file_name stringlengths 11 11 | content stringlengths 1.16k 56.6M |
|---|---|
1501557.cif | #------------------------------------------------------------------------------
#$Date: 2020-10-02 18:11:04 +0300 (Fri, 02 Oct 2020) $
#$Revision: 256942 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/50/15/1501557.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_1501557
loop_
_publ_author_name
'Mohamed Osman Awaleh'
'Francois Brisse'
'Youssouf Djibril Soubaneh'
'Thierry Maris'
_publ_section_title
;
Influence of the counteranion on silver(I)-dithioether coordination
polymers
;
_journal_name_full Polyhedron
_journal_page_first 2966
_journal_page_last 2975
_journal_paper_doi 10.1016/j.poly.2010.08.013
_journal_volume 29
_journal_year 2010
_chemical_compound_source 'Synthesized by the authors. See text'
_chemical_formula_sum 'C19 H22 Ag2 O4 S2'
_chemical_formula_weight 594.23
_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 94.775(2)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 25.7160(9)
_cell_length_b 7.8986(3)
_cell_length_c 9.9444(4)
_cell_measurement_reflns_used 7447
_cell_measurement_temperature 220(2)
_cell_measurement_theta_max 71.98
_cell_measurement_theta_min 3.45
_cell_volume 2012.90(13)
_computing_cell_refinement 'SMART (Bruker, 1999)'
_computing_data_collection 'SMART (Bruker, 1999)'
_computing_data_reduction 'SAINT (Bruker, 1999)'
_computing_molecular_graphics 'SHELXTL (Bruker, 1997)'
_computing_publication_material 'UdMX (local program)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 220(2)
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type 'Bruker Smart 2000'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'X-ray Sealed Tube'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.065
_diffrn_reflns_av_sigmaI/netI 0.0442
_diffrn_reflns_limit_h_max 31
_diffrn_reflns_limit_h_min -31
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_k_min -9
_diffrn_reflns_limit_l_max 12
_diffrn_reflns_limit_l_min -11
_diffrn_reflns_number 25844
_diffrn_reflns_theta_full 72.02
_diffrn_reflns_theta_max 72.02
_diffrn_reflns_theta_min 3.45
_diffrn_standards_decay_% -0.31
_diffrn_standards_number 73
_exptl_absorpt_coefficient_mu 17.741
_exptl_absorpt_correction_T_max 0.2360
_exptl_absorpt_correction_T_min 0.1600
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Sadabs (Sheldrick,1996)'
_exptl_crystal_colour Colorless
_exptl_crystal_density_diffrn 1.961
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description platelet
_exptl_crystal_F_000 1176
_exptl_crystal_size_max 0.16
_exptl_crystal_size_mid 0.10
_exptl_crystal_size_min 0.06
_refine_diff_density_max 1.630
_refine_diff_density_min -2.442
_refine_diff_density_rms 0.255
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.078
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 124
_refine_ls_number_reflns 1936
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.078
_refine_ls_R_factor_all 0.0538
_refine_ls_R_factor_gt 0.0513
_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^)+(0.1017P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1270
_refine_ls_wR_factor_ref 0.1326
_reflns_number_gt 1757
_reflns_number_total 1936
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file deposit.cif
_cod_data_source_block ande65
_cod_depositor_comments
;
Updated values of the _geom_bond_atom_site_label_*,
_geom_angle_atom_site_label_* and _geom_torsion_atom_site_label
data items to establish relationships between loop packets from
different data loops.
Antanas Vaitkus,
2020-10-02
;
_cod_original_sg_symbol_H-M C2/c
_cod_database_code 1501557
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
Ag1 Ag 0.028963(10) 0.12029(4) 0.92347(3) 0.0270(2) Uani 1 1 d .
S1 S 0.07582(4) 0.35457(13) 1.05782(12) 0.0272(3) Uani 1 1 d .
O1 O 0.05330(11) 0.1199(3) 0.6816(3) 0.0269(7) Uani 1 1 d .
O2 O 0.08565(14) 0.1053(4) 0.4805(3) 0.0310(7) Uani 1 1 d .
C1 C 0.08914(16) 0.1409(4) 0.6035(4) 0.0213(8) Uani 1 1 d .
C2 C 0.14027(14) 0.2158(5) 0.6631(4) 0.0241(8) Uani 1 1 d .
C3 C 0.15311(15) 0.2145(6) 0.8015(5) 0.0335(10) Uani 1 1 d .
H3 H 0.1310 0.1607 0.8587 0.040 Uiso 1 1 calc R
C4 C 0.19874(17) 0.2927(7) 0.8560(5) 0.0420(12) Uani 1 1 d .
H4 H 0.2073 0.2914 0.9497 0.050 Uiso 1 1 calc R
C5 C 0.23135(18) 0.3723(5) 0.7718(6) 0.0385(12) Uani 1 1 d .
H5 H 0.2615 0.4285 0.8084 0.046 Uiso 1 1 calc R
C6 C 0.2194(2) 0.3688(6) 0.6335(6) 0.0404(13) Uani 1 1 d .
H6 H 0.2423 0.4180 0.5759 0.048 Uiso 1 1 calc R
C7 C 0.17384(18) 0.2933(6) 0.5799(5) 0.0343(10) Uani 1 1 d .
H7 H 0.1655 0.2944 0.4860 0.041 Uiso 1 1 calc R
C11 C 0.12419(17) 0.2578(6) 1.1760(5) 0.0364(10) Uani 1 1 d .
H11A H 0.1452 0.3454 1.2223 0.055 Uiso 1 1 calc R
H11B H 0.1464 0.1842 1.1278 0.055 Uiso 1 1 calc R
H11C H 0.1069 0.1920 1.2415 0.055 Uiso 1 1 calc R
C12 C 0.03545(17) 0.4576(5) 1.1745(4) 0.0302(9) Uani 1 1 d .
H12A H 0.0584 0.5192 1.2413 0.036 Uiso 1 1 calc R
H12B H 0.0136 0.5416 1.1241 0.036 Uiso 1 1 calc R
C13 C 0.0000 0.3433(7) 1.2500 0.0278(12) Uani 1 2 d S
H13A H -0.0209 0.2708 1.1863 0.033 Uiso 0.50 1 calc PR
H13B H 0.0209 0.2708 1.3137 0.033 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
Ag1 0.0199(3) 0.0291(3) 0.0311(3) 0.00350(9) -0.00295(17) 0.00086(9)
S1 0.0246(5) 0.0255(5) 0.0311(6) 0.0011(4) -0.0008(4) -0.0046(3)
O1 0.0139(14) 0.0319(17) 0.0341(19) -0.0011(10) -0.0022(13) -0.0011(9)
O2 0.0345(18) 0.0326(17) 0.0250(18) -0.0038(11) -0.0029(14) -0.0130(12)
C1 0.0175(19) 0.0172(17) 0.028(2) 0.0018(13) -0.0028(16) 0.0027(13)
C2 0.0183(17) 0.0181(17) 0.036(2) -0.0072(15) 0.0014(15) 0.0040(14)
C3 0.0188(19) 0.047(3) 0.035(2) 0.0002(19) 0.0025(16) -0.0020(18)
C4 0.021(2) 0.064(3) 0.039(3) -0.008(2) -0.0066(18) -0.002(2)
C5 0.016(2) 0.040(3) 0.057(4) -0.0082(19) -0.009(2) -0.0028(15)
C6 0.028(3) 0.045(3) 0.047(3) 0.0068(19) 0.000(2) -0.0086(18)
C7 0.032(2) 0.037(2) 0.033(2) 0.0003(18) -0.0021(18) -0.0065(19)
C11 0.027(2) 0.041(3) 0.040(3) 0.0028(19) -0.0057(19) -0.0061(18)
C12 0.038(2) 0.0160(18) 0.037(2) -0.0010(14) 0.0029(19) -0.0003(16)
C13 0.028(3) 0.020(2) 0.034(3) 0.000 0.000(3) 0.000
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag 0.1306 4.2820 '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
O1 Ag1 O2 2_556 6_556 130.18(11) y
O1 Ag1 S1 2_556 . 128.78(7) y
O2 Ag1 S1 6_556 . 99.73(9) y
O1 Ag1 O1 2_556 . 81.85(11) y
O2 Ag1 O1 6_556 . 91.78(10) y
S1 Ag1 O1 . . 110.96(7) y
O1 Ag1 Ag1 2_556 5_557 75.16(8) y
O2 Ag1 Ag1 6_556 5_557 73.31(9) y
S1 Ag1 Ag1 . 5_557 116.25(3) y
O1 Ag1 Ag1 . 5_557 132.13(6) y
C11 S1 C12 . . 100.0(2) y
C11 S1 Ag1 . . 107.82(16) y
C12 S1 Ag1 . . 113.18(14) y
C1 O1 Ag1 . 2_556 114.5(3) y
C1 O1 Ag1 . . 146.4(3) y
Ag1 O1 Ag1 2_556 . 98.15(11) y
C1 O2 Ag1 . 6 113.6(3) y
O2 C1 O1 . . 125.1(4) y
O2 C1 C2 . . 117.3(4) y
O1 C1 C2 . . 117.6(4) y
C7 C2 C3 . . 119.1(4) y
C7 C2 C1 . . 120.1(4) y
C3 C2 C1 . . 120.7(4) y
C2 C3 C4 . . 120.3(4) y
C2 C3 H3 . . 119.8 ?
C4 C3 H3 . . 119.8 ?
C5 C4 C3 . . 119.9(5) y
C5 C4 H4 . . 120.1 ?
C3 C4 H4 . . 120.1 ?
C6 C5 C4 . . 119.8(4) y
C6 C5 H5 . . 120.1 ?
C4 C5 H5 . . 120.1 ?
C7 C6 C5 . . 120.2(5) y
C7 C6 H6 . . 119.9 ?
C5 C6 H6 . . 119.9 ?
C6 C7 C2 . . 120.7(5) y
C6 C7 H7 . . 119.7 ?
C2 C7 H7 . . 119.7 ?
S1 C11 H11A . . 109.5 ?
S1 C11 H11B . . 109.5 ?
H11A C11 H11B . . 109.5 ?
S1 C11 H11C . . 109.5 ?
H11A C11 H11C . . 109.5 ?
H11B C11 H11C . . 109.5 ?
C13 C12 S1 . . 116.6(3) y
C13 C12 H12A . . 108.2 ?
S1 C12 H12A . . 108.2 ?
C13 C12 H12B . . 108.2 ?
S1 C12 H12B . . 108.2 ?
H12A C12 H12B . . 107.3 ?
C12 C13 C12 2_557 . 107.3(5) y
C12 C13 H13A 2_557 . 110.2 ?
C12 C13 H13A . . 110.2 ?
C12 C13 H13B 2_557 . 110.2 ?
C12 C13 H13B . . 110.2 ?
H13A C13 H13B . . 108.5 ?
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
Ag1 O1 2_556 2.280(3) y
Ag1 O2 6_556 2.342(3) y
Ag1 S1 . 2.5285(11) y
Ag1 O1 . 2.535(3) y
Ag1 Ag1 5_557 2.9196(6) y
S1 C11 . 1.808(5) y
S1 C12 . 1.813(4) y
O1 C1 . 1.264(5) y
O1 Ag1 2_556 2.280(3) y
O2 C1 . 1.251(6) y
O2 Ag1 6 2.342(3) y
C1 C2 . 1.517(5) y
C2 C7 . 1.387(6) y
C2 C3 . 1.389(6) y
C3 C4 . 1.395(6) y
C3 H3 . 0.94 ?
C4 C5 . 1.385(8) y
C4 H4 . 0.94 ?
C5 C6 . 1.384(8) y
C5 H5 . 0.94 ?
C6 C7 . 1.382(7) y
C6 H6 . 0.94 ?
C7 H7 . 0.94 ?
C11 H11A . 0.97 ?
C11 H11B . 0.97 ?
C11 H11C . 0.97 ?
C12 C13 . 1.524(5) y
C12 H12A . 0.98 ?
C12 H12B . 0.98 ?
C13 C12 2_557 1.524(5) y
C13 H13A . 0.98 ?
C13 H13B . 0.98 ?
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_4
_geom_torsion
_geom_torsion_publ_flag
O1 Ag1 S1 C11 2_556 . 154.06(19) y
O2 Ag1 S1 C11 6_556 . -13.74(19) y
O1 Ag1 S1 C11 . . -109.45(19) y
Ag1 Ag1 S1 C11 5_557 . 62.35(17) y
O1 Ag1 S1 C12 2_556 . 44.5(2) y
O2 Ag1 S1 C12 6_556 . -123.34(18) y
O1 Ag1 S1 C12 . . 140.95(17) y
Ag1 Ag1 S1 C12 5_557 . -47.24(16) y
O1 Ag1 O1 C1 2_556 . 166.3(4) y
O2 Ag1 O1 C1 6_556 . -63.3(4) y
S1 Ag1 O1 C1 . . 37.8(4) y
Ag1 Ag1 O1 C1 5_557 . -132.3(4) y
O1 Ag1 O1 Ag1 2_556 2_556 0.15(13) y
O2 Ag1 O1 Ag1 6_556 2_556 130.51(11) y
S1 Ag1 O1 Ag1 . 2_556 -128.36(7) y
Ag1 Ag1 O1 Ag1 5_557 2_556 61.57(11) y
Ag1 O2 C1 O1 6 . -29.7(5) y
Ag1 O2 C1 C2 6 . 150.7(3) y
Ag1 O1 C1 O2 2_556 . -25.2(5) y
Ag1 O1 C1 O2 . . 169.9(3) y
Ag1 O1 C1 C2 2_556 . 154.4(2) y
Ag1 O1 C1 C2 . . -10.5(6) y
O2 C1 C2 C7 . . 21.1(5) y
O1 C1 C2 C7 . . -158.5(4) y
O2 C1 C2 C3 . . -161.6(4) y
O1 C1 C2 C3 . . 18.7(5) y
C7 C2 C3 C4 . . 1.1(7) y
C1 C2 C3 C4 . . -176.1(4) y
C2 C3 C4 C5 . . 0.1(8) y
C3 C4 C5 C6 . . -2.2(8) y
C4 C5 C6 C7 . . 3.1(7) y
C5 C6 C7 C2 . . -1.9(7) y
C3 C2 C7 C6 . . -0.2(7) y
C1 C2 C7 C6 . . 177.0(4) y
C11 S1 C12 C13 . . -74.1(3) y
Ag1 S1 C12 C13 . . 40.3(3) y
S1 C12 C13 C12 . 2_557 -172.0(4) y
|
1501558.cif | #------------------------------------------------------------------------------
#$Date: 2020-10-02 18:11:04 +0300 (Fri, 02 Oct 2020) $
#$Revision: 256942 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/50/15/1501558.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_1501558
loop_
_publ_author_name
'Mohamed Osman Awaleh'
'Francois Brisse'
'Youssouf Djibril Soubaneh'
'Thierry Maris'
_publ_section_title
;
Influence of the counteranion on silver(I)-dithioether coordination
polymers
;
_journal_name_full Polyhedron
_journal_page_first 2966
_journal_page_last 2975
_journal_paper_doi 10.1016/j.poly.2010.08.013
_journal_volume 29
_journal_year 2010
_chemical_compound_source 'Synthesized by the authors. See text'
_chemical_formula_sum 'C7 H12 Ag F3 O2 S2'
_chemical_formula_weight 357.16
_space_group_IT_number 61
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall '-P 2ac 2ab'
_symmetry_space_group_name_H-M 'P b c a'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 8
_cell_length_a 7.6138(9)
_cell_length_b 16.0573(19)
_cell_length_c 19.894(2)
_cell_measurement_reflns_used 3498
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 57.47
_cell_measurement_theta_min 4.45
_cell_volume 2432.2(5)
_computing_cell_refinement 'SMART (Bruker, 2003)'
_computing_data_collection 'SMART (Bruker, 2003)'
_computing_data_reduction 'SAINT (Bruker, 2004)'
_computing_molecular_graphics 'SHELXTL (Bruker, 1997)'
_computing_publication_material 'UdMX (local program)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.907
_diffrn_measured_fraction_theta_max 0.907
_diffrn_measurement_device_type 'Bruker Smart 6000'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator 'Montel 200 optics'
_diffrn_radiation_source 'Rotating Anode'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.125
_diffrn_reflns_av_sigmaI/netI 0.1258
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_h_min -8
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_l_max 21
_diffrn_reflns_limit_l_min -24
_diffrn_reflns_number 33365
_diffrn_reflns_theta_full 68.78
_diffrn_reflns_theta_max 68.78
_diffrn_reflns_theta_min 4.44
_diffrn_standards_decay_% -3.35
_diffrn_standards_number 99
_exptl_absorpt_coefficient_mu 16.735
_exptl_absorpt_correction_T_max 0.3600
_exptl_absorpt_correction_T_min 0.2450
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Sadabs (Sheldrick,1996)'
_exptl_crystal_colour Colorless
_exptl_crystal_density_diffrn 1.951
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description needle-like
_exptl_crystal_F_000 1408
_exptl_crystal_size_max 0.12
_exptl_crystal_size_mid 0.08
_exptl_crystal_size_min 0.06
_refine_diff_density_max 1.227
_refine_diff_density_min -1.382
_refine_diff_density_rms 0.178
_refine_ls_extinction_coef 0.00067(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 0.923
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 149
_refine_ls_number_reflns 2042
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.923
_refine_ls_R_factor_all 0.1477
_refine_ls_R_factor_gt 0.0722
_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^)+(0.1139P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1666
_refine_ls_wR_factor_ref 0.2064
_reflns_number_gt 974
_reflns_number_total 2042
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file deposit.cif
_cod_data_source_block ande56
_cod_depositor_comments
;
Updated values of the _geom_bond_atom_site_label_*,
_geom_angle_atom_site_label_* and _geom_torsion_atom_site_label
data items to establish relationships between loop packets from
different data loops.
Antanas Vaitkus,
2020-10-02
;
_cod_original_sg_symbol_H-M Pbca
_cod_database_code 1501558
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
Ag1 Ag 0.10352(12) 0.81297(5) 0.47276(5) 0.0672(5) Uani 1 1 d . . .
S1 S 0.0881(4) 0.87774(19) 0.35797(15) 0.0661(9) Uani 1 1 d . . .
S2 S 0.2384(4) 1.17312(16) 0.49079(16) 0.0593(9) Uani 1 1 d . . .
O1 O 0.2553(11) 0.8870(6) 0.5602(5) 0.086(3) Uani 1 1 d . . .
O2 O 0.1002(15) 0.7968(7) 0.6200(6) 0.124(4) Uani 1 1 d . . .
C1 C 0.2131(18) 0.8548(9) 0.6108(8) 0.071(3) Uani 1 1 d . A .
C2 C 0.2691(18) 0.8927(10) 0.6771(7) 0.085(4) Uani 1 1 d . . .
C11 C 0.206(3) 0.8195(8) 0.2970(7) 0.107(5) Uani 1 1 d . . .
H11A H 0.2151 0.8517 0.2554 0.161 Uiso 1 1 calc R . .
H11B H 0.1447 0.7670 0.2881 0.161 Uiso 1 1 calc R . .
H11C H 0.3245 0.8075 0.3140 0.161 Uiso 1 1 calc R . .
C12 C 0.2179(16) 0.9714(7) 0.3612(6) 0.067(3) Uani 1 1 d . . .
H12A H 0.3440 0.9565 0.3611 0.080 Uiso 1 1 calc R . .
H12B H 0.1943 1.0052 0.3205 0.080 Uiso 1 1 calc R . .
C13 C 0.1778(13) 1.0229(6) 0.4232(5) 0.054(3) Uani 1 1 d . . .
H13A H 0.2205 0.9935 0.4638 0.065 Uiso 1 1 calc R . .
H13B H 0.0492 1.0305 0.4275 0.065 Uiso 1 1 calc R . .
C14 C 0.2679(14) 1.1083(7) 0.4176(5) 0.061(3) Uani 1 1 d . . .
H14A H 0.2207 1.1379 0.3778 0.073 Uiso 1 1 calc R . .
H14B H 0.3952 1.0997 0.4101 0.073 Uiso 1 1 calc R . .
C21 C 0.3665(16) 1.1169(8) 0.5528(7) 0.079(4) Uani 1 1 d . . .
H21A H 0.3199 1.0603 0.5576 0.119 Uiso 1 1 calc R . .
H21B H 0.3596 1.1458 0.5961 0.119 Uiso 1 1 calc R . .
H21C H 0.4893 1.1142 0.5382 0.119 Uiso 1 1 calc R . .
F1 F 0.396(4) 0.944(3) 0.6782(14) 0.077(3) Uiso 0.41(6) 1 d P A 1
F3 F 0.403(4) 0.824(4) 0.6977(15) 0.077(3) Uiso 0.31(4) 1 d P A 1
F4 F 0.133(3) 0.904(2) 0.7146(13) 0.077(3) Uiso 0.41(2) 1 d P A 1
F2 F 0.352(5) 0.971(2) 0.6684(11) 0.077(3) Uiso 0.50(6) 1 d P A 2
F5 F 0.119(3) 0.951(2) 0.7008(13) 0.077(3) Uiso 0.31(2) 1 d P A 2
F6 F 0.322(4) 0.8510(14) 0.7276(12) 0.077(3) Uiso 0.392(17) 1 d P A 2
F7 F 0.206(5) 0.8727(18) 0.7363(14) 0.077(3) Uiso 0.313(19) 1 d P A 3
F8 F 0.250(19) 0.977(6) 0.680(4) 0.077(3) Uiso 0.09(2) 1 d P A 3
F9 F 0.420(6) 0.862(6) 0.698(2) 0.077(3) Uiso 0.19(4) 1 d P A 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
Ag1 0.0682(8) 0.0665(8) 0.0669(8) 0.0037(4) -0.0029(4) -0.0004(4)
S1 0.069(2) 0.065(2) 0.064(2) 0.0016(16) 0.0016(15) -0.0077(15)
S2 0.0491(17) 0.061(2) 0.068(2) -0.0012(14) 0.0053(14) -0.0019(13)
O1 0.081(6) 0.109(7) 0.066(6) 0.011(6) 0.004(5) 0.000(5)
O2 0.139(11) 0.104(8) 0.130(10) -0.028(7) 0.007(7) -0.033(7)
C1 0.060(9) 0.077(10) 0.075(10) -0.005(9) -0.004(8) 0.006(7)
C2 0.061(10) 0.118(13) 0.077(10) 0.020(9) 0.018(8) -0.002(8)
C11 0.162(15) 0.079(10) 0.081(10) -0.017(8) 0.011(11) -0.010(10)
C12 0.074(8) 0.065(8) 0.063(8) -0.002(6) 0.011(6) -0.009(6)
C13 0.049(6) 0.054(7) 0.059(7) 0.011(6) -0.003(5) -0.001(5)
C14 0.057(7) 0.066(7) 0.060(7) -0.010(6) 0.022(6) -0.007(6)
C21 0.076(9) 0.084(10) 0.077(9) 0.016(7) -0.008(7) 0.019(7)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag 0.1306 4.2820 '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
O1 Ag1 S1 . . 118.4(3) y
O1 Ag1 S2 . 8_655 96.1(2) y
S1 Ag1 S2 . 8_655 120.66(10) y
O1 Ag1 S2 . 5_576 103.1(2) y
S1 Ag1 S2 . 5_576 99.44(10) y
S2 Ag1 S2 8_655 5_576 118.93(7) y
C11 S1 C12 . . 100.7(6) y
C11 S1 Ag1 . . 112.2(5) y
C12 S1 Ag1 . . 106.7(4) y
C14 S2 C21 . . 101.3(6) y
C14 S2 Ag1 . 8_665 109.4(4) y
C21 S2 Ag1 . 8_665 106.1(5) y
C14 S2 Ag1 . 5_576 112.5(4) y
C21 S2 Ag1 . 5_576 112.1(4) y
Ag1 S2 Ag1 8_665 5_576 114.48(10) y
C1 O1 Ag1 . . 105.7(9) y
O1 C1 O2 . . 128.70(14) y
O1 C1 C2 . . 119.40(14) y
O2 C1 C2 . . 111.00(14) y
F6 C2 F1 . . 95(3) y
F6 C2 F4 . . 83(2) y
F1 C2 F4 . . 121(2) y
F6 C2 F9 . . 44(3) y
F1 C2 F9 . . 65(4) y
F4 C2 F9 . . 125(3) y
F6 C2 F7 . . 43.90(17) y
F1 C2 F7 . . 115(2) y
F4 C2 F7 . . 38.60(16) y
F9 C2 F7 . . 87(3) y
F6 C2 F8 . . 122(4) y
F1 C2 F8 . . 55(6) y
F4 C2 F8 . . 76(6) y
F9 C2 F8 . . 117(7) y
F7 C2 F8 . . 100(5) y
F6 C2 F2 . . 115(2) y
F1 C2 F2 . . 24.00(15) y
F4 C2 F2 . . 108(2) y
F9 C2 F2 . . 89(4) y
F7 C2 F2 . . 119.30(17) y
F8 C2 F2 . . 34(5) y
F6 C2 C1 . . 124.50(17) y
F1 C2 C1 . . 119.40(15) y
F4 C2 C1 . . 109.40(15) y
F9 C2 C1 . . 112(3) y
F7 C2 C1 . . 125.50(17) y
F8 C2 C1 . . 114(3) y
F2 C2 C1 . . 112.10(14) y
F6 C2 F5 . . 108(2) y
F1 C2 F5 . . 99(3) y
F4 C2 F5 . . 31.60(14) y
F9 C2 F5 . . 141(3) y
F7 C2 F5 . . 67(2) y
F8 C2 F5 . . 46(6) y
F2 C2 F5 . . 80(2) y
C1 C2 F5 . . 107.40(13) y
F6 C2 F3 . . 38.00(14) y
F1 C2 F3 . . 88(3) y
F4 C2 F3 . . 118(2) y
F9 C2 F3 . . 23(3) y
F7 C2 F3 . . 80(2) y
F8 C2 F3 . . 140(5) y
F2 C2 F3 . . 112(3) y
C1 C2 F3 . . 97.30(18) y
F5 C2 F3 . . 146.10(19) y
S1 C11 H11A . . 109.5 ?
S1 C11 H11B . . 109.5 ?
H11A C11 H11B . . 109.5 ?
S1 C11 H11C . . 109.5 ?
H11A C11 H11C . . 109.5 ?
H11B C11 H11C . . 109.5 ?
C13 C12 S1 . . 111.9(7) y
C13 C12 H12A . . 109.2 ?
S1 C12 H12A . . 109.2 ?
C13 C12 H12B . . 109.2 ?
S1 C12 H12B . . 109.2 ?
H12A C12 H12B . . 107.9 ?
C12 C13 C14 . . 109.7(8) y
C12 C13 H13A . . 109.7 ?
C14 C13 H13A . . 109.7 ?
C12 C13 H13B . . 109.7 ?
C14 C13 H13B . . 109.7 ?
H13A C13 H13B . . 108.2 ?
C13 C14 S2 . . 113.6(7) y
C13 C14 H14A . . 108.8 ?
S2 C14 H14A . . 108.8 ?
C13 C14 H14B . . 108.8 ?
S2 C14 H14B . . 108.8 ?
H14A C14 H14B . . 107.7 ?
S2 C21 H21A . . 109.5 ?
S2 C21 H21B . . 109.5 ?
H21A C21 H21B . . 109.5 ?
S2 C21 H21C . . 109.5 ?
H21A C21 H21C . . 109.5 ?
H21B C21 H21C . . 109.5 ?
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
Ag1 O1 . 2.404(9) y
Ag1 S1 . 2.512(3) y
Ag1 S2 8_655 2.573(3) y
Ag1 S2 5_576 2.712(3) y
S1 C11 . 1.776(14) y
S1 C12 . 1.801(11) y
S2 C14 . 1.804(10) y
S2 C21 . 1.814(12) y
S2 Ag1 8_665 2.573(3) y
S2 Ag1 5_576 2.712(3) y
O1 C1 . 1.177(15) y
O2 C1 . 1.280(16) y
C1 C2 . 1.513(18) y
C2 F6 . 1.27(2) y
C2 F1 . 1.28(2) y
C2 F4 . 1.29(2) y
C2 F9 . 1.31(5) y
C2 F7 . 1.31(3) y
C2 F8 . 1.37(9) y
C2 F2 . 1.42(3) y
C2 F5 . 1.55(3) y
C2 F3 . 1.56(4) y
C11 H11A . 0.98 ?
C11 H11B . 0.98 ?
C11 H11C . 0.98 ?
C12 C13 . 1.516(14) y
C12 H12A . 0.99 ?
C12 H12B . 0.99 ?
C13 C14 . 1.538(14) y
C13 H13A . 0.99 ?
C13 H13B . 0.99 ?
C14 H14A . 0.99 ?
C14 H14B . 0.99 ?
C21 H21A . 0.98 ?
C21 H21B . 0.98 ?
C21 H21C . 0.98 ?
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
_geom_torsion_publ_flag
O1 Ag1 S1 C11 . 114.0(7) y
S2 Ag1 S1 C11 8_655 -3.5(7) y
S2 Ag1 S1 C11 5_576 -135.4(6) y
O1 Ag1 S1 C12 . 4.5(5) y
S2 Ag1 S1 C12 8_655 -112.9(4) y
S2 Ag1 S1 C12 5_576 115.1(4) y
S1 Ag1 O1 C1 . 165.1(8) y
S2 Ag1 O1 C1 8_655 -65.1(9) y
S2 Ag1 O1 C1 5_576 56.6(9) y
Ag1 O1 C1 O2 . -5.00(18) y
Ag1 O1 C1 C2 . -173.0(9) y
O1 C1 C2 F6 . -139(2) y
O2 C1 C2 F6 . 51(2) y
O1 C1 C2 F1 . -18(3) y
O2 C1 C2 F1 . 172(3) y
O1 C1 C2 F4 . 127(2) y
O2 C1 C2 F4 . -43(3) y
O1 C1 C2 F9 . -91(4) y
O2 C1 C2 F9 . 99(4) y
O1 C1 C2 F7 . 167(3) y
O2 C1 C2 F7 . -3(3) y
O1 C1 C2 F8 . 44(7) y
O2 C1 C2 F8 . -126(7) y
O1 C1 C2 F2 . 7(3) y
O2 C1 C2 F2 . -163(2) y
O1 C1 C2 F5 . 93(2) y
O2 C1 C2 F5 . -77(2) y
O1 C1 C2 F3 . -110(2) y
O2 C1 C2 F3 . 80(2) y
C11 S1 C12 C13 . -163.8(9) y
Ag1 S1 C12 C13 . -46.4(9) y
S1 C12 C13 C14 . -170.5(8) y
C12 C13 C14 S2 . -177.0(8) y
C21 S2 C14 C13 . 68.4(9) y
Ag1 S2 C14 C13 8_665 -179.9(7) y
Ag1 S2 C14 C13 5_576 -51.4(9) y
|
1501559.cif | #------------------------------------------------------------------------------
#$Date: 2020-10-02 18:11:04 +0300 (Fri, 02 Oct 2020) $
#$Revision: 256942 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/50/15/1501559.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_1501559
loop_
_publ_author_name
'Mohamed Osman Awaleh'
'Francois Brisse'
'Youssouf Djibril Soubaneh'
'Thierry Maris'
_publ_section_title
;
Influence of the counteranion on silver(I)-dithioether coordination
polymers
;
_journal_name_full Polyhedron
_journal_page_first 2966
_journal_page_last 2975
_journal_paper_doi 10.1016/j.poly.2010.08.013
_journal_volume 29
_journal_year 2010
_chemical_compound_source 'Synthesized by the authors. See text'
_chemical_formula_sum 'C9 H12 Ag F7 O2 S2'
_chemical_formula_weight 457.18
_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 78.1150(10)
_cell_angle_beta 74.2710(10)
_cell_angle_gamma 77.7590(10)
_cell_formula_units_Z 2
_cell_length_a 7.8429(2)
_cell_length_b 8.1860(2)
_cell_length_c 12.5548(3)
_cell_measurement_reflns_used 7364
_cell_measurement_temperature 220(2)
_cell_measurement_theta_max 72.04
_cell_measurement_theta_min 3.70
_cell_volume 748.72(3)
_computing_cell_refinement 'SMART (Bruker, 1999)'
_computing_data_collection 'SMART (Bruker, 1999)'
_computing_data_reduction 'SAINT (Bruker, 1999)'
_computing_molecular_graphics 'SHELXTL (Bruker, 1997)'
_computing_publication_material 'UdMX (local program)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 220(2)
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type 'Bruker Smart 2000'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'X-ray Sealed Tube'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.077
_diffrn_reflns_av_sigmaI/netI 0.0585
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_number 8996
_diffrn_reflns_theta_full 72.03
_diffrn_reflns_theta_max 72.03
_diffrn_reflns_theta_min 3.70
_diffrn_standards_decay_% 1.26
_diffrn_standards_number 61
_exptl_absorpt_coefficient_mu 14.171
_exptl_absorpt_correction_T_max 0.2300
_exptl_absorpt_correction_T_min 0.1100
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Sadabs (Sheldrick,1996)'
_exptl_crystal_colour Colorless
_exptl_crystal_density_diffrn 2.028
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 448
_exptl_crystal_size_max 0.26
_exptl_crystal_size_mid 0.17
_exptl_crystal_size_min 0.11
_refine_diff_density_max 2.216
_refine_diff_density_min -1.513
_refine_diff_density_rms 0.195
_refine_ls_extinction_coef 0.0157(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 1.056
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 193
_refine_ls_number_reflns 2844
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.056
_refine_ls_R_factor_all 0.0657
_refine_ls_R_factor_gt 0.0647
_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^)+(0.1140P)^2^+2.2387P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1719
_refine_ls_wR_factor_ref 0.1749
_reflns_number_gt 2781
_reflns_number_total 2844
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file deposit.cif
_cod_data_source_block ande68
_cod_depositor_comments
;
Updated values of the _geom_bond_atom_site_label_*,
_geom_angle_atom_site_label_* and _geom_torsion_atom_site_label
data items to establish relationships between loop packets from
different data loops.
Antanas Vaitkus,
2020-10-02
;
_cod_original_sg_symbol_H-M P-1
_cod_database_code 1501559
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
Ag1 Ag 0.56830(6) 0.79357(5) 1.01768(3) 0.0445(3) Uani 1 1 d .
S1 S 0.2496(2) 0.89891(16) 1.00207(11) 0.0372(4) Uani 1 1 d .
S2 S 0.3415(2) 0.32550(19) 0.80291(12) 0.0387(4) Uani 1 1 d .
F1 F 1.0016(5) 0.8356(6) 0.6361(3) 0.0543(10) Uani 1 1 d .
F2 F 0.9037(6) 0.5984(5) 0.6609(3) 0.0529(10) Uani 1 1 d .
F3 F 0.5728(5) 0.8028(6) 0.6233(3) 0.0519(9) Uani 1 1 d .
F4 F 0.7265(7) 1.0096(5) 0.5586(3) 0.0528(10) Uani 1 1 d .
F5 F 0.7257(10) 0.8760(7) 0.3916(4) 0.0825(17) Uani 1 1 d .
F6 F 0.9827(7) 0.7763(7) 0.4271(4) 0.0686(13) Uani 1 1 d .
F7 F 0.7790(8) 0.6200(6) 0.4748(4) 0.0674(13) Uani 1 1 d .
O1 O 0.7532(7) 0.6699(8) 0.8604(4) 0.0612(15) Uani 1 1 d .
O2 O 0.6798(10) 0.9389(7) 0.7985(4) 0.0693(17) Uani 1 1 d .
C1 C 0.7510(8) 0.7950(8) 0.7871(4) 0.0346(12) Uani 1 1 d .
C2 C 0.8527(7) 0.7656(7) 0.6665(4) 0.0326(11) Uani 1 1 d .
C3 C 0.7380(8) 0.8422(7) 0.5800(5) 0.0359(12) Uani 1 1 d .
C4 C 0.8082(11) 0.7780(9) 0.4653(5) 0.0502(16) Uani 1 1 d .
C11 C 0.1144(8) 0.7937(8) 1.1261(5) 0.0404(13) Uani 1 1 d .
H11A H -0.0099 0.8179 1.1211 0.061 Uiso 1 1 calc R
H11B H 0.1241 0.8340 1.1913 0.061 Uiso 1 1 calc R
H11C H 0.1562 0.6726 1.1327 0.061 Uiso 1 1 calc R
C12 C 0.2112(9) 0.8068(8) 0.8931(5) 0.0424(14) Uani 1 1 d .
H12A H 0.0815 0.8156 0.9027 0.051 Uiso 1 1 calc R
H12B H 0.2582 0.8723 0.8202 0.051 Uiso 1 1 calc R
C13 C 0.2984(8) 0.6217(7) 0.8928(5) 0.0353(12) Uani 1 1 d .
H13A H 0.2695 0.5590 0.9690 0.042 Uiso 1 1 calc R
H13B H 0.4292 0.6140 0.8683 0.042 Uiso 1 1 calc R
C14 C 0.2325(8) 0.5424(8) 0.8147(6) 0.0417(13) Uani 1 1 d .
H14A H 0.2536 0.6111 0.7401 0.050 Uiso 1 1 calc R
H14B H 0.1027 0.5448 0.8423 0.050 Uiso 1 1 calc R
C21 C 0.5472(9) 0.3579(10) 0.7015(6) 0.0476(15) Uani 1 1 d .
H21A H 0.5203 0.4219 0.6322 0.071 Uiso 1 1 calc R
H21B H 0.6195 0.2492 0.6875 0.071 Uiso 1 1 calc R
H21C H 0.6131 0.4202 0.7300 0.071 Uiso 1 1 calc R
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ag1 0.0572(4) 0.0432(4) 0.0265(3) -0.0117(2) 0.0070(2) -0.0102(2)
S1 0.0537(8) 0.0276(6) 0.0247(7) -0.0079(5) 0.0025(6) -0.0064(5)
S2 0.0450(8) 0.0450(8) 0.0316(7) -0.0197(6) -0.0018(6) -0.0154(6)
F1 0.0405(19) 0.086(3) 0.036(2) -0.0014(19) -0.0021(15) -0.0272(19)
F2 0.074(3) 0.043(2) 0.0318(19) -0.0137(15) -0.0048(17) 0.0103(18)
F3 0.0412(19) 0.076(3) 0.040(2) -0.0183(19) -0.0067(15) -0.0091(18)
F4 0.084(3) 0.0407(19) 0.0287(18) -0.0050(15) -0.0127(18) -0.0022(18)
F5 0.134(5) 0.085(3) 0.035(2) -0.016(2) -0.042(3) 0.003(3)
F6 0.076(3) 0.093(3) 0.027(2) -0.023(2) 0.0159(19) -0.018(3)
F7 0.103(4) 0.062(3) 0.045(2) -0.030(2) -0.011(2) -0.019(2)
O1 0.062(3) 0.073(3) 0.023(2) 0.006(2) 0.009(2) 0.007(3)
O2 0.112(5) 0.052(3) 0.035(3) -0.028(2) 0.016(3) -0.016(3)
C1 0.038(3) 0.053(3) 0.015(2) -0.010(2) -0.002(2) -0.014(2)
C2 0.034(3) 0.041(3) 0.021(2) -0.007(2) -0.002(2) -0.008(2)
C3 0.044(3) 0.040(3) 0.022(3) -0.009(2) -0.003(2) -0.005(2)
C4 0.074(5) 0.055(4) 0.021(3) -0.012(3) -0.008(3) -0.011(3)
C11 0.041(3) 0.044(3) 0.030(3) -0.009(2) 0.004(2) -0.006(2)
C12 0.055(3) 0.039(3) 0.030(3) -0.012(2) -0.014(3) 0.009(3)
C13 0.045(3) 0.034(3) 0.028(3) -0.011(2) -0.012(2) 0.001(2)
C14 0.038(3) 0.049(3) 0.044(3) -0.021(3) -0.016(3) 0.004(2)
C21 0.047(3) 0.057(4) 0.034(3) -0.013(3) 0.003(3) -0.009(3)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag 0.1306 4.2820 '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
O1 Ag1 S2 . 2_667 114.45(13) y
O1 Ag1 S1 . . 113.20(15) y
S2 Ag1 S1 2_667 . 124.36(5) y
O1 Ag1 Ag1 . 2_677 118.20(13) y
S2 Ag1 Ag1 2_667 2_677 114.53(4) y
S1 Ag1 Ag1 . 2_677 62.42(3) y
C11 S1 C12 . . 101.9(3) y
C11 S1 Ag1 . . 105.1(2) y
C12 S1 Ag1 . . 108.5(2) y
C21 S2 C14 . . 101.2(3) y
C21 S2 Ag1 . 2_667 105.0(2) y
C14 S2 Ag1 . 2_667 106.2(2) y
C1 O1 Ag1 . . 99.8(4) y
O2 C1 O1 . . 127.4(6) y
O2 C1 C2 . . 116.3(5) y
O1 C1 C2 . . 116.3(5) y
F1 C2 F2 . . 107.6(5) y
F1 C2 C1 . . 109.4(5) y
F2 C2 C1 . . 111.1(5) y
F1 C2 C3 . . 108.6(5) y
F2 C2 C3 . . 107.5(4) y
C1 C2 C3 . . 112.6(4) y
F4 C3 F3 . . 109.3(5) y
F4 C3 C2 . . 110.2(5) y
F3 C3 C2 . . 108.4(5) y
F4 C3 C4 . . 106.8(5) y
F3 C3 C4 . . 106.6(5) y
C2 C3 C4 . . 115.5(5) y
F5 C4 F6 . . 108.7(6) y
F5 C4 F7 . . 108.6(6) y
F6 C4 F7 . . 107.3(6) y
F5 C4 C3 . . 110.0(6) y
F6 C4 C3 . . 111.4(6) y
F7 C4 C3 . . 110.8(6) y
S1 C11 H11A . . 109.5 ?
S1 C11 H11B . . 109.5 ?
H11A C11 H11B . . 109.5 ?
S1 C11 H11C . . 109.5 ?
H11A C11 H11C . . 109.5 ?
H11B C11 H11C . . 109.5 ?
C13 C12 S1 . . 113.6(4) y
C13 C12 H12A . . 108.9 ?
S1 C12 H12A . . 108.9 ?
C13 C12 H12B . . 108.9 ?
S1 C12 H12B . . 108.9 ?
H12A C12 H12B . . 107.7 ?
C12 C13 C14 . . 110.9(5) y
C12 C13 H13A . . 109.5 ?
C14 C13 H13A . . 109.5 ?
C12 C13 H13B . . 109.5 ?
C14 C13 H13B . . 109.5 ?
H13A C13 H13B . . 108 ?
C13 C14 S2 . . 113.5(4) y
C13 C14 H14A . . 108.9 ?
S2 C14 H14A . . 108.9 ?
C13 C14 H14B . . 108.9 ?
S2 C14 H14B . . 108.9 ?
H14A C14 H14B . . 107.7 ?
S2 C21 H21A . . 109.5 ?
S2 C21 H21B . . 109.5 ?
H21A C21 H21B . . 109.5 ?
S2 C21 H21C . . 109.5 ?
H21A C21 H21C . . 109.5 ?
H21B C21 H21C . . 109.5 ?
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
Ag1 O1 . 2.382(5) y
Ag1 S2 2_667 2.4883(16) y
Ag1 S1 . 2.5124(16) y
Ag1 Ag1 2_677 3.2972(8) y
S1 C11 . 1.797(6) y
S1 C12 . 1.810(6) y
S2 C21 . 1.795(7) y
S2 C14 . 1.817(6) y
S2 Ag1 2_667 2.4883(16) y
F1 C2 . 1.338(7) y
F2 C2 . 1.353(7) y
F3 C3 . 1.343(7) y
F4 C3 . 1.330(7) y
F5 C4 . 1.310(9) y
F6 C4 . 1.32(1) y
F7 C4 . 1.337(9) y
O1 C1 . 1.228(8) y
O2 C1 . 1.212(8) y
C1 C2 . 1.549(7) y
C2 C3 . 1.546(8) y
C3 C4 . 1.553(8) y
C11 H11A . 0.97 ?
C11 H11B . 0.97 ?
C11 H11C . 0.97 ?
C12 C13 . 1.525(8) y
C12 H12A . 0.98 ?
C12 H12B . 0.98 ?
C13 C14 . 1.526(8) y
C13 H13A . 0.98 ?
C13 H13B . 0.98 ?
C14 H14A . 0.98 ?
C14 H14B . 0.98 ?
C21 H21A . 0.97 ?
C21 H21B . 0.97 ?
C21 H21C . 0.97 ?
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
_geom_torsion_publ_flag
O1 Ag1 S1 C11 . 124.2(3) y
S2 Ag1 S1 C11 2_667 -22.9(2) y
Ag1 Ag1 S1 C11 2_677 -125.0(2) y
O1 Ag1 S1 C12 . 15.7(3) y
S2 Ag1 S1 C12 2_667 -131.3(2) y
Ag1 Ag1 S1 C12 2_677 126.6(2) y
S2 Ag1 O1 C1 2_667 -144.8(4) y
S1 Ag1 O1 C1 . 64.8(5) y
Ag1 Ag1 O1 C1 2_677 -5.2(5) y
Ag1 O1 C1 O2 . 3.4(8) y
Ag1 O1 C1 C2 . -177.4(4) y
O2 C1 C2 F1 . 70.4(7) y
O1 C1 C2 F1 . -108.8(6) y
O2 C1 C2 F2 . -171.0(6) y
O1 C1 C2 F2 . 9.7(7) y
O2 C1 C2 C3 . -50.3(7) y
O1 C1 C2 C3 . 130.4(6) y
F1 C2 C3 F4 . -46.4(6) y
F2 C2 C3 F4 . -162.5(5) y
C1 C2 C3 F4 . 74.8(6) y
F1 C2 C3 F3 . -165.9(5) y
F2 C2 C3 F3 . 78.0(6) y
C1 C2 C3 F3 . -44.7(6) y
F1 C2 C3 C4 . 74.7(6) y
F2 C2 C3 C4 . -41.4(7) y
C1 C2 C3 C4 . -164.1(5) y
F4 C3 C4 F5 . -43.3(8) y
F3 C3 C4 F5 . 73.4(7) y
C2 C3 C4 F5 . -166.2(6) y
F4 C3 C4 F6 . 77.2(7) y
F3 C3 C4 F6 . -166.1(5) y
C2 C3 C4 F6 . -45.7(8) y
F4 C3 C4 F7 . -163.4(6) y
F3 C3 C4 F7 . -46.7(7) y
C2 C3 C4 F7 . 73.7(8) y
C11 S1 C12 C13 . -70.5(5) y
Ag1 S1 C12 C13 . 40.1(5) y
S1 C12 C13 C14 . 169.2(5) y
C12 C13 C14 S2 . 176.2(5) y
C21 S2 C14 C13 . -81.7(5) y
Ag1 S2 C14 C13 2_667 27.7(5) y
|
1501560.cif | #------------------------------------------------------------------------------
#$Date: 2020-10-02 18:11:04 +0300 (Fri, 02 Oct 2020) $
#$Revision: 256942 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/50/15/1501560.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_1501560
loop_
_publ_author_name
'Mohamed Osman Awaleh'
'Francois Brisse'
'Youssouf Djibril Soubaneh'
'Thierry Maris'
_publ_section_title
;
Influence of the counteranion on silver(I)-dithioether coordination
polymers
;
_journal_name_full Polyhedron
_journal_page_first 2966
_journal_page_last 2975
_journal_paper_doi 10.1016/j.poly.2010.08.013
_journal_volume 29
_journal_year 2010
_chemical_compound_source 'Synthesized by the authors. See text'
_chemical_formula_sum 'C7 H12 Ag F2 O2 S2'
_chemical_formula_weight 338.16
_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 112.090(2)
_cell_angle_beta 107.066(2)
_cell_angle_gamma 94.179(2)
_cell_formula_units_Z 2
_cell_length_a 7.6593(4)
_cell_length_b 8.3150(4)
_cell_length_c 10.0000(4)
_cell_measurement_reflns_used 4418
_cell_measurement_temperature 220(2)
_cell_measurement_theta_max 71.90
_cell_measurement_theta_min 5.09
_cell_volume 551.93(5)
_computing_cell_refinement 'SMART (Bruker, 1999)'
_computing_data_collection 'SMART (Bruker, 1999)'
_computing_data_reduction 'SAINT (Bruker, 1999)'
_computing_molecular_graphics 'SHELXTL (Bruker, 1997)'
_computing_publication_material 'UdMX (local program)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 220(2)
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type 'Bruker Smart 2000'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'X-ray Sealed Tube'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.068
_diffrn_reflns_av_sigmaI/netI 0.0587
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_h_min -9
_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 6677
_diffrn_reflns_theta_full 71.87
_diffrn_reflns_theta_max 71.87
_diffrn_reflns_theta_min 5.09
_diffrn_standards_decay_% -0.57
_diffrn_standards_number 37
_exptl_absorpt_coefficient_mu 18.256
_exptl_absorpt_correction_T_max 0.5600
_exptl_absorpt_correction_T_min 0.3200
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Sadabs (Sheldrick,1996)'
_exptl_crystal_colour Colorless
_exptl_crystal_density_diffrn 2.035
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 334
_exptl_crystal_size_max 0.16
_exptl_crystal_size_mid 0.12
_exptl_crystal_size_min 0.10
_refine_diff_density_max 1.020
_refine_diff_density_min -0.838
_refine_diff_density_rms 0.178
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.045
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 129
_refine_ls_number_reflns 2106
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.045
_refine_ls_R_factor_all 0.0482
_refine_ls_R_factor_gt 0.0455
_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^)+(0.0900P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1141
_refine_ls_wR_factor_ref 0.1182
_reflns_number_gt 1935
_reflns_number_total 2106
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file deposit.cif
_cod_data_source_block ande62
_cod_depositor_comments
;
Updated values of the _geom_bond_atom_site_label_*,
_geom_angle_atom_site_label_* and _geom_torsion_atom_site_label
data items to establish relationships between loop packets from
different data loops.
Antanas Vaitkus,
2020-10-02
;
_cod_original_cell_volume 551.93(4)
_cod_original_sg_symbol_H-M P-1
_cod_database_code 1501560
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
Ag1 Ag 0.59059(4) 0.70595(4) 0.52948(3) 0.03563(17) Uani 1 1 d .
S1 S 0.80618(15) 0.88163(13) 0.79575(11) 0.0303(3) Uani 1 1 d .
S3 S 0.23881(15) 0.61656(13) 0.45487(12) 0.0324(3) Uani 1 1 d .
F1 F 0.7028(4) 0.6294(5) 0.0178(4) 0.0499(8) Uani 1 1 d .
F2 F 0.6706(4) 0.3765(4) 0.0326(3) 0.0439(7) Uani 1 1 d .
O1 O 0.6559(7) 0.7845(5) 0.2863(5) 0.0645(12) Uani 1 1 d .
O2 O 0.5901(7) 0.5214(7) 0.2871(4) 0.0604(11) Uani 1 1 d .
C1 C 0.6188(6) 0.6224(7) 0.2278(5) 0.0352(10) Uani 1 1 d .
C2 C 0.6004(5) 0.5272(5) 0.0571(4) 0.0247(8) Uani 1 1 d .
