.0003(7)
Cl2 0.0499(10) 0.0539(11) 0.0501(10) -0.0022(8) 0.0356(8) -0.0091(8)
N1 0.033(3) 0.046(3) 0.039(3) 0.006(2) 0.018(2) 0.000(2)
N2 0.026(2) 0.030(3) 0.028(2) 0.001(2) 0.013(2) 0.0006(19)
C1 0.017(3) 0.029(3) 0.032(3) -0.001(2) 0.008(2) -0.005(2)
C2 0.034(3) 0.045(4) 0.047(4) 0.005(3) 0.020(3) 0.000(3)
C3 0.027(3) 0.048(4) 0.038(3) 0.000(3) 0.016(3) -0.001(3)
C4 0.039(3) 0.054(4) 0.040(3) 0.013(3) 0.024(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'
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
Cl2 Zn Cl2 111.35(10) 2_656 . ?
Cl2 Zn Cl1 109.81(6) 2_656 . ?
Cl2 Zn Cl1 107.24(6) . . ?
Cl2 Zn Cl1 107.24(6) 2_656 2_656 ?
Cl2 Zn Cl1 109.81(6) . 2_656 ?
Cl1 Zn Cl1 111.43(9) . 2_656 ?
C1 N1 C2 109.0(5) . . ?
C1 N2 C3 108.5(5) . . ?
C1 N2 C4 126.1(5) . . ?
C3 N2 C4 125.4(5) . . ?
N2 C1 N1 108.1(4) . . ?
N2 C1 C1 126.3(6) . 2_656 ?
N1 C1 C1 125.6(5) . 2_656 ?
C3 C2 N1 106.3(5) . . ?
C2 C3 N2 108.1(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
Zn Cl2 2.2597(16) 2_656 ?
Zn Cl2 2.2597(16) . ?
Zn Cl1 2.2881(16) . ?
Zn Cl1 2.2881(15) 2_656 ?
N1 C1 1.342(7) . ?
N1 C2 1.374(8) . ?
N2 C1 1.335(7) . ?
N2 C3 1.367(7) . ?
N2 C4 1.475(7) . ?
C1 C1 1.463(10) 2_656 ?
C2 C3 1.355(8) . ?
|
1100975.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100975.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_1100975
loop_
_publ_author_name
'Ruili Sang'
'Li Xu'
_publ_section_title
;
A Series of Single, Double, and Triple Me2biim-Bridged Dinuclear,
Trinuclear, and Polymeric Complexes: Syntheses, Crystal Structures, and
Luminescent Properties
;
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3731
_journal_page_last 3737
_journal_paper_doi 10.1021/ic048280x
_journal_volume 44
_journal_year 2005
_chemical_formula_sum 'C16 H20 Cl4 N8 Zn2'
_chemical_formula_weight 596.94
_chemical_name_common '[Zn2Cl4(Me2biim)2]'
_space_group_IT_number 60
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall '-P 2n 2ab'
_symmetry_space_group_name_H-M 'P b c n'
_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 90.00
_cell_formula_units_Z 4
_cell_length_a 11.747(3)
_cell_length_b 13.566(4)
_cell_length_c 14.367(4)
_cell_measurement_reflns_used 4804
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 27.4835
_cell_measurement_theta_min 3.0043
_cell_volume 2289.5(11)
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 293(2)
_diffrn_measured_fraction_theta_full 0.999
_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 0.0375
_diffrn_reflns_av_sigmaI/netI 0.0213
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_number 16589
_diffrn_reflns_theta_full 27.48
_diffrn_reflns_theta_max 27.48
_diffrn_reflns_theta_min 3.00
_exptl_absorpt_coefficient_mu 2.583
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_correction_T_min 0.7696
_exptl_absorpt_correction_type multi-scan
_exptl_crystal_colour blue
_exptl_crystal_density_diffrn 1.732
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 1200
_exptl_crystal_size_max 0.20
_exptl_crystal_size_mid 0.20
_exptl_crystal_size_min 0.20
_refine_diff_density_max 0.899
_refine_diff_density_min -0.517
_refine_diff_density_rms 0.088
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.137
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 136
_refine_ls_number_reflns 2628
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.137
_refine_ls_R_factor_all 0.0453
_refine_ls_R_factor_gt 0.0414
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1409
_refine_ls_wR_factor_ref 0.1452
_reflns_number_gt 2479
_reflns_number_total 2628
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file ic048280xsi20041208_095610_2.cif
_cod_data_source_block '[Zn2Cl4(Me2biim)2](2)'
_cod_database_code 1100975
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn Zn 0.70612(3) 0.14367(3) 0.26112(3) 0.01592(17) Uani 1 1 d . . .
Cl1 Cl 0.81157(7) 0.22266(6) 0.15533(6) 0.0291(2) Uani 1 1 d . . .
Cl2 Cl 0.79637(6) 0.06033(6) 0.37429(6) 0.0263(2) Uani 1 1 d . . .
N1 N 0.6069(2) 0.24222(19) 0.32896(17) 0.0167(5) Uani 1 1 d . . .
N2 N 0.4852(2) 0.35913(19) 0.3655(2) 0.0194(6) Uani 1 1 d . . .
N3 N 0.61317(19) 0.04948(18) 0.18255(18) 0.0165(5) Uani 1 1 d . . .
N4 N 0.5085(2) -0.07612(19) 0.13540(17) 0.0170(5) Uani 1 1 d . . .
C1 C 0.5232(2) 0.2996(2) 0.29783(19) 0.0156(6) Uani 1 1 d . . .
C2 C 0.6225(2) 0.2674(2) 0.4209(2) 0.0180(6) Uani 1 1 d . . .
H2A H 0.6759 0.2393 0.4607 0.022 Uiso 1 1 calc R . .
C3 C 0.5476(3) 0.3396(2) 0.4444(2) 0.0197(6) Uani 1 1 d . . .
H3A H 0.5400 0.3698 0.5021 0.024 Uiso 1 1 calc R . .
C4 C 0.3974(3) 0.4348(3) 0.3571(3) 0.0317(8) Uani 1 1 d . . .
H4A H 0.3669 0.4343 0.2951 0.047 Uiso 1 1 calc R . .
H4B H 0.4300 0.4983 0.3699 0.047 Uiso 1 1 calc R . .
H4C H 0.3375 0.4217 0.4009 0.047 Uiso 1 1 calc R . .
C5 C 0.5302(2) -0.0129(2) 0.20517(19) 0.0162(6) Uani 1 1 d . . .
C6 C 0.5819(3) -0.0537(2) 0.0642(2) 0.0202(6) Uani 1 1 d . . .
H6A H 0.5873 -0.0856 0.0070 0.024 Uiso 1 1 calc R . .
C7 C 0.6453(2) 0.0244(2) 0.09347(19) 0.0178(6) Uani 1 1 d . . .
H7A H 0.7014 0.0559 0.0588 0.021 Uiso 1 1 calc R . .
C8 C 0.4213(3) -0.1534(2) 0.1342(2) 0.0259(7) Uani 1 1 d . . .
H8A H 0.3817 -0.1539 0.1926 0.039 Uiso 1 1 calc R . .
H8B H 0.4569 -0.2162 0.1243 0.039 Uiso 1 1 calc R . .
H8C H 0.3683 -0.1406 0.0848 0.039 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
Zn 0.0158(2) 0.0184(3) 0.0136(3) 0.00036(13) 0.00134(11) 0.00019(12)
Cl1 0.0359(5) 0.0317(5) 0.0198(4) -0.0006(3) 0.0093(3) -0.0133(3)
Cl2 0.0273(4) 0.0312(5) 0.0204(4) 0.0038(3) -0.0023(3) 0.0093(3)
N1 0.0196(11) 0.0176(12) 0.0130(11) 0.0000(9) -0.0004(9) 0.0004(10)
N2 0.0198(12) 0.0223(14) 0.0161(13) -0.0032(9) -0.0018(10) 0.0034(10)
N3 0.0148(11) 0.0191(12) 0.0155(12) -0.0004(9) 0.0007(9) 0.0024(9)
N4 0.0157(12) 0.0182(13) 0.0170(12) -0.0004(10) -0.0026(9) 0.0020(9)
C1 0.0163(12) 0.0166(14) 0.0139(14) 0.0009(11) 0.0013(11) -0.0028(11)
C2 0.0227(14) 0.0182(14) 0.0132(13) 0.0010(11) -0.0036(11) -0.0027(11)
C3 0.0236(15) 0.0222(15) 0.0133(14) -0.0030(11) -0.0027(11) -0.0006(12)
C4 0.0345(19) 0.0348(19) 0.0257(17) -0.0089(14) -0.0053(14) 0.0157(15)
C5 0.0147(12) 0.0181(14) 0.0158(14) -0.0006(11) -0.0006(11) 0.0030(11)
C6 0.0221(14) 0.0237(16) 0.0149(14) -0.0037(12) -0.0015(12) 0.0064(12)
C7 0.0152(12) 0.0219(15) 0.0164(14) 0.0007(11) 0.0020(10) 0.0044(11)
C8 0.0296(17) 0.0251(16) 0.0231(17) -0.0049(13) -0.0005(14) -0.0071(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'
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
N1 Zn N3 112.02(10) . . ?
N1 Zn Cl1 109.27(8) . . ?
N3 Zn Cl1 102.85(8) . . ?
N1 Zn Cl2 104.81(7) . . ?
N3 Zn Cl2 109.90(8) . . ?
Cl1 Zn Cl2 118.17(4) . . ?
C1 N1 C2 106.0(2) . . ?
C1 N1 Zn 130.5(2) . . ?
C2 N1 Zn 123.32(19) . . ?
C1 N2 C3 107.7(3) . . ?
C1 N2 C4 126.8(3) . . ?
C3 N2 C4 125.4(3) . . ?
C5 N3 C7 105.7(2) . . ?
C5 N3 Zn 131.3(2) . . ?
C7 N3 Zn 121.77(19) . . ?
C5 N4 C6 107.2(2) . . ?
C5 N4 C8 126.7(2) . . ?
C6 N4 C8 126.1(3) . . ?
N1 C1 N2 110.8(2) . . ?
N1 C1 C1 125.7(3) . 3_655 ?
N2 C1 C1 123.5(3) . 3_655 ?
C3 C2 N1 109.3(3) . . ?
C2 C3 N2 106.2(3) . . ?
N3 C5 N4 111.3(2) . . ?
N3 C5 C5 124.6(2) . 3_655 ?
N4 C5 C5 124.2(2) . 3_655 ?
C7 C6 N4 106.6(3) . . ?
C6 C7 N3 109.3(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
Zn N1 2.024(2) . ?
Zn N3 2.025(3) . ?
Zn Cl1 2.2344(9) . ?
Zn Cl2 2.2463(9) . ?
N1 C1 1.332(4) . ?
N1 C2 1.376(4) . ?
N2 C1 1.340(4) . ?
N2 C3 1.375(4) . ?
N2 C4 1.460(4) . ?
N3 C5 1.330(4) . ?
N3 C7 1.377(4) . ?
N4 C5 1.344(4) . ?
N4 C6 1.373(4) . ?
N4 C8 1.465(4) . ?
C1 C1 1.478(5) 3_655 ?
C2 C3 1.360(4) . ?
C5 C5 1.471(5) 3_655 ?
C6 C7 1.361(4) . ?
|
1100976.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100976.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_1100976
loop_
_publ_author_name
'Ruili Sang'
'Li Xu'
_publ_section_title
;
A Series of Single, Double, and Triple Me2biim-Bridged Dinuclear,
Trinuclear, and Polymeric Complexes: Syntheses, Crystal Structures, and
Luminescent Properties
;
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3731
_journal_page_last 3737
_journal_paper_doi 10.1021/ic048280x
_journal_volume 44
_journal_year 2005
_chemical_formula_moiety '[CdCl2(C8N4H10)]n'
_chemical_formula_sum 'C8 H10 Cd Cl2 N4'
_chemical_formula_weight 345.50
_space_group_IT_number 7
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall 'P -2yac'
_symmetry_space_group_name_H-M 'P 1 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 97.240(3)
_cell_angle_gamma 90.00
_cell_formula_units_Z 2
_cell_length_a 8.5217(12)
_cell_length_b 5.1528(8)
_cell_length_c 13.719(2)
_cell_measurement_reflns_used 1236
_cell_measurement_temperature 273(2)
_cell_volume 597.61(15)
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 273(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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 0.0287
_diffrn_reflns_av_sigmaI/netI 0.0328
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -4
_diffrn_reflns_limit_k_max 6
_diffrn_reflns_limit_k_min -5
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_number 1769
_diffrn_reflns_theta_full 25.07
_diffrn_reflns_theta_max 25.07
_diffrn_reflns_theta_min 2.67
_exptl_absorpt_coefficient_mu 2.247
_exptl_absorpt_correction_T_max 1.000
_exptl_absorpt_correction_T_min 0.744
_exptl_absorpt_correction_type SADABS
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.920
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 336
_exptl_crystal_size_max 0.30
_exptl_crystal_size_mid 0.26
_exptl_crystal_size_min 0.12
_refine_diff_density_max 0.886
_refine_diff_density_min -0.889
_refine_diff_density_rms 0.154
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack 0.14(12)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.136
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 136
_refine_ls_number_reflns 1285
_refine_ls_number_restraints 2
_refine_ls_restrained_S_all 1.135
_refine_ls_R_factor_all 0.0513
_refine_ls_R_factor_gt 0.0443
_refine_ls_shift/su_max 3.214
_refine_ls_shift/su_mean 0.179
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1243
_refine_ls_wR_factor_ref 0.1358
_reflns_number_gt 1125
_reflns_number_total 1285
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file ic048280xsi20041208_095610_3.cif
_cod_data_source_block '[CdCl2(N,N'-Dimethylbiimidazole]n(3)'
_cod_original_cell_volume 597.59(15)
_cod_database_code 1100976
loop_
_symmetry_equiv_pos_as_xyz
'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
Cd1 Cd -0.0057(3) -0.49785(12) -0.5886(2) 0.0397(3) Uani 1 1 d . . .
Cl1 Cl 0.2464(4) -0.2848(7) -0.5640(2) 0.0643(9) Uani 1 1 d . . .
Cl2 Cl -0.1219(4) -0.7050(6) -0.4584(2) 0.0626(9) Uani 1 1 d . . .
N1 N 0.0214(10) -0.7505(15) -0.7183(7) 0.038(2) Uani 1 1 d . . .
N2 N -0.0109(17) -1.0280(15) -0.8410(9) 0.042(3) Uani 1 1 d . . .
N3 N -0.2051(11) -0.2320(14) -0.6523(7) 0.039(2) Uani 1 1 d . . .
N4 N -0.3537(15) 0.0450(19) -0.7423(9) 0.044(3) Uani 1 1 d . . .
C1 C -0.0682(16) -0.943(2) -0.7594(10) 0.039(3) Uani 1 1 d . . .
C2 C 0.1190(16) -0.879(3) -0.8529(10) 0.055(3) Uani 1 1 d . . .
H2A H 0.1812 -0.8913 -0.9038 0.066 Uiso 1 1 calc R . .
C3 C 0.1382(14) -0.718(2) -0.7792(9) 0.048(3) Uani 1 1 d . . .
H3A H 0.2196 -0.5974 -0.7687 0.057 Uiso 1 1 calc R . .
C4 C -0.083(2) -1.226(2) -0.9098(9) 0.059(4) Uani 1 1 d . . .
H4A H -0.1730 -1.3010 -0.8843 0.088 Uiso 1 1 calc R . .
H4B H -0.0072 -1.3595 -0.9176 0.088 Uiso 1 1 calc R . .
H4C H -0.1170 -1.1474 -0.9723 0.088 Uiso 1 1 calc R . .
C5 C -0.2068(16) -0.0465(19) -0.7186(8) 0.035(2) Uani 1 1 d . . .
C6 C -0.3577(16) -0.257(2) -0.6313(8) 0.053(3) Uani 1 1 d . . .
H6A H -0.3919 -0.3718 -0.5861 0.064 Uiso 1 1 calc R . .
C7 C -0.4505(16) -0.085(3) -0.6881(11) 0.055(3) Uani 1 1 d . . .
H7A H -0.5590 -0.0622 -0.6894 0.067 Uiso 1 1 calc R . .
C8 C -0.4080(18) 0.244(2) -0.8147(11) 0.057(3) Uani 1 1 d . . .
H8A H -0.3191 0.3128 -0.8427 0.085 Uiso 1 1 calc R . .
H8B H -0.4592 0.3808 -0.7833 0.085 Uiso 1 1 calc R . .
H8C H -0.4815 0.1684 -0.8657 0.085 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
Cd1 0.0321(4) 0.0513(5) 0.0359(4) 0.0032(3) 0.0049(3) -0.0075(3)
Cl1 0.0425(19) 0.085(2) 0.0650(19) 0.0005(18) 0.0047(16) -0.0254(17)
Cl2 0.064(2) 0.075(2) 0.0515(17) 0.0119(15) 0.0180(16) -0.0221(19)
N1 0.020(5) 0.047(5) 0.048(5) -0.002(4) 0.007(4) 0.001(4)
N2 0.047(7) 0.043(5) 0.040(6) -0.006(4) 0.020(5) 0.005(4)
N3 0.033(5) 0.038(4) 0.043(5) 0.004(4) 0.002(4) 0.002(4)
N4 0.035(6) 0.052(6) 0.046(6) 0.007(4) 0.011(5) 0.001(4)
C1 0.040(7) 0.041(5) 0.039(6) 0.007(5) 0.013(5) 0.005(5)
C2 0.042(8) 0.076(8) 0.053(7) 0.012(8) 0.025(6) 0.011(7)
C3 0.032(6) 0.054(6) 0.060(7) 0.008(6) 0.018(5) 0.004(5)
C4 0.080(11) 0.048(7) 0.048(7) -0.001(5) 0.011(7) 0.007(6)
C5 0.037(7) 0.038(5) 0.029(5) 0.001(4) 0.000(5) -0.006(4)
C6 0.057(9) 0.066(8) 0.038(6) 0.002(5) 0.012(6) -0.019(6)
C7 0.030(7) 0.075(8) 0.065(8) 0.007(8) 0.021(6) 0.006(7)
C8 0.051(8) 0.043(7) 0.072(9) 0.015(5) -0.010(7) 0.008(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'
Cd Cd -0.8075 1.2024 '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 Cd1 N3 101.1(3) . . ?
N1 Cd1 Cl1 101.4(3) . . ?
N3 Cd1 Cl1 113.1(2) . . ?
N1 Cd1 Cl2 115.2(2) . . ?
N3 Cd1 Cl2 101.3(3) . . ?
Cl1 Cd1 Cl2 123.01(17) . . ?
C1 N1 C3 104.5(9) . . ?
C1 N1 Cd1 131.1(8) . . ?
C3 N1 Cd1 124.2(7) . . ?
C1 N2 C2 107.4(11) . . ?
C1 N2 C4 126.2(13) . . ?
C2 N2 C4 126.1(12) . . ?
C5 N3 C6 106.6(10) . . ?
C5 N3 Cd1 130.2(8) . . ?
C6 N3 Cd1 123.0(7) . . ?
C5 N4 C7 107.9(10) . . ?
C5 N4 C8 128.2(12) . . ?
C7 N4 C8 123.9(12) . . ?
N1 C1 N2 110.2(11) . . ?
N1 C1 C5 123.7(11) . 1_545 ?
N2 C1 C5 126.2(11) . 1_545 ?
C3 C2 N2 106.7(11) . . ?
C2 C3 N1 111.2(10) . . ?
N3 C5 N4 110.6(11) . . ?
N3 C5 C1 126.0(11) . 1_565 ?
N4 C5 C1 123.4(10) . 1_565 ?
C7 C6 N3 108.4(10) . . ?
N4 C7 C6 106.6(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
Cd1 N1 2.240(9) . ?
Cd1 N3 2.270(9) . ?
Cd1 Cl1 2.398(4) . ?
Cd1 Cl2 2.400(4) . ?
N1 C1 1.332(16) . ?
N1 C3 1.388(13) . ?
N2 C1 1.349(18) . ?
N2 C2 1.373(19) . ?
N2 C4 1.473(17) . ?
N3 C5 1.318(14) . ?
N3 C6 1.373(16) . ?
N4 C5 1.339(19) . ?
N4 C7 1.356(19) . ?
N4 C8 1.461(15) . ?
C1 C5 1.469(19) 1_545 ?
C2 C3 1.303(19) . ?
C5 C1 1.469(19) 1_565 ?
C6 C7 1.36(2) . ?
|
1100977.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100977.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_1100977
loop_
_publ_author_name
'Ruili Sang'
'Li Xu'
_publ_section_title
;
A Series of Single, Double, and Triple Me2biim-Bridged Dinuclear,
Trinuclear, and Polymeric Complexes: Syntheses, Crystal Structures, and
Luminescent Properties
;
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3731
_journal_page_last 3737
_journal_paper_doi 10.1021/ic048280x
_journal_volume 44
_journal_year 2005
_chemical_formula_sum 'C8 H10 Br2 Cd N4 O0'
_chemical_formula_weight 434.42
_chemical_name_common '[CdBr2(N,N'-dimethylbiimidazole)]n'
_space_group_IT_number 43
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall 'F 2 -2d'
_symmetry_space_group_name_H-M 'F d d 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 90.00
_cell_formula_units_Z 8
_cell_length_a 30.503(5)
_cell_length_b 4.8598(9)
_cell_length_c 16.322(3)
_cell_measurement_reflns_used 1807
_cell_measurement_temperature 273(2)
_cell_volume 2419.5(7)
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 273(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_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 0.0390
_diffrn_reflns_av_sigmaI/netI 0.0316
_diffrn_reflns_limit_h_max 33
_diffrn_reflns_limit_h_min -36
_diffrn_reflns_limit_k_max 5
_diffrn_reflns_limit_k_min -5
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_number 2879
_diffrn_reflns_theta_full 25.03
_diffrn_reflns_theta_max 25.03
_diffrn_reflns_theta_min 2.67
_exptl_absorpt_coefficient_mu 8.384
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_correction_T_min 0.3983
_exptl_absorpt_correction_type SADABS
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 2.385
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 1632
_exptl_crystal_size_max 0.30
_exptl_crystal_size_mid 0.16
_exptl_crystal_size_min 0.12
_refine_diff_density_max 2.614
_refine_diff_density_min -1.329
_refine_diff_density_rms 0.271
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack -0.07(4)
_refine_ls_extinction_coef 0.0010(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 1.512
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 70
_refine_ls_number_reflns 962
_refine_ls_number_restraints 1
_refine_ls_restrained_S_all 1.511
_refine_ls_R_factor_all 0.0978
_refine_ls_R_factor_gt 0.0861
_refine_ls_shift/su_max 0.003
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1527P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2436
_refine_ls_wR_factor_ref 0.2717
_reflns_number_gt 788
_reflns_number_total 962
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file ic048280xsi20041208_095610_4.cif
_cod_data_source_block '[CdBr2(N,N'-dimethylbiimidazole)]n'
_cod_original_cell_volume 2419.6(7)
_cod_database_code 1100977
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, 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
Cd Cd 0.5000 0.0000 0.12845(14) 0.0594(8) Uani 1 2 d S . .
Br Br 0.44072(8) 0.2702(3) 0.05554(9) 0.0698(9) Uani 1 1 d . . .
N1 N 0.4633(6) -0.252(3) 0.2211(11) 0.054(4) Uani 1 1 d . . .
N2 N 0.4439(6) -0.554(3) 0.3193(12) 0.055(3) Uani 1 1 d . . .
C1 C 0.4782(6) -0.460(3) 0.2711(14) 0.057(5) Uani 1 1 d . . .
C2 C 0.4031(8) -0.427(5) 0.2960(16) 0.077(6) Uani 1 1 d . . .
H2A H 0.3750 -0.4645 0.3151 0.092 Uiso 1 1 calc R . .
C3 C 0.4159(5) -0.239(4) 0.2390(13) 0.073(7) Uani 1 1 d . . .
H3A H 0.3968 -0.1149 0.2141 0.088 Uiso 1 1 calc R . .
C4 C 0.4487(11) -0.768(5) 0.385(3) 0.107(13) Uani 1 1 d . . .
H4A H 0.4789 -0.8207 0.3890 0.161 Uiso 1 1 calc R . .
H4B H 0.4314 -0.9264 0.3705 0.161 Uiso 1 1 calc R . .
H4C H 0.4388 -0.6948 0.4359 0.161 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
Cd 0.0533(12) 0.0730(14) 0.0520(12) 0.000 0.000 0.0054(7)
Br 0.0631(15) 0.0722(14) 0.0740(17) 0.0066(11) -0.0152(10) 0.0021(6)
N1 0.062(10) 0.060(8) 0.039(9) 0.003(5) 0.022(7) 0.004(6)
N2 0.056(8) 0.052(6) 0.058(9) 0.009(6) -0.007(7) 0.016(6)
C1 0.039(10) 0.058(9) 0.075(13) 0.022(8) -0.015(9) -0.002(7)
C2 0.063(13) 0.105(13) 0.063(13) -0.007(12) 0.030(11) -0.009(11)
C3 0.019(7) 0.15(2) 0.051(11) -0.023(9) 0.031(8) 0.008(8)
C4 0.087(17) 0.094(18) 0.14(3) -0.003(13) 0.09(2) -0.001(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'
Br Br -0.2901 2.4595 '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
N1 Cd N1 95.3(10) 2_655 . ?
N1 Cd Br 104.1(5) 2_655 2_655 ?
N1 Cd Br 112.9(4) . 2_655 ?
N1 Cd Br 112.9(4) 2_655 . ?
N1 Cd Br 104.1(5) . . ?
Br Cd Br 123.92(13) 2_655 . ?
C1 N1 C3 103.8(15) . . ?
C1 N1 Cd 129.5(15) . . ?
C3 N1 Cd 126.7(13) . . ?
C1 N2 C2 111.2(15) . . ?
C1 N2 C4 124.0(16) . . ?
C2 N2 C4 125(2) . . ?
N1 C1 C1 121.4(17) . 2_645 ?
N1 C1 N2 109.2(16) . . ?
C1 C1 N2 129.3(14) 2_645 . ?
C3 C2 N2 102.8(17) . . ?
C2 C3 N1 112.7(18) . . ?
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
Cd N1 2.244(15) 2_655 ?
Cd N1 2.244(15) . ?
Cd Br 2.532(2) 2_655 ?
Cd Br 2.532(2) . ?
N1 C1 1.38(2) . ?
N1 C3 1.48(2) . ?
N2 C1 1.39(3) . ?
N2 C2 1.44(3) . ?
N2 C4 1.50(4) . ?
C1 C1 1.38(4) 2_645 ?
C2 C3 1.36(3) . ?
|
1100978.cif | #------------------------------------------------------------------------------
#$Date: 2017-07-04 18:40:50 +0300 (Tue, 04 Jul 2017) $
#$Revision: 198386 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/09/1100978.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_1100978
loop_
_publ_author_name
'Ruili Sang'
'Li Xu'
_publ_section_title
;
A Series of Single, Double, and Triple Me2biim-Bridged Dinuclear,
Trinuclear, and Polymeric Complexes: Syntheses, Crystal Structures, and
Luminescent Properties
;
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3731
_journal_page_last 3737
_journal_paper_doi 10.1021/ic048280x
_journal_volume 44
_journal_year 2005
_chemical_formula_sum 'C8 H10 Cd I2 N4'
_chemical_formula_weight 528.40
_chemical_name_common '[CdI2(N,N'-dimethylbiimidazole)]n'
_space_group_crystal_system monoclinic
_space_group_IT_number 9
_space_group_name_Hall 'C -2yc'
_space_group_name_H-M_alt 'C 1 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 96.989(3)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 5.3546(12)
_cell_length_b 15.7642(8)
_cell_length_c 15.773(2)
_cell_measurement_reflns_used 892
_cell_measurement_temperature 273(2)
_cell_volume 1321.5(3)
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 273(2)
_diffrn_measured_fraction_theta_full 0.476
_diffrn_measured_fraction_theta_max 0.476
_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 0.0472
_diffrn_reflns_av_sigmaI/netI 0.0629
_diffrn_reflns_limit_h_max 6
_diffrn_reflns_limit_h_min -6
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_limit_l_min -10
_diffrn_reflns_number 1966
_diffrn_reflns_theta_full 25.03
_diffrn_reflns_theta_max 25.03
_diffrn_reflns_theta_min 2.58
_exptl_absorpt_coefficient_mu 6.301
_exptl_absorpt_correction_T_max 1.000
_exptl_absorpt_correction_T_min 0.638
_exptl_absorpt_correction_type SADABS
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 2.656
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 960
_exptl_crystal_size_max 0.34
_exptl_crystal_size_mid 0.06
_exptl_crystal_size_min 0.04
_refine_diff_density_max 0.704
_refine_diff_density_min -0.647
_refine_diff_density_rms 0.152
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack -0.04(19)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.813
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 136
_refine_ls_number_reflns 1294
_refine_ls_number_restraints 2
_refine_ls_restrained_S_all 1.812
_refine_ls_R_factor_all 0.1072
_refine_ls_R_factor_gt 0.0790
_refine_ls_shift/su_max 2.565
_refine_ls_shift/su_mean 0.101
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0374P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1394
_refine_ls_wR_factor_ref 0.1528
_reflns_number_gt 1024
_reflns_number_total 1294
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file ic048280xsi20041208_095610_5.cif
_cod_data_source_block '[CdI2(N,N'-Dimethylbiimidazole]n(5)'
_cod_depositor_comments
;
Changing the space group from 'P -2yc' to 'C -2yc' after consulting the
original publication. All related space group information was changed
accordingly.
Antanas Vaitkus,
2017-07-04
;
_cod_database_code 1100978
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 x,-y,z+1/2
3 x+1/2,y+1/2,z
4 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 -0.3663(12) -0.19740(10) -0.2135(5) 0.0352(5) Uani 1 1 d . . .
I1 I -0.0591(3) -0.1161(3) -0.08836(12) 0.0462(13) Uani 1 1 d . . .
I2 I -0.6610(3) -0.1162(3) -0.33913(13) 0.0468(13) Uani 1 1 d . . .
N1 N -0.094(12) -0.294(3) -0.280(2) 0.10(2) Uani 1 1 d . . .
N2 N 0.169(5) -0.3765(16) -0.3204(15) 0.010(7) Uani 1 1 d . . .
N3 N -0.582(5) -0.2852(19) -0.136(3) 0.048(15) Uani 1 1 d . . .
N4 N -0.852(7) -0.383(3) -0.108(5) 0.11(3) Uani 1 1 d . . .
C1 C 0.085(4) -0.3377(14) -0.2540(17) 0.000(5) Uani 1 1 d . . .
C2 C -0.038(11) -0.350(3) -0.397(2) 0.07(2) Uani 1 1 d . . .
H2A H -0.0377 -0.3670 -0.4535 0.083 Uiso 1 1 calc R . .
C3 C -0.193(5) -0.306(2) -0.371(2) 0.024(9) Uani 1 1 d . . .
H3A H -0.3405 -0.2846 -0.4010 0.029 Uiso 1 1 calc R . .
C4 C 0.359(7) -0.434(2) -0.322(3) 0.040(13) Uani 1 1 d . . .
H4A H 0.4574 -0.4370 -0.2675 0.060 Uiso 1 1 calc R . .
H4B H 0.4640 -0.4178 -0.3647 0.060 Uiso 1 1 calc R . .
H4C H 0.2880 -0.4894 -0.3368 0.060 Uiso 1 1 calc R . .
C5 C -0.77(3) -0.310(3) -0.176(6) 0.66(15) Uani 1 1 d . . .
C6 C -0.724(9) -0.371(2) -0.039(4) 0.049(17) Uani 1 1 d . . .
H6A H -0.7330 -0.3980 0.0132 0.059 Uiso 1 1 calc R . .
C7 C -0.56(2) -0.303(5) -0.057(3) 0.28(9) Uani 1 1 d . . .
H7A H -0.4465 -0.2753 -0.0160 0.340 Uiso 1 1 calc R . .
C8 C -1.080(7) -0.446(3) -0.121(3) 0.052(17) Uani 1 1 d . . .
H8A H -1.0902 -0.4768 -0.0683 0.079 Uiso 1 1 calc R . .
H8B H -1.0572 -0.4858 -0.1653 0.079 Uiso 1 1 calc R . .
H8C H -1.2331 -0.4151 -0.1356 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
Cd1 0.0346(10) 0.0362(9) 0.0343(10) 0.000(3) 0.0023(8) -0.001(3)
I1 0.042(3) 0.054(3) 0.039(3) -0.013(2) -0.007(2) -0.005(2)
I2 0.043(3) 0.049(3) 0.048(3) 0.005(2) 0.003(2) 0.007(2)
N1 0.19(6) 0.09(4) 0.000(16) 0.00(2) -0.01(2) -0.09(4)
N2 0.014(15) 0.017(14) 0.000(10) -0.008(11) 0.000(10) 0.016(12)
N3 0.000(13) 0.006(15) 0.13(4) -0.04(2) -0.021(16) -0.024(11)
N4 0.000(17) 0.08(3) 0.25(7) -0.13(4) -0.01(3) 0.020(18)
C1 0.000(12) 0.000(12) 0.000(12) -0.023(10) -0.002(9) 0.021(9)
C2 0.16(6) 0.03(3) 0.000(17) -0.017(17) -0.06(2) -0.04(3)
C3 0.000(13) 0.036(19) 0.03(2) -0.018(16) -0.023(12) 0.042(14)
C4 0.05(2) 0.003(13) 0.05(2) 0.011(14) -0.040(18) -0.034(16)
C5 1.6(3) 0.02(2) 0.60(16) 0.09(5) 1.0(2) 0.17(7)
C6 0.06(3) 0.015(18) 0.09(4) -0.05(2) 0.06(3) -0.037(19)
C7 0.60(19) 0.25(9) 0.00(2) 0.06(4) 0.03(5) 0.41(13)
C8 0.03(2) 0.09(3) 0.05(2) 0.00(2) 0.05(2) -0.06(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'
Cd Cd -0.8075 1.2024 '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
N3 Cd1 N1 103.0(9) . . ?
N3 Cd1 I2 113.3(9) . . ?
N1 Cd1 I2 108.0(11) . . ?
N3 Cd1 I1 101.5(9) . . ?
N1 Cd1 I1 105.3(11) . . ?
I2 Cd1 I1 123.67(8) . . ?
C1 N1 C3 115(4) . . ?
C1 N1 Cd1 135(3) . . ?
C3 N1 Cd1 110(4) . . ?
C1 N2 C4 130(3) . . ?
C1 N2 C2 102(3) . . ?
C4 N2 C2 127(3) . . ?
C5 N3 C7 116(7) . . ?
C5 N3 Cd1 112(3) . . ?
C7 N3 Cd1 132(7) . . ?
C6 N4 C8 124(7) . . ?
C6 N4 C5 107(7) . . ?
C8 N4 C5 129(7) . . ?
N1 C1 N2 109(3) . . ?
N1 C1 C5 116(4) . 1_655 ?
N2 C1 C5 127(4) . 1_655 ?
C3 C2 N2 110(3) . . ?
C2 C3 N1 103(3) . . ?
N3 C5 C1 153(4) . 1_455 ?
N3 C5 N4 99(8) . . ?
C1 C5 N4 100(7) 1_455 . ?
N4 C6 C7 103(6) . . ?
N3 C7 C6 111(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
Cd1 N3 2.26(4) . ?
Cd1 N1 2.43(6) . ?
Cd1 I2 2.702(7) . ?
Cd1 I1 2.730(7) . ?
N1 C1 1.21(6) . ?
N1 C3 1.49(5) . ?
N2 C1 1.34(3) . ?
N2 C4 1.37(5) . ?
N2 C2 1.59(5) . ?
N3 C5 1.18(18) . ?
N3 C7 1.27(7) . ?
N4 C6 1.24(8) . ?
N4 C8 1.57(6) . ?
N4 C5 1.67(8) . ?
C1 C5 1.44(15) 1_655 ?
C2 C3 1.20(6) . ?
C5 C1 1.44(15) 1_455 ?
C6 C7 1.44(14) . ?
|
1100979.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100979.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_1100979
loop_
_publ_author_name
'Ruili Sang'
'Li Xu'
_publ_section_title
;
A Series of Single, Double, and Triple Me2biim-Bridged Dinuclear,
Trinuclear, and Polymeric Complexes: Syntheses, Crystal Structures, and
Luminescent Properties
;
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3731
_journal_page_last 3737
_journal_paper_doi 10.1021/ic048280x
_journal_volume 44
_journal_year 2005
_chemical_formula_sum 'C24 H36 N16 O15 Zn2'
_chemical_formula_weight 919.43
_chemical_name_common '[Zn2(Me2biim)3][NO3]4'
_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 82.5350(10)
_cell_angle_beta 86.4190(10)
_cell_angle_gamma 68.4430(10)
_cell_formula_units_Z 2
_cell_length_a 9.85700(10)
_cell_length_b 12.1339(3)
_cell_length_c 16.9110(4)
_cell_measurement_reflns_used 3960
_cell_measurement_temperature 273(2)
_cell_volume 1864.96(7)
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 273(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_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 0.0440
_diffrn_reflns_av_sigmaI/netI 0.0641
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -9
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -20
_diffrn_reflns_number 9615
_diffrn_reflns_theta_full 24.99
_diffrn_reflns_theta_max 24.99
_diffrn_reflns_theta_min 1.21
_exptl_absorpt_coefficient_mu 1.375
_exptl_absorpt_correction_T_max 1.000
_exptl_absorpt_correction_T_min 0.170
_exptl_absorpt_correction_type SADABS
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.637
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 944
_exptl_crystal_size_max 0.40
_exptl_crystal_size_mid 0.20
_exptl_crystal_size_min 0.16
_refine_diff_density_max 0.668
_refine_diff_density_min -0.678
_refine_diff_density_rms 0.115
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 2.141
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 514
_refine_ls_number_reflns 6455
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 2.141
_refine_ls_R_factor_all 0.1371
_refine_ls_R_factor_gt 0.0999
_refine_ls_shift/su_max 0.003
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1650
_refine_ls_wR_factor_ref 0.1775
_reflns_number_gt 4846
_reflns_number_total 6455
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file ic048280xsi20041208_095610_6.cif
_cod_data_source_block '[Zn2(Me2biim)3][NO3]4'
_cod_database_code 1100979
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
Zn1 Zn 0.01347(8) 0.68101(7) 0.34571(5) 0.0421(3) Uani 1 1 d . . .
Zn2 Zn 0.22038(8) 0.76933(7) 0.15182(5) 0.0394(3) Uani 1 1 d . . .
O1 O -0.1057(6) 0.6605(5) 0.4387(3) 0.0641(15) Uani 1 1 d . . .
O2 O 0.3605(5) 0.7870(4) 0.0689(3) 0.0532(14) Uani 1 1 d . . .
O11 O 0.4609(6) 0.9587(5) 0.0870(4) 0.0651(16) Uani 1 1 d . . .
O12 O 0.4053(8) 1.1479(6) 0.0771(4) 0.100(2) Uani 1 1 d . . .
O13 O 0.2369(7) 1.0728(7) 0.0934(4) 0.098(2) Uani 1 1 d . . .
O21 O -0.1976(7) 0.4751(6) 0.4650(4) 0.090(2) Uani 1 1 d . . .
O22 O -0.1317(8) 0.2964(6) 0.4311(5) 0.104(2) Uani 1 1 d . . .
O23 O -0.0544(7) 0.4269(7) 0.3640(4) 0.092(2) Uani 1 1 d . . .
O31 O 0.3623(6) 0.7034(6) -0.0678(4) 0.0757(18) Uani 1 1 d . . .
O32 O 0.2656(7) 0.6008(7) -0.1234(4) 0.104(3) Uani 1 1 d . . .
O33 O 0.1529(7) 0.6986(7) -0.0284(4) 0.096(2) Uani 1 1 d . . .
O41 O 0.7614(10) 0.8544(10) 0.5134(6) 0.131(3) Uani 1 1 d . . .
O42 O 0.6695(7) 0.9144(7) 0.3997(5) 0.105(2) Uani 1 1 d . . .
O43 O 0.6539(11) 1.0394(10) 0.4777(8) 0.204(7) Uani 1 1 d . . .
O1W O 0.6239(14) 0.8688(8) 0.6619(7) 0.203(6) Uani 1 1 d . . .
N1 N 0.3658(8) 1.0622(6) 0.0855(4) 0.0591(18) Uani 1 1 d . . .
N2 N -0.1266(8) 0.3979(7) 0.4201(5) 0.0642(19) Uani 1 1 d . . .
N3 N 0.2567(7) 0.6693(6) -0.0741(4) 0.0567(17) Uani 1 1 d . . .
N4 N 0.6881(11) 0.9479(14) 0.4608(7) 0.113(4) Uani 1 1 d . . .
N11 N 0.2173(6) 0.5623(5) 0.3445(3) 0.0433(14) Uani 1 1 d . . .
N12 N 0.4540(6) 0.4773(5) 0.3263(4) 0.0496(16) Uani 1 1 d . . .
N13 N 0.3171(6) 0.7768(5) 0.2525(3) 0.0386(14) Uani 1 1 d . . .
N14 N 0.4056(6) 0.7442(5) 0.3724(3) 0.0427(14) Uani 1 1 d . . .
N21 N 0.0089(6) 0.8494(5) 0.3416(3) 0.0388(14) Uani 1 1 d . . .
N22 N -0.0109(7) 1.0368(5) 0.3101(4) 0.0517(17) Uani 1 1 d . . .
N23 N 0.0153(6) 0.8843(5) 0.1453(3) 0.0390(14) Uani 1 1 d . . .
N24 N -0.2059(6) 1.0016(5) 0.1749(4) 0.0484(16) Uani 1 1 d . . .
N31 N -0.0902(5) 0.6762(5) 0.2486(3) 0.0385(14) Uani 1 1 d . . .
N32 N -0.1540(6) 0.6548(5) 0.1311(4) 0.0435(14) Uani 1 1 d . . .
N33 N 0.2195(6) 0.6043(5) 0.1489(3) 0.0370(13) Uani 1 1 d . . .
N34 N 0.1631(6) 0.4450(4) 0.1507(3) 0.0377(13) Uani 1 1 d . . .
C11 C 0.3404(8) 0.5819(6) 0.3292(4) 0.0437(18) Uani 1 1 d . . .
C12 C 0.2562(9) 0.4400(6) 0.3523(5) 0.054(2) Uani 1 1 d . . .
H12A H 0.1920 0.3997 0.3640 0.065 Uiso 1 1 calc R . .
C13 C 0.4007(9) 0.3881(7) 0.3404(5) 0.061(2) Uani 1 1 d . . .
H13A H 0.4538 0.3067 0.3415 0.073 Uiso 1 1 calc R . .
C14 C 0.6047(8) 0.4623(8) 0.3026(6) 0.076(3) Uani 1 1 d . . .
H14A H 0.6153 0.5385 0.2963 0.115 Uiso 1 1 calc R . .
H14B H 0.6279 0.4284 0.2529 0.115 Uiso 1 1 calc R . .