C3 C 0.1596(8) 0.7574(8) 0.6027(6) 0.0458(12) Uani 1 1 d .
H3A H 0.2032 0.8806 0.6260 0.069 Uiso 1 1 calc R
H3B H 0.2087 0.7370 0.6947 0.069 Uiso 1 1 calc R
H3C H 0.0243 0.7303 0.5669 0.069 Uiso 1 1 calc R
C13 C 0.9048(6) 1.0911(6) 0.8029(5) 0.0323(9) Uani 1 1 d .
H13A H 0.9248 1.1851 0.9044 0.039 Uiso 1 1 calc R
H13B H 1.0270 1.0844 0.7910 0.039 Uiso 1 1 calc R
C12 C 0.6469(8) 0.9494(7) 0.8983(6) 0.0412(11) Uani 1 1 d .
H12A H 0.7172 1.0225 1.0061 0.062 Uiso 1 1 calc R
H12B H 0.5694 0.8452 0.8887 0.062 Uiso 1 1 calc R
H12C H 0.5684 1.0168 0.8551 0.062 Uiso 1 1 calc R
C31 C 0.1307(6) 0.6746(6) 0.2967(5) 0.0356(9) Uani 1 1 d .
H31A H 0.1405 0.5866 0.2025 0.043 Uiso 1 1 calc R
H31B H -0.0023 0.6682 0.2820 0.043 Uiso 1 1 calc R
C32 C 0.2159(6) 0.8585(6) 0.3195(5) 0.0316(9) Uani 1 1 d .
H32A H 0.2269 0.9456 0.4217 0.038 Uiso 1 1 calc R
H32B H 0.3414 0.8595 0.3135 0.038 Uiso 1 1 calc R
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ag1 0.0498(3) 0.0308(2) 0.0221(2) 0.00693(16) 0.01155(15) 0.01042(15)
S1 0.0418(5) 0.0276(5) 0.0215(5) 0.0101(4) 0.0093(4) 0.0144(4)
S3 0.0436(6) 0.0229(5) 0.0331(5) 0.0122(4) 0.0155(4) 0.0091(4)
F1 0.0397(15) 0.064(2) 0.0412(16) 0.0264(15) 0.0075(12) -0.0131(13)
F2 0.0482(15) 0.0402(15) 0.0329(14) 0.0049(12) 0.0091(11) 0.0266(12)
O1 0.071(3) 0.039(2) 0.046(2) -0.0161(18) 0.0125(19) 0.0085(19)
O2 0.086(3) 0.075(3) 0.0283(18) 0.026(2) 0.0240(19) 0.021(2)
C1 0.031(2) 0.044(2) 0.0163(18) 0.0014(18) 0.0021(14) 0.0125(18)
C2 0.027(2) 0.0228(18) 0.0220(18) 0.0067(15) 0.0085(15) 0.0058(14)
C3 0.048(3) 0.049(3) 0.044(3) 0.016(2) 0.026(2) 0.011(2)
C13 0.034(2) 0.034(2) 0.0253(19) 0.0106(17) 0.0070(15) 0.0101(16)
C12 0.059(3) 0.039(2) 0.032(2) 0.014(2) 0.024(2) 0.014(2)
C31 0.037(2) 0.028(2) 0.030(2) 0.0091(17) 0.0012(16) 0.0016(16)
C32 0.0278(19) 0.033(2) 0.031(2) 0.0151(18) 0.0043(15) 0.0048(16)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag 0.1306 4.2820 '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
O2 Ag1 S1 . . 141.04(12) y
O2 Ag1 S3 . . 93.55(12) y
S1 Ag1 S3 . . 124.12(4) y
O2 Ag1 Ag1 . 2_666 74.57(12) y
S1 Ag1 Ag1 . 2_666 112.53(3) y
S3 Ag1 Ag1 . 2_666 61.53(2) y
C12 S1 C13 . . 101.1(2) y
C12 S1 Ag1 . . 102.04(18) y
C13 S1 Ag1 . . 106.65(14) y
C3 S3 C31 . . 101.9(3) y
C3 S3 Ag1 . . 110.88(19) y
C31 S3 Ag1 . . 107.19(16) y
C1 O2 Ag1 . . 105.1(3) y
O1 C1 O2 . . 128.3(5) y
O1 C1 C2 . . 117.4(5) y
O2 C1 C2 . . 114.3(4) y
F1 C2 F2 . . 105.6(3) y
F1 C2 C2 . 2_665 107.9(4) y
F2 C2 C2 . 2_665 107.0(4) y
F1 C2 C1 . . 111.0(4) y
F2 C2 C1 . . 110.4(3) y
C2 C2 C1 2_665 . 114.5(4) y
S3 C3 H3A . . 109.5 ?
S3 C3 H3B . . 109.5 ?
H3A C3 H3B . . 109.5 ?
S3 C3 H3C . . 109.5 ?
H3A C3 H3C . . 109.5 ?
H3B C3 H3C . . 109.5 ?
C32 C13 S1 2_676 . 114.0(3) y
C32 C13 H13A 2_676 . 108.8 ?
S1 C13 H13A . . 108.8 ?
C32 C13 H13B 2_676 . 108.8 ?
S1 C13 H13B . . 108.8 ?
H13A C13 H13B . . 107.7 ?
S1 C12 H12A . . 109.5 ?
S1 C12 H12B . . 109.5 ?
H12A C12 H12B . . 109.5 ?
S1 C12 H12C . . 109.5 ?
H12A C12 H12C . . 109.5 ?
H12B C12 H12C . . 109.5 ?
C32 C31 S3 . . 114.2(3) y
C32 C31 H31A . . 108.7 ?
S3 C31 H31A . . 108.7 ?
C32 C31 H31B . . 108.7 ?
S3 C31 H31B . . 108.7 ?
H31A C31 H31B . . 107.6 ?
C13 C32 C31 2_676 . 110.4(3) y
C13 C32 H32A 2_676 . 109.6 ?
C31 C32 H32A . . 109.6 ?
C13 C32 H32B 2_676 . 109.6 ?
C31 C32 H32B . . 109.6 ?
H32A C32 H32B . . 108.1 ?
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
Ag1 O2 . 2.329(4) y
Ag1 S1 . 2.4684(10) y
Ag1 S3 . 2.5456(11) y
Ag1 Ag1 2_666 3.3633(6) y
S1 C12 . 1.805(5) y
S1 C13 . 1.815(5) y
S3 C3 . 1.804(5) y
S3 C31 . 1.812(5) y
F1 C2 . 1.351(5) y
F2 C2 . 1.365(5) y
O1 C1 . 1.222(7) y
O2 C1 . 1.237(7) y
C1 C2 . 1.545(6) y
C2 C2 2_665 1.534(7) y
C3 H3A . 0.97 ?
C3 H3B . 0.97 ?
C3 H3C . 0.97 ?
C13 C32 2_676 1.518(5) y
C13 H13A . 0.98 ?
C13 H13B . 0.98 ?
C12 H12A . 0.97 ?
C12 H12B . 0.97 ?
C12 H12C . 0.97 ?
C31 C32 . 1.523(6) y
C31 H31A . 0.98 ?
C31 H31B . 0.98 ?
C32 C13 2_676 1.518(5) y
C32 H32A . 0.98 ?
C32 H32B . 0.98 ?
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_4
_geom_torsion
_geom_torsion_publ_flag
O2 Ag1 S1 C12 . . -172.1(2) y
S3 Ag1 S1 C12 . . -9.00(18) y
Ag1 Ag1 S1 C12 2_666 . -78.98(17) y
O2 Ag1 S1 C13 . . 82.2(2) y
S3 Ag1 S1 C13 . . -114.65(15) y
Ag1 Ag1 S1 C13 2_666 . 175.37(15) y
O2 Ag1 S3 C3 . . -170.3(2) y
S1 Ag1 S3 C3 . . 20.2(2) y
Ag1 Ag1 S3 C3 2_666 . 119.4(2) y
O2 Ag1 S3 C31 . . -59.9(2) y
S1 Ag1 S3 C31 . . 130.61(16) y
Ag1 Ag1 S3 C31 2_666 . -130.24(16) y
S1 Ag1 O2 C1 . . -86.7(3) y
S3 Ag1 O2 C1 . . 107.2(3) y
Ag1 Ag1 O2 C1 2_666 . 166.4(4) y
Ag1 O2 C1 O1 . . 5.8(7) y
Ag1 O2 C1 C2 . . -172.9(3) y
O1 C1 C2 F1 . . 26.4(6) y
O2 C1 C2 F1 . . -154.8(4) y
O1 C1 C2 F2 . . 143.1(4) y
O2 C1 C2 F2 . . -38.0(5) y
O1 C1 C2 C2 . 2_665 -96.0(6) y
O2 C1 C2 C2 . 2_665 82.8(6) y
C12 S1 C13 C32 . 2_676 -82.1(4) y
Ag1 S1 C13 C32 . 2_676 24.2(4) y
C3 S3 C31 C32 . . 71.4(4) y
Ag1 S3 C31 C32 . . -45.1(4) y
S3 C31 C32 C13 . 2_676 -169.4(3) y
|
1501561.cif | #------------------------------------------------------------------------------
#$Date: 2020-10-02 18:49:34 +0300 (Fri, 02 Oct 2020) $
#$Revision: 256944 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/50/15/1501561.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_1501561
loop_
_publ_author_name
'Mohamed Osman Awaleh'
'Francois Brisse'
'Youssouf Djibril Soubaneh'
'Thierry Maris'
'Elias Said Dirieh'
_publ_section_title
;
Four New Ag(I) Coordination Polymers: Synthesis, Crystal Structures and
Thermal Stability
;
_journal_name_full 'J. Inorg. Organomet. Polym.'
_journal_page_first 816
_journal_page_last 824
_journal_paper_doi 10.1007/s10904-010-9407-0
_journal_volume 20
_journal_year 2010
_chemical_compound_source 'Synthesized by the authors. See text'
_chemical_formula_moiety 'C57 H48 Ag6 F12 O12 S6'
_chemical_formula_sum 'C57 H48 Ag6 F12 O12 S6'
_chemical_formula_weight 1992.53
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 93.8680(10)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 10.4359(2)
_cell_length_b 23.9932(4)
_cell_length_c 25.6039(4)
_cell_measurement_reflns_used 7347
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 72.94
_cell_measurement_theta_min 2.53
_cell_volume 6396.37(19)
_computing_cell_refinement 'SMART (Bruker, 1999)'
_computing_data_collection 'SMART (Bruker, 1999)'
_computing_data_reduction 'SAINT (Bruker, 1999)'
_computing_molecular_graphics 'SHELXTL (Bruker, 1997)'
_computing_publication_material 'UdMX (local program)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type 'Bruker Smart 2000'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'Sealed Tube'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.053
_diffrn_reflns_av_sigmaI/netI 0.0360
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 29
_diffrn_reflns_limit_k_min -29
_diffrn_reflns_limit_l_max 31
_diffrn_reflns_limit_l_min -31
_diffrn_reflns_number 77743
_diffrn_reflns_theta_full 72.93
_diffrn_reflns_theta_max 72.93
_diffrn_reflns_theta_min 2.53
_diffrn_standards_decay_% 0.00
_diffrn_standards_number 529
_exptl_absorpt_coefficient_mu 17.122
_exptl_absorpt_correction_T_max 0.302
_exptl_absorpt_correction_T_min 0.103
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Sadabs (Sheldrick,1996)'
_exptl_crystal_colour Colourless
_exptl_crystal_density_diffrn 2.069
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 3888
_exptl_crystal_size_max 0.39
_exptl_crystal_size_mid 0.14
_exptl_crystal_size_min 0.07
_refine_diff_density_max 1.490
_refine_diff_density_min -0.897
_refine_diff_density_rms 0.143
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.013
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 838
_refine_ls_number_reflns 12258
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.013
_refine_ls_R_factor_all 0.0414
_refine_ls_R_factor_gt 0.0343
_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^)+(0.0574P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0871
_refine_ls_wR_factor_ref 0.0896
_reflns_number_gt 10405
_reflns_number_total 12258
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file deposit.cif
_cod_data_source_block Complex1
_cod_depositor_comments
;
Updated values of the _geom_angle_atom_site_label_* and
_geom_bond_atom_site_label_* data items to establish
relationships between loop packets from different data loops.
Antanas Vaitkus,
2020-10-02
;
_cod_original_sg_symbol_H-M P21/c
_cod_database_code 1501561
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
Ag1 Ag 1.02757(3) 0.790511(13) 0.038509(13) 0.02231(8) Uani 1 1 d .
Ag2 Ag 0.94376(3) 0.689716(12) -0.020086(12) 0.02058(8) Uani 1 1 d .
Ag3 Ag 0.68150(3) 0.693445(12) 0.043634(11) 0.01898(8) Uani 1 1 d .
Ag4 Ag 0.96716(3) 0.976598(13) 0.054765(12) 0.02187(8) Uani 1 1 d .
Ag5 Ag 0.52636(3) 0.447978(12) -0.028389(11) 0.01876(8) Uani 1 1 d .
Ag6 Ag 1.35184(3) 0.678475(13) -0.034493(11) 0.01991(8) Uani 1 1 d .
S1 S 1.24171(10) 0.77507(4) -0.03855(4) 0.0183(2) Uani 1 1 d .
S2 S 1.12261(10) 0.88875(4) 0.05768(4) 0.0175(2) Uani 1 1 d .
S3 S 0.12638(10) 0.62642(4) -0.05458(4) 0.0194(2) Uani 1 1 d .
S4 S 0.30798(10) 0.41081(4) -0.06519(4) 0.0166(2) Uani 1 1 d .
S5 S 0.80463(10) 0.76911(4) 0.08841(4) 0.0170(2) Uani 1 1 d .
S6 S 0.76056(12) 0.99837(4) 0.10378(4) 0.0240(2) Uani 1 1 d .
F1 F 0.6767(3) 0.67945(11) -0.15756(9) 0.0255(6) Uani 1 1 d .
F2 F 0.4796(2) 0.67333(11) -0.13577(9) 0.0242(6) Uani 1 1 d .
F3 F 0.7193(3) 0.57584(11) -0.14708(10) 0.0262(6) Uani 1 1 d .
F4 F 0.5158(3) 0.57727(11) -0.17290(9) 0.0268(6) Uani 1 1 d .
F5 F 0.6724(3) 0.81290(10) -0.12665(11) 0.0276(6) Uani 1 1 d .
F6 F 0.8478(3) 0.85455(11) -0.14436(9) 0.0262(6) Uani 1 1 d .
F7 F 0.6340(2) 0.87961(11) -0.04749(10) 0.0262(6) Uani 1 1 d .
F8 F 0.6606(3) 0.92455(10) -0.12044(10) 0.0263(6) Uani 1 1 d .
F9 F 1.1257(3) 0.64614(11) 0.17081(10) 0.0270(6) Uani 1 1 d .
F10 F 1.1858(3) 0.58783(10) 0.11186(10) 0.0277(6) Uani 1 1 d .
F11 F 1.3278(3) 0.70771(11) 0.16713(9) 0.0246(6) Uani 1 1 d .
F12 F 1.3897(3) 0.62126(11) 0.16639(10) 0.0302(6) Uani 1 1 d .
O1 O 0.7460(3) 0.64441(12) -0.05120(11) 0.0199(6) Uani 1 1 d .
O2 O 0.5823(3) 0.70296(12) -0.04171(11) 0.0213(7) Uani 1 1 d .
O3 O 0.6248(3) 0.51275(12) -0.07490(12) 0.0241(7) Uani 1 1 d .
O4 O 0.4820(3) 0.58021(12) -0.05840(11) 0.0202(6) Uani 1 1 d .
O5 O 0.8840(3) 0.82811(14) -0.02219(12) 0.0309(8) Uani 1 1 d .
O6 O 0.8698(3) 0.75591(13) -0.07794(13) 0.0294(8) Uani 1 1 d .
O7 O 0.8020(3) 0.95332(13) -0.01002(12) 0.0269(7) Uani 1 1 d .
O8 O 0.9195(3) 0.94401(14) -0.07965(13) 0.0301(8) Uani 1 1 d .
O9 O 1.1586(3) 0.72499(12) 0.07613(11) 0.0197(6) Uani 1 1 d .
O10 O 1.0125(3) 0.65609(12) 0.06226(12) 0.0227(7) Uani 1 1 d .
O11 O 1.3686(3) 0.63878(12) 0.05010(11) 0.0221(7) Uani 1 1 d .
O12 O 1.4833(3) 0.70871(14) 0.08950(12) 0.0262(7) Uani 1 1 d .
C11 C 1.2599(4) 0.80332(17) -0.10239(16) 0.0191(9) Uani 1 1 d .
C12 C 1.3745(5) 0.7980(2) -0.12657(18) 0.0302(11) Uani 1 1 d .
H12 H 1.4466 0.7802 -0.1091 0.036 Uiso 1 1 calc R
C13 C 1.3819(6) 0.8188(3) -0.1763(2) 0.0436(15) Uani 1 1 d .
H13 H 1.4599 0.8151 -0.1931 0.052 Uiso 1 1 calc R
C14 C 1.2790(5) 0.8449(2) -0.20223(18) 0.0356(12) Uani 1 1 d .
H14 H 1.2860 0.8592 -0.2365 0.043 Uiso 1 1 calc R
C15 C 1.1651(5) 0.8503(2) -0.17792(19) 0.0328(12) Uani 1 1 d .
H15 H 1.0933 0.8680 -0.1957 0.039 Uiso 1 1 calc R
C16 C 1.1558(5) 0.8298(2) -0.12752(19) 0.0283(11) Uani 1 1 d .
H16 H 1.0782 0.8340 -0.1105 0.034 Uiso 1 1 calc R
C17 C 1.3588(4) 0.81380(18) 0.00344(16) 0.0199(9) Uani 1 1 d .
H17A H 1.3494 0.8027 0.0402 0.024 Uiso 1 1 calc R
H17B H 1.4461 0.8028 -0.0055 0.024 Uiso 1 1 calc R
C18 C 1.3475(4) 0.87714(18) -0.00044(16) 0.0207(9) Uani 1 1 d .
H18A H 1.4039 0.8933 0.0283 0.025 Uiso 1 1 calc R
H18B H 1.3832 0.8886 -0.0337 0.025 Uiso 1 1 calc R
C19 C 1.2161(4) 0.90419(17) 0.00147(15) 0.0178(9) Uani 1 1 d .
H19A H 1.1640 0.8932 -0.0306 0.021 Uiso 1 1 calc R
H19B H 1.2280 0.9451 0.0000 0.021 Uiso 1 1 calc R
C21 C 1.2398(4) 0.89149(18) 0.11208(15) 0.0182(9) Uani 1 1 d .
C22 C 1.2871(4) 0.84274(18) 0.13453(17) 0.0220(9) Uani 1 1 d .
H22 H 1.2557 0.8076 0.1224 0.026 Uiso 1 1 calc R
C23 C 1.3823(5) 0.8461(2) 0.17554(17) 0.0268(10) Uani 1 1 d .
H23 H 1.4167 0.8130 0.1912 0.032 Uiso 1 1 calc R
C24 C 1.4272(5) 0.8978(2) 0.19370(17) 0.0300(11) Uani 1 1 d .
H24 H 1.4932 0.8999 0.2211 0.036 Uiso 1 1 calc R
C25 C 1.3744(5) 0.9464(2) 0.17135(18) 0.0300(11) Uani 1 1 d .
H25 H 1.4031 0.9816 0.1843 0.036 Uiso 1 1 calc R
C26 C 1.2806(5) 0.9437(2) 0.13047(17) 0.0265(10) Uani 1 1 d .
H26 H 1.2447 0.9768 0.1153 0.032 Uiso 1 1 calc R
C31 C 0.1053(5) 0.62433(18) -0.12423(17) 0.0216(9) Uani 1 1 d .
C32 C -0.0158(5) 0.6325(2) -0.14860(18) 0.0271(10) Uani 1 1 d .
H32 H -0.0876 0.6388 -0.1285 0.033 Uiso 1 1 calc R
C33 C -0.0306(6) 0.6313(2) -0.2027(2) 0.0344(12) Uani 1 1 d .
H33 H -0.1132 0.6358 -0.2202 0.041 Uiso 1 1 calc R
C34 C 0.0771(6) 0.6234(2) -0.2313(2) 0.0402(14) Uani 1 1 d .
H34 H 0.0679 0.6238 -0.2685 0.048 Uiso 1 1 calc R
C35 C 0.1938(6) 0.6153(2) -0.2070(2) 0.0398(14) Uani 1 1 d .
H35 H 0.2657 0.6092 -0.2271 0.048 Uiso 1 1 calc R
C36 C 0.2103(5) 0.6158(2) -0.1527(2) 0.0305(11) Uani 1 1 d .
H36 H 0.2930 0.6103 -0.1356 0.037 Uiso 1 1 calc R
C37 C 0.1004(5) 0.55371(17) -0.03621(17) 0.0209(9) Uani 1 1 d .
H37A H 0.1089 0.5504 0.0024 0.025 Uiso 1 1 calc R
H37B H 0.0119 0.5426 -0.0482 0.025 Uiso 1 1 calc R
C38 C 0.1953(4) 0.51422(16) -0.05966(17) 0.0193(9) Uani 1 1 d .
H38A H 0.2838 0.5269 -0.0496 0.023 Uiso 1 1 calc R
H38B H 0.1829 0.5158 -0.0983 0.023 Uiso 1 1 calc R
C39 C 0.1801(4) 0.45410(16) -0.04177(16) 0.0168(8) Uani 1 1 d .
H39A H 0.0957 0.4395 -0.0555 0.020 Uiso 1 1 calc R
H39B H 0.1831 0.4527 -0.0031 0.020 Uiso 1 1 calc R
C41 C 0.2857(4) 0.41845(17) -0.13458(15) 0.0174(9) Uani 1 1 d .
C42 C 0.1836(5) 0.39213(19) -0.16135(18) 0.0258(10) Uani 1 1 d .
H42 H 0.1237 0.3711 -0.1432 0.031 Uiso 1 1 calc R
C43 C 0.1706(5) 0.3972(2) -0.21579(19) 0.0351(12) Uani 1 1 d .
H43 H 0.1006 0.3796 -0.2349 0.042 Uiso 1 1 calc R
C44 C 0.2583(6) 0.4274(2) -0.24193(19) 0.0390(13) Uani 1 1 d .
H44 H 0.2495 0.4300 -0.2790 0.047 Uiso 1 1 calc R
C45 C 0.3587(5) 0.4538(2) -0.21449(19) 0.0394(14) Uani 1 1 d .
H45 H 0.4180 0.4751 -0.2328 0.047 Uiso 1 1 calc R
C46 C 0.3743(5) 0.44957(19) -0.16060(17) 0.0264(10) Uani 1 1 d .
H46 H 0.4440 0.4676 -0.1417 0.032 Uiso 1 1 calc R
C51 C 0.8194(5) 0.75691(17) 0.15754(16) 0.0206(9) Uani 1 1 d .
C52 C 0.9421(5) 0.75626(18) 0.18221(17) 0.0250(10) Uani 1 1 d .
H52 H 1.0156 0.7618 0.1629 0.030 Uiso 1 1 calc R
C53 C 0.9544(6) 0.7473(2) 0.23581(19) 0.0343(12) Uani 1 1 d .
H53 H 1.0375 0.7461 0.2533 0.041 Uiso 1 1 calc R
C54 C 0.8480(6) 0.7402(2) 0.26389(19) 0.0366(13) Uani 1 1 d .
H54 H 0.8577 0.7349 0.3007 0.044 Uiso 1 1 calc R
C55 C 0.7276(6) 0.7407(2) 0.2386(2) 0.0383(13) Uani 1 1 d .
H55 H 0.6545 0.7359 0.2583 0.046 Uiso 1 1 calc R
C56 C 0.7111(5) 0.7481(2) 0.18517(19) 0.0284(11) Uani 1 1 d .
H56 H 0.6279 0.7471 0.1677 0.034 Uiso 1 1 calc R
C57 C 0.6968(4) 0.82911(17) 0.08229(16) 0.0178(9) Uani 1 1 d .
H57A H 0.6708 0.8355 0.0449 0.021 Uiso 1 1 calc R
H57B H 0.6185 0.8212 0.1007 0.021 Uiso 1 1 calc R
C58 C 0.7611(5) 0.88133(17) 0.10517(18) 0.0224(9) Uani 1 1 d .
H58A H 0.8443 0.8871 0.0895 0.027 Uiso 1 1 calc R
H58B H 0.7783 0.8767 0.1434 0.027 Uiso 1 1 calc R
C59 C 0.6752(4) 0.93235(18) 0.09431(18) 0.0226(9) Uani 1 1 d .
H59A H 0.6036 0.9312 0.1178 0.027 Uiso 1 1 calc R
H59B H 0.6376 0.9304 0.0578 0.027 Uiso 1 1 calc R
C61 C 0.7999(5) 1.00034(18) 0.17254(18) 0.0252(10) Uani 1 1 d .
C62 C 0.9263(5) 0.9955(2) 0.1916(2) 0.0342(12) Uani 1 1 d .
H62 H 0.9918 0.9887 0.1683 0.041 Uiso 1 1 calc R
C63 C 0.9570(6) 1.0007(2) 0.2456(2) 0.0434(14) Uani 1 1 d .
H63 H 1.0440 0.9982 0.2590 0.052 Uiso 1 1 calc R
C64 C 0.8616(6) 1.0095(2) 0.2791(2) 0.0428(15) Uani 1 1 d .
H64 H 0.8829 1.0122 0.3156 0.051 Uiso 1 1 calc R
C65 C 0.7361(7) 1.0143(2) 0.2604(2) 0.0451(16) Uani 1 1 d .
H65 H 0.6706 1.0205 0.2837 0.054 Uiso 1 1 calc R
C66 C 0.7057(6) 1.0102(2) 0.2068(2) 0.0376(13) Uani 1 1 d .
H66 H 0.6189 1.0143 0.1936 0.045 Uiso 1 1 calc R
C71 C 0.6465(4) 0.66967(17) -0.06668(16) 0.0188(9) Uani 1 1 d .
C72 C 0.6004(4) 0.65464(18) -0.12326(16) 0.0180(9) Uani 1 1 d .
C73 C 0.6032(4) 0.59070(18) -0.13208(15) 0.0179(9) Uani 1 1 d .
C74 C 0.5679(4) 0.55742(17) -0.08317(15) 0.0171(9) Uani 1 1 d .
C75 C 0.8509(4) 0.80389(17) -0.06378(17) 0.0181(9) Uani 1 1 d .
C76 C 0.7724(4) 0.84131(18) -0.10428(17) 0.0210(9) Uani 1 1 d .
C77 C 0.7241(4) 0.89499(18) -0.08084(16) 0.0206(9) Uani 1 1 d .
C78 C 0.8262(4) 0.93436(18) -0.05302(16) 0.0199(9) Uani 1 1 d .
C79 C 1.4024(4) 0.67176(18) 0.08713(16) 0.0196(9) Uani 1 1 d .
C80 C 1.3270(4) 0.66136(18) 0.13684(16) 0.0202(9) Uani 1 1 d .
C81 C 1.1876(4) 0.64230(18) 0.12530(16) 0.0196(9) Uani 1 1 d .
C82 C 1.1119(4) 0.67777(17) 0.08335(16) 0.0177(9) Uani 1 1 d .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ag1 0.02617(19) 0.01164(16) 0.02811(17) 0.00267(12) -0.00558(13) -0.00074(12)
Ag2 0.02462(19) 0.01252(16) 0.02408(16) -0.00213(11) -0.00225(12) 0.00241(12)
Ag3 0.02687(19) 0.01451(16) 0.01579(14) -0.00181(11) 0.00305(11) -0.00210(12)
Ag4 0.02470(19) 0.01917(17) 0.02265(16) -0.00385(12) 0.00818(12) -0.00536(12)
Ag5 0.02758(19) 0.01309(15) 0.01600(14) -0.00034(11) 0.00433(11) 0.00194(12)
Ag6 0.02554(19) 0.01708(16) 0.01741(14) 0.00080(11) 0.00374(11) 0.00308(12)
S1 0.0222(6) 0.0142(5) 0.0189(5) 0.0002(4) 0.0038(4) 0.0016(4)
S2 0.0229(6) 0.0117(5) 0.0183(5) -0.0017(4) 0.0043(4) -0.0018(4)
S3 0.0214(6) 0.0118(5) 0.0256(5) -0.0021(4) 0.0049(4) 0.0020(4)
S4 0.0226(6) 0.0118(5) 0.0158(4) -0.0006(4) 0.0037(4) 0.0012(4)
S5 0.0216(6) 0.0134(5) 0.0165(4) -0.0012(4) 0.0057(4) -0.0009(4)
S6 0.0318(7) 0.0160(5) 0.0252(5) 0.0008(4) 0.0087(4) -0.0007(4)
F1 0.0368(17) 0.0239(14) 0.0167(12) 0.0049(10) 0.0092(11) -0.0038(11)
F2 0.0243(15) 0.0276(14) 0.0203(12) 0.0024(10) -0.0014(10) 0.0064(11)
F3 0.0296(16) 0.0247(15) 0.0259(13) -0.0020(11) 0.0139(11) 0.0000(11)
F4 0.0384(17) 0.0278(15) 0.0138(12) -0.0012(10) -0.0006(10) -0.0075(12)
F5 0.0297(16) 0.0195(14) 0.0320(14) -0.0041(11) -0.0083(11) -0.0022(11)
F6 0.0404(17) 0.0233(14) 0.0159(12) 0.0012(10) 0.0096(11) 0.0059(11)
F7 0.0231(15) 0.0298(15) 0.0267(13) 0.0040(11) 0.0082(10) -0.0015(11)
F8 0.0363(17) 0.0168(13) 0.0246(13) 0.0023(10) -0.0072(11) 0.0053(11)
F9 0.0304(16) 0.0340(16) 0.0177(12) 0.0066(11) 0.0094(10) 0.0011(12)
F10 0.0399(17) 0.0125(13) 0.0309(14) 0.0042(11) 0.0025(12) -0.0002(11)
F11 0.0314(16) 0.0266(15) 0.0162(12) -0.0059(10) 0.0038(10) -0.0001(11)
F12 0.0344(17) 0.0327(16) 0.0232(13) 0.0099(11) 0.0002(11) 0.0103(12)
O1 0.0244(18) 0.0137(15) 0.0213(15) 0.0023(12) 0.0001(12) 0.0003(12)
O2 0.0275(19) 0.0218(16) 0.0149(14) 0.0001(12) 0.0043(12) 0.0031(13)
O3 0.0287(19) 0.0183(17) 0.0257(16) 0.0032(13) 0.0052(13) -0.0021(13)
O4 0.0228(18) 0.0224(17) 0.0161(14) 0.0019(12) 0.0064(12) 0.0007(12)
O5 0.045(2) 0.0232(18) 0.0225(16) -0.0034(13) -0.0105(14) 0.0140(15)
O6 0.044(2) 0.0137(16) 0.0294(17) -0.0003(13) -0.0051(14) 0.0041(14)
O7 0.034(2) 0.0237(18) 0.0236(16) -0.0062(13) 0.0043(13) 0.0030(14)
O8 0.033(2) 0.0243(18) 0.0344(18) -0.0048(14) 0.0119(15) -0.0099(14)
O9 0.0228(18) 0.0153(16) 0.0212(15) 0.0016(12) 0.0033(12) 0.0005(12)
O10 0.0259(19) 0.0181(16) 0.0238(15) 0.0048(12) 0.0004(13) -0.0077(13)
O11 0.035(2) 0.0158(16) 0.0155(14) 0.0014(12) 0.0047(12) 0.0085(13)
O12 0.0243(19) 0.0275(18) 0.0274(17) -0.0002(14) 0.0063(13) -0.0014(14)
C11 0.025(3) 0.017(2) 0.0154(19) -0.0040(16) -0.0003(16) 0.0014(17)
C12 0.032(3) 0.037(3) 0.022(2) 0.005(2) 0.0056(19) 0.015(2)
C13 0.048(4) 0.061(4) 0.024(3) 0.008(3) 0.017(2) 0.016(3)
C14 0.052(4) 0.039(3) 0.015(2) 0.000(2) -0.001(2) 0.006(3)
C15 0.039(3) 0.032(3) 0.026(2) 0.004(2) -0.009(2) 0.000(2)
C16 0.023(3) 0.034(3) 0.028(2) 0.003(2) -0.0023(19) 0.001(2)
C17 0.020(2) 0.023(2) 0.0166(19) -0.0015(17) -0.0004(16) 0.0044(17)
C18 0.027(3) 0.019(2) 0.0161(19) -0.0007(16) 0.0007(16) -0.0049(18)
C19 0.029(3) 0.011(2) 0.0137(18) 0.0013(15) 0.0034(16) 0.0011(16)
C21 0.022(2) 0.018(2) 0.0148(19) -0.0034(16) 0.0043(16) -0.0033(17)
C22 0.027(3) 0.018(2) 0.021(2) -0.0027(17) 0.0040(17) -0.0022(18)
C23 0.031(3) 0.032(3) 0.018(2) 0.0036(19) 0.0058(18) 0.006(2)
C24 0.033(3) 0.044(3) 0.013(2) -0.003(2) 0.0022(18) -0.009(2)
C25 0.036(3) 0.030(3) 0.025(2) -0.007(2) 0.004(2) -0.010(2)
C26 0.037(3) 0.021(2) 0.022(2) -0.0024(18) 0.0037(19) -0.005(2)
C31 0.030(3) 0.014(2) 0.022(2) 0.0020(16) 0.0058(18) 0.0007(17)
C32 0.029(3) 0.025(3) 0.028(2) 0.0003(19) 0.0057(19) 0.000(2)
C33 0.045(3) 0.030(3) 0.028(3) 0.004(2) -0.002(2) 0.002(2)
C34 0.056(4) 0.039(3) 0.026(3) 0.006(2) 0.010(2) 0.006(3)
C35 0.038(4) 0.047(3) 0.037(3) 0.006(2) 0.021(2) 0.001(2)
C36 0.028(3) 0.029(3) 0.036(3) 0.005(2) 0.011(2) 0.000(2)
C37 0.031(3) 0.009(2) 0.023(2) -0.0009(16) 0.0091(18) 0.0017(17)
C38 0.024(3) 0.012(2) 0.023(2) 0.0010(16) 0.0077(17) 0.0002(17)
C39 0.019(2) 0.014(2) 0.0182(19) 0.0007(16) 0.0061(16) 0.0048(16)
C41 0.028(3) 0.014(2) 0.0106(18) -0.0007(15) 0.0028(16) 0.0003(17)
C42 0.035(3) 0.019(2) 0.023(2) 0.0027(18) -0.0004(19) -0.0065(19)
C43 0.046(3) 0.033(3) 0.024(2) 0.001(2) -0.009(2) -0.011(2)
C44 0.055(4) 0.045(3) 0.017(2) 0.001(2) -0.002(2) -0.007(3)
C45 0.044(4) 0.054(4) 0.022(2) 0.009(2) 0.009(2) -0.014(3)
C46 0.034(3) 0.026(3) 0.019(2) -0.0008(18) 0.0024(18) -0.004(2)
C51 0.036(3) 0.010(2) 0.0159(19) -0.0009(15) 0.0050(17) -0.0028(17)
C52 0.037(3) 0.016(2) 0.023(2) -0.0012(17) 0.0044(19) 0.0000(19)
C53 0.051(4) 0.024(3) 0.026(2) -0.003(2) -0.011(2) 0.002(2)
C54 0.066(4) 0.025(3) 0.019(2) 0.006(2) 0.004(2) -0.002(2)
C55 0.057(4) 0.033(3) 0.027(3) 0.003(2) 0.018(2) -0.005(2)
C56 0.036(3) 0.022(3) 0.029(2) 0.0013(19) 0.011(2) -0.003(2)
C57 0.017(2) 0.016(2) 0.020(2) 0.0020(16) 0.0032(16) 0.0040(16)
C58 0.027(3) 0.012(2) 0.029(2) -0.0007(17) 0.0075(18) -0.0027(17)
C59 0.024(3) 0.017(2) 0.027(2) -0.0019(18) 0.0076(18) -0.0058(18)
C61 0.040(3) 0.013(2) 0.025(2) -0.0049(17) 0.014(2) -0.0072(18)
C62 0.045(4) 0.027(3) 0.031(3) -0.001(2) 0.009(2) -0.001(2)
C63 0.057(4) 0.035(3) 0.038(3) 0.001(2) -0.002(3) -0.004(3)
C64 0.073(5) 0.027(3) 0.029(3) 0.000(2) 0.008(3) -0.009(3)
C65 0.065(5) 0.038(3) 0.035(3) -0.009(2) 0.029(3) -0.008(3)
C66 0.044(4) 0.035(3) 0.036(3) -0.010(2) 0.017(2) -0.006(2)
C71 0.030(3) 0.011(2) 0.0156(19) 0.0028(16) 0.0044(17) -0.0037(17)
C72 0.021(2) 0.020(2) 0.0145(19) 0.0025(16) 0.0068(16) 0.0023(17)
C73 0.021(2) 0.021(2) 0.0120(18) -0.0005(16) 0.0026(15) -0.0001(17)
C74 0.019(2) 0.019(2) 0.0137(18) 0.0025(16) 0.0010(15) -0.0104(17)
C75 0.017(2) 0.015(2) 0.022(2) 0.0029(16) 0.0024(16) -0.0017(16)
C76 0.024(3) 0.020(2) 0.019(2) 0.0015(17) -0.0004(17) -0.0051(18)
C77 0.025(3) 0.018(2) 0.019(2) 0.0034(17) 0.0017(17) 0.0008(17)
C78 0.027(3) 0.012(2) 0.021(2) 0.0031(16) 0.0025(17) 0.0060(17)
C79 0.021(3) 0.023(2) 0.0152(19) 0.0031(17) 0.0029(16) 0.0109(18)
C80 0.026(3) 0.019(2) 0.016(2) 0.0023(16) 0.0037(16) 0.0056(18)
C81 0.026(3) 0.016(2) 0.017(2) 0.0024(16) 0.0063(17) 0.0017(17)
C82 0.023(3) 0.013(2) 0.0172(19) -0.0005(16) 0.0078(16) 0.0033(17)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag 0.1306 4.2820 '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
O9 Ag1 O5 . . 157.15(11) y
O9 Ag1 S2 . . 109.86(8) y
O5 Ag1 S2 . . 89.69(9) y
O9 Ag1 S5 . . 100.20(8) y
O5 Ag1 S5 . . 81.6(1) y
S2 Ag1 S5 . . 113.76(3) y
O9 Ag1 Ag2 . . 78.23(7) y
O5 Ag1 Ag2 . . 79.53(8) y
S2 Ag1 Ag2 . . 159.95(3) y
S5 Ag1 Ag2 . . 81.57(2) y
O6 Ag2 O10 . . 154.76(11) y
O6 Ag2 O1 . . 81.64(11) y
O10 Ag2 O1 . . 110.29(10) y
O6 Ag2 S3 . 1_655 113.95(9) y
O10 Ag2 S3 . 1_655 85.31(8) y
O1 Ag2 S3 . 1_655 104.53(7) y
O6 Ag2 Ag1 . . 80.46(8) y
O10 Ag2 Ag1 . . 76.13(7) y
O1 Ag2 Ag1 . . 138.89(7) y
S3 Ag2 Ag1 1_655 . 116.55(3) y
O6 Ag2 Ag3 . . 92.71(9) y
O10 Ag2 Ag3 . . 77.01(8) y
O1 Ag2 Ag3 . . 56.92(7) y
S3 Ag2 Ag3 1_655 . 145.97(3) y
Ag1 Ag2 Ag3 . . 87.326(12) y
O2 Ag3 S5 . . 122.77(8) y
O2 Ag3 O12 . 1_455 95.52(11) y
S5 Ag3 O12 . 1_455 95.54(8) y
O2 Ag3 S4 . 3_665 107.64(8) y
S5 Ag3 S4 . 3_665 127.30(4) y
O12 Ag3 S4 1_455 3_665 93.86(8) y
O2 Ag3 Ag2 . . 82.60(7) y
S5 Ag3 Ag2 . . 79.92(3) y
O12 Ag3 Ag2 1_455 . 172.95(8) y
S4 Ag3 Ag2 3_665 . 93.18(3) y
O8 Ag4 O7 3_775 . 136.08(12) y
O8 Ag4 S6 3_775 . 97.24(9) y
O7 Ag4 S6 . . 78.43(8) y
O8 Ag4 S2 3_775 . 110.26(9) y
O7 Ag4 S2 . . 104.23(8) y
S6 Ag4 S2 . . 131.70(3) y
O8 Ag4 Ag4 3_775 3_775 79.21(8) y
O7 Ag4 Ag4 . 3_775 69.66(8) y
S6 Ag4 Ag4 . 3_775 126.37(3) y
S2 Ag4 Ag4 . 3_775 98.00(3) y
O3 Ag5 O4 . 3_665 138.92(11) y
O3 Ag5 O11 . 3_765 103.96(11) y
O4 Ag5 O11 3_665 3_765 90.92(10) y
O3 Ag5 S4 . . 118.16(9) y
O4 Ag5 S4 3_665 . 99.19(8) y
O11 Ag5 S4 3_765 . 91.22(8) y
O3 Ag5 Ag5 . 3_665 77.51(8) y
O4 Ag5 Ag5 3_665 3_665 75.89(7) y
O11 Ag5 Ag5 3_765 3_665 159.25(7) y
S4 Ag5 Ag5 . 3_665 106.47(3) y
O11 Ag6 O2 . 1_655 98.67(10) y
O11 Ag6 S1 . . 113.80(7) y
O2 Ag6 S1 1_655 . 102.36(7) y
O11 Ag6 S3 . 1_655 89.88(8) y
O2 Ag6 S3 1_655 1_655 158.89(7) y
S1 Ag6 S3 . 1_655 91.60(3) y
C11 S1 C17 . . 103.7(2) y
C11 S1 Ag6 . . 107.55(14) y
C17 S1 Ag6 . . 98.88(14) y
C21 S2 C19 . . 103.4(2) y
C21 S2 Ag1 . . 114.40(14) y
C19 S2 Ag1 . . 104.64(14) y
C21 S2 Ag4 . . 112.08(14) y
C19 S2 Ag4 . . 100.04(13) y
Ag1 S2 Ag4 . . 119.41(4) y
C31 S3 C37 . . 102.7(2) y
C31 S3 Ag2 . 1_455 107.94(15) y
C37 S3 Ag2 . 1_455 109.88(15) y
C31 S3 Ag6 . 1_455 104.62(16) y
C37 S3 Ag6 . 1_455 122.48(16) y
Ag2 S3 Ag6 1_455 1_455 108.19(4) y
C41 S4 C39 . . 102.7(2) y
C41 S4 Ag3 . 3_665 108.38(14) y
C39 S4 Ag3 . 3_665 120.44(14) y
C41 S4 Ag5 . . 112.48(15) y
C39 S4 Ag5 . . 109.43(14) y
Ag3 S4 Ag5 3_665 . 103.65(4) y
C51 S5 C57 . . 103.0(2) y
C51 S5 Ag3 . . 110.31(14) y
C57 S5 Ag3 . . 104.01(14) y
C51 S5 Ag1 . . 117.80(16) y
C57 S5 Ag1 . . 110.17(14) y
Ag3 S5 Ag1 . . 110.44(4) y
C61 S6 C59 . . 103.4(2) y
C61 S6 Ag4 . . 109.68(17) y
C59 S6 Ag4 . . 99.99(15) y
C71 O1 Ag2 . . 124.1(3) y
C71 O2 Ag3 . . 101.2(3) y
C71 O2 Ag6 . 1_455 116.2(3) y
Ag3 O2 Ag6 . 1_455 105.85(11) y
C74 O3 Ag5 . . 117.3(3) y
C74 O4 Ag5 . 3_665 115.4(3) y
C75 O5 Ag1 . . 122.3(3) y
C75 O6 Ag2 . . 121.2(3) y
C78 O7 Ag4 . . 121.8(3) y
C78 O8 Ag4 . 3_775 114.0(3) y
C82 O9 Ag1 . . 117.6(3) y
C82 O10 Ag2 . . 116.3(3) y
C79 O11 Ag6 . . 115.7(3) y
C79 O11 Ag5 . 3_765 126.8(3) y
Ag6 O11 Ag5 . 3_765 98.17(10) y
C79 O12 Ag3 . 1_655 117.7(3) y
C16 C11 C12 . . 120.6(4) y
C16 C11 S1 . . 118.1(4) y
C12 C11 S1 . . 121.3(3) y
C13 C12 C11 . . 118.9(5) y
C13 C12 H12 . . 120.6 ?
C11 C12 H12 . . 120.6 ?
C12 C13 C14 . . 121.5(5) y
C12 C13 H13 . . 119.3 ?
C14 C13 H13 . . 119.3 ?
C13 C14 C15 . . 119.5(5) y
C13 C14 H14 . . 120.3 ?
C15 C14 H14 . . 120.3 ?
C14 C15 C16 . . 120.0(5) y
C14 C15 H15 . . 120 ?
C16 C15 H15 . . 120 ?
C11 C16 C15 . . 119.6(5) y
C11 C16 H16 . . 120.2 ?
C15 C16 H16 . . 120.2 ?
C18 C17 S1 . . 115.0(3) y
C18 C17 H17A . . 108.5 ?
S1 C17 H17A . . 108.5 ?
C18 C17 H17B . . 108.5 ?
S1 C17 H17B . . 108.5 ?
H17A C17 H17B . . 107.5 ?
C19 C18 C17 . . 119.2(4) y
C19 C18 H18A . . 107.5 ?
C17 C18 H18A . . 107.5 ?
C19 C18 H18B . . 107.5 ?
C17 C18 H18B . . 107.5 ?
H18A C18 H18B . . 107 ?
C18 C19 S2 . . 118.0(3) y
C18 C19 H19A . . 107.8 ?
S2 C19 H19A . . 107.8 ?
C18 C19 H19B . . 107.8 ?
S2 C19 H19B . . 107.8 ?
H19A C19 H19B . . 107.2 ?
C22 C21 C26 . . 121.9(4) y
C22 C21 S2 . . 119.9(3) y
C26 C21 S2 . . 118.2(3) y
C21 C22 C23 . . 118.7(4) y
C21 C22 H22 . . 120.7 ?
C23 C22 H22 . . 120.7 ?
C24 C23 C22 . . 120.5(4) y
C24 C23 H23 . . 119.7 ?
C22 C23 H23 . . 119.7 ?
C23 C24 C25 . . 119.4(4) y
C23 C24 H24 . . 120.3 ?
C25 C24 H24 . . 120.3 ?
C26 C25 C24 . . 120.7(4) y
C26 C25 H25 . . 119.6 ?
C24 C25 H25 . . 119.6 ?
C25 C26 C21 . . 118.7(4) y
C25 C26 H26 . . 120.6 ?
C21 C26 H26 . . 120.6 ?
C36 C31 C32 . . 121.3(4) y
C36 C31 S3 . . 119.1(4) y
C32 C31 S3 . . 119.6(3) y
C33 C32 C31 . . 119.0(5) y
C33 C32 H32 . . 120.5 ?
C31 C32 H32 . . 120.5 ?
C32 C33 C34 . . 119.2(5) y
C32 C33 H33 . . 120.4 ?
C34 C33 H33 . . 120.4 ?
C35 C34 C33 . . 120.9(5) y
C35 C34 H34 . . 119.5 ?
C33 C34 H34 . . 119.5 ?
C34 C35 C36 . . 120.7(5) y
C34 C35 H35 . . 119.7 ?
C36 C35 H35 . . 119.7 ?
C31 C36 C35 . . 118.9(5) y
C31 C36 H36 . . 120.6 ?
C35 C36 H36 . . 120.6 ?
C38 C37 S3 . . 112.3(3) y
C38 C37 H37A . . 109.1 ?
S3 C37 H37A . . 109.1 ?
C38 C37 H37B . . 109.1 ?
S3 C37 H37B . . 109.1 ?
H37A C37 H37B . . 107.9 ?
C37 C38 C39 . . 112.7(3) y
C37 C38 H38A . . 109 ?
C39 C38 H38A . . 109 ?
C37 C38 H38B . . 109 ?
C39 C38 H38B . . 109 ?
H38A C38 H38B . . 107.8 ?
C38 C39 S4 . . 110.3(3) y
C38 C39 H39A . . 109.6 ?
S4 C39 H39A . . 109.6 ?
C38 C39 H39B . . 109.6 ?
S4 C39 H39B . . 109.6 ?
H39A C39 H39B . . 108.1 ?
C42 C41 C46 . . 121.5(4) y
C42 C41 S4 . . 119.4(3) y
C46 C41 S4 . . 119.0(3) y
C41 C42 C43 . . 118.4(4) y
C41 C42 H42 . . 120.8 ?
C43 C42 H42 . . 120.8 ?
C44 C43 C42 . . 120.5(5) y
C44 C43 H43 . . 119.7 ?
C42 C43 H43 . . 119.7 ?
C45 C44 C43 . . 120.2(5) y
C45 C44 H44 . . 119.9 ?
C43 C44 H44 . . 119.9 ?
C44 C45 C46 . . 120.7(5) y
C44 C45 H45 . . 119.7 ?
C46 C45 H45 . . 119.7 ?
C45 C46 C41 . . 118.7(5) y
C45 C46 H46 . . 120.7 ?
C41 C46 H46 . . 120.7 ?
C56 C51 C52 . . 121.5(4) y
C56 C51 S5 . . 120.7(4) y
C52 C51 S5 . . 117.8(3) y
C53 C52 C51 . . 118.2(5) y
C53 C52 H52 . . 120.9 ?
C51 C52 H52 . . 120.9 ?
C54 C53 C52 . . 120.9(5) y
C54 C53 H53 . . 119.5 ?
C52 C53 H53 . . 119.5 ?
C53 C54 C55 . . 119.9(5) y
C53 C54 H54 . . 120.1 ?
C55 C54 H54 . . 120.1 ?
C54 C55 C56 . . 121.2(5) y
C54 C55 H55 . . 119.4 ?
C56 C55 H55 . . 119.4 ?
C55 C56 C51 . . 118.3(5) y
C55 C56 H56 . . 120.9 ?
C51 C56 H56 . . 120.9 ?
C58 C57 S5 . . 111.3(3) y
C58 C57 H57A . . 109.4 ?
S5 C57 H57A . . 109.4 ?
C58 C57 H57B . . 109.4 ?
S5 C57 H57B . . 109.4 ?
H57A C57 H57B . . 108 ?
C57 C58 C59 . . 110.6(4) y
C57 C58 H58A . . 109.5 ?
C59 C58 H58A . . 109.5 ?
C57 C58 H58B . . 109.5 ?
C59 C58 H58B . . 109.5 ?
H58A C58 H58B . . 108.1 ?
C58 C59 S6 . . 113.2(3) y
C58 C59 H59A . . 108.9 ?
S6 C59 H59A . . 108.9 ?
C58 C59 H59B . . 108.9 ?
S6 C59 H59B . . 108.9 ?
H59A C59 H59B . . 107.7 ?
C62 C61 C66 . . 119.6(5) y
C62 C61 S6 . . 119.8(4) y
C66 C61 S6 . . 120.4(4) y
C61 C62 C63 . . 119.3(5) y
C61 C62 H62 . . 120.3 ?
C63 C62 H62 . . 120.3 ?
C64 C63 C62 . . 120.1(6) y
C64 C63 H63 . . 120 ?
C62 C63 H63 . . 120 ?
C65 C64 C63 . . 120.8(5) y
C65 C64 H64 . . 119.6 ?
C63 C64 H64 . . 119.6 ?
C64 C65 C66 . . 119.3(5) y
C64 C65 H65 . . 120.4 ?
C66 C65 H65 . . 120.4 ?
C61 C66 C65 . . 120.9(6) y
C61 C66 H66 . . 119.5 ?
C65 C66 H66 . . 119.5 ?
O1 C71 O2 . . 128.0(4) y
O1 C71 C72 . . 112.8(4) y
O2 C71 C72 . . 119.2(4) y
F2 C72 F1 . . 106.2(3) y
F2 C72 C71 . . 111.8(3) y
F1 C72 C71 . . 110.2(3) y
F2 C72 C73 . . 108.6(3) y
F1 C72 C73 . . 108.7(3) y
C71 C72 C73 . . 111.2(3) y
F3 C73 F4 . . 106.5(3) y
F3 C73 C74 . . 111.2(3) y
F4 C73 C74 . . 108.1(3) y
F3 C73 C72 . . 109.3(3) y
F4 C73 C72 . . 108.9(3) y
C74 C73 C72 . . 112.6(3) y
O3 C74 O4 . . 129.9(4) y
O3 C74 C73 . . 116.6(4) y
O4 C74 C73 . . 113.6(4) y
O6 C75 O5 . . 130.6(4) y
O6 C75 C76 . . 115.5(4) y
O5 C75 C76 . . 113.8(4) y
F5 C76 F6 . . 105.5(3) y
F5 C76 C77 . . 109.3(4) y
F6 C76 C77 . . 108.7(3) y
F5 C76 C75 . . 110.5(3) y
F6 C76 C75 . . 109.1(4) y
C77 C76 C75 . . 113.4(3) y
F7 C77 F8 . . 106.5(4) y
F7 C77 C76 . . 106.2(3) y
F8 C77 C76 . . 107.6(3) y
F7 C77 C78 . . 110.9(3) y
F8 C77 C78 . . 107.8(3) y
C76 C77 C78 . . 117.3(4) y
O7 C78 O8 . . 129.4(4) y
O7 C78 C77 . . 117.1(4) y
O8 C78 C77 . . 113.4(4) y
O12 C79 O11 . . 130.3(4) y
O12 C79 C80 . . 117.4(4) y
O11 C79 C80 . . 112.4(4) y
F11 C80 F12 . . 106.1(3) y
F11 C80 C81 . . 108.9(3) y
F12 C80 C81 . . 108.0(4) y
F11 C80 C79 . . 110.6(4) y
F12 C80 C79 . . 108.4(3) y
C81 C80 C79 . . 114.5(3) y
F10 C81 F9 . . 106.4(3) y
F10 C81 C80 . . 109.5(4) y
F9 C81 C80 . . 108.1(3) y
F10 C81 C82 . . 111.0(3) y
F9 C81 C82 . . 107.8(3) y
C80 C81 C82 . . 113.8(3) y
O10 C82 O9 . . 129.2(4) y
O10 C82 C81 . . 116.2(4) y
O9 C82 C81 . . 114.6(4) y
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
Ag1 O9 . 2.256(3) y
Ag1 O5 . 2.271(3) y
Ag1 S2 . 2.5912(10) y
Ag1 S5 . 2.7768(11) y
Ag1 Ag2 . 2.9474(4) y
Ag2 O6 . 2.271(3) y
Ag2 O10 . 2.325(3) y
Ag2 O1 . 2.420(3) y
Ag2 S3 1_655 2.6355(11) y
Ag2 Ag3 . 3.2807(5) y
Ag3 O2 . 2.365(3) y
Ag3 S5 . 2.4622(10) y
Ag3 O12 1_455 2.474(3) y
Ag3 S4 3_665 2.5623(10) y
Ag4 O8 3_775 2.309(3) y
Ag4 O7 . 2.377(3) y
Ag4 S6 . 2.6194(12) y
Ag4 S2 . 2.6578(11) y
Ag4 Ag4 3_775 3.1392(6) y
Ag5 O3 . 2.248(3) y
Ag5 O4 3_665 2.330(3) y
Ag5 O11 3_765 2.434(3) y
Ag5 S4 . 2.5666(11) y
Ag5 Ag5 3_665 2.9590(6) y
Ag6 O11 . 2.362(3) y
Ag6 O2 1_655 2.494(3) y
Ag6 S1 . 2.5859(10) y
Ag6 S3 1_655 2.6829(11) y
S1 C11 . 1.791(4) y
S1 C17 . 1.826(4) y
S2 C21 . 1.792(4) y
S2 C19 . 1.831(4) y
S3 C31 . 1.783(4) y
S3 C37 . 1.832(4) y
S3 Ag2 1_455 2.6355(11) y
S3 Ag6 1_455 2.6829(11) y
S4 C41 . 1.786(4) y
S4 C39 . 1.824(4) y
S4 Ag3 3_665 2.5623(10) y
S5 C51 . 1.790(4) y
S5 C57 . 1.827(4) y
S6 C61 . 1.781(5) y
S6 C59 . 1.826(4) y
F1 C72 . 1.362(5) y
F2 C72 . 1.357(5) y
F3 C73 . 1.343(5) y
F4 C73 . 1.378(5) y
F5 C76 . 1.342(5) y
F6 C76 . 1.372(5) y
F7 C77 . 1.363(5) y
F8 C77 . 1.371(5) y
F9 C81 . 1.373(5) y
F10 C81 . 1.351(5) y
F11 C80 . 1.356(5) y
F12 C80 . 1.364(5) y
O1 C71 . 1.243(5) y
O2 C71 . 1.247(5) y
O2 Ag6 1_455 2.494(3) y
O3 C74 . 1.236(5) y
O4 C74 . 1.258(5) y
O4 Ag5 3_665 2.330(3) y
O5 C75 . 1.242(5) y
O6 C75 . 1.227(5) y
O7 C78 . 1.233(5) y
O8 C78 . 1.247(5) y
O8 Ag4 3_775 2.309(3) y
O9 C82 . 1.252(5) y
O10 C82 . 1.250(5) y
O11 C79 . 1.267(5) y
O11 Ag5 3_765 2.434(3) y
O12 C79 . 1.223(6) y
O12 Ag3 1_655 2.474(3) y
C11 C16 . 1.380(6) y
C11 C12 . 1.389(6) y
C12 C13 . 1.375(6) y
C12 H12 . 0.95 ?
C13 C14 . 1.375(8) y
C13 H13 . 0.95 ?
C14 C15 . 1.384(8) y
C14 H14 . 0.95 ?
C15 C16 . 1.391(7) y
C15 H15 . 0.95 ?
C16 H16 . 0.95 ?
C17 C18 . 1.527(6) y
C17 H17A . 0.99 ?
C17 H17B . 0.99 ?
C18 C19 . 1.521(6) y
C18 H18A . 0.99 ?
C18 H18B . 0.99 ?
C19 H19A . 0.99 ?
C19 H19B . 0.99 ?
C21 C22 . 1.380(6) y
C21 C26 . 1.394(6) y
C22 C23 . 1.398(6) y
C22 H22 . 0.95 ?
C23 C24 . 1.394(7) y
C23 H23 . 0.95 ?
C24 C25 . 1.395(7) y
C24 H24 . 0.95 ?
C25 C26 . 1.386(7) y
C25 H25 . 0.95 ?
C26 H26 . 0.95 ?
C31 C36 . 1.373(6) y
C31 C32 . 1.385(7) y
C32 C33 . 1.384(7) y
C32 H32 . 0.95 ?
C33 C34 . 1.395(8) y
C33 H33 . 0.95 ?
C34 C35 . 1.345(8) y
C34 H34 . 0.95 ?
C35 C36 . 1.388(7) y
C35 H35 . 0.95 ?
C36 H36 . 0.95 ?
C37 C38 . 1.523(6) y
C37 H37A . 0.99 ?
C37 H37B . 0.99 ?
C38 C39 . 1.525(5) y
C38 H38A . 0.99 ?
C38 H38B . 0.99 ?
C39 H39A . 0.99 ?
C39 H39B . 0.99 ?
C41 C42 . 1.380(6) y
C41 C46 . 1.392(6) y
C42 C43 . 1.397(6) y
C42 H42 . 0.95 ?
C43 C44 . 1.376(7) y
C43 H43 . 0.95 ?
C44 C45 . 1.376(7) y
C44 H44 . 0.95 ?
C45 C46 . 1.382(6) y
C45 H45 . 0.95 ?
C46 H46 . 0.95 ?
C51 C56 . 1.389(6) y
C51 C52 . 1.390(6) y
C52 C53 . 1.386(6) y
C52 H52 . 0.95 ?
C53 C54 . 1.373(8) y
C53 H53 . 0.95 ?
C54 C55 . 1.374(8) y
C54 H54 . 0.95 ?
C55 C56 . 1.379(7) y
C55 H55 . 0.95 ?
C56 H56 . 0.95 ?
C57 C58 . 1.520(6) y
C57 H57A . 0.99 ?
C57 H57B . 0.99 ?
C58 C59 . 1.532(6) y
C58 H58A . 0.99 ?
C58 H58B . 0.99 ?
C59 H59A . 0.99 ?
C59 H59B . 0.99 ?
C61 C62 . 1.380(7) y
C61 C66 . 1.382(7) y
C62 C63 . 1.404(7) y
C62 H62 . 0.95 ?
C63 C64 . 1.374(8) y
C63 H63 . 0.95 ?
C64 C65 . 1.368(9) y
C64 H64 . 0.95 ?
C65 C66 . 1.390(8) y
C65 H65 . 0.95 ?
C66 H66 . 0.95 ?
C71 C72 . 1.538(5) y
C72 C73 . 1.551(6) y
C73 C74 . 1.551(5) y
C75 C76 . 1.561(6) y
C76 C77 . 1.521(6) y
C77 C78 . 1.560(6) y
C79 C80 . 1.561(6) y
C80 C81 . 1.535(6) y
C81 C82 . 1.545(6) y
|
1501562.cif | #------------------------------------------------------------------------------
#$Date: 2020-10-02 18:49:34 +0300 (Fri, 02 Oct 2020) $
#$Revision: 256944 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/50/15/1501562.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_1501562
loop_
_publ_author_name
'Mohamed Osman Awaleh'
'Francois Brisse'
'Youssouf Djibril Soubaneh'
'Thierry Maris'
'Elias Said Dirieh'
_publ_section_title
;
Four New Ag(I) Coordination Polymers: Synthesis, Crystal Structures and
Thermal Stability
;
_journal_name_full 'J. Inorg. Organomet. Polym.'
_journal_page_first 816
_journal_page_last 824
_journal_paper_doi 10.1007/s10904-010-9407-0
_journal_volume 20
_journal_year 2010
_chemical_compound_source 'Synthesized by the authors. See text'
_chemical_formula_moiety 'C35 H32 Ag5 F15 O15 S9, 2(C3 H6 O)'
_chemical_formula_sum 'C41 H44 Ag5 F15 O17 S9'
_chemical_formula_weight 1921.65
_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
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 104.5950(10)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 17.4256(2)
_cell_length_b 24.3524(3)
_cell_length_c 14.9472(2)
_cell_measurement_reflns_used 8079
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 72.80
_cell_measurement_theta_min 2.62
_cell_volume 6138.24(13)
_computing_cell_refinement 'SMART (Bruker, 1999)'
_computing_data_collection 'SMART (Bruker, 1999)'
_computing_data_reduction 'SAINT (Bruker, 1999)'
_computing_molecular_graphics 'SHELXTL (Bruker, 1997)'
_computing_publication_material 'UdMX (local program)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type 'Bruker Smart 2000'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'Sealed Tube'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.052
_diffrn_reflns_av_sigmaI/netI 0.0622
_diffrn_reflns_limit_h_max 21
_diffrn_reflns_limit_h_min -21
_diffrn_reflns_limit_k_max 29
_diffrn_reflns_limit_k_min -29
_diffrn_reflns_limit_l_max 14
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_number 74657
_diffrn_reflns_theta_full 72.98
_diffrn_reflns_theta_max 72.98
_diffrn_reflns_theta_min 2.62
_diffrn_standards_decay_% -0.07
_diffrn_standards_number 430
_exptl_absorpt_coefficient_mu 16.427
_exptl_absorpt_correction_T_max 0.518
_exptl_absorpt_correction_T_min 0.202
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Sadabs (Sheldrick,1996)'
_exptl_crystal_colour Colourless
_exptl_crystal_density_diffrn 2.079
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description Platelet
_exptl_crystal_F_000 3760
_exptl_crystal_size_max 0.34
_exptl_crystal_size_mid 0.10
_exptl_crystal_size_min 0.04
_refine_diff_density_max 1.597
_refine_diff_density_min -1.223
_refine_diff_density_rms 0.215
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.820
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 788
_refine_ls_number_reflns 11903
_refine_ls_number_restraints 7
_refine_ls_restrained_S_all 0.822
_refine_ls_R_factor_all 0.0614
_refine_ls_R_factor_gt 0.0421
_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^)+(0.0699P)^2^+51.5879P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0984
_refine_ls_wR_factor_ref 0.1199
_reflns_number_gt 9045
_reflns_number_total 11903
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file deposit.cif
_cod_data_source_block Complex2
_cod_depositor_comments
;
Updated values of the _geom_angle_atom_site_label_*,
_geom_bond_atom_site_label_* and _geom_torsion_atom_site_label_*
data items to establish relationships between loop packets from
different data loops.
Antanas Vaitkus,
2020-10-02
;
_cod_original_sg_symbol_H-M P21/c
_cod_database_code 1501562
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
Ag1 Ag 0.31612(3) 0.728744(17) 0.33461(3) 0.01858(11) Uani 1 1 d .
Ag2 Ag 0.48241(2) 0.748354(16) 0.20461(3) 0.01612(10) Uani 1 1 d .
Ag3 Ag 0.65515(2) 0.748041(17) 0.07230(3) 0.01733(10) Uani 1 1 d .
Ag4 Ag 0.98513(3) 0.692712(18) 0.19160(3) 0.02101(11) Uani 1 1 d .
Ag5 Ag 0.97113(3) 0.75089(2) 0.44404(4) 0.02893(13) Uani 1 1 d .
S1 S 0.35030(8) 0.69902(5) 0.18719(10) 0.0125(3) Uani 1 1 d .
S2 S 0.61541(8) 0.71234(5) 0.21188(9) 0.0121(3) Uani 1 1 d .
S3 S 0.91460(7) 0.68775(5) 0.31481(9) 0.0114(3) Uani 1 1 d .
S5 S 0.49736(8) 0.80963(5) 0.41944(10) 0.0137(3) Uani 1 1 d D
S6 S 0.46295(8) 0.66310(5) 0.53197(10) 0.0163(3) Uani 1 1 d .
S7 S 0.81908(8) 0.66595(5) 0.00178(10) 0.0143(3) Uani 1 1 d .
S8 S 0.94035(9) 0.82821(6) 0.17600(11) 0.0223(3) Uani 1 1 d D
S9 S 0.15640(8) 0.66536(6) 0.39212(10) 0.0163(3) Uani 1 1 d .
F1 F 0.4877(3) 0.57040(16) 0.6231(3) 0.0436(12) Uani 1 1 d .
F2 F 0.3812(3) 0.57170(17) 0.5129(4) 0.0477(12) Uani 1 1 d .
F3 F 0.4943(3) 0.56454(16) 0.4824(3) 0.0413(11) Uani 1 1 d .
F4 F 0.5213(2) 0.89127(16) 0.3148(3) 0.0293(9) Uani 1 1 d .
F5 F 0.4347(2) 0.90753(15) 0.3927(3) 0.0317(9) Uani 1 1 d .
F6 F 0.5588(2) 0.90794(15) 0.4606(3) 0.0313(9) Uani 1 1 d .
F7 F 1.0915(3) 0.80415(19) 0.2343(3) 0.0472(12) Uani 1 1 d .
F8 F 1.0627(3) 0.8557(2) 0.1135(3) 0.0484(12) Uani 1 1 d .
F9 F 1.0646(3) 0.88945(17) 0.2449(3) 0.0401(11) Uani 1 1 d .
F10 F 0.1980(3) 0.58565(17) 0.5126(3) 0.0372(10) Uani 1 1 d .
F11 F 0.2100(2) 0.56649(15) 0.3764(3) 0.0334(9) Uani 1 1 d .
F12 F 0.0948(2) 0.56854(16) 0.4032(3) 0.0354(10) Uani 1 1 d .
F13 F 0.8058(2) 0.58530(15) -0.1162(3) 0.0299(9) Uani 1 1 d .
F14 F 0.7425(2) 0.57284(15) -0.0112(3) 0.0320(9) Uani 1 1 d .
F15 F 0.6968(2) 0.62887(14) -0.1245(2) 0.0223(8) Uani 1 1 d .
O1 O 0.2698(2) 0.81673(17) 0.3607(3) 0.0217(9) Uani 1 1 d .
O2 O 0.4266(3) 0.67495(18) 0.4363(3) 0.0280(10) Uani 1 1 d .
O3 O 0.4200(3) 0.68204(17) 0.5969(3) 0.0245(10) Uani 1 1 d .
O4 O 0.5475(3) 0.67296(18) 0.5602(3) 0.0288(11) Uani 1 1 d .
O5 O 0.4412(2) 0.79103(16) 0.3357(3) 0.0195(9) Uani 1 1 d .
O6 O 0.4691(2) 0.80771(16) 0.5019(3) 0.0193(9) Uani 1 1 d .
O7 O 0.5776(2) 0.79057(17) 0.4284(3) 0.0190(9) Uani 1 1 d .
O8 O 0.7089(3) 0.82776(17) 0.0279(3) 0.0226(9) Uani 1 1 d .
O9 O 0.9313(3) 0.78429(19) 0.1082(3) 0.0299(11) Uani 1 1 d .
O10 O 0.8991(3) 0.87924(19) 0.1419(3) 0.0303(11) Uani 1 1 d .
O11 O 0.9348(3) 0.8107(2) 0.2665(3) 0.0334(12) Uani 1 1 d .
O12 O 0.1054(3) 0.68697(18) 0.4453(3) 0.0255(10) Uani 1 1 d .
O13 O 0.1234(3) 0.66446(19) 0.2934(3) 0.0261(10) Uani 1 1 d .
O14 O 0.2375(2) 0.68433(18) 0.4201(3) 0.0231(9) Uani 1 1 d .
O15 O 0.8407(3) 0.69967(18) -0.0672(3) 0.0240(10) Uani 1 1 d .
O16 O 0.8844(2) 0.63763(17) 0.0630(3) 0.0216(9) Uani 1 1 d .
O17 O 0.7627(3) 0.68937(19) 0.0467(3) 0.0283(11) Uani 1 1 d .
C1 C 0.2778(5) 0.8609(3) 0.2215(5) 0.0356(17) Uani 1 1 d .
H1A H 0.2841 0.8234 0.2006 0.053 Uiso 1 1 calc R
H1B H 0.3256 0.8823 0.2222 0.053 Uiso 1 1 calc R
H1C H 0.2318 0.8781 0.1793 0.053 Uiso 1 1 calc R
C2 C 0.2653(3) 0.8592(2) 0.3164(4) 0.0188(12) Uani 1 1 d .
C3 C 0.2454(4) 0.9122(3) 0.3586(5) 0.0309(16) Uani 1 1 d .
H3A H 0.1957 0.9077 0.3771 0.046 Uiso 1 1 calc R
H3B H 0.2395 0.9418 0.3131 0.046 Uiso 1 1 calc R
H3C H 0.2882 0.9213 0.4130 0.046 Uiso 1 1 calc R
C4 C 0.5038(3) 0.8829(2) 0.3960(4) 0.0212(13) Uani 1 1 d D
C5 C 0.4558(4) 0.5881(2) 0.5387(4) 0.0234(14) Uani 1 1 d .
C6 C 0.7144(4) 0.8711(3) 0.0690(5) 0.0228(14) Uani 1 1 d .
C7 C 0.7152(4) 0.8750(3) 0.1685(5) 0.0329(16) Uani 1 1 d .
H7A H 0.7124 0.8380 0.1934 0.049 Uiso 1 1 calc R
H7B H 0.6694 0.8965 0.1752 0.049 Uiso 1 1 calc R
H7C H 0.7642 0.8930 0.2025 0.049 Uiso 1 1 calc R
C8 C 0.7220(4) 0.9242(3) 0.0200(5) 0.0318(16) Uani 1 1 d .
H8A H 0.7198 0.9166 -0.0450 0.048 Uiso 1 1 calc R
H8B H 0.7728 0.9417 0.0495 0.048 Uiso 1 1 calc R
H8C H 0.6785 0.9488 0.0237 0.048 Uiso 1 1 calc R
C9 C 0.7632(3) 0.6100(2) -0.0662(4) 0.0200(13) Uani 1 1 d .
C10 C 0.1653(4) 0.5926(2) 0.4234(4) 0.0200(13) Uani 1 1 d .
C11 C 0.3531(3) 0.6258(2) 0.1803(4) 0.0166(12) Uani 1 1 d .
C12 C 0.3319(4) 0.5953(2) 0.2491(4) 0.0188(12) Uani 1 1 d .
H12 H 0.3136 0.6130 0.2964 0.023 Uiso 1 1 calc R
C13 C 0.3383(4) 0.5384(2) 0.2472(5) 0.0238(14) Uani 1 1 d .
H13 H 0.3243 0.5172 0.2940 0.029 Uiso 1 1 calc R
C14 C 0.3645(4) 0.5123(2) 0.1783(4) 0.0238(14) Uani 1 1 d .
H14 H 0.3685 0.4734 0.1779 0.029 Uiso 1 1 calc R
C15 C 0.3849(4) 0.5433(3) 0.1096(5) 0.0243(14) Uani 1 1 d .
H15 H 0.4022 0.5254 0.0617 0.029 Uiso 1 1 calc R
C16 C 0.3802(4) 0.6005(2) 0.1107(5) 0.0232(14) Uani 1 1 d .
H16 H 0.3953 0.6217 0.0647 0.028 Uiso 1 1 calc R
C17 C 0.2931(3) 0.7208(2) 0.0730(4) 0.0154(12) Uani 1 1 d .
H17A H 0.2894 0.7613 0.0725 0.019 Uiso 1 1 calc R
H17B H 0.3227 0.7102 0.0271 0.019 Uiso 1 1 calc R
C18 C 0.2101(3) 0.6974(2) 0.0422(4) 0.0157(12) Uani 1 1 d .
H18A H 0.2131 0.6568 0.0422 0.019 Uiso 1 1 calc R
H18B H 0.1856 0.7096 -0.0218 0.019 Uiso 1 1 calc R
C19 C 1.0385(4) 0.8430(3) 0.1955(4) 0.0326(18) Uani 1 1 d DU
C21 C 0.6073(3) 0.6393(2) 0.2189(4) 0.0161(12) Uani 1 1 d .
C22 C 0.5666(3) 0.6170(2) 0.2795(4) 0.0207(13) Uani 1 1 d .
H22 H 0.5418 0.6402 0.3150 0.025 Uiso 1 1 calc R
C23 C 0.5630(4) 0.5605(3) 0.2873(5) 0.0281(15) Uani 1 1 d .
H23 H 0.5351 0.5445 0.3278 0.034 Uiso 1 1 calc R
C24 C 0.6004(5) 0.5270(3) 0.2355(5) 0.0332(17) Uani 1 1 d .
H24 H 0.5991 0.4883 0.2419 0.040 Uiso 1 1 calc R
C25 C 0.6393(5) 0.5500(3) 0.1749(5) 0.0350(17) Uani 1 1 d .
H25 H 0.6637 0.5268 0.1390 0.042 Uiso 1 1 calc R
C26 C 0.6431(4) 0.6061(2) 0.1657(5) 0.0243(14) Uani 1 1 d .
H26 H 0.6697 0.6218 0.1237 0.029 Uiso 1 1 calc R
C27 C 0.6852(3) 0.7265(2) 0.3244(4) 0.0144(11) Uani 1 1 d .
H27A H 0.6976 0.7663 0.3284 0.017 Uiso 1 1 calc R
H27B H 0.6592 0.7175 0.3742 0.017 Uiso 1 1 calc R
C28 C 0.7623(3) 0.6946(2) 0.3405(4) 0.0147(12) Uani 1 1 d .
H28A H 0.7946 0.7021 0.4039 0.018 Uiso 1 1 calc R
H28B H 0.7501 0.6548 0.3363 0.018 Uiso 1 1 calc R
C29 C 0.8108(3) 0.7084(2) 0.2723(4) 0.0167(12) Uani 1 1 d .
H29A H 0.8083 0.7485 0.2607 0.020 Uiso 1 1 calc R
H29B H 0.7876 0.6897 0.2128 0.020 Uiso 1 1 calc R
C31 C 0.9086(3) 0.6165(2) 0.3425(4) 0.0146(12) Uani 1 1 d .
C32 C 0.9139(4) 0.6010(2) 0.4323(4) 0.0192(13) Uani 1 1 d .
H32 H 0.9187 0.6280 0.4793 0.023 Uiso 1 1 calc R
C33 C 0.9120(4) 0.5459(3) 0.4537(5) 0.0251(14) Uani 1 1 d .
H33 H 0.9159 0.5349 0.5156 0.030 Uiso 1 1 calc R
C34 C 0.9046(4) 0.5068(3) 0.3854(5) 0.0261(15) Uani 1 1 d .
H34 H 0.9032 0.4689 0.4003 0.031 Uiso 1 1 calc R
C35 C 0.8992(4) 0.5228(3) 0.2947(5) 0.0302(16) Uani 1 1 d .
H35 H 0.8943 0.4956 0.2480 0.036 Uiso 1 1 calc R
C36 C 0.9008(4) 0.5777(2) 0.2716(5) 0.0224(13) Uani 1 1 d .
H36 H 0.8967 0.5887 0.2096 0.027 Uiso 1 1 calc R
C47 C 0.1584(3) 0.7155(2) 0.1047(4) 0.0151(12) Uani 1 1 d .
H47A H 0.1584 0.7561 0.1079 0.018 Uiso 1 1 calc R
H47B H 0.1814 0.7014 0.1679 0.018 Uiso 1 1 calc R
S4 S 0.05559(8) 0.69111(5) 0.06451(10) 0.0130(3) Uani 1 1 d .
C41 C 0.0669(3) 0.6214(2) 0.0338(4) 0.0148(11) Uani 1 1 d .
C42 C 0.1130(4) 0.5864(3) 0.0992(5) 0.0235(14) Uani 1 1 d .
H42 H 0.1358 0.5989 0.1603 0.028 Uiso 1 1 calc R
C46 C 0.0316(4) 0.6036(3) -0.0545(4) 0.0218(13) Uani 1 1 d .
H46 H -0.0004 0.6280 -0.0981 0.026 Uiso 1 1 calc R
C45 C 0.0431(4) 0.5496(3) -0.0793(5) 0.0279(15) Uani 1 1 d .
H45 H 0.0187 0.5369 -0.1399 0.033 Uiso 1 1 calc R
C44 C 0.0902(4) 0.5147(3) -0.0156(5) 0.0284(15) Uani 1 1 d .
H44 H 0.0986 0.4781 -0.0328 0.034 Uiso 1 1 calc R
C43 C 0.1253(4) 0.5330(3) 0.0737(6) 0.0352(18) Uani 1 1 d .
H43 H 0.1576 0.5088 0.1172 0.042 Uiso 1 1 calc R
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ag1 0.0165(2) 0.0173(2) 0.0233(2) -0.00009(16) 0.00757(17) -0.00036(16)
Ag2 0.00781(19) 0.0158(2) 0.0240(2) 0.00115(16) 0.00269(16) 0.00069(15)
Ag3 0.0146(2) 0.0184(2) 0.0191(2) -0.00066(15) 0.00441(16) -0.00052(16)
Ag4 0.0212(2) 0.0202(2) 0.0258(3) 0.00285(17) 0.01364(18) 0.00173(17)
Ag5 0.0216(2) 0.0308(3) 0.0306(3) -0.0173(2) -0.0004(2) -0.0054(2)
S1 0.0085(6) 0.0119(6) 0.0169(7) -0.0005(5) 0.0028(5) -0.0015(5)
S2 0.0080(6) 0.0127(6) 0.0150(7) 0.0000(5) 0.0015(5) 0.0001(5)
S3 0.0069(6) 0.0125(6) 0.0142(7) -0.0006(5) 0.0018(5) 0.0000(5)
S5 0.0108(6) 0.0119(6) 0.0180(7) 0.0003(5) 0.0029(5) -0.0001(5)
S6 0.0121(7) 0.0127(6) 0.0222(8) -0.0009(5) 0.0009(5) -0.0009(5)
S7 0.0099(6) 0.0154(6) 0.0168(7) 0.0001(5) 0.0016(5) 0.0005(5)
S8 0.0217(8) 0.0200(7) 0.0254(8) 0.0010(6) 0.0062(6) -0.0007(6)
S9 0.0126(7) 0.0154(6) 0.0208(8) 0.0006(5) 0.0041(5) -0.0016(5)
F1 0.073(3) 0.020(2) 0.032(2) 0.0094(17) 0.002(2) -0.001(2)
F2 0.039(3) 0.029(2) 0.073(3) -0.007(2) 0.010(2) -0.018(2)
F3 0.062(3) 0.023(2) 0.045(3) -0.0058(18) 0.025(2) 0.011(2)
F4 0.033(2) 0.028(2) 0.027(2) 0.0092(16) 0.0075(17) -0.0071(17)
F5 0.027(2) 0.0204(19) 0.046(3) 0.0050(17) 0.0061(18) 0.0079(16)
F6 0.035(2) 0.0217(19) 0.032(2) -0.0021(16) -0.0014(17) -0.0099(16)
F7 0.028(2) 0.048(3) 0.057(3) -0.005(2) -0.006(2) 0.005(2)
F8 0.042(3) 0.064(3) 0.046(3) -0.012(2) 0.024(2) -0.014(2)
F9 0.038(2) 0.034(2) 0.052(3) -0.015(2) 0.017(2) -0.0178(19)
F10 0.041(3) 0.036(2) 0.032(2) 0.0168(18) 0.0049(19) 0.0034(19)
F11 0.033(2) 0.0210(19) 0.051(3) -0.0012(17) 0.021(2) 0.0071(16)
F12 0.024(2) 0.023(2) 0.060(3) 0.0032(18) 0.0119(19) -0.0079(16)
F13 0.033(2) 0.0228(19) 0.031(2) -0.0071(15) 0.0030(17) 0.0105(16)
F14 0.031(2) 0.0223(19) 0.038(2) 0.0089(16) -0.0011(18) -0.0128(16)
F15 0.0173(18) 0.0240(18) 0.0204(19) -0.0012(14) -0.0047(14) 0.0013(14)
O1 0.020(2) 0.018(2) 0.029(3) 0.0025(17) 0.0083(18) 0.0033(17)
O2 0.028(3) 0.020(2) 0.032(3) 0.0014(19) -0.001(2) 0.0058(19)
O3 0.020(2) 0.020(2) 0.033(3) -0.0086(18) 0.0044(19) 0.0004(17)
O4 0.014(2) 0.022(2) 0.046(3) 0.001(2) 0.000(2) -0.0010(18)
O5 0.015(2) 0.018(2) 0.025(2) -0.0043(17) 0.0025(17) -0.0016(16)
O6 0.018(2) 0.018(2) 0.024(2) -0.0011(16) 0.0084(18) 0.0011(16)
O7 0.013(2) 0.023(2) 0.021(2) 0.0033(17) 0.0027(16) 0.0032(16)
O8 0.023(2) 0.025(2) 0.022(2) -0.0053(18) 0.0104(18) -0.0064(18)
O9 0.033(3) 0.023(2) 0.031(3) -0.0034(19) 0.004(2) 0.002(2)
O10 0.025(3) 0.030(3) 0.036(3) -0.003(2) 0.009(2) 0.004(2)
O11 0.038(3) 0.030(3) 0.031(3) 0.001(2) 0.007(2) -0.010(2)
O12 0.025(2) 0.023(2) 0.033(3) -0.0017(19) 0.015(2) 0.0007(18)
O13 0.020(2) 0.030(2) 0.026(3) 0.0046(19) 0.0018(19) 0.0036(19)
O14 0.015(2) 0.024(2) 0.029(3) -0.0005(18) 0.0038(18) -0.0039(17)
O15 0.021(2) 0.021(2) 0.027(3) 0.0086(18) 0.0006(19) -0.0015(18)
O16 0.015(2) 0.020(2) 0.025(2) 0.0052(17) -0.0041(17) 0.0005(17)
O17 0.019(2) 0.032(3) 0.034(3) -0.012(2) 0.007(2) 0.0038(19)
C1 0.040(4) 0.030(4) 0.034(4) 0.006(3) 0.005(3) -0.001(3)
C2 0.012(3) 0.024(3) 0.019(3) 0.001(2) 0.001(2) 0.001(2)
C3 0.032(4) 0.026(3) 0.033(4) 0.001(3) 0.004(3) 0.007(3)
C4 0.012(3) 0.017(3) 0.029(4) 0.005(2) -0.004(2) -0.003(2)
C5 0.031(4) 0.016(3) 0.022(3) -0.003(2) 0.004(3) -0.003(3)
C6 0.015(3) 0.024(3) 0.029(4) -0.006(3) 0.005(3) -0.002(2)
C7 0.032(4) 0.040(4) 0.027(4) -0.008(3) 0.007(3) -0.010(3)
C8 0.037(4) 0.026(3) 0.034(4) -0.002(3) 0.011(3) -0.003(3)
C9 0.014(3) 0.011(3) 0.031(4) 0.001(2) -0.002(3) 0.001(2)
C10 0.018(3) 0.017(3) 0.027(4) 0.001(2) 0.009(3) -0.002(2)
C11 0.010(3) 0.010(3) 0.028(3) -0.002(2) 0.001(2) -0.001(2)
C12 0.017(3) 0.014(3) 0.026(3) -0.002(2) 0.006(2) -0.001(2)
C13 0.026(4) 0.017(3) 0.030(4) 0.002(2) 0.009(3) -0.004(2)
C14 0.026(3) 0.013(3) 0.029(4) -0.004(2) 0.000(3) -0.002(2)
C15 0.026(3) 0.019(3) 0.028(4) -0.009(2) 0.006(3) 0.004(3)
C16 0.017(3) 0.015(3) 0.036(4) -0.001(2) 0.003(3) 0.000(2)
C17 0.012(3) 0.015(3) 0.017(3) 0.005(2) 0.000(2) 0.001(2)
C18 0.013(3) 0.018(3) 0.016(3) -0.001(2) 0.003(2) 0.000(2)
C19 0.059(5) 0.023(3) 0.009(3) -0.006(2) -0.005(3) 0.029(3)
C21 0.011(3) 0.014(3) 0.020(3) 0.000(2) -0.001(2) -0.001(2)
C22 0.013(3) 0.015(3) 0.032(4) -0.001(2) 0.002(3) 0.002(2)
C23 0.026(4) 0.021(3) 0.034(4) 0.005(3) 0.001(3) -0.007(3)
C24 0.047(5) 0.013(3) 0.036(4) 0.001(3) 0.003(3) -0.006(3)
C25 0.045(5) 0.015(3) 0.043(5) -0.005(3) 0.008(4) 0.005(3)
C26 0.026(4) 0.015(3) 0.029(4) 0.000(2) 0.004(3) 0.003(2)
C27 0.011(3) 0.018(3) 0.013(3) -0.006(2) 0.000(2) 0.000(2)
C28 0.005(3) 0.014(3) 0.022(3) 0.000(2) -0.001(2) 0.001(2)
C29 0.010(3) 0.017(3) 0.021(3) 0.000(2) -0.001(2) 0.004(2)
C31 0.010(3) 0.007(2) 0.025(3) 0.004(2) 0.002(2) 0.001(2)
C32 0.024(3) 0.022(3) 0.012(3) 0.003(2) 0.007(2) -0.001(2)
C33 0.027(4) 0.025(3) 0.023(4) 0.009(3) 0.007(3) 0.006(3)
C34 0.031(4) 0.017(3) 0.034(4) 0.007(3) 0.016(3) 0.005(3)
C35 0.042(4) 0.015(3) 0.036(4) -0.005(3) 0.014(3) -0.004(3)
C36 0.024(3) 0.017(3) 0.026(4) 0.001(2) 0.007(3) -0.003(2)
C47 0.004(3) 0.018(3) 0.021(3) 0.000(2) 0.000(2) -0.004(2)
S4 0.0085(6) 0.0123(6) 0.0179(7) 0.0021(5) 0.0028(5) 0.0008(5)
C41 0.012(3) 0.012(3) 0.021(3) 0.003(2) 0.005(2) -0.001(2)
C42 0.018(3) 0.022(3) 0.024(4) 0.004(2) -0.006(3) 0.001(2)
C46 0.028(4) 0.023(3) 0.017(3) 0.001(2) 0.010(3) 0.001(3)
C45 0.037(4) 0.023(3) 0.026(4) -0.003(3) 0.013(3) -0.008(3)
C44 0.025(4) 0.016(3) 0.048(5) -0.004(3) 0.016(3) 0.000(3)
C43 0.025(4) 0.016(3) 0.055(5) 0.002(3) -0.008(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 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag 0.1306 4.2820 '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
O1 Ag1 O14 . . 93.26(15) y
O1 Ag1 O2 . . 128.23(15) y
O14 Ag1 O2 . . 83.90(15) y
O1 Ag1 S1 . . 124.77(11) y
O14 Ag1 S1 . . 129.60(11) y
O2 Ag1 S1 . . 93.76(11) y
O3 Ag2 S2 4_575 . 123.03(11) y
O3 Ag2 O5 4_575 . 93.52(15) y
S2 Ag2 O5 . . 124.96(10) y
O3 Ag2 S1 4_575 . 91.11(11) y
S2 Ag2 S1 . . 130.84(4) y
O5 Ag2 S1 . . 81.06(10) y
O8 Ag3 O7 . 4_575 104.19(15) y
O8 Ag3 O17 . . 93.62(16) y
O7 Ag3 O17 4_575 . 85.03(14) y
O8 Ag3 S2 . . 137.85(11) y
O7 Ag3 S2 4_575 . 113.19(10) y
O17 Ag3 S2 . . 107.93(12) y
S3 Ag4 S4 . 1_655 176.24(5) y
S3 Ag4 O13 . 1_655 96.50(11) y
S4 Ag4 O13 1_655 1_655 83.14(11) y
S4 Ag5 S3 4_676 . 167.22(5) y
S4 Ag5 O15 4_676 4_576 97.83(10) y
S3 Ag5 O15 . 4_576 93.99(10) y
C11 S1 C17 . . 104.6(3) y
C11 S1 Ag1 . . 110.6(2) y
C17 S1 Ag1 . . 122.6(2) y
C11 S1 Ag2 . . 116.01(19) y
C17 S1 Ag2 . . 102.98(19) y
Ag1 S1 Ag2 . . 100.42(5) y
C21 S2 C27 . . 100.1(3) y
C21 S2 Ag2 . . 105.69(19) y
C27 S2 Ag2 . . 111.87(18) y
C21 S2 Ag3 . . 115.8(2) y
C27 S2 Ag3 . . 115.8(2) y
Ag2 S2 Ag3 . . 107.11(5) y
C31 S3 C29 . . 103.7(3) y
C31 S3 Ag4 . . 106.8(2) y
C29 S3 Ag4 . . 111.3(2) y
C31 S3 Ag5 . . 117.2(2) y
C29 S3 Ag5 . . 105.34(19) y
Ag4 S3 Ag5 . . 112.24(5) y
O6 S5 O7 . . 116.2(3) y
O6 S5 O5 . . 115.2(3) y
O7 S5 O5 . . 113.9(2) y
O6 S5 C4 . . 104.3(3) y
O7 S5 C4 . . 103.1(3) y
O5 S5 C4 . . 101.5(3) y
O2 S6 O3 . . 115.5(3) y
O2 S6 O4 . . 114.7(3) y
O3 S6 O4 . . 114.4(3) y
O2 S6 C5 . . 103.6(3) y
O3 S6 C5 . . 103.2(3) y
O4 S6 C5 . . 103.1(3) y
O17 S7 O15 . . 116.1(3) y
O17 S7 O16 . . 114.5(3) y
O15 S7 O16 . . 114.8(3) y
O17 S7 C9 . . 103.0(3) y
O15 S7 C9 . . 103.1(3) y
O16 S7 C9 . . 102.7(3) y
O11 S8 O9 . . 114.5(3) y
O11 S8 O10 . . 115.8(3) y
O9 S8 O10 . . 115.1(3) y
O11 S8 C19 . . 101.7(3) y
O9 S8 C19 . . 101.7(3) y
O10 S8 C19 . . 105.3(3) y
O12 S9 O13 . . 115.4(3) y
O12 S9 O14 . . 114.8(3) y
O13 S9 O14 . . 114.2(3) y
O12 S9 C10 . . 103.8(3) y
O13 S9 C10 . . 103.5(3) y
O14 S9 C10 . . 102.9(3) y
C2 O1 Ag1 . . 131.2(4) y
S6 O2 Ag1 . . 142.0(3) y
S6 O3 Ag2 . 4_576 116.9(2) y
S5 O5 Ag2 . . 123.0(2) y
S5 O7 Ag3 . 4_576 121.1(2) y
C6 O8 Ag3 . . 124.7(4) y
S9 O13 Ag4 . 1_455 131.8(3) y
S9 O14 Ag1 . . 130.5(3) y
S7 O15 Ag5 . 4_575 127.9(2) y
S7 O17 Ag3 . . 159.6(3) y
C2 C1 H1A . . 109.5 ?
C2 C1 H1B . . 109.5 ?
H1A C1 H1B . . 109.5 ?
C2 C1 H1C . . 109.5 ?
H1A C1 H1C . . 109.5 ?
H1B C1 H1C . . 109.5 ?
O1 C2 C1 . . 122.4(6) y
O1 C2 C3 . . 119.1(6) y
C1 C2 C3 . . 118.5(6) y
C2 C3 H3A . . 109.5 ?
C2 C3 H3B . . 109.5 ?
H3A C3 H3B . . 109.5 ?
C2 C3 H3C . . 109.5 ?
H3A C3 H3C . . 109.5 ?
H3B C3 H3C . . 109.5 ?
F6 C4 F5 . . 107.5(5) y
F6 C4 F4 . . 107.7(5) y
F5 C4 F4 . . 107.9(5) y
F6 C4 S5 . . 112.2(4) y
F5 C4 S5 . . 110.3(4) y
F4 C4 S5 . . 111.1(4) y
F1 C5 F2 . . 109.1(6) y
F1 C5 F3 . . 107.8(6) y
F2 C5 F3 . . 107.5(5) y
F1 C5 S6 . . 111.1(4) y
F2 C5 S6 . . 111.1(5) y
F3 C5 S6 . . 110.1(4) y
O8 C6 C7 . . 122.7(6) y
O8 C6 C8 . . 120.4(6) y
C7 C6 C8 . . 116.9(6) y
C6 C7 H7A . . 109.5 ?
C6 C7 H7B . . 109.5 ?
H7A C7 H7B . . 109.5 ?
C6 C7 H7C . . 109.5 ?
H7A C7 H7C . . 109.5 ?
H7B C7 H7C . . 109.5 ?
C6 C8 H8A . . 109.5 ?
C6 C8 H8B . . 109.5 ?
H8A C8 H8B . . 109.5 ?
C6 C8 H8C . . 109.5 ?
H8A C8 H8C . . 109.5 ?
H8B C8 H8C . . 109.5 ?
F13 C9 F14 . . 108.5(5) y
F13 C9 F15 . . 107.6(5) y
F14 C9 F15 . . 108.1(5) y
F13 C9 S7 . . 110.9(4) y
F14 C9 S7 . . 110.7(4) y
F15 C9 S7 . . 110.9(4) y
F10 C10 F12 . . 108.3(5) y
F10 C10 F11 . . 108.0(5) y
F12 C10 F11 . . 107.5(5) y
F10 C10 S9 . . 111.6(4) y
F12 C10 S9 . . 110.8(4) y
F11 C10 S9 . . 110.4(4) y
C16 C11 C12 . . 121.3(5) y
C16 C11 S1 . . 120.3(5) y
C12 C11 S1 . . 118.2(5) y
C13 C12 C11 . . 118.6(6) y
C13 C12 H12 . . 120.7 ?
C11 C12 H12 . . 120.7 ?
C14 C13 C12 . . 121.1(6) y
C14 C13 H13 . . 119.4 ?
C12 C13 H13 . . 119.4 ?
C13 C14 C15 . . 119.6(6) y
C13 C14 H14 . . 120.2 ?
C15 C14 H14 . . 120.2 ?
C14 C15 C16 . . 120.4(6) y
C14 C15 H15 . . 119.8 ?
C16 C15 H15 . . 119.8 ?
C11 C16 C15 . . 118.9(6) y
C11 C16 H16 . . 120.6 ?
C15 C16 H16 . . 120.6 ?
C18 C17 S1 . . 115.4(4) y
C18 C17 H17A . . 108.4 ?
S1 C17 H17A . . 108.4 ?
C18 C17 H17B . . 108.4 ?
S1 C17 H17B . . 108.4 ?
H17A C17 H17B . . 107.5 ?
C17 C18 C47 . . 112.0(5) y
C17 C18 H18A . . 109.2 ?
C47 C18 H18A . . 109.2 ?
C17 C18 H18B . . 109.2 ?
C47 C18 H18B . . 109.2 ?
H18A C18 H18B . . 107.9 ?
F7 C19 F9 . . 104.5(5) y
F7 C19 F8 . . 101.7(5) y
F9 C19 F8 . . 98.9(6) y
F7 C19 S8 . . 118.4(5) y
F9 C19 S8 . . 116.9(5) y
F8 C19 S8 . . 113.6(4) y
C26 C21 C22 . . 121.4(6) y
C26 C21 S2 . . 119.5(5) y
C22 C21 S2 . . 119.1(4) y
C23 C22 C21 . . 118.9(6) y
C23 C22 H22 . . 120.5 ?
C21 C22 H22 . . 120.5 ?
C22 C23 C24 . . 119.8(6) y
C22 C23 H23 . . 120.1 ?
C24 C23 H23 . . 120.1 ?
C25 C24 C23 . . 120.3(6) y
C25 C24 H24 . . 119.9 ?
C23 C24 H24 . . 119.9 ?
C26 C25 C24 . . 120.8(7) y
C26 C25 H25 . . 119.6 ?
C24 C25 H25 . . 119.6 ?
C25 C26 C21 . . 118.8(7) y
C25 C26 H26 . . 120.6 ?
C21 C26 H26 . . 120.6 ?
C28 C27 S2 . . 113.8(4) y
C28 C27 H27A . . 108.8 ?
S2 C27 H27A . . 108.8 ?
C28 C27 H27B . . 108.8 ?
S2 C27 H27B . . 108.8 ?
H27A C27 H27B . . 107.7 ?
C29 C28 C27 . . 113.5(5) y
C29 C28 H28A . . 108.9 ?
C27 C28 H28A . . 108.9 ?
C29 C28 H28B . . 108.9 ?
C27 C28 H28B . . 108.9 ?
H28A C28 H28B . . 107.7 ?
C28 C29 S3 . . 112.0(4) y
C28 C29 H29A . . 109.2 ?
S3 C29 H29A . . 109.2 ?
C28 C29 H29B . . 109.2 ?
S3 C29 H29B . . 109.2 ?
H29A C29 H29B . . 107.9 ?
C32 C31 C36 . . 121.6(5) y
C32 C31 S3 . . 119.8(4) y
C36 C31 S3 . . 118.6(4) y
C31 C32 C33 . . 119.5(6) y
C31 C32 H32 . . 120.3 ?
C33 C32 H32 . . 120.3 ?
C34 C33 C32 . . 120.3(6) y
C34 C33 H33 . . 119.9 ?
C32 C33 H33 . . 119.9 ?
C33 C34 C35 . . 119.9(6) y
C33 C34 H34 . . 120.1 ?
C35 C34 H34 . . 120.1 ?
C36 C35 C34 . . 120.9(6) y
C36 C35 H35 . . 119.5 ?
C34 C35 H35 . . 119.5 ?
C35 C36 C31 . . 117.9(6) y
C35 C36 H36 . . 121.1 ?
C31 C36 H36 . . 121.1 ?
C18 C47 S4 . . 112.7(4) y
C18 C47 H47A . . 109 ?
S4 C47 H47A . . 109 ?
C18 C47 H47B . . 109 ?
S4 C47 H47B . . 109 ?
H47A C47 H47B . . 107.8 ?
C41 S4 C47 . . 103.3(3) y
C41 S4 Ag5 . 4_475 116.3(2) y
C47 S4 Ag5 . 4_475 114.01(19) y
C41 S4 Ag4 . 1_455 108.46(19) y
C47 S4 Ag4 . 1_455 111.7(2) y
Ag5 S4 Ag4 4_475 1_455 103.20(5) y
C46 C41 C42 . . 121.5(6) y
C46 C41 S4 . . 119.5(4) y
C42 C41 S4 . . 119.0(5) y
C43 C42 C41 . . 118.9(6) y
C43 C42 H42 . . 120.5 ?
C41 C42 H42 . . 120.5 ?
C41 C46 C45 . . 119.3(6) y
C41 C46 H46 . . 120.3 ?
C45 C46 H46 . . 120.3 ?
C44 C45 C46 . . 119.8(6) y
C44 C45 H45 . . 120.1 ?
C46 C45 H45 . . 120.1 ?
C45 C44 C43 . . 120.3(6) y
C45 C44 H44 . . 119.8 ?
C43 C44 H44 . . 119.8 ?
C42 C43 C44 . . 120.1(6) y
C42 C43 H43 . . 119.9 ?
C44 C43 H43 . . 119.9 ?