H14C H 0.6697 0.4101 0.3429 0.115 Uiso 1 1 calc R . .
C15 C 0.3547(7) 0.6989(6) 0.3173(4) 0.0413(17) Uani 1 1 d . . .
C16 C 0.3450(7) 0.8753(7) 0.2686(5) 0.0473(19) Uani 1 1 d . . .
H16A H 0.3293 0.9448 0.2340 0.057 Uiso 1 1 calc R . .
C17 C 0.3986(8) 0.8543(7) 0.3424(5) 0.054(2) Uani 1 1 d . . .
H17A H 0.4257 0.9062 0.3680 0.065 Uiso 1 1 calc R . .
C18 C 0.4538(9) 0.6856(8) 0.4540(5) 0.068(2) Uani 1 1 d . . .
H18A H 0.4501 0.6069 0.4606 0.102 Uiso 1 1 calc R . .
H18B H 0.3905 0.7318 0.4928 0.102 Uiso 1 1 calc R . .
H18C H 0.5520 0.6802 0.4613 0.102 Uiso 1 1 calc R . .
C21 C -0.0240(7) 0.9394(6) 0.2840(4) 0.0417(18) Uani 1 1 d . . .
C22 C 0.0332(9) 1.0055(7) 0.3860(5) 0.058(2) Uani 1 1 d . . .
H22A H 0.0509 1.0547 0.4186 0.069 Uiso 1 1 calc R . .
C23 C 0.0480(7) 0.8892(7) 0.4071(4) 0.0478(19) Uani 1 1 d . . .
H23A H 0.0785 0.8447 0.4561 0.057 Uiso 1 1 calc R . .
C24 C -0.0286(11) 1.1498(7) 0.2621(5) 0.085(3) Uani 1 1 d . . .
H24A H -0.0155 1.2038 0.2950 0.127 Uiso 1 1 calc R . .
H24B H -0.1246 1.1834 0.2401 0.127 Uiso 1 1 calc R . .
H24C H 0.0428 1.1365 0.2196 0.127 Uiso 1 1 calc R . .
C25 C -0.0705(7) 0.9416(6) 0.2030(4) 0.0381(16) Uani 1 1 d . . .
C26 C -0.2068(8) 0.9821(6) 0.0972(5) 0.0507(19) Uani 1 1 d . . .
H26A H -0.2861 1.0128 0.0633 0.061 Uiso 1 1 calc R . .
C27 C -0.0722(7) 0.9105(6) 0.0793(4) 0.0424(17) Uani 1 1 d . . .
H27A H -0.0418 0.8825 0.0301 0.051 Uiso 1 1 calc R . .
C28 C -0.3347(9) 1.0713(8) 0.2204(5) 0.077(3) Uani 1 1 d . . .
H28A H -0.4173 1.1051 0.1861 0.116 Uiso 1 1 calc R . .
H28B H -0.3155 1.1342 0.2410 0.116 Uiso 1 1 calc R . .
H28C H -0.3549 1.0200 0.2639 0.116 Uiso 1 1 calc R . .
C31 C -0.0415(7) 0.6310(6) 0.1809(4) 0.0358(16) Uani 1 1 d . . .
C32 C -0.2394(7) 0.7307(7) 0.2415(5) 0.050(2) Uani 1 1 d . . .
H32A H -0.3030 0.7706 0.2802 0.060 Uiso 1 1 calc R . .
C33 C -0.2779(8) 0.7172(7) 0.1707(5) 0.058(2) Uani 1 1 d . . .
H33A H -0.3724 0.7452 0.1514 0.070 Uiso 1 1 calc R . .
C34 C -0.1440(8) 0.6288(7) 0.0472(4) 0.060(2) Uani 1 1 d . . .
H34A H -0.2403 0.6549 0.0260 0.090 Uiso 1 1 calc R . .
H34B H -0.0965 0.5445 0.0452 0.090 Uiso 1 1 calc R . .
H34C H -0.0887 0.6702 0.0161 0.090 Uiso 1 1 calc R . .
C35 C 0.1123(7) 0.5625(6) 0.1601(4) 0.0341(15) Uani 1 1 d . . .
C36 C 0.3078(7) 0.4124(6) 0.1328(4) 0.0456(18) Uani 1 1 d . . .
H36A H 0.3710 0.3368 0.1230 0.055 Uiso 1 1 calc R . .
C37 C 0.3432(7) 0.5102(6) 0.1320(4) 0.0423(18) Uani 1 1 d . . .
H37A H 0.4356 0.5133 0.1218 0.051 Uiso 1 1 calc R . .
C38 C 0.0832(8) 0.3625(6) 0.1686(5) 0.057(2) Uani 1 1 d . . .
H38A H -0.0175 0.4072 0.1795 0.086 Uiso 1 1 calc R . .
H38B H 0.1249 0.3069 0.2143 0.086 Uiso 1 1 calc R . .
H38C H 0.0904 0.3198 0.1235 0.086 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 0.0415(5) 0.0387(5) 0.0457(5) -0.0096(4) 0.0070(4) -0.0139(4)
Zn2 0.0388(5) 0.0347(5) 0.0468(5) -0.0098(4) 0.0050(4) -0.0150(4)
O1 0.072(4) 0.067(4) 0.061(4) -0.013(3) 0.024(3) -0.036(3)
O2 0.060(3) 0.057(3) 0.056(3) -0.019(3) 0.024(3) -0.036(3)
O11 0.058(3) 0.039(3) 0.095(5) -0.005(3) -0.001(3) -0.015(3)
O12 0.129(6) 0.048(4) 0.132(7) -0.023(4) -0.017(5) -0.036(4)
O13 0.054(4) 0.110(6) 0.114(6) -0.031(4) -0.003(4) -0.005(4)
O21 0.096(5) 0.094(5) 0.090(5) -0.035(4) 0.031(4) -0.044(4)
O22 0.134(7) 0.063(5) 0.121(6) 0.005(4) -0.016(5) -0.045(5)
O23 0.092(5) 0.123(6) 0.066(5) -0.009(4) 0.020(4) -0.050(5)
O31 0.069(4) 0.101(5) 0.080(4) -0.035(4) 0.023(3) -0.052(4)
O32 0.095(5) 0.142(7) 0.111(6) -0.079(5) 0.024(4) -0.069(5)
O33 0.061(4) 0.138(6) 0.095(5) -0.045(5) 0.028(4) -0.038(4)
O41 0.107(7) 0.172(10) 0.100(7) -0.044(6) 0.006(5) -0.027(7)
O42 0.081(5) 0.135(7) 0.110(6) -0.053(5) 0.006(4) -0.039(5)
O43 0.178(10) 0.169(10) 0.317(16) -0.199(12) 0.093(10) -0.082(8)
O1W 0.331(15) 0.096(7) 0.191(10) -0.041(7) 0.113(10) -0.099(9)
N1 0.072(5) 0.052(5) 0.051(4) -0.014(3) -0.007(4) -0.017(4)
N2 0.051(4) 0.070(6) 0.069(5) -0.001(4) -0.014(4) -0.018(4)
N3 0.047(4) 0.062(5) 0.058(5) -0.016(4) 0.004(3) -0.013(4)
N4 0.072(7) 0.185(13) 0.101(8) -0.080(9) 0.020(6) -0.050(8)
N11 0.039(3) 0.037(4) 0.050(4) -0.004(3) 0.000(3) -0.010(3)
N12 0.042(4) 0.043(4) 0.062(4) -0.016(3) -0.003(3) -0.009(3)
N13 0.035(3) 0.039(3) 0.046(4) -0.006(3) 0.004(3) -0.018(3)
N14 0.039(3) 0.046(4) 0.046(4) -0.012(3) -0.003(3) -0.015(3)
N21 0.043(3) 0.031(3) 0.039(3) -0.009(3) 0.009(3) -0.008(3)
N22 0.075(5) 0.034(4) 0.051(4) -0.017(3) 0.020(3) -0.025(3)
N23 0.035(3) 0.036(3) 0.048(4) -0.007(3) 0.006(3) -0.016(3)
N24 0.044(4) 0.039(4) 0.046(4) 0.002(3) 0.006(3) 0.001(3)
N31 0.036(3) 0.036(3) 0.044(4) -0.009(3) 0.007(3) -0.015(3)
N32 0.040(3) 0.038(3) 0.053(4) -0.006(3) -0.003(3) -0.013(3)
N33 0.033(3) 0.033(3) 0.045(4) -0.011(3) 0.003(3) -0.010(3)
N34 0.040(3) 0.028(3) 0.048(4) -0.018(3) 0.006(3) -0.013(3)
C11 0.043(4) 0.040(4) 0.045(4) -0.011(3) 0.001(3) -0.010(4)
C12 0.059(5) 0.033(4) 0.064(5) -0.003(4) -0.004(4) -0.010(4)
C13 0.064(6) 0.032(4) 0.079(6) -0.010(4) -0.004(5) -0.007(4)
C14 0.040(5) 0.082(7) 0.104(8) -0.031(6) -0.004(5) -0.011(5)
C15 0.037(4) 0.029(4) 0.057(5) -0.014(4) 0.008(3) -0.009(3)
C16 0.051(5) 0.052(5) 0.054(5) -0.019(4) 0.013(4) -0.035(4)
C17 0.055(5) 0.063(6) 0.060(5) -0.028(4) 0.006(4) -0.033(4)
C18 0.071(6) 0.081(7) 0.054(5) -0.021(5) -0.017(4) -0.024(5)
C21 0.037(4) 0.033(4) 0.056(5) -0.014(4) 0.018(3) -0.014(3)
C22 0.070(6) 0.056(5) 0.056(6) -0.027(4) 0.022(4) -0.030(5)
C23 0.052(5) 0.046(5) 0.041(4) -0.019(4) 0.007(3) -0.009(4)
C24 0.147(9) 0.038(5) 0.073(7) -0.009(4) 0.026(6) -0.041(6)
C25 0.039(4) 0.028(4) 0.047(4) -0.008(3) 0.008(3) -0.012(3)
C26 0.041(4) 0.047(5) 0.055(5) 0.003(4) -0.006(4) -0.007(4)
C27 0.041(4) 0.042(4) 0.043(4) -0.005(3) -0.002(3) -0.014(4)
C28 0.054(5) 0.077(7) 0.076(7) -0.013(5) 0.015(5) 0.004(5)
C31 0.037(4) 0.035(4) 0.043(4) -0.009(3) 0.004(3) -0.021(3)
C32 0.036(4) 0.052(5) 0.063(5) -0.015(4) 0.014(4) -0.017(4)
C33 0.026(4) 0.061(5) 0.083(6) -0.009(5) -0.004(4) -0.010(4)
C34 0.063(5) 0.066(6) 0.055(5) -0.017(4) -0.005(4) -0.024(5)
C35 0.038(4) 0.029(4) 0.034(4) -0.010(3) 0.003(3) -0.009(3)
C36 0.037(4) 0.041(4) 0.054(5) -0.015(4) 0.003(3) -0.006(4)
C37 0.028(4) 0.046(5) 0.054(5) -0.016(4) 0.005(3) -0.012(3)
C38 0.066(5) 0.037(4) 0.080(6) -0.016(4) 0.013(4) -0.030(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'
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
O1 Zn1 N11 115.8(2) . . ?
O1 Zn1 N31 107.7(2) . . ?
N11 Zn1 N31 109.5(2) . . ?
O1 Zn1 N21 105.1(2) . . ?
N11 Zn1 N21 111.8(2) . . ?
N31 Zn1 N21 106.5(2) . . ?
O2 Zn2 N23 118.9(2) . . ?
O2 Zn2 N33 105.2(2) . . ?
N23 Zn2 N33 108.3(2) . . ?
O2 Zn2 N13 102.2(2) . . ?
N23 Zn2 N13 111.5(2) . . ?
N33 Zn2 N13 110.4(2) . . ?
O12 N1 O13 122.7(8) . . ?
O12 N1 O11 118.9(8) . . ?
O13 N1 O11 118.3(7) . . ?
O22 N2 O23 121.4(8) . . ?
O22 N2 O21 120.3(8) . . ?
O23 N2 O21 118.2(8) . . ?
O33 N3 O32 121.0(7) . . ?
O33 N3 O31 119.8(7) . . ?
O32 N3 O31 119.0(7) . . ?
O43 N4 O42 129.8(17) . . ?
O43 N4 O41 119.6(13) . . ?
O42 N4 O41 110.6(13) . . ?
C11 N11 C12 105.6(6) . . ?
C11 N11 Zn1 128.6(5) . . ?
C12 N11 Zn1 125.5(5) . . ?
C11 N12 C13 107.7(6) . . ?
C11 N12 C14 126.6(7) . . ?
C13 N12 C14 125.3(7) . . ?
C15 N13 C16 105.8(6) . . ?
C15 N13 Zn2 129.8(5) . . ?
C16 N13 Zn2 124.1(5) . . ?
C17 N14 C15 108.2(6) . . ?
C17 N14 C18 125.6(6) . . ?
C15 N14 C18 126.1(6) . . ?
C21 N21 C23 106.7(6) . . ?
C21 N21 Zn1 132.1(5) . . ?
C23 N21 Zn1 121.2(5) . . ?
C22 N22 C21 107.2(6) . . ?
C22 N22 C24 126.4(7) . . ?
C21 N22 C24 126.1(7) . . ?
C25 N23 C27 106.0(6) . . ?
C25 N23 Zn2 128.8(5) . . ?
C27 N23 Zn2 124.8(4) . . ?
C25 N24 C26 108.3(6) . . ?
C25 N24 C28 126.6(7) . . ?
C26 N24 C28 125.1(7) . . ?
C31 N31 C32 106.1(6) . . ?
C31 N31 Zn1 131.8(4) . . ?
C32 N31 Zn1 122.0(5) . . ?
C31 N32 C33 106.7(6) . . ?
C31 N32 C34 126.9(6) . . ?
C33 N32 C34 126.2(6) . . ?
C35 N33 C37 106.7(5) . . ?
C35 N33 Zn2 131.1(4) . . ?
C37 N33 Zn2 122.2(4) . . ?
C35 N34 C36 107.3(5) . . ?
C35 N34 C38 126.6(5) . . ?
C36 N34 C38 125.5(6) . . ?
N11 C11 N12 110.3(6) . . ?
N11 C11 C15 125.8(6) . . ?
N12 C11 C15 123.9(6) . . ?
C13 C12 N11 109.7(7) . . ?
C12 C13 N12 106.7(7) . . ?
N13 C15 N14 109.9(6) . . ?
N13 C15 C11 125.8(7) . . ?
N14 C15 C11 124.3(7) . . ?
C17 C16 N13 108.9(7) . . ?
C16 C17 N14 107.1(6) . . ?
N21 C21 N22 110.3(7) . . ?
N21 C21 C25 127.5(6) . . ?
N22 C21 C25 122.1(6) . . ?
N22 C22 C23 108.4(7) . . ?
C22 C23 N21 107.3(7) . . ?
N23 C25 N24 109.3(6) . . ?
N23 C25 C21 125.3(6) . . ?
N24 C25 C21 125.4(6) . . ?
C27 C26 N24 106.8(7) . . ?
C26 C27 N23 109.5(6) . . ?
N31 C31 N32 110.2(6) . . ?
N31 C31 C35 126.6(6) . . ?
N32 C31 C35 123.2(6) . . ?
C33 C32 N31 109.3(6) . . ?
C32 C33 N32 107.7(6) . . ?
N33 C35 N34 110.0(5) . . ?
N33 C35 C31 126.4(6) . . ?
N34 C35 C31 123.6(6) . . ?
C37 C36 N34 107.4(6) . . ?
C36 C37 N33 108.5(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
Zn1 O1 1.948(5) . ?
Zn1 N11 1.997(5) . ?
Zn1 N31 2.005(5) . ?
Zn1 N21 2.019(5) . ?
Zn2 O2 1.954(4) . ?
Zn2 N23 1.990(5) . ?
Zn2 N33 2.013(5) . ?
Zn2 N13 2.031(6) . ?
O11 N1 1.259(8) . ?
O12 N1 1.227(8) . ?
O13 N1 1.230(8) . ?
O21 N2 1.257(9) . ?
O22 N2 1.240(9) . ?
O23 N2 1.242(8) . ?
O31 N3 1.267(8) . ?
O32 N3 1.230(8) . ?
O33 N3 1.215(7) . ?
O41 N4 1.348(14) . ?
O42 N4 1.206(10) . ?
O43 N4 1.105(13) . ?
N11 C11 1.324(8) . ?
N11 C12 1.380(9) . ?
N12 C11 1.354(8) . ?
N12 C13 1.357(9) . ?
N12 C14 1.465(9) . ?
N13 C15 1.324(9) . ?
N13 C16 1.384(8) . ?
N14 C17 1.345(9) . ?
N14 C15 1.347(8) . ?
N14 C18 1.488(9) . ?
N21 C21 1.323(9) . ?
N21 C23 1.391(8) . ?
N22 C22 1.342(10) . ?
N22 C21 1.364(8) . ?
N22 C24 1.457(9) . ?
N23 C25 1.338(8) . ?
N23 C27 1.384(8) . ?
N24 C25 1.347(8) . ?
N24 C26 1.366(9) . ?
N24 C28 1.476(8) . ?
N31 C31 1.320(8) . ?
N31 C32 1.379(8) . ?
N32 C31 1.357(8) . ?
N32 C33 1.365(8) . ?
N32 C34 1.483(9) . ?
N33 C35 1.324(8) . ?
N33 C37 1.374(8) . ?
N34 C35 1.355(7) . ?
N34 C36 1.358(8) . ?
N34 C38 1.478(8) . ?
C11 C15 1.464(9) . ?
C12 C13 1.343(10) . ?
C16 C17 1.342(10) . ?
C21 C25 1.466(10) . ?
C22 C23 1.366(10) . ?
C26 C27 1.333(9) . ?
C31 C35 1.482(9) . ?
C32 C33 1.325(10) . ?
C36 C37 1.352(9) . ?
|
1100980.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100980.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_1100980
loop_
_publ_author_name
'Ruili Sang'
'Li Xu'
_publ_section_title
;
A Series of Single, Double, and Triple Me2biim-Bridged Dinuclear,
Trinuclear, and Polymeric Complexes: Syntheses, Crystal Structures, and
Luminescent Properties
;
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3731
_journal_page_last 3737
_journal_paper_doi 10.1021/ic048280x
_journal_volume 44
_journal_year 2005
_chemical_formula_sum 'C64 H86 Cd3 Cl6 N32 O27'
_chemical_formula_weight 2285.55
_chemical_name_common '[Cd3(Mebiim)8][ClO4]12'
_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 77.647(5)
_cell_angle_beta 79.185(5)
_cell_angle_gamma 86.666(7)
_cell_formula_units_Z 2
_cell_length_a 13.681(3)
_cell_length_b 15.381(4)
_cell_length_c 21.740(5)
_cell_measurement_reflns_used 7473
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 27.4835
_cell_measurement_theta_min 3.0132
_cell_volume 4388.6(18)
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 293(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_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 0.0260
_diffrn_reflns_av_sigmaI/netI 0.0561
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_k_max 19
_diffrn_reflns_limit_k_min -19
_diffrn_reflns_limit_l_max 25
_diffrn_reflns_limit_l_min -28
_diffrn_reflns_number 33173
_diffrn_reflns_theta_full 27.48
_diffrn_reflns_theta_max 27.48
_diffrn_reflns_theta_min 3.06
_exptl_absorpt_coefficient_mu 0.998
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_correction_T_min 0.8035
_exptl_absorpt_correction_type multi-scan
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.730
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 2312
_exptl_crystal_size_max 0.25
_exptl_crystal_size_mid 0.20
_exptl_crystal_size_min 0.10
_refine_diff_density_max 1.889
_refine_diff_density_min -1.731
_refine_diff_density_rms 0.124
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.231
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 1237
_refine_ls_number_reflns 19394
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.231
_refine_ls_R_factor_all 0.0799
_refine_ls_R_factor_gt 0.0632
_refine_ls_shift/su_max 0.060
_refine_ls_shift/su_mean 0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0900P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1599
_refine_ls_wR_factor_ref 0.1725
_reflns_number_gt 15535
_reflns_number_total 19394
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file ic048280xsi20041208_095610_7.cif
_cod_data_source_block '[Cd3(Mebiim)8][ClO4]12(7)'
_cod_original_cell_volume 4388.3(19)
_cod_database_code 1100980
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
Cd1 Cd 0.5000 1.0000 0.0000 0.02048(10) Uani 1 2 d S . .
Cd2 Cd 0.66264(3) 0.70362(2) 0.02253(2) 0.03915(12) Uani 1 1 d . . .
Cd3 Cd 0.89318(2) 0.28802(2) 0.384290(16) 0.02688(10) Uani 1 1 d . . .
Cd4 Cd 1.0000 0.5000 0.5000 0.02243(11) Uani 1 2 d S . .
Cl1 Cl 0.75889(11) 0.56386(10) -0.10148(9) 0.0575(4) Uani 1 1 d . . .
Cl2 Cl 1.36673(9) 0.22497(7) 0.59969(6) 0.0327(2) Uani 1 1 d . . .
Cl3 Cl 0.46163(9) 0.47856(9) 0.32113(6) 0.0398(3) Uani 1 1 d . . .
Cl4 Cl 0.08026(10) 0.82486(9) 0.21452(7) 0.0484(4) Uani 1 1 d . . .
Cl5 Cl 0.87792(14) 0.15534(12) 0.11340(12) 0.0753(6) Uani 1 1 d . . .
Cl6 Cl 0.3604(3) 1.04741(16) 0.3644(2) 0.1523(18) Uani 1 1 d . . .
O1 O 0.9130(4) 0.2867(3) 0.2689(2) 0.0638(13) Uani 1 1 d . . .
O2 O 1.3775(3) 0.3046(2) 0.6214(2) 0.0510(10) Uani 1 1 d . . .
O3 O 1.2656(3) 0.2180(3) 0.59146(19) 0.0467(9) Uani 1 1 d . . .
O4 O 1.4308(3) 0.2247(3) 0.5399(2) 0.0589(12) Uani 1 1 d . . .
O5 O 1.3875(4) 0.1507(3) 0.6479(3) 0.0690(15) Uani 1 1 d . . .
O6 O 0.5175(4) 0.5528(3) 0.2826(2) 0.0655(14) Uani 1 1 d . . .
O7 O 0.3987(8) 0.4920(6) 0.3775(4) 0.095(3) Uani 0.70 1 d P . .
O7B O 0.3697(8) 0.5076(12) 0.3278(8) 0.059(5) Uani 0.30 1 d P . .
O8 O 0.5245(5) 0.4057(5) 0.3301(4) 0.066(2) Uani 0.70 1 d P . .
O8B O 0.4703(14) 0.3951(10) 0.3037(8) 0.062(4) Uani 0.30 1 d P . .
O9 O 0.3906(5) 0.4574(6) 0.2804(4) 0.073(2) Uani 0.70 1 d P . .
O9B O 0.4975(11) 0.4658(11) 0.3843(6) 0.054(4) Uani 0.30 1 d P . .
O11 O 0.6833(4) 0.6155(3) -0.0700(3) 0.0686(14) Uani 1 1 d . . .
O12 O 0.7161(4) 0.5148(4) -0.1370(3) 0.0867(18) Uani 1 1 d . . .
O13 O 0.8040(4) 0.5042(4) -0.0549(4) 0.0909(19) Uani 1 1 d . . .
O14 O 0.8330(5) 0.6215(4) -0.1433(3) 0.099(2) Uani 1 1 d . . .
O10 O 0.1017(5) 0.7369(5) 0.2341(6) 0.139(4) Uani 1 1 d . . .
O15 O 0.1225(7) 0.8491(7) 0.2690(4) 0.148(4) Uani 1 1 d . . .
O16 O -0.0158(5) 0.8559(4) 0.2329(3) 0.108(2) Uani 1 1 d . . .
O17 O 0.1406(6) 0.8741(4) 0.1615(3) 0.104(2) Uani 1 1 d . . .
O18 O 0.8841(15) 0.0662(6) 0.1300(6) 0.240(8) Uani 1 1 d . . .
O19 O 0.7815(6) 0.1723(14) 0.1192(6) 0.243(8) Uani 1 1 d . . .
O20 O 0.9296(5) 0.1897(9) 0.0581(5) 0.202(6) Uani 1 1 d . . .
O21 O 0.9198(6) 0.1806(8) 0.1605(6) 0.180(5) Uani 1 1 d . . .
O22 O 0.4025(8) 0.9968(7) 0.4098(4) 0.159(4) Uani 1 1 d . . .
O23 O 0.2574(9) 1.0578(9) 0.3722(7) 0.206(6) Uani 1 1 d . . .
O24 O 0.3793(10) 0.9731(8) 0.3167(5) 0.190(5) Uani 1 1 d . . .
O25 O 0.3911(17) 1.1230(12) 0.3357(19) 0.32(2) Uani 0.60 1 d P . .
O1W O 0.5516(5) 0.2461(5) 0.2778(3) 0.098(2) Uani 1 1 d . . .
O2W O 0.7498(11) 0.1840(8) 0.2519(7) 0.092(4) Uani 0.50 1 d P . .
O3W O 0.7443(8) 0.2798(8) 0.2232(5) 0.068(3) Uani 0.50 1 d P . .
O4W O 0.0349(16) 0.7737(14) 0.1739(11) 0.176(11) Uani 0.50 1 d P . .
N1 N 0.6306(3) 0.5616(3) 0.0795(3) 0.0458(12) Uani 1 1 d . . .
N2 N 0.6721(4) 0.4477(3) 0.1507(2) 0.0473(12) Uani 1 1 d . . .
N3 N 0.8199(3) 0.6366(3) 0.0534(3) 0.0488(12) Uani 1 1 d . . .
N4 N 0.8937(3) 0.5090(3) 0.0884(2) 0.0414(10) Uani 1 1 d . . .
N5 N 0.2655(3) 1.1920(3) 0.0596(2) 0.0451(12) Uani 1 1 d . . .
N6 N 0.2365(3) 1.0980(4) 0.1529(3) 0.0510(13) Uani 1 1 d . . .
N7 N 0.4868(3) 1.0970(3) 0.07538(17) 0.0266(8) Uani 1 1 d . . .
N8 N 0.4487(4) 1.1813(3) 0.1478(2) 0.0464(12) Uani 1 1 d . . .
N9 N 0.4962(3) 0.7093(3) 0.0115(2) 0.0332(9) Uani 1 1 d . . .
N10 N 0.3314(3) 0.7128(3) 0.0299(2) 0.0352(9) Uani 1 1 d . . .
N11 N 0.4445(3) 0.8786(2) 0.08371(17) 0.0269(8) Uani 1 1 d . . .
N12 N 0.3801(3) 0.7618(3) 0.15517(19) 0.0355(10) Uani 1 1 d . . .
N13 N 0.6441(3) 0.7653(3) 0.1108(2) 0.0363(10) Uani 1 1 d . . .
N14 N 0.6623(5) 0.8520(3) 0.1765(3) 0.0617(17) Uani 1 1 d . . .
N15 N 0.6678(3) 0.9674(2) 0.0161(2) 0.0306(9) Uani 1 1 d . . .
N16 N 0.8135(4) 0.9281(3) 0.0456(3) 0.0585(16) Uani 1 1 d . . .
N17 N 0.7378(3) 0.2206(3) 0.3854(3) 0.0421(11) Uani 1 1 d . . .
N18 N 0.6647(3) 0.0895(3) 0.4172(3) 0.0445(11) Uani 1 1 d . . .
N19 N 0.9298(3) 0.1303(3) 0.3825(2) 0.0390(10) Uani 1 1 d . . .
N20 N 0.8777(3) 0.0352(2) 0.3332(2) 0.0296(8) Uani 1 1 d . . .
N21 N 0.8398(3) 0.2590(3) 0.4929(2) 0.0308(8) Uani 1 1 d . . .
N22 N 0.7558(3) 0.2612(3) 0.5900(2) 0.0417(10) Uani 1 1 d . . .
N23 N 1.1662(3) 0.5271(2) 0.50576(17) 0.0264(8) Uani 1 1 d . . .
N24 N 1.3224(3) 0.5656(3) 0.4973(2) 0.0357(9) Uani 1 1 d . . .
N25 N 0.8423(3) 0.4319(3) 0.3534(2) 0.0296(8) Uani 1 1 d . . .
N26 N 0.8334(3) 0.5768(2) 0.31479(19) 0.0272(8) Uani 1 1 d . . .
N27 N 1.0446(3) 0.5069(2) 0.38719(17) 0.0234(7) Uani 1 1 d . . .
N28 N 1.0650(3) 0.5246(2) 0.28190(18) 0.0267(8) Uani 1 1 d . . .
N29 N 1.0608(3) 0.3023(3) 0.37315(19) 0.0280(8) Uani 1 1 d . . .
N30 N 1.2131(3) 0.2943(3) 0.3950(2) 0.0354(9) Uani 1 1 d . . .
N31 N 1.0325(3) 0.3423(2) 0.52137(18) 0.0269(8) Uani 1 1 d . . .
N32 N 1.0717(3) 0.1992(3) 0.5272(2) 0.0338(9) Uani 1 1 d . . .
C1 C 0.7043(4) 0.5194(3) 0.1043(3) 0.0361(11) Uani 1 1 d . . .
C2 C 0.5693(5) 0.4469(4) 0.1546(3) 0.0464(14) Uani 1 1 d . . .
H22A H 0.5256 0.4056 0.1821 0.056 Uiso 1 1 calc R . .
C3 C 0.5453(4) 0.5173(3) 0.1112(3) 0.0467(14) Uani 1 1 d . . .
H23A H 0.4813 0.5334 0.1038 0.056 Uiso 1 1 calc R . .
C4 C 0.7181(10) 0.3952(9) 0.1969(6) 0.131(5) Uani 1 1 d . . .
H24A H 0.7885 0.4050 0.1863 0.196 Uiso 1 1 calc R . .
H24B H 0.7057 0.3337 0.1991 0.196 Uiso 1 1 calc R . .
H24C H 0.6923 0.4102 0.2376 0.196 Uiso 1 1 calc R . .
C5 C 0.8052(4) 0.5531(3) 0.0834(3) 0.0383(11) Uani 1 1 d . . .
C6 C 0.9211(4) 0.6465(4) 0.0405(4) 0.0574(18) Uani 1 1 d . . .
H18A H 0.9536 0.6993 0.0206 0.069 Uiso 1 1 calc R . .
C7 C 0.9669(4) 0.5679(4) 0.0610(3) 0.0503(15) Uani 1 1 d . . .
H19A H 1.0351 0.5567 0.0570 0.060 Uiso 1 1 calc R . .
C8 C 0.9090(6) 0.4129(5) 0.1076(5) 0.082(3) Uani 1 1 d . . .
H20A H 0.8460 0.3852 0.1253 0.123 Uiso 1 1 calc R . .
H20B H 0.9513 0.4010 0.1392 0.123 Uiso 1 1 calc R . .
H20C H 0.9399 0.3895 0.0710 0.123 Uiso 1 1 calc R . .
C9 C 0.3076(4) 1.1405(4) 0.1046(3) 0.0373(11) Uani 1 1 d . . .
C10 C 0.1466(4) 1.1224(5) 0.1362(4) 0.067(2) Uani 1 1 d . . .
H30A H 0.0848 1.1031 0.1596 0.080 Uiso 1 1 calc R . .
C11 C 0.1637(4) 1.1793(5) 0.0798(4) 0.068(2) Uani 1 1 d . . .
H11B H 0.1148 1.2065 0.0573 0.081 Uiso 1 1 calc R . .
C12 C 0.2507(5) 1.0376(5) 0.2112(3) 0.0551(16) Uani 1 1 d . . .
H32A H 0.1872 1.0174 0.2357 0.083 Uiso 1 1 calc R . .
H32B H 0.2837 1.0677 0.2357 0.083 Uiso 1 1 calc R . .
H32C H 0.2907 0.9875 0.2010 0.083 Uiso 1 1 calc R . .
C13 C 0.4128(4) 1.1383(3) 0.1085(2) 0.0308(10) Uani 1 1 d . . .
C14 C 0.5491(5) 1.1680(4) 0.1396(3) 0.0480(14) Uani 1 1 d . . .
H26A H 0.5931 1.1895 0.1604 0.058 Uiso 1 1 calc R . .
C15 C 0.5723(4) 1.1160(3) 0.0941(2) 0.0340(10) Uani 1 1 d . . .
H27A H 0.6361 1.0968 0.0785 0.041 Uiso 1 1 calc R . .
C16 C 0.3873(6) 1.2352(6) 0.1904(4) 0.072(2) Uani 1 1 d . . .
H28A H 0.3186 1.2333 0.1866 0.109 Uiso 1 1 calc R . .
H28B H 0.4090 1.2957 0.1781 0.109 Uiso 1 1 calc R . .
H28C H 0.3945 1.2114 0.2339 0.109 Uiso 1 1 calc R . .
C17 C 0.4154(3) 0.7420(3) 0.0432(2) 0.0285(9) Uani 1 1 d . . .
C18 C 0.4619(4) 0.6554(4) -0.0236(3) 0.0462(14) Uani 1 1 d . . .
H10A H 0.5022 0.6229 -0.0504 0.055 Uiso 1 1 calc R . .
C19 C 0.3620(4) 0.6572(4) -0.0130(3) 0.0459(14) Uani 1 1 d . . .
H11A H 0.3213 0.6272 -0.0309 0.055 Uiso 1 1 calc R . .
C20 C 0.2280(4) 0.7335(4) 0.0549(3) 0.0448(13) Uani 1 1 d . . .
H12A H 0.2260 0.7744 0.0828 0.067 Uiso 1 1 calc R . .
H12B H 0.1950 0.6798 0.0782 0.067 Uiso 1 1 calc R . .
H12C H 0.1949 0.7600 0.0200 0.067 Uiso 1 1 calc R . .
C21 C 0.4127(3) 0.7960(3) 0.0917(2) 0.0234(8) Uani 1 1 d . . .
C22 C 0.4318(4) 0.8966(3) 0.1441(2) 0.0357(11) Uani 1 1 d . . .
H15A H 0.4475 0.9499 0.1534 0.043 Uiso 1 1 calc R . .
C23 C 0.3929(5) 0.8250(4) 0.1879(2) 0.0439(13) Uani 1 1 d . . .
H14A H 0.3778 0.8199 0.2321 0.053 Uiso 1 1 calc R . .
C24 C 0.3429(4) 0.6714(3) 0.1848(3) 0.0445(13) Uani 1 1 d . . .
H16A H 0.3388 0.6396 0.1519 0.067 Uiso 1 1 calc R . .
H16B H 0.2781 0.6755 0.2103 0.067 Uiso 1 1 calc R . .
H16C H 0.3877 0.6403 0.2115 0.067 Uiso 1 1 calc R . .
C25 C 0.6697(4) 0.8460(3) 0.1148(3) 0.0388(12) Uani 1 1 d . . .
C26 C 0.6265(6) 0.7723(4) 0.2137(3) 0.0614(19) Uani 1 1 d . . .
H2A H 0.6124 0.7574 0.2582 0.074 Uiso 1 1 calc R . .
C27 C 0.6160(4) 0.7202(4) 0.1729(3) 0.0470(14) Uani 1 1 d . . .
H3A H 0.5931 0.6622 0.1850 0.056 Uiso 1 1 calc R . .
C28 C 0.6791(11) 0.9307(6) 0.2006(4) 0.131(6) Uani 1 1 d . . .
H4A H 0.7015 0.9784 0.1652 0.196 Uiso 1 1 calc R . .
H4B H 0.7286 0.9169 0.2273 0.196 Uiso 1 1 calc R . .
H4C H 0.6180 0.9482 0.2250 0.196 Uiso 1 1 calc R . .
C29 C 0.7143(4) 0.9145(3) 0.0594(3) 0.0399(13) Uani 1 1 d . . .
C30 C 0.7421(4) 1.0144(3) -0.0268(3) 0.0411(13) Uani 1 1 d . . .
H7A H 0.7327 1.0564 -0.0630 0.049 Uiso 1 1 calc R . .
C31 C 0.8304(4) 0.9916(4) -0.0093(4) 0.0588(19) Uani 1 1 d . . .
H6A H 0.8917 1.0148 -0.0306 0.071 Uiso 1 1 calc R . .
C32 C 0.8905(6) 0.8810(5) 0.0803(5) 0.091(3) Uani 1 1 d . . .
H8A H 0.9548 0.9038 0.0593 0.136 Uiso 1 1 calc R . .
H8B H 0.8895 0.8185 0.0807 0.136 Uiso 1 1 calc R . .
H8C H 0.8774 0.8899 0.1235 0.136 Uiso 1 1 calc R . .
C33 C 0.7506(4) 0.1326(3) 0.3895(3) 0.0378(12) Uani 1 1 d . . .
C34 C 0.5948(5) 0.1521(4) 0.4327(4) 0.0546(16) Uani 1 1 d . . .
H34A H 0.5290 0.1420 0.4528 0.066 Uiso 1 1 calc R . .
C35 C 0.6405(4) 0.2324(4) 0.4130(3) 0.0496(15) Uani 1 1 d . . .
H35A H 0.6102 0.2869 0.4177 0.060 Uiso 1 1 calc R . .
C36 C 0.6468(5) -0.0057(4) 0.4357(3) 0.0547(16) Uani 1 1 d . . .
H36A H 0.7053 -0.0377 0.4202 0.082 Uiso 1 1 calc R . .
H36B H 0.5921 -0.0193 0.4177 0.082 Uiso 1 1 calc R . .
H36C H 0.6310 -0.0229 0.4815 0.082 Uiso 1 1 calc R . .
C37 C 0.8498(4) 0.0964(3) 0.3690(2) 0.0328(10) Uani 1 1 d . . .
C38 C 1.0109(4) 0.0892(3) 0.3521(3) 0.0360(11) Uani 1 1 d . . .
H38A H 1.0769 0.1010 0.3519 0.043 Uiso 1 1 calc R . .
C39 C 0.9811(4) 0.0295(3) 0.3228(3) 0.0346(11) Uani 1 1 d . . .
H39A H 1.0215 -0.0081 0.3001 0.042 Uiso 1 1 calc R . .
C40 C 0.8147(4) -0.0117(4) 0.3033(3) 0.0426(13) Uani 1 1 d . . .
H40A H 0.7459 0.0013 0.3182 0.064 Uiso 1 1 calc R . .
H40B H 0.8271 -0.0746 0.3145 0.064 Uiso 1 1 calc R . .
H40C H 0.8301 0.0078 0.2576 0.064 Uiso 1 1 calc R . .
C41 C 0.7931(3) 0.3109(3) 0.5310(2) 0.0322(10) Uani 1 1 d . . .
C42 C 0.7803(5) 0.1739(4) 0.5879(3) 0.0501(15) Uani 1 1 d . . .
H42A H 0.7640 0.1248 0.6211 0.060 Uiso 1 1 calc R . .
C43 C 0.8320(4) 0.1723(3) 0.5291(3) 0.0402(12) Uani 1 1 d . . .
H43A H 0.8583 0.1215 0.5149 0.048 Uiso 1 1 calc R . .
C44 C 0.7014(5) 0.2941(5) 0.6449(3) 0.0557(16) Uani 1 1 d . . .
H44A H 0.6845 0.2449 0.6803 0.084 Uiso 1 1 calc R . .
H44B H 0.6416 0.3243 0.6341 0.084 Uiso 1 1 calc R . .
H44C H 0.7420 0.3346 0.6564 0.084 Uiso 1 1 calc R . .
C45 C 1.2297(3) 0.5940(3) 0.4886(2) 0.0268(9) Uani 1 1 d . . .
C46 C 1.3191(4) 0.4761(3) 0.5218(3) 0.0365(11) Uani 1 1 d . . .
H62A H 1.3718 0.4387 0.5327 0.044 Uiso 1 1 calc R . .
C47 C 1.2232(3) 0.4527(3) 0.5268(2) 0.0311(10) Uani 1 1 d . . .
H63A H 1.1992 0.3953 0.5421 0.037 Uiso 1 1 calc R . .
C48 C 1.4131(4) 0.6173(4) 0.4824(3) 0.0423(13) Uani 1 1 d . . .
H64A H 1.4680 0.5789 0.4931 0.063 Uiso 1 1 calc R . .
H64B H 1.4048 0.6633 0.5067 0.063 Uiso 1 1 calc R . .
H64C H 1.4261 0.6437 0.4375 0.063 Uiso 1 1 calc R . .
C49 C 0.8913(3) 0.5072(3) 0.3378(2) 0.0236(8) Uani 1 1 d . . .
C50 C 0.7485(4) 0.4542(3) 0.3395(3) 0.0361(11) Uani 1 1 d . . .
H55A H 0.6971 0.4145 0.3457 0.043 Uiso 1 1 calc R . .
C51 C 0.7429(4) 0.5427(3) 0.3155(3) 0.0342(11) Uani 1 1 d . . .
H54A H 0.6881 0.5744 0.3020 0.041 Uiso 1 1 calc R . .
C52 C 0.8604(4) 0.6708(3) 0.2943(3) 0.0332(10) Uani 1 1 d . . .
H56A H 0.9281 0.6771 0.2984 0.050 Uiso 1 1 calc R . .
H56B H 0.8173 0.7052 0.3206 0.050 Uiso 1 1 calc R . .
H56C H 0.8534 0.6917 0.2504 0.050 Uiso 1 1 calc R . .
C53 C 0.9983(3) 0.5147(3) 0.3374(2) 0.0234(8) Uani 1 1 d . . .
C54 C 1.1449(3) 0.5113(3) 0.3611(2) 0.0289(10) Uani 1 1 d . . .
H59A H 1.1960 0.5071 0.3844 0.035 Uiso 1 1 calc R . .
C55 C 1.1577(3) 0.5225(3) 0.2965(2) 0.0282(9) Uani 1 1 d . . .
H55 H 1.2178 0.5277 0.2678 0.034 Uiso 1 1 calc R . .
C56 C 1.0411(4) 0.5330(4) 0.2176(2) 0.0377(11) Uani 1 1 d . . .
H60A H 0.9701 0.5341 0.2205 0.057 Uiso 1 1 calc R . .
H60B H 1.0694 0.4832 0.1999 0.057 Uiso 1 1 calc R . .
H60C H 1.0681 0.5872 0.1905 0.057 Uiso 1 1 calc R . .
C57 C 1.1149(4) 0.2948(3) 0.4199(2) 0.0281(9) Uani 1 1 d . . .
C58 C 1.1289(4) 0.3080(3) 0.3175(2) 0.0328(10) Uani 1 1 d . . .
H47A H 1.1131 0.3144 0.2769 0.039 Uiso 1 1 calc R . .
C59 C 1.2229(4) 0.3028(4) 0.3305(3) 0.0412(12) Uani 1 1 d . . .
H46A H 1.2821 0.3046 0.3011 0.049 Uiso 1 1 calc R . .
C60 C 1.2967(4) 0.2853(5) 0.4306(3) 0.0562(17) Uani 1 1 d . . .
H48A H 1.2709 0.2795 0.4754 0.084 Uiso 1 1 calc R . .
H48B H 1.3373 0.3370 0.4156 0.084 Uiso 1 1 calc R . .