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
Ag1 O1 . 2.357(4) y
Ag1 O14 . 2.359(4) y
Ag1 O2 . 2.501(4) y
Ag1 S1 . 2.5290(14) y
Ag2 O3 4_575 2.401(4) y
Ag2 S2 . 2.4547(13) y
Ag2 O5 . 2.479(4) y
Ag2 S1 . 2.5512(13) y
Ag3 O8 . 2.324(4) y
Ag3 O7 4_575 2.423(4) y
Ag3 O17 . 2.462(4) y
Ag3 S2 . 2.5130(14) y
Ag4 S3 . 2.4613(14) y
Ag4 S4 1_655 2.5086(14) y
Ag4 O13 1_655 2.597(4) y
Ag5 S4 4_676 2.4634(14) y
Ag5 S3 . 2.4712(13) y
Ag5 O15 4_576 2.540(4) y
S1 C11 . 1.788(5) y
S1 C17 . 1.825(6) y
S2 C21 . 1.790(6) y
S2 C27 . 1.843(6) y
S3 C31 . 1.793(5) y
S3 C29 . 1.830(6) y
S5 O6 . 1.439(4) y
S5 O7 . 1.447(4) y
S5 O5 . 1.453(4) y
S5 C4 . 1.828(6) y
S6 O2 . 1.440(5) y
S6 O3 . 1.443(5) y
S6 O4 . 1.447(4) y
S6 C5 . 1.835(6) y
S7 O17 . 1.440(4) y
S7 O15 . 1.441(4) y
S7 O16 . 1.443(4) y
S7 C9 . 1.827(6) y
S8 O11 . 1.445(5) y
S8 O9 . 1.455(5) y
S8 O10 . 1.461(5) y
S8 C19 . 1.700(8) y
S9 O12 . 1.433(4) y
S9 O13 . 1.443(5) y
S9 O14 . 1.444(4) y
S9 C10 . 1.830(6) y
F1 C5 . 1.317(7) y
F2 C5 . 1.322(8) y
F3 C5 . 1.331(7) y
F4 C4 . 1.339(7) y
F5 C4 . 1.335(7) y
F6 C4 . 1.324(7) y
F7 C19 . 1.348(7) y
F8 C19 . 1.427(8) y
F9 C19 . 1.364(7) y
F10 C10 . 1.322(7) y
F11 C10 . 1.335(7) y
F12 C10 . 1.325(7) y
F13 C9 . 1.324(7) y
F14 C9 . 1.332(7) y
F15 C9 . 1.343(7) y
O1 C2 . 1.220(7) y
O3 Ag2 4_576 2.401(4) y
O7 Ag3 4_576 2.423(4) y
O8 C6 . 1.214(7) y
O13 Ag4 1_455 2.597(4) y
O15 Ag5 4_575 2.540(4) y
C1 C2 . 1.489(9) y
C1 H1A . 0.98 ?
C1 H1B . 0.98 ?
C1 H1C . 0.98 ?
C2 C3 . 1.514(9) y
C3 H3A . 0.98 ?
C3 H3B . 0.98 ?
C3 H3C . 0.98 ?
C6 C7 . 1.488(9) y
C6 C8 . 1.508(9) y
C7 H7A . 0.98 ?
C7 H7B . 0.98 ?
C7 H7C . 0.98 ?
C8 H8A . 0.98 ?
C8 H8B . 0.98 ?
C8 H8C . 0.98 ?
C11 C16 . 1.390(9) y
C11 C12 . 1.392(8) y
C12 C13 . 1.390(8) y
C12 H12 . 0.95 ?
C13 C14 . 1.383(9) y
C13 H13 . 0.95 ?
C14 C15 . 1.391(9) y
C14 H14 . 0.95 ?
C15 C16 . 1.396(8) y
C15 H15 . 0.95 ?
C16 H16 . 0.95 ?
C17 C18 . 1.514(7) y
C17 H17A . 0.99 ?
C17 H17B . 0.99 ?
C18 C47 . 1.518(8) y
C18 H18A . 0.99 ?
C18 H18B . 0.99 ?
C21 C26 . 1.387(9) y
C21 C22 . 1.394(8) y
C22 C23 . 1.384(8) y
C22 H22 . 0.95 ?
C23 C24 . 1.394(10) y
C23 H23 . 0.95 ?
C24 C25 . 1.378(10) y
C24 H24 . 0.95 ?
C25 C26 . 1.377(9) y
C25 H25 . 0.95 ?
C26 H26 . 0.95 ?
C27 C28 . 1.518(7) y
C27 H27A . 0.99 ?
C27 H27B . 0.99 ?
C28 C29 . 1.517(8) y
C28 H28A . 0.99 ?
C28 H28B . 0.99 ?
C29 H29A . 0.99 ?
C29 H29B . 0.99 ?
C31 C32 . 1.376(8) y
C31 C36 . 1.400(8) y
C32 C33 . 1.382(8) y
C32 H32 . 0.95 ?
C33 C34 . 1.377(9) y
C33 H33 . 0.95 ?
C34 C35 . 1.391(9) y
C34 H34 . 0.95 ?
C35 C36 . 1.383(8) y
C35 H35 . 0.95 ?
C36 H36 . 0.95 ?
C47 S4 . 1.839(5) y
C47 H47A . 0.99 ?
C47 H47B . 0.99 ?
S4 C41 . 1.783(6) y
S4 Ag5 4_475 2.4634(13) y
S4 Ag4 1_455 2.5085(14) y
C41 C46 . 1.378(8) y
C41 C42 . 1.388(8) y
C42 C43 . 1.387(9) y
C42 H42 . 0.95 ?
C46 C45 . 1.395(9) y
C46 H46 . 0.95 ?
C45 C44 . 1.381(10) y
C45 H45 . 0.95 ?
C44 C43 . 1.394(10) y
C44 H44 . 0.95 ?
C43 H43 . 0.95 ?
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_4
_geom_torsion
O1 Ag1 S1 C11 . . -162.0(2)
O14 Ag1 S1 C11 . . -30.4(2)
O2 Ag1 S1 C11 . . 54.8(2)
O1 Ag1 S1 C17 . . -38.0(3)
O14 Ag1 S1 C17 . . 93.7(3)
O2 Ag1 S1 C17 . . 178.9(2)
O1 Ag1 S1 Ag2 . . 74.94(14)
O14 Ag1 S1 Ag2 . . -153.45(14)
O2 Ag1 S1 Ag2 . . -68.26(11)
O3 Ag2 S1 C11 4_575 . 138.3(3)
S2 Ag2 S1 C11 . . 0.8(2)
O5 Ag2 S1 C11 . . -128.3(3)
O3 Ag2 S1 C17 4_575 . 24.8(2)
S2 Ag2 S1 C17 . . -112.7(2)
O5 Ag2 S1 C17 . . 118.2(2)
O3 Ag2 S1 Ag1 4_575 . -102.46(12)
S2 Ag2 S1 Ag1 . . 120.04(6)
O5 Ag2 S1 Ag1 . . -9.07(10)
O3 Ag2 S2 C21 4_575 . -134.4(2)
O5 Ag2 S2 C21 . . 102.6(2)
S1 Ag2 S2 C21 . . -8.1(2)
O3 Ag2 S2 C27 4_575 . 117.5(2)
O5 Ag2 S2 C27 . . -5.4(2)
S1 Ag2 S2 C27 . . -116.1(2)
O3 Ag2 S2 Ag3 4_575 . -10.41(14)
O5 Ag2 S2 Ag3 . . -133.37(12)
S1 Ag2 S2 Ag3 . . 115.92(6)
O8 Ag3 S2 C21 . . -160.1(3)
O7 Ag3 S2 C21 4_575 . 49.3(2)
O17 Ag3 S2 C21 . . -42.9(2)
O8 Ag3 S2 C27 . . -43.3(3)
O7 Ag3 S2 C27 4_575 . 166.2(2)
O17 Ag3 S2 C27 . . 73.9(2)
O8 Ag3 S2 Ag2 . . 82.34(17)
O7 Ag3 S2 Ag2 4_575 . -68.23(12)
O17 Ag3 S2 Ag2 . . -160.50(11)
O13 Ag4 S3 C31 1_655 . -70.0(2)
O13 Ag4 S3 C29 1_655 . 177.5(2)
O13 Ag4 S3 Ag5 1_655 . 59.69(11)
S4 Ag5 S3 C31 4_676 . 89.9(3)
O15 Ag5 S3 C31 4_576 . -112.5(2)
S4 Ag5 S3 C29 4_676 . -155.4(3)
O15 Ag5 S3 C29 4_576 . 2.2(2)
S4 Ag5 S3 Ag4 4_676 . -34.2(2)
O15 Ag5 S3 Ag4 4_576 . 123.39(11)
O14 Ag1 O1 C2 . . -154.7(5)
O2 Ag1 O1 C2 . . 120.5(5)
S1 Ag1 O1 C2 . . -9.9(6)
O3 S6 O2 Ag1 . . 10.0(6)
O4 S6 O2 Ag1 . . -126.4(4)
C5 S6 O2 Ag1 . . 122.0(4)
O1 Ag1 O2 S6 . . 37.1(5)
O14 Ag1 O2 S6 . . -52.2(5)
S1 Ag1 O2 S6 . . 178.3(4)
O2 S6 O3 Ag2 . 4_576 -115.1(3)
O4 S6 O3 Ag2 . 4_576 21.4(4)
C5 S6 O3 Ag2 . 4_576 132.7(3)
O6 S5 O5 Ag2 . . -150.7(2)
O7 S5 O5 Ag2 . . -12.7(4)
C4 S5 O5 Ag2 . . 97.3(3)
O3 Ag2 O5 S5 4_575 . -119.9(3)
S2 Ag2 O5 S5 . . 15.3(3)
S1 Ag2 O5 S5 . . 149.6(3)
O6 S5 O7 Ag3 . 4_576 4.1(4)
O5 S5 O7 Ag3 . 4_576 -133.4(3)
C4 S5 O7 Ag3 . 4_576 117.5(3)
O7 Ag3 O8 C6 4_575 . 139.2(5)
O17 Ag3 O8 C6 . . -135.0(5)
S2 Ag3 O8 C6 . . -13.1(6)
O12 S9 O13 Ag4 . 1_455 -1.9(4)
O14 S9 O13 Ag4 . 1_455 -138.2(3)
C10 S9 O13 Ag4 . 1_455 110.8(3)
O12 S9 O14 Ag1 . . -124.0(3)
O13 S9 O14 Ag1 . . 12.6(4)
C10 S9 O14 Ag1 . . 124.0(3)
O1 Ag1 O14 S9 . . 86.3(3)
O2 Ag1 O14 S9 . . -145.6(4)
S1 Ag1 O14 S9 . . -55.7(4)
O17 S7 O15 Ag5 . 4_575 107.6(3)
O16 S7 O15 Ag5 . 4_575 -29.7(4)
C9 S7 O15 Ag5 . 4_575 -140.6(3)
O15 S7 O17 Ag3 . . 23.7(9)
O16 S7 O17 Ag3 . . 161.2(7)
C9 S7 O17 Ag3 . . -88.1(8)
O8 Ag3 O17 S7 . . -47.9(8)
O7 Ag3 O17 S7 4_575 . 56.1(8)
S2 Ag3 O17 S7 . . 168.9(8)
Ag1 O1 C2 C1 . . 10.9(9)
Ag1 O1 C2 C3 . . -169.9(4)
O6 S5 C4 F6 . . 66.2(5)
O7 S5 C4 F6 . . -55.6(5)
O5 S5 C4 F6 . . -173.7(5)
O6 S5 C4 F5 . . -53.5(5)
O7 S5 C4 F5 . . -175.3(4)
O5 S5 C4 F5 . . 66.5(5)
O6 S5 C4 F4 . . -173.2(4)
O7 S5 C4 F4 . . 65.0(4)
O5 S5 C4 F4 . . -53.1(4)
O2 S6 C5 F1 . . 179.4(5)
O3 S6 C5 F1 . . -59.8(5)
O4 S6 C5 F1 . . 59.6(5)
O2 S6 C5 F2 . . -58.9(5)
O3 S6 C5 F2 . . 61.9(5)
O4 S6 C5 F2 . . -178.7(5)
O2 S6 C5 F3 . . 60.0(5)
O3 S6 C5 F3 . . -179.2(4)
O4 S6 C5 F3 . . -59.8(5)
Ag3 O8 C6 C7 . . 22.6(9)
Ag3 O8 C6 C8 . . -158.1(5)
O17 S7 C9 F13 . . 177.0(4)
O15 S7 C9 F13 . . 55.8(5)
O16 S7 C9 F13 . . -63.8(5)
O17 S7 C9 F14 . . -62.5(5)
O15 S7 C9 F14 . . 176.3(4)
O16 S7 C9 F14 . . 56.7(5)
O17 S7 C9 F15 . . 57.4(5)
O15 S7 C9 F15 . . -63.7(5)
O16 S7 C9 F15 . . 176.7(4)
O12 S9 C10 F10 . . -61.6(5)
O13 S9 C10 F10 . . 177.5(4)
O14 S9 C10 F10 . . 58.3(5)
O12 S9 C10 F12 . . 59.2(5)
O13 S9 C10 F12 . . -61.7(5)
O14 S9 C10 F12 . . 179.1(4)
O12 S9 C10 F11 . . 178.2(4)
O13 S9 C10 F11 . . 57.4(5)
O14 S9 C10 F11 . . -61.8(5)
C17 S1 C11 C16 . . 54.1(5)
Ag1 S1 C11 C16 . . -172.0(4)
Ag2 S1 C11 C16 . . -58.6(5)
C17 S1 C11 C12 . . -129.6(5)
Ag1 S1 C11 C12 . . 4.3(5)
Ag2 S1 C11 C12 . . 117.7(4)
C16 C11 C12 C13 . . -0.1(9)
S1 C11 C12 C13 . . -176.4(5)
C11 C12 C13 C14 . . -0.4(9)
C12 C13 C14 C15 . . 0.0(1)
C13 C14 C15 C16 . . 1.0(11)
C12 C11 C16 C15 . . 1.0(9)
S1 C11 C16 C15 . . 177.2(5)
C14 C15 C16 C11 . . -1.5(9)
C11 S1 C17 C18 . . 58.1(5)
Ag1 S1 C17 C18 . . -68.7(5)
Ag2 S1 C17 C18 . . 179.7(4)
S1 C17 C18 C47 . . 62.7(6)
O11 S8 C19 F7 . . 53.9(5)
O9 S8 C19 F7 . . -64.4(5)
O10 S8 C19 F7 . . 175.1(5)
O11 S8 C19 F9 . . -72.6(5)
O9 S8 C19 F9 . . 169.1(5)
O10 S8 C19 F9 . . 48.6(6)
O11 S8 C19 F8 . . 173.2(4)
O9 S8 C19 F8 . . 54.8(5)
O10 S8 C19 F8 . . -65.6(5)
C27 S2 C21 C26 . . -107.5(5)
Ag2 S2 C21 C26 . . 136.2(5)
Ag3 S2 C21 C26 . . 17.9(5)
C27 S2 C21 C22 . . 71.1(5)
Ag2 S2 C21 C22 . . -45.2(5)
Ag3 S2 C21 C22 . . -163.6(4)
C26 C21 C22 C23 . . 0.9(9)
S2 C21 C22 C23 . . -177.7(5)
C21 C22 C23 C24 . . 0.6(10)
C22 C23 C24 C25 . . -1.6(11)
C23 C24 C25 C26 . . 1.2(12)
C24 C25 C26 C21 . . 0.3(11)
C22 C21 C26 C25 . . -1.3(9)
S2 C21 C26 C25 . . 177.2(5)
C21 S2 C27 C28 . . 55.5(5)
Ag2 S2 C27 C28 . . 167.1(3)
Ag3 S2 C27 C28 . . -69.8(4)
S2 C27 C28 C29 . . 63.0(6)
C27 C28 C29 S3 . . 161.1(4)
C31 S3 C29 C28 . . 53.7(5)
Ag4 S3 C29 C28 . . 168.1(3)
Ag5 S3 C29 C28 . . -70.0(4)
C29 S3 C31 C32 . . -97.8(5)
Ag4 S3 C31 C32 . . 144.6(4)
Ag5 S3 C31 C32 . . 17.8(5)
C29 S3 C31 C36 . . 83.9(5)
Ag4 S3 C31 C36 . . -33.7(5)
Ag5 S3 C31 C36 . . -160.5(4)
C36 C31 C32 C33 . . 0.5(9)
S3 C31 C32 C33 . . -177.7(5)
C31 C32 C33 C34 . . -0.2(11)
C32 C33 C34 C35 . . 0.1(11)
C33 C34 C35 C36 . . -0.3(11)
C34 C35 C36 C31 . . 0.5(11)
C32 C31 C36 C35 . . -0.6(9)
S3 C31 C36 C35 . . 177.7(5)
C17 C18 C47 S4 . . 176.5(4)
C18 C47 S4 C41 . . 44.1(5)
C18 C47 S4 Ag5 . 4_475 -83.0(4)
C18 C47 S4 Ag4 . 1_455 160.5(3)
C47 S4 C41 C46 . . -123.3(5)
Ag5 S4 C41 C46 4_475 . 2.4(6)
Ag4 S4 C41 C46 1_455 . 118.1(5)
C47 S4 C41 C42 . . 55.1(5)
Ag5 S4 C41 C42 4_475 . -179.2(4)
Ag4 S4 C41 C42 1_455 . -63.5(5)
C46 C41 C42 C43 . . 1.8(10)
S4 C41 C42 C43 . . -176.6(5)
C42 C41 C46 C45 . . -0.9(9)
S4 C41 C46 C45 . . 177.5(5)
C41 C46 C45 C44 . . -0.6(10)
C46 C45 C44 C43 . . 0.9(11)
C41 C42 C43 C44 . . -1.4(11)
C45 C44 C43 C42 . . 0.1(11)
|
1501563.cif | #------------------------------------------------------------------------------
#$Date: 2020-10-02 18:49:34 +0300 (Fri, 02 Oct 2020) $
#$Revision: 256944 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/50/15/1501563.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_1501563
loop_
_publ_author_name
'Mohamed Osman Awaleh'
'Francois Brisse'
'Youssouf Djibril Soubaneh'
'Thierry Maris'
'Elias Said Dirieh'
_publ_section_title
;
Four New Ag(I) Coordination Polymers: Synthesis, Crystal Structures and
Thermal Stability
;
_journal_name_full 'J. Inorg. Organomet. Polym.'
_journal_page_first 816
_journal_page_last 824
_journal_paper_doi 10.1007/s10904-010-9407-0
_journal_volume 20
_journal_year 2010
_chemical_compound_source 'Synthesized by the authors. See text'
_chemical_formula_moiety 'C13 H15 Ag O3 S3'
_chemical_formula_sum 'C13 H15 Ag O3 S3'
_chemical_formula_weight 423.30
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 110.3900(10)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 8.3129(2)
_cell_length_b 21.5540(5)
_cell_length_c 8.9118(2)
_cell_measurement_reflns_used 3506
_cell_measurement_temperature 150(2)
_cell_measurement_theta_max 68.70
_cell_measurement_theta_min 4.10
_cell_volume 1496.73(6)
_computing_cell_refinement 'SMART (Bruker, 2003)'
_computing_data_collection 'SMART (Bruker, 2003)'
_computing_data_reduction 'SAINT (Bruker, 2004)'
_computing_molecular_graphics 'SHELXTL (Bruker, 1997)'
_computing_publication_material 'UdMX (local program)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 150(2)
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type 'Bruker Smart 6000'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator 'Montel 200 optics'
_diffrn_radiation_source 'Rotating Anode'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.047
_diffrn_reflns_av_sigmaI/netI 0.0511
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 26
_diffrn_reflns_limit_k_min -26
_diffrn_reflns_limit_l_max 10
_diffrn_reflns_limit_l_min -10
_diffrn_reflns_number 20576
_diffrn_reflns_theta_full 68.69
_diffrn_reflns_theta_max 68.69
_diffrn_reflns_theta_min 4.10
_diffrn_standards_decay_% 0.54
_diffrn_standards_number 63
_exptl_absorpt_coefficient_mu 14.752
_exptl_absorpt_correction_T_max 0.750
_exptl_absorpt_correction_T_min 0.732
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Sadabs (Sheldrick,1996)'
_exptl_crystal_colour Colorless
_exptl_crystal_density_diffrn 1.879
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description needle-like
_exptl_crystal_F_000 848
_exptl_crystal_size_max 0.18
_exptl_crystal_size_mid 0.02
_exptl_crystal_size_min 0.02
_refine_diff_density_max 1.295
_refine_diff_density_min -0.953
_refine_diff_density_rms 0.152
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.130
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 181
_refine_ls_number_reflns 2714
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.130
_refine_ls_R_factor_all 0.0809
_refine_ls_R_factor_gt 0.0646
_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^)+(0.0850P)^2^+19.7035P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1924
_refine_ls_wR_factor_ref 0.1988
_reflns_number_gt 2146
_reflns_number_total 2714
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file deposit.cif
_cod_data_source_block Complex3
_cod_depositor_comments
;
Updated values of the _geom_angle_atom_site_label_*,
_geom_bond_atom_site_label_* and _geom_torsion_atom_site_label_*
data items to establish relationships between loop packets from
different data loops.
Antanas Vaitkus,
2020-10-02
;
_cod_original_sg_symbol_H-M P21/c
_cod_database_code 1501563
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
Ag1 Ag 0.20357(10) 0.51266(4) 0.54182(9) 0.0337(3) Uani 1 1 d .
S1 S 0.2661(3) 0.48742(13) 0.8311(3) 0.0323(6) Uani 1 1 d .
S2 S 0.0518(3) 0.58654(12) 0.3272(3) 0.0277(6) Uani 1 1 d .
S3 S 0.3638(3) 0.41358(13) 0.3374(3) 0.0290(6) Uani 1 1 d .
O31 O 0.3177(11) 0.4162(4) 0.4808(9) 0.040(2) Uani 1 1 d .
O32 O 0.2765(10) 0.4606(4) 0.2205(9) 0.0377(18) Uani 1 1 d .
O33 O 0.5468(10) 0.4106(4) 0.3716(10) 0.041(2) Uani 1 1 d .
C11 C 0.0697(14) 0.4586(5) 0.8453(12) 0.032(2) Uani 1 1 d .
H11A H -0.0010 0.4940 0.8567 0.038 Uiso 1 1 calc R
H11B H 0.0962 0.4325 0.9424 0.038 Uiso 1 1 calc R
C12 C 0.3905(15) 0.4169(6) 0.8653(15) 0.044(3) Uani 1 1 d .
H12A H 0.4053 0.4008 0.9722 0.066 Uiso 1 1 calc R
H12B H 0.5032 0.4255 0.8579 0.066 Uiso 1 1 calc R
H12C H 0.3305 0.3860 0.7845 0.066 Uiso 1 1 calc R
C21 C 0.2180(15) 0.6138(6) 0.2577(15) 0.041(3) Uani 1 1 d .
H21A H 0.2753 0.5782 0.2295 0.061 Uiso 1 1 calc R
H21B H 0.3020 0.6379 0.3425 0.061 Uiso 1 1 calc R
H21C H 0.1674 0.6401 0.1632 0.061 Uiso 1 1 calc R
C31 C 0.2836(13) 0.3412(5) 0.2444(13) 0.031(2) Uani 1 1 d .
C32 C 0.1048(14) 0.3266(5) 0.1879(13) 0.030(2) Uani 1 1 d .
C33 C -0.0249(13) 0.3651(6) 0.2132(14) 0.036(3) Uani 1 1 d .
H33 H 0.0056 0.4032 0.2697 0.043 Uiso 1 1 calc R
C34 C -0.1910(15) 0.3465(6) 0.1554(16) 0.041(3) Uani 1 1 d .
H34 H -0.2748 0.3721 0.1744 0.050 Uiso 1 1 calc R
C35 C -0.2455(16) 0.2914(6) 0.0691(14) 0.041(3) Uani 1 1 d .
H35 H -0.3640 0.2810 0.0280 0.049 Uiso 1 1 calc R
C36 C -0.1276(16) 0.2528(6) 0.0448(15) 0.042(3) Uani 1 1 d .
H36 H -0.1640 0.2153 -0.0127 0.050 Uiso 1 1 calc R
C37 C 0.0540(14) 0.2687(5) 0.1061(12) 0.028(2) Uani 1 1 d .
C38 C 0.1759(15) 0.2278(6) 0.0856(15) 0.038(3) Uani 1 1 d .
H38 H 0.1394 0.1898 0.0304 0.046 Uiso 1 1 calc R
C39 C 0.3441(15) 0.2419(6) 0.1432(16) 0.042(3) Uani 1 1 d .
H39 H 0.4254 0.2134 0.1303 0.050 Uiso 1 1 calc R
C40 C 0.4019(14) 0.2997(6) 0.2238(14) 0.035(3) Uani 1 1 d .
H40 H 0.5207 0.3095 0.2631 0.042 Uiso 1 1 calc R
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ag1 0.0356(5) 0.0379(5) 0.0285(4) 0.0044(4) 0.0122(3) -0.0033(4)
S1 0.0352(15) 0.0359(14) 0.0259(13) -0.0005(11) 0.0107(11) -0.0052(12)
S2 0.0226(13) 0.0329(14) 0.0289(13) 0.0017(11) 0.0105(11) -0.0008(10)
S3 0.0257(14) 0.0336(14) 0.0271(12) 0.0012(11) 0.0084(11) 0.0018(10)
O31 0.054(5) 0.041(5) 0.030(4) -0.001(3) 0.019(4) 0.007(4)
O32 0.042(5) 0.035(4) 0.034(4) 0.004(3) 0.010(4) 0.003(4)
O33 0.027(4) 0.040(5) 0.057(5) -0.008(4) 0.015(4) -0.011(3)
C11 0.032(6) 0.041(6) 0.026(5) 0.004(5) 0.015(5) 0.005(5)
C12 0.027(6) 0.065(9) 0.042(7) 0.004(6) 0.015(6) 0.007(6)
C21 0.028(6) 0.051(7) 0.043(7) 0.012(6) 0.013(5) -0.005(5)
C31 0.018(5) 0.045(7) 0.030(5) 0.003(5) 0.009(4) -0.004(4)
C32 0.027(6) 0.033(6) 0.031(6) 0.006(5) 0.010(5) 0.002(4)
C33 0.016(5) 0.044(7) 0.039(6) 0.011(5) -0.002(5) -0.001(5)
C34 0.024(6) 0.044(7) 0.060(8) 0.011(6) 0.019(6) 0.000(5)
C35 0.031(6) 0.045(7) 0.042(7) 0.011(6) 0.008(5) 0.004(5)
C36 0.048(8) 0.040(7) 0.037(6) 0.006(5) 0.013(6) -0.004(5)
C37 0.030(6) 0.026(5) 0.025(5) -0.001(4) 0.007(5) -0.006(4)
C38 0.042(7) 0.037(7) 0.042(7) -0.006(5) 0.022(6) -0.005(5)
C39 0.030(7) 0.036(7) 0.066(9) -0.007(6) 0.024(6) 0.001(5)
C40 0.025(6) 0.043(7) 0.036(6) -0.002(5) 0.010(5) -0.002(5)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag 0.1306 4.2820 '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
O31 Ag1 S2 . . 120.88(19) y
O31 Ag1 S1 . . 95.03(19) y
S2 Ag1 S1 . . 143.45(10) y
O31 Ag1 O33 . 3_666 106.4(3) y
S2 Ag1 O33 . 3_666 87.6(2) y
S1 Ag1 O33 . 3_666 88.5(2) y
O31 Ag1 Ag1 . 3_566 105.2(2) y
S2 Ag1 Ag1 . 3_566 73.76(6) y
S1 Ag1 Ag1 . 3_566 91.48(7) y
O33 Ag1 Ag1 3_666 3_566 148.24(19) y
C11 S1 C12 . . 100.2(6) y
C11 S1 Ag1 . . 106.3(4) y
C12 S1 Ag1 . . 105.0(4) y
C11 S2 C21 3_566 . 98.7(5) y
C11 S2 Ag1 3_566 . 107.2(4) y
C21 S2 Ag1 . . 103.3(4) y
O33 S3 O32 . . 114.1(5) y
O33 S3 O31 . . 113.3(5) y
O32 S3 O31 . . 112.5(5) y
O33 S3 C31 . . 104.8(5) y
O32 S3 C31 . . 105.3(5) y
O31 S3 C31 . . 105.7(5) y
S3 O31 Ag1 . . 118.2(5) y
S3 O33 Ag1 . 3_666 136.1(5) y
S1 C11 S2 . 3_566 112.4(5) y
S1 C11 H11A . . 109.1 ?
S2 C11 H11A 3_566 . 109.1 ?
S1 C11 H11B . . 109.1 ?
S2 C11 H11B 3_566 . 109.1 ?
H11A C11 H11B . . 107.9 ?
S1 C12 H12A . . 109.5 ?
S1 C12 H12B . . 109.5 ?
H12A C12 H12B . . 109.5 ?
S1 C12 H12C . . 109.5 ?
H12A C12 H12C . . 109.5 ?
H12B C12 H12C . . 109.5 ?
S2 C21 H21A . . 109.5 ?
S2 C21 H21B . . 109.5 ?
H21A C21 H21B . . 109.5 ?
S2 C21 H21C . . 109.5 ?
H21A C21 H21C . . 109.5 ?
H21B C21 H21C . . 109.5 ?
C40 C31 C32 . . 120.6(10) y
C40 C31 S3 . . 117.2(8) y
C32 C31 S3 . . 122.1(8) y
C33 C32 C37 . . 118.6(11) y
C33 C32 C31 . . 124.2(10) y
C37 C32 C31 . . 117.2(10) y
C34 C33 C32 . . 119.3(11) y
C34 C33 H33 . . 120.4 ?
C32 C33 H33 . . 120.4 ?
C33 C34 C35 . . 123.4(12) y
C33 C34 H34 . . 118.2 ?
C35 C34 H34 . . 118.2 ?
C36 C35 C34 . . 119.5(13) y
C36 C35 H35 . . 120.3 ?
C34 C35 H35 . . 120.3 ?
C35 C36 C37 . . 120.5(11) y
C35 C36 H36 . . 119.7 ?
C37 C36 H36 . . 119.7 ?
C38 C37 C32 . . 121.0(11) y
C38 C37 C36 . . 120.3(10) y
C32 C37 C36 . . 118.6(11) y
C39 C38 C37 . . 120.7(12) y
C39 C38 H38 . . 119.7 ?
C37 C38 H38 . . 119.7 ?
C38 C39 C40 . . 120.6(12) y
C38 C39 H39 . . 119.7 ?
C40 C39 H39 . . 119.7 ?
C31 C40 C39 . . 119.8(11) y
C31 C40 H40 . . 120.1 ?
C39 C40 H40 . . 120.1 ?
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
Ag1 O31 . 2.425(8) y
Ag1 S2 . 2.471(3) y
Ag1 S1 . 2.505(3) y
Ag1 O33 3_666 2.553(7) y
Ag1 Ag1 3_566 3.2481(16) y
S1 C11 . 1.793(11) y
S1 C12 . 1.804(13) y
S2 C11 3_566 1.802(11) y
S2 C21 . 1.799(11) y
S3 O33 . 1.445(8) y
S3 O32 . 1.453(8) y
S3 O31 . 1.457(8) y
S3 C31 . 1.784(12) y
O33 Ag1 3_666 2.553(7) y
C11 S2 3_566 1.802(11) y
C11 H11A . 0.99 ?
C11 H11B . 0.99 ?
C12 H12A . 0.98 ?
C12 H12B . 0.98 ?
C12 H12C . 0.98 ?
C21 H21A . 0.98 ?
C21 H21B . 0.98 ?
C21 H21C . 0.98 ?
C31 C40 . 1.387(16) y
C31 C32 . 1.428(15) y
C32 C33 . 1.439(16) y
C32 C37 . 1.432(15) y
C33 C34 . 1.356(16) y
C33 H33 . 0.95 ?
C34 C35 . 1.401(18) y
C34 H34 . 0.95 ?
C35 C36 . 1.358(17) y
C35 H35 . 0.95 ?
C36 C37 . 1.457(16) y
C36 H36 . 0.95 ?
C37 C38 . 1.402(16) y
C38 C39 . 1.345(17) y
C38 H38 . 0.95 ?
C39 C40 . 1.434(17) y
C39 H39 . 0.95 ?
C40 H40 . 0.95 ?
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_4
_geom_torsion
O31 Ag1 S1 C11 . . -97.9(5)
S2 Ag1 S1 C11 . . 71.7(4)
O33 Ag1 S1 C11 3_666 . 155.8(4)
Ag1 Ag1 S1 C11 3_566 . 7.5(4)
O31 Ag1 S1 C12 . . 7.8(5)
S2 Ag1 S1 C12 . . 177.4(4)
O33 Ag1 S1 C12 3_666 . -98.6(5)
Ag1 Ag1 S1 C12 3_566 . 113.2(4)
O31 Ag1 S2 C11 . 3_566 36.5(4)
S1 Ag1 S2 C11 . 3_566 -131.5(4)
O33 Ag1 S2 C11 3_666 3_566 144.2(4)
Ag1 Ag1 S2 C11 3_566 3_566 -61.8(3)
O31 Ag1 S2 C21 . . -67.2(5)
S1 Ag1 S2 C21 . . 124.8(5)
O33 Ag1 S2 C21 3_666 . 40.5(5)
Ag1 Ag1 S2 C21 3_566 . -165.5(5)
O33 S3 O31 Ag1 . . 109.4(5)
O32 S3 O31 Ag1 . . -21.9(7)
C31 S3 O31 Ag1 . . -136.4(5)
S2 Ag1 O31 S3 . . 26.5(6)
S1 Ag1 O31 S3 . . -160.7(5)
O33 Ag1 O31 S3 3_666 . -70.8(6)
Ag1 Ag1 O31 S3 3_566 . 106.4(5)
O32 S3 O33 Ag1 . 3_666 53.4(9)
O31 S3 O33 Ag1 . 3_666 -77.2(8)
C31 S3 O33 Ag1 . 3_666 168.0(7)
C12 S1 C11 S2 . 3_566 -73.4(7)
Ag1 S1 C11 S2 . 3_566 35.7(7)
O33 S3 C31 C40 . . -0.3(10)
O32 S3 C31 C40 . . 120.4(9)
O31 S3 C31 C40 . . -120.3(9)
O33 S3 C31 C32 . . -178.2(9)
O32 S3 C31 C32 . . -57.6(10)
O31 S3 C31 C32 . . 61.8(10)
C40 C31 C32 C33 . . 175.9(11)
S3 C31 C32 C33 . . -6.2(16)
C40 C31 C32 C37 . . -1.7(16)
S3 C31 C32 C37 . . 176.1(8)
C37 C32 C33 C34 . . -1.9(17)
C31 C32 C33 C34 . . -179.4(11)
C32 C33 C34 C35 . . -0.9(19)
C33 C34 C35 C36 . . 2(2)
C34 C35 C36 C37 . . -0.7(18)
C33 C32 C37 C38 . . -176.6(11)
C31 C32 C37 C38 . . 1.2(16)
C33 C32 C37 C36 . . 3.2(15)
C31 C32 C37 C36 . . -179.1(10)
C35 C36 C37 C38 . . 177.8(12)
C35 C36 C37 C32 . . -1.9(17)
C32 C37 C38 C39 . . 0.3(18)
C36 C37 C38 C39 . . -179.4(12)
C37 C38 C39 C40 . . -1.4(19)
C32 C31 C40 C39 . . 0.8(17)
S3 C31 C40 C39 . . -177.1(9)
C38 C39 C40 C31 . . 0.8(19)
|
1501564.cif | #------------------------------------------------------------------------------
#$Date: 2020-10-02 18:49:34 +0300 (Fri, 02 Oct 2020) $
#$Revision: 256944 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/50/15/1501564.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_1501564
loop_
_publ_author_name
'Mohamed Osman Awaleh'
'Francois Brisse'
'Youssouf Djibril Soubaneh'
'Thierry Maris'
'Elias Said Dirieh'
_publ_section_title
;
Four New Ag(I) Coordination Polymers: Synthesis, Crystal Structures and
Thermal Stability
;
_journal_name_full 'J. Inorg. Organomet. Polym.'
_journal_page_first 816
_journal_page_last 824
_journal_paper_doi 10.1007/s10904-010-9407-0
_journal_volume 20
_journal_year 2010
_chemical_compound_source 'Synthesized by the authors. See text'
_chemical_formula_moiety 'C56 H56 Ag10 N10 O30 S8'
_chemical_formula_sum 'C56 H56 Ag10 N10 O30 S8'
_chemical_formula_weight 2684.29
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2yn'
_symmetry_space_group_name_H-M 'P 1 21/n 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 96.9290(10)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 9.6877(2)
_cell_length_b 25.1542(6)
_cell_length_c 32.2345(7)
_cell_measurement_reflns_used 15612
_cell_measurement_temperature 150(2)
_cell_measurement_theta_max 68.31
_cell_measurement_theta_min 2.76
_cell_volume 7797.7(3)
_computing_cell_refinement 'SMART (Bruker, 2003)'
_computing_data_collection 'SMART (Bruker, 2003)'
_computing_data_reduction 'SAINT (Bruker, 2004)'
_computing_molecular_graphics 'SHELXTL (Bruker, 1997)'
_computing_publication_material 'UdMX (local program)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 150(2)
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type 'Bruker Smart 6000'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'Sealed Tube'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.065
_diffrn_reflns_av_sigmaI/netI 0.0581
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 30
_diffrn_reflns_limit_k_min -30
_diffrn_reflns_limit_l_max 38
_diffrn_reflns_limit_l_min -38
_diffrn_reflns_number 103482
_diffrn_reflns_theta_full 68.64
_diffrn_reflns_theta_max 68.64
_diffrn_reflns_theta_min 2.23
_diffrn_standards_decay_% -1.63
_diffrn_standards_number 207
_exptl_absorpt_coefficient_mu 22.452
_exptl_absorpt_correction_T_max 0.2030
_exptl_absorpt_correction_T_min 0.1010
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Sadabs (Sheldrick,1996)'
_exptl_crystal_colour Colourless
_exptl_crystal_density_diffrn 2.286
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 5200
_exptl_crystal_size_max 0.14
_exptl_crystal_size_mid 0.10
_exptl_crystal_size_min 0.07
_refine_diff_density_max 1.158
_refine_diff_density_min -1.359
_refine_diff_density_rms 0.139
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.922
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 1027
_refine_ls_number_reflns 14270
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.922
_refine_ls_R_factor_all 0.0690
_refine_ls_R_factor_gt 0.0412
_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^)+(0.0547P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0963
_refine_ls_wR_factor_ref 0.1051
_reflns_number_gt 9349
_reflns_number_total 14270
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file deposit.cif
_cod_data_source_block complex4
_cod_depositor_comments
;
Updated values of the _geom_angle_atom_site_label_*,
_geom_bond_atom_site_label_* and _geom_torsion_atom_site_label_*
data items to establish relationships between loop packets from
different data loops.
Antanas Vaitkus,
2020-10-02
;
_cod_original_sg_symbol_H-M P21/n
_cod_database_code 1501564
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
Ag1 Ag -0.19774(6) 0.49553(2) 0.125089(19) 0.04860(16) Uani 1 1 d .
Ag2 Ag 0.13916(6) 0.57501(2) 0.207872(16) 0.04032(14) Uani 1 1 d .
Ag3 Ag 0.56785(6) 0.60273(2) 0.16023(2) 0.05206(17) Uani 1 1 d .
Ag4 Ag 0.68411(5) 0.74635(2) 0.214102(16) 0.03946(14) Uani 1 1 d .
Ag5 Ag 1.21218(5) 0.74713(2) 0.282372(16) 0.03893(14) Uani 1 1 d .
Ag6 Ag 1.14179(6) 0.60109(2) 0.33928(2) 0.05179(17) Uani 1 1 d .
Ag7 Ag 0.67132(6) 0.57634(2) 0.292789(17) 0.04119(14) Uani 1 1 d .
Ag8 Ag 0.40841(7) 0.48943(3) 0.38327(3) 0.0841(3) Uani 1 1 d .
Ag9 Ag 0.26770(5) 0.37006(2) 0.281999(17) 0.04212(14) Uani 1 1 d .
Ag10 Ag -0.25637(5) 0.36927(2) 0.217637(16) 0.04141(14) Uani 1 1 d .
S1 S -0.18608(17) 0.39350(7) 0.14713(5) 0.0334(4) Uani 1 1 d .
S2 S 0.05206(17) 0.49742(6) 0.15448(5) 0.0304(4) Uani 1 1 d .
S3 S 0.30441(17) 0.61655(6) 0.16134(5) 0.0304(4) Uani 1 1 d .
S4 S 0.55964(17) 0.70914(7) 0.14935(5) 0.0331(4) Uani 1 1 d .
S5 S 1.14392(17) 0.70744(7) 0.34682(5) 0.0328(4) Uani 1 1 d .
S6 S 0.87523(17) 0.61735(6) 0.33825(5) 0.0300(4) Uani 1 1 d .
S7 S 0.62364(17) 0.49827(6) 0.34734(6) 0.0334(4) Uani 1 1 d .
S8 S 0.39591(17) 0.39107(6) 0.35344(6) 0.0337(4) Uani 1 1 d .
O11 O -0.1611(4) 0.35375(19) 0.28866(15) 0.0373(11) Uani 1 1 d .
O12 O 0.0177(5) 0.3761(2) 0.25828(15) 0.0453(13) Uani 1 1 d .
O13 O 0.0467(5) 0.3534(2) 0.32289(15) 0.0449(13) Uani 1 1 d .
O21 O 0.3106(5) 0.35149(19) 0.21214(15) 0.0400(12) Uani 1 1 d .
O22 O 0.4911(5) 0.3510(2) 0.17794(15) 0.0458(13) Uani 1 1 d .
O23 O 0.5123(5) 0.3767(2) 0.24188(16) 0.0468(13) Uani 1 1 d .
O31 O 0.5852(7) 0.5320(3) 0.2324(2) 0.088(2) Uani 1 1 d .
O32 O 0.6295(6) 0.5019(3) 0.17529(19) 0.077(2) Uani 1 1 d .
O33 O 0.7559(6) 0.4784(2) 0.2322(2) 0.0706(19) Uani 1 1 d .
O41 O 0.6691(5) 0.5700(2) 0.09698(16) 0.0549(15) Uani 1 1 d .
O42 O 0.5764(6) 0.5813(2) 0.03394(17) 0.0613(16) Uani 1 1 d .
O43 O 0.6932(6) 0.5102(2) 0.05186(16) 0.0500(14) Uani 1 1 d .
O51 O 0.7389(5) 0.6392(2) 0.22807(16) 0.0512(14) Uani 1 1 d .
O52 O 0.8368(6) 0.6005(2) 0.17945(17) 0.0609(16) Uani 1 1 d .
O53 O 0.9638(6) 0.6307(2) 0.23352(19) 0.0624(17) Uani 1 1 d .
O61 O 0.9296(5) 0.7598(2) 0.24663(16) 0.0495(14) Uani 1 1 d .
O62 O 0.9099(6) 0.7539(3) 0.18023(17) 0.0633(17) Uani 1 1 d .
O63 O 1.1118(5) 0.7675(2) 0.21420(15) 0.0413(12) Uani 1 1 d .
O71 O 1.4646(6) 0.7562(2) 0.31692(16) 0.0561(15) Uani 1 1 d .
O72 O 1.4323(5) 0.7595(2) 0.25060(15) 0.0460(13) Uani 1 1 d .
O73 O 1.6412(5) 0.76657(19) 0.28232(15) 0.0387(12) Uani 1 1 d .
O81 O 1.2452(8) 0.5866(3) 0.4655(2) 0.101(3) Uani 1 1 d .
O82 O 1.2886(6) 0.5656(2) 0.40443(18) 0.0560(15) Uani 1 1 d .
O83 O 1.3499(8) 0.5128(4) 0.4534(3) 0.116(3) Uani 1 1 d .
O91 O 0.4807(6) 0.6330(2) 0.2662(2) 0.0683(18) Uani 1 1 d .
O92 O 0.2614(5) 0.6400(2) 0.27048(16) 0.0531(15) Uani 1 1 d .
O93 O 0.3944(6) 0.6026(2) 0.31974(18) 0.0585(15) Uani 1 1 d .
O121 O 0.2063(8) 0.5002(4) 0.3250(2) 0.102(3) Uani 1 1 d .
O122 O 0.1102(7) 0.5344(3) 0.2711(2) 0.086(2) Uani 1 1 d .
O123 O 0.2685(7) 0.4768(2) 0.2659(2) 0.0717(18) Uani 1 1 d .
N1 N -0.0312(6) 0.3615(2) 0.29021(17) 0.0333(13) Uani 1 1 d .
N2 N 0.4392(6) 0.3604(2) 0.21012(18) 0.0336(13) Uani 1 1 d .
N3 N 0.6584(7) 0.5036(2) 0.2137(2) 0.0411(15) Uani 1 1 d .
N4 N 0.6454(6) 0.5540(3) 0.06005(19) 0.0411(15) Uani 1 1 d .
N5 N 0.8484(6) 0.6236(2) 0.21337(19) 0.0390(14) Uani 1 1 d .
N6 N 0.9840(6) 0.7600(2) 0.21330(19) 0.0362(14) Uani 1 1 d .
N7 N 1.5123(6) 0.7605(2) 0.28364(18) 0.0352(14) Uani 1 1 d .
N8 N 1.2929(7) 0.5566(3) 0.4419(2) 0.0566(19) Uani 1 1 d .
N9 N 0.3805(6) 0.6254(2) 0.28510(19) 0.0381(14) Uani 1 1 d .
N12 N 0.1972(7) 0.5027(3) 0.2868(2) 0.0447(16) Uani 1 1 d .
C11 C -0.2417(7) 0.3486(3) 0.1058(2) 0.0327(16) Uani 1 1 d .
C12 C -0.1934(8) 0.2976(3) 0.1044(2) 0.0411(18) Uani 1 1 d .
H12 H -0.1241 0.2852 0.1255 0.049 Uiso 1 1 calc R
C13 C -0.2458(8) 0.2645(3) 0.0723(2) 0.0441(19) Uani 1 1 d .
H13 H -0.2096 0.2295 0.0711 0.053 Uiso 1 1 calc R
C14 C -0.3488(8) 0.2808(3) 0.0421(2) 0.0416(18) Uani 1 1 d .
H14 H -0.3853 0.2574 0.0204 0.050 Uiso 1 1 calc R
C15 C -0.3976(9) 0.3317(3) 0.0441(3) 0.058(2) Uani 1 1 d .
H15 H -0.4706 0.3434 0.0238 0.070 Uiso 1 1 calc R
C16 C -0.3423(9) 0.3663(3) 0.0750(2) 0.053(2) Uani 1 1 d .
H16 H -0.3735 0.4021 0.0751 0.064 Uiso 1 1 calc R
C17 C 0.0022(6) 0.3880(3) 0.1543(2) 0.0358(17) Uani 1 1 d .
H17A H 0.0302 0.3537 0.1679 0.043 Uiso 1 1 calc R
H17B H 0.0383 0.3892 0.1269 0.043 Uiso 1 1 calc R
C18 C 0.0620(7) 0.4343(2) 0.1818(2) 0.0331(16) Uani 1 1 d .
H18A H 0.1604 0.4266 0.1920 0.040 Uiso 1 1 calc R
H18B H 0.0105 0.4371 0.2064 0.040 Uiso 1 1 calc R
C21 C 0.1667(7) 0.4851(2) 0.1158(2) 0.0294(15) Uani 1 1 d .
C22 C 0.1135(7) 0.4808(3) 0.0743(2) 0.0350(16) Uani 1 1 d .
H22 H 0.0163 0.4832 0.0659 0.042 Uiso 1 1 calc R
C23 C 0.2063(8) 0.4727(3) 0.0451(2) 0.0421(18) Uani 1 1 d .
H23 H 0.1727 0.4707 0.0162 0.050 Uiso 1 1 calc R
C24 C 0.3476(8) 0.4678(3) 0.0580(2) 0.048(2) Uani 1 1 d .
H24 H 0.4108 0.4617 0.0381 0.057 Uiso 1 1 calc R
C25 C 0.3947(8) 0.4716(3) 0.0995(2) 0.0446(19) Uani 1 1 d .
H25 H 0.4916 0.4680 0.1081 0.054 Uiso 1 1 calc R
C26 C 0.3080(7) 0.4805(3) 0.1289(2) 0.0372(17) Uani 1 1 d .
H26 H 0.3431 0.4835 0.1576 0.045 Uiso 1 1 calc R
C31 C 0.2090(7) 0.6166(3) 0.1101(2) 0.0335(16) Uani 1 1 d .
C32 C 0.2805(8) 0.6089(3) 0.0754(2) 0.0418(18) Uani 1 1 d .
H32 H 0.3790 0.6061 0.0789 0.050 Uiso 1 1 calc R
C33 C 0.2082(11) 0.6054(3) 0.0369(3) 0.062(3) Uani 1 1 d .
H33 H 0.2565 0.5989 0.0134 0.075 Uiso 1 1 calc R
C34 C 0.0643(11) 0.6111(3) 0.0311(3) 0.064(3) Uani 1 1 d .
H34 H 0.0150 0.6091 0.0038 0.077 Uiso 1 1 calc R
C35 C -0.0057(9) 0.6197(3) 0.0647(3) 0.060(3) Uani 1 1 d .
H35 H -0.1039 0.6240 0.0607 0.071 Uiso 1 1 calc R
C36 C 0.0652(8) 0.6221(3) 0.1052(3) 0.048(2) Uani 1 1 d .
H36 H 0.0162 0.6274 0.1286 0.057 Uiso 1 1 calc R
C38 C 0.3731(6) 0.7225(2) 0.1459(2) 0.0312(15) Uani 1 1 d .
H38A H 0.3583 0.7601 0.1531 0.037 Uiso 1 1 calc R
H38B H 0.3300 0.7166 0.1168 0.037 Uiso 1 1 calc R
C39 C 0.3037(7) 0.6870(2) 0.1749(2) 0.0322(15) Uani 1 1 d .
H39A H 0.2062 0.6987 0.1750 0.039 Uiso 1 1 calc R
H39B H 0.3514 0.6915 0.2037 0.039 Uiso 1 1 calc R
C41 C 0.6038(6) 0.7428(3) 0.1038(2) 0.0304(15) Uani 1 1 d .
C42 C 0.6211(7) 0.7142(3) 0.0687(2) 0.0429(18) Uani 1 1 d .
H42 H 0.6119 0.6766 0.0685 0.051 Uiso 1 1 calc R
C43 C 0.6525(8) 0.7412(4) 0.0333(3) 0.055(2) Uani 1 1 d .
H43 H 0.6642 0.7219 0.0086 0.066 Uiso 1 1 calc R
C44 C 0.6666(7) 0.7957(4) 0.0338(2) 0.048(2) Uani 1 1 d .
H44 H 0.6871 0.8139 0.0094 0.058 Uiso 1 1 calc R
C45 C 0.6511(7) 0.8239(3) 0.0694(2) 0.0427(19) Uani 1 1 d .
H45 H 0.6613 0.8615 0.0697 0.051 Uiso 1 1 calc R
C46 C 0.6211(7) 0.7979(3) 0.1044(2) 0.0353(16) Uani 1 1 d .
H46 H 0.6119 0.8173 0.1292 0.042 Uiso 1 1 calc R
C51 C 1.2400(7) 0.7388(3) 0.3913(2) 0.0324(16) Uani 1 1 d .
C52 C 1.2327(8) 0.7930(3) 0.3971(2) 0.0462(19) Uani 1 1 d .
H52 H 1.1750 0.8143 0.3778 0.055 Uiso 1 1 calc R
C53 C 1.3100(8) 0.8162(3) 0.4314(2) 0.047(2) Uani 1 1 d .
H53 H 1.3041 0.8534 0.4359 0.057 Uiso 1 1 calc R
C54 C 1.3953(8) 0.7853(3) 0.4589(2) 0.0436(19) Uani 1 1 d .
H54 H 1.4506 0.8010 0.4820 0.052 Uiso 1 1 calc R
C55 C 1.3993(8) 0.7311(3) 0.4524(2) 0.051(2) Uani 1 1 d .