H48C H 1.3361 0.2333 0.4237 0.084 Uiso 1 1 calc R . .
C61 C 1.0736(3) 0.2817(3) 0.4884(2) 0.0275(9) Uani 1 1 d . . .
C62 C 1.0030(3) 0.2964(3) 0.5829(2) 0.0287(9) Uani 1 1 d . . .
H50A H 0.9715 0.3217 0.6168 0.034 Uiso 1 1 calc R . .
C63 C 1.0262(4) 0.2089(3) 0.5872(2) 0.0363(11) Uani 1 1 d . . .
H51A H 1.0137 0.1640 0.6238 0.044 Uiso 1 1 calc R . .
C64 C 1.1046(5) 0.1161(4) 0.5073(3) 0.0486(14) Uani 1 1 d . . .
H52A H 1.0946 0.0677 0.5438 0.073 Uiso 1 1 calc R . .
H52B H 1.1740 0.1194 0.4885 0.073 Uiso 1 1 calc R . .
H52C H 1.0669 0.1064 0.4764 0.073 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
Cd1 0.0151(2) 0.0245(2) 0.0189(2) 0.00317(15) -0.00280(15) -0.00617(16)
Cd2 0.01678(17) 0.02663(18) 0.0659(3) 0.00221(16) -0.00034(16) -0.00114(13)
Cd3 0.02109(17) 0.02490(16) 0.03641(19) -0.00483(13) -0.01129(13) -0.00050(12)
Cd4 0.0132(2) 0.0254(2) 0.0242(2) 0.00513(16) -0.00251(16) -0.00487(16)
Cl1 0.0294(7) 0.0407(7) 0.1014(13) -0.0319(8) 0.0110(7) -0.0018(6)
Cl2 0.0302(6) 0.0277(5) 0.0380(6) -0.0010(4) -0.0065(5) -0.0019(4)
Cl3 0.0258(6) 0.0466(7) 0.0376(6) 0.0040(5) 0.0033(5) 0.0000(5)
Cl4 0.0319(7) 0.0390(7) 0.0584(8) 0.0085(6) 0.0117(6) -0.0035(5)
Cl5 0.0451(9) 0.0590(10) 0.1220(17) -0.0017(10) -0.0282(10) -0.0228(8)
Cl6 0.180(3) 0.0605(12) 0.234(4) 0.0558(18) -0.163(3) -0.0566(16)
O1 0.085(4) 0.057(3) 0.056(3) -0.012(2) -0.030(3) 0.004(3)
O2 0.059(3) 0.0329(19) 0.060(3) -0.0105(18) -0.004(2) -0.0068(18)
O3 0.0253(19) 0.062(2) 0.049(2) -0.0077(19) -0.0009(16) -0.0065(18)
O4 0.035(2) 0.086(3) 0.057(3) -0.027(2) 0.0052(19) -0.008(2)
O5 0.094(4) 0.040(2) 0.079(3) 0.009(2) -0.052(3) -0.006(2)
O6 0.057(3) 0.072(3) 0.060(3) 0.026(2) -0.026(2) -0.038(2)
O7 0.104(7) 0.088(6) 0.069(5) -0.014(4) 0.043(5) -0.004(5)
O7B 0.005(5) 0.107(13) 0.050(9) 0.012(9) -0.001(5) 0.016(6)
O8 0.037(4) 0.059(4) 0.105(6) -0.011(4) -0.025(4) 0.009(3)
O8B 0.064(11) 0.042(8) 0.068(10) -0.011(7) 0.023(9) -0.008(8)
O9 0.038(4) 0.101(6) 0.073(5) 0.016(4) -0.026(3) -0.021(4)
O9B 0.046(8) 0.079(10) 0.038(7) -0.005(7) -0.011(6) -0.020(8)
O11 0.054(3) 0.058(3) 0.088(4) -0.026(3) 0.007(3) 0.020(2)
O12 0.052(3) 0.088(4) 0.131(5) -0.065(4) 0.006(3) -0.009(3)
O13 0.046(3) 0.078(4) 0.152(6) -0.034(4) -0.022(3) 0.021(3)
O14 0.081(4) 0.085(4) 0.122(5) -0.045(4) 0.045(4) -0.038(3)
O10 0.064(4) 0.068(4) 0.233(10) 0.024(5) 0.036(5) 0.006(3)
O15 0.140(8) 0.212(10) 0.081(5) -0.001(6) -0.007(5) -0.058(7)
O16 0.096(5) 0.083(4) 0.114(5) 0.000(4) 0.023(4) 0.041(4)
O17 0.141(6) 0.096(4) 0.060(3) -0.021(3) 0.042(3) -0.070(4)
O18 0.44(3) 0.089(6) 0.171(10) 0.034(6) -0.060(13) -0.097(10)
O19 0.039(4) 0.53(3) 0.171(10) -0.081(13) -0.030(5) -0.025(8)
O20 0.053(4) 0.306(13) 0.172(8) 0.144(9) -0.037(5) -0.064(6)
O21 0.086(5) 0.230(10) 0.309(14) -0.189(11) -0.116(8) 0.075(6)
O22 0.181(9) 0.230(10) 0.083(5) -0.057(6) -0.070(6) 0.096(8)
O23 0.156(10) 0.276(15) 0.255(14) -0.150(12) -0.125(10) 0.074(10)
O24 0.230(13) 0.194(10) 0.151(9) 0.030(8) -0.095(9) -0.104(9)
O25 0.169(19) 0.103(12) 0.63(6) 0.11(2) -0.14(3) -0.055(13)
O1W 0.098(5) 0.115(5) 0.084(4) -0.015(4) -0.025(4) -0.025(4)
O2W 0.105(10) 0.076(7) 0.109(10) -0.020(7) -0.056(8) 0.004(7)
O3W 0.056(6) 0.088(7) 0.062(6) -0.018(5) -0.015(5) 0.003(5)
O4W 0.163(18) 0.163(16) 0.20(2) -0.132(16) 0.102(16) -0.115(15)
N1 0.021(2) 0.027(2) 0.081(4) -0.001(2) 0.001(2) -0.0037(17)
N2 0.051(3) 0.050(3) 0.038(2) 0.003(2) -0.010(2) -0.021(2)
N3 0.026(2) 0.040(2) 0.076(3) 0.000(2) -0.010(2) -0.002(2)
N4 0.030(2) 0.037(2) 0.052(3) -0.004(2) -0.002(2) 0.0095(19)
N5 0.020(2) 0.039(2) 0.065(3) 0.004(2) 0.005(2) -0.0053(18)
N6 0.021(2) 0.059(3) 0.058(3) 0.006(2) 0.008(2) -0.003(2)
N7 0.0173(18) 0.035(2) 0.0257(18) -0.0042(15) -0.0003(14) -0.0052(15)
N8 0.035(3) 0.059(3) 0.049(3) -0.028(2) 0.001(2) -0.004(2)
N9 0.0188(19) 0.0277(19) 0.051(2) -0.0087(18) 0.0002(17) -0.0020(16)
N10 0.0159(19) 0.031(2) 0.058(3) -0.0102(19) -0.0029(18) -0.0053(16)
N11 0.0235(19) 0.0269(18) 0.0252(18) 0.0063(15) -0.0032(15) -0.0061(15)
N12 0.033(2) 0.031(2) 0.032(2) 0.0139(17) -0.0019(17) -0.0099(18)
N13 0.025(2) 0.030(2) 0.047(2) 0.0118(18) -0.0117(18) -0.0054(17)
N14 0.086(4) 0.053(3) 0.051(3) 0.020(2) -0.052(3) -0.035(3)
N15 0.0202(19) 0.0269(19) 0.044(2) 0.0018(17) -0.0138(17) -0.0030(15)
N16 0.029(2) 0.044(3) 0.096(4) 0.022(3) -0.034(3) -0.013(2)
N17 0.021(2) 0.041(2) 0.071(3) -0.024(2) -0.011(2) 0.0002(18)
N18 0.025(2) 0.042(2) 0.068(3) -0.023(2) 0.002(2) -0.0092(19)
N19 0.025(2) 0.037(2) 0.060(3) -0.017(2) -0.011(2) -0.0058(18)
N20 0.0221(19) 0.0263(18) 0.041(2) -0.0097(16) -0.0040(16) -0.0040(15)
N21 0.025(2) 0.0262(18) 0.039(2) 0.0021(16) -0.0089(17) -0.0086(16)
N22 0.035(2) 0.045(2) 0.036(2) 0.0067(19) 0.0027(19) -0.017(2)
N23 0.0161(18) 0.0311(19) 0.0262(18) 0.0075(15) -0.0027(14) -0.0070(15)
N24 0.0132(18) 0.041(2) 0.049(2) -0.0031(19) -0.0009(17) -0.0082(17)
N25 0.0161(18) 0.0282(19) 0.044(2) -0.0025(16) -0.0109(16) -0.0001(15)
N26 0.0178(18) 0.0256(18) 0.034(2) 0.0010(15) -0.0047(15) 0.0024(15)
N27 0.0123(16) 0.0288(18) 0.0243(17) 0.0028(14) -0.0004(13) -0.0003(14)
N28 0.0188(18) 0.0311(19) 0.0286(19) -0.0039(15) -0.0023(15) -0.0026(15)
N29 0.0213(19) 0.0293(18) 0.033(2) -0.0021(15) -0.0092(16) -0.0019(15)
N30 0.0172(19) 0.051(3) 0.036(2) -0.0015(19) -0.0099(16) 0.0026(18)
N31 0.0183(18) 0.0276(18) 0.0300(19) 0.0054(15) -0.0047(15) -0.0021(15)
N32 0.033(2) 0.0294(19) 0.036(2) 0.0040(16) -0.0101(18) -0.0019(17)
C1 0.031(3) 0.025(2) 0.049(3) -0.007(2) -0.001(2) 0.003(2)
C2 0.052(4) 0.044(3) 0.043(3) -0.011(2) 0.000(3) -0.020(3)
C3 0.025(3) 0.034(3) 0.077(4) -0.016(3) 0.011(3) -0.009(2)
C4 0.139(11) 0.142(11) 0.102(8) 0.028(8) -0.053(8) -0.028(9)
C5 0.027(3) 0.034(3) 0.052(3) -0.005(2) -0.007(2) 0.002(2)
C6 0.022(3) 0.048(3) 0.090(5) 0.009(3) -0.003(3) -0.004(2)
C7 0.028(3) 0.049(3) 0.068(4) -0.003(3) -0.003(3) 0.000(2)
C8 0.055(5) 0.063(4) 0.105(6) 0.001(4) 0.012(4) 0.026(4)
C9 0.024(2) 0.042(3) 0.042(3) -0.005(2) 0.004(2) -0.005(2)
C10 0.016(3) 0.070(4) 0.093(5) 0.018(4) 0.006(3) -0.008(3)
C11 0.017(3) 0.062(4) 0.105(6) 0.019(4) -0.005(3) -0.002(3)
C12 0.041(3) 0.070(4) 0.043(3) -0.001(3) 0.012(3) -0.013(3)
C13 0.023(2) 0.033(2) 0.035(2) -0.0079(19) 0.0001(19) -0.0037(19)
C14 0.037(3) 0.066(4) 0.047(3) -0.026(3) -0.003(2) -0.008(3)
C15 0.023(2) 0.040(3) 0.041(3) -0.009(2) -0.008(2) -0.007(2)
C16 0.064(5) 0.091(5) 0.070(5) -0.052(4) 0.008(4) -0.003(4)
C17 0.016(2) 0.024(2) 0.041(3) 0.0015(18) -0.0026(18) -0.0045(17)
C18 0.029(3) 0.047(3) 0.065(4) -0.025(3) 0.002(3) -0.002(2)
C19 0.027(3) 0.044(3) 0.070(4) -0.026(3) -0.001(3) -0.008(2)
C20 0.020(2) 0.051(3) 0.064(4) -0.017(3) 0.001(2) -0.009(2)
C21 0.0151(19) 0.024(2) 0.027(2) 0.0033(16) -0.0039(16) -0.0028(16)
C22 0.047(3) 0.038(3) 0.020(2) 0.0046(19) -0.006(2) -0.020(2)
C23 0.052(3) 0.049(3) 0.024(2) 0.009(2) -0.001(2) -0.022(3)
C24 0.039(3) 0.031(3) 0.047(3) 0.016(2) 0.006(2) -0.007(2)
C25 0.033(3) 0.036(3) 0.048(3) 0.010(2) -0.026(2) -0.008(2)
C26 0.081(5) 0.048(3) 0.056(4) 0.022(3) -0.044(4) -0.023(3)
C27 0.043(3) 0.034(3) 0.058(4) 0.016(2) -0.020(3) -0.011(2)
C28 0.272(16) 0.074(5) 0.067(5) 0.023(4) -0.099(8) -0.095(8)
C29 0.029(3) 0.026(2) 0.065(3) 0.008(2) -0.026(2) -0.007(2)
C30 0.025(2) 0.032(2) 0.057(3) 0.012(2) -0.006(2) -0.010(2)
C31 0.023(3) 0.043(3) 0.097(5) 0.023(3) -0.015(3) -0.016(2)
C32 0.052(4) 0.059(4) 0.156(9) 0.036(5) -0.067(5) -0.019(4)
C33 0.019(2) 0.040(3) 0.059(3) -0.022(2) -0.006(2) -0.006(2)
C34 0.029(3) 0.058(4) 0.081(4) -0.031(3) 0.003(3) -0.006(3)
C35 0.028(3) 0.045(3) 0.082(4) -0.031(3) -0.006(3) 0.003(2)
C36 0.045(4) 0.040(3) 0.075(4) -0.017(3) 0.008(3) -0.014(3)
C37 0.026(2) 0.033(2) 0.043(3) -0.015(2) -0.007(2) 0.0027(19)
C38 0.017(2) 0.038(3) 0.050(3) -0.005(2) -0.003(2) -0.0004(19)
C39 0.029(3) 0.027(2) 0.045(3) -0.005(2) -0.002(2) 0.0000(19)
C40 0.036(3) 0.049(3) 0.049(3) -0.025(3) 0.000(2) -0.014(2)
C41 0.019(2) 0.036(2) 0.038(3) 0.000(2) -0.0024(19) -0.0089(19)
C42 0.054(4) 0.040(3) 0.049(3) 0.013(2) -0.009(3) -0.021(3)
C43 0.038(3) 0.027(2) 0.054(3) 0.003(2) -0.015(2) -0.012(2)
C44 0.053(4) 0.066(4) 0.034(3) 0.006(3) 0.013(3) -0.021(3)
C45 0.013(2) 0.034(2) 0.029(2) -0.0007(18) 0.0009(16) -0.0056(17)
C46 0.018(2) 0.038(3) 0.053(3) -0.006(2) -0.008(2) 0.000(2)
C47 0.019(2) 0.034(2) 0.035(2) 0.0042(19) -0.0016(18) -0.0014(18)
C48 0.013(2) 0.052(3) 0.060(3) -0.013(3) 0.003(2) -0.012(2)
C49 0.016(2) 0.026(2) 0.027(2) -0.0026(16) -0.0032(16) -0.0007(16)
C50 0.018(2) 0.037(3) 0.053(3) -0.003(2) -0.014(2) 0.000(2)
C51 0.021(2) 0.034(2) 0.048(3) -0.001(2) -0.015(2) -0.0005(19)
C52 0.020(2) 0.028(2) 0.045(3) 0.007(2) -0.006(2) -0.0005(18)
C53 0.018(2) 0.0238(19) 0.027(2) -0.0017(16) -0.0036(16) -0.0032(16)
C54 0.014(2) 0.036(2) 0.032(2) 0.0051(19) -0.0042(17) -0.0054(18)
C55 0.015(2) 0.037(2) 0.029(2) -0.0013(18) 0.0004(17) -0.0019(18)
C56 0.033(3) 0.054(3) 0.024(2) -0.004(2) -0.0067(19) 0.006(2)
C57 0.028(2) 0.027(2) 0.030(2) -0.0009(17) -0.0098(18) -0.0019(18)
C58 0.028(2) 0.041(3) 0.028(2) -0.004(2) -0.0059(19) 0.001(2)
C59 0.029(3) 0.052(3) 0.040(3) -0.008(2) -0.004(2) 0.005(2)
C60 0.020(3) 0.097(5) 0.046(3) 0.001(3) -0.012(2) 0.002(3)
C61 0.016(2) 0.028(2) 0.035(2) 0.0051(18) -0.0104(18) -0.0043(17)
C62 0.025(2) 0.033(2) 0.024(2) 0.0043(17) -0.0036(17) -0.0078(19)
C63 0.040(3) 0.030(2) 0.034(3) 0.0079(19) -0.010(2) -0.006(2)
C64 0.058(4) 0.035(3) 0.049(3) 0.002(2) -0.017(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 0.0033 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'
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
N11 Cd1 N11 180.000(1) 2_675 . ?
N11 Cd1 N15 90.03(13) 2_675 . ?
N11 Cd1 N15 89.97(13) . . ?
N11 Cd1 N15 89.97(13) 2_675 2_675 ?
N11 Cd1 N15 90.03(13) . 2_675 ?
N15 Cd1 N15 180.00(19) . 2_675 ?
N11 Cd1 N7 89.17(13) 2_675 . ?
N11 Cd1 N7 90.83(13) . . ?
N15 Cd1 N7 87.59(13) . . ?
N15 Cd1 N7 92.41(13) 2_675 . ?
N11 Cd1 N7 90.83(13) 2_675 2_675 ?
N11 Cd1 N7 89.17(13) . 2_675 ?
N15 Cd1 N7 92.41(13) . 2_675 ?
N15 Cd1 N7 87.59(13) 2_675 2_675 ?
N7 Cd1 N7 180.00(11) . 2_675 ?
N5 Cd2 N13 105.71(17) 2_675 . ?
N5 Cd2 N1 155.65(18) 2_675 . ?
N13 Cd2 N1 94.79(17) . . ?
N5 Cd2 N9 104.11(16) 2_675 . ?
N13 Cd2 N9 98.07(15) . . ?
N1 Cd2 N9 85.46(15) . . ?
N5 Cd2 N3 95.90(17) 2_675 . ?
N13 Cd2 N3 86.42(17) . . ?
N1 Cd2 N3 72.00(16) . . ?
N9 Cd2 N3 157.34(15) . . ?
N5 Cd2 O11 80.15(18) 2_675 . ?
N13 Cd2 O11 173.63(15) . . ?
N1 Cd2 O11 78.94(18) . . ?
N9 Cd2 O11 82.66(15) . . ?
N3 Cd2 O11 90.52(17) . . ?
N25 Cd3 N29 101.84(14) . . ?
N25 Cd3 N21 103.03(15) . . ?
N29 Cd3 N21 103.63(14) . . ?
N25 Cd3 N17 96.67(14) . . ?
N29 Cd3 N17 158.38(14) . . ?
N21 Cd3 N17 82.73(16) . . ?
N25 Cd3 N19 159.93(15) . . ?
N29 Cd3 N19 85.99(14) . . ?
N21 Cd3 N19 92.84(15) . . ?
N17 Cd3 N19 72.96(14) . . ?
N25 Cd3 O1 83.95(15) . . ?
N29 Cd3 O1 89.83(16) . . ?
N21 Cd3 O1 162.98(16) . . ?
N17 Cd3 O1 81.04(18) . . ?
N19 Cd3 O1 77.56(16) . . ?
N23 Cd4 N23 180.00(17) 2_766 . ?
N23 Cd4 N27 89.04(12) 2_766 . ?
N23 Cd4 N27 90.96(13) . . ?
N23 Cd4 N27 90.96(13) 2_766 2_766 ?
N23 Cd4 N27 89.04(12) . 2_766 ?
N27 Cd4 N27 180.000(1) . 2_766 ?
N23 Cd4 N31 90.66(13) 2_766 2_766 ?
N23 Cd4 N31 89.34(13) . 2_766 ?
N27 Cd4 N31 89.24(13) . 2_766 ?
N27 Cd4 N31 90.76(13) 2_766 2_766 ?
N23 Cd4 N31 89.34(13) 2_766 . ?
N23 Cd4 N31 90.66(13) . . ?
N27 Cd4 N31 90.76(13) . . ?
N27 Cd4 N31 89.24(13) 2_766 . ?
N31 Cd4 N31 180.000(1) 2_766 . ?
O12 Cl1 O13 109.3(4) . . ?
O12 Cl1 O11 109.5(3) . . ?
O13 Cl1 O11 109.3(4) . . ?
O12 Cl1 O14 109.7(4) . . ?
O13 Cl1 O14 109.3(4) . . ?
O11 Cl1 O14 109.7(3) . . ?
O4 Cl2 O2 110.9(3) . . ?
O4 Cl2 O5 111.5(3) . . ?
O2 Cl2 O5 108.2(3) . . ?
O4 Cl2 O3 108.3(3) . . ?
O2 Cl2 O3 110.0(3) . . ?
O5 Cl2 O3 107.8(3) . . ?
O7B Cl3 O8 146.2(8) . . ?
O7B Cl3 O8B 111.3(12) . . ?
O8 Cl3 O8B 44.7(8) . . ?
O7B Cl3 O7 52.1(8) . . ?
O8 Cl3 O7 114.0(6) . . ?
O8B Cl3 O7 121.4(7) . . ?
O7B Cl3 O6 104.4(8) . . ?
O8 Cl3 O6 108.9(4) . . ?
O8B Cl3 O6 121.3(6) . . ?
O7 Cl3 O6 117.3(5) . . ?
O7B Cl3 O9B 109.7(10) . . ?
O8 Cl3 O9B 68.3(7) . . ?
O8B Cl3 O9B 106.8(10) . . ?
O7 Cl3 O9B 57.7(7) . . ?
O6 Cl3 O9B 102.9(6) . . ?
O7B Cl3 O9 58.6(9) . . ?
O8 Cl3 O9 105.9(5) . . ?
O8B Cl3 O9 61.3(10) . . ?
O7 Cl3 O9 104.0(6) . . ?
O6 Cl3 O9 105.6(3) . . ?
O9B Cl3 O9 151.1(6) . . ?
O10 Cl4 O17 119.1(5) . . ?
O10 Cl4 O16 118.7(4) . . ?
O17 Cl4 O16 118.7(4) . . ?
O10 Cl4 O15 91.9(7) . . ?
O17 Cl4 O15 101.0(4) . . ?
O16 Cl4 O15 95.8(5) . . ?
O10 Cl4 O4W 72.4(10) . . ?
O17 Cl4 O4W 92.9(7) . . ?
O16 Cl4 O4W 86.1(9) . . ?
O15 Cl4 O4W 162.8(11) . . ?
O20 Cl5 O19 114.8(7) . . ?
O20 Cl5 O18 114.8(10) . . ?
O19 Cl5 O18 103.8(11) . . ?
O20 Cl5 O21 108.2(8) . . ?
O19 Cl5 O21 113.1(7) . . ?
O18 Cl5 O21 101.5(8) . . ?
O25 Cl6 O22 123.0(14) . . ?
O25 Cl6 O23 103.4(12) . . ?
O22 Cl6 O23 120.6(9) . . ?
O25 Cl6 O24 112.5(19) . . ?
O22 Cl6 O24 94.3(6) . . ?
O23 Cl6 O24 100.3(6) . . ?
O7B O7 Cl3 59.5(7) . . ?
O7B O7 O9B 124.3(10) . . ?
Cl3 O7 O9B 65.0(7) . . ?
O7 O7B Cl3 68.5(7) . . ?
O7 O7B O9 126.1(13) . . ?
Cl3 O7B O9 68.6(8) . . ?
O8B O8 Cl3 69.2(9) . . ?
O8B O8 O9B 120.3(11) . . ?
Cl3 O8 O9B 59.9(6) . . ?
O8 O8B Cl3 66.1(10) . . ?
O8 O8B O9 129.2(14) . . ?
Cl3 O8B O9 63.2(7) . . ?
O7B O9 O8B 101.3(10) . . ?
O7B O9 Cl3 52.8(6) . . ?
O8B O9 Cl3 55.5(7) . . ?
O7 O9B Cl3 57.3(6) . . ?
O7 O9B O8 100.0(9) . . ?
Cl3 O9B O8 51.8(5) . . ?
Cl1 O11 Cd2 137.6(3) . . ?
Cl4 O10 O4W 58.4(6) . . ?
O2W O3W C4 170.5(11) . . ?
Cl4 O4W O10 49.2(8) . . ?
C1 N1 C3 106.8(5) . . ?
C1 N1 Cd2 115.8(3) . . ?
C3 N1 Cd2 134.0(4) . . ?
C1 N2 C4 131.3(7) . . ?
C1 N2 C2 105.8(5) . . ?
C4 N2 C2 121.4(7) . . ?
C5 N3 C6 105.6(5) . . ?
C5 N3 Cd2 109.5(3) . . ?
C6 N3 Cd2 143.1(4) . . ?
C7 N4 C5 107.3(4) . . ?
C7 N4 C8 124.9(5) . . ?
C5 N4 C8 126.8(5) . . ?
C9 N5 C11 105.3(5) . . ?
C9 N5 Cd2 127.9(3) . 2_675 ?
C11 N5 Cd2 126.0(4) . 2_675 ?
C10 N6 C9 107.4(5) . . ?
C10 N6 C12 124.6(5) . . ?
C9 N6 C12 128.1(5) . . ?
C13 N7 C15 105.7(4) . . ?
C13 N7 Cd1 136.1(3) . . ?
C15 N7 Cd1 118.2(3) . . ?
C13 N8 C14 108.2(4) . . ?
C13 N8 C16 124.8(5) . . ?
C14 N8 C16 127.0(5) . . ?
C17 N9 C18 105.5(4) . . ?
C17 N9 Cd2 132.1(3) . . ?
C18 N9 Cd2 120.8(3) . . ?
C17 N10 C19 106.7(4) . . ?
C17 N10 C20 128.2(4) . . ?
C19 N10 C20 125.1(4) . . ?
C21 N11 C22 105.9(4) . . ?
C21 N11 Cd1 139.4(3) . . ?
C22 N11 Cd1 114.5(3) . . ?
C23 N12 C21 107.5(4) . . ?
C23 N12 C24 124.9(4) . . ?
C21 N12 C24 127.5(5) . . ?
C25 N13 C27 105.5(5) . . ?
C25 N13 Cd2 128.7(4) . . ?
C27 N13 Cd2 125.2(4) . . ?
C25 N14 C26 107.3(5) . . ?
C25 N14 C28 127.1(5) . . ?
C26 N14 C28 125.3(6) . . ?
C29 N15 C30 104.7(4) . . ?
C29 N15 Cd1 137.3(3) . . ?
C30 N15 Cd1 117.9(3) . . ?
C29 N16 C31 106.5(4) . . ?
C29 N16 C32 127.6(5) . . ?
C31 N16 C32 125.8(6) . . ?
C33 N17 C35 105.5(5) . . ?
C33 N17 Cd3 110.4(3) . . ?
C35 N17 Cd3 134.8(4) . . ?
C33 N18 C34 107.4(5) . . ?
C33 N18 C36 129.3(5) . . ?
C34 N18 C36 123.0(5) . . ?
C37 N19 C38 105.7(4) . . ?
C37 N19 Cd3 107.7(3) . . ?
C38 N19 Cd3 131.1(3) . . ?
C37 N20 C39 107.4(4) . . ?
C37 N20 C40 128.0(4) . . ?
C39 N20 C40 124.3(4) . . ?
C41 N21 C43 106.0(4) . . ?
C41 N21 Cd3 130.6(3) . . ?
C43 N21 Cd3 121.9(4) . . ?
C41 N22 C42 106.9(5) . . ?
C41 N22 C44 126.9(5) . . ?
C42 N22 C44 126.3(5) . . ?
C45 N23 C47 104.7(4) . . ?
C45 N23 Cd4 138.8(3) . . ?
C47 N23 Cd4 116.1(3) . . ?
C45 N24 C46 107.8(4) . . ?
C45 N24 C48 128.2(4) . . ?
C46 N24 C48 124.0(4) . . ?
C49 N25 C50 105.6(4) . . ?
C49 N25 Cd3 131.6(3) . . ?
C50 N25 Cd3 122.4(3) . . ?
C49 N26 C51 106.6(4) . . ?
C49 N26 C52 127.4(4) . . ?
C51 N26 C52 125.9(4) . . ?
C53 N27 C54 105.1(4) . . ?
C53 N27 Cd4 137.7(3) . . ?
C54 N27 Cd4 117.0(3) . . ?
C53 N28 C55 107.9(4) . . ?
C53 N28 C56 125.8(4) . . ?
C55 N28 C56 126.3(4) . . ?
C57 N29 C58 105.5(4) . . ?
C57 N29 Cd3 127.7(3) . . ?
C58 N29 Cd3 126.2(3) . . ?
C57 N30 C59 108.0(4) . . ?
C57 N30 C60 126.9(4) . . ?
C59 N30 C60 125.1(4) . . ?
C61 N31 C62 105.7(4) . . ?
C61 N31 Cd4 137.1(3) . . ?
C62 N31 Cd4 117.2(3) . . ?
C61 N32 C63 106.9(4) . . ?
C61 N32 C64 126.3(4) . . ?
C63 N32 C64 126.7(4) . . ?
N1 C1 N2 111.4(5) . . ?
N1 C1 C5 120.4(5) . . ?
N2 C1 C5 128.1(5) . . ?
C3 C2 N2 106.9(5) . . ?
C2 C3 N1 109.1(5) . . ?
N2 C4 O3W 137.5(10) . . ?
N3 C5 N4 110.7(5) . . ?
N3 C5 C1 120.2(5) . . ?
N4 C5 C1 129.2(5) . . ?
C7 C6 N3 110.0(5) . . ?
N4 C7 C6 106.4(5) . . ?
N5 C9 N6 110.4(5) . . ?
N5 C9 C13 125.8(5) . . ?
N6 C9 C13 123.2(5) . . ?
C11 C10 N6 107.0(5) . . ?
C10 C11 N5 110.0(6) . . ?
N7 C13 N8 110.6(4) . . ?
N7 C13 C9 127.1(4) . . ?
N8 C13 C9 122.3(4) . . ?
N8 C14 C15 105.9(5) . . ?
N7 C15 C14 109.7(5) . . ?
N9 C17 N10 111.3(4) . . ?
N9 C17 C21 126.1(4) . . ?
N10 C17 C21 122.4(4) . . ?
C19 C18 N9 109.9(5) . . ?
C18 C19 N10 106.6(5) . . ?
N11 C21 N12 110.1(4) . . ?
N11 C21 C17 128.4(4) . . ?
N12 C21 C17 121.3(4) . . ?
C23 C22 N11 109.6(4) . . ?
C22 C23 N12 106.9(4) . . ?
N13 C25 N14 110.7(5) . . ?
N13 C25 C29 124.3(5) . . ?
N14 C25 C29 124.4(5) . . ?
C27 C26 N14 106.3(6) . . ?
C26 C27 N13 110.1(5) . . ?
N15 C29 N16 111.1(5) . . ?
N15 C29 C25 127.6(5) . . ?
N16 C29 C25 121.3(4) . . ?
C31 C30 N15 110.4(5) . . ?
C30 C31 N16 107.2(5) . . ?
N17 C33 N18 110.7(5) . . ?
N17 C33 C37 119.5(5) . . ?
N18 C33 C37 129.6(5) . . ?
C35 C34 N18 106.6(5) . . ?
C34 C35 N17 109.8(5) . . ?
N20 C37 N19 110.5(4) . . ?
N20 C37 C33 129.8(4) . . ?
N19 C37 C33 119.5(4) . . ?
C39 C38 N19 110.2(4) . . ?
C38 C39 N20 106.2(4) . . ?
N21 C41 N22 110.5(4) . . ?
N21 C41 C45 125.7(4) . 2_766 ?
N22 C41 C45 123.2(5) . 2_766 ?
C43 C42 N22 107.5(5) . . ?
C42 C43 N21 109.1(5) . . ?
N23 C45 N24 111.3(4) . . ?
N23 C45 C41 127.6(4) . 2_766 ?
N24 C45 C41 120.7(4) . 2_766 ?
C47 C46 N24 106.1(4) . . ?
C46 C47 N23 110.1(4) . . ?
N25 C49 N26 111.4(4) . . ?
N25 C49 C53 125.0(4) . . ?
N26 C49 C53 123.2(4) . . ?
C51 C50 N25 109.5(4) . . ?
C50 C51 N26 106.9(4) . . ?
N27 C53 N28 110.7(4) . . ?
N27 C53 C49 128.3(4) . . ?
N28 C53 C49 120.8(4) . . ?
C55 C54 N27 110.0(4) . . ?
C54 C55 N28 106.3(4) . . ?
N29 C57 N30 110.2(4) . . ?
N29 C57 C61 125.0(4) . . ?
N30 C57 C61 124.6(4) . . ?
C59 C58 N29 109.8(4) . . ?
C58 C59 N30 106.4(5) . . ?
N31 C61 N32 110.7(4) . . ?
N31 C61 C57 128.3(4) . . ?
N32 C61 C57 121.1(4) . . ?
C63 C62 N31 110.2(4) . . ?
C62 C63 N32 106.6(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
Cd1 N11 2.360(3) 2_675 ?
Cd1 N11 2.360(3) . ?
Cd1 N15 2.395(4) . ?
Cd1 N15 2.395(4) 2_675 ?
Cd1 N7 2.418(4) . ?
Cd1 N7 2.418(4) 2_675 ?
Cd2 N5 2.242(4) 2_675 ?
Cd2 N13 2.283(5) . ?
Cd2 N1 2.290(4) . ?
Cd2 N9 2.329(4) . ?
Cd2 N3 2.476(5) . ?
Cd2 O11 2.622(5) . ?
Cd3 N25 2.278(4) . ?
Cd3 N29 2.279(4) . ?
Cd3 N21 2.290(4) . ?
Cd3 N17 2.413(4) . ?
Cd3 N19 2.456(4) . ?
Cd3 O1 2.476(5) . ?
Cd4 N23 2.365(4) 2_766 ?
Cd4 N23 2.365(4) . ?
Cd4 N27 2.394(4) . ?
Cd4 N27 2.394(4) 2_766 ?
Cd4 N31 2.402(4) 2_766 ?
Cd4 N31 2.402(4) . ?
Cl1 O12 1.406(6) . ?
Cl1 O13 1.422(7) . ?
Cl1 O11 1.428(4) . ?
Cl1 O14 1.433(6) . ?
Cl2 O4 1.426(4) . ?
Cl2 O2 1.429(4) . ?
Cl2 O5 1.431(4) . ?
Cl2 O3 1.441(4) . ?
Cl3 O7B 1.302(11) . ?
Cl3 O8 1.375(7) . ?
Cl3 O8B 1.406(15) . ?
Cl3 O7 1.407(7) . ?
Cl3 O6 1.429(4) . ?
Cl3 O9B 1.514(13) . ?
Cl3 O9 1.522(7) . ?
Cl4 O10 1.361(7) . ?
Cl4 O17 1.387(5) . ?
Cl4 O16 1.388(6) . ?
Cl4 O15 1.532(9) . ?
Cl4 O4W 1.531(18) . ?
Cl5 O20 1.294(8) . ?
Cl5 O19 1.317(9) . ?
Cl5 O18 1.343(10) . ?
Cl5 O21 1.394(9) . ?
Cl6 O25 1.251(17) . ?
Cl6 O22 1.321(7) . ?
Cl6 O23 1.392(12) . ?
Cl6 O24 1.679(14) . ?
O7 O7B 1.192(17) . ?
O7 O9B 1.413(18) . ?
O7B O9 1.40(2) . ?
O8 O8B 1.06(2) . ?
O8 O9B 1.626(17) . ?
O8B O9 1.50(2) . ?
O10 O4W 1.71(3) . ?
O2W O3W 1.475(16) . ?
O3W C4 1.782(16) . ?
N1 C1 1.305(7) . ?
N1 C3 1.375(6) . ?
N2 C1 1.358(7) . ?
N2 C4 1.374(11) . ?
N2 C2 1.392(8) . ?
N3 C5 1.318(7) . ?
N3 C6 1.370(7) . ?
N4 C7 1.352(7) . ?
N4 C5 1.365(7) . ?
N4 C8 1.460(8) . ?
N5 C9 1.320(7) . ?
N5 C11 1.392(7) . ?
N5 Cd2 2.242(4) 2_675 ?
N6 C10 1.357(8) . ?
N6 C9 1.368(6) . ?
N6 C12 1.440(8) . ?
N7 C13 1.340(6) . ?
N7 C15 1.374(6) . ?
N8 C13 1.357(7) . ?
N8 C14 1.360(8) . ?
N8 C16 1.486(8) . ?
N9 C17 1.322(6) . ?
N9 C18 1.392(7) . ?
N10 C17 1.359(6) . ?
N10 C19 1.388(7) . ?
N10 C20 1.461(6) . ?
N11 C21 1.332(6) . ?
N11 C22 1.377(6) . ?
N12 C23 1.358(7) . ?
N12 C21 1.365(6) . ?
N12 C24 1.478(6) . ?
N13 C25 1.335(7) . ?
N13 C27 1.374(7) . ?
N14 C25 1.349(8) . ?
N14 C26 1.377(7) . ?
N14 C28 1.462(9) . ?
N15 C29 1.338(6) . ?
N15 C30 1.366(6) . ?
N16 C29 1.352(7) . ?
N16 C31 1.362(8) . ?
N16 C32 1.477(7) . ?
N17 C33 1.340(7) . ?
N17 C35 1.373(7) . ?
N18 C33 1.356(7) . ?
N18 C34 1.367(8) . ?
N18 C36 1.455(7) . ?
N19 C37 1.344(6) . ?
N19 C38 1.375(7) . ?
N20 C37 1.342(6) . ?
N20 C39 1.390(6) . ?
N20 C40 1.472(6) . ?
N21 C41 1.327(7) . ?
N21 C43 1.395(6) . ?
N22 C41 1.368(6) . ?
N22 C42 1.374(8) . ?
N22 C44 1.453(8) . ?
N23 C45 1.331(6) . ?
N23 C47 1.390(6) . ?
N24 C45 1.352(6) . ?
N24 C46 1.365(7) . ?
N24 C48 1.459(6) . ?
N25 C49 1.320(6) . ?
N25 C50 1.380(6) . ?
N26 C49 1.359(5) . ?
N26 C51 1.368(6) . ?
N26 C52 1.466(6) . ?
N27 C53 1.335(6) . ?
N27 C54 1.382(5) . ?
N28 C53 1.354(6) . ?
N28 C55 1.360(6) . ?
N28 C56 1.471(6) . ?
N29 C57 1.347(6) . ?
N29 C58 1.371(6) . ?
N30 C57 1.351(6) . ?
N30 C59 1.362(7) . ?
N30 C60 1.481(6) . ?
N31 C61 1.331(6) . ?
N31 C62 1.370(6) . ?
N32 C61 1.364(6) . ?
N32 C63 1.372(7) . ?
N32 C64 1.456(7) . ?
C1 C5 1.459(7) . ?
C2 C3 1.345(9) . ?
C6 C7 1.356(8) . ?
C9 C13 1.456(7) . ?
C10 C11 1.336(10) . ?
C14 C15 1.381(8) . ?
C17 C21 1.469(7) . ?
C18 C19 1.342(8) . ?
C22 C23 1.355(6) . ?
C25 C29 1.479(7) . ?
C26 C27 1.348(9) . ?
C30 C31 1.339(8) . ?
C33 C37 1.462(7) . ?
C34 C35 1.364(9) . ?
C38 C39 1.345(7) . ?
C41 C45 1.466(7) 2_766 ?
C42 C43 1.345(9) . ?
C45 C41 1.466(7) 2_766 ?
C46 C47 1.359(7) . ?
C49 C53 1.474(6) . ?
C50 C51 1.354(7) . ?
C54 C55 1.357(6) . ?
C57 C61 1.464(7) . ?
C58 C59 1.362(7) . ?
C62 C63 1.352(7) . ?
|
1100981.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100981.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_1100981
loop_
_publ_author_name
'Swarnalatha Kokatam'
'Thomas Weyherm\"uller'
'Eberhard Bothe'
'Phalguni Chaudhuri'
'Karl Wieghardt'
_publ_section_title
;
Structural Characterization of Four Members of the Electron-Transfer Series
[PdII(L)2)2]n (L = o-Iminophenolate Derivative; n= 2-, 1-, 0, 1+, 2+).
Ligand Mixed Valency in the Monocation and Monoanion with S=1/2 Ground States
;
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3709
_journal_page_last 3717
_journal_paper_doi 10.1021/ic048292i
_journal_volume 44
_journal_year 2005
_chemical_formula_moiety '[C42 H48 F6 N2 O2 Pd]+, (B F4)-'
_chemical_formula_sum 'C42 H48 B F10 N2 O2 Pd'
_chemical_formula_weight 920.03
_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 95.586(5)
_cell_angle_gamma 90.00
_cell_formula_units_Z 8
_cell_length_a 21.5769(6)
_cell_length_b 13.2251(3)
_cell_length_c 30.9126(8)
_cell_measurement_temperature 100(2)
_cell_volume 8779.2(4)
_computing_cell_refinement 'Nonius Collect Software'
_computing_data_collection 'Nonius Collect Software'
_computing_data_reduction 'Nonius Collect Software'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 100(2)
_diffrn_measured_fraction_theta_full 0.478
_diffrn_measured_fraction_theta_max 0.478
_diffrn_measurement_device_type 'Nonius Kappa-CCD'
_diffrn_measurement_method
'553 images at 0.6 deg. in phi, 975 images at 0.6 deg. in \w, 42 sec./frame'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'rotating anode'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0760
_diffrn_reflns_av_sigmaI/netI 0.0468
_diffrn_reflns_limit_h_max 28
_diffrn_reflns_limit_h_min -28
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_l_max 41
_diffrn_reflns_limit_l_min -41
_diffrn_reflns_number 76289
_diffrn_reflns_theta_full 28.28
_diffrn_reflns_theta_max 28.28
_diffrn_reflns_theta_min 3.08
_exptl_absorpt_coefficient_mu 0.501
_exptl_absorpt_correction_type 'not measured'
_exptl_crystal_colour 'dark red'
_exptl_crystal_density_diffrn 1.392
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description 'transparent parallelepiped'
_exptl_crystal_F_000 3768
_exptl_crystal_size_max 0.10
_exptl_crystal_size_mid 0.05
_exptl_crystal_size_min 0.05
_refine_diff_density_max 0.805
_refine_diff_density_min -0.743
_refine_diff_density_rms 0.076
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.140
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 535
_refine_ls_number_reflns 10873
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.140
_refine_ls_R_factor_all 0.0668
_refine_ls_R_factor_gt 0.0482
_refine_ls_shift/su_max 0.009
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0193P)^2^+19.7222P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0819
_refine_ls_wR_factor_ref 0.0870
_reflns_number_gt 8927
_reflns_number_total 10873
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file ic048292isi20041206_054204_2.cif
_cod_data_source_block 2
_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:
'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0193P)^2^+19.7222P] 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^)+(0.0193P)^2^+19.7222P] where P=(Fo^2^+2Fc^2^)/3'.
Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas
;
_cod_database_code 1100981
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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.854355(9) 1.602206(14) 1.126752(6) 0.01646(5) Uani 1 d . . .
O1 O 0.87299(8) 1.46605(12) 1.10525(6) 0.0202(4) Uani 1 d . . .
C1 C 0.93044(11) 1.45786(17) 1.09508(8) 0.0168(5) Uani 1 d . . .
C2 C 0.95451(12) 1.36618(18) 1.07900(8) 0.0185(5) Uani 1 d . . .
C3 C 1.01447(12) 1.36999(18) 1.06745(8) 0.0198(5) Uani 1 d . . .
H3 H 1.0306 1.3109 1.0552 0.024 Uiso 1 calc R . .
C4 C 1.05459(11) 1.45749(18) 1.07266(8) 0.0180(5) Uani 1 d . . .
C5 C 1.03234(11) 1.54277(18) 1.09039(8) 0.0184(5) Uani 1 d . . .
H5 H 1.0586 1.6000 1.0957 0.022 Uiso 1 calc R . .
C6 C 0.96994(11) 1.54586(18) 1.10095(8) 0.0174(5) Uani 1 d . . .
N7 N 0.94115(9) 1.62745(14) 1.11556(7) 0.0169(4) Uani 1 d . . .
C8 C 0.97371(11) 1.71781(18) 1.13001(8) 0.0179(5) Uani 1 d . . .
C9 C 0.97163(12) 1.80610(19) 1.10470(9) 0.0231(5) Uani 1 d . . .
C10 C 1.00040(13) 1.8931(2) 1.12205(10) 0.0305(6) Uani 1 d . . .
H10 H 0.9996 1.9531 1.1051 0.037 Uiso 1 calc R . .
C11 C 1.03018(13) 1.8928(2) 1.16380(10) 0.0315(6) Uani 1 d . . .
H11 H 1.0491 1.9529 1.1756 0.038 Uiso 1 calc R . .
C12 C 1.03243(12) 1.8060(2) 1.18824(10) 0.0285(6) Uani 1 d . . .
H12 H 1.0534 1.8061 1.2167 0.034 Uiso 1 calc R . .
C13 C 1.00419(12) 1.71777(19) 1.17165(9) 0.0231(6) Uani 1 d . . .
H13 H 1.0058 1.6579 1.1887 0.028 Uiso 1 calc R . .
C14 C 0.91439(13) 1.26967(19) 1.07579(9) 0.0245(6) Uani 1 d . . .
C15 C 0.89364(15) 1.2447(2) 1.12087(10) 0.0322(6) Uani 1 d . . .
H15A H 0.9304 1.2373 1.1419 0.048 Uiso 1 calc R . .
H15B H 0.8700 1.1813 1.1193 0.048 Uiso 1 calc R . .
H15C H 0.8673 1.2994 1.1301 0.048 Uiso 1 calc R . .
C16 C 0.95085(16) 1.1784(2) 1.06121(11) 0.0365(7) Uani 1 d . . .
H16A H 0.9882 1.1683 1.0814 0.055 Uiso 1 calc R . .
H16B H 0.9630 1.1905 1.0319 0.055 Uiso 1 calc R . .
H16C H 0.9246 1.1178 1.0610 0.055 Uiso 1 calc R . .
C17 C 0.85668(15) 1.2849(2) 1.04312(10) 0.0353(7) Uani 1 d . . .
H17A H 0.8699 1.2992 1.0143 0.053 Uiso 1 calc R . .
H17B H 0.8321 1.3418 1.0525 0.053 Uiso 1 calc R . .
H17C H 0.8313 1.2233 1.0418 0.053 Uiso 1 calc R . .
C18 C 1.11911(12) 1.45270(19) 1.05632(8) 0.0209(5) Uani 1 d . . .
C19 C 1.11048(14) 1.4583(2) 1.00643(9) 0.0291(6) Uani 1 d . . .
H19A H 1.1512 1.4548 0.9950 0.044 Uiso 1 calc R . .
H19B H 1.0901 1.5221 0.9974 0.044 Uiso 1 calc R . .
H19C H 1.0846 1.4015 0.9950 0.044 Uiso 1 calc R . .
C20 C 1.16022(12) 1.5419(2) 1.07328(10) 0.0290(6) Uani 1 d . . .
H20A H 1.2015 1.5353 1.0629 0.044 Uiso 1 calc R . .
H20B H 1.1644 1.5416 1.1051 0.044 Uiso 1 calc R . .
H20C H 1.1410 1.6055 1.0627 0.044 Uiso 1 calc R . .
C21 C 1.15314(14) 1.3541(2) 1.07039(11) 0.0354(7) Uani 1 d . . .
H21A H 1.1954 1.3557 1.0614 0.053 Uiso 1 calc R . .
H21B H 1.1305 1.2964 1.0567 0.053 Uiso 1 calc R . .
H21C H 1.1552 1.3474 1.1021 0.053 Uiso 1 calc R . .
C22 C 0.94153(16) 1.8068(2) 1.05932(10) 0.0339(7) Uani 1 d . . .
F23 F 0.94060(12) 1.89938(14) 1.04153(6) 0.0603(6) Uani 1 d . . .
F24 F 0.88232(8) 1.77404(14) 1.05539(6) 0.0389(4) Uani 1 d . . .
F25 F 0.97225(10) 1.74746(15) 1.03304(6) 0.0465(5) Uani 1 d . . .
O31 O 0.83599(8) 1.74006(12) 1.14857(6) 0.0191(4) Uani 1 d . . .
C31 C 0.78344(11) 1.74987(18) 1.16224(8) 0.0171(5) Uani 1 d . . .
C32 C 0.76266(11) 1.84365(17) 1.18039(8) 0.0167(5) Uani 1 d . . .
C33 C 0.70556(11) 1.84133(18) 1.19473(8) 0.0175(5) Uani 1 d . . .
H33 H 0.6914 1.9013 1.2075 0.021 Uiso 1 calc R . .
C34 C 0.66332(11) 1.75306(18) 1.19209(8) 0.0176(5) Uani 1 d . . .
C35 C 0.68188(11) 1.66561(19) 1.17461(8) 0.0191(5) Uani 1 d . . .
H35 H 0.6551 1.6084 1.1728 0.023 Uiso 1 calc R . .
C36 C 0.74167(11) 1.65982(18) 1.15892(8) 0.0179(5) Uani 1 d . . .
N37 N 0.76609(9) 1.58146(14) 1.14058(7) 0.0172(4) Uani 1 d . . .
C38 C 0.73432(11) 1.48523(18) 1.13747(8) 0.0182(5) Uani 1 d . . .
C39 C 0.70020(12) 1.45347(19) 1.09921(9) 0.0237(6) Uani 1 d . . .
C40 C 0.67240(14) 1.3578(2) 1.09826(10) 0.0311(7) Uani 1 d . . .
H40 H 0.6489 1.3353 1.0725 0.037 Uiso 1 calc R . .
C41 C 0.67872(14) 1.2958(2) 1.13418(10) 0.0313(7) Uani 1 d . . .
H41 H 0.6595 1.2311 1.1331 0.038 Uiso 1 calc R . .
C42 C 0.71295(14) 1.3277(2) 1.17180(10) 0.0294(6) Uani 1 d . . .
H42 H 0.7173 1.2849 1.1966 0.035 Uiso 1 calc R . .
C43 C 0.74110(13) 1.42236(19) 1.17335(9) 0.0251(6) Uani 1 d . . .
H43 H 0.7650 1.4439 1.1991 0.030 Uiso 1 calc R . .
C44 C 0.80665(11) 1.93518(18) 1.18294(9) 0.0197(5) Uani 1 d . . .
C45 C 0.82525(13) 1.9617(2) 1.13750(9) 0.0267(6) Uani 1 d . . .
H45A H 0.8470 1.9042 1.1259 0.040 Uiso 1 calc R . .
H45B H 0.8528 2.0208 1.1395 0.040 Uiso 1 calc R . .
H45C H 0.7878 1.9770 1.1181 0.040 Uiso 1 calc R . .
C46 C 0.86534(12) 1.9110(2) 1.21385(9) 0.0262(6) Uani 1 d . . .
H46A H 0.8863 1.8517 1.2030 0.039 Uiso 1 calc R . .
H46B H 0.8533 1.8967 1.2430 0.039 Uiso 1 calc R . .
H46C H 0.8937 1.9691 1.2151 0.039 Uiso 1 calc R . .
C47 C 0.77500(12) 2.02810(19) 1.20066(10) 0.0263(6) Uani 1 d . . .
H47A H 0.7648 2.0143 1.2303 0.039 Uiso 1 calc R . .
H47B H 0.7367 2.0433 1.1820 0.039 Uiso 1 calc R . .
H47C H 0.8033 2.0862 1.2010 0.039 Uiso 1 calc R . .
C48 C 0.60027(11) 1.76581(18) 1.20980(8) 0.0182(5) Uani 1 d . . .
C49 C 0.56516(12) 1.8562(2) 1.18731(9) 0.0246(6) Uani 1 d . . .
H49A H 0.5247 1.8639 1.1988 0.037 Uiso 1 calc R . .
H49B H 0.5588 1.8439 1.1559 0.037 Uiso 1 calc R . .
H49C H 0.5897 1.9180 1.1929 0.037 Uiso 1 calc R . .
C50 C 0.61083(12) 1.7847(2) 1.25907(8) 0.0228(5) Uani 1 d . . .
H50A H 0.5705 1.7929 1.2708 0.034 Uiso 1 calc R . .
H50B H 0.6357 1.8462 1.2646 0.034 Uiso 1 calc R . .
H50C H 0.6330 1.7270 1.2732 0.034 Uiso 1 calc R . .
C51 C 0.56004(12) 1.67041(19) 1.20173(9) 0.0235(6) Uani 1 d . . .
H51A H 0.5196 1.6810 1.2129 0.035 Uiso 1 calc R . .
H51B H 0.5811 1.6128 1.2167 0.035 Uiso 1 calc R . .
H51C H 0.5538 1.6567 1.1705 0.035 Uiso 1 calc R . .
C52 C 0.69129(16) 1.5211(2) 1.06018(10) 0.0376(7) Uani 1 d . . .
F53 F 0.65912(13) 1.60310(16) 1.06804(7) 0.0724(7) Uani 1 d . . .
F54 F 0.66042(11) 1.47640(15) 1.02624(6) 0.0595(6) Uani 1 d . . .
F55 F 0.74460(11) 1.5536(2) 1.04721(7) 0.0730(8) Uani 1 d . . .
B60 B 0.63959(14) 0.8833(2) 0.74469(10) 0.0232(6) Uani 1 d . . .
F61 F 0.65324(8) 0.97835(12) 0.76269(6) 0.0352(4) Uani 1 d . . .
F62 F 0.58787(8) 0.84406(14) 0.76166(6) 0.0383(4) Uani 1 d . . .
F63 F 0.69102(8) 0.82012(12) 0.75559(5) 0.0318(4) Uani 1 d . . .
F64 F 0.62969(7) 0.89196(13) 0.69971(5) 0.0319(4) Uani 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
Pd1 0.01739(9) 0.01081(8) 0.02177(10) -0.00314(8) 0.00498(6) -0.00234(8)
O1 0.0224(9) 0.0125(8) 0.0265(10) -0.0046(7) 0.0070(7) -0.0020(7)
C1 0.0231(12) 0.0122(11) 0.0149(12) 0.0006(9) 0.0010(10) 0.0008(9)
C2 0.0296(14) 0.0120(11) 0.0137(12) 0.0008(9) 0.0012(10) -0.0014(10)
C3 0.0295(14) 0.0132(11) 0.0170(12) -0.0019(9) 0.0030(10) 0.0041(10)
C4 0.0222(12) 0.0178(12) 0.0141(12) 0.0033(9) 0.0014(9) 0.0045(10)
C5 0.0205(12) 0.0151(12) 0.0194(13) -0.0005(10) 0.0018(10) -0.0009(9)
C6 0.0228(13) 0.0122(11) 0.0173(12) 0.0002(9) 0.0027(10) 0.0002(9)
N7 0.0177(10) 0.0105(9) 0.0228(11) -0.0031(8) 0.0042(8) -0.0020(8)
C8 0.0162(12) 0.0131(11) 0.0255(13) -0.0041(10) 0.0073(10) -0.0018(9)
C9 0.0261(13) 0.0162(12) 0.0279(14) -0.0004(11) 0.0071(11) -0.0018(10)
C10 0.0364(15) 0.0140(12) 0.0419(17) 0.0011(13) 0.0081(13) -0.0060(12)
C11 0.0286(14) 0.0174(13) 0.0477(18) -0.0095(13) -0.0004(12) -0.0048(12)
C12 0.0226(13) 0.0274(14) 0.0339(16) -0.0067(12) -0.0055(12) 0.0000(11)
C13 0.0210(13) 0.0181(12) 0.0301(15) -0.0011(11) 0.0020(11) 0.0007(10)
C14 0.0349(15) 0.0120(12) 0.0270(15) -0.0010(10) 0.0042(12) -0.0029(10)
C15 0.0476(18) 0.0169(13) 0.0336(16) 0.0007(11) 0.0114(13) -0.0045(12)
C16 0.052(2) 0.0151(13) 0.0447(19) -0.0065(13) 0.0149(15) -0.0029(13)
C17 0.0459(18) 0.0210(14) 0.0376(18) -0.0053(13) -0.0027(14) -0.0106(13)
C18 0.0230(13) 0.0192(13) 0.0207(13) 0.0004(10) 0.0040(10) 0.0050(10)
C19 0.0335(15) 0.0325(16) 0.0222(14) -0.0010(12) 0.0079(12) -0.0018(12)
C20 0.0201(13) 0.0340(16) 0.0331(16) -0.0092(13) 0.0034(11) 0.0001(12)
C21 0.0333(16) 0.0285(15) 0.0460(19) 0.0088(14) 0.0118(14) 0.0142(13)
C22 0.055(2) 0.0189(14) 0.0284(16) 0.0028(12) 0.0060(14) -0.0055(13)
F23 0.1083(18) 0.0285(10) 0.0405(11) 0.0168(9) -0.0106(11) -0.0148(11)
F24 0.0429(11) 0.0407(10) 0.0312(10) 0.0041(8) -0.0069(8) -0.0051(8)
F25 0.0662(13) 0.0461(11) 0.0294(10) -0.0074(9) 0.0165(9) -0.0110(10)
O31 0.0183(9) 0.0127(8) 0.0270(10) -0.0028(7) 0.0062(7) -0.0017(7)
C31 0.0186(12) 0.0148(11) 0.0181(12) 0.0007(10) 0.0025(10) -0.0015(9)
C32 0.0184(12) 0.0114(11) 0.0200(13) 0.0004(9) 0.0012(9) 0.0002(9)
C33 0.0205(12) 0.0120(11) 0.0197(13) -0.0018(9) 0.0008(10) -0.0006(9)
C34 0.0188(12) 0.0175(12) 0.0163(12) 0.0012(10) 0.0002(9) -0.0014(9)
C35 0.0186(12) 0.0178(12) 0.0211(13) -0.0007(10) 0.0025(10) -0.0039(9)
C36 0.0198(12) 0.0143(11) 0.0196(13) -0.0008(10) 0.0014(10) -0.0006(9)
N37 0.0198(10) 0.0105(10) 0.0215(11) -0.0016(8) 0.0025(8) -0.0027(8)
C38 0.0179(12) 0.0120(11) 0.0258(13) -0.0040(10) 0.0076(10) -0.0015(9)
C39 0.0239(13) 0.0188(13) 0.0281(15) -0.0030(11) 0.0011(11) -0.0026(10)
C40 0.0330(16) 0.0245(14) 0.0347(17) -0.0101(13) -0.0023(13) -0.0093(12)
C41 0.0336(16) 0.0161(13) 0.0454(18) -0.0046(12) 0.0100(13) -0.0092(11)
C42 0.0359(16) 0.0190(13) 0.0343(16) 0.0025(12) 0.0092(13) -0.0036(12)
C43 0.0299(14) 0.0209(14) 0.0246(14) -0.0017(11) 0.0028(11) -0.0033(11)
C44 0.0195(12) 0.0113(11) 0.0281(14) -0.0012(10) 0.0013(10) -0.0016(9)
C45 0.0272(14) 0.0184(13) 0.0355(16) 0.0047(12) 0.0082(12) -0.0008(11)
C46 0.0219(13) 0.0191(13) 0.0368(16) -0.0040(12) -0.0022(11) -0.0023(10)
C47 0.0229(13) 0.0125(12) 0.0438(17) -0.0069(12) 0.0042(12) -0.0013(10)
C48 0.0165(12) 0.0159(12) 0.0227(13) 0.0002(10) 0.0049(10) -0.0008(9)
C49 0.0207(13) 0.0230(13) 0.0300(15) 0.0041(11) 0.0020(11) 0.0011(11)
C50 0.0260(14) 0.0204(13) 0.0227(14) 0.0000(10) 0.0059(11) 0.0012(10)
C51 0.0193(12) 0.0191(13) 0.0331(15) -0.0040(11) 0.0080(11) -0.0029(10)
C52 0.049(2) 0.0304(16) 0.0313(17) -0.0015(13) -0.0081(14) -0.0101(14)
F53 0.122(2) 0.0354(11) 0.0558(14) 0.0081(11) -0.0125(13) 0.0267(13)
F54 0.0872(17) 0.0476(12) 0.0371(11) 0.0006(10) -0.0273(11) -0.0155(11)
F55 0.0657(15) 0.108(2) 0.0429(13) 0.0351(13) -0.0051(11) -0.0366(14)
B60 0.0248(14) 0.0174(14) 0.0276(16) 0.0001(12) 0.0033(12) -0.0042(11)
F61 0.0405(10) 0.0185(8) 0.0455(11) -0.0052(7) -0.0010(8) -0.0026(7)
F62 0.0348(10) 0.0417(10) 0.0401(10) 0.0000(8) 0.0122(8) -0.0134(8)
F63 0.0392(10) 0.0259(9) 0.0303(9) 0.0050(7) 0.0039(7) 0.0079(7)
F64 0.0288(8) 0.0382(9) 0.0280(8) 0.0048(8) -0.0016(7) -0.0062(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'
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'
Pd Pd -0.9988 1.0072 '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
N7 Pd1 O1 82.35(7) . . ?
N7 Pd1 O31 97.36(7) . . ?
O1 Pd1 O31 179.70(8) . . ?
N7 Pd1 N37 177.17(8) . . ?
O1 Pd1 N37 100.10(7) . . ?
O31 Pd1 N37 80.19(7) . . ?
C1 O1 Pd1 112.57(14) . . ?
O1 C1 C2 122.5(2) . . ?
O1 C1 C6 117.6(2) . . ?
C2 C1 C6 119.9(2) . . ?
C3 C2 C1 116.3(2) . . ?
C3 C2 C14 123.4(2) . . ?
C1 C2 C14 120.4(2) . . ?
C2 C3 C4 124.7(2) . . ?
C5 C4 C3 118.5(2) . . ?
C5 C4 C18 122.4(2) . . ?
C3 C4 C18 119.0(2) . . ?
C4 C5 C6 119.8(2) . . ?
N7 C6 C5 125.5(2) . . ?
N7 C6 C1 113.7(2) . . ?
C5 C6 C1 120.7(2) . . ?
C6 N7 C8 123.0(2) . . ?
C6 N7 Pd1 113.70(16) . . ?
C8 N7 Pd1 122.17(15) . . ?
C13 C8 C9 120.3(2) . . ?
C13 C8 N7 117.5(2) . . ?
C9 C8 N7 122.1(2) . . ?
C10 C9 C8 119.0(3) . . ?
C10 C9 C22 119.8(2) . . ?
C8 C9 C22 121.2(2) . . ?
C11 C10 C9 120.5(3) . . ?
C12 C11 C10 120.2(3) . . ?
C11 C12 C13 120.5(3) . . ?
C8 C13 C12 119.5(2) . . ?
C16 C14 C17 108.4(2) . . ?
C16 C14 C2 111.8(2) . . ?
C17 C14 C2 110.4(2) . . ?
C16 C14 C15 107.4(2) . . ?
C17 C14 C15 109.5(2) . . ?
C2 C14 C15 109.3(2) . . ?
C4 C18 C20 111.7(2) . . ?
C4 C18 C19 107.7(2) . . ?
C20 C18 C19 108.4(2) . . ?
C4 C18 C21 111.5(2) . . ?
C20 C18 C21 108.1(2) . . ?
C19 C18 C21 109.4(2) . . ?
F23 C22 F24 106.3(3) . . ?
F23 C22 F25 105.8(2) . . ?
F24 C22 F25 106.1(2) . . ?
F23 C22 C9 112.3(2) . . ?
F24 C22 C9 114.0(2) . . ?
F25 C22 C9 111.7(3) . . ?
C31 O31 Pd1 115.06(15) . . ?
O31 C31 C32 122.8(2) . . ?
O31 C31 C36 117.0(2) . . ?
C32 C31 C36 120.1(2) . . ?
C33 C32 C31 115.7(2) . . ?
C33 C32 C44 125.5(2) . . ?
C31 C32 C44 118.8(2) . . ?
C32 C33 C34 125.3(2) . . ?
C35 C34 C33 119.5(2) . . ?
C35 C34 C48 123.1(2) . . ?
C33 C34 C48 117.4(2) . . ?
C34 C35 C36 119.7(2) . . ?
N37 C36 C35 127.1(2) . . ?
N37 C36 C31 113.2(2) . . ?
C35 C36 C31 119.7(2) . . ?
C36 N37 C38 121.0(2) . . ?
C36 N37 Pd1 114.30(16) . . ?
C38 N37 Pd1 124.00(15) . . ?
C43 C38 C39 120.3(2) . . ?
C43 C38 N37 117.6(2) . . ?
C39 C38 N37 122.0(2) . . ?
C38 C39 C40 118.7(3) . . ?
C38 C39 C52 121.2(2) . . ?
C40 C39 C52 120.1(3) . . ?
C41 C40 C39 120.9(3) . . ?
C40 C41 C42 120.0(3) . . ?
C41 C42 C43 120.0(3) . . ?
C38 C43 C42 120.1(3) . . ?
C47 C44 C32 110.8(2) . . ?
C47 C44 C45 108.0(2) . . ?
C32 C44 C45 110.4(2) . . ?
C47 C44 C46 108.2(2) . . ?
C32 C44 C46 109.5(2) . . ?
C45 C44 C46 109.9(2) . . ?
C34 C48 C51 111.1(2) . . ?
C34 C48 C50 108.8(2) . . ?
C51 C48 C50 108.7(2) . . ?
C34 C48 C49 109.9(2) . . ?
C51 C48 C49 108.5(2) . . ?
C50 C48 C49 109.8(2) . . ?
F53 C52 F54 106.2(3) . . ?
F53 C52 F55 106.0(3) . . ?
F54 C52 F55 106.8(3) . . ?
F53 C52 C39 111.7(3) . . ?
F54 C52 C39 112.7(2) . . ?
F55 C52 C39 112.9(3) . . ?
F62 B60 F64 111.1(2) . . ?
F62 B60 F61 109.5(2) . . ?
F64 B60 F61 109.3(2) . . ?
F62 B60 F63 109.6(2) . . ?
F64 B60 F63 109.3(2) . . ?
F61 B60 F63 108.0(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
Pd1 N7 1.966(2) . ?
Pd1 O1 1.9743(16) . ?
Pd1 O31 1.9969(16) . ?
Pd1 N37 2.011(2) . ?
O1 C1 1.313(3) . ?
C1 C2 1.427(3) . ?
C1 C6 1.443(3) . ?
C2 C3 1.376(4) . ?
C2 C14 1.540(3) . ?
C3 C4 1.445(3) . ?
C4 C5 1.362(3) . ?
C4 C18 1.528(3) . ?
C5 C6 1.417(3) . ?
C6 N7 1.345(3) . ?
N7 C8 1.436(3) . ?
C8 C13 1.387(4) . ?
C8 C9 1.404(3) . ?
C9 C10 1.390(4) . ?
C9 C22 1.487(4) . ?
C10 C11 1.384(4) . ?
C11 C12 1.373(4) . ?
C12 C13 1.391(4) . ?
C14 C16 1.533(4) . ?
C14 C17 1.538(4) . ?
C14 C15 1.541(4) . ?
C18 C20 1.536(4) . ?
C18 C19 1.537(4) . ?
C18 C21 1.538(4) . ?
C22 F23 1.341(3) . ?
C22 F24 1.343(4) . ?
C22 F25 1.349(4) . ?
O31 C31 1.255(3) . ?
C31 C32 1.450(3) . ?
C31 C36 1.491(3) . ?
C32 C33 1.350(3) . ?
C32 C44 1.536(3) . ?
C33 C34 1.478(3) . ?
C34 C35 1.353(3) . ?
C34 C48 1.524(3) . ?
C35 C36 1.424(3) . ?
C36 N37 1.316(3) . ?
N37 C38 1.444(3) . ?
C38 C43 1.383(4) . ?
C38 C39 1.396(4) . ?
C39 C40 1.400(4) . ?
C39 C52 1.499(4) . ?
C40 C41 1.376(4) . ?
C41 C42 1.382(4) . ?
C42 C43 1.390(4) . ?
C44 C47 1.533(3) . ?
C44 C45 1.538(4) . ?
C44 C46 1.544(4) . ?
C48 C51 1.538(3) . ?
C48 C50 1.539(4) . ?
C48 C49 1.544(3) . ?
C52 F53 1.323(4) . ?
C52 F54 1.325(3) . ?
C52 F55 1.326(4) . ?
B60 F62 1.380(3) . ?
B60 F64 1.391(3) . ?
B60 F61 1.395(3) . ?
B60 F63 1.403(3) . ?
|
1100982.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100982.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_1100982
loop_
_publ_author_name
'Swarnalatha Kokatam'
'Thomas Weyherm\"uller'
'Eberhard Bothe'
'Phalguni Chaudhuri'
'Karl Wieghardt'
_publ_section_title
;
Structural Characterization of Four Members of the Electron-Transfer Series
[PdII(L)2)2]n (L = o-Iminophenolate Derivative; n= 2-, 1-, 0, 1+, 2+).
Ligand Mixed Valency in the Monocation and Monoanion with S=1/2 Ground States
;
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3709
_journal_page_last 3717
_journal_paper_doi 10.1021/ic048292i
_journal_volume 44
_journal_year 2005
_chemical_formula_moiety '[C10 H10 Co]+, [C42 H48 F6 N2 O2 Pd]-'
_chemical_formula_sum 'C52 H58 Co F6 N2 O2 Pd'
_chemical_formula_weight 1022.33
_chemical_name_systematic
;
?
;
_space_group_IT_number 1
_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 67.012(5)
_cell_angle_beta 73.738(5)
_cell_angle_gamma 88.769(5)
_cell_formula_units_Z 1
_cell_length_a 10.1173(6)
_cell_length_b 10.4874(6)
_cell_length_c 12.6206(6)
_cell_measurement_temperature 100(2)
_cell_volume 1177.57(13)
_computing_cell_refinement 'Nonius Collect Software'
_computing_data_collection 'Nonius Collect Software'
_computing_data_reduction 'Nonius Collect Software'
_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_measurement_device_type 'Nonius Kappa-CCD'
_diffrn_measurement_method
'242 images at 1.5 deg. in phi, 406 images at 1.5 deg. in \w, 30 sec./frame'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'rotating anode'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0227
_diffrn_reflns_av_sigmaI/netI 0.0301
_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 18
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_number 31169
_diffrn_reflns_theta_full 31.02
_diffrn_reflns_theta_max 31.02
_diffrn_reflns_theta_min 3.14
_exptl_absorpt_coefficient_mu 0.800
_exptl_absorpt_correction_T_max 0.9474
_exptl_absorpt_correction_T_min 0.8608
_exptl_absorpt_correction_type 'Gaussian, face-indexed'
_exptl_crystal_colour 'dark green'
_exptl_crystal_density_diffrn 1.442
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description 'transparent parallelepiped'
_exptl_crystal_F_000 527
_exptl_crystal_size_max 0.20
_exptl_crystal_size_mid 0.17
_exptl_crystal_size_min 0.07
_refine_diff_density_max 1.788
_refine_diff_density_min -0.681
_refine_diff_density_rms 0.068
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack 0.278(11)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.024
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 604
_refine_ls_number_reflns 14161
_refine_ls_number_restraints 147
_refine_ls_restrained_S_all 1.030
_refine_ls_R_factor_all 0.0308
_refine_ls_R_factor_gt 0.0300
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0316P)^2^+0.9716P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0736
_refine_ls_wR_factor_ref 0.0742
_reflns_number_gt 13937
_reflns_number_total 14161
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file ic048292isi20041206_054204_3.cif
_cod_data_source_block 3
_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
The following automatic conversions were performed:
'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0316P)^2^+0.9716P] 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^)+(0.0316P)^2^+0.9716P] 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 1177.57(11)
_cod_database_code 1100982
loop_
_symmetry_equiv_pos_as_xyz
'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
Pd1 Pd 0.848210(9) 0.275421(9) 0.707199(9) 0.01543(3) Uani 1 d . . .
O1 O 0.91625(19) 0.0870(2) 0.76427(17) 0.0192(4) Uani 1 d . . .
C1 C 0.9961(3) 0.0588(3) 0.6744(2) 0.0165(5) Uani 1 d . . .
C2 C 1.0587(3) -0.0683(3) 0.6933(2) 0.0174(4) Uani 1 d . . .
C3 C 1.1467(3) -0.0814(3) 0.5910(3) 0.0190(5) Uani 1 d . . .
H3 H 1.1917 -0.1641 0.6022 0.023 Uiso 1 calc R . .
C4 C 1.1724(3) 0.0197(3) 0.4733(2) 0.0186(5) Uani 1 d . . .
C5 C 1.1042(3) 0.1393(3) 0.4554(3) 0.0207(5) Uani 1 d . . .
H5 H 1.1158 0.2069 0.3761 0.025 Uiso 1 calc R . .
C6 C 1.0179(3) 0.1600(3) 0.5549(2) 0.0168(4) Uani 1 d . . .
N7 N 0.9505(2) 0.2767(2) 0.54991(19) 0.0153(4) Uani 1 d D . .
C14 C 1.0259(3) -0.1865(3) 0.8185(3) 0.0209(5) Uani 1 d . . .
C15 C 1.0567(3) -0.1383(3) 0.9099(3) 0.0243(5) Uani 1 d . . .
H15A H 1.0432 -0.2184 0.9868 0.036 Uiso 1 calc R . .
H15B H 0.9939 -0.0694 0.9217 0.036 Uiso 1 calc R . .
H15C H 1.1526 -0.0964 0.8797 0.036 Uiso 1 calc R . .
C16 C 0.8713(3) -0.2412(3) 0.8607(3) 0.0269(5) Uani 1 d . . .
H16A H 0.8489 -0.3159 0.9416 0.040 Uiso 1 calc R . .
H16B H 0.8530 -0.2772 0.8047 0.040 Uiso 1 calc R . .
H16C H 0.8140 -0.1651 0.8626 0.040 Uiso 1 calc R . .
C17 C 1.1119(4) -0.3098(3) 0.8177(3) 0.0314(6) Uani 1 d . . .
H17A H 1.0889 -0.3828 0.8994 0.047 Uiso 1 calc R . .
H17B H 1.2107 -0.2777 0.7897 0.047 Uiso 1 calc R . .
H17C H 1.0907 -0.3470 0.7636 0.047 Uiso 1 calc R . .
C18 C 1.2762(3) 0.0037(3) 0.3643(2) 0.0227(5) Uani 1 d . . .
C19 C 1.2063(3) 0.0233(4) 0.2666(3) 0.0316(6) Uani 1 d . . .
H19A H 1.1766 0.1173 0.2389 0.047 Uiso 1 calc R . .
H19B H 1.1256 -0.0455 0.2998 0.047 Uiso 1 calc R . .
H19C H 1.2720 0.0107 0.1986 0.047 Uiso 1 calc R . .
C20 C 1.4004(3) 0.1159(4) 0.3143(3) 0.0358(7) Uani 1 d . . .
H20A H 1.3676 0.2086 0.2885 0.054 Uiso 1 calc R . .
H20B H 1.4678 0.1068 0.2454 0.054 Uiso 1 calc R . .
H20C H 1.4442 0.1032 0.3774 0.054 Uiso 1 calc R . .
C21 C 1.3326(4) -0.1379(4) 0.3989(3) 0.0358(7) Uani 1 d . . .
H21A H 1.2558 -0.2114 0.4340 0.054 Uiso 1 calc R . .
H21B H 1.3822 -0.1491 0.4580 0.054 Uiso 1 calc R . .
H21C H 1.3961 -0.1443 0.3270 0.054 Uiso 1 calc R . .
O31 O 0.78453(19) 0.4634(2) 0.64541(17) 0.0178(4) Uani 1 d . . .
C31 C 0.7048(2) 0.4985(3) 0.7324(2) 0.0149(4) Uani 1 d . . .
C32 C 0.6475(3) 0.6263(3) 0.7095(2) 0.0170(4) Uani 1 d . . .
C33 C 0.5642(3) 0.6484(3) 0.8084(2) 0.0170(4) Uani 1 d . . .
H33 H 0.5245 0.7343 0.7936 0.020 Uiso 1 calc R . .
C34 C 0.5356(3) 0.5518(3) 0.9279(2) 0.0175(4) Uani 1 d . . .
C35 C 0.5952(3) 0.4268(3) 0.9495(2) 0.0185(5) Uani 1 d . . .
H35 H 0.5777 0.3594 1.0297 0.022 Uiso 1 calc R . .
C36 C 0.6813(2) 0.3997(3) 0.8534(2) 0.0158(4) Uani 1 d . . .
N37 N 0.7422(2) 0.2780(3) 0.8655(2) 0.0202(5) Uani 1 d D . .
C44 C 0.6798(3) 0.7375(3) 0.5802(2) 0.0233(5) Uani 1 d . . .
C45 C 0.6313(4) 0.6791(3) 0.5005(3) 0.0306(6) Uani 1 d . . .
H45A H 0.5327 0.6460 0.5367 0.046 Uiso 1 calc R . .
H45B H 0.6845 0.6016 0.4946 0.046 Uiso 1 calc R . .
H45C H 0.6461 0.7526 0.4199 0.046 Uiso 1 calc R . .
C46 C 0.6074(4) 0.8686(3) 0.5753(3) 0.0323(6) Uani 1 d . . .
H46A H 0.5071 0.8440 0.6086 0.048 Uiso 1 calc R . .
H46B H 0.6294 0.9362 0.4915 0.048 Uiso 1 calc R . .
H46C H 0.6393 0.9094 0.6227 0.048 Uiso 1 calc R . .
C47 C 0.8359(3) 0.7800(3) 0.5282(3) 0.0349(7) Uani 1 d . . .
H47A H 0.8656 0.8232 0.5751 0.052 Uiso 1 calc R . .
H47B H 0.8571 0.8467 0.4441 0.052 Uiso 1 calc R . .
H47C H 0.8848 0.6974 0.5321 0.052 Uiso 1 calc R . .
C48 C 0.4381(3) 0.5766(3) 1.0337(2) 0.0225(5) Uani 1 d . . .
C49 C 0.5076(3) 0.5456(3) 1.1348(3) 0.0251(5) Uani 1 d . . .
H49A H 0.4461 0.5648 1.2009 0.038 Uiso 1 calc R . .
H49B H 0.5952 0.6049 1.1027 0.038 Uiso 1 calc R . .
H49C H 0.5257 0.4476 1.1646 0.038 Uiso 1 calc R . .
C50 C 0.3037(3) 0.4785(4) 1.0838(3) 0.0315(6) Uani 1 d . . .
H50A H 0.2445 0.4881 1.1559 0.047 Uiso 1 calc R . .
H50B H 0.3265 0.3821 1.1048 0.047 Uiso 1 calc R . .
H50C H 0.2548 0.5029 1.0227 0.047 Uiso 1 calc R . .
C51 C 0.4014(4) 0.7276(3) 0.9969(3) 0.0371(7) Uani 1 d . . .
H51A H 0.3463 0.7410 1.0684 0.056 Uiso 1 calc R . .
H51B H 0.3480 0.7471 0.9393 0.056 Uiso 1 calc R . .
H51C H 0.4867 0.7911 0.9593 0.056 Uiso 1 calc R . .
Co1 Co 0.35202(3) 1.24539(4) 0.73426(3) 0.02481(8) Uani 1 d . . .
C61 C 0.4091(3) 1.0893(3) 0.6801(3) 0.0407(7) Uani 1 d . . .
H61 H 0.3726 0.9945 0.7233 0.049 Uiso 1 calc R . .
C62 C 0.3589(3) 1.1903(4) 0.5947(3) 0.0399(8) Uani 1 d . . .
H62 H 0.2833 1.1764 0.5683 0.048 Uiso 1 calc R . .
C63 C 0.4395(3) 1.3156(4) 0.5547(3) 0.0379(7) Uani 1 d . . .
H63 H 0.4260 1.4022 0.4974 0.045 Uiso 1 calc R . .
C64 C 0.5442(3) 1.2944(4) 0.6123(3) 0.0309(6) Uani 1 d . . .
H64 H 0.6139 1.3624 0.5999 0.037 Uiso 1 calc R . .
C65 C 0.5254(3) 1.1525(3) 0.6921(3) 0.0352(6) Uani 1 d . . .
H65 H 0.5796 1.1075 0.7440 0.042 Uiso 1 calc R . .
C66 C 0.1520(3) 1.2310(4) 0.8317(3) 0.0329(7) Uani 1 d . . .
H66 H 0.0747 1.1880 0.8251 0.039 Uiso 1 calc R . .
C67 C 0.2054(4) 1.3711(4) 0.7666(4) 0.0457(8) Uani 1 d . . .
H67 H 0.1718 1.4410 0.7083 0.055 Uiso 1 calc R . .
C68 C 0.3246(4) 1.3873(5) 0.8075(4) 0.0522(11) Uani 1 d . . .
H68 H 0.3831 1.4705 0.7796 0.063 Uiso 1 calc R . .
C69 C 0.3362(3) 1.2590(5) 0.8942(3) 0.0528(10) Uani 1 d . . .
H69 H 0.4038 1.2395 0.9362 0.063 Uiso 1 calc R . .
C70 C 0.2324(3) 1.1653(5) 0.9084(3) 0.0440(8) Uani 1 d . . .
H70 H 0.2175 1.0700 0.9624 0.053 Uiso 1 calc R . .