H55 H 1.4573 0.7097 0.4715 0.062 Uiso 1 1 calc R
C56 C 1.3214(8) 0.7076(3) 0.4190(2) 0.048(2) Uani 1 1 d .
H56 H 1.3240 0.6701 0.4153 0.057 Uiso 1 1 calc R
C57 C 0.9642(7) 0.7227(3) 0.3535(2) 0.0332(16) Uani 1 1 d .
H57A H 0.9492 0.7167 0.3829 0.040 Uiso 1 1 calc R
H57B H 0.9449 0.7606 0.3467 0.040 Uiso 1 1 calc R
C58 C 0.8655(7) 0.6879(3) 0.3252(2) 0.0343(16) Uani 1 1 d .
H58A H 0.8860 0.6924 0.2960 0.041 Uiso 1 1 calc R
H58B H 0.7692 0.7004 0.3265 0.041 Uiso 1 1 calc R
C61 C 0.8221(7) 0.6180(2) 0.3897(2) 0.0283(15) Uani 1 1 d .
C62 C 0.9228(7) 0.6165(3) 0.4238(2) 0.0346(16) Uani 1 1 d .
H62 H 1.0186 0.6166 0.4202 0.042 Uiso 1 1 calc R
C63 C 0.8816(8) 0.6148(3) 0.4636(2) 0.0452(19) Uani 1 1 d .
H63 H 0.9501 0.6140 0.4873 0.054 Uiso 1 1 calc R
C64 C 0.7434(9) 0.6143(3) 0.4692(2) 0.046(2) Uani 1 1 d .
H64 H 0.7164 0.6122 0.4966 0.055 Uiso 1 1 calc R
C65 C 0.6438(8) 0.6169(3) 0.4346(2) 0.0414(18) Uani 1 1 d .
H65 H 0.5479 0.6173 0.4382 0.050 Uiso 1 1 calc R
C66 C 0.6831(7) 0.6190(2) 0.3948(2) 0.0316(15) Uani 1 1 d .
H66 H 0.6146 0.6211 0.3712 0.038 Uiso 1 1 calc R
C71 C 0.7763(7) 0.4850(2) 0.3827(2) 0.0326(16) Uani 1 1 d .
C72 C 0.9017(7) 0.4797(3) 0.3674(2) 0.0356(16) Uani 1 1 d .
H72 H 0.9071 0.4826 0.3383 0.043 Uiso 1 1 calc R
C73 C 1.0214(8) 0.4700(3) 0.3950(3) 0.048(2) Uani 1 1 d .
H73 H 1.1088 0.4656 0.3849 0.057 Uiso 1 1 calc R
C74 C 1.0107(9) 0.4669(3) 0.4375(3) 0.050(2) Uani 1 1 d .
H74 H 1.0920 0.4607 0.4564 0.060 Uiso 1 1 calc R
C75 C 0.8869(9) 0.4724(3) 0.4525(2) 0.047(2) Uani 1 1 d .
H75 H 0.8817 0.4699 0.4816 0.057 Uiso 1 1 calc R
C76 C 0.7671(8) 0.4819(3) 0.4250(2) 0.0391(17) Uani 1 1 d .
H76 H 0.6799 0.4861 0.4353 0.047 Uiso 1 1 calc R
C77 C 0.6083(7) 0.4364(3) 0.3177(2) 0.0340(16) Uani 1 1 d .
H77A H 0.5326 0.4402 0.2943 0.041 Uiso 1 1 calc R
H77B H 0.6958 0.4303 0.3054 0.041 Uiso 1 1 calc R
C78 C 0.5783(6) 0.3880(3) 0.3438(2) 0.0335(16) Uani 1 1 d .
H78A H 0.6398 0.3882 0.3707 0.040 Uiso 1 1 calc R
H78B H 0.5956 0.3549 0.3287 0.040 Uiso 1 1 calc R
C81 C 0.3793(7) 0.3406(3) 0.3912(2) 0.0333(16) Uani 1 1 d .
C82 C 0.4768(7) 0.3007(3) 0.4015(2) 0.0395(17) Uani 1 1 d .
H82 H 0.5588 0.2993 0.3881 0.047 Uiso 1 1 calc R
C83 C 0.4543(8) 0.2633(3) 0.4311(2) 0.0425(18) Uani 1 1 d .
H83 H 0.5212 0.2361 0.4380 0.051 Uiso 1 1 calc R
C84 C 0.3374(7) 0.2647(3) 0.4507(2) 0.0399(18) Uani 1 1 d .
H84 H 0.3237 0.2388 0.4713 0.048 Uiso 1 1 calc R
C85 C 0.2390(7) 0.3036(3) 0.4406(2) 0.0417(18) Uani 1 1 d .
H85 H 0.1569 0.3043 0.4540 0.050 Uiso 1 1 calc R
C86 C 0.2596(7) 0.3420(3) 0.4110(2) 0.0369(17) Uani 1 1 d .
H86 H 0.1920 0.3690 0.4042 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
Ag1 0.0364(3) 0.0546(4) 0.0544(4) 0.0078(3) 0.0038(3) 0.0128(3)
Ag2 0.0423(3) 0.0441(3) 0.0356(3) 0.0003(2) 0.0091(2) -0.0065(2)
Ag3 0.0364(3) 0.0442(3) 0.0738(4) -0.0108(3) -0.0005(3) 0.0115(3)
Ag4 0.0323(3) 0.0442(3) 0.0412(3) -0.0042(2) 0.0018(2) 0.0008(2)
Ag5 0.0331(3) 0.0434(3) 0.0409(3) 0.0037(2) 0.0070(2) 0.0002(2)
Ag6 0.0443(4) 0.0407(3) 0.0735(4) 0.0013(3) 0.0202(3) 0.0079(3)
Ag7 0.0385(3) 0.0465(3) 0.0370(3) -0.0028(3) -0.0021(2) -0.0042(2)
Ag8 0.0434(4) 0.0731(5) 0.1408(8) -0.0513(5) 0.0321(4) -0.0021(3)
Ag9 0.0271(3) 0.0580(4) 0.0414(3) -0.0002(3) 0.0047(2) -0.0020(2)
Ag10 0.0277(3) 0.0586(4) 0.0380(3) 0.0028(3) 0.0046(2) -0.0015(2)
S1 0.0309(9) 0.0310(9) 0.0389(10) -0.0016(8) 0.0062(7) -0.0018(7)
S2 0.0304(9) 0.0272(9) 0.0344(9) 0.0012(7) 0.0073(7) -0.0013(7)
S3 0.0322(9) 0.0263(9) 0.0327(9) -0.0006(7) 0.0039(7) -0.0015(7)
S4 0.0281(9) 0.0330(9) 0.0378(10) 0.0013(8) 0.0023(7) -0.0018(7)
S5 0.0295(9) 0.0341(10) 0.0350(9) -0.0013(7) 0.0048(7) -0.0047(7)
S6 0.0299(9) 0.0288(9) 0.0310(9) 0.0008(7) 0.0023(7) -0.0044(7)
S7 0.0285(9) 0.0241(9) 0.0463(10) -0.0019(8) -0.0015(7) -0.0013(7)
S8 0.0274(9) 0.0291(9) 0.0442(10) 0.0020(8) 0.0026(7) -0.0004(7)
O11 0.021(3) 0.046(3) 0.044(3) 0.002(2) 0.001(2) -0.001(2)
O12 0.033(3) 0.056(3) 0.049(3) 0.020(3) 0.010(2) -0.003(2)
O13 0.037(3) 0.056(3) 0.040(3) 0.006(3) -0.002(2) -0.005(2)
O21 0.021(3) 0.045(3) 0.055(3) -0.002(2) 0.008(2) -0.002(2)
O22 0.041(3) 0.058(4) 0.041(3) -0.008(3) 0.015(2) -0.010(2)
O23 0.036(3) 0.060(4) 0.044(3) -0.017(3) 0.002(2) -0.011(2)
O31 0.075(5) 0.121(6) 0.064(4) -0.050(4) -0.012(4) 0.025(4)
O32 0.055(4) 0.127(6) 0.047(4) -0.023(4) 0.004(3) 0.013(4)
O33 0.059(4) 0.055(4) 0.091(5) -0.002(3) -0.021(4) 0.006(3)
O41 0.052(3) 0.077(4) 0.035(3) -0.009(3) 0.001(2) 0.018(3)
O42 0.082(4) 0.057(4) 0.043(3) 0.008(3) 0.000(3) 0.030(3)
O43 0.065(4) 0.038(3) 0.047(3) -0.005(3) 0.004(3) 0.017(3)
O51 0.045(3) 0.067(4) 0.043(3) 0.010(3) 0.012(2) 0.021(3)
O52 0.063(4) 0.069(4) 0.050(4) -0.020(3) 0.005(3) 0.010(3)
O53 0.035(3) 0.072(4) 0.076(4) -0.019(3) -0.011(3) 0.013(3)
O61 0.047(3) 0.061(4) 0.042(3) 0.000(3) 0.013(3) -0.006(3)
O62 0.054(4) 0.092(5) 0.040(3) 0.008(3) -0.006(3) -0.016(3)
O63 0.027(3) 0.050(3) 0.047(3) -0.001(2) 0.007(2) 0.003(2)
O71 0.049(3) 0.080(4) 0.041(3) -0.010(3) 0.012(3) -0.016(3)
O72 0.042(3) 0.057(4) 0.037(3) -0.006(3) -0.004(2) -0.007(2)
O73 0.027(3) 0.044(3) 0.045(3) 0.002(2) 0.005(2) 0.007(2)
O81 0.086(6) 0.134(7) 0.089(5) -0.039(5) 0.043(4) -0.005(5)
O82 0.052(4) 0.065(4) 0.051(4) -0.003(3) 0.005(3) 0.008(3)
O83 0.088(6) 0.122(7) 0.143(8) 0.072(6) 0.037(5) 0.036(5)
O91 0.049(4) 0.078(5) 0.083(4) 0.023(4) 0.029(3) 0.024(3)
O92 0.043(3) 0.073(4) 0.043(3) -0.007(3) 0.003(2) 0.016(3)
O93 0.051(4) 0.068(4) 0.056(4) 0.018(3) 0.004(3) 0.014(3)
O121 0.098(6) 0.157(8) 0.053(4) 0.027(5) 0.010(4) 0.024(5)
O122 0.085(5) 0.115(6) 0.064(4) 0.049(4) 0.031(4) 0.047(4)
O123 0.073(5) 0.061(4) 0.087(5) -0.012(4) 0.034(4) 0.007(3)
N1 0.031(3) 0.035(3) 0.035(3) 0.002(3) 0.006(3) -0.001(3)
N2 0.033(4) 0.029(3) 0.039(4) 0.000(3) 0.006(3) 0.002(2)
N3 0.047(4) 0.034(4) 0.043(4) -0.012(3) 0.011(3) -0.008(3)
N4 0.037(4) 0.050(4) 0.038(4) -0.001(3) 0.009(3) 0.000(3)
N5 0.040(4) 0.032(3) 0.046(4) 0.002(3) 0.009(3) 0.003(3)
N6 0.033(4) 0.028(3) 0.046(4) 0.010(3) 0.002(3) 0.003(3)
N7 0.036(4) 0.030(3) 0.040(4) -0.006(3) 0.005(3) 0.000(3)
N8 0.041(4) 0.067(5) 0.065(5) 0.012(4) 0.016(4) -0.001(4)
N9 0.033(4) 0.038(4) 0.042(4) 0.004(3) 0.002(3) 0.006(3)
N12 0.056(4) 0.037(4) 0.040(4) 0.010(3) 0.004(3) -0.002(3)
C11 0.028(4) 0.033(4) 0.039(4) 0.006(3) 0.009(3) -0.002(3)
C12 0.045(5) 0.032(4) 0.045(4) 0.005(4) 0.001(3) -0.002(3)
C13 0.057(5) 0.029(4) 0.046(5) -0.003(4) 0.007(4) 0.005(4)
C14 0.045(5) 0.041(5) 0.040(4) -0.005(4) 0.012(3) -0.006(4)
C15 0.063(6) 0.055(6) 0.052(5) -0.003(4) -0.017(4) 0.011(4)
C16 0.066(6) 0.037(5) 0.051(5) -0.006(4) -0.011(4) 0.015(4)
C17 0.025(4) 0.029(4) 0.053(5) 0.005(3) 0.005(3) -0.001(3)
C18 0.032(4) 0.032(4) 0.035(4) 0.007(3) 0.001(3) -0.005(3)
C21 0.035(4) 0.022(4) 0.031(4) -0.003(3) 0.004(3) -0.002(3)
C22 0.039(4) 0.026(4) 0.042(4) 0.001(3) 0.008(3) -0.005(3)
C23 0.054(5) 0.039(4) 0.035(4) -0.006(3) 0.012(4) -0.005(4)
C24 0.049(5) 0.045(5) 0.054(5) -0.010(4) 0.026(4) -0.005(4)
C25 0.033(4) 0.048(5) 0.054(5) -0.005(4) 0.013(4) 0.002(3)
C26 0.038(4) 0.032(4) 0.042(4) -0.006(3) 0.007(3) -0.001(3)
C31 0.035(4) 0.021(4) 0.042(4) 0.004(3) -0.004(3) -0.006(3)
C32 0.058(5) 0.037(4) 0.030(4) 0.000(3) 0.002(3) -0.010(4)
C33 0.107(8) 0.038(5) 0.042(5) 0.000(4) 0.009(5) -0.013(5)
C34 0.097(8) 0.036(5) 0.052(6) 0.003(4) -0.021(6) -0.007(5)
C35 0.056(6) 0.027(4) 0.088(7) 0.012(5) -0.026(5) -0.005(4)
C36 0.044(5) 0.030(4) 0.069(6) 0.014(4) 0.005(4) 0.001(3)
C38 0.030(4) 0.020(3) 0.042(4) 0.001(3) -0.003(3) 0.000(3)
C39 0.029(4) 0.030(4) 0.036(4) -0.004(3) 0.002(3) 0.002(3)
C41 0.023(4) 0.032(4) 0.035(4) -0.002(3) 0.002(3) 0.004(3)
C42 0.042(5) 0.038(4) 0.048(5) -0.008(4) 0.002(4) -0.003(3)
C43 0.036(5) 0.086(7) 0.045(5) -0.008(5) 0.016(4) -0.007(4)
C44 0.034(4) 0.068(6) 0.045(5) 0.010(4) 0.011(3) -0.006(4)
C45 0.026(4) 0.048(5) 0.055(5) 0.011(4) 0.005(3) -0.008(3)
C46 0.029(4) 0.039(4) 0.039(4) -0.002(3) 0.008(3) -0.002(3)
C51 0.034(4) 0.035(4) 0.028(4) 0.001(3) 0.005(3) -0.003(3)
C52 0.052(5) 0.037(5) 0.048(5) 0.006(4) 0.000(4) 0.001(4)
C53 0.059(5) 0.030(4) 0.053(5) -0.009(4) 0.007(4) -0.008(4)
C54 0.050(5) 0.045(5) 0.035(4) -0.007(4) 0.002(3) -0.007(4)
C55 0.049(5) 0.054(5) 0.048(5) -0.004(4) -0.006(4) 0.006(4)
C56 0.058(5) 0.036(4) 0.047(5) -0.007(4) -0.005(4) 0.006(4)
C57 0.035(4) 0.027(4) 0.039(4) 0.003(3) 0.010(3) 0.001(3)
C58 0.036(4) 0.029(4) 0.038(4) 0.008(3) 0.007(3) 0.001(3)
C61 0.034(4) 0.018(3) 0.032(4) 0.000(3) 0.001(3) -0.003(3)
C62 0.039(4) 0.029(4) 0.034(4) 0.005(3) -0.001(3) -0.003(3)
C63 0.054(5) 0.042(5) 0.036(4) 0.003(4) -0.011(4) -0.003(4)
C64 0.078(6) 0.033(4) 0.029(4) 0.000(3) 0.012(4) -0.002(4)
C65 0.047(5) 0.025(4) 0.055(5) -0.006(3) 0.021(4) 0.000(3)
C66 0.033(4) 0.024(4) 0.037(4) -0.003(3) 0.000(3) 0.002(3)
C71 0.027(4) 0.018(3) 0.052(5) 0.002(3) 0.001(3) -0.002(3)
C72 0.031(4) 0.033(4) 0.043(4) -0.002(3) 0.004(3) -0.003(3)
C73 0.031(4) 0.035(4) 0.076(6) 0.002(4) 0.003(4) -0.004(3)
C74 0.051(5) 0.032(4) 0.061(6) 0.007(4) -0.018(4) -0.007(4)
C75 0.062(6) 0.040(5) 0.037(4) 0.002(4) -0.004(4) 0.003(4)
C76 0.050(5) 0.025(4) 0.042(4) 0.000(3) 0.004(3) -0.003(3)
C77 0.030(4) 0.033(4) 0.038(4) 0.000(3) -0.002(3) -0.006(3)
C78 0.025(4) 0.031(4) 0.044(4) -0.004(3) 0.003(3) 0.003(3)
C81 0.034(4) 0.029(4) 0.035(4) -0.003(3) -0.001(3) -0.001(3)
C82 0.037(4) 0.038(4) 0.044(4) -0.004(4) 0.004(3) -0.001(3)
C83 0.046(5) 0.037(4) 0.044(5) 0.002(4) 0.001(4) 0.002(3)
C84 0.032(4) 0.049(5) 0.037(4) 0.003(3) -0.003(3) -0.010(3)
C85 0.034(4) 0.057(5) 0.035(4) -0.007(4) 0.006(3) -0.007(4)
C86 0.030(4) 0.037(4) 0.043(4) -0.007(3) 0.003(3) 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 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag 0.1306 4.2820 '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
O41 Ag1 O32 1_455 1_455 79.6(2) y
O41 Ag1 S2 1_455 . 125.76(15) y
O32 Ag1 S2 1_455 . 116.98(14) y
O41 Ag1 O43 1_455 1_455 51.52(16) y
O32 Ag1 O43 1_455 1_455 111.55(19) y
S2 Ag1 O43 . 1_455 129.66(14) y
O41 Ag1 S1 1_455 . 149.38(15) y
O32 Ag1 S1 1_455 . 84.15(18) y
S2 Ag1 S1 . . 84.77(5) y
O43 Ag1 S1 1_455 . 113.26(13) y
O122 Ag2 O53 . 1_455 77.9(2) y
O122 Ag2 S3 . . 147.86(18) y
O53 Ag2 S3 1_455 . 118.70(16) y
O122 Ag2 S2 . . 100.5(2) y
O53 Ag2 S2 1_455 . 117.54(14) y
S3 Ag2 S2 . . 95.31(5) y
O41 Ag3 S3 . . 122.71(13) y
O41 Ag3 S4 . . 103.18(14) y
S3 Ag3 S4 . . 81.63(5) y
O73 Ag4 S4 1_455 . 138.85(12) y
O73 Ag4 O61 1_455 . 81.07(16) y
S4 Ag4 O61 . . 138.47(12) y
O73 Ag4 O62 1_455 . 129.80(17) y
S4 Ag4 O62 . . 91.30(13) y
O61 Ag4 O62 . . 49.68(16) y
O63 Ag5 S5 . . 138.86(12) y
O63 Ag5 O72 . . 82.35(16) y
S5 Ag5 O72 . . 136.54(12) y
O63 Ag5 O71 . . 130.57(17) y
S5 Ag5 O71 . . 90.50(13) y
O72 Ag5 O71 . . 49.56(16) y
O82 Ag6 O93 . 1_655 75.94(18) y
O82 Ag6 S6 . . 121.17(13) y
O93 Ag6 S6 1_655 . 162.39(13) y
O82 Ag6 S5 . . 106.05(13) y
O93 Ag6 S5 1_655 . 90.57(14) y
S6 Ag6 S5 . . 80.90(5) y
O31 Ag7 O91 . . 78.6(2) y
O31 Ag7 S6 . . 149.44(18) y
O91 Ag7 S6 . . 118.46(17) y
O31 Ag7 S7 . . 97.1(2) y
O91 Ag7 S7 . . 118.44(15) y
S6 Ag7 S7 . . 95.84(5) y
O82 Ag8 O83 1_455 1_455 51.1(2) y
O82 Ag8 S7 1_455 . 121.37(15) y
O83 Ag8 S7 1_455 . 134.1(2) y
O82 Ag8 O121 1_455 . 76.6(2) y
O83 Ag8 O121 1_455 . 114.0(2) y
S7 Ag8 O121 . . 104.84(17) y
O82 Ag8 S8 1_455 . 148.40(14) y
O83 Ag8 S8 1_455 . 123.3(2) y
S7 Ag8 S8 . . 85.39(5) y
O121 Ag8 S8 . . 80.5(2) y
O21 Ag9 O12 . . 89.76(16) y
O21 Ag9 S8 . . 140.90(11) y
O12 Ag9 S8 . . 128.78(13) y
O11 Ag10 O23 . 1_455 88.26(16) y
O11 Ag10 S1 . . 141.74(11) y
O23 Ag10 S1 1_455 . 128.36(13) y
C11 S1 C17 . . 104.8(3) y
C11 S1 Ag10 . . 115.5(2) y
C17 S1 Ag10 . . 104.0(2) y
C11 S1 Ag1 . . 114.4(2) y
C17 S1 Ag1 . . 96.8(2) y
Ag10 S1 Ag1 . . 117.76(7) y
C21 S2 C18 . . 100.7(3) y
C21 S2 Ag1 . . 112.7(2) y
C18 S2 Ag1 . . 99.2(2) y
C21 S2 Ag2 . . 113.6(2) y
C18 S2 Ag2 . . 109.5(2) y
Ag1 S2 Ag2 . . 118.43(6) y
C31 S3 C39 . . 101.8(3) y
C31 S3 Ag2 . . 104.6(2) y
C39 S3 Ag2 . . 103.7(2) y
C31 S3 Ag3 . . 112.9(2) y
C39 S3 Ag3 . . 99.6(2) y
Ag2 S3 Ag3 . . 130.24(7) y
C41 S4 C38 . . 101.3(3) y
C41 S4 Ag4 . . 111.9(2) y
C38 S4 Ag4 . . 111.2(2) y
C41 S4 Ag3 . . 124.7(2) y
C38 S4 Ag3 . . 101.7(2) y
Ag4 S4 Ag3 . . 105.23(6) y
C51 S5 C57 . . 103.0(3) y
C51 S5 Ag5 . . 109.2(2) y
C57 S5 Ag5 . . 111.8(2) y
C51 S5 Ag6 . . 120.5(2) y
C57 S5 Ag6 . . 102.9(2) y
Ag5 S5 Ag6 . . 109.08(6) y
C61 S6 C58 . . 101.1(3) y
C61 S6 Ag7 . . 104.3(2) y
C58 S6 Ag7 . . 104.3(2) y
C61 S6 Ag6 . . 112.5(2) y
C58 S6 Ag6 . . 100.3(2) y
Ag7 S6 Ag6 . . 130.14(7) y
C71 S7 C77 . . 100.6(3) y
C71 S7 Ag8 . . 111.0(2) y
C77 S7 Ag8 . . 98.4(2) y
C71 S7 Ag7 . . 110.9(2) y
C77 S7 Ag7 . . 106.7(2) y
Ag8 S7 Ag7 . . 125.32(7) y
C81 S8 C78 . . 104.7(3) y
C81 S8 Ag9 . . 113.4(2) y
C78 S8 Ag9 . . 102.4(2) y
C81 S8 Ag8 . . 114.9(2) y
C78 S8 Ag8 . . 95.6(2) y
Ag9 S8 Ag8 . . 121.30(7) y
N1 O11 Ag10 . . 106.2(4) y
N1 O12 Ag9 . . 100.6(4) y
N2 O21 Ag9 . . 107.3(4) y
N2 O23 Ag10 . 1_655 99.4(4) y
N3 O31 Ag7 . . 121.9(5) y
N3 O32 Ag1 . 1_655 124.7(5) y
N4 O41 Ag1 . 1_655 97.8(4) y
N4 O41 Ag3 . . 146.6(4) y
Ag1 O41 Ag3 1_655 . 101.26(19) y
N4 O43 Ag1 . 1_655 93.2(4) y
N5 O53 Ag2 . 1_655 111.4(4) y
N6 O61 Ag4 . . 96.8(4) y
N6 O62 Ag4 . . 94.6(4) y
N6 O63 Ag5 . . 106.7(4) y
N7 O71 Ag5 . . 93.9(4) y
N7 O72 Ag5 . . 97.3(4) y
N7 O73 Ag4 . 1_655 107.0(4) y
N8 O82 Ag8 . 1_655 100.0(5) y
N8 O82 Ag6 . . 145.7(5) y
Ag8 O82 Ag6 1_655 . 106.8(2) y
N8 O83 Ag8 . 1_655 94.5(6) y
N9 O91 Ag7 . . 110.6(5) y
N9 O93 Ag6 . 1_455 102.7(4) y
N12 O121 Ag8 . . 134.4(6) y
N12 O122 Ag2 . . 119.9(5) y
O13 N1 O12 . . 120.1(6) y
O13 N1 O11 . . 120.6(5) y
O12 N1 O11 . . 119.3(6) y
O22 N2 O23 . . 120.6(6) y
O22 N2 O21 . . 120.7(6) y
O23 N2 O21 . . 118.6(6) y
O31 N3 O33 . . 121.5(7) y
O31 N3 O32 . . 116.2(7) y
O33 N3 O32 . . 122.3(7) y
O42 N4 O43 . . 122.8(6) y
O42 N4 O41 . . 119.7(6) y
O43 N4 O41 . . 117.4(6) y
O52 N5 O53 . . 120.9(6) y
O52 N5 O51 . . 119.0(6) y
O53 N5 O51 . . 120.1(6) y
O62 N6 O63 . . 121.1(6) y
O62 N6 O61 . . 119.0(6) y
O63 N6 O61 . . 119.9(6) y
O71 N7 O72 . . 119.3(6) y
O71 N7 O73 . . 121.3(6) y
O72 N7 O73 . . 119.4(6) y
O81 N8 O82 . . 122.5(8) y
O81 N8 O83 . . 123.2(9) y
O82 N8 O83 . . 114.4(8) y
O91 N9 O92 . . 121.3(6) y
O91 N9 O93 . . 120.8(6) y
O92 N9 O93 . . 117.9(6) y
O123 N12 O121 . . 123.8(8) y
O123 N12 O122 . . 122.0(7) y
O121 N12 O122 . . 114.2(8) y
C12 C11 C16 . . 119.7(7) y
C12 C11 S1 . . 123.1(6) y
C16 C11 S1 . . 117.1(5) y
C11 C12 C13 . . 119.7(7) y
C11 C12 H12 . . 120.1 ?
C13 C12 H12 . . 120.1 ?
C14 C13 C12 . . 121.6(7) y
C14 C13 H13 . . 119.2 ?
C12 C13 H13 . . 119.2 ?
C15 C14 C13 . . 118.2(7) y
C15 C14 H14 . . 120.9 ?
C13 C14 H14 . . 120.9 ?
C14 C15 C16 . . 121.1(8) y
C14 C15 H15 . . 119.5 ?
C16 C15 H15 . . 119.5 ?
C11 C16 C15 . . 119.6(7) y
C11 C16 H16 . . 120.2 ?
C15 C16 H16 . . 120.2 ?
C18 C17 S1 . . 108.6(5) y
C18 C17 H17A . . 110 ?
S1 C17 H17A . . 110 ?
C18 C17 H17B . . 110 ?
S1 C17 H17B . . 110 ?
H17A C17 H17B . . 108.3 ?
C17 C18 S2 . . 113.0(5) y
C17 C18 H18A . . 109 ?
S2 C18 H18A . . 109 ?
C17 C18 H18B . . 109 ?
S2 C18 H18B . . 109 ?
H18A C18 H18B . . 107.8 ?
C22 C21 C26 . . 122.0(6) y
C22 C21 S2 . . 119.9(5) y
C26 C21 S2 . . 118.2(5) y
C21 C22 C23 . . 118.1(7) y
C21 C22 H22 . . 121 ?
C23 C22 H22 . . 121 ?
C24 C23 C22 . . 120.3(7) y
C24 C23 H23 . . 119.8 ?
C22 C23 H23 . . 119.8 ?
C25 C24 C23 . . 119.2(7) y
C25 C24 H24 . . 120.4 ?
C23 C24 H24 . . 120.4 ?
C26 C25 C24 . . 122.3(7) y
C26 C25 H25 . . 118.9 ?
C24 C25 H25 . . 118.9 ?
C25 C26 C21 . . 118.1(7) y
C25 C26 H26 . . 121 ?
C21 C26 H26 . . 121 ?
C36 C31 C32 . . 120.5(7) y
C36 C31 S3 . . 120.3(6) y
C32 C31 S3 . . 119.1(5) y
C33 C32 C31 . . 119.5(8) y
C33 C32 H32 . . 120.3 ?
C31 C32 H32 . . 120.3 ?
C32 C33 C34 . . 121.0(9) y
C32 C33 H33 . . 119.5 ?
C34 C33 H33 . . 119.5 ?
C35 C34 C33 . . 119.7(8) y
C35 C34 H34 . . 120.2 ?
C33 C34 H34 . . 120.2 ?
C34 C35 C36 . . 120.8(8) y
C34 C35 H35 . . 119.6 ?
C36 C35 H35 . . 119.6 ?
C31 C36 C35 . . 118.4(8) y
C31 C36 H36 . . 120.8 ?
C35 C36 H36 . . 120.8 ?
C39 C38 S4 . . 111.4(4) y
C39 C38 H38A . . 109.4 ?
S4 C38 H38A . . 109.4 ?
C39 C38 H38B . . 109.4 ?
S4 C38 H38B . . 109.4 ?
H38A C38 H38B . . 108 ?
C38 C39 S3 . . 114.2(5) y
C38 C39 H39A . . 108.7 ?
S3 C39 H39A . . 108.7 ?
C38 C39 H39B . . 108.7 ?
S3 C39 H39B . . 108.7 ?
H39A C39 H39B . . 107.6 ?
C42 C41 C46 . . 120.4(7) y
C42 C41 S4 . . 119.7(5) y
C46 C41 S4 . . 119.9(5) y
C41 C42 C43 . . 118.8(7) y
C41 C42 H42 . . 120.6 ?
C43 C42 H42 . . 120.6 ?
C44 C43 C42 . . 120.5(8) y
C44 C43 H43 . . 119.8 ?
C42 C43 H43 . . 119.8 ?
C45 C44 C43 . . 120.2(7) y
C45 C44 H44 . . 119.9 ?
C43 C44 H44 . . 119.9 ?
C46 C45 C44 . . 120.0(7) y
C46 C45 H45 . . 120 ?
C44 C45 H45 . . 120 ?
C45 C46 C41 . . 120.1(7) y
C45 C46 H46 . . 119.9 ?
C41 C46 H46 . . 119.9 ?
C56 C51 C52 . . 120.9(7) y
C56 C51 S5 . . 118.2(6) y
C52 C51 S5 . . 120.9(5) y
C51 C52 C53 . . 119.6(7) y
C51 C52 H52 . . 120.2 ?
C53 C52 H52 . . 120.2 ?
C54 C53 C52 . . 119.9(7) y
C54 C53 H53 . . 120 ?
C52 C53 H53 . . 120 ?
C53 C54 C55 . . 119.1(7) y
C53 C54 H54 . . 120.4 ?
C55 C54 H54 . . 120.4 ?
C56 C55 C54 . . 121.5(8) y
C56 C55 H55 . . 119.3 ?
C54 C55 H55 . . 119.3 ?
C51 C56 C55 . . 119.0(7) y
C51 C56 H56 . . 120.5 ?
C55 C56 H56 . . 120.5 ?
C58 C57 S5 . . 110.5(5) y
C58 C57 H57A . . 109.6 ?
S5 C57 H57A . . 109.6 ?
C58 C57 H57B . . 109.6 ?
S5 C57 H57B . . 109.6 ?
H57A C57 H57B . . 108.1 ?
C57 C58 S6 . . 114.3(5) y
C57 C58 H58A . . 108.7 ?
S6 C58 H58A . . 108.7 ?
C57 C58 H58B . . 108.7 ?
S6 C58 H58B . . 108.7 ?
H58A C58 H58B . . 107.6 ?
C66 C61 C62 . . 120.9(6) y
C66 C61 S6 . . 120.3(5) y
C62 C61 S6 . . 118.8(5) y
C61 C62 C63 . . 118.8(7) y
C61 C62 H62 . . 120.6 ?
C63 C62 H62 . . 120.6 ?
C64 C63 C62 . . 121.2(7) y
C64 C63 H63 . . 119.4 ?
C62 C63 H63 . . 119.4 ?
C63 C64 C65 . . 119.1(7) y
C63 C64 H64 . . 120.4 ?
C65 C64 H64 . . 120.4 ?
C66 C65 C64 . . 120.4(7) y
C66 C65 H65 . . 119.8 ?
C64 C65 H65 . . 119.8 ?
C61 C66 C65 . . 119.6(7) y
C61 C66 H66 . . 120.2 ?
C65 C66 H66 . . 120.2 ?
C72 C71 C76 . . 121.0(7) y
C72 C71 S7 . . 119.4(6) y
C76 C71 S7 . . 119.6(5) y
C71 C72 C73 . . 119.5(7) y
C71 C72 H72 . . 120.3 ?
C73 C72 H72 . . 120.3 ?
C74 C73 C72 . . 118.9(7) y
C74 C73 H73 . . 120.5 ?
C72 C73 H73 . . 120.5 ?
C75 C74 C73 . . 121.4(7) y
C75 C74 H74 . . 119.3 ?
C73 C74 H74 . . 119.3 ?
C74 C75 C76 . . 119.8(7) y
C74 C75 H75 . . 120.1 ?
C76 C75 H75 . . 120.1 ?
C71 C76 C75 . . 119.3(7) y
C71 C76 H76 . . 120.4 ?
C75 C76 H76 . . 120.4 ?
C78 C77 S7 . . 113.5(5) y
C78 C77 H77A . . 108.9 ?
S7 C77 H77A . . 108.9 ?
C78 C77 H77B . . 108.9 ?
S7 C77 H77B . . 108.9 ?
H77A C77 H77B . . 107.7 ?
C77 C78 S8 . . 108.1(4) y
C77 C78 H78A . . 110.1 ?
S8 C78 H78A . . 110.1 ?
C77 C78 H78B . . 110.1 ?
S8 C78 H78B . . 110.1 ?
H78A C78 H78B . . 108.4 ?
C86 C81 C82 . . 119.2(7) y
C86 C81 S8 . . 116.5(5) y
C82 C81 S8 . . 124.3(6) y
C83 C82 C81 . . 120.0(7) y
C83 C82 H82 . . 120 ?
C81 C82 H82 . . 120 ?
C84 C83 C82 . . 120.9(7) y
C84 C83 H83 . . 119.5 ?
C82 C83 H83 . . 119.5 ?
C83 C84 C85 . . 119.9(7) y
C83 C84 H84 . . 120 ?
C85 C84 H84 . . 120 ?
C84 C85 C86 . . 120.2(7) y
C84 C85 H85 . . 119.9 ?
C86 C85 H85 . . 119.9 ?
C85 C86 C81 . . 119.7(7) y
C85 C86 H86 . . 120.1 ?
C81 C86 H86 . . 120.1 ?
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
Ag1 O41 1_455 2.391(5) y
Ag1 O32 1_455 2.469(6) y
Ag1 S2 . 2.4905(17) y
Ag1 O43 1_455 2.495(5) y
Ag1 S1 . 2.6616(18) y
Ag2 O122 . 2.328(6) y
Ag2 O53 1_455 2.423(5) y
Ag2 S3 . 2.5463(17) y
Ag2 S2 . 2.6708(17) y
Ag3 O41 . 2.505(5) y
Ag3 S3 . 2.5802(17) y
Ag3 S4 . 2.6994(18) y
Ag4 O73 1_455 2.342(5) y
Ag4 S4 . 2.4658(18) y
Ag4 O61 . 2.504(5) y
Ag4 O62 . 2.567(6) y
Ag5 O63 . 2.350(5) y
Ag5 S5 . 2.4659(17) y
Ag5 O72 . 2.494(5) y
Ag5 O71 . 2.572(5) y
Ag6 O82 . 2.552(6) y
Ag6 O93 1_655 2.600(5) y
Ag6 S6 . 2.6108(17) y
Ag6 S5 . 2.6861(18) y
Ag7 O31 . 2.311(6) y
Ag7 O91 . 2.407(6) y
Ag7 S6 . 2.5330(17) y
Ag7 S7 . 2.7126(18) y
Ag8 O82 1_455 2.382(5) y
Ag8 O83 1_455 2.467(9) y
Ag8 S7 . 2.5143(19) y
Ag8 O121 . 2.559(7) y
Ag8 S8 . 2.6519(18) y
Ag9 O21 . 2.385(5) y
Ag9 O12 . 2.455(5) y
Ag9 S8 . 2.5368(18) y
Ag10 O11 . 2.395(5) y
Ag10 O23 1_455 2.468(5) y
Ag10 S1 . 2.5246(18) y
S1 C11 . 1.781(7) y
S1 C17 . 1.816(6) y
S2 C21 . 1.794(7) y
S2 C18 . 1.813(6) y
S3 C31 . 1.792(7) y
S3 C39 . 1.825(6) y
S4 C41 . 1.790(7) y
S4 C38 . 1.828(6) y
S5 C51 . 1.795(7) y
S5 C57 . 1.820(7) y
S6 C61 . 1.796(7) y
S6 C58 . 1.824(6) y
S7 C71 . 1.786(7) y
S7 C77 . 1.823(7) y
S8 C81 . 1.779(7) y
S8 C78 . 1.832(6) y
O11 N1 . 1.269(7) y
O12 N1 . 1.240(7) y
O13 N1 . 1.236(7) y
O21 N2 . 1.276(7) y
O22 N2 . 1.229(7) y
O23 N2 . 1.243(7) y
O23 Ag10 1_655 2.468(5) y
O31 N3 . 1.215(8) y
O32 N3 . 1.237(8) y
O32 Ag1 1_655 2.469(6) y
O33 N3 . 1.231(8) y
O41 N4 . 1.252(7) y
O41 Ag1 1_655 2.391(5) y
O42 N4 . 1.221(7) y
O43 N4 . 1.235(7) y
O43 Ag1 1_655 2.495(5) y
O51 N5 . 1.275(7) y
O52 N5 . 1.232(7) y
O53 N5 . 1.236(7) y
O53 Ag2 1_655 2.423(5) y
O61 N6 . 1.252(7) y
O62 N6 . 1.221(7) y
O63 N6 . 1.249(7) y
O71 N7 . 1.223(7) y
O72 N7 . 1.239(7) y
O73 N7 . 1.264(7) y
O73 Ag4 1_655 2.342(5) y
O81 N8 . 1.203(9) y
O82 N8 . 1.223(8) y
O82 Ag8 1_655 2.382(5) y
O83 N8 . 1.268(9) y
O83 Ag8 1_655 2.467(9) y
O91 N9 . 1.222(8) y
O92 N9 . 1.247(7) y
O93 N9 . 1.248(7) y
O93 Ag6 1_455 2.600(5) y
O121 N12 . 1.225(8) y
O122 N12 . 1.225(8) y
O123 N12 . 1.211(8) y
C11 C12 . 1.366(9) y
C11 C16 . 1.378(10) y
C12 C13 . 1.376(10) y
C12 H12 . 0.95 ?
C13 C14 . 1.37(1) y
C13 H13 . 0.95 ?
C14 C15 . 1.369(10) y
C14 H14 . 0.95 ?
C15 C16 . 1.383(11) y
C15 H15 . 0.95 ?
C16 H16 . 0.95 ?
C17 C18 . 1.533(9) y
C17 H17A . 0.99 ?
C17 H17B . 0.99 ?
C18 H18A . 0.99 ?
C18 H18B . 0.99 ?
C21 C22 . 1.378(9) y
C21 C26 . 1.388(9) y
C22 C23 . 1.393(9) y
C22 H22 . 0.95 ?
C23 C24 . 1.387(10) y
C23 H23 . 0.95 ?
C24 C25 . 1.365(10) y
C24 H24 . 0.95 ?
C25 C26 . 1.36(1) y
C25 H25 . 0.95 ?
C26 H26 . 0.95 ?
C31 C36 . 1.39(1) y
C31 C32 . 1.399(10) y
C32 C33 . 1.354(11) y
C32 H32 . 0.95 ?
C33 C34 . 1.392(13) y
C33 H33 . 0.95 ?
C34 C35 . 1.365(13) y
C34 H34 . 0.95 ?
C35 C36 . 1.399(11) y
C35 H35 . 0.95 ?
C36 H36 . 0.95 ?
C38 C39 . 1.509(9) y
C38 H38A . 0.99 ?
C38 H38B . 0.99 ?
C39 H39A . 0.99 ?
C39 H39B . 0.99 ?
C41 C42 . 1.369(9) y
C41 C46 . 1.396(9) y
C42 C43 . 1.394(11) y
C42 H42 . 0.95 ?
C43 C44 . 1.378(11) y
C43 H43 . 0.95 ?
C44 C45 . 1.373(11) y
C44 H44 . 0.95 ?
C45 C46 . 1.366(9) y
C45 H45 . 0.95 ?
C46 H46 . 0.95 ?
C51 C56 . 1.368(10) y
C51 C52 . 1.378(10) y
C52 C53 . 1.386(10) y
C52 H52 . 0.95 ?
C53 C54 . 1.378(10) y
C53 H53 . 0.95 ?
C54 C55 . 1.379(10) y
C54 H54 . 0.95 ?
C55 C56 . 1.372(10) y
C55 H55 . 0.95 ?
C56 H56 . 0.95 ?
C57 C58 . 1.517(9) y
C57 H57A . 0.99 ?
C57 H57B . 0.99 ?
C58 H58A . 0.99 ?
C58 H58B . 0.99 ?
C61 C66 . 1.376(9) y
C61 C62 . 1.380(9) y
C62 C63 . 1.387(10) y
C62 H62 . 0.95 ?
C63 C64 . 1.373(11) y
C63 H63 . 0.95 ?
C64 C65 . 1.388(10) y
C64 H64 . 0.95 ?
C65 C66 . 1.380(9) y
C65 H65 . 0.95 ?
C66 H66 . 0.95 ?
C71 C72 . 1.372(9) y
C71 C76 . 1.38(1) y
C72 C73 . 1.395(10) y
C72 H72 . 0.95 ?
C73 C74 . 1.386(11) y
C73 H73 . 0.95 ?
C74 C75 . 1.353(11) y
C74 H74 . 0.95 ?
C75 C76 . 1.392(10) y
C75 H75 . 0.95 ?
C76 H76 . 0.95 ?
C77 C78 . 1.530(9) y
C77 H77A . 0.99 ?
C77 H77B . 0.99 ?
C78 H78A . 0.99 ?
C78 H78B . 0.99 ?
C81 C86 . 1.389(9) y
C81 C82 . 1.391(9) y
C82 C83 . 1.377(10) y
C82 H82 . 0.95 ?
C83 C84 . 1.362(10) y
C83 H83 . 0.95 ?
C84 C85 . 1.379(10) y
C84 H84 . 0.95 ?
C85 C86 . 1.389(10) y
C85 H85 . 0.95 ?
C86 H86 . 0.95 ?