C38 C 0.7467(4) 0.1676(3) 0.9721(2) 0.0166(8) Uani 0.5207(16) d PGD A 1
C39 C 0.8184(4) 0.1886(3) 1.0441(3) 0.0229(6) Uani 0.5207(16) d PGD A 1
C40 C 0.8308(4) 0.0773(4) 1.1455(3) 0.053(2) Uani 0.5207(16) d PG A 1
H40 H 0.8797 0.0917 1.1947 0.063 Uiso 0.5207(16) calc PR A 1
C41 C 0.7714(5) -0.0550(3) 1.1748(3) 0.0486(13) Uani 0.5207(16) d PG A 1
H41 H 0.7799 -0.1311 1.2441 0.058 Uiso 0.5207(16) calc PR A 1
C42 C 0.6998(4) -0.0760(3) 1.1028(3) 0.0372(9) Uani 0.5207(16) d PG A 1
H42 H 0.6593 -0.1664 1.1229 0.045 Uiso 0.5207(16) calc PR A 1
C43 C 0.6874(4) 0.0353(3) 1.0015(3) 0.0266(7) Uani 0.5207(16) d PG A 1
H43 H 0.6384 0.0210 0.9522 0.032 Uiso 0.5207(16) calc PR A 1
C52 C 0.8873(5) 0.3251(5) 1.0196(4) 0.0285(7) Uani 0.5207(16) d PD A 1
F53 F 1.0008(3) 0.3113(4) 1.0591(3) 0.0356(5) Uani 0.5207(16) d PD A 1
F54 F 0.9308(3) 0.4108(4) 0.9037(3) 0.0365(5) Uani 0.5207(16) d PD A 1
F55 F 0.8047(4) 0.3966(4) 1.0762(3) 0.0475(7) Uani 0.5207(16) d PD A 1
C8 C 0.92811(18) 0.36617(17) 0.43704(14) 0.0190(6) Uani 0.8336(18) d PGD B 1
C9 C 0.99803(17) 0.49881(18) 0.37331(16) 0.0206(5) Uani 0.8336(18) d PGD B 1
C10 C 0.9634(2) 0.59188(17) 0.27356(16) 0.0321(7) Uani 0.8336(18) d PG B 1
H10 H 1.0112 0.6825 0.2300 0.038 Uiso 0.8336(18) calc PR B 1
C11 C 0.8589(2) 0.5523(2) 0.23755(16) 0.0395(8) Uani 0.8336(18) d PG B 1
H11 H 0.8353 0.6159 0.1694 0.047 Uiso 0.8336(18) calc PR B 1
C12 C 0.7890(2) 0.4197(2) 0.30128(18) 0.0393(8) Uani 0.8336(18) d PG B 1
H12 H 0.7176 0.3926 0.2767 0.047 Uiso 0.8336(18) calc PR B 1
C13 C 0.82361(19) 0.32659(18) 0.40103(17) 0.0275(6) Uani 0.8336(18) d PG B 1
H13 H 0.7758 0.2359 0.4446 0.033 Uiso 0.8336(18) calc PR B 1
C22 C 1.1206(3) 0.5386(3) 0.4020(2) 0.0234(5) Uani 0.8336(18) d PD B 1
F23 F 1.1893(2) 0.6605(2) 0.31787(17) 0.0380(5) Uani 0.8336(18) d PD B 1
F24 F 1.21509(17) 0.4451(2) 0.40784(18) 0.0306(4) Uani 0.8336(18) d PD B 1
F25 F 1.0888(2) 0.5513(2) 0.50814(16) 0.0321(4) Uani 0.8336(18) d PD B 1
C38X C 0.7834(4) 0.2109(3) 0.9769(3) 0.0166(8) Uani 0.4793(16) d PGD A 2
C39X C 0.7375(4) 0.0719(3) 1.0501(3) 0.0229(6) Uani 0.4793(16) d PGD A 2
C40X C 0.7816(5) 0.0043(3) 1.1513(3) 0.053(2) Uani 0.4793(16) d PG A 2
H40X H 0.7502 -0.0908 1.2014 0.063 Uiso 0.4793(16) calc PR A 2
C41X C 0.8716(5) 0.0757(4) 1.1793(3) 0.0486(13) Uani 0.4793(16) d PG A 2
H41X H 0.9018 0.0295 1.2485 0.058 Uiso 0.4793(16) calc PR A 2
C42X C 0.9175(4) 0.2147(4) 1.1061(3) 0.0372(9) Uani 0.4793(16) d PG A 2
H42X H 0.9791 0.2636 1.1253 0.045 Uiso 0.4793(16) calc PR A 2
C43X C 0.8735(4) 0.2823(3) 1.0049(3) 0.0266(7) Uani 0.4793(16) d PG A 2
H43X H 0.9048 0.3774 0.9548 0.032 Uiso 0.4793(16) calc PR A 2
C52X C 0.6281(5) -0.0026(5) 1.0328(4) 0.0285(7) Uani 0.4793(16) d PD A 2
F53X F 0.6589(4) -0.0147(4) 0.9270(3) 0.0356(5) Uani 0.4793(16) d PD A 2
F54X F 0.5105(3) 0.0612(4) 1.0405(3) 0.0365(5) Uani 0.4793(16) d PD A 2
F55X F 0.5933(5) -0.1330(4) 1.1186(3) 0.0475(7) Uani 0.4793(16) d PD A 2
C8X C 0.9628(11) 0.3964(8) 0.4431(7) 0.0190(6) Uani 0.1664(18) d PGD B 2
C9X C 0.8867(11) 0.3834(8) 0.3710(9) 0.0206(5) Uani 0.1664(18) d PGD B 2
C10X C 0.8799(12) 0.4982(11) 0.2697(9) 0.0321(7) Uani 0.1664(18) d PG B 2
H10X H 0.8279 0.4893 0.2204 0.038 Uiso 0.1664(18) calc PR B 2
C11X C 0.9492(13) 0.6260(9) 0.2404(9) 0.0395(8) Uani 0.1664(18) d PG B 2
H11X H 0.9446 0.7044 0.1712 0.047 Uiso 0.1664(18) calc PR B 2
C12X C 1.0253(12) 0.6390(8) 0.3125(10) 0.0393(8) Uani 0.1664(18) d PG B 2
H12X H 1.0726 0.7263 0.2925 0.047 Uiso 0.1664(18) calc PR B 2
C13X C 1.0321(11) 0.5242(10) 0.4138(9) 0.0275(6) Uani 0.1664(18) d PG B 2
H13X H 1.0840 0.5331 0.4631 0.033 Uiso 0.1664(18) calc PR B 2
C22X C 0.8197(9) 0.2492(9) 0.3897(8) 0.0234(5) Uani 0.1664(18) d PD B 2
F23X F 0.7727(11) 0.1554(10) 0.5044(6) 0.0380(5) Uani 0.1664(18) d PD B 2
F24X F 0.9003(8) 0.1822(10) 0.3271(8) 0.0306(4) Uani 0.1664(18) d PD B 2
F25X F 0.7102(8) 0.2796(10) 0.3463(7) 0.0321(4) Uani 0.1664(18) 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
Pd1 0.01465(6) 0.01472(6) 0.01433(6) -0.00439(4) -0.00275(4) 0.00543(4)
O1 0.0215(9) 0.0153(9) 0.0143(8) -0.0019(7) -0.0016(7) 0.0068(7)
C1 0.0158(10) 0.0159(12) 0.0174(11) -0.0074(9) -0.0035(8) 0.0048(8)
C2 0.0183(10) 0.0142(11) 0.0201(11) -0.0052(9) -0.0088(9) 0.0050(8)
C3 0.0171(10) 0.0211(12) 0.0240(11) -0.0141(10) -0.0072(8) 0.0069(8)
C4 0.0161(10) 0.0214(11) 0.0192(10) -0.0087(9) -0.0060(8) 0.0039(8)
C5 0.0215(11) 0.0201(12) 0.0182(11) -0.0067(9) -0.0042(9) 0.0079(9)
C6 0.0174(10) 0.0150(11) 0.0152(10) -0.0033(9) -0.0048(9) 0.0051(8)
N7 0.0176(10) 0.0098(10) 0.0142(10) -0.0006(8) -0.0047(8) 0.0068(8)
C14 0.0229(11) 0.0174(12) 0.0214(11) -0.0066(9) -0.0068(9) 0.0041(9)
C15 0.0270(12) 0.0243(13) 0.0191(12) -0.0041(10) -0.0100(10) 0.0061(10)
C16 0.0262(12) 0.0194(12) 0.0291(13) -0.0037(10) -0.0077(10) -0.0019(9)
C17 0.0414(16) 0.0211(13) 0.0293(13) -0.0058(11) -0.0141(12) 0.0137(11)
C18 0.0234(11) 0.0262(12) 0.0200(10) -0.0128(10) -0.0042(9) 0.0096(9)
C19 0.0347(14) 0.0412(17) 0.0264(13) -0.0197(12) -0.0116(11) 0.0099(12)
C20 0.0237(12) 0.0481(19) 0.0326(14) -0.0199(14) 0.0020(10) 0.0023(11)
C21 0.0425(16) 0.0393(17) 0.0316(13) -0.0226(13) -0.0090(12) 0.0201(13)
O31 0.0191(8) 0.0172(9) 0.0148(8) -0.0064(8) -0.0020(7) 0.0081(7)
C31 0.0129(9) 0.0146(11) 0.0141(10) -0.0023(9) -0.0042(8) 0.0021(8)
C32 0.0158(10) 0.0160(11) 0.0184(10) -0.0071(9) -0.0039(8) 0.0036(8)
C33 0.0172(10) 0.0139(10) 0.0198(10) -0.0061(9) -0.0063(8) 0.0039(8)
C34 0.0151(9) 0.0214(11) 0.0217(11) -0.0144(9) -0.0060(8) 0.0064(8)
C35 0.0187(10) 0.0220(12) 0.0132(10) -0.0064(9) -0.0037(8) 0.0055(9)
C36 0.0139(10) 0.0163(11) 0.0168(10) -0.0071(9) -0.0035(8) 0.0049(8)
N37 0.0217(11) 0.0213(13) 0.0171(11) -0.0094(10) -0.0029(9) 0.0091(9)
C44 0.0274(12) 0.0152(11) 0.0182(11) 0.0017(9) -0.0058(9) 0.0083(9)
C45 0.0432(16) 0.0293(15) 0.0208(13) -0.0093(12) -0.0140(12) 0.0176(12)
C46 0.0422(16) 0.0188(13) 0.0292(14) -0.0044(11) -0.0091(12) 0.0139(11)
C47 0.0294(13) 0.0245(13) 0.0311(14) 0.0036(11) -0.0007(11) 0.0021(10)
C48 0.0194(10) 0.0322(14) 0.0214(11) -0.0156(10) -0.0077(8) 0.0105(9)
C49 0.0243(11) 0.0348(14) 0.0225(11) -0.0175(11) -0.0077(9) 0.0064(10)
C50 0.0167(10) 0.0545(19) 0.0284(12) -0.0248(13) -0.0027(9) 0.0049(11)
C51 0.0515(18) 0.0375(16) 0.0294(13) -0.0207(12) -0.0137(13) 0.0300(14)
Co1 0.01438(13) 0.0331(2) 0.0350(2) -0.02331(17) -0.00529(14) 0.00238(14)
C61 0.0241(12) 0.0421(16) 0.0590(19) -0.0356(15) 0.0056(12) -0.0007(11)
C62 0.0212(12) 0.069(2) 0.0502(18) -0.0474(19) -0.0067(12) 0.0041(13)
C63 0.0252(12) 0.059(2) 0.0350(15) -0.0267(16) -0.0062(11) 0.0068(13)
C64 0.0155(10) 0.0459(17) 0.0385(15) -0.0253(13) -0.0067(10) 0.0060(10)
C65 0.0187(11) 0.0424(16) 0.0466(16) -0.0221(13) -0.0072(10) 0.0100(10)
C66 0.0170(11) 0.0445(17) 0.0482(17) -0.0344(15) -0.0032(10) 0.0028(10)
C67 0.0377(16) 0.0455(19) 0.058(2) -0.0354(17) 0.0005(14) 0.0122(13)
C68 0.0393(18) 0.059(2) 0.066(2) -0.052(2) 0.0132(16) -0.0206(16)
C69 0.0330(15) 0.092(3) 0.0467(18) -0.047(2) -0.0028(13) -0.0110(16)
C70 0.0282(13) 0.073(3) 0.0368(16) -0.0319(17) -0.0044(12) 0.0013(15)
C38 0.0227(19) 0.0116(18) 0.0100(12) -0.0012(12) -0.0015(12) 0.0081(13)
C39 0.0297(16) 0.0226(16) 0.0133(13) -0.0060(12) -0.0039(11) 0.0106(13)
C40 0.065(4) 0.067(5) 0.0103(14) 0.000(3) -0.013(2) 0.040(4)
C41 0.057(3) 0.054(3) 0.0158(18) 0.0023(19) -0.0080(18) 0.030(2)
C42 0.0337(19) 0.043(2) 0.0241(16) -0.0062(16) -0.0037(14) 0.0080(16)
C43 0.0214(15) 0.030(2) 0.0294(17) -0.0138(15) -0.0062(13) 0.0061(14)
C52 0.0245(16) 0.033(2) 0.0273(16) -0.0163(15) 0.0001(13) 0.0050(15)
F53 0.0317(11) 0.0401(13) 0.0377(12) -0.0193(11) -0.0083(9) -0.0018(10)
F54 0.0212(10) 0.0441(14) 0.0475(14) -0.0276(12) -0.0012(9) -0.0050(9)
F55 0.0615(18) 0.0379(15) 0.0397(14) -0.0204(12) -0.0017(13) -0.0079(13)
C8 0.0161(13) 0.0236(14) 0.0181(12) -0.0101(11) -0.0040(10) 0.0068(11)
C9 0.0202(11) 0.0241(13) 0.0144(11) -0.0055(9) -0.0043(9) 0.0069(9)
C10 0.0343(15) 0.0366(17) 0.0152(12) -0.0008(12) -0.0068(11) 0.0152(13)
C11 0.0381(17) 0.049(2) 0.0177(13) 0.0010(14) -0.0097(12) 0.0151(15)
C12 0.0226(13) 0.059(2) 0.0270(15) -0.0051(15) -0.0117(11) 0.0041(14)
C13 0.0190(12) 0.0352(16) 0.0225(12) -0.0045(12) -0.0074(10) 0.0002(11)
C22 0.0253(12) 0.0209(12) 0.0192(11) -0.0066(9) -0.0013(9) 0.0005(10)
F23 0.0477(11) 0.0278(10) 0.0265(9) -0.0070(7) 0.0028(8) -0.0147(8)
F24 0.0174(7) 0.0369(10) 0.0422(10) -0.0202(8) -0.0099(7) 0.0067(7)
F25 0.0307(9) 0.0427(11) 0.0233(8) -0.0180(8) -0.0012(7) -0.0024(8)
C38X 0.0227(19) 0.0116(18) 0.0100(12) -0.0012(12) -0.0015(12) 0.0081(13)
C39X 0.0297(16) 0.0226(16) 0.0133(13) -0.0060(12) -0.0039(11) 0.0106(13)
C40X 0.065(4) 0.067(5) 0.0103(14) 0.000(3) -0.013(2) 0.040(4)
C41X 0.057(3) 0.054(3) 0.0158(18) 0.0023(19) -0.0080(18) 0.030(2)
C42X 0.0337(19) 0.043(2) 0.0241(16) -0.0062(16) -0.0037(14) 0.0080(16)
C43X 0.0214(15) 0.030(2) 0.0294(17) -0.0138(15) -0.0062(13) 0.0061(14)
C52X 0.0245(16) 0.033(2) 0.0273(16) -0.0163(15) 0.0001(13) 0.0050(15)
F53X 0.0317(11) 0.0401(13) 0.0377(12) -0.0193(11) -0.0083(9) -0.0018(10)
F54X 0.0212(10) 0.0441(14) 0.0475(14) -0.0276(12) -0.0012(9) -0.0050(9)
F55X 0.0615(18) 0.0379(15) 0.0397(14) -0.0204(12) -0.0017(13) -0.0079(13)
C8X 0.0161(13) 0.0236(14) 0.0181(12) -0.0101(11) -0.0040(10) 0.0068(11)
C9X 0.0202(11) 0.0241(13) 0.0144(11) -0.0055(9) -0.0043(9) 0.0069(9)
C10X 0.0343(15) 0.0366(17) 0.0152(12) -0.0008(12) -0.0068(11) 0.0152(13)
C11X 0.0381(17) 0.049(2) 0.0177(13) 0.0010(14) -0.0097(12) 0.0151(15)
C12X 0.0226(13) 0.059(2) 0.0270(15) -0.0051(15) -0.0117(11) 0.0041(14)
C13X 0.0190(12) 0.0352(16) 0.0225(12) -0.0045(12) -0.0074(10) 0.0002(11)
C22X 0.0253(12) 0.0209(12) 0.0192(11) -0.0066(9) -0.0013(9) 0.0005(10)
F23X 0.0477(11) 0.0278(10) 0.0265(9) -0.0070(7) 0.0028(8) -0.0147(8)
F24X 0.0174(7) 0.0369(10) 0.0422(10) -0.0202(8) -0.0099(7) 0.0067(7)
F25X 0.0307(9) 0.0427(11) 0.0233(8) -0.0180(8) -0.0012(7) -0.0024(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'
F F 0.0171 0.0103 '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'
Pd Pd -0.9988 1.0072 '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
N7 Pd1 O31 96.62(8) . . ?
N7 Pd1 N37 178.71(12) . . ?
O31 Pd1 N37 82.10(9) . . ?
N7 Pd1 O1 81.59(8) . . ?
O31 Pd1 O1 178.20(9) . . ?
N37 Pd1 O1 99.68(9) . . ?
C1 O1 Pd1 112.61(17) . . ?
O1 C1 C6 117.9(2) . . ?
O1 C1 C2 122.7(2) . . ?
C6 C1 C2 119.4(2) . . ?
C3 C2 C1 116.8(2) . . ?
C3 C2 C14 121.9(2) . . ?
C1 C2 C14 121.3(2) . . ?
C4 C3 C2 124.1(2) . . ?
C5 C4 C3 118.5(2) . . ?
C5 C4 C18 119.4(2) . . ?
C3 C4 C18 122.1(2) . . ?
C4 C5 C6 119.9(3) . . ?
N7 C6 C5 125.6(2) . . ?
N7 C6 C1 113.2(2) . . ?
C5 C6 C1 121.2(2) . . ?
C6 N7 C8X 124.5(5) . . ?
C6 N7 C8 118.3(2) . . ?
C8X N7 C8 20.8(4) . . ?
C6 N7 Pd1 114.65(17) . . ?
C8X N7 Pd1 120.6(5) . . ?
C8 N7 Pd1 124.53(15) . . ?
C2 C14 C15 111.7(2) . . ?
C2 C14 C17 111.8(2) . . ?
C15 C14 C17 107.1(2) . . ?
C2 C14 C16 108.9(2) . . ?
C15 C14 C16 109.6(2) . . ?
C17 C14 C16 107.6(2) . . ?
C21 C18 C19 108.9(2) . . ?
C21 C18 C4 112.2(2) . . ?
C19 C18 C4 109.9(2) . . ?
C21 C18 C20 107.6(2) . . ?
C19 C18 C20 109.9(3) . . ?
C4 C18 C20 108.3(2) . . ?
C31 O31 Pd1 113.51(16) . . ?
O31 C31 C32 123.4(2) . . ?
O31 C31 C36 116.7(2) . . ?
C32 C31 C36 119.9(2) . . ?
C33 C32 C31 117.5(2) . . ?
C33 C32 C44 122.1(2) . . ?
C31 C32 C44 120.4(2) . . ?
C32 C33 C34 124.0(2) . . ?
C35 C34 C33 117.9(2) . . ?
C35 C34 C48 119.4(2) . . ?
C33 C34 C48 122.6(2) . . ?
C34 C35 C36 120.5(2) . . ?
N37 C36 C35 124.7(3) . . ?
N37 C36 C31 115.1(2) . . ?
C35 C36 C31 120.2(2) . . ?
C36 N37 C38 128.0(2) . . ?
C36 N37 C38X 115.2(2) . . ?
C38 N37 C38X 24.81(17) . . ?
C36 N37 Pd1 112.56(18) . . ?
C38 N37 Pd1 119.2(2) . . ?
C38X N37 Pd1 123.6(2) . . ?
C47 C44 C46 107.9(3) . . ?
C47 C44 C32 109.5(2) . . ?
C46 C44 C32 111.9(2) . . ?
C47 C44 C45 109.4(3) . . ?
C46 C44 C45 108.1(2) . . ?
C32 C44 C45 110.0(2) . . ?
C34 C48 C51 112.2(2) . . ?
C34 C48 C50 109.2(2) . . ?
C51 C48 C50 108.9(2) . . ?
C34 C48 C49 109.9(2) . . ?
C51 C48 C49 107.6(2) . . ?
C50 C48 C49 109.0(2) . . ?
C68 Co1 C63 117.35(17) . . ?
C68 Co1 C61 167.90(17) . . ?
C63 Co1 C61 67.70(15) . . ?
C68 Co1 C67 42.82(17) . . ?
C63 Co1 C67 108.14(16) . . ?
C61 Co1 C67 148.36(14) . . ?
C68 Co1 C66 69.18(13) . . ?
C63 Co1 C66 130.43(13) . . ?
C61 Co1 C66 116.87(12) . . ?
C67 Co1 C66 40.54(14) . . ?
C68 Co1 C70 67.34(17) . . ?
C63 Co1 C70 169.38(13) . . ?
C61 Co1 C70 109.77(16) . . ?
C67 Co1 C70 68.23(16) . . ?
C66 Co1 C70 40.50(14) . . ?
C68 Co1 C65 128.26(15) . . ?
C63 Co1 C65 68.28(14) . . ?
C61 Co1 C65 41.46(12) . . ?
C67 Co1 C65 168.71(15) . . ?
C66 Co1 C65 149.74(14) . . ?
C70 Co1 C65 117.22(15) . . ?
C68 Co1 C64 107.32(14) . . ?
C63 Co1 C64 40.76(12) . . ?
C61 Co1 C64 68.74(12) . . ?
C67 Co1 C64 129.79(15) . . ?
C66 Co1 C64 168.78(15) . . ?
C70 Co1 C64 149.13(13) . . ?
C65 Co1 C64 40.66(13) . . ?
C68 Co1 C69 40.13(18) . . ?
C63 Co1 C69 149.78(15) . . ?
C61 Co1 C69 130.29(17) . . ?
C67 Co1 C69 69.53(17) . . ?
C66 Co1 C69 68.29(13) . . ?
C70 Co1 C69 39.63(14) . . ?
C65 Co1 C69 107.82(15) . . ?
C64 Co1 C69 116.41(13) . . ?
C68 Co1 C62 150.5(2) . . ?
C63 Co1 C62 40.21(15) . . ?
C61 Co1 C62 40.03(15) . . ?
C67 Co1 C62 116.15(16) . . ?
C66 Co1 C62 109.00(12) . . ?
C70 Co1 C62 131.36(15) . . ?
C65 Co1 C62 68.57(13) . . ?
C64 Co1 C62 68.44(13) . . ?
C69 Co1 C62 168.60(18) . . ?
C62 C61 C65 108.5(3) . . ?
C62 C61 Co1 70.69(18) . . ?
C65 C61 Co1 69.49(16) . . ?
C61 C62 C63 107.7(3) . . ?
C61 C62 Co1 69.28(17) . . ?
C63 C62 Co1 68.89(18) . . ?
C62 C63 C64 109.7(3) . . ?
C62 C63 Co1 70.9(2) . . ?
C64 C63 Co1 70.57(19) . . ?
C63 C64 C65 106.8(3) . . ?
C63 C64 Co1 68.67(17) . . ?
C65 C64 Co1 69.24(16) . . ?
C64 C65 C61 107.3(3) . . ?
C64 C65 Co1 70.10(16) . . ?
C61 C65 Co1 69.05(15) . . ?
C70 C66 C67 108.2(3) . . ?
C70 C66 Co1 69.83(17) . . ?
C67 C66 Co1 69.69(17) . . ?
C66 C67 C68 105.7(4) . . ?
C66 C67 Co1 69.77(17) . . ?
C68 C67 Co1 68.2(2) . . ?
C69 C68 C67 107.9(3) . . ?
C69 C68 Co1 70.9(2) . . ?
C67 C68 Co1 68.99(17) . . ?
C70 C69 C68 108.0(3) . . ?
C70 C69 Co1 69.71(18) . . ?
C68 C69 Co1 68.9(2) . . ?
C69 C70 C66 110.2(4) . . ?
C69 C70 Co1 70.7(2) . . ?
C66 C70 Co1 69.68(19) . . ?
C39 C38 C43 120.0 . . ?
C39 C38 N37 119.9(2) . . ?
C43 C38 N37 119.9(2) . . ?
C40 C39 C38 120.0 . . ?
C40 C39 C52 115.8(3) . . ?
C38 C39 C52 124.2(3) . . ?
C39 C40 C41 120.0 . . ?
C42 C41 C40 120.0 . . ?
C43 C42 C41 120.0 . . ?
C42 C43 C38 120.0 . . ?
F54 C52 F55 105.9(4) . . ?
F54 C52 F53 105.6(3) . . ?
F55 C52 F53 104.9(4) . . ?
F54 C52 C39 114.6(4) . . ?
F55 C52 C39 112.7(4) . . ?
F53 C52 C39 112.4(4) . . ?
C9 C8 C13 120.0 . . ?
C9 C8 N7 119.79(15) . . ?
C13 C8 N7 119.65(15) . . ?
C10 C9 C8 120.0 . . ?
C10 C9 C22 118.76(15) . . ?
C8 C9 C22 120.91(15) . . ?
C9 C10 C11 120.0 . . ?
C12 C11 C10 120.0 . . ?
C13 C12 C11 120.0 . . ?
C12 C13 C8 120.0 . . ?
F25 C22 F23 106.4(2) . . ?
F25 C22 F24 105.6(2) . . ?
F23 C22 F24 105.4(2) . . ?
F25 C22 C9 113.8(2) . . ?
F23 C22 C9 112.2(2) . . ?
F24 C22 C9 112.8(2) . . ?
C39X C38X C43X 120.0 . . ?
C39X C38X N37 119.0(2) . . ?
C43X C38X N37 120.9(2) . . ?
C40X C39X C38X 120.0 . . ?
C40X C39X C52X 117.9(3) . . ?
C38X C39X C52X 121.6(3) . . ?
C39X C40X C41X 120.0 . . ?
C42X C41X C40X 120.0 . . ?
C41X C42X C43X 120.0 . . ?
C42X C43X C38X 120.0 . . ?
F53X C52X F55X 106.2(4) . . ?
F53X C52X F54X 105.2(4) . . ?
F55X C52X F54X 105.9(4) . . ?
F53X C52X C39X 115.6(4) . . ?
F55X C52X C39X 111.6(4) . . ?
F54X C52X C39X 111.6(4) . . ?
C9X C8X C13X 120.0 . . ?
C9X C8X N7 114.8(6) . . ?
C13X C8X N7 124.9(7) . . ?
C8X C9X C10X 120.0 . . ?
C8X C9X C22X 123.4(7) . . ?
C10X C9X C22X 116.4(7) . . ?
C11X C10X C9X 120.0 . . ?
C10X C11X C12X 120.0 . . ?
C13X C12X C11X 120.0 . . ?
C12X C13X C8X 120.0 . . ?
F23X C22X F25X 107.5(6) . . ?
F23X C22X F24X 106.2(6) . . ?
F25X C22X F24X 105.9(6) . . ?
F23X C22X C9X 116.4(8) . . ?
F25X C22X C9X 106.4(8) . . ?
F24X C22X C9X 113.8(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
Pd1 N7 1.960(2) . ?
Pd1 O31 1.9840(18) . ?
Pd1 N37 1.996(2) . ?
Pd1 O1 2.0010(18) . ?
O1 C1 1.329(3) . ?
C1 C6 1.422(4) . ?
C1 C2 1.426(4) . ?
C2 C3 1.403(4) . ?
C2 C14 1.529(4) . ?
C3 C4 1.401(4) . ?
C4 C5 1.388(4) . ?
C4 C18 1.546(4) . ?
C5 C6 1.406(4) . ?
C6 N7 1.377(3) . ?
N7 C8X 1.414(6) . ?
N7 C8 1.445(2) . ?
C14 C15 1.531(4) . ?
C14 C17 1.545(4) . ?
C14 C16 1.547(4) . ?
C18 C21 1.522(4) . ?
C18 C19 1.532(4) . ?
C18 C20 1.549(4) . ?
O31 C31 1.341(3) . ?
C31 C32 1.405(4) . ?
C31 C36 1.426(4) . ?
C32 C33 1.396(4) . ?
C32 C44 1.537(4) . ?
C33 C34 1.400(4) . ?
C34 C35 1.391(4) . ?
C34 C48 1.532(4) . ?
C35 C36 1.406(3) . ?
C36 N37 1.378(3) . ?
N37 C38 1.402(3) . ?
N37 C38X 1.479(3) . ?
C44 C47 1.531(4) . ?
C44 C46 1.532(4) . ?
C44 C45 1.548(4) . ?
C48 C51 1.536(4) . ?
C48 C50 1.542(4) . ?
C48 C49 1.548(4) . ?
Co1 C68 2.014(3) . ?
Co1 C63 2.015(3) . ?
Co1 C61 2.023(3) . ?
Co1 C67 2.025(3) . ?
Co1 C66 2.026(3) . ?
Co1 C70 2.028(3) . ?
Co1 C65 2.029(3) . ?
Co1 C64 2.040(3) . ?
Co1 C69 2.040(3) . ?
Co1 C62 2.041(3) . ?
C61 C62 1.391(5) . ?
C61 C65 1.434(4) . ?
C62 C63 1.395(5) . ?
C63 C64 1.412(4) . ?
C64 C65 1.414(5) . ?
C66 C70 1.403(5) . ?
C66 C67 1.404(5) . ?
C67 C68 1.475(6) . ?
C68 C69 1.391(6) . ?
C69 C70 1.379(5) . ?
C38 C39 1.3900 . ?
C38 C43 1.3900 . ?
C39 C40 1.3900 . ?
C39 C52 1.486(5) . ?
C40 C41 1.3900 . ?
C41 C42 1.3900 . ?
C42 C43 1.3900 . ?
C52 F54 1.331(5) . ?
C52 F55 1.353(5) . ?
C52 F53 1.358(5) . ?
C8 C9 1.3900 . ?
C8 C13 1.3900 . ?
C9 C10 1.3900 . ?
C9 C22 1.495(3) . ?
C10 C11 1.3900 . ?
C11 C12 1.3900 . ?
C12 C13 1.3900 . ?
C22 F25 1.346(3) . ?
C22 F23 1.346(3) . ?
C22 F24 1.350(3) . ?
C38X C39X 1.3900 . ?
C38X C43X 1.3900 . ?
C39X C40X 1.3900 . ?
C39X C52X 1.479(5) . ?
C40X C41X 1.3900 . ?
C41X C42X 1.3900 . ?
C42X C43X 1.3900 . ?
C52X F53X 1.340(5) . ?
C52X F55X 1.348(5) . ?
C52X F54X 1.351(5) . ?
C8X C9X 1.3900 . ?
C8X C13X 1.3900 . ?
C9X C10X 1.3900 . ?
C9X C22X 1.480(8) . ?
C10X C11X 1.3900 . ?
C11X C12X 1.3900 . ?
C12X C13X 1.3900 . ?
C22X F23X 1.345(7) . ?
C22X F25X 1.348(7) . ?
C22X F24X 1.354(7) . ?
|
1100983.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100983.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_1100983
loop_
_publ_author_name
'Swarnalatha Kokatam'
'Thomas Weyherm\"uller'
'Eberhard Bothe'
'Phalguni Chaudhuri'
'Karl Wieghardt'
_publ_section_title
;
Structural Characterization of Four Members of the Electron-Transfer Series
[PdII(L)2)2]n (L = o-Iminophenolate Derivative; n= 2-, 1-, 0, 1+, 2+).
Ligand Mixed Valency in the Monocation and Monoanion with S=1/2 Ground States
;
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3709
_journal_page_last 3717
_journal_paper_doi 10.1021/ic048292i
_journal_volume 44
_journal_year 2005
_chemical_formula_moiety
'3 [C42 H48 F6 N2 O2 Pd]2+, 6 (B F4)-, 2 HBF4, 4 CH2Cl2'
_chemical_formula_sum 'C43.33 H51.33 B2.67 Cl2.67 F16.67 N2 O2 Pd'
_chemical_formula_weight 1178.62
_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 78.548(5)
_cell_angle_beta 72.946(5)
_cell_angle_gamma 78.209(5)
_cell_formula_units_Z 3
_cell_length_a 13.5833(5)
_cell_length_b 16.8101(7)
_cell_length_c 18.3743(7)
_cell_measurement_temperature 100(2)
_cell_volume 3883.1(3)
_computing_cell_refinement 'Nonius Collect Software'
_computing_data_collection 'Nonius Collect Software'
_computing_data_reduction 'Nonius Collect Software'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type 'Nonius Kappa-CCD'
_diffrn_measurement_method
'851 images at 0.5 deg. in \w and 726 images at 0.5 deg. in phi, 15 sec./frame'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'rotating anode'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0351
_diffrn_reflns_av_sigmaI/netI 0.0335
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_h_min -17
_diffrn_reflns_limit_k_max 21
_diffrn_reflns_limit_k_min -21
_diffrn_reflns_limit_l_max 23
_diffrn_reflns_limit_l_min -23
_diffrn_reflns_number 54535
_diffrn_reflns_theta_full 27.50
_diffrn_reflns_theta_max 27.50
_diffrn_reflns_theta_min 3.02
_exptl_absorpt_coefficient_mu 0.593
_exptl_absorpt_correction_T_max 0.9065
_exptl_absorpt_correction_T_min 0.7185
_exptl_absorpt_correction_type 'Gaussian, face-indexed'
_exptl_crystal_colour 'deep green'
_exptl_crystal_density_diffrn 1.512
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description transparent
_exptl_crystal_F_000 1788
_exptl_crystal_size_max 0.64
_exptl_crystal_size_mid 0.24
_exptl_crystal_size_min 0.18
_refine_diff_density_max 1.178
_refine_diff_density_min -1.283
_refine_diff_density_rms 0.097
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.128
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 1012
_refine_ls_number_reflns 17684
_refine_ls_number_restraints 415
_refine_ls_restrained_S_all 1.156
_refine_ls_R_factor_all 0.0675
_refine_ls_R_factor_gt 0.0568
_refine_ls_shift/su_max 0.004
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0436P)^2^+12.9878P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1331
_refine_ls_wR_factor_ref 0.1401
_reflns_number_gt 15319
_reflns_number_total 17684
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file ic048292isi20041206_054204_4.cif
_cod_data_source_block 5
_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
The following automatic conversions were performed:
'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0436P)^2^+12.9878P] 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^)+(0.0436P)^2^+12.9878P] where P=(Fo^2^+2Fc^2^)/3'.
Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas
;
_cod_database_code 1100983
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
Pd1 Pd 1.06196(2) 1.085760(15) 1.167811(15) 0.01853(7) Uani 1 d . . .
O1 O 0.92583(19) 1.04982(15) 1.17797(15) 0.0229(5) Uani 1 d . . .
C1 C 0.9212(3) 0.9758(2) 1.2069(2) 0.0196(7) Uani 1 d . . .
C2 C 0.8275(3) 0.9400(2) 1.2250(2) 0.0235(7) Uani 1 d . . .
C3 C 0.8386(3) 0.8575(2) 1.2470(2) 0.0237(7) Uani 1 d . . .
H3 H 0.7798 0.8316 1.2543 0.028 Uiso 1 calc R . .
C4 C 0.9343(3) 0.8048(2) 1.2604(2) 0.0241(7) Uani 1 d . . .
C5 C 1.0217(3) 0.8380(2) 1.2483(2) 0.0233(7) Uani 1 d . . .
H5 H 1.0833 0.8047 1.2580 0.028 Uiso 1 calc R . .
C6 C 1.0200(3) 0.9241(2) 1.2206(2) 0.0199(7) Uani 1 d . . .
N7 N 1.0969(2) 0.96555(18) 1.20302(17) 0.0205(6) Uani 1 d . . .
C8 C 1.1977(3) 0.9300(2) 1.2150(2) 0.0247(7) Uani 1 d . . .
C9 C 1.2837(3) 0.9171(2) 1.1523(3) 0.0315(9) Uani 1 d . . .
C10 C 1.3813(3) 0.8883(3) 1.1653(3) 0.0451(12) Uani 1 d . . .
H10 H 1.4405 0.8788 1.1232 0.054 Uiso 1 calc R . .
C11 C 1.3926(4) 0.8736(3) 1.2394(4) 0.0486(14) Uani 1 d . . .
H11 H 1.4596 0.8539 1.2480 0.058 Uiso 1 calc R . .
C12 C 1.3073(4) 0.8874(3) 1.3005(3) 0.0445(12) Uani 1 d . . .
H12 H 1.3160 0.8773 1.3512 0.053 Uiso 1 calc R . .
C13 C 1.2081(3) 0.9160(2) 1.2895(2) 0.0301(8) Uani 1 d . . .
H13 H 1.1493 0.9256 1.3318 0.036 Uiso 1 calc R . .
C14 C 0.7252(3) 0.9943(2) 1.2173(3) 0.0305(8) Uani 1 d . . .
C15 C 0.7333(4) 1.0292(3) 1.1326(3) 0.0396(10) Uani 1 d . . .
H15A H 0.7899 1.0621 1.1130 0.059 Uiso 1 calc R . .
H15B H 0.6674 1.0638 1.1279 0.059 Uiso 1 calc R . .
H15C H 0.7478 0.9839 1.1027 0.059 Uiso 1 calc R . .
C16 C 0.7009(3) 1.0647(3) 1.2661(3) 0.0393(10) Uani 1 d . . .
H16A H 0.7028 1.0415 1.3191 0.059 Uiso 1 calc R . .
H16B H 0.6315 1.0957 1.2660 0.059 Uiso 1 calc R . .
H16C H 0.7531 1.1015 1.2441 0.059 Uiso 1 calc R . .
C17 C 0.6343(3) 0.9449(3) 1.2473(3) 0.0425(11) Uani 1 d . . .
H17A H 0.6296 0.9206 1.3011 0.064 Uiso 1 calc R . .
H17B H 0.6463 0.9011 1.2162 0.064 Uiso 1 calc R . .
H17C H 0.5691 0.9814 1.2439 0.064 Uiso 1 calc R . .
C18 C 0.9261(3) 0.7148(2) 1.2898(2) 0.0285(8) Uani 1 d . . .
C19 C 0.8313(3) 0.7087(3) 1.3614(2) 0.0338(9) Uani 1 d . . .
H19A H 0.8307 0.6510 1.3850 0.051 Uiso 1 calc R . .
H19B H 0.7667 0.7303 1.3458 0.051 Uiso 1 calc R . .
H19C H 0.8367 0.7408 1.3988 0.051 Uiso 1 calc R . .
C20 C 0.9098(4) 0.6755(3) 1.2261(3) 0.0368(10) Uani 1 d . . .
H20A H 0.8951 0.6195 1.2468 0.055 Uiso 1 calc R . .
H20B H 0.9730 0.6737 1.1832 0.055 Uiso 1 calc R . .
H20C H 0.8509 0.7082 1.2077 0.055 Uiso 1 calc R . .
C21 C 1.0240(4) 0.6678(3) 1.3135(3) 0.0437(11) Uani 1 d . . .
H21A H 1.0151 0.6103 1.3331 0.066 Uiso 1 calc R . .
H21B H 1.0347 0.6929 1.3538 0.066 Uiso 1 calc R . .
H21C H 1.0847 0.6700 1.2687 0.066 Uiso 1 calc R . .
C22 C 1.2719(3) 0.9325(3) 1.0716(3) 0.0406(10) Uani 1 d . . .
F23 F 1.2587(3) 1.01234(19) 1.04464(17) 0.0573(8) Uani 1 d . . .
F24 F 1.1904(2) 0.9043(2) 1.06682(17) 0.0554(8) Uani 1 d . . .
F25 F 1.3543(3) 0.8962(3) 1.0238(2) 0.0799(12) Uani 1 d . . .
O31 O 1.19628(18) 1.12013(15) 1.16290(14) 0.0213(5) Uani 1 d . . .
C31 C 1.1965(3) 1.1958(2) 1.1481(2) 0.0204(7) Uani 1 d . . .
C32 C 1.2838(3) 1.2332(2) 1.1476(2) 0.0230(7) Uani 1 d . . .
C33 C 1.2718(3) 1.3159(2) 1.1289(2) 0.0261(8) Uani 1 d . . .
H33 H 1.3270 1.3422 1.1296 0.031 Uiso 1 calc R . .
C34 C 1.1811(3) 1.3688(2) 1.1073(2) 0.0261(8) Uani 1 d . . .
C35 C 1.0972(3) 1.3362(2) 1.1107(2) 0.0260(8) Uani 1 d . . .
H35 H 1.0368 1.3705 1.0998 0.031 Uiso 1 calc R . .
C36 C 1.0997(3) 1.2490(2) 1.1311(2) 0.0206(7) Uani 1 d . . .
N37 N 1.0274(2) 1.20696(18) 1.13513(17) 0.0212(6) Uani 1 d . . .
C38 C 0.9250(3) 1.2456(2) 1.1287(2) 0.0230(7) Uani 1 d . . .
C39 C 0.8915(3) 1.2424(2) 1.0643(2) 0.0262(8) Uani 1 d . . .
C40 C 0.7891(3) 1.2760(3) 1.0632(3) 0.0325(9) Uani 1 d . . .
H40 H 0.7654 1.2744 1.0198 0.039 Uiso 1 calc R . .
C41 C 0.7219(3) 1.3115(3) 1.1247(3) 0.0341(9) Uani 1 d . . .
H41 H 0.6519 1.3332 1.1237 0.041 Uiso 1 calc R . .
C42 C 0.7559(3) 1.3157(2) 1.1878(3) 0.0338(9) Uani 1 d . . .
H42 H 0.7099 1.3417 1.2292 0.041 Uiso 1 calc R . .
C43 C 0.8576(3) 1.2817(2) 1.1904(2) 0.0293(8) Uani 1 d . . .
H43 H 0.8806 1.2832 1.2341 0.035 Uiso 1 calc R . .
C44 C 1.3819(3) 1.1780(2) 1.1646(2) 0.0281(8) Uani 1 d . . .
C45 C 1.3541(3) 1.1248(3) 1.2444(3) 0.0358(9) Uani 1 d . . .
H45A H 1.3052 1.0890 1.2448 0.054 Uiso 1 calc R . .
H45B H 1.3218 1.1605 1.2839 0.054 Uiso 1 calc R . .
H45C H 1.4177 1.0910 1.2551 0.054 Uiso 1 calc R . .
C46 C 1.4615(4) 1.2306(3) 1.1647(3) 0.0440(12) Uani 1 d . . .
H46A H 1.5215 1.1950 1.1795 0.066 Uiso 1 calc R . .
H46B H 1.4291 1.2693 1.2017 0.066 Uiso 1 calc R . .
H46C H 1.4849 1.2613 1.1132 0.066 Uiso 1 calc R . .
C47 C 1.4293(3) 1.1232(3) 1.1020(3) 0.0379(10) Uani 1 d . . .
H47A H 1.3788 1.0891 1.1022 0.057 Uiso 1 calc R . .
H47B H 1.4924 1.0879 1.1118 0.057 Uiso 1 calc R . .
H47C H 1.4472 1.1576 1.0517 0.057 Uiso 1 calc R . .
C48 C 1.1888(4) 1.4602(2) 1.0804(3) 0.0375(10) Uani 1 d . . .
C49 C 1.0930(4) 1.5069(3) 1.0561(4) 0.0569(16) Uani 1 d . . .
H49A H 1.0835 1.4825 1.0150 0.085 Uiso 1 calc R . .
H49B H 1.1019 1.5645 1.0374 0.085 Uiso 1 calc R . .
H49C H 1.0316 1.5041 1.1003 0.085 Uiso 1 calc R . .
C50 C 1.2844(5) 1.4670(3) 1.0096(3) 0.0561(14) Uani 1 d . . .
H50A H 1.2764 1.4402 0.9694 0.084 Uiso 1 calc R . .
H50B H 1.3480 1.4400 1.0249 0.084 Uiso 1 calc R . .
H50C H 1.2893 1.5250 0.9899 0.084 Uiso 1 calc R . .
C51 C 1.2018(5) 1.4983(3) 1.1457(3) 0.0505(13) Uani 1 d . . .
H51A H 1.2030 1.5573 1.1293 0.076 Uiso 1 calc R . .
H51B H 1.2673 1.4720 1.1583 0.076 Uiso 1 calc R . .
H51C H 1.1433 1.4899 1.1913 0.076 Uiso 1 calc R . .
C52 C 0.9659(3) 1.2084(3) 0.9961(2) 0.0360(10) Uani 1 d . . .
F53 F 0.9239(2) 1.21614(19) 0.93729(15) 0.0451(7) Uani 1 d . . .
F54 F 1.0492(2) 1.2467(2) 0.96900(16) 0.0573(9) Uani 1 d . . .
F55 F 1.0015(3) 1.1278(2) 1.01189(17) 0.0598(9) Uani 1 d . . .
Pd2 Pd 0.5000 1.5000 1.5000 0.01793(9) Uani 1 d S . .
O61 O 0.48923(18) 1.61540(14) 1.51979(15) 0.0208(5) Uani 1 d . . .
C61 C 0.5692(3) 1.6301(2) 1.5317(2) 0.0191(7) Uani 1 d . . .
C62 C 0.5794(3) 1.7093(2) 1.5466(2) 0.0204(7) Uani 1 d . . .
C63 C 0.6683(3) 1.7112(2) 1.5647(2) 0.0219(7) Uani 1 d . . .
H63 H 0.6763 1.7620 1.5758 0.026 Uiso 1 calc R . .
C64 C 0.7540(3) 1.6422(2) 1.5689(2) 0.0199(7) Uani 1 d . . .
C65 C 0.7488(3) 1.5692(2) 1.5514(2) 0.0209(7) Uani 1 d . . .
H65 H 0.8046 1.5248 1.5520 0.025 Uiso 1 calc R . .
C66 C 0.6584(3) 1.5600(2) 1.5318(2) 0.0196(7) Uani 1 d . . .
N67 N 0.6406(2) 1.49318(17) 1.51538(17) 0.0191(6) Uani 1 d . . .
C68 C 0.7091(3) 1.4167(2) 1.5223(2) 0.0196(7) Uani 1 d . . .
C69 C 0.7704(3) 1.3819(2) 1.4570(2) 0.0211(7) Uani 1 d . . .
C70 C 0.8272(3) 1.3037(2) 1.4670(2) 0.0249(7) Uani 1 d . . .
H70 H 0.8681 1.2789 1.4233 0.030 Uiso 1 calc R . .
C71 C 0.8242(3) 1.2617(2) 1.5404(3) 0.0294(8) Uani 1 d . . .
H71 H 0.8632 1.2082 1.5468 0.035 Uiso 1 calc R . .
C72 C 0.7648(3) 1.2971(2) 1.6044(2) 0.0288(8) Uani 1 d . . .
H72 H 0.7636 1.2681 1.6546 0.035 Uiso 1 calc R . .
C73 C 0.7069(3) 1.3753(2) 1.5955(2) 0.0237(7) Uani 1 d . . .
H73 H 0.6663 1.3999 1.6393 0.028 Uiso 1 calc R . .
C74 C 0.4920(3) 1.7822(2) 1.5424(2) 0.0275(8) Uani 1 d . . .
C75 C 0.4683(4) 1.7974(3) 1.4635(3) 0.0398(10) Uani 1 d . . .
H75A H 0.4168 1.8472 1.4599 0.060 Uiso 1 calc R . .
H75B H 0.4403 1.7503 1.4577 0.060 Uiso 1 calc R . .
H75C H 0.5325 1.8042 1.4227 0.060 Uiso 1 calc R . .
C76 C 0.3940(3) 1.7647(3) 1.6070(3) 0.0349(9) Uani 1 d . . .
H76A H 0.3371 1.8104 1.6033 0.052 Uiso 1 calc R . .
H76B H 0.4089 1.7586 1.6570 0.052 Uiso 1 calc R . .
H76C H 0.3736 1.7139 1.6018 0.052 Uiso 1 calc R . .
C77 C 0.5241(3) 1.8607(2) 1.5528(3) 0.0388(10) Uani 1 d . . .
H77A H 0.4681 1.9070 1.5487 0.058 Uiso 1 calc R . .
H77B H 0.5878 1.8718 1.5129 0.058 Uiso 1 calc R . .
H77C H 0.5371 1.8534 1.6037 0.058 Uiso 1 calc R . .
C78 C 0.8430(3) 1.6559(2) 1.5969(2) 0.0241(7) Uani 1 d . . .
C79 C 0.7977(4) 1.6673(4) 1.6819(3) 0.0485(13) Uani 1 d . . .
H79A H 0.8534 1.6739 1.7030 0.073 Uiso 1 calc R . .
H79B H 0.7665 1.6189 1.7109 0.073 Uiso 1 calc R . .
H79C H 0.7441 1.7163 1.6860 0.073 Uiso 1 calc R . .
C80 C 0.8888(3) 1.7325(3) 1.5510(3) 0.0369(10) Uani 1 d . . .
H80A H 0.9222 1.7236 1.4976 0.055 Uiso 1 calc R . .
H80B H 0.9407 1.7431 1.5739 0.055 Uiso 1 calc R . .
H80C H 0.8330 1.7799 1.5520 0.055 Uiso 1 calc R . .
C81 C 0.9298(4) 1.5825(3) 1.5915(4) 0.0492(14) Uani 1 d . . .
H81A H 0.9847 1.5928 1.6115 0.074 Uiso 1 calc R . .
H81B H 0.9588 1.5741 1.5376 0.074 Uiso 1 calc R . .
H81C H 0.9017 1.5334 1.6219 0.074 Uiso 1 calc R . .
C82 C 0.7774(3) 1.4294(2) 1.3777(2) 0.0262(8) Uani 1 d . . .
F83 F 0.68712(18) 1.44366(15) 1.35835(14) 0.0343(5) Uani 1 d . . .
F84 F 0.8053(2) 1.50333(14) 1.37132(14) 0.0350(5) Uani 1 d . . .
F85 F 0.8487(2) 1.39101(16) 1.32352(14) 0.0376(6) Uani 1 d . . .
B100 B 0.5241(7) 0.5395(4) 0.7456(4) 0.0396(13) Uani 0.679(9) d PD A 1
F101 F 0.5101(9) 0.6181(5) 0.7622(6) 0.145(6) Uani 0.679(9) d PD A 1
F102 F 0.6223(8) 0.4976(6) 0.7487(7) 0.072(2) Uani 0.679(9) d PD A 1
F103 F 0.5172(4) 0.5426(5) 0.6714(3) 0.0580(16) Uani 0.679(9) d PD A 1
F104 F 0.4456(11) 0.4986(8) 0.7962(5) 0.0554(14) Uani 0.679(9) d PD A 1
B105 B 0.5184(15) 0.5395(8) 0.7565(7) 0.0396(13) Uani 0.321(9) d PD A 2
F106 F 0.528(2) 0.5898(12) 0.8042(9) 0.145(6) Uani 0.321(9) d PD A 2
F107 F 0.609(2) 0.4830(12) 0.7397(17) 0.072(2) Uani 0.321(9) d PD A 2
F108 F 0.5035(10) 0.5859(10) 0.6884(7) 0.0580(16) Uani 0.321(9) d PD A 2
F109 F 0.433(2) 0.4992(16) 0.7929(11) 0.0554(14) Uani 0.321(9) d PD A 2
B200 B 1.5838(4) 0.6663(3) 1.2948(3) 0.0438(13) Uani 1 d . . .
F201 F 1.6502(3) 0.6124(2) 1.23237(19) 0.0606(8) Uani 1 d D . .
H201 H 1.684(5) 0.634(4) 1.1789(16) 0.091 Uiso 1 d D . .
F202 F 1.5892(4) 0.6210(2) 1.36330(19) 0.0973(17) Uani 1 d . . .
F203 F 1.4853(2) 0.6819(2) 1.2844(3) 0.0780(12) Uani 1 d . . .
F204 F 1.6249(2) 0.73656(18) 1.28043(17) 0.0483(7) Uani 1 d . . .
F304 F 0.74769(19) 0.79383(16) 1.00083(12) 0.0381(6) Uani 1 d D . .
B300 B 0.7041(3) 0.7708(2) 1.07838(19) 0.0352(13) Uani 0.826(4) d PD B 1
F301 F 0.7369(3) 0.8169(2) 1.11902(19) 0.0573(10) Uani 0.826(4) d PD B 1
F302 F 0.5966(2) 0.7842(3) 1.0944(2) 0.0640(12) Uani 0.826(4) d PD B 1
F303 F 0.7383(4) 0.6881(2) 1.1004(2) 0.0504(10) Uani 0.826(4) d PD B 1
B305 B 0.6802(7) 0.7648(6) 1.0691(4) 0.0352(13) Uani 0.174(4) d PD B 2
F306 F 0.6002(9) 0.7382(10) 1.0526(8) 0.0573(10) Uani 0.174(4) d PD B 2
F307 F 0.6389(10) 0.8267(10) 1.1142(6) 0.0640(12) Uani 0.174(4) d PD B 2
F308 F 0.7336(14) 0.6995(10) 1.1085(8) 0.0504(10) Uani 0.174(4) d PD B 2
B400 B 0.9958(4) 1.1357(3) 1.3475(3) 0.0336(10) Uani 1 d . . .
F401 F 1.0861(3) 1.0803(2) 1.33052(18) 0.0650(9) Uani 1 d . . .
F402 F 0.9190(3) 1.1160(2) 1.32219(19) 0.0655(9) Uani 1 d . . .
F403 F 1.0167(2) 1.21288(18) 1.30838(16) 0.0485(7) Uani 1 d . . .
F404 F 0.9635(2) 1.13626(16) 1.42658(15) 0.0398(6) Uani 1 d . . .
C500 C 1.5921(3) 1.3320(3) 0.8725(2) 0.0552(14) Uani 1 d D . .
H50D H 1.5729 1.3795 0.8352 0.066 Uiso 1 calc R . .
H50E H 1.5488 1.2896 0.8770 0.066 Uiso 1 calc R . .
Cl51 Cl 1.72595(11) 1.29155(10) 0.83999(13) 0.0762(5) Uani 1 d D . .
Cl52 Cl 1.56943(14) 1.36313(17) 0.96307(11) 0.0962(7) Uani 1 d D . .
C600 C 0.8649(3) 0.9732(5) 1.4883(3) 0.0389(13) Uani 0.800(4) d PD C 1
H60A H 0.9026 0.9482 1.5279 0.047 Uiso 0.800(4) calc PR C 1
H60B H 0.8817 1.0294 1.4685 0.047 Uiso 0.800(4) calc PR C 1
Cl61 Cl 0.9063(2) 0.91403(10) 1.41212(10) 0.0626(6) Uani 0.800(4) d PD C 1
Cl62 Cl 0.7293(2) 0.9784(2) 1.5301(2) 0.0813(8) Uani 0.800(4) d PD C 1
C605 C 0.8310(13) 0.975(2) 1.4900(14) 0.0389(13) Uani 0.200(4) d PD C 2
H60C H 0.8851 0.9452 1.5159 0.047 Uiso 0.200(4) calc PR C 2
H60D H 0.8491 1.0305 1.4665 0.047 Uiso 0.200(4) calc PR C 2
Cl66 Cl 0.8259(9) 0.9215(4) 1.4180(4) 0.0626(6) Uani 0.200(4) d PD C 2
Cl67 Cl 0.7078(11) 0.9846(11) 1.5577(8) 0.0813(8) Uani 0.200(4) 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
Pd1 0.01603(13) 0.01483(12) 0.02404(14) 0.00104(9) -0.00746(10) -0.00148(9)
O1 0.0181(12) 0.0191(12) 0.0326(14) -0.0007(10) -0.0114(10) -0.0012(9)
C1 0.0225(17) 0.0177(16) 0.0200(16) -0.0027(13) -0.0087(13) -0.0015(13)
C2 0.0216(17) 0.0245(18) 0.0264(18) -0.0052(14) -0.0081(14) -0.0038(14)
C3 0.0238(17) 0.0245(18) 0.0235(17) -0.0024(14) -0.0051(14) -0.0083(14)
C4 0.0302(19) 0.0213(17) 0.0207(17) -0.0014(13) -0.0065(14) -0.0060(14)
C5 0.0264(18) 0.0180(16) 0.0258(18) -0.0012(13) -0.0102(14) -0.0007(14)
C6 0.0195(16) 0.0192(16) 0.0202(16) -0.0032(13) -0.0055(13) -0.0006(13)
N7 0.0194(14) 0.0183(14) 0.0229(14) -0.0016(11) -0.0070(11) -0.0001(11)
C8 0.0197(17) 0.0149(16) 0.040(2) -0.0005(14) -0.0122(15) 0.0002(13)
C9 0.0212(18) 0.0245(19) 0.046(2) -0.0072(17) -0.0065(17) 0.0001(15)
C10 0.021(2) 0.028(2) 0.082(4) -0.007(2) -0.009(2) 0.0002(16)
C11 0.029(2) 0.023(2) 0.098(4) 0.008(2) -0.036(3) -0.0032(17)
C12 0.049(3) 0.026(2) 0.069(3) 0.012(2) -0.042(3) -0.0091(19)
C13 0.031(2) 0.0223(18) 0.038(2) 0.0055(16) -0.0173(17) -0.0048(15)
C14 0.0194(18) 0.0253(19) 0.048(2) -0.0068(17) -0.0110(17) -0.0024(15)
C15 0.033(2) 0.037(2) 0.054(3) 0.002(2) -0.028(2) -0.0034(18)
C16 0.023(2) 0.033(2) 0.062(3) -0.016(2) -0.0100(19) 0.0015(17)
C17 0.023(2) 0.033(2) 0.072(3) -0.009(2) -0.016(2) -0.0025(17)
C18 0.036(2) 0.0194(17) 0.033(2) 0.0015(15) -0.0141(17) -0.0066(15)
C19 0.040(2) 0.031(2) 0.031(2) 0.0026(16) -0.0109(18) -0.0137(18)
C20 0.056(3) 0.0239(19) 0.034(2) -0.0030(16) -0.012(2) -0.0129(19)
C21 0.044(3) 0.024(2) 0.063(3) 0.011(2) -0.024(2) -0.0046(18)
C22 0.029(2) 0.040(2) 0.045(3) -0.016(2) 0.0037(19) -0.0004(18)
F23 0.088(2) 0.0439(17) 0.0409(16) -0.0013(13) -0.0181(16) -0.0154(16)
F24 0.0556(18) 0.077(2) 0.0413(16) -0.0204(15) -0.0076(14) -0.0237(16)
F25 0.055(2) 0.102(3) 0.057(2) -0.030(2) 0.0141(16) 0.021(2)
O31 0.0168(11) 0.0200(12) 0.0260(13) 0.0014(10) -0.0078(10) -0.0022(9)
C31 0.0197(16) 0.0215(17) 0.0186(16) -0.0002(13) -0.0061(13) -0.0010(13)
C32 0.0192(16) 0.0244(18) 0.0255(18) -0.0007(14) -0.0079(14) -0.0033(14)
C33 0.0256(18) 0.0244(18) 0.0300(19) 0.0025(15) -0.0106(15) -0.0093(15)
C34 0.031(2) 0.0175(17) 0.0312(19) 0.0011(14) -0.0144(16) -0.0034(14)
C35 0.0281(19) 0.0185(17) 0.032(2) 0.0012(14) -0.0146(16) -0.0004(14)
C36 0.0216(17) 0.0196(16) 0.0208(16) -0.0012(13) -0.0082(13) -0.0012(13)
N37 0.0208(14) 0.0179(14) 0.0242(15) 0.0014(11) -0.0092(12) -0.0009(11)
C38 0.0187(16) 0.0158(16) 0.035(2) 0.0027(14) -0.0115(14) -0.0029(13)
C39 0.0252(18) 0.0225(17) 0.0313(19) 0.0052(15) -0.0115(15) -0.0076(14)
C40 0.030(2) 0.030(2) 0.039(2) 0.0102(17) -0.0180(18) -0.0102(16)
C41 0.0212(18) 0.029(2) 0.050(3) 0.0069(18) -0.0146(18) -0.0040(15)
C42 0.026(2) 0.0242(19) 0.047(2) -0.0021(17) -0.0091(18) 0.0018(15)
C43 0.0277(19) 0.0242(18) 0.037(2) -0.0045(16) -0.0139(17) 0.0018(15)
C44 0.0197(17) 0.0288(19) 0.037(2) 0.0008(16) -0.0128(16) -0.0044(15)
C45 0.035(2) 0.033(2) 0.042(2) 0.0043(18) -0.0228(19) -0.0012(17)
C46 0.029(2) 0.043(3) 0.066(3) 0.007(2) -0.028(2) -0.0115(19)
C47 0.0208(19) 0.041(2) 0.048(3) -0.008(2) -0.0074(18) 0.0028(17)
C48 0.045(2) 0.0182(18) 0.058(3) 0.0038(18) -0.029(2) -0.0097(17)
C49 0.059(3) 0.020(2) 0.103(5) 0.012(2) -0.051(3) -0.009(2)
C50 0.066(4) 0.036(3) 0.062(3) 0.015(2) -0.015(3) -0.022(2)
C51 0.065(3) 0.027(2) 0.072(4) -0.006(2) -0.035(3) -0.012(2)
C52 0.030(2) 0.050(3) 0.029(2) 0.0013(18) -0.0150(17) -0.0054(19)
F53 0.0425(15) 0.0694(19) 0.0314(13) -0.0043(13) -0.0207(12) -0.0134(13)
F54 0.0334(14) 0.109(3) 0.0340(14) -0.0055(16) -0.0071(12) -0.0281(16)
F55 0.077(2) 0.0562(19) 0.0358(15) -0.0124(13) -0.0167(15) 0.0220(16)
Pd2 0.01308(17) 0.01388(17) 0.0284(2) -0.00372(14) -0.00875(14) -0.00014(12)
O61 0.0168(11) 0.0159(11) 0.0311(13) -0.0036(10) -0.0095(10) -0.0008(9)
C61 0.0159(15) 0.0165(15) 0.0232(16) -0.0005(13) -0.0059(13) -0.0004(12)
C62 0.0176(16) 0.0162(15) 0.0262(17) -0.0041(13) -0.0051(13) -0.0002(12)
C63 0.0206(17) 0.0182(16) 0.0275(18) -0.0033(13) -0.0064(14) -0.0045(13)
C64 0.0172(16) 0.0222(17) 0.0204(16) -0.0019(13) -0.0047(13) -0.0051(13)
C65 0.0139(15) 0.0191(16) 0.0291(18) -0.0022(14) -0.0064(13) -0.0015(12)
C66 0.0163(15) 0.0165(15) 0.0244(17) -0.0003(13) -0.0060(13) -0.0006(12)
N67 0.0142(13) 0.0158(13) 0.0275(15) -0.0032(11) -0.0071(11) -0.0002(10)
C68 0.0144(15) 0.0132(15) 0.0326(19) -0.0028(13) -0.0100(13) -0.0003(12)
C69 0.0141(15) 0.0175(16) 0.0321(19) -0.0043(14) -0.0066(13) -0.0022(12)
C70 0.0164(16) 0.0198(17) 0.037(2) -0.0072(15) -0.0066(15) 0.0014(13)
C71 0.0234(18) 0.0178(17) 0.046(2) 0.0000(16) -0.0135(17) 0.0011(14)
C72 0.0282(19) 0.0228(18) 0.035(2) 0.0019(15) -0.0139(16) -0.0019(15)
C73 0.0184(16) 0.0226(17) 0.0305(19) -0.0030(14) -0.0087(14) -0.0017(13)
C74 0.0244(18) 0.0165(16) 0.044(2) -0.0073(15) -0.0148(17) 0.0018(14)
C75 0.048(3) 0.0210(19) 0.054(3) -0.0007(18) -0.029(2) 0.0038(18)
C76 0.0207(18) 0.031(2) 0.054(3) -0.0174(19) -0.0064(18) 0.0015(16)
C77 0.032(2) 0.0191(18) 0.071(3) -0.0143(19) -0.021(2) 0.0019(16)
C78 0.0226(17) 0.0229(17) 0.0315(19) -0.0034(14) -0.0134(15) -0.0051(14)
C79 0.044(3) 0.079(4) 0.032(2) -0.010(2) -0.015(2) -0.022(3)
C80 0.034(2) 0.036(2) 0.050(3) 0.0040(19) -0.022(2) -0.0195(18)
C81 0.031(2) 0.033(2) 0.100(4) -0.022(3) -0.042(3) 0.0055(18)
C82 0.0224(18) 0.0222(17) 0.034(2) -0.0065(15) -0.0074(15) -0.0015(14)
F83 0.0283(12) 0.0397(13) 0.0366(13) 0.0031(10) -0.0167(10) -0.0057(10)
F84 0.0418(14) 0.0265(12) 0.0363(13) 0.0004(10) -0.0075(11) -0.0136(10)
F85 0.0355(13) 0.0388(14) 0.0312(12) -0.0082(10) -0.0021(10) 0.0037(11)
B100 0.037(3) 0.040(3) 0.038(3) -0.004(2) -0.009(3) -0.002(2)
F101 0.136(7) 0.078(7) 0.191(11) -0.084(7) 0.078(9) -0.066(6)
F102 0.049(4) 0.079(4) 0.093(4) 0.006(3) -0.039(2) -0.009(3)
F103 0.056(3) 0.086(5) 0.036(2) 0.007(3) -0.014(2) -0.033(3)
F104 0.056(4) 0.063(2) 0.0433(18) -0.0045(15) 0.0004(18) -0.025(2)
B105 0.037(3) 0.040(3) 0.038(3) -0.004(2) -0.009(3) -0.002(2)
F106 0.136(7) 0.078(7) 0.191(11) -0.084(7) 0.078(9) -0.066(6)
F107 0.049(4) 0.079(4) 0.093(4) 0.006(3) -0.039(2) -0.009(3)
F108 0.056(3) 0.086(5) 0.036(2) 0.007(3) -0.014(2) -0.033(3)
F109 0.056(4) 0.063(2) 0.0433(18) -0.0045(15) 0.0004(18) -0.025(2)
B200 0.040(3) 0.032(3) 0.043(3) 0.001(2) 0.007(2) -0.002(2)
F201 0.0545(19) 0.060(2) 0.0535(19) -0.0021(15) -0.0039(15) -0.0004(15)
F202 0.159(4) 0.0431(19) 0.0380(18) 0.0105(14) 0.017(2) 0.022(2)
F203 0.0333(16) 0.057(2) 0.135(4) -0.033(2) 0.0049(19) -0.0112(15)
F204 0.0491(16) 0.0470(16) 0.0500(16) 0.0002(13) -0.0140(13) -0.0161(13)
F304 0.0341(13) 0.0514(16) 0.0250(12) -0.0008(11) -0.0067(10) -0.0049(11)
B300 0.028(3) 0.045(3) 0.028(3) -0.002(2) -0.003(2) -0.007(2)
F301 0.075(3) 0.063(2) 0.0390(19) -0.0162(17) -0.0138(18) -0.015(2)
F302 0.0239(17) 0.085(3) 0.066(3) 0.002(2) -0.0011(16) 0.0026(17)
F303 0.0448(17) 0.047(2) 0.0480(18) 0.0050(15) -0.0009(14) -0.0091(15)
B305 0.028(3) 0.045(3) 0.028(3) -0.002(2) -0.003(2) -0.007(2)
F306 0.075(3) 0.063(2) 0.0390(19) -0.0162(17) -0.0138(18) -0.015(2)
F307 0.0239(17) 0.085(3) 0.066(3) 0.002(2) -0.0011(16) 0.0026(17)
F308 0.0448(17) 0.047(2) 0.0480(18) 0.0050(15) -0.0009(14) -0.0091(15)
B400 0.036(3) 0.034(2) 0.035(2) -0.0128(19) -0.011(2) -0.004(2)
F401 0.063(2) 0.060(2) 0.0496(18) -0.0084(15) -0.0028(15) 0.0233(16)
F402 0.070(2) 0.086(3) 0.0567(19) -0.0028(17) -0.0249(17) -0.042(2)
F403 0.0655(19) 0.0443(16) 0.0419(15) 0.0027(12) -0.0245(14) -0.0162(14)
F404 0.0474(15) 0.0375(14) 0.0344(13) -0.0126(11) -0.0065(11) -0.0057(12)
C500 0.041(3) 0.056(3) 0.059(3) 0.000(3) -0.007(2) -0.005(2)
Cl51 0.0437(8) 0.0540(8) 0.1278(15) -0.0354(9) -0.0024(8) -0.0088(6)
Cl52 0.0582(10) 0.164(2) 0.0588(10) -0.0190(12) -0.0075(8) -0.0104(12)
C600 0.028(3) 0.040(3) 0.046(3) -0.005(2) -0.006(3) -0.007(3)
Cl61 0.1043(18) 0.0390(8) 0.0384(8) -0.0043(6) -0.0076(10) -0.0150(10)
Cl62 0.0368(14) 0.0698(13) 0.128(3) -0.0198(18) -0.0034(13) -0.0085(12)
C605 0.028(3) 0.040(3) 0.046(3) -0.005(2) -0.006(3) -0.007(3)
Cl66 0.1043(18) 0.0390(8) 0.0384(8) -0.0043(6) -0.0076(10) -0.0150(10)
Cl67 0.0368(14) 0.0698(13) 0.128(3) -0.0198(18) -0.0034(13) -0.0085(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'
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'
Pd Pd -0.9988 1.0072 '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
O31 Pd1 N7 98.86(11) . . ?
O31 Pd1 N37 80.43(11) . . ?
N7 Pd1 N37 178.46(12) . . ?
O31 Pd1 O1 177.38(10) . . ?
N7 Pd1 O1 80.06(11) . . ?
N37 Pd1 O1 100.60(11) . . ?
C1 O1 Pd1 114.4(2) . . ?
O1 C1 C2 122.9(3) . . ?
O1 C1 C6 116.8(3) . . ?
C2 C1 C6 120.3(3) . . ?
C3 C2 C1 115.6(3) . . ?
C3 C2 C14 124.4(3) . . ?
C1 C2 C14 120.0(3) . . ?
C2 C3 C4 125.4(3) . . ?
C5 C4 C3 119.9(3) . . ?
C5 C4 C18 124.1(3) . . ?
C3 C4 C18 115.9(3) . . ?
C4 C5 C6 119.1(3) . . ?
N7 C6 C5 127.6(3) . . ?
N7 C6 C1 112.9(3) . . ?
C5 C6 C1 119.4(3) . . ?
C6 N7 C8 122.9(3) . . ?
C6 N7 Pd1 115.4(2) . . ?
C8 N7 Pd1 121.4(2) . . ?
C13 C8 C9 121.3(4) . . ?
C13 C8 N7 118.1(3) . . ?
C9 C8 N7 120.3(3) . . ?
C10 C9 C8 119.1(4) . . ?
C10 C9 C22 119.8(4) . . ?
C8 C9 C22 121.1(4) . . ?
C11 C10 C9 120.1(5) . . ?
C12 C11 C10 120.2(4) . . ?
C11 C12 C13 121.1(5) . . ?
C8 C13 C12 118.2(4) . . ?
C2 C14 C15 109.7(3) . . ?
C2 C14 C17 110.8(3) . . ?
C15 C14 C17 108.5(4) . . ?
C2 C14 C16 109.6(3) . . ?
C15 C14 C16 110.6(4) . . ?
C17 C14 C16 107.7(4) . . ?
C4 C18 C21 112.0(3) . . ?
C4 C18 C20 109.0(3) . . ?
C21 C18 C20 109.3(4) . . ?
C4 C18 C19 108.8(3) . . ?
C21 C18 C19 108.1(3) . . ?
C20 C18 C19 109.6(3) . . ?
F24 C22 F25 106.5(4) . . ?
F24 C22 F23 106.2(4) . . ?
F25 C22 F23 108.1(4) . . ?
F24 C22 C9 112.5(4) . . ?
F25 C22 C9 111.6(4) . . ?
F23 C22 C9 111.6(4) . . ?
C31 O31 Pd1 114.7(2) . . ?
O31 C31 C32 122.9(3) . . ?
O31 C31 C36 117.1(3) . . ?
C32 C31 C36 120.0(3) . . ?
C33 C32 C31 115.2(3) . . ?
C33 C32 C44 125.5(3) . . ?
C31 C32 C44 119.3(3) . . ?
C32 C33 C34 125.9(3) . . ?
C35 C34 C33 120.0(3) . . ?
C35 C34 C48 123.0(3) . . ?
C33 C34 C48 117.0(3) . . ?
C34 C35 C36 119.3(3) . . ?
N37 C36 C35 127.6(3) . . ?
N37 C36 C31 113.0(3) . . ?
C35 C36 C31 119.4(3) . . ?
C36 N37 C38 122.3(3) . . ?
C36 N37 Pd1 114.7(2) . . ?
C38 N37 Pd1 122.3(2) . . ?
C43 C38 C39 120.6(3) . . ?
C43 C38 N37 118.1(3) . . ?
C39 C38 N37 121.1(3) . . ?
C40 C39 C38 118.9(4) . . ?
C40 C39 C52 120.5(4) . . ?
C38 C39 C52 120.5(3) . . ?
C41 C40 C39 120.6(4) . . ?
C40 C41 C42 120.4(4) . . ?
C41 C42 C43 120.0(4) . . ?
C38 C43 C42 119.6(4) . . ?
C47 C44 C46 109.4(4) . . ?
C47 C44 C32 108.5(3) . . ?
C46 C44 C32 110.2(3) . . ?
C47 C44 C45 110.2(4) . . ?
C46 C44 C45 108.2(3) . . ?
C32 C44 C45 110.4(3) . . ?
C49 C48 C34 111.8(3) . . ?
C49 C48 C51 108.9(4) . . ?
C34 C48 C51 109.6(4) . . ?
C49 C48 C50 108.1(4) . . ?
C34 C48 C50 107.8(4) . . ?
C51 C48 C50 110.5(4) . . ?
F54 C52 F53 106.1(3) . . ?
F54 C52 F55 107.0(4) . . ?
F53 C52 F55 106.1(4) . . ?
F54 C52 C39 111.6(4) . . ?
F53 C52 C39 112.9(3) . . ?
F55 C52 C39 112.7(3) . . ?
N67 Pd2 N67 179.999(2) . 2_688 ?
N67 Pd2 O61 80.60(11) . . ?
N67 Pd2 O61 99.40(11) 2_688 . ?
N67 Pd2 O61 99.40(11) . 2_688 ?
N67 Pd2 O61 80.60(11) 2_688 2_688 ?
O61 Pd2 O61 180.000(3) . 2_688 ?
C61 O61 Pd2 114.2(2) . . ?
O61 C61 C62 123.8(3) . . ?
O61 C61 C66 116.9(3) . . ?
C62 C61 C66 119.3(3) . . ?
C63 C62 C61 115.1(3) . . ?
C63 C62 C74 125.0(3) . . ?
C61 C62 C74 119.9(3) . . ?
C62 C63 C64 126.3(3) . . ?
C65 C64 C63 119.7(3) . . ?
C65 C64 C78 122.7(3) . . ?
C63 C64 C78 117.5(3) . . ?
C64 C65 C66 118.8(3) . . ?
N67 C66 C65 126.1(3) . . ?
N67 C66 C61 113.2(3) . . ?
C65 C66 C61 120.6(3) . . ?
C66 N67 C68 122.0(3) . . ?
C66 N67 Pd2 115.0(2) . . ?
C68 N67 Pd2 122.0(2) . . ?
C73 C68 C69 121.0(3) . . ?
C73 C68 N67 117.7(3) . . ?
C69 C68 N67 121.2(3) . . ?
C70 C69 C68 118.9(3) . . ?
C70 C69 C82 120.5(3) . . ?
C68 C69 C82 120.6(3) . . ?
C71 C70 C69 120.2(4) . . ?
C72 C71 C70 120.5(3) . . ?
C71 C72 C73 120.1(4) . . ?
C68 C73 C72 119.4(4) . . ?
C62 C74 C77 110.5(3) . . ?
C62 C74 C76 109.3(3) . . ?
C77 C74 C76 108.6(3) . . ?
C62 C74 C75 110.3(3) . . ?
C77 C74 C75 107.8(3) . . ?
C76 C74 C75 110.3(4) . . ?
C81 C78 C64 111.7(3) . . ?
C81 C78 C80 108.7(4) . . ?
C64 C78 C80 111.4(3) . . ?
C81 C78 C79 108.6(4) . . ?
C64 C78 C79 106.7(3) . . ?
C80 C78 C79 109.6(4) . . ?
F85 C82 F83 107.0(3) . . ?
F85 C82 F84 106.0(3) . . ?
F83 C82 F84 106.4(3) . . ?
F85 C82 C69 112.3(3) . . ?
F83 C82 C69 113.0(3) . . ?
F84 C82 C69 111.6(3) . . ?
F101 B100 F103 109.7(5) . . ?
F101 B100 F102 111.2(4) . . ?
F103 B100 F102 106.8(4) . . ?
F101 B100 F104 109.1(4) . . ?
F103 B100 F104 108.3(4) . . ?
F102 B100 F104 111.6(4) . . ?
F106 B105 F108 110.0(5) . . ?
F106 B105 F107 109.4(5) . . ?
F108 B105 F107 108.7(5) . . ?
F106 B105 F109 109.3(5) . . ?
F108 B105 F109 109.2(5) . . ?
F107 B105 F109 110.2(5) . . ?
F202 B200 F204 113.4(5) . . ?
F202 B200 F203 113.2(5) . . ?
F204 B200 F203 111.0(4) . . ?
F202 B200 F201 106.2(4) . . ?
F204 B200 F201 107.3(4) . . ?
F203 B200 F201 105.1(5) . . ?
B300 F304 B305 18.5(5) . . ?
F304 B300 F302 110.4(3) . . ?
F304 B300 F301 108.0(3) . . ?
F302 B300 F301 110.5(3) . . ?
F304 B300 F303 110.4(3) . . ?
F302 B300 F303 109.1(3) . . ?
F301 B300 F303 108.5(3) . . ?
F304 B305 F307 110.0(5) . . ?
F304 B305 F306 109.1(5) . . ?
F307 B305 F306 109.4(5) . . ?
F304 B305 F308 109.5(5) . . ?
F307 B305 F308 109.6(5) . . ?
F306 B305 F308 109.3(5) . . ?
F401 B400 F402 110.9(4) . . ?
F401 B400 F404 109.0(4) . . ?
F402 B400 F404 110.6(4) . . ?
F401 B400 F403 108.1(4) . . ?
F402 B400 F403 107.5(4) . . ?
F404 B400 F403 110.8(4) . . ?
Cl52 C500 Cl51 109.0(3) . . ?
Cl62 C600 Cl61 110.8(3) . . ?
Cl67 C605 Cl66 108.7(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
Pd1 O31 1.996(2) . ?
Pd1 N7 1.999(3) . ?
Pd1 N37 2.005(3) . ?
Pd1 O1 2.007(2) . ?
O1 C1 1.259(4) . ?
C1 C2 1.441(5) . ?
C1 C6 1.502(5) . ?
C2 C3 1.355(5) . ?
C2 C14 1.526(5) . ?
C3 C4 1.471(5) . ?
C4 C5 1.356(5) . ?
C4 C18 1.517(5) . ?
C5 C6 1.432(5) . ?
C6 N7 1.300(5) . ?
N7 C8 1.439(4) . ?
C8 C13 1.386(6) . ?
C8 C9 1.394(6) . ?
C9 C10 1.389(6) . ?
C9 C22 1.505(7) . ?
C10 C11 1.382(8) . ?
C11 C12 1.375(8) . ?
C12 C13 1.394(6) . ?
C14 C15 1.531(6) . ?
C14 C17 1.534(6) . ?
C14 C16 1.550(6) . ?
C18 C21 1.536(6) . ?
C18 C20 1.541(6) . ?
C18 C19 1.551(6) . ?
C22 F24 1.321(6) . ?
C22 F25 1.323(5) . ?
C22 F23 1.330(6) . ?
O31 C31 1.248(4) . ?
C31 C32 1.448(5) . ?
C31 C36 1.508(5) . ?
C32 C33 1.352(5) . ?
C32 C44 1.536(5) . ?
C33 C34 1.471(5) . ?
C34 C35 1.344(5) . ?
C34 C48 1.533(5) . ?
C35 C36 1.435(5) . ?
C36 N37 1.299(5) . ?
N37 C38 1.438(4) . ?
C38 C43 1.389(6) . ?
C38 C39 1.400(5) . ?
C39 C40 1.394(5) . ?
C39 C52 1.493(6) . ?
C40 C41 1.380(7) . ?
C41 C42 1.386(6) . ?
C42 C43 1.394(5) . ?
C44 C47 1.526(6) . ?
C44 C46 1.532(6) . ?
C44 C45 1.545(6) . ?
C48 C49 1.514(6) . ?
C48 C51 1.535(7) . ?
C48 C50 1.550(8) . ?
C52 F54 1.335(5) . ?
C52 F53 1.336(5) . ?
C52 F55 1.346(5) . ?
Pd2 N67 1.989(3) . ?
Pd2 N67 1.989(3) 2_688 ?
Pd2 O61 2.012(2) . ?
Pd2 O61 2.012(2) 2_688 ?
O61 C61 1.248(4) . ?
C61 C62 1.452(5) . ?
C61 C66 1.508(4) . ?
C62 C63 1.352(5) . ?
C62 C74 1.530(5) . ?
C63 C64 1.474(5) . ?
C64 C65 1.349(5) . ?
C64 C78 1.519(5) . ?
C65 C66 1.422(5) . ?
C66 N67 1.303(5) . ?
N67 C68 1.432(4) . ?
C68 C73 1.381(5) . ?
C68 C69 1.403(5) . ?
C69 C70 1.389(5) . ?
C69 C82 1.503(5) . ?
C70 C71 1.386(6) . ?
C71 C72 1.385(6) . ?
C72 C73 1.393(5) . ?
C74 C77 1.534(5) . ?
C74 C76 1.536(6) . ?
C74 C75 1.537(6) . ?
C78 C81 1.519(6) . ?
C78 C80 1.532(5) . ?
C78 C79 1.536(6) . ?
C82 F85 1.335(4) . ?
C82 F83 1.337(4) . ?
C82 F84 1.345(4) . ?
B100 F101 1.377(3) . ?
B100 F103 1.384(4) . ?
B100 F102 1.386(3) . ?
B100 F104 1.393(3) . ?
B105 F106 1.382(4) . ?
B105 F108 1.383(4) . ?
B105 F107 1.386(4) . ?
B105 F109 1.388(4) . ?
B200 F202 1.349(7) . ?
B200 F204 1.355(6) . ?
B200 F203 1.372(7) . ?
B200 F201 1.556(6) . ?
F304 B300 1.382(3) . ?
F304 B305 1.385(4) . ?
B300 F302 1.383(3) . ?
B300 F301 1.386(3) . ?
B300 F303 1.392(3) . ?
B305 F307 1.385(4) . ?
B305 F306 1.385(4) . ?
B305 F308 1.386(4) . ?
B400 F401 1.376(6) . ?
B400 F402 1.379(6) . ?
B400 F404 1.390(6) . ?
B400 F403 1.393(6) . ?
C500 Cl52 1.765(4) . ?
C500 Cl51 1.773(4) . ?
C600 Cl62 1.766(4) . ?
C600 Cl61 1.768(4) . ?
C605 Cl67 1.767(5) . ?
C605 Cl66 1.768(5) . ?
|
1100984.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100984.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_1100984
loop_
_publ_author_name
'Swarnalatha Kokatam'
'Thomas Weyherm\"uller'
'Eberhard Bothe'
'Phalguni Chaudhuri'
'Karl Wieghardt'
_publ_section_title
;
Structural Characterization of Four Members of the Electron-Transfer Series
[PdII(L)2)2]n (L = o-Iminophenolate Derivative; n= 2-, 1-, 0, 1+, 2+).
Ligand Mixed Valency in the Monocation and Monoanion with S=1/2 Ground States
;
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3709
_journal_page_last 3717
_journal_paper_doi 10.1021/ic048292i
_journal_volume 44
_journal_year 2005
_chemical_formula_sum 'C44 H52 Cl6 F6 N2 Ni O10'
_chemical_formula_weight 1154.29
_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 98.210(5)
_cell_angle_gamma 90.00
_cell_formula_units_Z 2
_cell_length_a 12.8217(3)
_cell_length_b 15.1119(3)
_cell_length_c 13.2926(3)
_cell_measurement_temperature 100(2)
_cell_volume 2549.18(10)
_computing_cell_refinement 'Nonius Collect Software'
_computing_data_collection 'Nonius Collect Software'
_computing_data_reduction 'Nonius Collect Software'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 100(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type 'Nonius Kappa-CCD'
_diffrn_measurement_method '708 images at 1.0 deg. in \w, 80 sec./frame'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'rotating anode'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0474
_diffrn_reflns_av_sigmaI/netI 0.0378
_diffrn_reflns_limit_h_max 18
_diffrn_reflns_limit_h_min -17
_diffrn_reflns_limit_k_max 21
_diffrn_reflns_limit_k_min -21
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 48195
_diffrn_reflns_theta_full 30.97
_diffrn_reflns_theta_max 30.97
_diffrn_reflns_theta_min 3.10
_exptl_absorpt_coefficient_mu 0.773
_exptl_absorpt_correction_T_max 0.9677
_exptl_absorpt_correction_T_min 0.9396
_exptl_absorpt_correction_type 'Gaussian, face-indexed'
_exptl_crystal_colour red
_exptl_crystal_density_diffrn 1.504
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description 'transparent parallelepiped'
_exptl_crystal_F_000 1188
_exptl_crystal_size_max 0.08
_exptl_crystal_size_mid 0.06
_exptl_crystal_size_min 0.04
_refine_diff_density_max 0.813
_refine_diff_density_min -1.021
_refine_diff_density_rms 0.070
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.029
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 335
_refine_ls_number_reflns 8089
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.029
_refine_ls_R_factor_all 0.0592
_refine_ls_R_factor_gt 0.0423
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0413P)^2^+2.3877P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0984
_refine_ls_wR_factor_ref 0.1071
_reflns_number_gt 6451
_reflns_number_total 8089
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file ic048292isi20041206_054204_5.cif
_cod_data_source_block 6
_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:
'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0413P)^2^+2.3877P] 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^)+(0.0413P)^2^+2.3877P] where P=(Fo^2^+2Fc^2^)/3'.
Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas
;
_cod_database_code 1100984
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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.5000 0.0000 0.5000 0.01281(7) Uani 1 d S . .
O1 O 0.54193(9) 0.02737(8) 0.36173(9) 0.0164(2) Uani 1 d . . .
C1 C 0.63445(12) 0.05179(10) 0.36349(12) 0.0129(3) Uani 1 d . . .
C2 C 0.67955(12) 0.07642(10) 0.27261(12) 0.0145(3) Uani 1 d . . .
C3 C 0.78070(13) 0.10549(11) 0.28815(12) 0.0167(3) Uani 1 d . . .
H3 H 0.8102 0.1242 0.2300 0.020 Uiso 1 calc R . .
C4 C 0.84892(12) 0.11068(10) 0.38704(12) 0.0143(3) Uani 1 d . . .
C5 C 0.80954(12) 0.08869(11) 0.47277(12) 0.0150(3) Uani 1 d . . .
H5 H 0.8531 0.0910 0.5368 0.018 Uiso 1 calc R . .
C6 C 0.70123(12) 0.06177(10) 0.46630(12) 0.0131(3) Uani 1 d . . .
N7 N 0.64953(10) 0.04760(9) 0.54168(10) 0.0142(2) Uani 1 d . . .
C8 C 0.69450(12) 0.06623(11) 0.64401(12) 0.0156(3) Uani 1 d . . .
C9 C 0.70889(13) -0.00531(12) 0.71139(13) 0.0200(3) Uani 1 d . . .
H9 H 0.6901 -0.0633 0.6877 0.024 Uiso 1 calc R . .
C10 C 0.75046(15) 0.00779(14) 0.81266(14) 0.0257(4) Uani 1 d . . .
H10 H 0.7615 -0.0413 0.8576 0.031 Uiso 1 calc R . .
C11 C 0.77585(15) 0.09244(15) 0.84818(14) 0.0280(4) Uani 1 d . . .
H11 H 0.8050 0.1014 0.9172 0.034 Uiso 1 calc R . .
C12 C 0.75868(15) 0.16366(14) 0.78309(15) 0.0265(4) Uani 1 d . . .
H12 H 0.7744 0.2217 0.8084 0.032 Uiso 1 calc R . .
C13 C 0.71835(13) 0.15195(12) 0.68011(13) 0.0196(3) Uani 1 d . . .
C14 C 0.61215(13) 0.06890(12) 0.16832(12) 0.0176(3) Uani 1 d . . .
C15 C 0.51386(14) 0.12831(12) 0.16323(14) 0.0220(3) Uani 1 d . . .
H15A H 0.4720 0.1234 0.0958 0.033 Uiso 1 calc R . .
H15B H 0.5358 0.1899 0.1757 0.033 Uiso 1 calc R . .
H15C H 0.4713 0.1094 0.2150 0.033 Uiso 1 calc R . .
C16 C 0.57895(15) -0.02825(12) 0.14949(14) 0.0238(4) Uani 1 d . . .
H16A H 0.5375 -0.0339 0.0819 0.036 Uiso 1 calc R . .
H16B H 0.5363 -0.0472 0.2012 0.036 Uiso 1 calc R . .
H16C H 0.6419 -0.0655 0.1533 0.036 Uiso 1 calc R . .
C17 C 0.67440(15) 0.09842(17) 0.08422(14) 0.0313(5) Uani 1 d . . .
H17A H 0.6303 0.0922 0.0181 0.047 Uiso 1 calc R . .
H17B H 0.7375 0.0615 0.0858 0.047 Uiso 1 calc R . .
H17C H 0.6953 0.1605 0.0950 0.047 Uiso 1 calc R . .
C18 C 0.96161(12) 0.14274(11) 0.38741(13) 0.0171(3) Uani 1 d . . .
C19 C 1.01733(14) 0.08413(14) 0.31634(15) 0.0248(4) Uani 1 d . . .