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_4
_geom_torsion
O11 Ag10 S1 C11 . . 125.0(3)
O23 Ag10 S1 C11 1_455 . -74.8(3)
O11 Ag10 S1 C17 . . 10.8(3)
O23 Ag10 S1 C17 1_455 . 171.0(3)
O11 Ag10 S1 Ag1 . . -94.8(2)
O23 Ag10 S1 Ag1 1_455 . 65.42(17)
O41 Ag1 S1 C11 1_455 . 58.5(4)
O32 Ag1 S1 C11 1_455 . 116.6(3)
S2 Ag1 S1 C11 . . -125.5(2)
O43 Ag1 S1 C11 1_455 . 5.6(3)
O41 Ag1 S1 C17 1_455 . 168.2(3)
O32 Ag1 S1 C17 1_455 . -133.7(3)
S2 Ag1 S1 C17 . . -15.9(2)
O43 Ag1 S1 C17 1_455 . 115.3(3)
O41 Ag1 S1 Ag10 1_455 . -82.1(3)
O32 Ag1 S1 Ag10 1_455 . -23.97(15)
S2 Ag1 S1 Ag10 . . 93.89(7)
O43 Ag1 S1 Ag10 1_455 . -134.94(15)
O41 Ag1 S2 C21 1_455 . -89.8(3)
O32 Ag1 S2 C21 1_455 . 173.5(3)
O43 Ag1 S2 C21 1_455 . -23.3(3)
S1 Ag1 S2 C21 . . 92.8(2)
O41 Ag1 S2 C18 1_455 . 164.5(3)
O32 Ag1 S2 C18 1_455 . 67.7(3)
O43 Ag1 S2 C18 1_455 . -129.0(3)
S1 Ag1 S2 C18 . . -13.0(2)
O41 Ag1 S2 Ag2 1_455 . 46.33(17)
O32 Ag1 S2 Ag2 1_455 . -50.4(2)
O43 Ag1 S2 Ag2 1_455 . 112.82(16)
S1 Ag1 S2 Ag2 . . -131.12(7)
O122 Ag2 S2 C21 . . -132.7(3)
O53 Ag2 S2 C21 1_455 . 145.6(3)
S3 Ag2 S2 C21 . . 19.2(2)
O122 Ag2 S2 C18 . . -21.0(3)
O53 Ag2 S2 C18 1_455 . -102.8(3)
S3 Ag2 S2 C18 . . 130.9(2)
O122 Ag2 S2 Ag1 . . 91.59(17)
O53 Ag2 S2 Ag1 1_455 . 9.82(19)
S3 Ag2 S2 Ag1 . . -116.51(7)
O122 Ag2 S3 C31 . . 162.5(4)
O53 Ag2 S3 C31 1_455 . -82.4(3)
S2 Ag2 S3 C31 . . 43.1(2)
O122 Ag2 S3 C39 . . -91.2(4)
O53 Ag2 S3 C39 1_455 . 23.9(3)
S2 Ag2 S3 C39 . . 149.3(2)
O122 Ag2 S3 Ag3 . . 24.3(4)
O53 Ag2 S3 Ag3 1_455 . 139.33(16)
S2 Ag2 S3 Ag3 . . -95.21(9)
O41 Ag3 S3 C31 . . -14.6(3)
S4 Ag3 S3 C31 . . 85.7(2)
O41 Ag3 S3 C39 . . -121.8(3)
S4 Ag3 S3 C39 . . -21.5(2)
O41 Ag3 S3 Ag2 . . 121.03(18)
S4 Ag3 S3 Ag2 . . -138.63(9)
O73 Ag4 S4 C41 1_455 . 140.7(3)
O61 Ag4 S4 C41 . . -59.8(3)
O62 Ag4 S4 C41 . . -41.7(3)
O73 Ag4 S4 C38 1_455 . 28.3(3)
O61 Ag4 S4 C38 . . -172.3(3)
O62 Ag4 S4 C38 . . -154.2(3)
O73 Ag4 S4 Ag3 1_455 . -81.05(19)
O61 Ag4 S4 Ag3 . . 78.4(2)
O62 Ag4 S4 Ag3 . . 96.49(15)
O41 Ag3 S4 C41 . . 5.1(3)
S3 Ag3 S4 C41 . . -116.7(3)
O41 Ag3 S4 C38 . . 117.8(3)
S3 Ag3 S4 C38 . . -3.9(2)
O41 Ag3 S4 Ag4 . . -126.15(13)
S3 Ag3 S4 Ag4 . . 112.08(7)
O63 Ag5 S5 C51 . . -146.8(3)
O72 Ag5 S5 C51 . . 57.2(3)
O71 Ag5 S5 C51 . . 36.2(3)
O63 Ag5 S5 C57 . . -33.5(3)
O72 Ag5 S5 C57 . . 170.4(3)
O71 Ag5 S5 C57 . . 149.5(3)
O63 Ag5 S5 Ag6 . . 79.6(2)
O72 Ag5 S5 Ag6 . . -76.42(19)
O71 Ag5 S5 Ag6 . . -97.37(14)
O82 Ag6 S5 C51 . . 1.1(3)
O93 Ag6 S5 C51 1_655 . -74.5(3)
S6 Ag6 S5 C51 . . 121.0(3)
O82 Ag6 S5 C57 . . -112.7(3)
O93 Ag6 S5 C57 1_655 . 171.8(3)
S6 Ag6 S5 C57 . . 7.3(2)
O82 Ag6 S5 Ag5 . . 128.48(14)
O93 Ag6 S5 Ag5 1_655 . 52.96(14)
S6 Ag6 S5 Ag5 . . -111.56(7)
O31 Ag7 S6 C61 . . -157.5(4)
O91 Ag7 S6 C61 . . 84.1(3)
S7 Ag7 S6 C61 . . -42.7(2)
O31 Ag7 S6 C58 . . 96.8(5)
O91 Ag7 S6 C58 . . -21.6(3)
S7 Ag7 S6 C58 . . -148.4(2)
O31 Ag7 S6 Ag6 . . -20.4(4)
O91 Ag7 S6 Ag6 . . -138.73(17)
S7 Ag7 S6 Ag6 . . 94.40(9)
O82 Ag6 S6 C61 . . 15.3(3)
O93 Ag6 S6 C61 1_655 . -149.9(5)
S5 Ag6 S6 C61 . . -88.0(2)
O82 Ag6 S6 C58 . . 122.0(3)
O93 Ag6 S6 C58 1_655 . -43.2(5)
S5 Ag6 S6 C58 . . 18.7(2)
O82 Ag6 S6 Ag7 . . -119.14(17)
O93 Ag6 S6 Ag7 1_655 . 75.6(5)
S5 Ag6 S6 Ag7 . . 137.53(9)
O82 Ag8 S7 C71 1_455 . 102.7(3)
O83 Ag8 S7 C71 1_455 . 38.4(4)
O121 Ag8 S7 C71 . . -174.1(3)
S8 Ag8 S7 C71 . . -95.2(2)
O82 Ag8 S7 C77 1_455 . -152.4(3)
O83 Ag8 S7 C77 1_455 . 143.2(3)
O121 Ag8 S7 C77 . . -69.2(3)
S8 Ag8 S7 C77 . . 9.7(2)
O82 Ag8 S7 Ag7 1_455 . -34.99(19)
O83 Ag8 S7 Ag7 1_455 . -99.3(3)
O121 Ag8 S7 Ag7 . . 48.2(2)
S8 Ag8 S7 Ag7 . . 127.12(8)
O31 Ag7 S7 C71 . . 129.5(3)
O91 Ag7 S7 C71 . . -149.6(3)
S6 Ag7 S7 C71 . . -22.8(2)
O31 Ag7 S7 C77 . . 20.8(3)
O91 Ag7 S7 C77 . . 101.7(3)
S6 Ag7 S7 C77 . . -131.4(2)
O31 Ag7 S7 Ag8 . . -92.74(18)
O91 Ag7 S7 Ag8 . . -11.9(2)
S6 Ag7 S7 Ag8 . . 114.99(8)
O21 Ag9 S8 C81 . . -114.3(3)
O12 Ag9 S8 C81 . . 77.2(3)
O21 Ag9 S8 C78 . . -2.0(3)
O12 Ag9 S8 C78 . . -170.6(3)
O21 Ag9 S8 Ag8 . . 102.5(2)
O12 Ag9 S8 Ag8 . . -66.05(17)
O82 Ag8 S8 C81 1_455 . -81.7(4)
O83 Ag8 S8 C81 1_455 . -13.2(3)
S7 Ag8 S8 C81 . . 128.3(3)
O121 Ag8 S8 C81 . . -125.8(3)
O82 Ag8 S8 C78 1_455 . 169.2(4)
O83 Ag8 S8 C78 1_455 . -122.3(3)
S7 Ag8 S8 C78 . . 19.2(2)
O121 Ag8 S8 C78 . . 125.1(3)
O82 Ag8 S8 Ag9 1_455 . 61.0(3)
O83 Ag8 S8 Ag9 1_455 . 129.6(2)
S7 Ag8 S8 Ag9 . . -88.95(8)
O121 Ag8 S8 Ag9 . . 16.95(18)
O23 Ag10 O11 N1 1_455 . -163.1(4)
S1 Ag10 O11 N1 . . 1.5(5)
O21 Ag9 O12 N1 . . 150.4(4)
S8 Ag9 O12 N1 . . -36.8(5)
O12 Ag9 O21 N2 . . 161.9(4)
S8 Ag9 O21 N2 . . -9.2(5)
O91 Ag7 O31 N3 . . 153.3(7)
S6 Ag7 O31 N3 . . 25.4(9)
S7 Ag7 O31 N3 . . -89.0(7)
S3 Ag3 O41 N4 . . -2.1(9)
S4 Ag3 O41 N4 . . -90.7(9)
S3 Ag3 O41 Ag1 . 1_655 -125.94(13)
S4 Ag3 O41 Ag1 . 1_655 145.62(15)
O73 Ag4 O61 N6 1_455 . -169.1(4)
S4 Ag4 O61 N6 . . 24.4(5)
O62 Ag4 O61 N6 . . 0.4(4)
O73 Ag4 O62 N6 1_455 . 13.2(5)
S4 Ag4 O62 N6 . . -164.7(4)
O61 Ag4 O62 N6 . . -0.4(4)
S5 Ag5 O63 N6 . . 8.9(5)
O72 Ag5 O63 N6 . . 172.6(4)
O71 Ag5 O63 N6 . . -175.0(4)
O63 Ag5 O71 N7 . . -16.6(5)
S5 Ag5 O71 N7 . . 160.8(4)
O72 Ag5 O71 N7 . . -0.4(4)
O63 Ag5 O72 N7 . . 168.0(4)
S5 Ag5 O72 N7 . . -27.7(5)
O71 Ag5 O72 N7 . . 0.4(4)
O93 Ag6 O82 N8 1_655 . 162.3(9)
S6 Ag6 O82 N8 . . -13.1(9)
S5 Ag6 O82 N8 . . 75.9(9)
O93 Ag6 O82 Ag8 1_655 1_655 -58.0(2)
S6 Ag6 O82 Ag8 . 1_655 126.60(16)
S5 Ag6 O82 Ag8 . 1_655 -144.44(16)
O31 Ag7 O91 N9 . . 101.8(6)
S6 Ag7 O91 N9 . . -105.3(5)
S7 Ag7 O91 N9 . . 9.8(6)
O82 Ag8 O121 N12 1_455 . 128.1(10)
O83 Ag8 O121 N12 1_455 . 163.9(9)
S7 Ag8 O121 N12 . . 8.7(11)
S8 Ag8 O121 N12 . . -73.7(9)
O53 Ag2 O122 N12 1_455 . -164.2(7)
S3 Ag2 O122 N12 . . -38.5(9)
S2 Ag2 O122 N12 . . 79.6(7)
Ag9 O12 N1 O13 . . 5.9(7)
Ag9 O12 N1 O11 . . -172.2(5)
Ag10 O11 N1 O13 . . -175.8(5)
Ag10 O11 N1 O12 . . 2.3(7)
Ag10 O23 N2 O22 1_655 . -6.3(7)
Ag10 O23 N2 O21 1_655 . 170.9(4)
Ag9 O21 N2 O22 . . 175.8(5)
Ag9 O21 N2 O23 . . -1.4(7)
Ag7 O31 N3 O33 . . 32.1(9)
Ag7 O31 N3 O32 . . -147.5(6)
Ag1 O32 N3 O31 1_655 . 143.6(6)
Ag1 O32 N3 O33 1_655 . -36.1(9)
Ag1 O43 N4 O42 1_655 . -179.6(6)
Ag1 O43 N4 O41 1_655 . -0.1(6)
Ag1 O41 N4 O42 1_655 . 179.6(6)
Ag3 O41 N4 O42 . . 54.9(12)
Ag1 O41 N4 O43 1_655 . 0.1(7)
Ag3 O41 N4 O43 . . -124.4(8)
Ag2 O53 N5 O52 1_655 . -15.1(8)
Ag2 O53 N5 O51 1_655 . 163.1(5)
Ag4 O62 N6 O63 . . -178.0(5)
Ag4 O62 N6 O61 . . 0.7(7)
Ag5 O63 N6 O62 . . -160.7(5)
Ag5 O63 N6 O61 . . 20.7(7)
Ag4 O61 N6 O62 . . -0.7(7)
Ag4 O61 N6 O63 . . 178.0(5)
Ag5 O71 N7 O72 . . 0.6(6)
Ag5 O71 N7 O73 . . 179.7(5)
Ag5 O72 N7 O71 . . -0.7(7)
Ag5 O72 N7 O73 . . -179.7(5)
Ag4 O73 N7 O71 1_655 . 162.9(5)
Ag4 O73 N7 O72 1_655 . -18.1(7)
Ag8 O82 N8 O81 1_655 . 178.4(7)
Ag6 O82 N8 O81 . . -40.5(13)
Ag8 O82 N8 O83 1_655 . -2.5(8)
Ag6 O82 N8 O83 . . 138.5(8)
Ag8 O83 N8 O81 1_655 . -178.6(7)
Ag8 O83 N8 O82 1_655 . 2.3(8)
Ag7 O91 N9 O92 . . -161.9(5)
Ag7 O91 N9 O93 . . 17.7(8)
Ag6 O93 N9 O91 1_455 . -179.7(6)
Ag6 O93 N9 O92 1_455 . -0.1(7)
Ag8 O121 N12 O123 . . 37.3(14)
Ag8 O121 N12 O122 . . -141.8(8)
Ag2 O122 N12 O123 . . -27.4(10)
Ag2 O122 N12 O121 . . 151.7(6)
C17 S1 C11 C12 . . 47.2(7)
Ag10 S1 C11 C12 . . -66.5(6)
Ag1 S1 C11 C12 . . 152.0(5)
C17 S1 C11 C16 . . -135.4(6)
Ag10 S1 C11 C16 . . 110.8(6)
Ag1 S1 C11 C16 . . -30.7(7)
C16 C11 C12 C13 . . -0.1(11)
S1 C11 C12 C13 . . 177.2(6)
C11 C12 C13 C14 . . -2.0(11)
C12 C13 C14 C15 . . 1.1(11)
C13 C14 C15 C16 . . 1.7(12)
C12 C11 C16 C15 . . 2.8(11)
S1 C11 C16 C15 . . -174.7(7)
C14 C15 C16 C11 . . -3.7(13)
C11 S1 C17 C18 . . 166.7(5)
Ag10 S1 C17 C18 . . -71.7(5)
Ag1 S1 C17 C18 . . 49.2(5)
S1 C17 C18 S2 . . -73.5(5)
C21 S2 C18 C17 . . -65.0(5)
Ag1 S2 C18 C17 . . 50.4(5)
Ag2 S2 C18 C17 . . 175.1(4)
C18 S2 C21 C22 . . 110.7(6)
Ag1 S2 C21 C22 . . 5.9(6)
Ag2 S2 C21 C22 . . -132.4(5)
C18 S2 C21 C26 . . -69.7(6)
Ag1 S2 C21 C26 . . -174.5(5)
Ag2 S2 C21 C26 . . 47.2(6)
C26 C21 C22 C23 . . -1.3(10)
S2 C21 C22 C23 . . 178.1(5)
C21 C22 C23 C24 . . 1.6(11)
C22 C23 C24 C25 . . -0.7(11)
C23 C24 C25 C26 . . -0.6(12)
C24 C25 C26 C21 . . 0.9(11)
C22 C21 C26 C25 . . 0.1(10)
S2 C21 C26 C25 . . -179.4(5)
C39 S3 C31 C36 . . -76.0(6)
Ag2 S3 C31 C36 . . 31.7(6)
Ag3 S3 C31 C36 . . 178.2(5)
C39 S3 C31 C32 . . 106.6(6)
Ag2 S3 C31 C32 . . -145.7(5)
Ag3 S3 C31 C32 . . 0.8(6)
C36 C31 C32 C33 . . -1.8(11)
S3 C31 C32 C33 . . 175.7(6)
C31 C32 C33 C34 . . 2.2(12)
C32 C33 C34 C35 . . -0.8(12)
C33 C34 C35 C36 . . -1.0(12)
C32 C31 C36 C35 . . 0.1(1)
S3 C31 C36 C35 . . -177.3(5)
C34 C35 C36 C31 . . 1.3(11)
C41 S4 C38 C39 . . 165.9(5)
Ag4 S4 C38 C39 . . -75.1(5)
Ag3 S4 C38 C39 . . 36.5(5)
S4 C38 C39 S3 . . -66.1(6)
C31 S3 C39 C38 . . -60.7(5)
Ag2 S3 C39 C38 . . -169.1(4)
Ag3 S3 C39 C38 . . 55.3(5)
C38 S4 C41 C42 . . -101.4(6)
Ag4 S4 C41 C42 . . 140.1(5)
Ag3 S4 C41 C42 . . 11.6(7)
C38 S4 C41 C46 . . 79.0(6)
Ag4 S4 C41 C46 . . -39.5(6)
Ag3 S4 C41 C46 . . -168.1(4)
C46 C41 C42 C43 . . -1.7(10)
S4 C41 C42 C43 . . 178.6(6)
C41 C42 C43 C44 . . 0.4(11)
C42 C43 C44 C45 . . 0.6(11)
C43 C44 C45 C46 . . -0.2(11)
C44 C45 C46 C41 . . -1.1(10)
C42 C41 C46 C45 . . 2.1(10)
S4 C41 C46 C45 . . -178.3(5)
C57 S5 C51 C56 . . 119.5(6)
Ag5 S5 C51 C56 . . -121.6(6)
Ag6 S5 C51 C56 . . 5.8(7)
C57 S5 C51 C52 . . -61.0(6)
Ag5 S5 C51 C52 . . 57.9(6)
Ag6 S5 C51 C52 . . -174.7(5)
C56 C51 C52 C53 . . 0.5(11)
S5 C51 C52 C53 . . -178.9(6)
C51 C52 C53 C54 . . 1.3(11)
C52 C53 C54 C55 . . -1.8(11)
C53 C54 C55 C56 . . 0.7(11)
C52 C51 C56 C55 . . -1.7(11)
S5 C51 C56 C55 . . 177.8(6)
C54 C55 C56 C51 . . 1.1(11)
C51 S5 C57 C58 . . -165.5(5)
Ag5 S5 C57 C58 . . 77.4(5)
Ag6 S5 C57 C58 . . -39.5(5)
S5 C57 C58 S6 . . 66.2(6)
C61 S6 C58 C57 . . 62.8(5)
Ag7 S6 C58 C57 . . 170.9(4)
Ag6 S6 C58 C57 . . -52.9(5)
C58 S6 C61 C66 . . 82.4(6)
Ag7 S6 C61 C66 . . -25.7(5)
Ag6 S6 C61 C66 . . -171.4(4)
C58 S6 C61 C62 . . -98.7(6)
Ag7 S6 C61 C62 . . 153.2(5)
Ag6 S6 C61 C62 . . 7.5(6)
C66 C61 C62 C63 . . 1.4(10)
S6 C61 C62 C63 . . -177.5(5)
C61 C62 C63 C64 . . 0.4(11)
C62 C63 C64 C65 . . -1.7(11)
C63 C64 C65 C66 . . 1.2(11)
C62 C61 C66 C65 . . -1.9(9)
S6 C61 C66 C65 . . 177.0(5)
C64 C65 C66 C61 . . 0.6(10)
C77 S7 C71 C72 . . 66.5(6)
Ag8 S7 C71 C72 . . 169.9(5)
Ag7 S7 C71 C72 . . -46.1(6)
C77 S7 C71 C76 . . -115.5(6)
Ag8 S7 C71 C76 . . -12.2(6)
Ag7 S7 C71 C76 . . 131.9(5)
C76 C71 C72 C73 . . 1.3(10)
S7 C71 C72 C73 . . 179.2(5)
C71 C72 C73 C74 . . -1.1(11)
C72 C73 C74 C75 . . 0.9(12)
C73 C74 C75 C76 . . -0.6(12)
C72 C71 C76 C75 . . -1.0(10)
S7 C71 C76 C75 . . -178.8(5)
C74 C75 C76 C71 . . 0.7(11)
C71 S7 C77 C78 . . 65.3(5)
Ag8 S7 C77 C78 . . -48.1(5)
Ag7 S7 C77 C78 . . -178.9(4)
S7 C77 C78 S8 . . 74.7(5)
C81 S8 C78 C77 . . -170.0(4)
Ag9 S8 C78 C77 . . 71.4(4)
Ag8 S8 C78 C77 . . -52.4(4)
C78 S8 C81 C86 . . 166.2(5)
Ag9 S8 C81 C86 . . -82.9(5)
Ag8 S8 C81 C86 . . 62.7(6)
C78 S8 C81 C82 . . -14.3(7)
Ag9 S8 C81 C82 . . 96.5(6)
Ag8 S8 C81 C82 . . -117.8(6)
C86 C81 C82 C83 . . -0.2(10)
S8 C81 C82 C83 . . -179.8(5)
C81 C82 C83 C84 . . -0.1(11)
C82 C83 C84 C85 . . 0.8(11)
C83 C84 C85 C86 . . -1.1(10)
C84 C85 C86 C81 . . 0.8(10)
C82 C81 C86 C85 . . -0.2(10)
S8 C81 C86 C85 . . 179.6(5)
|
1501565.cif | #------------------------------------------------------------------------------
#$Date: 2017-10-13 02:32:00 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201954 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/50/15/1501565.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_1501565
loop_
_publ_author_name
'Hung Dang'
'Thierry Maris'
'Ji-Hyun Yi'
'Federico Rosei'
'Antonio Nancy'
'James D. Wuest'
_publ_section_title
;
Ensuring Homology between 2D and 3D Molecular Crystals
;
_journal_name_full Langmuir
_journal_page_first 11980
_journal_page_last 11985
_journal_paper_doi 10.1021/la702885y
_journal_volume 23
_journal_year 2007
_chemical_absolute_configuration rmad
_chemical_compound_source 'Synthesized by the authors. See text'
_chemical_formula_moiety 'C16 H14'
_chemical_formula_sum 'C16 H14'
_chemical_formula_weight 206.27
_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 8
_cell_length_a 8.0049(4)
_cell_length_b 8.5815(4)
_cell_length_c 32.3805(16)
_cell_measurement_reflns_used 7031
_cell_measurement_temperature 296(2)
_cell_measurement_theta_max 72.57
_cell_measurement_theta_min 2.73
_cell_volume 2224.35(19)
_computing_cell_refinement 'SMART (Bruker, 1999)'
_computing_data_collection 'SMART (Bruker, 1999)'
_computing_data_reduction 'SAINT (Bruker, 1999)'
_computing_molecular_graphics 'SHELXTL (Bruker, 1997)'
_computing_publication_material 'UdMX (local program)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 296(2)
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type 'Bruker Smart 2000'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'X-ray Sealed Tube'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.046
_diffrn_reflns_av_sigmaI/netI 0.0857
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_l_max 40
_diffrn_reflns_limit_l_min -39
_diffrn_reflns_number 12852
_diffrn_reflns_theta_full 73.11
_diffrn_reflns_theta_max 73.11
_diffrn_reflns_theta_min 2.73
_diffrn_standards_decay_% 0.00
_diffrn_standards_number 5
_exptl_absorpt_coefficient_mu 0.521
_exptl_absorpt_correction_T_max 0.9100
_exptl_absorpt_correction_T_min 0.7100
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Sadabs (Sheldrick,1996)'
_exptl_crystal_colour Colorless
_exptl_crystal_density_diffrn 1.232
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 880
_exptl_crystal_size_max 0.60
_exptl_crystal_size_mid 0.35
_exptl_crystal_size_min 0.18
_refine_diff_density_max 0.140
_refine_diff_density_min -0.132
_refine_diff_density_rms 0.037
_refine_ls_abs_structure_details 'Flack H D (1983), XXXX Friedel Pairs'
_refine_ls_abs_structure_Flack 0.1(1)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.118
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 289
_refine_ls_number_reflns 4384
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.118
_refine_ls_R_factor_all 0.0461
_refine_ls_R_factor_gt 0.0418
_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^)+(0.0106P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0906
_refine_ls_wR_factor_ref 0.0912
_reflns_number_gt 3059
_reflns_number_total 4384
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file deposit.cif
_cod_data_source_block jw1153
_cod_original_sg_symbol_H-M P212121
_cod_database_code 1501565
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
C1 C 0.9927(3) 0.4640(2) 0.41537(7) 0.0584(6) Uani 1 1 d .
H1 H 1.1017 0.4893 0.4080 0.070 Uiso 1 1 calc R
C2 C 0.9513(3) 0.4450(3) 0.45606(7) 0.0608(6) Uani 1 1 d .
H2 H 1.0329 0.4580 0.4762 0.073 Uiso 1 1 calc R
C3 C 0.7907(3) 0.4070(2) 0.46767(7) 0.0585(6) Uani 1 1 d .
H3 H 0.7655 0.3938 0.4955 0.070 Uiso 1 1 calc R
C4 C 0.6656(3) 0.3882(3) 0.43804(7) 0.0557(6) Uani 1 1 d .
C5 C 0.7092(3) 0.4074(2) 0.39646(6) 0.0520(5) Uani 1 1 d .
C6 C 0.8721(3) 0.4455(2) 0.38514(6) 0.0541(6) Uani 1 1 d .
C7 C 0.9134(3) 0.4602(3) 0.33979(6) 0.0576(6) Uani 1 1 d .
H7A H 0.9395 0.3582 0.3286 0.069 Uiso 1 1 calc R
H7B H 1.0107 0.5263 0.3364 0.069 Uiso 1 1 calc R
C8 C 0.7652(2) 0.5302(3) 0.31642(6) 0.0555(6) Uani 1 1 d .
H8A H 0.7481 0.6371 0.3252 0.067 Uiso 1 1 calc R
H8B H 0.7887 0.5306 0.2870 0.067 Uiso 1 1 calc R
C9 C 0.6106(3) 0.4369(3) 0.32464(6) 0.0536(6) Uani 1 1 d .
C10 C 0.5814(3) 0.3821(2) 0.36445(6) 0.0520(6) Uani 1 1 d .
C11 C 0.4366(3) 0.2990(2) 0.37394(6) 0.0545(6) Uani 1 1 d .
C12 C 0.3239(3) 0.2662(3) 0.34262(6) 0.0582(6) Uani 1 1 d .
H12 H 0.2287 0.2082 0.3485 0.070 Uiso 1 1 calc R
C13 C 0.3506(3) 0.3177(3) 0.30341(7) 0.0617(6) Uani 1 1 d .
H13 H 0.2742 0.2946 0.2827 0.074 Uiso 1 1 calc R
C14 C 0.4917(3) 0.4043(3) 0.29454(6) 0.0564(6) Uani 1 1 d .
H14 H 0.5074 0.4417 0.2679 0.068 Uiso 1 1 calc R
C15 C 0.4147(3) 0.2386(3) 0.41726(6) 0.0567(6) Uani 1 1 d .
H15A H 0.4697 0.1383 0.4198 0.068 Uiso 1 1 calc R
H15B H 0.2968 0.2239 0.4229 0.068 Uiso 1 1 calc R
C16 C 0.4874(3) 0.3507(3) 0.44843(6) 0.0586(6) Uani 1 1 d .
H16A H 0.4220 0.4459 0.4487 0.070 Uiso 1 1 calc R
H16B H 0.4821 0.3048 0.4758 0.070 Uiso 1 1 calc R
C17 C 0.4777(3) 0.7814(3) 0.39635(7) 0.0575(6) Uani 1 1 d .
H17 H 0.5845 0.7597 0.3867 0.069 Uiso 1 1 calc R
C18 C 0.4441(3) 0.7744(2) 0.43811(6) 0.0568(6) Uani 1 1 d .
H18 H 0.5285 0.7476 0.4565 0.068 Uiso 1 1 calc R
C19 C 0.2862(3) 0.8069(2) 0.45259(6) 0.0556(6) Uani 1 1 d .
H19 H 0.2655 0.8016 0.4808 0.067 Uiso 1 1 calc R
C20 C 0.1575(3) 0.8471(3) 0.42612(6) 0.0535(6) Uani 1 1 d .
C21 C 0.1920(3) 0.8549(2) 0.38347(6) 0.0505(5) Uani 1 1 d .
C22 C 0.3518(3) 0.8209(2) 0.36881(6) 0.0530(6) Uani 1 1 d .
C23 C 0.3842(3) 0.8338(2) 0.32304(6) 0.0537(6) Uani 1 1 d .
H23A H 0.4780 0.7679 0.3156 0.064 Uiso 1 1 calc R
H23B H 0.4130 0.9405 0.3162 0.064 Uiso 1 1 calc R
C24 C 0.2325(2) 0.7853(3) 0.29855(6) 0.0563(6) Uani 1 1 d .
H24A H 0.2520 0.8053 0.2695 0.068 Uiso 1 1 calc R
H24B H 0.2144 0.6743 0.3020 0.068 Uiso 1 1 calc R
C25 C 0.0798(3) 0.8721(3) 0.31231(6) 0.0539(6) Uani 1 1 d .
C26 C 0.0578(3) 0.9005(2) 0.35454(6) 0.0481(5) Uani 1 1 d .
C27 C -0.0832(3) 0.9768(3) 0.36919(6) 0.0567(6) Uani 1 1 d .
C28 C -0.2037(3) 1.0259(3) 0.34114(7) 0.0580(6) Uani 1 1 d .
H28 H -0.2994 1.0761 0.3505 0.070 Uiso 1 1 calc R
C29 C -0.1816(3) 1.0005(3) 0.29984(7) 0.0578(6) Uani 1 1 d .
H29 H -0.2622 1.0349 0.2813 0.069 Uiso 1 1 calc R
C30 C -0.0429(2) 0.9253(2) 0.28545(7) 0.0554(6) Uani 1 1 d .
H30 H -0.0304 0.9095 0.2572 0.067 Uiso 1 1 calc R
C31 C -0.0977(3) 1.0082(2) 0.41490(5) 0.0555(6) Uani 1 1 d .
H31A H -0.2147 1.0173 0.4223 0.067 Uiso 1 1 calc R
H31B H -0.0435 1.1064 0.4213 0.067 Uiso 1 1 calc R
C32 C -0.0184(3) 0.8796(3) 0.44009(6) 0.0530(5) Uani 1 1 d .
H32A H -0.0173 0.9095 0.4690 0.064 Uiso 1 1 calc R
H32B H -0.0846 0.7855 0.4375 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
C1 0.0601(15) 0.0566(14) 0.0586(14) -0.0006(11) -0.0036(12) 0.0033(13)
C2 0.0573(16) 0.0613(15) 0.0637(15) -0.0009(11) 0.0002(13) 0.0021(13)
C3 0.0612(16) 0.0580(15) 0.0563(14) -0.0005(11) -0.0005(13) -0.0012(13)
C4 0.0542(15) 0.0537(13) 0.0593(14) 0.0004(11) 0.0015(12) -0.0005(12)
C5 0.0528(14) 0.0534(13) 0.0498(13) 0.0019(10) -0.0035(11) 0.0005(12)
C6 0.0542(14) 0.0546(13) 0.0534(14) -0.0007(10) -0.0012(12) -0.0012(12)
C7 0.0534(15) 0.0602(14) 0.0592(14) 0.0013(11) -0.0042(12) -0.0035(13)
C8 0.0530(15) 0.0574(13) 0.0560(13) -0.0017(11) 0.0010(11) 0.0003(12)
C9 0.0538(14) 0.0559(13) 0.0512(13) -0.0001(10) -0.0017(12) -0.0015(12)
C10 0.0553(15) 0.0492(12) 0.0515(12) 0.0010(10) -0.0004(12) -0.0019(12)
C11 0.0541(15) 0.0559(13) 0.0535(13) -0.0004(10) -0.0001(12) 0.0012(12)
C12 0.0592(16) 0.0562(14) 0.0592(14) 0.0011(11) -0.0007(12) 0.0010(13)
C13 0.0630(16) 0.0620(15) 0.0601(14) 0.0001(11) -0.0013(13) -0.0002(14)
C14 0.0527(14) 0.0612(15) 0.0553(14) 0.0002(11) 0.0002(11) -0.0018(13)
C15 0.0563(15) 0.0559(13) 0.0578(13) 0.0027(10) 0.0041(13) -0.0008(12)
C16 0.0600(15) 0.0578(14) 0.0581(13) -0.0030(11) -0.0026(12) -0.0028(13)
C17 0.0553(15) 0.0592(14) 0.0581(13) -0.0015(11) -0.0043(12) -0.0021(13)
C18 0.0585(15) 0.0567(13) 0.0552(14) 0.0019(11) 0.0028(12) 0.0000(12)
C19 0.0537(14) 0.0570(14) 0.0560(13) -0.0026(11) -0.0001(12) 0.0014(12)
C20 0.0538(14) 0.0537(13) 0.0529(13) 0.0020(10) -0.0026(11) -0.0018(12)
C21 0.0470(14) 0.0520(13) 0.0525(13) -0.0003(10) 0.0003(11) 0.0001(11)
C22 0.0551(15) 0.0516(13) 0.0523(13) 0.0010(10) -0.0034(12) 0.0037(12)
C23 0.0549(14) 0.0525(13) 0.0537(13) 0.0013(10) -0.0002(11) -0.0008(12)
C24 0.0583(14) 0.0566(13) 0.0542(13) -0.0016(10) 0.0032(12) 0.0009(13)
C25 0.0527(15) 0.0553(13) 0.0538(13) 0.0003(10) -0.0013(11) 0.0028(12)
C26 0.0487(14) 0.0503(13) 0.0452(12) 0.0007(9) -0.0018(11) 0.0015(11)
C27 0.0576(16) 0.0556(14) 0.0570(14) -0.0029(11) 0.0003(13) -0.0001(13)
C28 0.0582(16) 0.0559(14) 0.0598(14) -0.0020(11) -0.0001(12) 0.0013(13)
C29 0.0552(16) 0.0579(14) 0.0603(15) 0.0000(11) -0.0005(12) 0.0005(12)
C30 0.0509(15) 0.0581(14) 0.0573(13) 0.0030(11) -0.0017(12) 0.0008(13)
C31 0.0557(15) 0.0577(14) 0.0529(13) -0.0008(11) -0.0018(12) -0.0018(12)
C32 0.0541(14) 0.0524(13) 0.0523(13) 0.0001(10) 0.0006(11) 0.0001(12)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
C2 C1 C6 119.9(2) y
C2 C1 H1 120 ?
C6 C1 H1 120 ?
C1 C2 C3 121.1(2) y
C1 C2 H2 119.5 ?
C3 C2 H2 119.5 ?
C2 C3 C4 120.6(2) y
C2 C3 H3 119.7 ?
C4 C3 H3 119.7 ?
C3 C4 C5 117.9(2) y
C3 C4 C16 123.6(2) y
C5 C4 C16 118.5(2) y
C6 C5 C4 120.9(2) y
C6 C5 C10 119.99(19) y
C4 C5 C10 119.1(2) y
C1 C6 C5 119.6(2) y
C1 C6 C7 121.7(2) y
C5 C6 C7 118.7(2) y
C6 C7 C8 110.12(18) y
C6 C7 H7A 109.6 ?
C8 C7 H7A 109.6 ?
C6 C7 H7B 109.6 ?
C8 C7 H7B 109.6 ?
H7A C7 H7B 108.2 ?
C9 C8 C7 110.05(17) y
C9 C8 H8A 109.7 ?
C7 C8 H8A 109.7 ?
C9 C8 H8B 109.7 ?
C7 C8 H8B 109.7 ?
H8A C8 H8B 108.2 ?
C14 C9 C10 117.8(2) y
C14 C9 C8 123.25(19) y
C10 C9 C8 118.95(19) y
C9 C10 C11 121.1(2) y
C9 C10 C5 119.0(2) y
C11 C10 C5 119.85(19) y
C12 C11 C10 118.9(2) y
C12 C11 C15 122.5(2) y
C10 C11 C15 118.52(19) y
C13 C12 C11 121.0(2) y
C13 C12 H12 119.5 ?
C11 C12 H12 119.5 ?
C12 C13 C14 119.8(2) y
C12 C13 H13 120.1 ?
C14 C13 H13 120.1 ?
C13 C14 C9 121.4(2) y
C13 C14 H14 119.3 ?
C9 C14 H14 119.3 ?
C11 C15 C16 111.02(18) y
C11 C15 H15A 109.4 ?
C16 C15 H15A 109.4 ?
C11 C15 H15B 109.4 ?
C16 C15 H15B 109.4 ?
H15A C15 H15B 108 ?
C4 C16 C15 110.67(19) y
C4 C16 H16A 109.5 ?
C15 C16 H16A 109.5 ?
C4 C16 H16B 109.5 ?
C15 C16 H16B 109.5 ?
H16A C16 H16B 108.1 ?
C18 C17 C22 120.0(2) y
C18 C17 H17 120 ?
C22 C17 H17 120 ?
C19 C18 C17 120.2(2) y
C19 C18 H18 119.9 ?
C17 C18 H18 119.9 ?
C18 C19 C20 121.5(2) y
C18 C19 H19 119.2 ?
C20 C19 H19 119.2 ?
C19 C20 C21 118.2(2) y
C19 C20 C32 123.81(18) y
C21 C20 C32 117.95(18) y
C22 C21 C20 120.18(19) y
C22 C21 C26 120.40(18) y
C20 C21 C26 119.42(19) y
C17 C22 C21 119.9(2) y
C17 C22 C23 121.7(2) y
C21 C22 C23 118.44(18) y
C22 C23 C24 111.00(18) y
C22 C23 H23A 109.4 ?
C24 C23 H23A 109.4 ?
C22 C23 H23B 109.4 ?
C24 C23 H23B 109.4 ?
H23A C23 H23B 108 ?
C25 C24 C23 111.28(17) y
C25 C24 H24A 109.4 ?
C23 C24 H24A 109.4 ?
C25 C24 H24B 109.4 ?
C23 C24 H24B 109.4 ?
H24A C24 H24B 108 ?
C30 C25 C26 117.7(2) y
C30 C25 C24 123.6(2) y
C26 C25 C24 118.63(19) y
C27 C26 C25 121.21(19) y
C27 C26 C21 119.93(18) y
C25 C26 C21 118.79(19) y
C26 C27 C28 118.93(19) y
C26 C27 C31 118.82(19) y
C28 C27 C31 122.2(2) y
C29 C28 C27 120.1(2) y
C29 C28 H28 120 ?
C27 C28 H28 120 ?
C28 C29 C30 120.9(2) y
C28 C29 H29 119.5 ?
C30 C29 H29 119.5 ?
C29 C30 C25 121.1(2) y
C29 C30 H30 119.5 ?
C25 C30 H30 119.5 ?
C27 C31 C32 111.50(18) y
C27 C31 H31A 109.3 ?
C32 C31 H31A 109.3 ?
C27 C31 H31B 109.3 ?
C32 C31 H31B 109.3 ?
H31A C31 H31B 108 ?
C20 C32 C31 111.46(17) y
C20 C32 H32A 109.3 ?
C31 C32 H32A 109.3 ?
C20 C32 H32B 109.3 ?
C31 C32 H32B 109.3 ?
H32A C32 H32B 108 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
C1 C2 1.368(3) y
C1 C6 1.383(3) y
C1 H1 0.93 ?
C2 C3 1.378(3) y
C2 H2 0.93 ?
C3 C4 1.397(3) y
C3 H3 0.93 ?
C4 C5 1.401(3) y
C4 C16 1.500(3) y
C5 C6 1.394(3) y
C5 C10 1.473(3) y
C6 C7 1.511(2) y
C7 C8 1.530(3) y
C7 H7a 0.97 ?
C7 H7b 0.97 ?
C8 C9 1.498(3) y
C8 H8a 0.97 ?
C8 H8b 0.97 ?
C9 C14 1.391(3) y
C9 C10 1.392(3) y
C10 C11 1.395(3) y
C11 C12 1.386(3) y
C11 C15 1.506(2) y
C12 C13 1.361(3) y
C12 H12 0.93 ?
C13 C14 1.382(3) y
C13 H13 0.93 ?
C14 H14 0.93 ?
C15 C16 1.511(3) y
C15 H15a 0.97 ?
C15 H15b 0.97 ?
C16 H16a 0.97 ?
C16 H16b 0.97 ?
C17 C18 1.380(3) y
C17 C22 1.387(3) y
C17 H17 0.93 ?
C18 C19 1.377(3) y
C18 H18 0.93 ?
C19 C20 1.384(2) y
C19 H19 0.93 ?
C20 C21 1.410(2) y
C20 C32 1.505(3) y
C21 C22 1.396(3) y
C21 C26 1.478(2) y
C22 C23 1.508(2) y
C23 C24 1.509(3) y
C23 H23a 0.97 ?
C23 H23b 0.97 ?
C24 C25 1.500(3) y
C24 H24a 0.97 ?
C24 H24b 0.97 ?
C25 C30 1.389(3) y
C25 C26 1.400(3) y
C26 C27 1.388(3) y
C27 C28 1.390(3) y
C27 C31 1.509(2) y
C28 C29 1.366(2) y
C28 H28 0.93 ?
C29 C30 1.366(3) y
C29 H29 0.93 ?
C30 H30 0.93 ?
C31 C32 1.512(3) y
C31 H31a 0.97 ?
C31 H31b 0.97 ?
C32 H32a 0.97 ?
C32 H32b 0.97 ?
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
C6 C1 C2 C3 0.2(3) y
C1 C2 C3 C4 -0.6(3) y
C2 C3 C4 C5 0.7(3) y
C2 C3 C4 C16 -178.5(2) y
C3 C4 C5 C6 -0.6(3) y
C16 C4 C5 C6 178.7(2) y
C3 C4 C5 C10 177.6(2) y
C16 C4 C5 C10 -3.2(3) y
C2 C1 C6 C5 -0.1(3) y
C2 C1 C6 C7 -177.99(19) y
C4 C5 C6 C1 0.3(3) y
C10 C5 C6 C1 -177.87(19) y
C4 C5 C6 C7 178.27(19) y
C10 C5 C6 C7 0.1(3) y
C1 C6 C7 C8 -146.3(2) y
C5 C6 C7 C8 35.8(3) y
C6 C7 C8 C9 -54.2(2) y
C7 C8 C9 C14 -141.0(2) y
C7 C8 C9 C10 40.4(3) y
C14 C9 C10 C11 -0.8(3) y
C8 C9 C10 C11 177.91(18) y
C14 C9 C10 C5 176.75(19) y
C8 C9 C10 C5 -4.5(3) y
C6 C5 C10 C9 -17.5(3) y
C4 C5 C10 C9 164.4(2) y
C6 C5 C10 C11 160.2(2) y
C4 C5 C10 C11 -18.0(3) y
C9 C10 C11 C12 2.4(3) y
C5 C10 C11 C12 -175.1(2) y
C9 C10 C11 C15 178.2(2) y
C5 C10 C11 C15 0.6(3) y
C10 C11 C12 C13 -1.9(3) y
C15 C11 C12 C13 -177.5(2) y
C11 C12 C13 C14 -0.2(3) y
C12 C13 C14 C9 1.9(3) y
C10 C9 C14 C13 -1.3(3) y
C8 C9 C14 C13 179.98(19) y
C12 C11 C15 C16 -149.14(19) y
C10 C11 C15 C16 35.3(3) y
C3 C4 C16 C15 -141.9(2) y
C5 C4 C16 C15 38.8(3) y
C11 C15 C16 C4 -53.5(2) y
C22 C17 C18 C19 -0.2(3) y
C17 C18 C19 C20 0.0(3) y
C18 C19 C20 C21 -0.2(3) y
C18 C19 C20 C32 178.3(2) y
C19 C20 C21 C22 0.7(3) y
C32 C20 C21 C22 -177.98(19) y
C19 C20 C21 C26 -178.84(19) y
C32 C20 C21 C26 2.5(3) y
C18 C17 C22 C21 0.6(3) y
C18 C17 C22 C23 178.49(18) y
C20 C21 C22 C17 -0.9(3) y
C26 C21 C22 C17 178.7(2) y
C20 C21 C22 C23 -178.82(19) y
C26 C21 C22 C23 0.7(3) y
C17 C22 C23 C24 147.0(2) y
C21 C22 C23 C24 -35.1(3) y
C22 C23 C24 C25 52.8(2) y
C23 C24 C25 C30 141.4(2) y
C23 C24 C25 C26 -39.1(3) y
C30 C25 C26 C27 1.2(3) y
C24 C25 C26 C27 -178.4(2) y
C30 C25 C26 C21 -175.76(19) y
C24 C25 C26 C21 4.7(3) y
C22 C21 C26 C27 -161.2(2) y
C20 C21 C26 C27 18.3(3) y
C22 C21 C26 C25 15.8(3) y
C20 C21 C26 C25 -164.72(19) y
C25 C26 C27 C28 -0.3(3) y
C21 C26 C27 C28 176.62(19) y
C25 C26 C27 C31 -178.28(19) y
C21 C26 C27 C31 -1.4(3) y
C26 C27 C28 C29 -0.7(3) y
C31 C27 C28 C29 177.2(2) y
C27 C28 C29 C30 0.8(3) y
C28 C29 C30 C25 0.1(3) y
C26 C25 C30 C29 -1.1(3) y
C24 C25 C30 C29 178.4(2) y
C26 C27 C31 C32 -33.8(3) y
C28 C27 C31 C32 148.3(2) y
C19 C20 C32 C31 144.0(2) y
C21 C20 C32 C31 -37.5(3) y
C27 C31 C32 C20 51.9(2) y
loop_
_cod_related_entry_id
_cod_related_entry_code
_cod_related_entry_database
1 63101 ChemSpider
|
1501566.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501566.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_1501566
loop_
_publ_author_name
'Hung Dang'
'Thierry Maris'
'Ji-Hyun Yi'
'Federico Rosei'
'Antonio Nancy'
'James D. Wuest'
_publ_section_title
;
Ensuring Homology between 2D and 3D Molecular Crystals
;
_journal_name_full Langmuir
_journal_page_first 11980
_journal_page_last 11985
_journal_paper_doi 10.1021/la702885y
_journal_volume 23
_journal_year 2007
_chemical_compound_source 'Synthesized by the authors. See text'
_chemical_formula_moiety 'C18 H14 O4'
_chemical_formula_sum 'C18 H14 O4'
_chemical_formula_weight 294.29
_chemical_name_systematic
;
?
;
_space_group_IT_number 96
_symmetry_cell_setting tetragonal
_symmetry_space_group_name_Hall 'P 4nw 2abw'
_symmetry_space_group_name_H-M 'P 43 21 2'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 9.7778(2)
_cell_length_b 9.7778(2)
_cell_length_c 14.0111(5)
_cell_measurement_reflns_used 9305
_cell_measurement_temperature 150(2)
_cell_measurement_theta_max 66.73
_cell_measurement_theta_min 5.52
_cell_volume 1339.54(6)
_computing_cell_refinement 'SMART (Bruker, 2003)'
_computing_data_collection 'SMART (Bruker, 2003)'
_computing_data_reduction 'SAINT (Bruker, 2004)'
_computing_molecular_graphics 'SHELXTL (Bruker, 1997)'
_computing_publication_material 'UdMX (local program)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 150(2)
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type 'Bruker Microstar'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator 'Helios optics'
_diffrn_radiation_source 'Rotating anode'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.065
_diffrn_reflns_av_sigmaI/netI 0.12
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_number 14136
_diffrn_reflns_theta_full 66.74
_diffrn_reflns_theta_max 66.74
_diffrn_reflns_theta_min 5.52
_diffrn_standards_number 5
_exptl_absorpt_coefficient_mu 0.849
_exptl_absorpt_correction_T_max 0.900
_exptl_absorpt_correction_T_min 0.800
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Sadabs (Sheldrick,1996)'
_exptl_crystal_colour Colorless
_exptl_crystal_density_diffrn 1.459
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 616
_exptl_crystal_size_max 0.22
_exptl_crystal_size_mid 0.22
_exptl_crystal_size_min 0.12
_refine_diff_density_max 0.210
_refine_diff_density_min -0.264
_refine_diff_density_rms 0.062
_refine_ls_abs_structure_details 'Flack H D (1983), 450 Friedel Pairs'
_refine_ls_abs_structure_Flack 0.56(2)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.023
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 104
_refine_ls_number_reflns 1196
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.023
_refine_ls_R_factor_all 0.0564
_refine_ls_R_factor_gt 0.0548
_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^)+(0.1100P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1349
_refine_ls_wR_factor_ref 0.1351
_reflns_number_gt 1118
_reflns_number_total 1196
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file deposit.cif
_cod_data_source_block jw1146
_cod_original_sg_symbol_H-M P43212
_cod_database_code 1501566
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/4'
'-x+1/2, y+1/2, -z+3/4'
'-y, -x, -z+1/2'
'y, x, -z'
'y+1/2, -x+1/2, z+1/4'
'-y+1/2, x+1/2, z+3/4'
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
C1 C 0.44603(17) 0.55397(17) 0.2500 0.0288(6) Uani 1 2 d S . .
C2 C 0.55342(16) 0.44658(16) 0.2500 0.0279(6) Uani 1 2 d S . .
C3 C 0.68896(17) 0.48114(16) 0.22990(13) 0.0270(4) Uani 1 1 d . . .
H3 H 0.7124 0.5737 0.2175 0.032 Uiso 1 1 calc R . .
C4 C 0.78961(16) 0.38129(17) 0.22797(13) 0.0275(4) Uani 1 1 d . . .
C5 C 0.75457(17) 0.24543(17) 0.2500 0.0266(6) Uani 1 2 d S . .
C6 C 0.86135(16) 0.13865(16) 0.2500 0.0274(6) Uani 1 2 d S . .
C7 C 1.00027(16) 0.17686(17) 0.25173(15) 0.0282(4) Uani 1 1 d . . .
C8 C 1.10009(16) 0.07516(16) 0.25183(15) 0.0298(4) Uani 1 1 d . . .
H8 H 1.1941 0.0997 0.2532 0.036 Uiso 1 1 calc R . .
C9 C 1.06268(16) -0.06268(16) 0.2500 0.0294(6) Uani 1 2 d S . .
C10 C 1.17007(18) -0.17007(18) 0.2500 0.0324(6) Uani 1 2 d S . .
C11 C 0.93521(15) 0.41274(16) 0.19988(16) 0.0335(5) Uani 1 1 d . . .
H11A H 0.9541 0.5108 0.2116 0.040 Uiso 1 1 calc R . .
H11B H 0.9471 0.3951 0.1308 0.040 Uiso 1 1 calc R . .
C12 C 1.03734(17) 0.32608(15) 0.25600(18) 0.0330(5) Uani 1 1 d . . .
H12A H 1.1302 0.3393 0.2293 0.040 Uiso 1 1 calc R . .
H12B H 1.0386 0.3565 0.3234 0.040 Uiso 1 1 calc R . .
O1 O 0.48247(14) 0.67731(12) 0.23925(12) 0.0385(4) Uani 1 1 d . . .
H1 H 0.4134 0.7280 0.2405 0.058 Uiso 0.50 1 calc P A 1
O2 O 1.29373(13) -0.13334(13) 0.23852(13) 0.0434(5) Uani 1 1 d . . .
H2 H 1.3445 -0.2029 0.2372 0.065 Uiso 0.50 1 calc P 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
C1 0.0242(7) 0.0242(7) 0.0381(14) -0.0024(8) -0.0024(8) 0.0030(9)
C2 0.0222(7) 0.0222(7) 0.0395(14) -0.0041(7) -0.0041(7) 0.0021(8)
C3 0.0253(8) 0.0187(7) 0.0371(10) 0.0002(6) 0.0001(7) -0.0012(6)
C4 0.0247(8) 0.0211(8) 0.0367(9) -0.0012(7) -0.0012(6) -0.0013(6)
C5 0.0202(7) 0.0202(7) 0.0395(13) -0.0026(7) -0.0026(7) 0.0008(8)
C6 0.0212(7) 0.0212(7) 0.0399(13) -0.0007(7) -0.0007(7) 0.0004(9)
C7 0.0216(9) 0.0241(9) 0.0391(10) -0.0038(7) 0.0003(7) 0.0007(6)
C8 0.0217(7) 0.0264(8) 0.0414(10) -0.0008(8) 0.0007(7) 0.0010(6)
C9 0.0252(8) 0.0252(8) 0.0379(14) 0.0003(8) 0.0003(8) 0.0040(9)
C10 0.0278(8) 0.0278(8) 0.0414(14) 0.0030(8) 0.0030(8) 0.0034(9)
C11 0.0244(8) 0.0226(7) 0.0535(11) 0.0022(7) 0.0065(8) -0.0011(6)
C12 0.0212(8) 0.0214(8) 0.0564(12) -0.0034(8) 0.0027(8) 0.0002(5)
O1 0.0310(7) 0.0216(6) 0.0629(11) -0.0006(5) -0.0023(6) 0.0024(4)
O2 0.0220(6) 0.0293(7) 0.0789(12) 0.0025(7) 0.0006(6) 0.0058(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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
O1 C1 O1 5_665 . 123.4(2) y
O1 C1 C2 5_665 . 118.32(10) y
O1 C1 C2 . . 118.32(10) y
C3 C2 C3 5_665 . 120.0(2) y
C3 C2 C1 5_665 . 120.0(1) y
C3 C2 C1 . . 120.0(1) y
C4 C3 C2 . . 120.47(15) y
C4 C3 H3 . . 119.8 ?
C2 C3 H3 . . 119.8 ?
C3 C4 C5 . . 119.21(15) y
C3 C4 C11 . . 122.09(14) y
C5 C4 C11 . . 118.67(15) y
C4 C5 C4 5_665 . 120.6(2) y
C4 C5 C6 5_665 . 119.72(10) y
C4 C5 C6 . . 119.72(10) y
C7 C6 C7 5_665 . 120.8(2) y
C7 C6 C5 5_665 . 119.61(10) y
C7 C6 C5 . . 119.61(10) y
C8 C7 C6 . . 119.08(15) y
C8 C7 C12 . . 121.55(14) y
C6 C7 C12 . . 119.35(15) y
C7 C8 C9 . . 120.34(15) y
C7 C8 H8 . . 119.8 ?
C9 C8 H8 . . 119.8 ?
C8 C9 C8 . 5_665 120.4(2) y
C8 C9 C10 . . 119.81(10) y
C8 C9 C10 5_665 . 119.81(10) y
O2 C10 O2 5_665 . 123.6(2) y
O2 C10 C9 5_665 . 118.21(10) y
O2 C10 C9 . . 118.21(10) y
C4 C11 C12 . . 111.68(15) y
C4 C11 H11A . . 109.3 ?
C12 C11 H11A . . 109.3 ?
C4 C11 H11B . . 109.3 ?
C12 C11 H11B . . 109.3 ?
H11A C11 H11B . . 107.9 ?
C7 C12 C11 . . 111.10(15) y
C7 C12 H12A . . 109.4 ?
C11 C12 H12A . . 109.4 ?
C7 C12 H12B . . 109.4 ?
C11 C12 H12B . . 109.4 ?
H12A C12 H12B . . 108 ?
C1 O1 H1 . . 109.5 ?
C10 O2 H2 . . 109.5 ?
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
C1 O1 5_665 1.2665(15) y
C1 O1 . 1.2665(15) y
C1 C2 . 1.485(3) y
C2 C3 5_665 1.3964(18) y
C2 C3 . 1.3964(18) y
C3 C4 . 1.386(2) y
C3 H3 . 0.95 ?
C4 C5 . 1.406(2) y
C4 C11 . 1.509(2) y
C5 C4 5_665 1.406(2) y
C5 C6 . 1.477(3) y
C6 C7 5_665 1.4089(18) y
C6 C7 . 1.4089(18) y
C7 C8 . 1.393(2) y
C7 C12 . 1.5046(19) y
C8 C9 . 1.3967(18) y
C8 H8 . 0.95 ?
C9 C8 5_665 1.3968(18) y
C9 C10 . 1.485(3) y
C10 O2 5_665 1.2715(18) y
C10 O2 . 1.2715(18) y
C11 C12 . 1.528(3) y
C11 H11a . 0.99 ?
C11 H11b . 0.99 ?
C12 H12a . 0.99 ?
C12 H12b . 0.99 ?
O1 H1 . 0.84 ?
O2 H2 . 0.84 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2 H2 O1 0.84 1.79 2.6141(17) 166.8 1_645
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_4
_geom_torsion
_geom_torsion_publ_flag
O1 C1 C2 C3 5_665 5_665 -5.70(12) y
O1 C1 C2 C3 . 5_665 174.30(12) y
O1 C1 C2 C3 5_665 . 174.30(12) y
O1 C1 C2 C3 . . -5.70(12) y
C3 C2 C3 C4 5_665 . 1.20(13) y
C1 C2 C3 C4 . . -178.80(13) y
C2 C3 C4 C5 . . -2.4(2) y
C2 C3 C4 C11 . . 175.65(14) y
C3 C4 C5 C4 . 5_665 1.17(12) y
C11 C4 C5 C4 . 5_665 -176.90(18) y
C3 C4 C5 C6 . . -178.83(12) y
C11 C4 C5 C6 . . 3.10(18) y
C4 C5 C6 C7 5_665 5_665 15.77(13) y
C4 C5 C6 C7 . 5_665 -164.23(13) y
C4 C5 C6 C7 5_665 . -164.23(13) y
C4 C5 C6 C7 . . 15.77(13) y
C7 C6 C7 C8 5_665 . -0.08(14) y
C5 C6 C7 C8 . . 179.92(14) y
C7 C6 C7 C12 5_665 . -178.5(2) y
C5 C6 C7 C12 . . 1.5(2) y
C6 C7 C8 C9 . . 0.2(3) y
C12 C7 C8 C9 . . 178.55(17) y
C7 C8 C9 C8 . 5_665 -0.08(15) y
C7 C8 C9 C10 . . 179.92(15) y
C8 C9 C10 O2 . 5_665 170.53(13) y
C8 C9 C10 O2 5_665 5_665 -9.47(13) y
C8 C9 C10 O2 . . -9.47(13) y
C8 C9 C10 O2 5_665 . 170.53(13) y
C3 C4 C11 C12 . . 145.43(19) y
C5 C4 C11 C12 . . -36.6(2) y
C8 C7 C12 C11 . . 146.89(19) y
C6 C7 C12 C11 . . -34.7(3) y
C4 C11 C12 C7 . . 50.8(2) y
|
1501567.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501567.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_1501567
loop_
_publ_author_name
'Litasov, Konstantin D.'