H19A H 1.0911 0.1025 0.3201 0.037 Uiso 1 calc R . .
H19B H 0.9820 0.0905 0.2463 0.037 Uiso 1 calc R . .
H19C H 1.0143 0.0221 0.3374 0.037 Uiso 1 calc R . .
C20 C 1.02496(13) 0.14021(13) 0.49396(14) 0.0225(3) Uani 1 d . . .
H20A H 1.0966 0.1616 0.4911 0.034 Uiso 1 calc R . .
H20B H 1.0279 0.0793 0.5195 0.034 Uiso 1 calc R . .
H20C H 0.9910 0.1781 0.5395 0.034 Uiso 1 calc R . .
C21 C 0.95721(15) 0.23893(13) 0.34910(17) 0.0294(4) Uani 1 d . . .
H21A H 1.0290 0.2611 0.3491 0.044 Uiso 1 calc R . .
H21B H 0.9209 0.2757 0.3939 0.044 Uiso 1 calc R . .
H21C H 0.9189 0.2412 0.2799 0.044 Uiso 1 calc R . .
C22 C 0.70310(15) 0.23570(12) 0.61832(16) 0.0259(4) Uani 1 d . . .
F23 F 0.65100(10) 0.22755(8) 0.52527(10) 0.0328(3) Uani 1 d . . .
F24 F 0.79726(11) 0.27096(10) 0.60553(13) 0.0477(4) Uani 1 d . . .
F25 F 0.65422(15) 0.29704(9) 0.66553(12) 0.0546(4) Uani 1 d . . .
C40 C 0.05030(19) 0.14835(17) 0.83751(19) 0.0395(5) Uani 1 d . . .
H40A H 0.0437 0.2064 0.8705 0.047 Uiso 1 calc R . .
H40B H -0.0163 0.1368 0.7919 0.047 Uiso 1 calc R . .
Cl41 Cl 0.06917(6) 0.06566(5) 0.93112(5) 0.05146(17) Uani 1 d . . .
Cl42 Cl 0.15510(5) 0.15279(5) 0.76477(6) 0.04982(17) Uani 1 d . . .
Cl30 Cl 0.36089(7) 0.17816(4) 0.53311(5) 0.01920(13) Uani 0.847(2) d P A 1
O31 O 0.45730(14) 0.13295(12) 0.51132(18) 0.0297(5) Uani 0.847(2) d P A 1
O32 O 0.38836(16) 0.26845(12) 0.5561(2) 0.0406(5) Uani 0.847(2) d P A 1
O33 O 0.32136(16) 0.13469(13) 0.61552(15) 0.0327(4) Uani 0.847(2) d P A 1
O34 O 0.28443(13) 0.17287(12) 0.44356(13) 0.0319(4) Uani 0.847(2) d P A 1
Cl35 Cl 0.3915(3) 0.1746(3) 0.5475(4) 0.01920(13) Uani 0.153(2) d P A 2
O36 O 0.4333(9) 0.1217(8) 0.4703(11) 0.0297(5) Uani 0.153(2) d P A 2
O37 O 0.3674(10) 0.2574(8) 0.5075(12) 0.0406(5) Uani 0.153(2) d P A 2
O38 O 0.2964(9) 0.1310(8) 0.5672(9) 0.0327(4) Uani 0.153(2) d P A 2
O39 O 0.4653(7) 0.1764(7) 0.6388(7) 0.0319(4) Uani 0.153(2) d P A 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
Ni1 0.00901(12) 0.01661(13) 0.01298(13) 0.00205(10) 0.00220(9) -0.00126(10)
O1 0.0117(5) 0.0222(6) 0.0152(5) 0.0017(4) 0.0017(4) -0.0032(4)
C1 0.0126(6) 0.0136(6) 0.0125(6) 0.0007(5) 0.0014(5) 0.0010(5)
C2 0.0141(7) 0.0161(7) 0.0134(7) 0.0008(5) 0.0024(5) -0.0006(5)
C3 0.0142(7) 0.0206(7) 0.0156(7) 0.0022(6) 0.0030(6) -0.0018(6)
C4 0.0113(6) 0.0147(7) 0.0170(7) 0.0003(5) 0.0024(5) -0.0004(5)
C5 0.0106(6) 0.0190(7) 0.0152(7) -0.0004(6) 0.0010(5) -0.0019(5)
C6 0.0102(6) 0.0156(7) 0.0134(7) 0.0007(5) 0.0016(5) 0.0000(5)
N7 0.0114(6) 0.0187(6) 0.0121(6) 0.0003(5) 0.0010(5) -0.0007(5)
C8 0.0113(6) 0.0220(8) 0.0137(7) -0.0016(6) 0.0029(5) -0.0011(6)
C9 0.0179(7) 0.0253(8) 0.0165(7) 0.0003(6) 0.0020(6) -0.0001(6)
C10 0.0236(8) 0.0368(10) 0.0162(8) 0.0036(7) 0.0014(6) 0.0006(7)
C11 0.0236(9) 0.0463(12) 0.0145(8) -0.0064(8) 0.0034(7) -0.0058(8)
C12 0.0231(9) 0.0330(10) 0.0241(9) -0.0130(8) 0.0062(7) -0.0073(7)
C13 0.0168(7) 0.0224(8) 0.0205(8) -0.0033(6) 0.0057(6) -0.0028(6)
C14 0.0155(7) 0.0246(8) 0.0123(7) 0.0021(6) 0.0010(5) -0.0023(6)
C15 0.0210(8) 0.0239(8) 0.0191(8) 0.0053(6) -0.0033(6) 0.0015(6)
C16 0.0273(9) 0.0231(8) 0.0193(8) -0.0038(7) -0.0022(7) -0.0001(7)
C17 0.0223(9) 0.0582(14) 0.0131(8) 0.0068(8) 0.0010(7) -0.0085(9)
C18 0.0117(7) 0.0194(7) 0.0205(8) 0.0013(6) 0.0039(6) -0.0031(6)
C19 0.0159(8) 0.0346(10) 0.0254(9) -0.0009(7) 0.0084(7) -0.0003(7)
C20 0.0134(7) 0.0313(9) 0.0223(8) -0.0017(7) 0.0006(6) -0.0058(6)
C21 0.0234(9) 0.0230(9) 0.0419(11) 0.0071(8) 0.0044(8) -0.0070(7)
C22 0.0272(9) 0.0195(8) 0.0316(10) -0.0065(7) 0.0063(8) -0.0028(7)
F23 0.0416(7) 0.0210(5) 0.0341(7) 0.0039(5) -0.0001(5) -0.0010(5)
F24 0.0355(7) 0.0401(8) 0.0669(10) 0.0132(7) 0.0054(7) -0.0179(6)
F25 0.0882(12) 0.0285(7) 0.0537(9) -0.0039(6) 0.0331(9) 0.0191(7)
C40 0.0331(11) 0.0446(13) 0.0396(13) 0.0026(10) 0.0017(9) 0.0043(10)
Cl41 0.0628(4) 0.0466(4) 0.0453(4) 0.0071(3) 0.0084(3) -0.0026(3)
Cl42 0.0336(3) 0.0549(4) 0.0613(4) 0.0209(3) 0.0078(3) 0.0089(3)
Cl30 0.0154(3) 0.0204(2) 0.0218(3) -0.00169(19) 0.0027(2) 0.0036(3)
O31 0.0170(9) 0.0163(8) 0.0586(15) -0.0037(8) 0.0151(9) 0.0005(6)
O32 0.0340(10) 0.0183(8) 0.0686(17) -0.0151(9) 0.0044(11) 0.0027(7)
O33 0.0395(10) 0.0390(9) 0.0228(9) 0.0077(8) 0.0148(8) 0.0137(8)
O34 0.0272(8) 0.0427(10) 0.0239(8) 0.0056(7) -0.0031(7) 0.0017(7)
Cl35 0.0154(3) 0.0204(2) 0.0218(3) -0.00169(19) 0.0027(2) 0.0036(3)
O36 0.0170(9) 0.0163(8) 0.0586(15) -0.0037(8) 0.0151(9) 0.0005(6)
O37 0.0340(10) 0.0183(8) 0.0686(17) -0.0151(9) 0.0044(11) 0.0027(7)
O38 0.0395(10) 0.0390(9) 0.0228(9) 0.0077(8) 0.0148(8) 0.0137(8)
O39 0.0272(8) 0.0427(10) 0.0239(8) 0.0056(7) -0.0031(7) 0.0017(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'
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'
Cl Cl 0.1484 0.1585 '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
O1 Ni1 O1 180.0 3_656 . ?
O1 Ni1 O36 78.4(4) 3_656 3_656 ?
O1 Ni1 O36 101.6(4) . 3_656 ?
O1 Ni1 O36 101.6(4) 3_656 . ?
O1 Ni1 O36 78.4(4) . . ?
O36 Ni1 O36 179.999(2) 3_656 . ?
O1 Ni1 N7 79.32(5) 3_656 3_656 ?
O1 Ni1 N7 100.68(5) . 3_656 ?
O36 Ni1 N7 94.9(3) 3_656 3_656 ?
O36 Ni1 N7 85.1(3) . 3_656 ?
O1 Ni1 N7 100.68(5) 3_656 . ?
O1 Ni1 N7 79.32(5) . . ?
O36 Ni1 N7 85.1(3) 3_656 . ?
O36 Ni1 N7 94.9(3) . . ?
N7 Ni1 N7 180.0 3_656 . ?
O1 Ni1 O31 88.59(7) 3_656 3_656 ?
O1 Ni1 O31 91.41(7) . 3_656 ?
O36 Ni1 O31 16.9(4) 3_656 3_656 ?
O36 Ni1 O31 163.1(4) . 3_656 ?
N7 Ni1 O31 83.56(6) 3_656 3_656 ?
N7 Ni1 O31 96.44(6) . 3_656 ?
O1 Ni1 O31 91.41(7) 3_656 . ?
O1 Ni1 O31 88.59(7) . . ?
O36 Ni1 O31 163.1(4) 3_656 . ?
O36 Ni1 O31 16.9(4) . . ?
N7 Ni1 O31 96.44(6) 3_656 . ?
N7 Ni1 O31 83.56(6) . . ?
O31 Ni1 O31 180.0 3_656 . ?
C1 O1 Ni1 114.84(10) . . ?
O1 C1 C2 123.46(14) . . ?
O1 C1 C6 117.61(13) . . ?
C2 C1 C6 118.81(13) . . ?
C3 C2 C1 116.07(14) . . ?
C3 C2 C14 124.48(14) . . ?
C1 C2 C14 119.45(13) . . ?
C2 C3 C4 125.86(15) . . ?
C5 C4 C3 119.56(14) . . ?
C5 C4 C18 122.93(15) . . ?
C3 C4 C18 117.50(14) . . ?
C4 C5 C6 119.53(14) . . ?
N7 C6 C5 126.65(14) . . ?
N7 C6 C1 113.32(13) . . ?
C5 C6 C1 119.96(13) . . ?
C6 N7 C8 121.51(13) . . ?
C6 N7 Ni1 114.28(10) . . ?
C8 N7 Ni1 124.19(10) . . ?
C9 C8 C13 119.55(15) . . ?
C9 C8 N7 117.13(15) . . ?
C13 C8 N7 123.22(15) . . ?
C10 C9 C8 120.49(17) . . ?
C11 C10 C9 120.03(18) . . ?
C12 C11 C10 119.86(17) . . ?
C11 C12 C13 121.15(18) . . ?
C8 C13 C12 118.87(17) . . ?
C8 C13 C22 125.85(16) . . ?
C12 C13 C22 115.28(16) . . ?
C2 C14 C17 110.76(14) . . ?
C2 C14 C16 109.01(14) . . ?
C17 C14 C16 108.69(15) . . ?
C2 C14 C15 110.44(14) . . ?
C17 C14 C15 107.86(15) . . ?
C16 C14 C15 110.07(14) . . ?
C4 C18 C20 111.91(14) . . ?
C4 C18 C21 108.03(14) . . ?
C20 C18 C21 108.65(15) . . ?
C4 C18 C19 109.71(14) . . ?
C20 C18 C19 108.76(14) . . ?
C21 C18 C19 109.76(15) . . ?
F23 C22 F25 107.31(17) . . ?
F23 C22 F24 105.03(16) . . ?
F25 C22 F24 105.95(16) . . ?
F23 C22 C13 116.10(15) . . ?
F25 C22 C13 111.26(16) . . ?
F24 C22 C13 110.54(16) . . ?
Cl41 C40 Cl42 112.13(13) . . ?
O33 Cl30 O32 112.19(14) . . ?
O33 Cl30 O34 109.60(13) . . ?
O32 Cl30 O34 110.43(14) . . ?
O33 Cl30 O31 109.61(13) . . ?
O32 Cl30 O31 107.19(13) . . ?
O34 Cl30 O31 107.69(12) . . ?
Cl30 O31 Ni1 133.87(11) . . ?
O37 Cl35 O39 113.3(8) . . ?
O37 Cl35 O38 109.6(8) . . ?
O39 Cl35 O38 109.2(7) . . ?
O37 Cl35 O36 108.0(9) . . ?
O39 Cl35 O36 110.0(7) . . ?
O38 Cl35 O36 106.4(7) . . ?
Cl35 O36 Ni1 122.8(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
Ni1 O1 2.0298(11) 3_656 ?
Ni1 O1 2.0298(11) . ?
Ni1 O36 2.043(12) 3_656 ?
Ni1 O36 2.043(12) . ?
Ni1 N7 2.0486(13) 3_656 ?
Ni1 N7 2.0487(13) . ?
Ni1 O31 2.0933(18) 3_656 ?
Ni1 O31 2.0934(18) . ?
O1 C1 1.2394(18) . ?
C1 C2 1.460(2) . ?
C1 C6 1.513(2) . ?
C2 C3 1.357(2) . ?
C2 C14 1.529(2) . ?
C3 C4 1.473(2) . ?
C4 C5 1.352(2) . ?
C4 C18 1.523(2) . ?
C5 C6 1.438(2) . ?
C6 N7 1.296(2) . ?
N7 C8 1.428(2) . ?
C8 C9 1.399(2) . ?
C8 C13 1.400(2) . ?
C9 C10 1.389(2) . ?
C10 C11 1.386(3) . ?
C11 C12 1.379(3) . ?
C12 C13 1.404(3) . ?
C13 C22 1.506(3) . ?
C14 C17 1.530(2) . ?
C14 C16 1.539(2) . ?
C14 C15 1.541(2) . ?
C18 C20 1.529(2) . ?
C18 C21 1.539(2) . ?
C18 C19 1.543(2) . ?
C22 F23 1.325(2) . ?
C22 F25 1.326(2) . ?
C22 F24 1.352(2) . ?
C40 Cl41 1.756(3) . ?
C40 Cl42 1.765(2) . ?
Cl30 O33 1.4308(19) . ?
Cl30 O32 1.431(2) . ?
Cl30 O34 1.4321(18) . ?
Cl30 O31 1.4769(19) . ?
Cl35 O37 1.377(14) . ?
Cl35 O39 1.428(10) . ?
Cl35 O38 1.443(13) . ?
Cl35 O36 1.462(13) . ?
|
1100985.cif | #------------------------------------------------------------------------------
#$Date: 2022-09-14 17:31:13 +0300 (Wed, 14 Sep 2022) $
#$Revision: 277831 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/09/1100985.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_1100985
loop_
_publ_author_name
'Yamamura, Kimiaki'
'Kawashima Taiga'
'Eda, Kazuo'
'Tajima, Fukue'
'Hashimoto, Masao'
_publ_section_title
;
Solid solution of triptycenequinone and triptycenehydroquinone as
a non-stoichiometric quinhydrone. Bathochromic changes in color
caused by local intermolecular interaction between p-benzoquinone
and hydroquinone moieties
;
_journal_issue 1
_journal_name_full 'Journal of Molecular Structure'
_journal_page_first 1
_journal_page_last 6
_journal_paper_doi 10.1016/j.molstruc.2004.10.002
_journal_volume 737
_journal_year 2005
_chemical_formula_moiety 'C20 H12 O2 and C20 H14 O2'
_chemical_formula_sum 'C20 H12.4 O2'
_chemical_formula_weight 284.70
_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_space_group_name_Hall '-P 2ac 2n'
_symmetry_space_group_name_H-M 'P n m a'
_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 90.00
_cell_formula_units_Z 4
_cell_length_a 13.9840(10)
_cell_length_b 12.722(2)
_cell_length_c 8.024(2)
_cell_measurement_reflns_used 22
_cell_measurement_temperature 299.2
_cell_measurement_theta_max 14.8
_cell_measurement_theta_min 12.7
_cell_volume 1427.5(4)
_diffrn_ambient_temperature 299.2
_diffrn_measurement_device_type 'scintillation counter'
_diffrn_measurement_method \w-2\q
_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 0.0593
_diffrn_reflns_limit_h_max 18
_diffrn_reflns_limit_h_min 0
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_l_max 0
_diffrn_reflns_limit_l_min -10
_diffrn_reflns_number 1718
_diffrn_reflns_theta_max 27.50
_diffrn_reflns_theta_min 2.91
_diffrn_standards_decay_% 3.77
_diffrn_standards_interval_count 150
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 0.0846
_exptl_absorpt_correction_T_max 1.000
_exptl_absorpt_correction_T_min 0.967
_exptl_absorpt_correction_type psi-scan
_exptl_absorpt_process_details 'Absorption correction given as psi-scan'
_exptl_crystal_colour brown
_exptl_crystal_density_diffrn 1.325
_exptl_crystal_density_meas 1.32
_exptl_crystal_density_method 'floating method'
_exptl_crystal_description prismatic
_exptl_crystal_F_000 594
_exptl_crystal_size_max 0.60
_exptl_crystal_size_mid 0.35
_exptl_crystal_size_min 0.30
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.075
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 132
_refine_ls_number_reflns 1718
_refine_ls_number_restraints 1
_refine_ls_restrained_S_all 1.075
_refine_ls_R_factor_all 0.1592
_refine_ls_R_factor_gt 0.0882
_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^)+(0.1591P)^2^+0.1126P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2639
_refine_ls_wR_factor_ref 0.2835
_reflns_number_gt 897
_reflns_number_total 1718
_reflns_threshold_expression >2sigma(I)
_cod_original_formula_sum 'C20 H12.40 O2'
_cod_database_code 1100985
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x+1/2, -y, z+1/2'
'-x, -y, -z'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, 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
O1 O 0.4178(3) 0.0404(4) 0.0844(7) 0.082(2) Uani 0.523(8) 1 d P . .
O2 O 0.7517(6) 0.0447(7) 0.0847(13) 0.136(5) Uani 0.397(8) 1 d P . .
O3 O 0.5695(13) 0.0390(16) 0.557(2) 0.029(7) Uiso 0.080(6) 1 d P . .
C1 C 0.4200(2) 0.1391(3) 0.0793(3) 0.0566(9) Uani 1 1 d . . .
C2 C 0.3456(2) 0.1972(3) -0.0019(4) 0.0699(11) Uani 1 1 d . . .
C3 C 0.7444(3) 0.1369(4) 0.0798(4) 0.0746(12) Uani 1 1 d . . .
C4 C 0.8183(3) 0.1960(4) 0.0028(4) 0.0982(19) Uani 1 1 d . . .
C5 C 0.5823(2) 0.1488(3) 0.2413(3) 0.0475(8) Uani 1 1 d . . .
C6 C 0.49599(17) 0.1969(2) 0.1547(3) 0.0433(7) Uani 1 1 d . . .
C7 C 0.5808(2) 0.1405(3) 0.5648(3) 0.0632(11) Uani 1 1 d . . .
C8 C 0.5814(2) 0.1960(3) 0.7128(4) 0.0805(14) Uani 1 1 d . . .
C9 C 0.66859(17) 0.1951(3) 0.1541(3) 0.0526(8) Uani 1 1 d . . .
C10 C 0.58228(16) 0.1948(2) 0.4154(3) 0.0465(8) Uani 1 1 d . . .
H1 H 0.575(2) 0.079(3) 0.249(4) 0.060(9) Uiso 1 1 d . . .
H3 H 0.877(3) 0.136(4) -0.053(5) 0.123(15) Uiso 1 1 d . . .
H4 H 0.586(2) 0.168(3) 0.831(5) 0.105(13) Uiso 1 1 d . . .
H2 H 0.293(2) 0.159(2) -0.071(3) 0.060(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
O1 0.075(4) 0.063(3) 0.108(4) -0.020(2) -0.024(3) -0.018(3)
O2 0.084(6) 0.090(6) 0.236(13) -0.072(7) -0.008(6) 0.010(5)
C1 0.0445(17) 0.076(2) 0.0498(16) -0.0131(15) 0.0011(15) -0.0085(18)
C2 0.0396(17) 0.106(3) 0.0646(18) -0.0135(19) -0.0093(13) -0.0095(18)
C3 0.0464(19) 0.115(4) 0.063(2) -0.025(2) -0.0049(16) 0.017(2)
C4 0.0407(17) 0.192(6) 0.0623(18) -0.021(2) 0.0031(14) 0.012(2)
C5 0.0422(15) 0.0510(17) 0.0494(15) 0.0000(13) -0.0028(12) 0.0005(15)
C6 0.0388(14) 0.0576(16) 0.0336(12) -0.0022(12) 0.0040(11) -0.0035(13)
C7 0.0395(16) 0.099(3) 0.0514(17) 0.0208(16) -0.0066(14) 0.0021(18)
C8 0.060(2) 0.148(4) 0.0335(14) 0.0172(16) 0.0010(13) 0.006(2)
C9 0.0295(13) 0.091(2) 0.0375(13) -0.0085(14) -0.0029(11) 0.0048(13)
C10 0.0324(13) 0.0668(18) 0.0404(13) 0.0047(11) -0.0037(11) -0.0050(15)
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
2 -2 -2
0 -3 -2
3 -3 -1
|
1100986.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100986.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_1100986
_chemical_formula_sum 'K2 Mo4 O13'
_chemical_formula_weight 669.96
_chemical_name_common 'potassium tetramolybdate'
_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 107.104(4)
_cell_angle_beta 102.884(5)
_cell_angle_gamma 109.765(5)
_cell_formula_units_Z 2
_cell_length_a 7.977(2)
_cell_length_b 8.346(2)
_cell_length_c 10.018(3)
_cell_measurement_reflns_used 892
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 26.892
_cell_measurement_theta_min 2.832
_cell_volume 560.0(3)
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean ?
_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 0.0255
_diffrn_reflns_av_sigmaI/netI 0.0493
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -4
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_l_max 12
_diffrn_reflns_limit_l_min -12
_diffrn_reflns_number 3202
_diffrn_reflns_theta_max 27.22
_diffrn_reflns_theta_min 2.28
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 5.089
_exptl_absorpt_correction_T_max ?
_exptl_absorpt_correction_T_min ?
_exptl_absorpt_correction_type 'SADABS ver. 2.03(Sheldrick)'
_exptl_absorpt_process_details ?
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 3.973
_exptl_crystal_density_meas 3.98(5)
_exptl_crystal_density_method pycnometry
_exptl_crystal_description needle
_exptl_crystal_F_000 594
_exptl_crystal_size_max 0.25
_exptl_crystal_size_mid 0.04
_exptl_crystal_size_min 0.02
_refine_ls_extinction_coef ?
_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 172
_refine_ls_number_reflns 2172
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.053
_refine_ls_R_factor_all 0.0464
_refine_ls_R_factor_gt 0.0355
_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^)+(0.0481P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0875
_refine_ls_wR_factor_ref 0.0935
_reflns_number_gt 1711
_reflns_number_total 2172
_reflns_threshold_expression >2sigma(I)
_cod_original_sg_symbol_H-M P-1
_cod_database_code 1100986
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
Mo1 Mo 0.22480(9) 0.89721(8) 0.27148(6) 0.01149(17) Uani 1 1 d . . .
Mo2 Mo 0.18990(8) 0.99621(8) -0.04826(6) 0.01047(17) Uani 1 1 d . . .
Mo3 Mo 0.17060(8) 0.59255(8) -0.06205(6) 0.01160(17) Uani 1 1 d . . .
Mo4 Mo -0.22353(8) 0.70302(8) -0.29193(6) 0.01128(17) Uani 1 1 d . . .
K1 K 0.2545(3) 0.7153(2) 0.56403(19) 0.0235(4) Uani 1 1 d . . .
K2 K 0.6893(3) 0.7390(3) 0.3091(2) 0.0300(4) Uani 1 1 d . . .
O1 O 0.4120(7) 0.8589(7) 0.3457(6) 0.0205(12) Uani 1 1 d . . .
O2 O 0.1009(7) 0.8848(7) 0.3898(5) 0.0197(11) Uani 1 1 d . . .
O3 O 0.3639(7) 1.1581(6) 0.3383(5) 0.0158(11) Uani 1 1 d . . .
O4 O 0.0420(7) 0.9887(6) 0.1369(5) 0.0113(10) Uani 1 1 d . . .
O5 O 0.2958(7) 0.8698(6) 0.0584(5) 0.0128(10) Uani 1 1 d . . .
O6 O 0.0513(7) 0.6366(6) 0.1179(5) 0.0131(10) Uani 1 1 d . . .
O7 O 0.3224(7) 1.2221(6) 0.0875(5) 0.0156(11) Uani 1 1 d . . .
O8 O 0.2818(7) 0.9871(7) -0.1859(5) 0.0178(11) Uani 1 1 d . . .
O9 O -0.0217(7) 0.7141(6) -0.1430(5) 0.0134(10) Uani 1 1 d . . .
O10 O 0.3464(8) 0.5610(7) 0.0397(6) 0.0219(12) Uani 1 1 d . . .
O11 O 0.2035(8) 0.5574(7) -0.2287(6) 0.0234(13) Uani 1 1 d . . .
O12 O -0.3998(7) 0.4848(7) -0.3532(5) 0.0182(11) Uani 1 1 d . . .
O13 O -0.1270(8) 0.6900(7) -0.4291(5) 0.0211(12) 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
Mo1 0.0154(3) 0.0092(3) 0.0088(3) 0.0025(2) 0.0028(3) 0.0060(3)
Mo2 0.0110(3) 0.0092(3) 0.0113(3) 0.0037(2) 0.0041(2) 0.0047(2)
Mo3 0.0137(3) 0.0092(3) 0.0131(3) 0.0037(2) 0.0064(3) 0.0059(3)
Mo4 0.0133(3) 0.0081(3) 0.0098(3) 0.0016(2) 0.0019(3) 0.0047(3)
K1 0.0264(9) 0.0237(9) 0.0214(9) 0.0080(7) 0.0106(8) 0.0115(8)
K2 0.0282(10) 0.0332(11) 0.0458(12) 0.0252(9) 0.0210(9) 0.0200(9)
O10 0.023(3) 0.019(3) 0.026(3) 0.009(2) 0.009(3) 0.012(3)
O6 0.017(3) 0.012(2) 0.011(2) 0.004(2) 0.006(2) 0.006(2)
O5 0.014(3) 0.008(2) 0.014(3) 0.002(2) 0.003(2) 0.006(2)
O1 0.023(3) 0.018(3) 0.020(3) 0.004(2) 0.006(2) 0.012(2)
O2 0.021(3) 0.019(3) 0.019(3) 0.005(2) 0.007(2) 0.010(2)
O7 0.013(3) 0.014(3) 0.017(3) 0.003(2) 0.006(2) 0.006(2)
O13 0.025(3) 0.022(3) 0.017(3) 0.006(2) 0.009(2) 0.012(3)
O12 0.020(3) 0.018(3) 0.012(3) 0.005(2) 0.003(2) 0.006(2)
O8 0.021(3) 0.017(3) 0.017(3) 0.006(2) 0.008(2) 0.010(2)
O11 0.035(3) 0.021(3) 0.023(3) 0.009(2) 0.019(3) 0.015(3)
O9 0.013(2) 0.012(2) 0.016(3) 0.009(2) 0.003(2) 0.005(2)
O3 0.015(3) 0.014(3) 0.017(3) 0.006(2) 0.001(2) 0.007(2)
O4 0.014(2) 0.004(2) 0.012(2) -0.0009(19) 0.003(2) 0.004(2)
|
1100987.cif | #------------------------------------------------------------------------------
#$Date: 2017-07-04 17:40:00 +0300 (Tue, 04 Jul 2017) $
#$Revision: 198384 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/09/1100987.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_1100987
loop_
_publ_author_name
'He, M'
'Chen, X'
'Lan, Y'
'Li, H'
'Xu, Y'
_publ_section_title
;
Ab initio structure determination of new compound LiAlB~2~O~5~
;
_journal_name_full 'Journal of Solid State Chemistry'
_journal_page_first 181
_journal_page_last 184
_journal_paper_doi 10.1006/jssc.2000.8979
_journal_volume 156
_journal_year 2001
_chemical_formula_structural 'Li Al B2 O5'
_chemical_formula_sum 'Al B2 Li O5'
_chemical_name_systematic
;
Lithium Aluminium Boron Oxide (1/1/2/5)
;
_space_group_crystal_system monoclinic
_space_group_IT_number 15
_space_group_name_Hall '-C 2yc'
_space_group_name_H-M_alt 'C 1 2/c 1'
_cell_angle_alpha 90
_cell_angle_beta 120.0681(3)
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 9.9096(1)
_cell_length_b 10.0634(1)
_cell_length_c 9.3552(1)
_cell_volume 807.39
_refine_ls_R_factor_all 0.07
_cod_duplicate_entry 1100045
_cod_depositor_comments
;
Changing the space group from 'P 1 2/c 1' to 'C 1 2/c 1' after consulting
the original publication. All related space group information was changed
accordingly.
Antanas Vaitkus,
2017-07-04
;
_cod_original_sg_symbol_H-M 'C 2/c'
_cod_database_code 1100987
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,y,-z+1/2
3 -x,-y,-z
4 x,-y,z+1/2
5 x+1/2,y+1/2,z
6 -x+1/2,y+1/2,-z+1/2
7 -x+1/2,-y+1/2,-z
8 x+1/2,-y+1/2,z+1/2
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_calc_flag
Al1 Al3+ 8 f 0.1948(2) 0.1523(2) 0.1510(2) 1. 0 d
B1 B3+ 8 f -0.0662(7) 0.3266(7) -0.0308(8) 1. 0 d
B2 B3+ 8 f 0.2341(8) -0.0050(6) 0.4071(8) 1. 0 d
Li1 Li1+ 4 e 0. 0.378(1) 0.25 1. 0 d
Li2 Li1+ 4 e 0. 0.159(2) 0.75 1. 0 d
O1 O2- 8 f 0.0582(4) 0.2754(3) 0.1104(4) 1. 0 d
O2 O2- 8 f -0.1232(3) 0.2944(3) -0.1897(3) 1. 0 d
O3 O2- 8 f -0.1386(4) 0.4271(3) 0.0238(4) 1. 0 d
O4 O2- 8 f 0.1581(4) 0.0184(3) 0.2428(4) 1. 0 d
O5 O2- 8 f 0.1846(4) 0.1071(3) -0.0311(4) 1. 0 d
loop_
_atom_type_symbol
_atom_type_oxidation_number
Al3+ 2.000
B3+ 3.000
Li1+ 1.000
O2- -2.000
|
1100988.cif | #------------------------------------------------------------------------------
#$Date: 2022-09-14 17:31:13 +0300 (Wed, 14 Sep 2022) $
#$Revision: 277831 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/09/1100988.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_1100988
loop_
_publ_author_name
'Maldonado, Carmen R.'
'Quir\'os, Miguel'
'Salas, Juan M.'
'S\'anchez, M. Purificaci\'on'
_publ_section_title
;
5,7-Dimethyl-1,2,4-triazolo[1,5-a]pyrimidinium
tetrachlorocobaltate(II) monohydrate
;
_journal_coden_ASTM ACSEBH
_journal_coeditor_code YA6255
_journal_issue 9
_journal_name_full
;
Acta Crystallographica, Section E: Structure Reports Online
;
_journal_page_first m1721
_journal_page_last m1723
_journal_paper_doi 10.1107/S1600536805024633
_journal_volume 61
_journal_year 2005
_chemical_formula_moiety '(C7 H9 N4 1+)2, Cl4 Co 2-, H2 O'
_chemical_formula_sum 'C14 H20 Cl4 Co N8 O'
_chemical_formula_weight 517.11
_chemical_name_systematic
;
5,7-dimethyl-1,2,4-triazolo-[1,5-a]pyrimidinium
tetrachlorocobaltate(II) monohydrate.
;
_space_group_IT_number 2
_space_group_name_Hall '-P 1'
_space_group_name_H-M_alt 'P -1'
_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 heavy
_atom_sites_solution_secondary difmap
_cell_angle_alpha 84.952(1)
_cell_angle_beta 84.505(1)
_cell_angle_gamma 65.275(1)
_cell_formula_units_Z 2
_cell_length_a 7.6369(4)
_cell_length_b 8.5190(4)
_cell_length_c 18.2777(9)
_cell_measurement_reflns_used 5772
_cell_measurement_temperature 298(2)
_cell_measurement_theta_max 27.2
_cell_measurement_theta_min 2.2
_cell_volume 1073.64(9)
_diffrn_ambient_temperature 298(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measurement_device_type 'Bruker SMART APEX CCD system'
_diffrn_measurement_method '\f and \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 0.019
_diffrn_reflns_av_sigmaI/netI 0.023
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 23
_diffrn_reflns_limit_l_min -24
_diffrn_reflns_number 12624
_diffrn_reflns_theta_max 28.3
_diffrn_reflns_theta_min 2.2
_diffrn_standards_decay_% 0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number 222
_exptl_absorpt_coefficient_mu 1.32
_exptl_absorpt_correction_T_max 0.751
_exptl_absorpt_correction_T_min 0.668
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)'
_exptl_crystal_colour blue
_exptl_crystal_density_diffrn 1.600
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prismatic
_exptl_crystal_F_000 526
_exptl_crystal_size_max 0.46
_exptl_crystal_size_mid 0.29
_exptl_crystal_size_min 0.23
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.04
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 263
_refine_ls_number_reflns 4866
_refine_ls_number_restraints 3
_refine_ls_restrained_S_all 1.04
_refine_ls_R_factor_all 0.037
_refine_ls_R_factor_gt 0.031
_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^)+(0.04P)^2^+0.25P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.077
_refine_ls_wR_factor_ref 0.080
_reflns_number_gt 4217
_reflns_number_total 4866
_reflns_threshold_expression I>2\s(I)
_cod_duplicate_entry 2206828
_cod_database_code 1100988
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
Co Co 0.11422(3) 0.44963(3) 0.248561(13) 0.03963(9) Uani 1 1 d . . .
Cl1 Cl 0.00141(7) 0.64882(6) 0.33725(3) 0.05152(13) Uani 1 1 d . . .
Cl2 Cl 0.34565(7) 0.48632(7) 0.17064(3) 0.05223(13) Uani 1 1 d . . .
Cl3 Cl -0.12146(8) 0.46295(8) 0.17920(3) 0.06222(15) Uani 1 1 d . . .
Cl4 Cl 0.25025(11) 0.19090(7) 0.31175(3) 0.06899(18) Uani 1 1 d . . .
N1A N 0.3772(2) 0.7362(2) 0.00403(9) 0.0445(4) Uani 1 1 d . . .
C2A C 0.2741(3) 0.6835(2) -0.03184(11) 0.0455(4) Uani 1 1 d . . .
H2A H 0.3227 0.6178 -0.0730 0.055 Uiso 1 1 d R . .
N3A N 0.0906(2) 0.73306(19) -0.00317(9) 0.0424(3) Uani 1 1 d . . .
H3A H 0.0017 0.7113 -0.0196 0.051 Uiso 1 1 d R . .
C3aA C 0.0734(2) 0.8231(2) 0.05597(10) 0.0375(4) Uani 1 1 d . . .
N4A N -0.0789(2) 0.89762(19) 0.10141(9) 0.0420(3) Uani 1 1 d . . .
C5A C -0.0487(3) 0.9754(2) 0.15607(11) 0.0440(4) Uani 1 1 d . . .
C51A C -0.2146(3) 1.0602(3) 0.21017(13) 0.0600(6) Uani 1 1 d . . .
H51A H -0.3298 1.1240 0.1846 0.072 Uiso 1 1 d R . .
H52A H -0.1877 1.1377 0.2376 0.072 Uiso 1 1 d R . .
H53A H -0.2328 0.9735 0.2433 0.072 Uiso 1 1 d R . .
C6A C 0.1319(3) 0.9785(2) 0.16388(11) 0.0467(4) Uani 1 1 d . . .
H6A H 0.1460 1.0338 0.2031 0.056 Uiso 1 1 d R . .
C7A C 0.2853(3) 0.9025(2) 0.11524(11) 0.0434(4) Uani 1 1 d . . .
C71A C 0.4817(3) 0.8951(3) 0.11745(14) 0.0605(6) Uani 1 1 d . . .
H71A H 0.5717 0.7766 0.1246 0.073 Uiso 1 1 d R . .
H72A H 0.4844 0.9597 0.1574 0.073 Uiso 1 1 d R . .
H73A H 0.5167 0.9434 0.0719 0.073 Uiso 1 1 d R . .
N8A N 0.2486(2) 0.82536(18) 0.05973(8) 0.0377(3) Uani 1 1 d . . .
N1B N 0.4223(3) 0.2049(2) 0.54414(10) 0.0509(4) Uani 1 1 d . . .
C2B C 0.3349(3) 0.2344(3) 0.48328(11) 0.0518(5) Uani 1 1 d . . .
H2B H 0.3406 0.1463 0.4552 0.062 Uiso 1 1 d R . .
N3B N 0.2361(2) 0.4043(2) 0.46483(9) 0.0507(4) Uani 1 1 d . . .
H3B H 0.1699 0.4480 0.4269 0.061 Uiso 1 1 d R . .
C3aB C 0.2623(3) 0.4920(2) 0.51784(10) 0.0434(4) Uani 1 1 d . . .
N4B N 0.1948(3) 0.6608(2) 0.52371(9) 0.0516(4) Uani 1 1 d . . .
C5B C 0.2455(3) 0.7079(3) 0.58343(11) 0.0514(5) Uani 1 1 d . . .
C51B C 0.1717(4) 0.8983(3) 0.59242(15) 0.0736(7) Uani 1 1 d . . .
H51B H 0.0565 0.9367 0.6246 0.088 Uiso 1 1 d R . .
H52B H 0.2690 0.9214 0.6130 0.088 Uiso 1 1 d R . .
H53B H 0.1435 0.9590 0.5452 0.088 Uiso 1 1 d R . .
C6B C 0.3597(3) 0.5869(3) 0.63552(11) 0.0507(5) Uani 1 1 d . . .
H6B H 0.3912 0.6264 0.6760 0.061 Uiso 1 1 d R . .
C7B C 0.4265(3) 0.4134(3) 0.62791(11) 0.0461(4) Uani 1 1 d . . .
C71B C 0.5435(4) 0.2725(3) 0.67934(13) 0.0646(6) Uani 1 1 d . . .
H71B H 0.5600 0.3210 0.7223 0.078 Uiso 1 1 d R . .
H72B H 0.4791 0.1979 0.6936 0.078 Uiso 1 1 d R . .
H73B H 0.6676 0.2071 0.6554 0.078 Uiso 1 1 d R . .
N8B N 0.3753(2) 0.37010(19) 0.56583(8) 0.0407(3) Uani 1 1 d . . .
O1W O 0.2132(2) 0.3126(2) 0.04297(9) 0.0669(5) Uani 1 1 d D . .
H11W H 0.324(2) 0.298(3) 0.0241(12) 0.080 Uiso 1 1 d D . .
H12W H 0.195(3) 0.359(3) 0.0834(8) 0.080 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
Co 0.04355(15) 0.03955(14) 0.03598(14) -0.00496(10) -0.00103(10) -0.01714(11)
Cl1 0.0591(3) 0.0440(3) 0.0459(3) -0.0120(2) 0.0016(2) -0.0150(2)
Cl2 0.0497(3) 0.0594(3) 0.0497(3) -0.0059(2) 0.0065(2) -0.0261(2)
Cl3 0.0493(3) 0.0757(4) 0.0647(3) -0.0168(3) -0.0104(2) -0.0248(3)
Cl4 0.1134(5) 0.0401(3) 0.0502(3) 0.0007(2) -0.0190(3) -0.0262(3)
N1A 0.0373(8) 0.0475(9) 0.0453(9) -0.0042(7) -0.0028(7) -0.0138(7)
C2A 0.0426(10) 0.0467(10) 0.0450(10) -0.0064(8) -0.0033(8) -0.0154(8)
N3A 0.0409(8) 0.0438(8) 0.0457(9) -0.0082(7) -0.0069(7) -0.0188(7)
C3aA 0.0376(9) 0.0340(8) 0.0432(9) 0.0014(7) -0.0089(7) -0.0164(7)
N4A 0.0374(8) 0.0394(8) 0.0487(9) -0.0044(7) -0.0026(6) -0.0149(6)
C5A 0.0471(10) 0.0361(9) 0.0458(10) -0.0027(8) -0.0050(8) -0.0139(8)
C51A 0.0601(13) 0.0608(13) 0.0573(13) -0.0176(10) 0.0079(10) -0.0229(11)
C6A 0.0533(11) 0.0434(10) 0.0457(10) -0.0070(8) -0.0112(9) -0.0196(9)
C7A 0.0443(10) 0.0400(9) 0.0493(10) 0.0003(8) -0.0150(8) -0.0188(8)
C71A 0.0490(12) 0.0706(14) 0.0698(15) -0.0093(12) -0.0161(10) -0.0289(11)
N8A 0.0349(7) 0.0369(7) 0.0407(8) -0.0009(6) -0.0058(6) -0.0140(6)
N1B 0.0606(10) 0.0428(9) 0.0512(10) -0.0115(7) -0.0021(8) -0.0217(8)
C2B 0.0609(13) 0.0516(12) 0.0495(11) -0.0127(9) 0.0001(9) -0.0285(10)
N3B 0.0585(10) 0.0572(10) 0.0401(9) -0.0066(7) -0.0042(7) -0.0267(8)
C3aB 0.0470(10) 0.0491(10) 0.0363(9) -0.0066(8) 0.0058(8) -0.0232(9)
N4B 0.0613(11) 0.0446(9) 0.0460(9) -0.0032(7) 0.0029(8) -0.0201(8)
C5B 0.0618(13) 0.0450(11) 0.0489(11) -0.0104(9) 0.0120(9) -0.0253(10)
C51B 0.101(2) 0.0473(12) 0.0685(16) -0.0127(11) 0.0049(14) -0.0273(13)
C6B 0.0595(12) 0.0528(11) 0.0453(11) -0.0139(9) 0.0039(9) -0.0279(10)
C7B 0.0481(11) 0.0501(11) 0.0429(10) -0.0068(8) 0.0001(8) -0.0230(9)
C71B 0.0742(15) 0.0571(13) 0.0612(14) -0.0048(11) -0.0230(12) -0.0215(11)
N8B 0.0442(8) 0.0394(8) 0.0404(8) -0.0072(6) 0.0026(6) -0.0192(7)
O1W 0.0530(9) 0.1006(13) 0.0621(10) -0.0345(9) 0.0058(7) -0.0426(9)
loop_
_cod_changelog_entry_id
_cod_changelog_entry_author
_cod_changelog_entry_date
_cod_changelog_entry_text
1 'Vaitkus, Antanas' 2021-10-23T22:30:00+03:00
'Updated bibliographic information.'
|
1100989.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100989.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_1100989
loop_
_publ_author_name
'Hashimoto, Masao'
'Tajima, Fukue'
'Eda, Kazuo'
'Yamamura, Kimiaki'
'Okazaki, Tadashi'
_publ_section_title
;
Exploration of plastic-like phases in alkylurea systems.