'Shatskiy, Anton'
'Fei, Yingwei'
'Suzuki, Akio'
'Ohtani, Eiji'
'Funakoshi, Kenichi'
_publ_section_title
;
Pressure-volume-temperature equation of state of tungsten carbide to 32
GPa and 1673 K
;
_journal_issue 5
_journal_name_full 'Journal of Applied Physics'
_journal_paper_doi 10.1063/1.3481667
_journal_volume 108
_journal_year 2010
_chemical_formula_structural WC
_chemical_formula_sum 'C W'
_space_group_IT_number 187
_symmetry_cell_setting hexagonal
_symmetry_space_group_name_Hall 'P -6 2'
_symmetry_space_group_name_H-M 'P -6 m 2'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 1
_cell_length_a 2.89827(9)
_cell_length_b 2.89827(9)
_cell_length_c 2.83315(13)
_cell_volume 20.6100(13)
_diffrn_ambient_pressure 5437500
_diffrn_ambient_temperature 873
_journal_article_reference 053513
_cod_data_source_file WC_P-6m2_DC72.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'W C'
_cod_database_code 1501567
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
y-x,-x,-z
-y,x-y,+z
+x,+y,-z
y-x,-x,+z
-y,x-y,-z
y-x,+y,+z
+x,x-y,-z
-y,-x,+z
y-x,+y,-z
+x,x-y,+z
-y,-x,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
W W 0. 0. 0. 1.0 0.0
C C 0.66667 0.3333 0.5 1.0 0.0
|
1501568.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501568.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_1501568
loop_
_publ_author_name
'Litasov, Konstantin D.'
'Shatskiy, Anton'
'Fei, Yingwei'
'Suzuki, Akio'
'Ohtani, Eiji'
'Funakoshi, Kenichi'
_publ_section_title
;
Pressure-volume-temperature equation of state of tungsten carbide to 32
GPa and 1673 K
;
_journal_issue 5
_journal_name_full 'Journal of Applied Physics'
_journal_paper_doi 10.1063/1.3481667
_journal_volume 108
_journal_year 2010
_chemical_formula_structural WC
_chemical_formula_sum 'C W'
_space_group_IT_number 187
_symmetry_cell_setting hexagonal
_symmetry_space_group_name_Hall 'P -6 2'
_symmetry_space_group_name_H-M 'P -6 m 2'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 1
_cell_length_a 2.88660(9)
_cell_length_b 2.88660(9)
_cell_length_c 2.82430(14)
_cell_volume 20.3805(14)
_diffrn_ambient_pressure 10052000
_diffrn_ambient_temperature 873
_journal_article_reference 053513
_cod_data_source_file WC_P-6m2_DC73.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'W C'
_cod_database_code 1501568
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
y-x,-x,-z
-y,x-y,+z
+x,+y,-z
y-x,-x,+z
-y,x-y,-z
y-x,+y,+z
+x,x-y,-z
-y,-x,+z
y-x,+y,-z
+x,x-y,+z
-y,-x,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
W W 0. 0. 0. 1.0 0.0
C C 0.66667 0.3333 0.5 1.0 0.0
|
1501569.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501569.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_1501569
loop_
_publ_author_name
'Litasov, Konstantin D.'
'Shatskiy, Anton'
'Fei, Yingwei'
'Suzuki, Akio'
'Ohtani, Eiji'
'Funakoshi, Kenichi'
_publ_section_title
;
Pressure-volume-temperature equation of state of tungsten carbide to 32
GPa and 1673 K
;
_journal_issue 5
_journal_name_full 'Journal of Applied Physics'
_journal_paper_doi 10.1063/1.3481667
_journal_volume 108
_journal_year 2010
_chemical_formula_structural WC
_chemical_formula_sum 'C W'
_space_group_IT_number 187
_symmetry_cell_setting hexagonal
_symmetry_space_group_name_Hall 'P -6 2'
_symmetry_space_group_name_H-M 'P -6 m 2'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 1
_cell_length_a 2.87816(9)
_cell_length_b 2.87816(9)
_cell_length_c 2.81895(14)
_cell_volume 20.2231(13)
_diffrn_ambient_pressure 13470000
_diffrn_ambient_temperature 873
_journal_article_reference 053513
_cod_data_source_file WC_P-6m2_DC74.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'W C'
_cod_database_code 1501569
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
y-x,-x,-z
-y,x-y,+z
+x,+y,-z
y-x,-x,+z
-y,x-y,-z
y-x,+y,+z
+x,x-y,-z
-y,-x,+z
y-x,+y,-z
+x,x-y,+z
-y,-x,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
W W 0. 0. 0. 1.0 0.0
C C 0.66667 0.3333 0.5 1.0 0.0
|
1501570.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501570.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_1501570
loop_
_publ_author_name
'Litasov, Konstantin D.'
'Shatskiy, Anton'
'Fei, Yingwei'
'Suzuki, Akio'
'Ohtani, Eiji'
'Funakoshi, Kenichi'
_publ_section_title
;
Pressure-volume-temperature equation of state of tungsten carbide to 32
GPa and 1673 K
;
_journal_issue 5
_journal_name_full 'Journal of Applied Physics'
_journal_paper_doi 10.1063/1.3481667
_journal_volume 108
_journal_year 2010
_chemical_formula_structural WC
_chemical_formula_sum 'C W'
_space_group_IT_number 187
_symmetry_cell_setting hexagonal
_symmetry_space_group_name_Hall 'P -6 2'
_symmetry_space_group_name_H-M 'P -6 m 2'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 1
_cell_length_a 2.86093(9)
_cell_length_b 2.86093(9)
_cell_length_c 2.80662(12)
_cell_volume 19.8943(12)
_diffrn_ambient_pressure 20935000
_diffrn_ambient_temperature 873
_journal_article_reference 053513
_cod_data_source_file WC_P-6m2_DC75.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'W C'
_cod_database_code 1501570
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
y-x,-x,-z
-y,x-y,+z
+x,+y,-z
y-x,-x,+z
-y,x-y,-z
y-x,+y,+z
+x,x-y,-z
-y,-x,+z
y-x,+y,-z
+x,x-y,+z
-y,-x,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
W W 0. 0. 0. 1.0 0.0
C C 0.66667 0.3333 0.5 1.0 0.0
|
1501571.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501571.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_1501571
loop_
_publ_author_name
'Litasov, Konstantin D.'
'Shatskiy, Anton'
'Fei, Yingwei'
'Suzuki, Akio'
'Ohtani, Eiji'
'Funakoshi, Kenichi'
_publ_section_title
;
Pressure-volume-temperature equation of state of tungsten carbide to 32
GPa and 1673 K
;
_journal_issue 5
_journal_name_full 'Journal of Applied Physics'
_journal_paper_doi 10.1063/1.3481667
_journal_volume 108
_journal_year 2010
_chemical_formula_structural WC
_chemical_formula_sum 'C W'
_space_group_IT_number 187
_symmetry_cell_setting hexagonal
_symmetry_space_group_name_Hall 'P -6 2'
_symmetry_space_group_name_H-M 'P -6 m 2'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 1
_cell_length_a 2.85397(9)
_cell_length_b 2.85397(9)
_cell_length_c 2.80110(12)
_cell_volume 19.7587(12)
_diffrn_ambient_pressure 24277500
_diffrn_ambient_temperature 873
_journal_article_reference 053513
_cod_data_source_file WC_P-6m2_DC76.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'W C'
_cod_database_code 1501571
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
y-x,-x,-z
-y,x-y,+z
+x,+y,-z
y-x,-x,+z
-y,x-y,-z
y-x,+y,+z
+x,x-y,-z
-y,-x,+z
y-x,+y,-z
+x,x-y,+z
-y,-x,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
W W 0. 0. 0. 1.0 0.0
C C 0.66667 0.3333 0.5 1.0 0.0
|
1501572.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501572.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_1501572
loop_
_publ_author_name
'Litasov, Konstantin D.'
'Shatskiy, Anton'
'Fei, Yingwei'
'Suzuki, Akio'
'Ohtani, Eiji'
'Funakoshi, Kenichi'
_publ_section_title
;
Pressure-volume-temperature equation of state of tungsten carbide to 32
GPa and 1673 K
;
_journal_issue 5
_journal_name_full 'Journal of Applied Physics'
_journal_paper_doi 10.1063/1.3481667
_journal_volume 108
_journal_year 2010
_chemical_formula_structural WC
_chemical_formula_sum 'C W'
_space_group_IT_number 187
_symmetry_cell_setting hexagonal
_symmetry_space_group_name_Hall 'P -6 2'
_symmetry_space_group_name_H-M 'P -6 m 2'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 1
_cell_length_a 2.84777(9)
_cell_length_b 2.84777(9)
_cell_length_c 2.79727(12)
_cell_volume 19.6460(12)
_diffrn_ambient_pressure 27037500
_diffrn_ambient_temperature 873
_journal_article_reference 053513
_cod_data_source_file WC_P-6m2_DC77.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'W C'
_cod_database_code 1501572
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
y-x,-x,-z
-y,x-y,+z
+x,+y,-z
y-x,-x,+z
-y,x-y,-z
y-x,+y,+z
+x,x-y,-z
-y,-x,+z
y-x,+y,-z
+x,x-y,+z
-y,-x,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
W W 0. 0. 0. 1.0 0.0
C C 0.66667 0.3333 0.5 1.0 0.0
|
1501573.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501573.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_1501573
loop_
_publ_author_name
'Litasov, Konstantin D.'
'Shatskiy, Anton'
'Fei, Yingwei'
'Suzuki, Akio'
'Ohtani, Eiji'
'Funakoshi, Kenichi'
_publ_section_title
;
Pressure-volume-temperature equation of state of tungsten carbide to 32
GPa and 1673 K
;
_journal_issue 5
_journal_name_full 'Journal of Applied Physics'
_journal_paper_doi 10.1063/1.3481667
_journal_volume 108
_journal_year 2010
_chemical_formula_structural WC
_chemical_formula_sum 'C W'
_space_group_IT_number 187
_symmetry_cell_setting hexagonal
_symmetry_space_group_name_Hall 'P -6 2'
_symmetry_space_group_name_H-M 'P -6 m 2'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 1
_cell_length_a 2.84075(9)
_cell_length_b 2.84075(9)
_cell_length_c 2.78931(16)
_cell_volume 19.4937(14)
_diffrn_ambient_pressure 31232500
_diffrn_ambient_temperature 873
_journal_article_reference 053513
_cod_data_source_file WC_P-6m2_DC78.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'W C'
_cod_database_code 1501573
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
y-x,-x,-z
-y,x-y,+z
+x,+y,-z
y-x,-x,+z
-y,x-y,-z
y-x,+y,+z
+x,x-y,-z
-y,-x,+z
y-x,+y,-z
+x,x-y,+z
-y,-x,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
W W 0. 0. 0. 1.0 0.0
C C 0.66667 0.3333 0.5 1.0 0.0
|
1501574.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501574.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_1501574
loop_
_publ_author_name
'Litasov, Konstantin D.'
'Shatskiy, Anton'
'Fei, Yingwei'
'Suzuki, Akio'
'Ohtani, Eiji'
'Funakoshi, Kenichi'
_publ_section_title
;
Pressure-volume-temperature equation of state of tungsten carbide to 32
GPa and 1673 K
;
_journal_issue 5
_journal_name_full 'Journal of Applied Physics'
_journal_paper_doi 10.1063/1.3481667
_journal_volume 108
_journal_year 2010
_chemical_formula_structural WC
_chemical_formula_sum 'C W'
_space_group_IT_number 187
_symmetry_cell_setting hexagonal
_symmetry_space_group_name_Hall 'P -6 2'
_symmetry_space_group_name_H-M 'P -6 m 2'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 1
_cell_length_a 2.89879(9)
_cell_length_b 2.89879(9)
_cell_length_c 2.83552(13)
_cell_volume 20.6346(13)
_diffrn_ambient_pressure 6082500
_diffrn_ambient_temperature 1073
_journal_article_reference 053513
_cod_data_source_file WC_P-6m2_DC79.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'W C'
_cod_database_code 1501574
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
y-x,-x,-z
-y,x-y,+z
+x,+y,-z
y-x,-x,+z
-y,x-y,-z
y-x,+y,+z
+x,x-y,-z
-y,-x,+z
y-x,+y,-z
+x,x-y,+z
-y,-x,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
W W 0. 0. 0. 1.0 0.0
C C 0.66667 0.3333 0.5 1.0 0.0
|
1501575.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501575.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_1501575
loop_
_publ_author_name
'Litasov, Konstantin D.'
'Shatskiy, Anton'
'Fei, Yingwei'
'Suzuki, Akio'
'Ohtani, Eiji'
'Funakoshi, Kenichi'
_publ_section_title
;
Pressure-volume-temperature equation of state of tungsten carbide to 32
GPa and 1673 K
;
_journal_issue 5
_journal_name_full 'Journal of Applied Physics'
_journal_paper_doi 10.1063/1.3481667
_journal_volume 108
_journal_year 2010
_chemical_formula_structural WC
_chemical_formula_sum 'C W'
_space_group_IT_number 187
_symmetry_cell_setting hexagonal
_symmetry_space_group_name_Hall 'P -6 2'
_symmetry_space_group_name_H-M 'P -6 m 2'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 1
_cell_length_a 2.88816(9)
_cell_length_b 2.88816(9)
_cell_length_c 2.82564(12)
_cell_volume 20.4122(12)
_diffrn_ambient_pressure 10370000
_diffrn_ambient_temperature 1073
_journal_article_reference 053513
_cod_data_source_file WC_P-6m2_DC80.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'W C'
_cod_database_code 1501575
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
y-x,-x,-z
-y,x-y,+z
+x,+y,-z
y-x,-x,+z
-y,x-y,-z
y-x,+y,+z
+x,x-y,-z
-y,-x,+z
y-x,+y,-z
+x,x-y,+z
-y,-x,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
W W 0. 0. 0. 1.0 0.0
C C 0.66667 0.3333 0.5 1.0 0.0
|
1501576.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501576.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_1501576
loop_
_publ_author_name
'Litasov, Konstantin D.'
'Shatskiy, Anton'
'Fei, Yingwei'
'Suzuki, Akio'
'Ohtani, Eiji'
'Funakoshi, Kenichi'
_publ_section_title
;
Pressure-volume-temperature equation of state of tungsten carbide to 32
GPa and 1673 K
;
_journal_issue 5
_journal_name_full 'Journal of Applied Physics'
_journal_paper_doi 10.1063/1.3481667
_journal_volume 108
_journal_year 2010
_chemical_formula_structural WC
_chemical_formula_sum 'C W'
_space_group_IT_number 187
_symmetry_cell_setting hexagonal
_symmetry_space_group_name_Hall 'P -6 2'
_symmetry_space_group_name_H-M 'P -6 m 2'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 1
_cell_length_a 2.88063(9)
_cell_length_b 2.88063(9)
_cell_length_c 2.82034(14)
_cell_volume 20.2678(13)
_diffrn_ambient_pressure 14042500
_diffrn_ambient_temperature 1073
_journal_article_reference 053513
_cod_data_source_file WC_P-6m2_DC81.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'W C'
_cod_database_code 1501576
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
y-x,-x,-z
-y,x-y,+z
+x,+y,-z
y-x,-x,+z
-y,x-y,-z
y-x,+y,+z
+x,x-y,-z
-y,-x,+z
y-x,+y,-z
+x,x-y,+z
-y,-x,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
W W 0. 0. 0. 1.0 0.0
C C 0.66667 0.3333 0.5 1.0 0.0
|
1501577.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501577.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_1501577
loop_
_publ_author_name
'Litasov, Konstantin D.'
'Shatskiy, Anton'
'Fei, Yingwei'
'Suzuki, Akio'
'Ohtani, Eiji'
'Funakoshi, Kenichi'
_publ_section_title
;
Pressure-volume-temperature equation of state of tungsten carbide to 32
GPa and 1673 K
;
_journal_issue 5
_journal_name_full 'Journal of Applied Physics'
_journal_paper_doi 10.1063/1.3481667
_journal_volume 108
_journal_year 2010
_chemical_formula_structural WC
_chemical_formula_sum 'C W'
_space_group_IT_number 187
_symmetry_cell_setting hexagonal
_symmetry_space_group_name_Hall 'P -6 2'
_symmetry_space_group_name_H-M 'P -6 m 2'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 1
_cell_length_a 2.86254(9)
_cell_length_b 2.86254(9)
_cell_length_c 2.80711(12)
_cell_volume 19.9202(12)
_diffrn_ambient_pressure 21605000
_diffrn_ambient_temperature 1073
_journal_article_reference 053513
_cod_data_source_file WC_P-6m2_DC82.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'W C'
_cod_database_code 1501577
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
y-x,-x,-z
-y,x-y,+z
+x,+y,-z
y-x,-x,+z
-y,x-y,-z
y-x,+y,+z
+x,x-y,-z
-y,-x,+z
y-x,+y,-z
+x,x-y,+z
-y,-x,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
W W 0. 0. 0. 1.0 0.0
C C 0.66667 0.3333 0.5 1.0 0.0
|
1501578.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501578.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_1501578
loop_
_publ_author_name
'Litasov, Konstantin D.'
'Shatskiy, Anton'
'Fei, Yingwei'
'Suzuki, Akio'
'Ohtani, Eiji'
'Funakoshi, Kenichi'
_publ_section_title
;
Pressure-volume-temperature equation of state of tungsten carbide to 32
GPa and 1673 K
;
_journal_issue 5
_journal_name_full 'Journal of Applied Physics'
_journal_paper_doi 10.1063/1.3481667
_journal_volume 108
_journal_year 2010
_chemical_formula_structural WC
_chemical_formula_sum 'C W'
_space_group_IT_number 187
_symmetry_cell_setting hexagonal
_symmetry_space_group_name_Hall 'P -6 2'
_symmetry_space_group_name_H-M 'P -6 m 2'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 1
_cell_length_a 2.85513(9)
_cell_length_b 2.85513(9)
_cell_length_c 2.80302(12)
_cell_volume 19.7883(12)
_diffrn_ambient_pressure 24780000
_diffrn_ambient_temperature 1073
_journal_article_reference 053513
_cod_data_source_file WC_P-6m2_DC83.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'W C'
_cod_database_code 1501578
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
y-x,-x,-z
-y,x-y,+z
+x,+y,-z
y-x,-x,+z
-y,x-y,-z
y-x,+y,+z
+x,x-y,-z
-y,-x,+z
y-x,+y,-z
+x,x-y,+z
-y,-x,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
W W 0. 0. 0. 1.0 0.0
C C 0.66667 0.3333 0.5 1.0 0.0
|
1501579.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501579.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_1501579
loop_
_publ_author_name
'Litasov, Konstantin D.'
'Shatskiy, Anton'
'Fei, Yingwei'
'Suzuki, Akio'
'Ohtani, Eiji'
'Funakoshi, Kenichi'
_publ_section_title
;
Pressure-volume-temperature equation of state of tungsten carbide to 32
GPa and 1673 K
;
_journal_issue 5
_journal_name_full 'Journal of Applied Physics'
_journal_paper_doi 10.1063/1.3481667
_journal_volume 108
_journal_year 2010
_chemical_formula_structural WC
_chemical_formula_sum 'C W'
_space_group_IT_number 187
_symmetry_cell_setting hexagonal
_symmetry_space_group_name_Hall 'P -6 2'
_symmetry_space_group_name_H-M 'P -6 m 2'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 1
_cell_length_a 2.84955(9)
_cell_length_b 2.84955(9)
_cell_length_c 2.79821(12)
_cell_volume 19.6772(12)
_diffrn_ambient_pressure 27320000
_diffrn_ambient_temperature 1073
_journal_article_reference 053513
_cod_data_source_file WC_P-6m2_DC84.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'W C'
_cod_database_code 1501579
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
y-x,-x,-z
-y,x-y,+z
+x,+y,-z
y-x,-x,+z
-y,x-y,-z
y-x,+y,+z
+x,x-y,-z
-y,-x,+z
y-x,+y,-z
+x,x-y,+z
-y,-x,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
W W 0. 0. 0. 1.0 0.0
C C 0.66667 0.3333 0.5 1.0 0.0
|
1501580.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501580.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_1501580
loop_
_publ_author_name
'Litasov, Konstantin D.'
'Shatskiy, Anton'
'Fei, Yingwei'
'Suzuki, Akio'
'Ohtani, Eiji'
'Funakoshi, Kenichi'
_publ_section_title
;
Pressure-volume-temperature equation of state of tungsten carbide to 32
GPa and 1673 K
;
_journal_issue 5
_journal_name_full 'Journal of Applied Physics'
_journal_paper_doi 10.1063/1.3481667
_journal_volume 108
_journal_year 2010
_chemical_formula_structural WC
_chemical_formula_sum 'C W'
_space_group_IT_number 187
_symmetry_cell_setting hexagonal
_symmetry_space_group_name_Hall 'P -6 2'
_symmetry_space_group_name_H-M 'P -6 m 2'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 1
_cell_length_a 2.84464(9)
_cell_length_b 2.84464(9)
_cell_length_c 2.79388(12)
_cell_volume 19.5791(12)
_diffrn_ambient_pressure 30240000
_diffrn_ambient_temperature 1073
_journal_article_reference 053513
_cod_data_source_file WC_P-6m2_DC85.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'W C'
_cod_database_code 1501580
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
y-x,-x,-z
-y,x-y,+z
+x,+y,-z
y-x,-x,+z
-y,x-y,-z
y-x,+y,+z
+x,x-y,-z
-y,-x,+z
y-x,+y,-z
+x,x-y,+z
-y,-x,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
W W 0. 0. 0. 1.0 0.0
C C 0.66667 0.3333 0.5 1.0 0.0
|
1501581.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501581.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_1501581
loop_
_publ_author_name
'Litasov, Konstantin D.'
'Shatskiy, Anton'
'Fei, Yingwei'
'Suzuki, Akio'
'Ohtani, Eiji'
'Funakoshi, Kenichi'
_publ_section_title
;
Pressure-volume-temperature equation of state of tungsten carbide to 32
GPa and 1673 K
;
_journal_issue 5
_journal_name_full 'Journal of Applied Physics'
_journal_paper_doi 10.1063/1.3481667
_journal_volume 108
_journal_year 2010
_chemical_formula_structural WC
_chemical_formula_sum 'C W'
_space_group_IT_number 187
_symmetry_cell_setting hexagonal
_symmetry_space_group_name_Hall 'P -6 2'
_symmetry_space_group_name_H-M 'P -6 m 2'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 1
_cell_length_a 2.89984(9)
_cell_length_b 2.89984(9)
_cell_length_c 2.83753(13)
_cell_volume 20.6642(13)
_diffrn_ambient_pressure 6627500
_diffrn_ambient_temperature 1273
_journal_article_reference 053513
_cod_data_source_file WC_P-6m2_DC86.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'W C'
_cod_database_code 1501581
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
y-x,-x,-z
-y,x-y,+z
+x,+y,-z
y-x,-x,+z
-y,x-y,-z
y-x,+y,+z
+x,x-y,-z
-y,-x,+z
y-x,+y,-z
+x,x-y,+z
-y,-x,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
W W 0. 0. 0. 1.0 0.0
C C 0.66667 0.3333 0.5 1.0 0.0
|
1501582.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501582.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_1501582
loop_
_publ_author_name
'Litasov, Konstantin D.'
'Shatskiy, Anton'
'Fei, Yingwei'
'Suzuki, Akio'
'Ohtani, Eiji'
'Funakoshi, Kenichi'
_publ_section_title
;
Pressure-volume-temperature equation of state of tungsten carbide to 32
GPa and 1673 K
;
_journal_issue 5
_journal_name_full 'Journal of Applied Physics'
_journal_paper_doi 10.1063/1.3481667
_journal_volume 108
_journal_year 2010
_chemical_formula_structural WC
_chemical_formula_sum 'C W'
_space_group_IT_number 187
_symmetry_cell_setting hexagonal
_symmetry_space_group_name_Hall 'P -6 2'
_symmetry_space_group_name_H-M 'P -6 m 2'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 1
_cell_length_a 2.89234(9)
_cell_length_b 2.89234(9)
_cell_length_c 2.82986(12)
_cell_volume 20.5019(13)
_diffrn_ambient_pressure 10102500
_diffrn_ambient_temperature 1273
_journal_article_reference 053513
_cod_data_source_file WC_P-6m2_DC87.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'W C'
_cod_database_code 1501582
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
y-x,-x,-z
-y,x-y,+z
+x,+y,-z
y-x,-x,+z
-y,x-y,-z
y-x,+y,+z
+x,x-y,-z
-y,-x,+z
y-x,+y,-z
+x,x-y,+z
-y,-x,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
W W 0. 0. 0. 1.0 0.0
C C 0.66667 0.3333 0.5 1.0 0.0
|
1501583.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501583.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_1501583
loop_
_publ_author_name
'Litasov, Konstantin D.'
'Shatskiy, Anton'
'Fei, Yingwei'
'Suzuki, Akio'
'Ohtani, Eiji'
'Funakoshi, Kenichi'
_publ_section_title
;
Pressure-volume-temperature equation of state of tungsten carbide to 32
GPa and 1673 K
;
_journal_issue 5
_journal_name_full 'Journal of Applied Physics'
_journal_paper_doi 10.1063/1.3481667
_journal_volume 108
_journal_year 2010
_chemical_formula_structural WC
_chemical_formula_sum 'C W'
_space_group_IT_number 187
_symmetry_cell_setting hexagonal
_symmetry_space_group_name_Hall 'P -6 2'
_symmetry_space_group_name_H-M 'P -6 m 2'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 1
_cell_length_a 2.88073(9)
_cell_length_b 2.88073(9)
_cell_length_c 2.82265(14)
_cell_volume 20.2858(13)
_diffrn_ambient_pressure 14622500
_diffrn_ambient_temperature 1273
_journal_article_reference 053513
_cod_data_source_file WC_P-6m2_DC88.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'W C'
_cod_database_code 1501583
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
y-x,-x,-z
-y,x-y,+z
+x,+y,-z
y-x,-x,+z
-y,x-y,-z
y-x,+y,+z
+x,x-y,-z
-y,-x,+z
y-x,+y,-z
+x,x-y,+z
-y,-x,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
W W 0. 0. 0. 1.0 0.0
C C 0.66667 0.3333 0.5 1.0 0.0
|
1501584.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501584.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_1501584
loop_
_publ_author_name
'Litasov, Konstantin D.'
'Shatskiy, Anton'
'Fei, Yingwei'
'Suzuki, Akio'
'Ohtani, Eiji'
'Funakoshi, Kenichi'
_publ_section_title
;
Pressure-volume-temperature equation of state of tungsten carbide to 32
GPa and 1673 K
;
_journal_issue 5
_journal_name_full 'Journal of Applied Physics'
_journal_paper_doi 10.1063/1.3481667
_journal_volume 108
_journal_year 2010
_chemical_formula_structural WC
_chemical_formula_sum 'C W'
_space_group_IT_number 187
_symmetry_cell_setting hexagonal
_symmetry_space_group_name_Hall 'P -6 2'
_symmetry_space_group_name_H-M 'P -6 m 2'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 1
_cell_length_a 2.86285(9)
_cell_length_b 2.86285(9)
_cell_length_c 2.81008(12)
_cell_volume 19.9456(12)
_diffrn_ambient_pressure 21965000
_diffrn_ambient_temperature 1273
_journal_article_reference 053513
_cod_data_source_file WC_P-6m2_DC89.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'W C'
_cod_database_code 1501584
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
y-x,-x,-z
-y,x-y,+z
+x,+y,-z
y-x,-x,+z
-y,x-y,-z
y-x,+y,+z
+x,x-y,-z
-y,-x,+z
y-x,+y,-z
+x,x-y,+z
-y,-x,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
W W 0. 0. 0. 1.0 0.0
C C 0.66667 0.3333 0.5 1.0 0.0
|
1501585.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501585.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_1501585
loop_
_publ_author_name
'Litasov, Konstantin D.'
'Shatskiy, Anton'
'Fei, Yingwei'
'Suzuki, Akio'
'Ohtani, Eiji'
'Funakoshi, Kenichi'
_publ_section_title
;
Pressure-volume-temperature equation of state of tungsten carbide to 32
GPa and 1673 K
;
_journal_issue 5
_journal_name_full 'Journal of Applied Physics'
_journal_paper_doi 10.1063/1.3481667
_journal_volume 108
_journal_year 2010
_chemical_formula_structural WC
_chemical_formula_sum 'C W'
_space_group_IT_number 187
_symmetry_cell_setting hexagonal
_symmetry_space_group_name_Hall 'P -6 2'
_symmetry_space_group_name_H-M 'P -6 m 2'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 1
_cell_length_a 2.85783(9)
_cell_length_b 2.85783(9)
_cell_length_c 2.80520(12)
_cell_volume 19.8412(12)
_diffrn_ambient_pressure 25382500
_diffrn_ambient_temperature 1273
_journal_article_reference 053513
_cod_data_source_file WC_P-6m2_DC90.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'W C'
_cod_database_code 1501585
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
y-x,-x,-z
-y,x-y,+z
+x,+y,-z
y-x,-x,+z
-y,x-y,-z
y-x,+y,+z
+x,x-y,-z
-y,-x,+z
y-x,+y,-z
+x,x-y,+z
-y,-x,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
W W 0. 0. 0. 1.0 0.0
C C 0.66667 0.3333 0.5 1.0 0.0
|
1501586.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501586.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_1501586
loop_
_publ_author_name
'Litasov, Konstantin D.'
'Shatskiy, Anton'
'Fei, Yingwei'
'Suzuki, Akio'
'Ohtani, Eiji'
'Funakoshi, Kenichi'
_publ_section_title
;
Pressure-volume-temperature equation of state of tungsten carbide to 32
GPa and 1673 K
;
_journal_issue 5
_journal_name_full 'Journal of Applied Physics'
_journal_paper_doi 10.1063/1.3481667
_journal_volume 108
_journal_year 2010
_chemical_formula_structural WC
_chemical_formula_sum 'C W'
_space_group_IT_number 187
_symmetry_cell_setting hexagonal
_symmetry_space_group_name_Hall 'P -6 2'
_symmetry_space_group_name_H-M 'P -6 m 2'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 1
_cell_length_a 2.85251(9)
_cell_length_b 2.85251(9)
_cell_length_c 2.80017(12)
_cell_volume 19.7319(12)
_diffrn_ambient_pressure 27812500
_diffrn_ambient_temperature 1273
_journal_article_reference 053513
_cod_data_source_file WC_P-6m2_DC91.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'W C'
_cod_database_code 1501586
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
y-x,-x,-z
-y,x-y,+z
+x,+y,-z
y-x,-x,+z
-y,x-y,-z
y-x,+y,+z
+x,x-y,-z
-y,-x,+z
y-x,+y,-z
+x,x-y,+z
-y,-x,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
W W 0. 0. 0. 1.0 0.0
C C 0.66667 0.3333 0.5 1.0 0.0
|
1501587.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501587.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_1501587
loop_
_publ_author_name
'Litasov, Konstantin D.'
'Shatskiy, Anton'
'Fei, Yingwei'
'Suzuki, Akio'
'Ohtani, Eiji'
'Funakoshi, Kenichi'
_publ_section_title
;
Pressure-volume-temperature equation of state of tungsten carbide to 32
GPa and 1673 K
;
_journal_issue 5
_journal_name_full 'Journal of Applied Physics'
_journal_paper_doi 10.1063/1.3481667
_journal_volume 108
_journal_year 2010
_chemical_formula_structural WC
_chemical_formula_sum 'C W'
_space_group_IT_number 187
_symmetry_cell_setting hexagonal
_symmetry_space_group_name_Hall 'P -6 2'
_symmetry_space_group_name_H-M 'P -6 m 2'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 1
_cell_length_a 2.84905(9)
_cell_length_b 2.84905(9)
_cell_length_c 2.79704(12)
_cell_volume 19.6621(12)
_diffrn_ambient_pressure 29417500
_diffrn_ambient_temperature 1273
_journal_article_reference 053513
_cod_data_source_file WC_P-6m2_DC92.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'W C'
_cod_database_code 1501587
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
y-x,-x,-z
-y,x-y,+z
+x,+y,-z
y-x,-x,+z
-y,x-y,-z
y-x,+y,+z
+x,x-y,-z
-y,-x,+z
y-x,+y,-z
+x,x-y,+z
-y,-x,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
W W 0. 0. 0. 1.0 0.0
C C 0.66667 0.3333 0.5 1.0 0.0
|
1501588.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501588.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_1501588
loop_
_publ_author_name
'Litasov, Konstantin D.'
'Shatskiy, Anton'
'Fei, Yingwei'
'Suzuki, Akio'
'Ohtani, Eiji'
'Funakoshi, Kenichi'
_publ_section_title
;
Pressure-volume-temperature equation of state of tungsten carbide to 32
GPa and 1673 K
;
_journal_issue 5
_journal_name_full 'Journal of Applied Physics'
_journal_paper_doi 10.1063/1.3481667
_journal_volume 108
_journal_year 2010
_chemical_formula_structural WC
_chemical_formula_sum 'C W'
_space_group_IT_number 187
_symmetry_cell_setting hexagonal
_symmetry_space_group_name_Hall 'P -6 2'
_symmetry_space_group_name_H-M 'P -6 m 2'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 1
_cell_length_a 2.90540(9)
_cell_length_b 2.90540(9)
_cell_length_c 2.84015(13)
_cell_volume 20.7627(13)
_diffrn_ambient_pressure 6060000
_diffrn_ambient_temperature 1473
_journal_article_reference 053513
_cod_data_source_file WC_P-6m2_DC93.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'W C'
_cod_database_code 1501588
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
y-x,-x,-z
-y,x-y,+z
+x,+y,-z
y-x,-x,+z
-y,x-y,-z
y-x,+y,+z
+x,x-y,-z
-y,-x,+z
y-x,+y,-z
+x,x-y,+z
-y,-x,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
W W 0. 0. 0. 1.0 0.0
C C 0.66667 0.3333 0.5 1.0 0.0
|
1501589.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501589.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_1501589
loop_
_publ_author_name
'Litasov, Konstantin D.'
'Shatskiy, Anton'
'Fei, Yingwei'
'Suzuki, Akio'
'Ohtani, Eiji'
'Funakoshi, Kenichi'
_publ_section_title
;
Pressure-volume-temperature equation of state of tungsten carbide to 32
GPa and 1673 K
;
_journal_issue 5
_journal_name_full 'Journal of Applied Physics'
_journal_paper_doi 10.1063/1.3481667
_journal_volume 108
_journal_year 2010
_chemical_formula_structural WC
_chemical_formula_sum 'C W'
_space_group_IT_number 187
_symmetry_cell_setting hexagonal
_symmetry_space_group_name_Hall 'P -6 2'
_symmetry_space_group_name_H-M 'P -6 m 2'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 1
_cell_length_a 2.89823(9)
_cell_length_b 2.89823(9)
_cell_length_c 2.83484(13)
_cell_volume 20.6217(13)
_diffrn_ambient_pressure 9107500
_diffrn_ambient_temperature 1473
_journal_article_reference 053513
_cod_data_source_file WC_P-6m2_DC94.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'W C'
_cod_database_code 1501589
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
y-x,-x,-z
-y,x-y,+z
+x,+y,-z
y-x,-x,+z
-y,x-y,-z
y-x,+y,+z
+x,x-y,-z
-y,-x,+z
y-x,+y,-z
+x,x-y,+z
-y,-x,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
W W 0. 0. 0. 1.0 0.0
C C 0.66667 0.3333 0.5 1.0 0.0
|
1501590.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501590.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_1501590
loop_
_publ_author_name
'Litasov, Konstantin D.'
'Shatskiy, Anton'
'Fei, Yingwei'
'Suzuki, Akio'
'Ohtani, Eiji'
'Funakoshi, Kenichi'
_publ_section_title
;
Pressure-volume-temperature equation of state of tungsten carbide to 32
GPa and 1673 K
;
_journal_issue 5
_journal_name_full 'Journal of Applied Physics'
_journal_paper_doi 10.1063/1.3481667
_journal_volume 108
_journal_year 2010
_chemical_formula_structural WC
_chemical_formula_sum 'C W'
_space_group_IT_number 187
_symmetry_cell_setting hexagonal
_symmetry_space_group_name_Hall 'P -6 2'
_symmetry_space_group_name_H-M 'P -6 m 2'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 1
_cell_length_a 2.88207(9)
_cell_length_b 2.88207(9)
_cell_length_c 2.82387(12)
_cell_volume 20.3135(12)
_diffrn_ambient_pressure 15405000
_diffrn_ambient_temperature 1473
_journal_article_reference 053513
_cod_data_source_file WC_P-6m2_DC95.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'W C'
_cod_database_code 1501590
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
y-x,-x,-z
-y,x-y,+z
+x,+y,-z
y-x,-x,+z
-y,x-y,-z
y-x,+y,+z
+x,x-y,-z
-y,-x,+z
y-x,+y,-z
+x,x-y,+z
-y,-x,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
W W 0. 0. 0. 1.0 0.0
C C 0.66667 0.3333 0.5 1.0 0.0
|
1501591.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501591.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_1501591
loop_
_publ_author_name
'Litasov, Konstantin D.'
'Shatskiy, Anton'
'Fei, Yingwei'
'Suzuki, Akio'
'Ohtani, Eiji'
'Funakoshi, Kenichi'
_publ_section_title
;
Pressure-volume-temperature equation of state of tungsten carbide to 32
GPa and 1673 K
;
_journal_issue 5
_journal_name_full 'Journal of Applied Physics'
_journal_paper_doi 10.1063/1.3481667
_journal_volume 108
_journal_year 2010
_chemical_formula_structural WC
_chemical_formula_sum 'C W'
_space_group_IT_number 187
_symmetry_cell_setting hexagonal
_symmetry_space_group_name_Hall 'P -6 2'
_symmetry_space_group_name_H-M 'P -6 m 2'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 1
_cell_length_a 2.86543(9)
_cell_length_b 2.86543(9)
_cell_length_c 2.81093(12)
_cell_volume 19.9876(12)
_diffrn_ambient_pressure 22660000
_diffrn_ambient_temperature 1473
_journal_article_reference 053513
_cod_data_source_file WC_P-6m2_DC96.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'W C'
_cod_database_code 1501591
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
y-x,-x,-z
-y,x-y,+z
+x,+y,-z
y-x,-x,+z
-y,x-y,-z
y-x,+y,+z
+x,x-y,-z
-y,-x,+z
y-x,+y,-z
+x,x-y,+z
-y,-x,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
W W 0. 0. 0. 1.0 0.0
C C 0.66667 0.3333 0.5 1.0 0.0
|
1501592.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501592.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_1501592
loop_
_publ_author_name
'Litasov, Konstantin D.'
'Shatskiy, Anton'
'Fei, Yingwei'
'Suzuki, Akio'
'Ohtani, Eiji'
'Funakoshi, Kenichi'
_publ_section_title
;
Pressure-volume-temperature equation of state of tungsten carbide to 32
GPa and 1673 K
;
_journal_issue 5
_journal_name_full 'Journal of Applied Physics'
_journal_paper_doi 10.1063/1.3481667
_journal_volume 108
_journal_year 2010
_chemical_formula_structural WC
_chemical_formula_sum 'C W'
_space_group_IT_number 187
_symmetry_cell_setting hexagonal
_symmetry_space_group_name_Hall 'P -6 2'
_symmetry_space_group_name_H-M 'P -6 m 2'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 1
_cell_length_a 2.85951(9)
_cell_length_b 2.85951(9)
_cell_length_c 2.80634(12)
_cell_volume 19.8726(12)
_diffrn_ambient_pressure 25870000
_diffrn_ambient_temperature 1473
_journal_article_reference 053513
_cod_data_source_file WC_P-6m2_DC97.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'W C'
_cod_database_code 1501592
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
y-x,-x,-z
-y,x-y,+z
+x,+y,-z
y-x,-x,+z
-y,x-y,-z
y-x,+y,+z
+x,x-y,-z
-y,-x,+z
y-x,+y,-z
+x,x-y,+z
-y,-x,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
W W 0. 0. 0. 1.0 0.0
C C 0.66667 0.3333 0.5 1.0 0.0
|
1501593.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501593.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_1501593
loop_
_publ_author_name
'Litasov, Konstantin D.'
'Shatskiy, Anton'
'Fei, Yingwei'
'Suzuki, Akio'
'Ohtani, Eiji'
'Funakoshi, Kenichi'
_publ_section_title
;
Pressure-volume-temperature equation of state of tungsten carbide to 32
GPa and 1673 K
;
_journal_issue 5
_journal_name_full 'Journal of Applied Physics'
_journal_paper_doi 10.1063/1.3481667
_journal_volume 108
_journal_year 2010
_chemical_formula_structural WC
_chemical_formula_sum 'C W'
_space_group_IT_number 187
_symmetry_cell_setting hexagonal
_symmetry_space_group_name_Hall 'P -6 2'
_symmetry_space_group_name_H-M 'P -6 m 2'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 1
_cell_length_a 2.85474(9)
_cell_length_b 2.85474(9)
_cell_length_c 2.80138(12)
_cell_volume 19.7713(12)
_diffrn_ambient_pressure 28442500
_diffrn_ambient_temperature 1473
_journal_article_reference 053513
_cod_data_source_file WC_P-6m2_DC98.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'W C'
_cod_database_code 1501593
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
y-x,-x,-z
-y,x-y,+z
+x,+y,-z
y-x,-x,+z
-y,x-y,-z
y-x,+y,+z
+x,x-y,-z
-y,-x,+z
y-x,+y,-z
+x,x-y,+z
-y,-x,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
W W 0. 0. 0. 1.0 0.0
C C 0.66667 0.3333 0.5 1.0 0.0
|
1501594.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501594.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_1501594
loop_
_publ_author_name
'Litasov, Konstantin D.'
'Shatskiy, Anton'
'Fei, Yingwei'
'Suzuki, Akio'
'Ohtani, Eiji'
'Funakoshi, Kenichi'
_publ_section_title
;
Pressure-volume-temperature equation of state of tungsten carbide to 32
GPa and 1673 K
;
_journal_issue 5
_journal_name_full 'Journal of Applied Physics'
_journal_paper_doi 10.1063/1.3481667
_journal_volume 108
_journal_year 2010
_chemical_formula_structural WC
_chemical_formula_sum 'C W'
_space_group_IT_number 187
_symmetry_cell_setting hexagonal
_symmetry_space_group_name_Hall 'P -6 2'
_symmetry_space_group_name_H-M 'P -6 m 2'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 1
_cell_length_a 2.85294(9)
_cell_length_b 2.85294(9)
_cell_length_c 2.80009(12)
_cell_volume 19.7373(12)
_diffrn_ambient_pressure 29342500
_diffrn_ambient_temperature 1473
_journal_article_reference 053513
_cod_data_source_file WC_P-6m2_DC99.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'W C'
_cod_database_code 1501594
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
y-x,-x,-z
-y,x-y,+z
+x,+y,-z
y-x,-x,+z
-y,x-y,-z
y-x,+y,+z
+x,x-y,-z
-y,-x,+z
y-x,+y,-z
+x,x-y,+z
-y,-x,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
W W 0. 0. 0. 1.0 0.0
C C 0.66667 0.3333 0.5 1.0 0.0
|
1501595.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501595.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_1501595
loop_
_publ_author_name
'Litasov, Konstantin D.'
'Shatskiy, Anton'
'Fei, Yingwei'
'Suzuki, Akio'
'Ohtani, Eiji'
'Funakoshi, Kenichi'
_publ_section_title
;
Pressure-volume-temperature equation of state of tungsten carbide to 32
GPa and 1673 K
;
_journal_issue 5
_journal_name_full 'Journal of Applied Physics'
_journal_paper_doi 10.1063/1.3481667
_journal_volume 108
_journal_year 2010
_chemical_formula_structural WC
_chemical_formula_sum 'C W'
_space_group_IT_number 187
_symmetry_cell_setting hexagonal
_symmetry_space_group_name_Hall 'P -6 2'
_symmetry_space_group_name_H-M 'P -6 m 2'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 1
_cell_length_a 2.85683(9)
_cell_length_b 2.85683(9)
_cell_length_c 2.80223(12)
_cell_volume 19.8063(12)
_diffrn_ambient_pressure 29282500
_diffrn_ambient_temperature 1673
_journal_article_reference 053513
_cod_data_source_file WC_P-6m2_DC100.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'W C'
_cod_database_code 1501595
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
y-x,-x,-z
-y,x-y,+z
+x,+y,-z
y-x,-x,+z
-y,x-y,-z
y-x,+y,+z
+x,x-y,-z
-y,-x,+z
y-x,+y,-z
+x,x-y,+z
-y,-x,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
W W 0. 0. 0. 1.0 0.0
C C 0.66667 0.3333 0.5 1.0 0.0
|
1501596.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501596.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_1501596
loop_
_publ_author_name
'Nadia Malek'
'Thierry Maris'
'Marie-Eve Perron'
'James D. Wuest'
_publ_section_title
;
Molecular Tectonics: Porous Cleavable Networks Constructed by
Dipole-Directed Stacking of Hydrogen-Bonded Sheets
;
_journal_name_full 'Angew. Chem. Int. Ed.'
_journal_page_first 4021
_journal_page_last 4025
_journal_paper_doi 10.1002/anie.200500198
_journal_volume 44
_journal_year 2005
_chemical_compound_source 'Synthesized by the authors. See text'
_chemical_formula_moiety 'C15 H12 O4 P, 3(C3 H6 O2)'
_chemical_formula_sum 'C24 H30 N3 O10 P'
_chemical_formula_weight 551.48
_chemical_name_systematic
;
?
;
_space_group_IT_number 147
_symmetry_cell_setting trigonal
_symmetry_space_group_name_Hall '-P 3'
_symmetry_space_group_name_H-M 'P -3'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 120.00
_cell_formula_units_Z 2
_cell_length_a 17.1474(4)
_cell_length_b 17.1474(4)
_cell_length_c 5.3885(2)
_cell_measurement_reflns_used 5017
_cell_measurement_temperature 220(2)
_cell_measurement_theta_max 72.10
_cell_measurement_theta_min 2.98
_cell_volume 1372.13(7)
_computing_cell_refinement 'SMART (Bruker, 1999)'
_computing_data_collection 'SMART (Bruker, 1999)'
_computing_data_reduction 'SAINT (Bruker, 1999)'
_computing_molecular_graphics 'SHELXTL (Bruker, 1997)'
_computing_publication_material 'UdMX (local program)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 220(2)
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.931
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_device_type 'Bruker AXS Smart 2K/Platform'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'Sealed Tube'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.049
_diffrn_reflns_av_sigmaI/netI 0.0372
_diffrn_reflns_limit_h_max 20
_diffrn_reflns_limit_h_min -17
_diffrn_reflns_limit_k_max 20
_diffrn_reflns_limit_k_min -19
_diffrn_reflns_limit_l_max 5
_diffrn_reflns_limit_l_min -5
_diffrn_reflns_number 6995
_diffrn_reflns_theta_full 72.46
_diffrn_reflns_theta_max 72.46
_diffrn_reflns_theta_min 2.98
_diffrn_standards_decay_% -0.87
_diffrn_standards_number 141
_exptl_absorpt_coefficient_mu 1.402
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_correction_T_min 0.5300
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Sadabs (Sheldrick,1996)'
_exptl_crystal_colour Colourless
_exptl_crystal_density_diffrn 1.335
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 580
_exptl_crystal_size_max 0.40
_exptl_crystal_size_mid 0.40
_exptl_crystal_size_min 0.20
_refine_diff_density_max 0.403
_refine_diff_density_min -0.241
_refine_diff_density_rms 0.070
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.071
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 117
_refine_ls_number_reflns 1691
_refine_ls_number_restraints 2
_refine_ls_restrained_S_all 1.071
_refine_ls_R_factor_all 0.0773
_refine_ls_R_factor_gt 0.0682
_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^)+(0.1409P)^2^+0.2982P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1984
_refine_ls_wR_factor_ref 0.2065
_reflns_number_gt 1403
_reflns_number_total 1691
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file deposit.cif
_cod_data_source_block jiw383
_cod_original_sg_symbol_H-M P-3
_cod_database_code 1501596
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -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
P1 P 0.3333 0.6667 -0.1050(2) 0.0318(4) Uani 1 3 d S . .
O1 O 0.3333 0.6667 -0.3801(6) 0.0423(8) Uani 1 3 d S . .
O5 O 0.44136(15) 0.41566(13) 0.2857(4) 0.0546(6) Uani 1 1 d . . .
N4 N 0.44593(15) 0.54937(14) 0.2954(4) 0.0374(6) Uani 1 1 d . . .
H4 H 0.4826 0.5647 0.4208 0.045 Uiso 1 1 calc . . .
C2 C 0.36544(16) 0.58972(16) 0.0178(5) 0.0326(6) Uani 1 1 d . . .
C3 C 0.42290(17) 0.60967(16) 0.2131(5) 0.0352(6) Uani 1 1 d . . .
H3 H 0.4468 0.6660 0.2915 0.042 Uiso 1 1 calc . . .
C5 C 0.41525(18) 0.46578(17) 0.1941(6) 0.0399(7) Uani 1 1 d . . .
C6 C 0.3556(2) 0.44377(18) -0.0100(6) 0.0488(8) Uani 1 1 d . . .
H6 H 0.3323 0.3874 -0.0876 0.059 Uiso 1 1 calc . . .
C7 C 0.33191(19) 0.50376(18) -0.0939(6) 0.0440(7) Uani 1 1 d . . .
H7 H 0.2923 0.4880 -0.2294 0.053 Uiso 1 1 calc . . .