A thermal and X-ray study
;
_journal_issue 1-3
_journal_name_full 'Journal of Molecular Structure'
_journal_page_first 23
_journal_page_last 33
_journal_paper_doi 10.1016/j.molstruc.2004.08.008
_journal_volume 734
_journal_year 2005
_chemical_formula_moiety 'C3 H8 N2 O'
_chemical_formula_sum 'C3 H8 N2 O'
_chemical_formula_weight 88.11
_chemical_melting_point 356.7
_chemical_name_common n-ethylurea
_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 107.483(17)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 8.315(7)
_cell_length_b 7.046(6)
_cell_length_c 9.099(8)
_cell_measurement_reflns_used 712
_cell_measurement_temperature 297(2)
_cell_measurement_theta_max 23.283
_cell_measurement_theta_min 2.561
_cell_volume 508.4(8)
_diffrn_ambient_temperature 297(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 0.0640
_diffrn_reflns_av_sigmaI/netI 0.0774
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -5
_diffrn_reflns_limit_k_max 8
_diffrn_reflns_limit_k_min -8
_diffrn_reflns_limit_l_max 11
_diffrn_reflns_limit_l_min -10
_diffrn_reflns_number 2691
_diffrn_reflns_theta_max 27.13
_diffrn_reflns_theta_min 2.57
_exptl_absorpt_coefficient_mu 0.087
_exptl_absorpt_correction_T_max 0.9870
_exptl_absorpt_correction_T_min 0.1187
_exptl_absorpt_correction_type empirical
_exptl_absorpt_process_details 'program SADABS ver. 2.03(Sheldrick)'
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.151
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 192
_exptl_crystal_size_max 0.65
_exptl_crystal_size_mid 0.33
_exptl_crystal_size_min 0.15
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.942
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 76
_refine_ls_number_reflns 1043
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.942
_refine_ls_R_factor_all 0.1562
_refine_ls_R_factor_gt 0.0856
_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^)+(0.1377P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2040
_refine_ls_wR_factor_ref 0.2321
_reflns_number_gt 490
_reflns_number_total 1043
_reflns_threshold_expression >2sigma(I)
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 1100989
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 0.1304(6) 0.4741(6) 0.8484(5) 0.0914(13) Uani 1 1 d . . .
C2 C 0.2156(6) 0.6526(6) 0.9051(6) 0.1167(17) Uani 1 1 d . . .
H2A H 0.3183 0.6270 0.9855 0.175 Uiso 1 1 calc R . .
H2B H 0.1435 0.7304 0.9449 0.175 Uiso 1 1 calc R . .
H2C H 0.2410 0.7179 0.8222 0.175 Uiso 1 1 calc R . .
C1U C 0.3281(4) 0.2084(4) 0.8732(3) 0.0630(10) Uani 1 1 d . . .
H3 H 0.491(4) 0.023(5) 0.853(4) 0.063(10) Uiso 1 1 d . . .
H2 H 0.421(5) 0.124(5) 0.728(6) 0.093(13) Uiso 1 1 d . . .
H1 H 0.245(4) 0.355(4) 0.710(5) 0.068(9) Uiso 1 1 d . . .
H1A H 0.105(6) 0.419(7) 0.928(6) 0.126(16) Uiso 1 1 d . . .
H1B H 0.028(5) 0.532(6) 0.764(6) 0.123(15) Uiso 1 1 d . . .
N1 N 0.2296(4) 0.3434(4) 0.7899(3) 0.0773(10) Uani 1 1 d . . .
N2 N 0.4159(5) 0.1050(4) 0.8040(3) 0.0798(12) Uani 1 1 d . . .
O1 O 0.3348(3) 0.1798(3) 1.0105(2) 0.0789(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 0.122(4) 0.089(3) 0.080(3) 0.004(2) 0.056(3) 0.015(2)
C2 0.142(5) 0.088(3) 0.130(4) -0.008(2) 0.055(3) 0.003(3)
C1U 0.100(3) 0.0627(15) 0.0345(14) -0.0061(13) 0.0335(15) -0.0066(16)
N1 0.113(3) 0.0877(18) 0.0438(15) 0.0075(13) 0.0428(16) 0.0151(16)
N2 0.135(3) 0.0804(18) 0.0362(13) 0.0066(13) 0.0450(17) 0.0207(19)
O1 0.132(2) 0.0858(15) 0.0344(11) 0.0011(9) 0.0479(12) 0.0041(12)
|
1100990.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100990.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_1100990
loop_
_publ_author_name
'Kazuo Eda'
'Yuichi Iriki'
_journal_name_full 'Chemistry Letters'
_chemical_formula_moiety 'Mo36 O126, 4(C3 N2), 36(O)'
_chemical_formula_sum 'C12 Mo36 N8 O162'
_chemical_formula_weight 6302.04
_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 107.455(2)
_cell_angle_gamma 90.00
_cell_formula_units_Z 2
_cell_length_a 14.2137(15)
_cell_length_b 28.849(3)
_cell_length_c 19.059(2)
_cell_measurement_reflns_used 6880
_cell_measurement_temperature 193(2)
_cell_measurement_theta_max 27.361
_cell_measurement_theta_min 2.349
_cell_volume 7455.2(14)
_diffrn_ambient_temperature 193(2)
_diffrn_detector_area_resol_mean ?
_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 0.0556
_diffrn_reflns_av_sigmaI/netI 0.0720
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_k_max 37
_diffrn_reflns_limit_k_min -37
_diffrn_reflns_limit_l_max 24
_diffrn_reflns_limit_l_min -20
_diffrn_reflns_number 42627
_diffrn_reflns_theta_max 27.48
_diffrn_reflns_theta_min 1.66
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 3.046
_exptl_absorpt_correction_T_max 0.8626
_exptl_absorpt_correction_T_min 0.5721
_exptl_absorpt_correction_type empirical
_exptl_absorpt_process_details 'program SADABS ver. 2.03(Sheldrick)'
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 2.807
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description ?
_exptl_crystal_F_000 5872
_exptl_crystal_size_max 0.12
_exptl_crystal_size_mid 0.10
_exptl_crystal_size_min 0.05
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.062
_refine_ls_hydrogen_treatment undef
_refine_ls_matrix_type full
_refine_ls_number_parameters 982
_refine_ls_number_reflns 15490
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.062
_refine_ls_R_factor_all 0.0830
_refine_ls_R_factor_gt 0.0509
_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^)+(0.0609P)^2^+60.8314P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1176
_refine_ls_wR_factor_ref 0.1358
_reflns_number_gt 10968
_reflns_number_total 15490
_reflns_threshold_expression >2sigma(I)
_cod_duplicate_entry 8000014
_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 'P 21/n'
_cod_database_code 1100990
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
Mo11 Mo 0.57169(6) 0.13343(3) 0.87936(4) 0.01085(17) Uani 1 1 d . . .
Mo12 Mo 0.32922(6) 0.09448(3) 0.71955(4) 0.01054(17) Uani 1 1 d . . .
Mo13 Mo 0.38209(6) -0.02982(3) 0.67189(4) 0.01143(17) Uani 1 1 d . . .
Mo14 Mo 0.61392(6) -0.07676(3) 0.80855(4) 0.01176(18) Uani 1 1 d . . .
Mo15 Mo 0.75308(6) 0.02885(3) 0.91746(4) 0.01241(18) Uani 1 1 d . . .
Mo16 Mo 0.51335(6) 0.02799(3) 0.81791(4) 0.01042(17) Uani 1 1 d . . .
Mo17 Mo 0.84437(6) 0.14170(3) 1.00535(4) 0.01422(18) Uani 1 1 d . . .
Mo18 Mo 0.16357(6) 0.02691(3) 0.54719(4) 0.01247(18) Uani 1 1 d . . .
Mo21 Mo 0.60694(6) 0.21635(3) 0.77384(4) 0.01047(17) Uani 1 1 d . . .
Mo22 Mo 0.36492(6) 0.17639(3) 0.61374(4) 0.01046(17) Uani 1 1 d . . .
Mo23 Mo 0.45779(6) 0.14096(3) 0.45089(4) 0.01119(17) Uani 1 1 d . . .
Mo24 Mo 0.72701(6) 0.17230(3) 0.49204(4) 0.01290(18) Uani 1 1 d . . .
Mo25 Mo 0.82745(6) 0.20411(3) 0.69302(4) 0.01275(18) Uani 1 1 d . . .
Mo26 Mo 0.58504(6) 0.19848(3) 0.59970(4) 0.01028(17) Uani 1 1 d . . .
Mo27 Mo 0.88370(6) 0.22515(3) 0.89393(4) 0.01181(18) Uani 1 1 d . . .
Mo28 Mo 0.19781(6) 0.11405(3) 0.43987(4) 0.01259(18) Uani 1 1 d . . .
Mo31 Mo 0.56309(6) 0.10568(3) 0.70078(4) 0.00968(17) Uani 1 1 d . . .
Mo41 Mo 0.57646(6) 0.15993(3) 0.29482(4) 0.01208(18) Uani 1 1 d . . .
O101 O 0.4772(5) 0.0970(2) 0.7892(3) 0.0138(14) Uani 1 1 d . . .
O201 O 0.5136(5) 0.1839(2) 0.6770(3) 0.0124(14) Uani 1 1 d . . .
O102 O 0.3883(5) 0.0312(2) 0.7322(3) 0.0123(14) Uani 1 1 d . . .
O202 O 0.4496(5) 0.1717(2) 0.5496(3) 0.0139(14) Uani 1 1 d . . .
O103 O 0.4894(5) -0.0335(2) 0.7703(3) 0.0130(14) Uani 1 1 d . . .
O203 O 0.5811(4) 0.1781(2) 0.4998(3) 0.0108(13) Uani 1 1 d . . .
O104 O 0.6357(4) -0.0108(2) 0.8561(3) 0.0112(13) Uani 1 1 d . . .
O204 O 0.7232(5) 0.2004(2) 0.5919(3) 0.0139(14) Uani 1 1 d . . .
O105 O 0.6186(5) 0.0690(2) 0.8803(3) 0.0119(14) Uani 1 1 d . . .
O205 O 0.6786(5) 0.2099(2) 0.7003(3) 0.0134(14) Uani 1 1 d . . .
O106 O 0.6832(5) 0.1496(2) 0.9407(3) 0.0144(14) Uani 1 1 d . . .
O206 O 0.7162(5) 0.2285(2) 0.8426(3) 0.0148(14) Uani 1 1 d . . .
O107 O 0.8052(5) 0.0789(2) 0.9792(3) 0.0172(15) Uani 1 1 d . . .
O207 O 0.8657(5) 0.2244(2) 0.7909(3) 0.0176(15) Uani 1 1 d . . .
O108 O 0.2331(5) 0.0756(2) 0.6439(3) 0.0143(14) Uani 1 1 d . . .
O208 O 0.2672(5) 0.1528(2) 0.5454(3) 0.0152(14) Uani 1 1 d . . .
O109 O 0.2591(5) -0.0118(2) 0.6147(3) 0.0156(14) Uani 1 1 d . . .
O209 O 0.3230(5) 0.1319(2) 0.4277(3) 0.0174(15) Uani 1 1 d . . .
O111 O 0.4939(5) 0.1300(2) 0.9303(4) 0.0175(15) Uani 1 1 d . . .
O211 O 0.5486(5) 0.2683(2) 0.7510(4) 0.0190(15) Uani 1 1 d . . .
O012 O 0.6387(5) 0.1385(2) 0.7839(4) 0.0146(14) Uani 1 1 d . . .
O013 O 0.5287(5) 0.1906(2) 0.8303(3) 0.0160(15) Uani 1 1 d . . .
O121 O 0.2803(5) 0.0967(2) 0.7897(4) 0.0190(15) Uani 1 1 d . . .
O221 O 0.3421(5) 0.2334(2) 0.6120(3) 0.0147(14) Uani 1 1 d . . .
O022 O 0.4286(5) 0.1030(2) 0.6460(3) 0.0123(14) Uani 1 1 d . . .
O023 O 0.3320(5) 0.1593(2) 0.7000(3) 0.0149(14) Uani 1 1 d . . .
O131 O 0.2827(5) -0.0482(3) 0.7542(4) 0.0222(16) Uani 1 1 d . . .
O132 O 0.4518(5) -0.0130(3) 0.6199(4) 0.0204(16) Uani 1 1 d . . .
O232 O 0.5001(5) 0.0885(2) 0.4849(4) 0.0207(16) Uani 1 1 d . . .
O133 O 0.3814(5) -0.0895(2) 0.6643(4) 0.0196(16) Uani 1 1 d . . .
O233 O 0.4814(5) 0.1438(2) 0.3677(3) 0.0158(14) Uani 1 1 d . . .
O141 O 0.5454(6) -0.0884(3) 0.9050(4) 0.0237(17) Uani 1 1 d . . .
O241 O 0.6882(5) 0.2523(2) 0.4653(4) 0.0187(15) Uani 1 1 d . . .
O142 O 0.6566(6) -0.0669(2) 0.7370(4) 0.0238(17) Uani 1 1 d . . .
O242 O 0.7394(6) 0.1157(3) 0.5183(4) 0.0256(17) Uani 1 1 d . . .
O143 O 0.7153(5) -0.0989(2) 0.8729(4) 0.0219(16) Uani 1 1 d . . .
O243 O 0.8471(5) 0.1891(2) 0.5065(3) 0.0183(15) Uani 1 1 d . . .
O144 O 0.5334(5) -0.1279(2) 0.7732(3) 0.0161(15) Uani 1 1 d . . .
O244 O 0.6738(5) 0.1704(2) 0.3916(3) 0.0147(14) Uani 1 1 d . . .
O151 O 0.6751(5) 0.0146(3) 1.0054(4) 0.0233(17) Uani 1 1 d . . .
O251 O 0.7903(6) 0.2839(2) 0.6711(4) 0.0253(17) Uani 1 1 d . . .
O152 O 0.7926(5) 0.0429(2) 0.8448(4) 0.0191(15) Uani 1 1 d . . .
O252 O 0.8367(6) 0.1469(3) 0.7056(4) 0.0264(18) Uani 1 1 d . . .
O153 O 0.8255(5) -0.0170(2) 0.9557(4) 0.0203(16) Uani 1 1 d . . .
O253 O 0.9240(6) 0.2167(3) 0.6616(4) 0.0290(19) Uani 1 1 d . . .
O161 O 0.4565(5) 0.0207(2) 0.8808(3) 0.0166(15) Uani 1 1 d . . .
O261 O 0.5518(5) 0.2534(2) 0.5831(3) 0.0172(15) Uani 1 1 d . . .
O162 O 0.5899(5) 0.0481(2) 0.7261(3) 0.0130(14) Uani 1 1 d . . .
O262 O 0.6197(5) 0.1195(2) 0.6356(3) 0.0125(14) Uani 1 1 d . . .
O171 O 0.8154(6) 0.1477(3) 1.0850(4) 0.0285(18) Uani 1 1 d . . .
O271 O 0.8930(5) 0.2832(2) 0.9123(4) 0.0179(15) Uani 1 1 d . . .
O072 O 0.8445(5) 0.1442(2) 0.8770(3) 0.0127(14) Uani 1 1 d . . .
O173 O 0.9686(5) 0.1352(2) 1.0325(4) 0.0256(17) Uani 1 1 d . . .
O273 O 1.0019(5) 0.2065(2) 0.9220(3) 0.0193(16) Uani 1 1 d . . .
O074 O 0.8397(5) 0.2053(2) 0.9736(4) 0.0181(15) Uani 1 1 d . . .
O181 O 0.0631(5) 0.0173(2) 0.5755(4) 0.0227(16) Uani 1 1 d . . .
O281 O 0.1253(5) 0.1604(2) 0.4049(4) 0.0213(16) Uani 1 1 d . . .
O082 O 0.3084(5) 0.0557(2) 0.5185(3) 0.0126(14) Uani 1 1 d . . .
O183 O 0.1491(5) -0.0072(2) 0.4725(4) 0.0219(16) Uani 1 1 d . . .
O283 O 0.1701(5) 0.0749(2) 0.3708(4) 0.0214(16) Uani 1 1 d . . .
O084 O 0.1281(5) 0.0864(2) 0.5009(3) 0.0143(14) Uani 1 1 d . . .
O411 O 0.5338(6) 0.2152(2) 0.2829(4) 0.0250(17) Uani 1 1 d . . .
O413 O 0.6541(6) 0.1579(2) 0.2436(4) 0.0237(17) Uani 1 1 d . . .
N100 N 0.7789(7) 0.0003(3) 0.7076(5) 0.022(2) Uani 1 1 d . . .
C101 C 0.8274(8) 0.0431(4) 0.6893(6) 0.024(2) Uani 1 1 d . . .
C102 C 0.9370(8) 0.0325(4) 0.6995(6) 0.025(2) Uani 1 1 d . . .
C103 C 0.9919(9) 0.0746(4) 0.6881(6) 0.028(3) Uani 1 1 d . . .
N104 N 0.9496(7) 0.0944(3) 0.6111(5) 0.024(2) Uani 1 1 d . . .
N200 N 0.3245(8) 0.3005(3) 0.7177(5) 0.030(2) Uani 1 1 d . . .
C201 C 0.3108(9) 0.2615(4) 0.7695(6) 0.030(3) Uani 1 1 d . . .
C202 C 0.3774(9) 0.2710(4) 0.8457(6) 0.027(3) Uani 1 1 d . . .
C203 C 0.3672(9) 0.2291(4) 0.8914(7) 0.031(3) Uani 1 1 d . . .
N204 N 0.4399(7) 0.2349(4) 0.9670(5) 0.035(3) Uani 1 1 d . . .
O01W O 0.6471(6) 0.2506(3) 0.9772(4) 0.0275(18) Uani 1 1 d . . .
O02W O 0.6182(6) 0.0051(3) 0.5578(4) 0.0263(17) Uani 1 1 d . . .
O03W O 0.5467(6) 0.8105(3) 0.9035(4) 0.034(2) Uani 1 1 d . . .
O04W O 0.3499(6) 0.9168(3) 0.8980(4) 0.0278(18) Uani 1 1 d . . .
O05W O 0.9832(6) 0.0975(3) 0.8582(4) 0.0305(18) Uani 1 1 d . . .
O06W O 0.3276(5) 0.0768(3) 0.9556(4) 0.0231(17) Uani 1 1 d . . .
O07W O 0.9496(6) 0.9923(3) 0.1043(4) 0.040(2) Uani 1 1 d . . .
O08W O 0.6687(6) 0.3321(3) 0.5484(4) 0.0267(18) Uani 1 1 d . . .
O09W O 0.1360(7) 0.2599(4) 0.6203(5) 0.053(3) Uani 1 1 d . . .
O10W O 0.6041(6) 0.4481(3) 0.6647(5) 0.035(2) Uani 1 1 d . . .
O11W O 0.1697(6) 0.1354(3) 0.9056(4) 0.0332(19) Uani 1 1 d . . .
O12W O 0.2404(7) 0.1633(3) 0.2729(4) 0.037(2) Uani 1 1 d . . .
O13W O 0.1836(7) 0.0137(3) 0.8114(5) 0.043(2) Uani 1 1 d . . .
O14W O 0.1227(7) 0.1913(3) 0.7835(5) 0.049(2) Uani 1 1 d . . .
O15W O 0.1230(7) 0.8889(3) 0.7107(5) 0.046(2) Uani 1 1 d . . .
O16W O 0.5268(7) 0.3695(3) 0.7092(5) 0.051(3) Uani 1 1 d . . .
O17W O 0.9235(8) 0.1049(4) 0.4392(6) 0.072(4) Uani 1 1 d . . .
O18W O 0.0893(8) 0.1635(3) 0.6166(6) 0.058(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
Mo11 0.0129(4) 0.0066(4) 0.0122(4) -0.0005(3) 0.0023(3) -0.0002(3)
Mo12 0.0113(4) 0.0070(4) 0.0126(4) 0.0003(3) 0.0026(3) 0.0006(3)
Mo13 0.0130(4) 0.0065(4) 0.0126(4) -0.0007(3) 0.0006(3) 0.0007(3)
Mo14 0.0125(4) 0.0061(4) 0.0150(4) -0.0002(3) 0.0015(3) 0.0002(3)
Mo15 0.0131(4) 0.0081(4) 0.0136(4) -0.0007(3) 0.0003(3) -0.0003(3)
Mo16 0.0110(4) 0.0064(4) 0.0119(4) -0.0001(3) 0.0004(3) 0.0002(3)
Mo17 0.0177(5) 0.0093(4) 0.0123(4) -0.0005(3) -0.0005(3) -0.0031(3)
Mo18 0.0101(4) 0.0105(4) 0.0145(4) 0.0005(3) 0.0003(3) -0.0002(3)
Mo21 0.0124(4) 0.0069(4) 0.0114(4) -0.0009(3) 0.0024(3) -0.0013(3)
Mo22 0.0108(4) 0.0084(4) 0.0114(4) 0.0003(3) 0.0022(3) 0.0012(3)
Mo23 0.0123(4) 0.0091(4) 0.0118(4) -0.0021(3) 0.0031(3) -0.0007(3)
Mo24 0.0126(4) 0.0122(4) 0.0129(4) -0.0016(3) 0.0025(3) 0.0006(3)
Mo25 0.0120(4) 0.0122(4) 0.0124(4) -0.0017(3) 0.0011(3) -0.0004(3)
Mo26 0.0109(4) 0.0086(4) 0.0103(4) 0.0003(3) 0.0015(3) -0.0006(3)
Mo27 0.0129(4) 0.0091(4) 0.0118(4) -0.0014(3) 0.0012(3) -0.0026(3)
Mo28 0.0113(4) 0.0118(4) 0.0131(4) -0.0005(3) 0.0012(3) -0.0005(3)
Mo31 0.0106(4) 0.0061(4) 0.0110(4) -0.0005(3) 0.0012(3) -0.0001(3)
Mo41 0.0148(4) 0.0072(4) 0.0130(4) 0.0002(3) 0.0023(3) -0.0015(3)
O101 0.014(3) 0.007(3) 0.016(3) 0.001(3) -0.002(3) 0.000(3)
O201 0.014(3) 0.011(3) 0.010(3) -0.005(2) -0.001(3) -0.004(3)
O102 0.014(3) 0.009(3) 0.011(3) 0.000(2) 0.001(3) -0.003(3)
O202 0.008(3) 0.015(4) 0.014(3) 0.004(3) -0.003(3) 0.002(3)
O103 0.017(4) 0.004(3) 0.014(3) -0.001(2) 0.000(3) 0.001(3)
O203 0.006(3) 0.011(3) 0.014(3) -0.003(3) 0.002(3) 0.001(3)
O104 0.008(3) 0.003(3) 0.018(3) 0.000(2) -0.003(3) 0.003(3)
O204 0.012(3) 0.015(4) 0.014(3) 0.000(3) 0.003(3) -0.002(3)
O105 0.017(4) 0.004(3) 0.012(3) 0.001(2) 0.000(3) -0.001(3)
O205 0.009(3) 0.012(3) 0.018(3) 0.002(3) 0.004(3) -0.002(3)
O106 0.014(3) 0.008(3) 0.018(3) -0.003(3) 0.000(3) 0.000(3)
O206 0.014(3) 0.018(4) 0.013(3) 0.000(3) 0.004(3) 0.001(3)
O107 0.018(4) 0.015(4) 0.015(3) 0.001(3) 0.000(3) -0.001(3)
O207 0.016(4) 0.020(4) 0.015(3) -0.006(3) 0.002(3) -0.005(3)
O108 0.018(4) 0.003(3) 0.021(3) 0.003(3) 0.006(3) 0.001(3)
O208 0.015(4) 0.013(4) 0.018(3) -0.002(3) 0.006(3) 0.000(3)
O109 0.015(4) 0.007(3) 0.020(3) 0.000(3) -0.002(3) 0.002(3)
O209 0.016(4) 0.022(4) 0.014(3) 0.003(3) 0.003(3) -0.001(3)
O111 0.025(4) 0.003(3) 0.021(4) -0.001(3) 0.002(3) 0.004(3)
O211 0.024(4) 0.011(4) 0.022(4) 0.007(3) 0.008(3) 0.001(3)
O012 0.018(4) 0.006(3) 0.023(4) 0.003(3) 0.010(3) 0.001(3)
O013 0.018(4) 0.013(4) 0.017(3) -0.005(3) 0.006(3) -0.002(3)
O121 0.017(4) 0.012(4) 0.026(4) 0.002(3) 0.002(3) 0.004(3)
O221 0.011(3) 0.012(4) 0.022(4) 0.003(3) 0.007(3) 0.004(3)
O022 0.015(3) 0.006(3) 0.015(3) 0.000(2) 0.002(3) 0.002(3)
O023 0.015(4) 0.011(3) 0.017(3) -0.005(3) 0.002(3) 0.005(3)
O131 0.023(4) 0.025(4) 0.019(4) 0.003(3) 0.005(3) 0.000(3)
O132 0.016(4) 0.026(4) 0.017(3) -0.005(3) 0.003(3) -0.002(3)
O232 0.018(4) 0.017(4) 0.024(4) 0.002(3) 0.002(3) 0.005(3)
O133 0.018(4) 0.019(4) 0.018(4) -0.001(3) -0.001(3) 0.000(3)
O233 0.013(3) 0.016(4) 0.019(3) -0.003(3) 0.007(3) -0.002(3)
O141 0.030(4) 0.023(4) 0.021(4) -0.005(3) 0.010(3) -0.005(3)
O241 0.018(4) 0.015(4) 0.022(4) 0.007(3) 0.004(3) 0.001(3)
O142 0.031(4) 0.013(4) 0.030(4) -0.001(3) 0.013(3) 0.000(3)
O242 0.029(4) 0.021(4) 0.024(4) -0.001(3) 0.004(3) 0.004(3)
O143 0.019(4) 0.015(4) 0.026(4) 0.000(3) -0.001(3) 0.002(3)
O243 0.014(4) 0.023(4) 0.016(3) -0.005(3) 0.002(3) 0.003(3)
O144 0.025(4) 0.008(3) 0.014(3) -0.002(3) 0.004(3) -0.002(3)
O244 0.019(4) 0.008(3) 0.017(3) -0.004(3) 0.006(3) -0.001(3)
O151 0.029(4) 0.022(4) 0.020(4) 0.003(3) 0.009(3) 0.002(3)
O251 0.035(5) 0.013(4) 0.028(4) 0.003(3) 0.008(3) -0.001(3)
O152 0.013(4) 0.022(4) 0.022(4) -0.008(3) 0.005(3) -0.003(3)
O252 0.029(4) 0.017(4) 0.029(4) -0.003(3) 0.003(3) 0.003(3)
O153 0.023(4) 0.007(3) 0.025(4) -0.002(3) -0.001(3) 0.001(3)
O253 0.024(4) 0.046(5) 0.016(4) -0.001(3) 0.005(3) 0.000(4)
O161 0.014(4) 0.011(3) 0.019(3) -0.005(3) -0.004(3) 0.001(3)
O261 0.021(4) 0.015(4) 0.016(3) 0.003(3) 0.005(3) -0.003(3)
O162 0.016(4) 0.006(3) 0.015(3) -0.003(3) 0.003(3) 0.000(3)
O262 0.009(3) 0.010(3) 0.015(3) -0.008(3) -0.001(3) 0.000(3)
O171 0.045(5) 0.017(4) 0.024(4) -0.001(3) 0.012(4) -0.005(4)
O271 0.023(4) 0.014(4) 0.017(3) -0.001(3) 0.006(3) -0.003(3)
O072 0.019(4) 0.002(3) 0.019(3) -0.003(2) 0.008(3) -0.004(3)
O173 0.023(4) 0.018(4) 0.027(4) 0.001(3) -0.005(3) 0.000(3)
O273 0.017(4) 0.018(4) 0.016(3) -0.003(3) -0.006(3) -0.002(3)
O074 0.016(4) 0.019(4) 0.018(3) -0.009(3) 0.004(3) -0.001(3)
O181 0.027(4) 0.018(4) 0.025(4) 0.003(3) 0.011(3) 0.007(3)
O281 0.030(4) 0.016(4) 0.017(4) 0.000(3) 0.006(3) 0.005(3)
O082 0.011(3) 0.011(3) 0.013(3) 0.004(3) -0.002(3) -0.001(3)
O183 0.021(4) 0.018(4) 0.022(4) -0.002(3) -0.001(3) -0.001(3)
O283 0.025(4) 0.013(4) 0.025(4) -0.006(3) 0.005(3) -0.005(3)
O084 0.008(3) 0.020(4) 0.015(3) -0.002(3) 0.004(3) 0.001(3)
O411 0.030(4) 0.011(4) 0.031(4) -0.003(3) 0.004(3) -0.008(3)
O413 0.036(5) 0.022(4) 0.011(3) -0.003(3) 0.003(3) -0.008(3)
N100 0.022(5) 0.008(4) 0.038(5) -0.009(4) 0.011(4) -0.012(4)
C101 0.024(6) 0.015(5) 0.037(6) 0.005(5) 0.016(5) 0.003(5)
C102 0.029(6) 0.021(6) 0.022(5) -0.010(4) 0.002(5) -0.006(5)
C103 0.029(6) 0.028(7) 0.027(6) -0.009(5) 0.010(5) -0.011(5)
N104 0.020(5) 0.024(5) 0.030(5) 0.000(4) 0.009(4) -0.003(4)
N200 0.045(6) 0.027(5) 0.024(5) 0.001(4) 0.016(5) 0.010(5)
C201 0.039(7) 0.028(7) 0.020(6) 0.004(5) 0.003(5) 0.001(5)
C202 0.035(7) 0.018(6) 0.029(6) 0.002(5) 0.015(5) 0.004(5)
C203 0.025(6) 0.033(7) 0.039(7) 0.008(5) 0.016(5) 0.008(5)
N204 0.034(6) 0.040(6) 0.037(6) 0.022(5) 0.019(5) 0.021(5)
O01W 0.032(5) 0.025(4) 0.029(4) 0.001(3) 0.014(4) -0.007(4)
O02W 0.028(4) 0.024(4) 0.029(4) -0.011(3) 0.011(3) -0.002(3)
O03W 0.047(5) 0.026(5) 0.030(4) 0.007(3) 0.014(4) 0.003(4)
O04W 0.035(5) 0.024(4) 0.028(4) -0.001(3) 0.015(4) 0.004(4)
O05W 0.027(4) 0.024(4) 0.041(5) -0.004(4) 0.011(4) -0.002(4)
O06W 0.030(4) 0.024(4) 0.018(4) 0.004(3) 0.011(3) -0.003(3)
O07W 0.037(5) 0.044(6) 0.033(5) 0.007(4) 0.004(4) 0.001(4)
O08W 0.028(4) 0.023(4) 0.028(4) -0.004(3) 0.006(3) -0.001(3)
O09W 0.050(6) 0.064(7) 0.043(6) -0.008(5) 0.012(5) 0.001(5)
O10W 0.033(5) 0.026(5) 0.049(5) -0.002(4) 0.017(4) -0.002(4)
O11W 0.035(5) 0.033(5) 0.032(4) 0.003(4) 0.010(4) 0.008(4)
O12W 0.047(6) 0.036(5) 0.030(4) 0.008(4) 0.013(4) 0.003(4)
O13W 0.047(6) 0.030(5) 0.059(6) -0.004(4) 0.026(5) -0.007(4)
O14W 0.060(7) 0.029(5) 0.050(6) 0.011(4) 0.006(5) 0.002(5)
O15W 0.041(6) 0.027(5) 0.066(6) 0.001(4) 0.011(5) 0.001(4)
O16W 0.060(7) 0.029(5) 0.055(6) 0.012(4) 0.003(5) -0.003(5)
O17W 0.040(6) 0.110(10) 0.068(7) 0.043(7) 0.021(5) 0.024(6)
O18W 0.050(6) 0.042(6) 0.090(8) 0.005(5) 0.033(6) -0.002(5)
|
1100991.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100991.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_1100991
loop_
_publ_author_name
'Eda, Kazuo'
'Okazaki, Tadashi'
'Yamamura, Kimiaki'
'Hashimoto, Masao'
_publ_section_title
;
Three-dimensional supramolecular assembly having infinite two-dimensional
interlocking networks built up only from simple and non-rigid organic
molecules via hydrogen bonds. Crystal structures of \a,\w-diureidoalkanes
H~2~N(CO)NH--(CH~2~)n--NH(CO)NH~2~ with n=4 and 5
;
_journal_issue 1-3
_journal_name_full 'Journal of Molecular Structure'
_journal_page_first 93
_journal_page_last 97
_journal_paper_doi 10.1016/j.molstruc.2005.05.042
_journal_volume 752
_journal_year 2005
_chemical_formula_moiety 'C6 H14 N4 O2'
_chemical_formula_sum 'C6 H14 N4 O2'
_chemical_formula_weight 174.21
_chemical_melting_point 496
_chemical_name_common 1,4-diureidoalkane
_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
_cell_angle_alpha 90.00
_cell_angle_beta 103.348(4)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 13.092(3)
_cell_length_b 7.2470(18)
_cell_length_c 9.288(2)
_cell_measurement_reflns_used 1053
_cell_measurement_temperature 297(2)
_cell_measurement_theta_max 26.495
_cell_measurement_theta_min 3.199
_cell_volume 857.4(4)
_diffrn_ambient_temperature 297(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 0.0290
_diffrn_reflns_av_sigmaI/netI 0.0410
_diffrn_reflns_limit_h_max 16
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_k_min -5
_diffrn_reflns_limit_l_max 11
_diffrn_reflns_limit_l_min -11
_diffrn_reflns_number 2344
_diffrn_reflns_theta_max 27.43
_diffrn_reflns_theta_min 3.20
_exptl_absorpt_coefficient_mu 0.103
_exptl_absorpt_correction_T_max 0.9918
_exptl_absorpt_correction_T_min 0.8290
_exptl_absorpt_correction_type empirical
_exptl_absorpt_process_details 'program SADABS ver. 2.03(Sheldrick)'
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.350
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 376
_exptl_crystal_size_max 0.26
_exptl_crystal_size_mid 0.20
_exptl_crystal_size_min 0.08
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.136
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 83
_refine_ls_number_reflns 895
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.136
_refine_ls_R_factor_all 0.0620
_refine_ls_R_factor_gt 0.0448
_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^)+(0.0431P)^2^+0.4158P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1072
_refine_ls_wR_factor_ref 0.1168
_reflns_number_gt 651
_reflns_number_total 895
_reflns_threshold_expression >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_chemical_melting_point' value '496 K' was changed to '496' - the
value should be numeric and without a unit designator.
Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana
;
_cod_original_sg_symbol_H-M 'C 2/c'
_cod_database_code 1100991
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
O1 O 0.32707(11) 1.04200(18) 0.58755(13) 0.0463(4) Uani 1 1 d . . .
N2 N 0.38200(13) 0.8689(2) 0.41754(17) 0.0397(4) Uani 1 1 d . . .
C1U C 0.33588(14) 1.0199(2) 0.45769(19) 0.0341(4) Uani 1 1 d . . .
N1 N 0.29944(15) 1.1443(2) 0.35197(18) 0.0477(5) Uani 1 1 d . . .
C1 C 0.42364(17) 0.7223(3) 0.5205(2) 0.0386(5) Uani 1 1 d . . .
C2 C 0.47763(17) 0.5782(3) 0.4479(2) 0.0390(5) Uani 1 1 d . . .
H22 H 0.4310(17) 0.538(3) 0.364(2) 0.051(6) Uiso 1 1 d . . .
H11 H 0.3697(16) 0.667(3) 0.560(2) 0.047(6) Uiso 1 1 d . . .
H21 H 0.5354(16) 0.637(3) 0.414(2) 0.049(6) Uiso 1 1 d . . .
H12 H 0.4710(16) 0.774(3) 0.606(2) 0.049(6) Uiso 1 1 d . . .
H2 H 0.3008(17) 1.120(3) 0.260(3) 0.055(6) Uiso 1 1 d . . .
H1 H 0.2661(18) 1.245(4) 0.374(2) 0.056(6) Uiso 1 1 d . . .
H3 H 0.3908(17) 0.861(3) 0.327(3) 0.057(7) 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
O1 0.0744(10) 0.0388(8) 0.0299(7) 0.0025(6) 0.0207(6) 0.0158(7)
N2 0.0568(10) 0.0343(9) 0.0299(8) 0.0006(7) 0.0137(7) 0.0140(7)
C1U 0.0415(10) 0.0302(10) 0.0311(9) -0.0002(7) 0.0095(7) 0.0018(8)
N1 0.0743(13) 0.0401(10) 0.0304(9) 0.0036(7) 0.0153(8) 0.0230(9)
C1 0.0493(12) 0.0327(10) 0.0353(10) 0.0024(8) 0.0131(9) 0.0080(9)
C2 0.0505(12) 0.0314(10) 0.0354(10) -0.0006(8) 0.0108(9) 0.0067(9)
|
1100992.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100992.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_1100992
loop_
_publ_author_name
'Hashimoto, Masao'
'Tajima, Fukue'
'Eda, Kazuo'
'Yamamura, Kimiaki'
'Okazaki, Tadashi'
_publ_section_title
;
Exploration of plastic-like phases in alkylurea systems.
A thermal and X-ray study
;
_journal_issue 1-3
_journal_name_full 'Journal of Molecular Structure'
_journal_page_first 23
_journal_page_last 33
_journal_paper_doi 10.1016/j.molstruc.2004.08.008
_journal_volume 734
_journal_year 2005
_chemical_formula_moiety 'C5 H12 N2 O'
_chemical_formula_sum 'C5 H12 N2 O'
_chemical_formula_weight 116.17
_chemical_melting_point 365.4
_chemical_name_common n-butylurea
_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 94.627(5)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 4.6629(15)
_cell_length_b 5.7364(19)
_cell_length_c 25.863(8)
_cell_measurement_reflns_used 734
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 24.741
_cell_measurement_theta_min 3.161
_cell_volume 689.5(4)
_diffrn_ambient_temperature 293(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 0.0325
_diffrn_reflns_av_sigmaI/netI 0.0391
_diffrn_reflns_limit_h_max 6
_diffrn_reflns_limit_h_min -5
_diffrn_reflns_limit_k_max 6
_diffrn_reflns_limit_k_min -7
_diffrn_reflns_limit_l_max 32
_diffrn_reflns_limit_l_min -32
_diffrn_reflns_number 3708
_diffrn_reflns_theta_max 27.38
_diffrn_reflns_theta_min 3.16
_exptl_absorpt_coefficient_mu 0.079
_exptl_absorpt_correction_T_max 0.9898
_exptl_absorpt_correction_T_min 0.6893
_exptl_absorpt_correction_type empirical
_exptl_absorpt_process_details 'program SADABS ver. 2.03(Sheldrick)'
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.119
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 256
_exptl_crystal_size_max 0.50
_exptl_crystal_size_mid 0.36
_exptl_crystal_size_min 0.13
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.988
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 121
_refine_ls_number_reflns 1396
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.988
_refine_ls_R_factor_all 0.0652
_refine_ls_R_factor_gt 0.0489
_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^)+(0.0786P)^2^+0.1031P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1320
_refine_ls_wR_factor_ref 0.1412
_reflns_number_gt 1050
_reflns_number_total 1396
_reflns_threshold_expression >2sigma(I)
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 1100992
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 0.6200(4) 0.6949(3) 0.13543(8) 0.0582(5) Uani 1 1 d . . .
C2 C 0.8139(4) 0.5436(3) 0.10599(8) 0.0551(5) Uani 1 1 d . . .
C3 C 0.6454(5) 0.3625(4) 0.07336(9) 0.0663(6) Uani 1 1 d . . .
C4 C 0.8312(7) 0.2065(5) 0.04329(11) 0.0849(7) Uani 1 1 d . . .
C1U C 0.6468(3) 1.0202(3) 0.19626(6) 0.0421(4) Uani 1 1 d . . .
H1 H 0.965(4) 0.875(3) 0.1665(7) 0.057(5) Uiso 1 1 d . . .
H2 H 1.005(5) 1.173(3) 0.2202(7) 0.061(5) Uiso 1 1 d . . .
H3 H 0.738(4) 1.274(3) 0.2446(7) 0.059(5) Uiso 1 1 d . . .
H1A H 0.470(6) 0.774(4) 0.1118(9) 0.089(7) Uiso 1 1 d . . .
H2A H 0.924(5) 0.637(4) 0.0837(9) 0.078(6) Uiso 1 1 d . . .
H3A H 0.527(5) 0.448(4) 0.0505(9) 0.086(7) Uiso 1 1 d . . .
H4A H 0.941(7) 0.292(5) 0.0184(11) 0.116(10) Uiso 1 1 d . . .
H2B H 0.959(5) 0.463(4) 0.1331(8) 0.081(6) Uiso 1 1 d . . .
H3B H 0.538(5) 0.274(4) 0.0973(9) 0.084(7) Uiso 1 1 d . . .
H4B H 0.719(6) 0.088(5) 0.0241(11) 0.113(9) Uiso 1 1 d . . .
H4C H 0.975(7) 0.121(5) 0.0648(11) 0.128(12) Uiso 1 1 d . . .
H1B H 0.505(5) 0.605(4) 0.1590(8) 0.073(6) Uiso 1 1 d . . .
N1 N 0.7803(3) 0.8697(3) 0.16634(5) 0.0510(4) Uani 1 1 d . . .
N2 N 0.8144(3) 1.1723(3) 0.22352(6) 0.0587(5) Uani 1 1 d . . .
O1 O 0.3821(2) 1.0165(2) 0.19826(4) 0.0544(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
C1 0.0368(9) 0.0642(11) 0.0734(12) -0.0119(9) 0.0026(8) -0.0042(8)
C2 0.0472(10) 0.0530(10) 0.0656(11) -0.0046(8) 0.0068(8) -0.0015(8)
C3 0.0626(13) 0.0637(12) 0.0718(13) -0.0083(10) -0.0002(10) -0.0045(10)
C4 0.0910(18) 0.0714(15) 0.0932(17) -0.0262(14) 0.0130(15) -0.0069(13)
C1U 0.0279(7) 0.0481(8) 0.0509(8) 0.0041(7) 0.0064(6) 0.0020(6)
N1 0.0240(7) 0.0617(9) 0.0675(9) -0.0130(7) 0.0051(6) -0.0010(6)
N2 0.0260(7) 0.0720(10) 0.0787(10) -0.0243(8) 0.0084(7) -0.0005(7)
O1 0.0242(6) 0.0632(8) 0.0768(8) -0.0038(6) 0.0103(5) 0.0006(5)
|