C11 C 0.2302(6) 0.0876(4) 0.8046(14) 0.121(3) Uani 0.870(4) 1 d P A 1
H11A H 0.2007 0.0225 0.8184 0.182 Uiso 1 1 calc R A 1
H11B H 0.1852 0.1059 0.7951 0.182 Uiso 1 1 calc R A 1
H11C H 0.2681 0.1150 0.9488 0.182 Uiso 1 1 calc R A 1
C12 C 0.2847(4) 0.1162(3) 0.5845(12) 0.1047(18) Uani 1 1 d . A 1
H12A H 0.2456 0.0870 0.4411 0.126 Uiso 1 1 calc R A 1
H12B H 0.3278 0.0946 0.5935 0.126 Uiso 1 1 calc R A 1
C13 C 0.3357(3) 0.2153(3) 0.5394(9) 0.0598(11) Uani 0.870(4) 1 d P A 1
O14 O 0.3456(4) 0.2693(3) 0.6941(8) 0.1185(18) Uani 0.870(4) 1 d P A 1
O15 O 0.3614(3) 0.23867(19) 0.3114(7) 0.0897(12) Uani 0.870(4) 1 d P A 1
H15 H 0.3780 0.2928 0.2928 0.135 Uiso 1 1 calc R A 1
C21 C 0.1808(5) 0.0705(5) 0.6292(7) 0.080 Uiso 0.130(4) 1 d PR A 2
C23 C 0.3103(4) 0.1960(7) 0.6105(8) 0.080 Uiso 0.130(4) 1 d PRD A 2
O24 O 0.3115(7) 0.2433(8) 0.4609(11) 0.080 Uiso 0.130(4) 1 d PRD A 2
O25 O 0.4162(5) 0.2157(10) 0.5737(10) 0.080 Uiso 0.130(4) 1 d PRD 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
P1 0.0352(4) 0.0352(4) 0.0250(7) 0.000 0.000 0.0176(2)
O1 0.0512(12) 0.0512(12) 0.025(2) 0.000 0.000 0.0256(6)
O5 0.0645(13) 0.0444(11) 0.0635(17) -0.0051(9) -0.0159(11) 0.0336(10)
N4 0.0439(12) 0.0388(11) 0.0337(15) -0.0058(9) -0.0081(9) 0.0239(10)
C2 0.0346(12) 0.0338(12) 0.0283(16) -0.0020(9) 0.0022(9) 0.0162(10)
C3 0.0422(13) 0.0351(12) 0.0312(16) -0.0046(9) -0.0037(10) 0.0216(11)
C5 0.0408(14) 0.0354(13) 0.0447(19) -0.0013(11) -0.0029(11) 0.0199(11)
C6 0.0534(16) 0.0357(14) 0.055(2) -0.0140(12) -0.0160(13) 0.0205(12)
C7 0.0488(15) 0.0424(14) 0.0417(19) -0.0112(11) -0.0145(12) 0.0235(12)
C11 0.159(7) 0.080(4) 0.105(6) 0.014(3) 0.035(5) 0.046(4)
C12 0.107(4) 0.065(3) 0.143(6) 0.005(3) 0.003(3) 0.044(3)
C13 0.054(2) 0.057(2) 0.068(3) -0.0060(19) 0.0002(19) 0.0273(18)
O14 0.176(5) 0.071(2) 0.085(3) -0.020(2) 0.005(3) 0.045(3)
O15 0.122(3) 0.0520(17) 0.098(3) -0.0048(16) 0.022(2) 0.0455(19)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 P1 C2 . 3_565 111.68(9) y
O1 P1 C2 . 2_665 111.68(9) y
C2 P1 C2 3_565 2_665 107.18(9) y
O1 P1 C2 . . 111.68(9) y
C2 P1 C2 3_565 . 107.18(9) y
C2 P1 C2 2_665 . 107.18(9) y
C3 N4 C5 . . 124.3(2) y
C3 N4 H4 . . 117.9 ?
C5 N4 H4 . . 117.9 ?
C3 C2 C7 . . 117.0(2) y
C3 C2 P1 . . 123.37(19) y
C7 C2 P1 . . 119.6(2) y
N4 C3 C2 . . 120.8(2) y
N4 C3 H3 . . 119.6 ?
C2 C3 H3 . . 119.6 ?
O5 C5 N4 . . 118.6(3) y
O5 C5 C6 . . 125.5(3) y
N4 C5 C6 . . 115.8(2) y
C7 C6 C5 . . 120.4(2) y
C7 C6 H6 . . 119.8 ?
C5 C6 H6 . . 119.8 ?
C6 C7 C2 . . 121.7(2) y
C6 C7 H7 . . 119.1 ?
C2 C7 H7 . . 119.1 ?
C12 C11 H11A . . 109.5 ?
C12 C11 H11B . . 109.5 ?
H11A C11 H11B . . 109.5 ?
C12 C11 H11C . . 109.5 ?
H11A C11 H11C . . 109.5 ?
H11B C11 H11C . . 109.5 ?
C11 C12 C13 . . 115.7(5) y
C11 C12 H12A . . 108.3 ?
C13 C12 H12A . . 108.3 ?
C11 C12 H12B . . 108.3 ?
C13 C12 H12B . . 108.3 ?
H12A C12 H12B . . 107.4 ?
O14 C13 O15 . . 121.7(4) y
O14 C13 C12 . . 123.1(5) y
O15 C13 C12 . . 114.9(4) y
O24 C23 O25 . . 98.05(19) y
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
P1 O1 . 1.482(4) y
P1 C2 3_565 1.791(2) y
P1 C2 2_665 1.791(2) y
P1 C2 . 1.791(2) y
O5 C5 . 1.252(3) y
N4 C3 . 1.353(3) y
N4 C5 . 1.369(3) y
N4 H4 . 0.87 ?
C2 C3 . 1.363(4) y
C2 C7 . 1.420(3) y
C3 H3 . 0.94 ?
C5 C6 . 1.419(4) y
C6 C7 . 1.358(4) y
C6 H6 . 0.94 ?
C7 H7 . 0.94 ?
C11 C12 . 1.435(8) y
C11 H11a . 0.97 ?
C11 H11b . 0.97 ?
C11 H11c . 0.97 ?
C12 C13 . 1.492(6) y
C12 H12a . 0.98 ?
C12 H12b . 0.98 ?
C13 O14 . 1.194(5) y
C13 O15 . 1.299(5) y
O15 H15 . 0.83 ?
C23 O24 . 1.136(6) y
C23 O25 . 1.684(6) y
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O15 H15 O5 0.83 1.82 2.636(3) 165.3 .
N4 H4 O5 0.87 1.97 2.834(3) 173.3 4_666
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
_geom_torsion_publ_flag
O1 P1 C2 C3 . 137.1(2) y
C2 P1 C2 C3 3_565 -100.25(17) y
C2 P1 C2 C3 2_665 14.5(3) y
O1 P1 C2 C7 . -41.4(2) y
C2 P1 C2 C7 3_565 81.2(3) y
C2 P1 C2 C7 2_665 -164.0(2) y
C5 N4 C3 C2 . 0.2(4) y
C7 C2 C3 N4 . -0.3(4) y
P1 C2 C3 N4 . -178.89(19) y
C3 N4 C5 O5 . 179.9(3) y
C3 N4 C5 C6 . 0.0(4) y
O5 C5 C6 C7 . -180.0(3) y
N4 C5 C6 C7 . -0.1(4) y
C5 C6 C7 C2 . 0.0(5) y
C3 C2 C7 C6 . 0.2(4) y
P1 C2 C7 C6 . 178.9(2) y
C11 C12 C13 O14 . 13.9(9) y
C11 C12 C13 O15 . -159.7(6) y
|
1501597.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501597.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_1501597
loop_
_publ_author_name
'Nadia Malek'
'Thierry Maris'
'Marie-Eve Perron'
'James D. Wuest'
_publ_section_title
;
Molecular Tectonics: Porous Cleavable Networks Constructed by
Dipole-Directed Stacking of Hydrogen-Bonded Sheets
;
_journal_name_full 'Angew. Chem. Int. Ed.'
_journal_page_first 4021
_journal_page_last 4025
_journal_paper_doi 10.1002/anie.200500198
_journal_volume 44
_journal_year 2005
_chemical_compound_source 'Synthesized by the authors. See text'
_chemical_formula_sum 'C21 H24 N3 O10 P'
_chemical_formula_weight 509.40
_chemical_name_systematic
;
?
;
_space_group_IT_number 147
_symmetry_cell_setting trigonal
_symmetry_space_group_name_Hall '-P 3'
_symmetry_space_group_name_H-M 'P -3'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 120.00
_cell_formula_units_Z 2
_cell_length_a 16.9535(8)
_cell_length_b 16.9535(8)
_cell_length_c 5.2396(3)
_cell_measurement_reflns_used 5990
_cell_measurement_temperature 223(2)
_cell_measurement_theta_max 69.61
_cell_measurement_theta_min 3.01
_cell_volume 1304.21(11)
_computing_cell_refinement 'SMART (Bruker, 1999)'
_computing_data_collection 'SMART (Bruker, 1999)'
_computing_data_reduction 'SAINT (Bruker, 1999)'
_computing_molecular_graphics 'SHELXTL (Bruker, 1997)'
_computing_publication_material 'UdMX (local program)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 223(2)
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type 'Bruker AXS Smart 2K/Platform'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'Sealed Tube'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.024
_diffrn_reflns_av_sigmaI/netI 0.0142
_diffrn_reflns_limit_h_max 20
_diffrn_reflns_limit_h_min -20
_diffrn_reflns_limit_k_max 20
_diffrn_reflns_limit_k_min -20
_diffrn_reflns_limit_l_max 6
_diffrn_reflns_limit_l_min -6
_diffrn_reflns_number 15509
_diffrn_reflns_theta_full 70.02
_diffrn_reflns_theta_max 70.02
_diffrn_reflns_theta_min 3.01
_diffrn_standards_decay_% -0.11
_diffrn_standards_number 83
_exptl_absorpt_coefficient_mu 1.433
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_correction_T_min 0.7800
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Sadabs (Sheldrick,1996)'
_exptl_crystal_colour Colourless
_exptl_crystal_density_diffrn 1.297
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 532
_exptl_crystal_size_max 0.40
_exptl_crystal_size_mid 0.15
_exptl_crystal_size_min 0.15
_refine_diff_density_max 0.605
_refine_diff_density_min -0.333
_refine_diff_density_rms 0.097
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.086
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 137
_refine_ls_number_reflns 1659
_refine_ls_number_restraints 73
_refine_ls_restrained_S_all 1.077
_refine_ls_R_factor_all 0.0841
_refine_ls_R_factor_gt 0.0772
_refine_ls_shift/su_max 0.674
_refine_ls_shift/su_mean 0.064
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1757P)^2^+0.8000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2660
_refine_ls_wR_factor_ref 0.2729
_reflns_number_gt 1404
_reflns_number_total 1659
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file deposit.cif
_cod_data_source_block jiw602
_cod_original_sg_symbol_H-M P-3
_cod_database_code 1501597
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -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
P1 P 0.3333 0.6667 1.1319(3) 0.0503(5) Uani 1 3 d S . .
O1 O 0.3333 0.6667 1.4119(8) 0.0668(12) Uani 1 3 d S . .
C1 C 0.3656(2) 0.7768(2) 1.0032(6) 0.0497(8) Uani 1 1 d . . .
C2 C 0.4242(2) 0.8139(2) 0.8041(6) 0.0514(8) Uani 1 1 d . . .
H2 H 0.4501 0.7817 0.7296 0.062 Uiso 1 1 calc . . .
N3 N 0.44561(19) 0.89688(18) 0.7119(5) 0.0540(8) Uani 1 1 d . . .
H3 H 0.4836 0.9185 0.5848 0.065 Uiso 1 1 calc . . .
C4 C 0.4111(2) 0.9489(2) 0.8066(7) 0.0592(9) Uani 1 1 d . . .
O4 O 0.4345(2) 1.02503(18) 0.7048(5) 0.0736(8) Uani 1 1 d . . .
C5 C 0.3513(3) 0.9115(3) 1.0192(8) 0.0665(10) Uani 1 1 d . . .
H5 H 0.3269 0.9448 1.0956 0.080 Uiso 1 1 calc . . .
C6 C 0.3295(3) 0.8289(3) 1.1118(7) 0.0619(9) Uani 1 1 d . . .
H6 H 0.2896 0.8052 1.2514 0.074 Uiso 1 1 calc . . .
O10 O 0.1540(13) 0.7647(11) 0.604(4) 0.202(7) Uani 0.598(10) 1 d PDU A 1
O11 O 0.0980(7) 0.7674(6) 0.226(3) 0.187(6) Uani 0.598(10) 1 d PDU A 1
H11 H 0.0919 0.7159 0.2085 0.280 Uiso 0.60 1 calc P A 1
C10 C 0.1332(6) 0.7997(8) 0.449(3) 0.165(9) Uani 0.598(10) 1 d PDU A 1
C11 C 0.1514(12) 0.8949(10) 0.528(5) 0.210(11) Uani 0.598(10) 1 d PDU A 1
H11A H 0.1462 0.9263 0.3803 0.315 Uiso 0.598(10) 1 calc PR A 1
H11B H 0.2123 0.9296 0.5992 0.315 Uiso 0.598(10) 1 calc PR A 1
H11C H 0.1071 0.8887 0.6559 0.315 Uiso 0.598(10) 1 calc PR A 1
O20 O 0.183(2) 0.795(3) 0.585(8) 0.202(7) Uani 0.311(9) 1 d PDU B 2
O21 O 0.0483(14) 0.7488(11) 0.463(6) 0.187(6) Uani 0.311(9) 1 d PDU B 2
H21 H 0.0548 0.7073 0.4019 0.280 Uiso 0.31 1 calc P B 2
C20 C 0.1193(16) 0.8020(15) 0.602(5) 0.165(9) Uani 0.311(9) 1 d PDU B 2
C21 C 0.122(2) 0.873(2) 0.789(9) 0.210(11) Uani 0.311(9) 1 d PDU B 2
H21A H 0.1044 0.8467 0.9572 0.315 Uiso 0.311(9) 1 calc PR B 2
H21B H 0.0809 0.8935 0.7309 0.315 Uiso 0.311(9) 1 calc PR B 2
H21C H 0.1838 0.9251 0.7953 0.315 Uiso 0.311(9) 1 calc PR B 2
O30 O 0.097(7) 0.764(7) 0.82(2) 0.240 Uiso 0.091(9) 1 d PD C 3
O31 O -0.018(7) 0.739(7) 0.583(19) 0.240 Uiso 0.091(9) 1 d PD C 3
H31 H -0.0535 0.7238 0.7064 0.360 Uiso 0.09 1 calc P C 3
C30 C 0.051(6) 0.729(5) 0.642(16) 0.240 Uiso 0.091(9) 1 d PD C 3
C31 C 0.077(10) 0.670(10) 0.48(2) 0.240 Uiso 0.091(9) 1 d PD C 3
H31A H 0.0735 0.6208 0.5803 0.360 Uiso 0.091(9) 1 calc PR C 3
H31B H 0.1385 0.7072 0.4135 0.360 Uiso 0.091(9) 1 calc PR C 3
H31C H 0.0350 0.6449 0.3352 0.360 Uiso 0.091(9) 1 calc PR C 3
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
P1 0.0513(6) 0.0513(6) 0.0483(8) 0.000 0.000 0.0257(3)
O1 0.0754(17) 0.0754(17) 0.050(2) 0.000 0.000 0.0377(9)
C1 0.0505(17) 0.0495(16) 0.0485(16) -0.0038(12) -0.0030(12) 0.0245(14)
C2 0.0550(18) 0.0473(16) 0.0515(17) -0.0055(13) -0.0020(13) 0.0253(14)
N3 0.0591(16) 0.0477(14) 0.0542(15) -0.0014(11) 0.0022(12) 0.0258(12)
C4 0.061(2) 0.0522(18) 0.068(2) -0.0018(15) -0.0039(16) 0.0302(16)
O4 0.0825(18) 0.0562(15) 0.090(2) 0.0102(13) 0.0124(15) 0.0402(14)
C5 0.070(2) 0.063(2) 0.078(2) 0.0008(17) 0.0122(18) 0.0419(18)
C6 0.063(2) 0.062(2) 0.064(2) 0.0005(15) 0.0093(16) 0.0338(17)
O10 0.292(17) 0.121(14) 0.194(9) -0.022(9) -0.074(10) 0.103(13)
O11 0.098(7) 0.089(5) 0.36(2) -0.008(8) -0.031(7) 0.035(5)
C10 0.072(6) 0.134(9) 0.27(2) 0.081(13) 0.009(10) 0.034(5)
C11 0.132(12) 0.095(9) 0.40(4) -0.032(15) -0.020(16) 0.056(9)
O20 0.292(17) 0.121(14) 0.194(9) -0.022(9) -0.074(10) 0.103(13)
O21 0.098(7) 0.089(5) 0.36(2) -0.008(8) -0.031(7) 0.035(5)
C20 0.072(6) 0.134(9) 0.27(2) 0.081(13) 0.009(10) 0.034(5)
C21 0.132(12) 0.095(9) 0.40(4) -0.032(15) -0.020(16) 0.056(9)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 '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
O1 P1 C1 . . 112.08(11) y
O1 P1 C1 . 2_665 112.08(11) y
C1 P1 C1 . 2_665 106.74(12) y
O1 P1 C1 . 3_565 112.08(11) y
C1 P1 C1 . 3_565 106.74(12) y
C1 P1 C1 2_665 3_565 106.74(12) y
C2 C1 C6 . . 117.5(3) y
C2 C1 P1 . . 122.9(2) y
C6 C1 P1 . . 119.6(2) y
N3 C2 C1 . . 120.6(3) y
N3 C2 H2 . . 119.7 ?
C1 C2 H2 . . 119.7 ?
C2 N3 C4 . . 124.0(3) y
C2 N3 H3 . . 118 ?
C4 N3 H3 . . 118 ?
O4 C4 N3 . . 119.1(3) y
O4 C4 C5 . . 125.1(3) y
N3 C4 C5 . . 115.8(3) y
C4 O4 C31 . 6_666 146(5) y
C6 C5 C4 . . 120.5(3) y
C6 C5 H5 . . 119.7 ?
C4 C5 H5 . . 119.7 ?
C5 C6 C1 . . 121.5(3) y
C5 C6 H6 . . 119.2 ?
C1 C6 H6 . . 119.2 ?
C10 O11 H11 . . 109.2 ?
O10 C10 O11 . . 127.30(14) y
O10 C10 C11 . . 113.20(14) y
O11 C10 C11 . . 119.50(13) y
C20 O21 H21 . . 109.5 ?
O20 C20 O21 . . 118(3) y
O20 C20 C21 . . 118(2) y
O21 C20 C21 . . 124(2) y
C20 C21 H21A . . 109.6 ?
C20 C21 H21B . . 109.6 ?
H21A C21 H21B . . 109.4 ?
C20 C21 H21C . . 109.4 ?
H21A C21 H21C . . 109.4 ?
H21B C21 H21C . . 109.4 ?
C30 O31 H31 . . 109.3 ?
O30 C30 O31 . . 122(3) y
O30 C30 C31 . . 117(3) y
O31 C30 C31 . . 121(3) y
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
P1 O1 . 1.467(4) y
P1 C1 . 1.794(3) y
P1 C1 2_665 1.794(3) y
P1 C1 3_565 1.794(3) y
C1 C2 . 1.359(5) y
C1 C6 . 1.420(5) y
C2 N3 . 1.353(4) y
C2 H2 . 0.94 ?
N3 C4 . 1.372(4) y
N3 H3 . 0.8699 ?
C4 O4 . 1.263(4) y
C4 C5 . 1.424(5) y
O4 C31 6_666 1.52(13) y
C5 C6 . 1.348(5) y
C5 H5 . 0.9401 ?
C6 H6 . 0.9401 ?
O10 C10 . 1.161(8) y
O11 C10 . 1.300(8) y
O11 H11 . 0.8316 ?
C10 C11 . 1.541(8) y
C11 H11a . 0.97 ?
C11 H11b . 0.97 ?
C11 H11c . 0.97 ?
O20 C20 . 1.148(19) y
O21 C20 . 1.306(18) y
O21 H21 . 0.8303 ?
C20 C21 . 1.536(19) y
C21 H21a . 0.9707 ?
C21 H21b . 0.9707 ?
C21 H21c . 0.9707 ?
O30 C30 . 1.16(2) y
O31 C30 . 1.31(2) y
O31 H31 . 0.8251 ?
C30 C31 . 1.54(2) y
C31 H31a . 1.0267 ?
C31 H31b . 1.0253 ?
C31 H31c . 1.0236 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N3 H3 O4 0.87 1.95 2.821(4) 175.0 4_676
O11 H11 O4 0.83 1.90 2.635(10) 147.3 5_456
O21 H21 O4 0.83 1.87 2.66(2) 159.3 5_456
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_4
_geom_torsion
_geom_torsion_publ_flag
O1 P1 C1 C2 . . 136.4(3) y
C1 P1 C1 C2 2_665 . -100.5(2) y
C1 P1 C1 C2 3_565 . 13.3(3) y
O1 P1 C1 C6 . . -43.3(3) y
C1 P1 C1 C6 2_665 . 79.8(4) y
C1 P1 C1 C6 3_565 . -166.3(3) y
C6 C1 C2 N3 . . -1.1(5) y
P1 C1 C2 N3 . . 179.2(2) y
C1 C2 N3 C4 . . -0.3(5) y
C2 N3 C4 O4 . . -179.1(3) y
C2 N3 C4 C5 . . 1.7(5) y
N3 C4 O4 C31 . 6_666 101(10) y
C5 C4 O4 C31 . 6_666 -80(10) y
O4 C4 C5 C6 . . 179.1(4) y
N3 C4 C5 C6 . . -1.8(6) y
C4 C5 C6 C1 . . 0.5(6) y
C2 C1 C6 C5 . . 1.0(6) y
P1 C1 C6 C5 . . -179.3(3) y
|
1501598.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501598.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_1501598
loop_
_publ_author_name
'Nadia Malek'
'Thierry Maris'
'Marie-Eve Perron'
'James D. Wuest'
_publ_section_title
;
Molecular Tectonics: Porous Cleavable Networks Constructed by
Dipole-Directed Stacking of Hydrogen-Bonded Sheets
;
_journal_name_full 'Angew. Chem. Int. Ed.'
_journal_page_first 4021
_journal_page_last 4025
_journal_paper_doi 10.1002/anie.200500198
_journal_volume 44
_journal_year 2005
_chemical_compound_source 'Synthesized by the authors. See text'
_chemical_formula_sum 'C24 H24 N3 O10 P'
_chemical_formula_weight 545.43
_chemical_name_systematic
;
?
;
_space_group_IT_number 147
_symmetry_cell_setting trigonal
_symmetry_space_group_name_Hall '-P 3'
_symmetry_space_group_name_H-M 'P -3'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 120.00
_cell_formula_units_Z 2
_cell_length_a 17.4823(8)
_cell_length_b 17.4823(8)
_cell_length_c 5.0683(8)
_cell_measurement_reflns_used 1755
_cell_measurement_temperature 223(2)
_cell_measurement_theta_max 47.15
_cell_measurement_theta_min 2.92
_cell_volume 1341.5(2)
_computing_cell_refinement 'SMART (Bruker, 1999)'
_computing_data_collection 'SMART (Bruker, 1999)'
_computing_data_reduction 'SAINT (Bruker, 1999)'
_computing_molecular_graphics 'SHELXTL (Bruker, 1997)'
_computing_publication_material 'UdMX (local program)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 223(2)
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type 'Bruker AXS Smart 2K/Platform'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'Sealed Tube'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.107
_diffrn_reflns_av_sigmaI/netI 0.0927
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -18
_diffrn_reflns_limit_k_max 19
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_l_max 5
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_number 6101
_diffrn_reflns_theta_full 58.73
_diffrn_reflns_theta_max 58.73
_diffrn_reflns_theta_min 2.92
_diffrn_standards_decay_% -1.25
_diffrn_standards_number 72
_exptl_absorpt_coefficient_mu 1.433
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_correction_T_min 0.2000
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Sadabs (Sheldrick,1996)'
_exptl_crystal_colour Colourless
_exptl_crystal_density_diffrn 1.350
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 568
_exptl_crystal_size_max 0.60
_exptl_crystal_size_mid 0.25
_exptl_crystal_size_min 0.25
_refine_diff_density_max 0.541
_refine_diff_density_min -0.243
_refine_diff_density_rms 0.079
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.031
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 115
_refine_ls_number_reflns 1211
_refine_ls_number_restraints 30
_refine_ls_restrained_S_all 1.020
_refine_ls_R_factor_all 0.1559
_refine_ls_R_factor_gt 0.0956
_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^)+(0.1426P)^2^+1.5870P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2542
_refine_ls_wR_factor_ref 0.2886
_reflns_number_gt 699
_reflns_number_total 1211
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file deposit.cif
_cod_data_source_block jiw629
_cod_original_sg_symbol_H-M P-3
_cod_database_code 1501598
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -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
P1 P 0.6667 0.3333 1.1167(5) 0.0636(11) Uani 1 3 d S
O1 O 0.6667 0.3333 1.4025(14) 0.077(2) Uani 1 3 d S
C1 C 0.7732(4) 0.3666(4) 0.9883(12) 0.0566(17) Uani 1 1 d .
C2 C 0.8120(4) 0.4248(4) 0.7944(12) 0.0587(17) Uani 1 1 d .
H2 H 0.7819 0.4508 0.7149 0.070 Uiso 1 1 calc .
N3 N 0.8925(3) 0.4467(3) 0.7114(9) 0.0632(16) Uani 1 1 d .
H3 H 0.9155 0.4856 0.5855 0.076 Uiso 1 1 calc .
C4 C 0.9417(5) 0.4125(4) 0.8104(13) 0.0679(19) Uani 1 1 d .
O4 O 1.0167(3) 0.4375(3) 0.7154(9) 0.0855(16) Uani 1 1 d .
C5 C 0.9056(5) 0.3542(5) 1.0164(15) 0.082(2) Uani 1 1 d .
H5 H 0.9376 0.3306 1.0972 0.098 Uiso 1 1 calc .
C6 C 0.8243(5) 0.3314(4) 1.1015(12) 0.074(2) Uani 1 1 d .
H6 H 0.7998 0.2907 1.2409 0.089 Uiso 1 1 calc .
C10 C 0.1353(8) 0.3425(9) 0.592(3) 0.123(4) Uani 1 1 d U
O10 O 0.0803(6) 0.3294(5) 0.7747(18) 0.156(3) Uani 1 1 d U
H10 H 0.0664 0.3683 0.7693 0.234 Uiso 1 1 calc .
O11 O 0.1598(6) 0.4004(6) 0.447(2) 0.173(4) Uani 1 1 d U
C11 C 0.1663(8) 0.2800(10) 0.588(3) 0.166(5) Uani 1 1 d U
H11 H 0.2019 0.2832 0.4448 0.199 Uiso 1 1 calc .
C12 C 0.1508(14) 0.2233(16) 0.754(5) 0.258(10) Uani 1 1 d U
H12A H 0.1155 0.2175 0.9008 0.310 Uiso 1 1 calc .
H12B H 0.1741 0.1854 0.7343 0.310 Uiso 1 1 calc .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
P1 0.0675(15) 0.0675(15) 0.0558(19) 0.000 0.000 0.0337(8)
O1 0.085(4) 0.085(4) 0.060(5) 0.000 0.000 0.0426(18)
C1 0.056(4) 0.058(4) 0.053(4) -0.003(3) -0.001(3) 0.026(3)
C2 0.044(4) 0.072(4) 0.056(4) -0.001(3) -0.005(3) 0.026(3)
N3 0.050(3) 0.068(4) 0.063(3) 0.009(3) -0.006(3) 0.023(3)
C4 0.054(5) 0.072(5) 0.074(5) 0.003(4) 0.004(4) 0.028(4)
O4 0.065(3) 0.101(4) 0.096(3) 0.018(3) 0.005(3) 0.045(3)
C5 0.068(5) 0.095(6) 0.093(5) 0.021(4) 0.012(4) 0.049(4)
C6 0.090(6) 0.072(5) 0.067(4) 0.012(3) 0.001(4) 0.044(4)
C10 0.073(7) 0.114(10) 0.171(12) 0.002(8) -0.020(7) 0.039(7)
O10 0.133(6) 0.162(7) 0.204(8) 0.041(6) 0.020(6) 0.096(6)
O11 0.181(8) 0.146(7) 0.209(9) 0.049(6) 0.040(6) 0.094(6)
C11 0.123(9) 0.129(10) 0.258(17) 0.002(10) -0.018(9) 0.073(9)
C12 0.261(19) 0.27(2) 0.33(3) 0.070(17) 0.027(18) 0.200(17)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 '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
O1 P1 C1 . . 111.5(2) y
O1 P1 C1 . 3_665 111.5(2) y
C1 P1 C1 . 3_665 107.4(2) y
O1 P1 C1 . 2_655 111.5(2) y
C1 P1 C1 . 2_655 107.4(2) y
C1 P1 C1 3_665 2_655 107.4(2) y
C2 C1 C6 . . 115.8(6) y
C2 C1 P1 . . 124.8(5) y
C6 C1 P1 . . 119.3(5) y
N3 C2 C1 . . 121.0(5) y
N3 C2 H2 . . 119.5 ?
C1 C2 H2 . . 119.5 ?
C2 N3 C4 . . 124.5(5) y
C2 N3 H3 . . 117.8 ?
C4 N3 H3 . . 117.8 ?
O4 C4 N3 . . 118.9(6) y
O4 C4 C5 . . 124.4(7) y
N3 C4 C5 . . 116.6(6) y
C6 C5 C4 . . 119.4(6) y
C6 C5 H5 . . 120.3 ?
C4 C5 H5 . . 120.3 ?
C5 C6 C1 . . 122.6(6) y
C5 C6 H6 . . 118.7 ?
C1 C6 H6 . . 118.7 ?
O11 C10 O10 . . 122.70(13) y
O11 C10 C11 . . 123.10(16) y
O10 C10 C11 . . 114.10(13) y
C10 O10 H10 . . 109.5 ?
C12 C11 C10 . . 126.20(18) y
C12 C11 H11 . . 116.9 ?
C10 C11 H11 . . 116.9 ?
C11 C12 H12A . . 120 ?
C11 C12 H12B . . 120 ?
H12A C12 H12B . . 120 ?
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
P1 O1 . 1.448(7) y
P1 C1 . 1.774(6) y
P1 C1 3_665 1.774(6) y
P1 C1 2_655 1.774(6) y
C1 C2 . 1.331(8) y
C1 C6 . 1.433(8) y
C2 N3 . 1.329(7) y
C2 H2 . 0.94 ?
N3 C4 . 1.366(8) y
N3 H3 . 0.87 ?
C4 O4 . 1.252(7) y
C4 C5 . 1.372(9) y
C5 C6 . 1.341(9) y
C5 H5 . 0.94 ?
C6 H6 . 0.94 ?
C10 O11 . 1.144(12) y
C10 O10 . 1.272(13) y
C10 C11 . 1.443(16) y
O10 H10 . 0.83 ?
C11 C12 . 1.221(19) y
C11 H11 . 0.94 ?
C12 H12a . 0.94 ?
C12 H12b . 0.94 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N3 H3 O4 0.87 1.99 2.843(7) 167.9 4_766
O10 H10 O4 0.83 1.83 2.646(8) 168.1 1_455
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
_geom_torsion_publ_flag
O1 P1 C1 C2 . -133.8(5) y
C1 P1 C1 C2 3_665 103.7(4) y
C1 P1 C1 C2 2_655 -11.4(7) y
O1 P1 C1 C6 . 44.3(5) y
C1 P1 C1 C6 3_665 -78.1(6) y
C1 P1 C1 C6 2_655 166.8(5) y
C6 C1 C2 N3 . 1.1(9) y
P1 C1 C2 N3 . 179.3(4) y
C1 C2 N3 C4 . 0.8(9) y
C2 N3 C4 O4 . 179.4(6) y
C2 N3 C4 C5 . -2.7(9) y
O4 C4 C5 C6 . -179.5(7) y
N3 C4 C5 C6 . 2.7(1) y
C4 C5 C6 C1 . -1.00(11) y
C2 C1 C6 C5 . -1.0(1) y
P1 C1 C6 C5 . -179.3(6) y
O11 C10 C11 C12 . 171.00(19) y
O10 C10 C11 C12 . -7(2) y
|
1501599.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501599.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_1501599
loop_
_publ_author_name
'Danielle Boils'
'Marie-Eve Perron'
'Francis Monchamp'
'Hugues Duval'
'Thierry Maris'
'James D. Wuest'
_publ_section_title
;
Molecular Tectonics. Disruption of Self-Association in Melts Derived from
Hydrogen-Bonded Solids
;
_journal_name_full Macromolecules
_journal_page_first 7351
_journal_page_last 7357
_journal_paper_doi 10.1021/ma035977d
_journal_volume 37
_journal_year 2004
_chemical_compound_source 'Synthesized by the authors. See text'
_chemical_formula_moiety 'C69 H100 N24, 10(C4 H8 O2)'
_chemical_formula_sum 'C109 H180 N24 O20'
_chemical_formula_weight 2146.77
_chemical_name_systematic
;
?
;
_space_group_IT_number 82
_symmetry_cell_setting tetragonal
_symmetry_space_group_name_Hall 'I -4'
_symmetry_space_group_name_H-M 'I -4'
_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 2
_cell_length_a 11.8715(3)
_cell_length_b 11.8715(3)
_cell_length_c 40.004(2)
_cell_measurement_reflns_used 29551
_cell_measurement_temperature 226(2)
_cell_measurement_theta_max 72.14
_cell_measurement_theta_min 2.16
_cell_volume 5637.9(3)
_computing_cell_refinement 'SMART (Bruker, 1999)'
_computing_data_collection 'SMART (Bruker, 1999)'
_computing_data_reduction 'SAINT (Bruker, 1999)'
_computing_molecular_graphics 'SHELXTL (Bruker, 1997)'
_computing_publication_material 'UdMX (local program)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 226(2)
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type 'Bruker AXS Smart 2K/Platform'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'Sealed Tube'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.076
_diffrn_reflns_av_sigmaI/netI 0.0330
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_l_max 40
_diffrn_reflns_limit_l_min -44
_diffrn_reflns_number 36656
_diffrn_reflns_theta_full 58.88
_diffrn_reflns_theta_max 58.88
_diffrn_reflns_theta_min 2.21
_diffrn_standards_decay_% 0.00
_diffrn_standards_interval_time 2880
_diffrn_standards_number 1
_exptl_absorpt_coefficient_mu 0.715
_exptl_absorpt_correction_T_max 0.8600
_exptl_absorpt_correction_T_min 0.2100
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Sadabs (Sheldrick,1996)'
_exptl_crystal_colour Colourless
_exptl_crystal_density_diffrn 1.265
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 2324
_exptl_crystal_size_max 0.55
_exptl_crystal_size_mid 0.40
_exptl_crystal_size_min 0.40
_refine_diff_density_max 0.467
_refine_diff_density_min -0.317
_refine_diff_density_rms 0.081
_refine_ls_abs_structure_details 'Flack H D (1983), 1960 Friedel Pairs'
_refine_ls_abs_structure_Flack 0.3(9)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.077
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 403
_refine_ls_number_reflns 4045
_refine_ls_number_restraints 450
_refine_ls_restrained_S_all 1.064
_refine_ls_R_factor_all 0.0876
_refine_ls_R_factor_gt 0.0868
_refine_ls_shift/su_max 0.027
_refine_ls_shift/su_mean 0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1511P)^2^+5.6939P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2183
_refine_ls_wR_factor_ref 0.2195
_reflns_number_gt 3953
_reflns_number_total 4045
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file deposit.cif
_cod_data_source_block jiw300
_cod_original_cell_volume 5637.9(4)
_cod_original_sg_symbol_H-M I-4
_cod_database_code 1501599
loop_
_symmetry_equiv_pos_as_xyz
'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'
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 0.0000 1.0000 0.0000 0.040(2) Uani 1 4 d S . .
N1 N 0.3687(4) 0.9333(3) 0.09221(11) 0.0436(10) Uani 1 1 d . . .
H1A H 0.4002 0.9963 0.0983 0.052 Uiso 1 1 calc R . .
C2 C 0.0995(5) 0.9760(4) 0.02419(14) 0.0446(12) Uani 1 1 d . . .
N2 N 0.5110(4) 0.8555(4) 0.12261(10) 0.0449(10) Uani 1 1 d . . .
C3 C 0.1354(5) 1.0602(5) 0.04606(14) 0.0466(13) Uani 1 1 d . . .
H3 H 0.0988 1.1303 0.0454 0.056 Uiso 1 1 calc R . .
N3 N 0.3624(5) 0.7396(4) 0.10132(13) 0.0552(12) Uani 1 1 d . . .
C4 C 0.2216(5) 1.0454(4) 0.06842(13) 0.0416(11) Uani 1 1 d . . .
H4 H 0.2430 1.1043 0.0828 0.050 Uiso 1 1 calc R . .
N4 N 0.5044(5) 0.6583(5) 0.13616(12) 0.0591(13) Uani 1 1 d . . .
C5 C 0.2771(4) 0.9424(5) 0.06964(14) 0.0426(12) Uani 1 1 d . . .
N5 N 0.3693(6) 0.5497(5) 0.11226(18) 0.0747(17) Uani 1 1 d . B .
H5A H 0.4009 0.4941 0.1229 0.090 Uiso 1 1 calc R . .
C6 C 0.2437(5) 0.8576(5) 0.04844(15) 0.0512(13) Uani 1 1 d . . .
H6 H 0.2789 0.7867 0.0493 0.061 Uiso 1 1 calc R . .
N6 N 0.6431(6) 0.7739(4) 0.15674(14) 0.0667(16) Uani 1 1 d . . .
H6A H 0.6741 0.7126 0.1644 0.080 Uiso 1 1 calc R . .
C7 C 0.1570(5) 0.8772(5) 0.02554(15) 0.0507(13) Uani 1 1 d . . .
H7 H 0.1377 0.8196 0.0105 0.061 Uiso 1 1 calc R . .
C9 C 0.4129(5) 0.8375(5) 0.10549(13) 0.0440(12) Uani 1 1 d . . .
C10 C 0.5509(5) 0.7631(4) 0.13702(15) 0.0468(13) Uani 1 1 d . . .
C11 C 0.4134(5) 0.6535(5) 0.11680(16) 0.0506(14) Uani 1 1 d . . .
C12 C 0.6943(6) 0.8820(5) 0.16611(18) 0.0644(17) Uani 1 1 d . . .
H12A H 0.6501 0.9434 0.1564 0.077 Uiso 1 1 calc R . .
H12B H 0.7705 0.8860 0.1567 0.077 Uiso 1 1 calc R . .
C13 C 0.7006(11) 0.8979(9) 0.2029(2) 0.103(3) Uani 1 1 d . . .
H13A H 0.6240 0.8938 0.2119 0.124 Uiso 1 1 calc R . .
H13B H 0.7431 0.8348 0.2124 0.124 Uiso 1 1 calc R . .
C14 C 0.7512(11) 1.0012(10) 0.2145(3) 0.107(3) Uani 1 1 d . . .
H14A H 0.8252 1.0111 0.2040 0.129 Uiso 1 1 calc R . .
H14B H 0.7619 0.9978 0.2388 0.129 Uiso 1 1 calc R . .
C15 C 0.6729(12) 1.1041(12) 0.2054(4) 0.135(5) Uani 1 1 d . . .
H15A H 0.6542 1.1013 0.1818 0.202 Uiso 1 1 calc R . .
H15B H 0.7121 1.1739 0.2102 0.202 Uiso 1 1 calc R . .
H15C H 0.6044 1.1002 0.2185 0.202 Uiso 1 1 calc R . .
C16 C 0.2735(7) 0.5234(5) 0.0910(2) 0.076(2) Uani 1 1 d . . .
H16A H 0.2695 0.5785 0.0728 0.091 Uiso 1 1 calc R A 1
H16B H 0.2040 0.5297 0.1041 0.091 Uiso 1 1 calc R A 1
C17A C 0.314(2) 0.502(3) 0.0571(5) 0.098(10) Uani 0.39(3) 1 d P B 2
H17A H 0.2492 0.5026 0.0420 0.117 Uiso 0.39(3) 1 calc PR B 2
H17B H 0.3633 0.5644 0.0506 0.117 Uiso 0.39(3) 1 calc PR B 2
C17 C 0.2815(18) 0.4011(14) 0.0757(6) 0.120(9) Uani 0.61(3) 1 d P B 1
H17A H 0.2950 0.3461 0.0936 0.144 Uiso 0.61(3) 1 calc PR B 1
H17B H 0.2106 0.3817 0.0646 0.144 Uiso 0.61(3) 1 calc PR B 1
C18 C 0.3749(15) 0.3985(12) 0.0515(3) 0.162(7) Uani 1 1 d . . .
H18A H 0.4463 0.4128 0.0630 0.194 Uiso 1 1 calc R B 1
H18B H 0.3641 0.4576 0.0347 0.194 Uiso 1 1 calc R B 1
C19 C 0.3792(15) 0.2809(12) 0.0341(3) 0.284(18) Uani 1 1 d R B .
H19A H 0.4001 0.2239 0.0503 0.426 Uiso 1 1 calc R . .
H19B H 0.4344 0.2825 0.0162 0.426 Uiso 1 1 calc R . .
H19C H 0.3057 0.2632 0.0249 0.426 Uiso 1 1 calc R . .
O50A O 1.0922(9) 0.7388(16) 0.3026(4) 0.155(5) Uani 0.692(11) 1 d PDU C 3
C50A C 0.9834(10) 0.7229(16) 0.3137(3) 0.126(4) Uani 0.692(11) 1 d PDU C 3
H50A H 0.9822 0.7232 0.3382 0.152 Uiso 0.692(11) 1 calc PR C 3
H50B H 0.9561 0.6493 0.3060 0.152 Uiso 0.692(11) 1 calc PR C 3
C51A C 0.9072(14) 0.8135(17) 0.3008(3) 0.144(5) Uani 0.692(11) 1 d PDU C 3
H51A H 0.8316 0.8061 0.3104 0.173 Uiso 0.692(11) 1 calc PR C 3
H51B H 0.9370 0.8882 0.3063 0.173 Uiso 0.692(11) 1 calc PR C 3
O51A O 0.9041(12) 0.7982(18) 0.2667(3) 0.171(5) Uani 0.692(11) 1 d PDU C 3
C52A C 1.0051(14) 0.8441(18) 0.2564(3) 0.158(4) Uani 0.692(11) 1 d PDU C 3
H52A H 1.0218 0.9155 0.2676 0.189 Uiso 0.692(11) 1 calc PR C 3
H52B H 1.0089 0.8539 0.2321 0.189 Uiso 0.692(11) 1 calc PR C 3
C53A C 1.0786(14) 0.750(2) 0.2685(3) 0.161(4) Uani 0.692(11) 1 d PDU C 3
H53A H 1.0475 0.6788 0.2600 0.193 Uiso 0.692(11) 1 calc PR C 3
H53B H 1.1534 0.7590 0.2585 0.193 Uiso 0.692(11) 1 calc PR C 3
O50B O 1.109(3) 0.788(3) 0.2941(8) 0.155(5) Uani 0.308(11) 1 d PDU C 4
C50B C 1.034(3) 0.876(3) 0.2918(7) 0.126(4) Uani 0.308(11) 1 d PDU C 4
H50A H 1.0536 0.9265 0.2732 0.152 Uiso 0.308(11) 1 calc PR C 4
H50B H 1.0330 0.9202 0.3126 0.152 Uiso 0.308(11) 1 calc PR C 4
C51B C 0.921(2) 0.823(4) 0.2858(9) 0.144(5) Uani 0.308(11) 1 d PDU C 4
H51C H 0.9082 0.7599 0.3013 0.173 Uiso 0.308(11) 1 calc PR C 4
H51D H 0.8599 0.8777 0.2883 0.173 Uiso 0.308(11) 1 calc PR C 4
O51B O 0.929(3) 0.785(4) 0.2532(7) 0.171(5) Uani 0.308(11) 1 d PDU C 4
C52B C 0.983(3) 0.683(4) 0.2570(8) 0.158(4) Uani 0.308(11) 1 d PDU C 4
H52C H 0.9817 0.6375 0.2366 0.189 Uiso 0.308(11) 1 calc PR C 4
H52D H 0.9541 0.6395 0.2759 0.189 Uiso 0.308(11) 1 calc PR C 4
C53B C 1.096(3) 0.735(4) 0.2637(11) 0.161(4) Uani 0.308(11) 1 d PDU C 4
H53C H 1.1528 0.6754 0.2621 0.193 Uiso 0.308(11) 1 calc PR C 4
H53D H 1.1116 0.7895 0.2460 0.193 Uiso 0.308(11) 1 calc PR C 4
O60A O 0.0285(14) 0.8493(12) 0.1140(4) 0.107(3) Uani 0.500(8) 1 d PDU D 5
C60A C 0.1027(13) 0.8502(12) 0.1404(3) 0.079(2) Uani 0.500(8) 1 d PDU D 5
H60A H 0.1034 0.9266 0.1496 0.094 Uiso 0.500(8) 1 calc PR D 5
H60B H 0.1781 0.8357 0.1314 0.094 Uiso 0.500(8) 1 calc PR D 5
C61A C 0.0845(15) 0.7707(16) 0.1687(3) 0.103(4) Uani 0.500(8) 1 d PDU D 5
H61A H 0.1360 0.7067 0.1664 0.124 Uiso 0.500(8) 1 calc PR D 5
H61B H 0.1026 0.8091 0.1898 0.124 Uiso 0.500(8) 1 calc PR D 5
O61A O -0.0242(14) 0.7316(19) 0.1702(3) 0.151(5) Uani 0.500(8) 1 d PDU D 5
C62A C -0.042(2) 0.690(2) 0.1384(4) 0.130(4) Uani 0.500(8) 1 d PDU D 5
H62A H -0.1236 0.6948 0.1345 0.156 Uiso 0.500(8) 1 calc PR D 5
H62B H -0.0235 0.6099 0.1392 0.156 Uiso 0.500(8) 1 calc PR D 5
C63A C 0.013(2) 0.7364(14) 0.1077(3) 0.120(4) Uani 0.500(8) 1 d PDU D 5
H63A H 0.0857 0.6992 0.1038 0.144 Uiso 0.500(8) 1 calc PR D 5
H63B H -0.0348 0.7255 0.0881 0.144 Uiso 0.500(8) 1 calc PR D 5
O60B O 0.0617(12) 0.8194(13) 0.1179(3) 0.107(3) Uani 0.500(8) 1 d PDU D 6
C60B C 0.0020(14) 0.8607(10) 0.1451(3) 0.079(2) Uani 0.500(8) 1 d PDU D 6
H60C H -0.0763 0.8771 0.1390 0.094 Uiso 0.500(8) 1 calc PR D 6
H60D H 0.0371 0.9291 0.1540 0.094 Uiso 0.500(8) 1 calc PR D 6
C61B C 0.009(2) 0.7654(12) 0.1696(3) 0.103(4) Uani 0.500(8) 1 d PDU D 6
H61C H 0.0870 0.7396 0.1716 0.124 Uiso 0.500(8) 1 calc PR D 6
H61D H -0.0169 0.7904 0.1916 0.124 Uiso 0.500(8) 1 calc PR D 6
O61B O -0.0587(16) 0.6786(16) 0.1580(4) 0.151(5) Uani 0.500(8) 1 d PDU D 6
C62B C -0.011(2) 0.6529(14) 0.1276(4) 0.130(4) Uani 0.500(8) 1 d PDU D 6
H62C H -0.0494 0.5875 0.1181 0.156 Uiso 0.500(8) 1 calc PR D 6
H62D H 0.0683 0.6323 0.1311 0.156 Uiso 0.500(8) 1 calc PR D 6
C63B C -0.017(2) 0.7489(15) 0.1032(4) 0.120(4) Uani 0.500(8) 1 d PDU D 6
H63C H 0.0059 0.7260 0.0807 0.144 Uiso 0.500(8) 1 calc PR D 6
H63D H -0.0919 0.7830 0.1025 0.144 Uiso 0.500(8) 1 calc PR D 6
C70A C 0.9373(17) 0.4238(18) 0.0347(4) 0.184(8) Uani 0.783(18) 1 d PDU E 7
H70A H 0.8682 0.4590 0.0263 0.221 Uiso 0.783(18) 1 calc PR E 7
H70B H 0.9180 0.3540 0.0465 0.221 Uiso 0.783(18) 1 calc PR E 7
C71A C 1.0205(15) 0.4018(8) 0.0065(4) 0.142(5) Uani 0.783(18) 1 d PDU E 7
H71A H 1.0983 0.3994 0.0146 0.170 Uiso 0.783(18) 1 calc PR E 7
H71B H 1.0032 0.3318 -0.0054 0.170 Uiso 0.783(18) 1 calc PR E 7
C70B C 0.903(3) 0.505(6) 0.0342(13) 0.184(8) Uani 0.217(18) 1 d PDU E 8
H70C H 0.8911 0.5818 0.0258 0.221 Uiso 0.217(18) 1 calc PR E 8
H70D H 0.8345 0.4808 0.0460 0.221 Uiso 0.217(18) 1 calc PR E 8
C71B C 0.930(4) 0.425(3) 0.0055(11) 0.142(5) Uani 0.217(18) 1 d PDU E 8
H71C H 0.9719 0.3582 0.0132 0.170 Uiso 0.217(18) 1 calc PR E 8
H71D H 0.8626 0.4008 -0.0066 0.170 Uiso 0.217(18) 1 calc PR E 8
O70 O 1.0000 0.5000 0.0560(3) 0.143(4) Uani 1 2 d SDU . .
O71 O 1.0000 0.5000 -0.0141(3) 0.251(11) Uani 1 2 d SDU . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.035(3) 0.035(3) 0.050(5) 0.000 0.000 0.000
N1 0.044(2) 0.026(2) 0.061(2) 0.0024(18) -0.007(2) 0.0034(18)
C2 0.045(3) 0.042(3) 0.047(3) 0.000(2) 0.019(2) 0.000(2)
N2 0.048(2) 0.036(2) 0.051(2) 0.0017(19) -0.003(2) 0.0071(19)
C3 0.050(3) 0.034(3) 0.055(3) 0.001(2) -0.009(3) -0.001(2)
N3 0.065(3) 0.036(3) 0.065(3) -0.004(2) -0.015(3) 0.003(2)
C4 0.051(3) 0.028(3) 0.046(3) 0.004(2) 0.002(2) -0.004(2)
N4 0.070(3) 0.052(3) 0.055(2) -0.001(2) -0.007(3) 0.006(2)
C5 0.030(3) 0.048(3) 0.051(3) 0.001(2) 0.003(2) 0.003(2)
N5 0.076(4) 0.039(3) 0.109(5) 0.005(3) -0.017(3) -0.001(3)
C6 0.048(3) 0.042(3) 0.064(3) -0.004(3) -0.006(3) 0.008(2)
N6 0.092(4) 0.030(2) 0.078(3) 0.002(2) -0.030(3) 0.014(3)
C7 0.050(3) 0.034(3) 0.068(3) -0.012(2) -0.009(3) -0.006(2)
C9 0.042(3) 0.043(3) 0.047(3) 0.007(2) 0.000(2) -0.006(2)
C10 0.052(3) 0.033(3) 0.055(3) 0.000(2) -0.013(3) 0.008(2)
C11 0.060(3) 0.026(3) 0.066(3) 0.005(3) -0.005(3) -0.001(2)
C12 0.065(4) 0.047(3) 0.081(4) 0.008(3) -0.034(3) -0.008(3)
C13 0.128(8) 0.102(7) 0.080(5) -0.017(5) -0.029(6) 0.007(6)
C14 0.119(8) 0.107(7) 0.096(6) -0.002(6) -0.003(6) -0.030(7)
C15 0.128(10) 0.128(10) 0.149(11) 0.013(8) -0.044(9) -0.005(8)
C16 0.082(5) 0.041(3) 0.106(5) 0.005(4) -0.032(4) -0.010(3)
C17A 0.084(15) 0.14(2) 0.065(12) 0.000(13) 0.000(10) 0.025(14)
C17 0.134(16) 0.072(10) 0.154(18) 0.035(11) -0.058(14) -0.058(10)
C18 0.198(18) 0.171(15) 0.115(9) -0.035(10) -0.044(12) 0.002(14)
C19 0.49(5) 0.179(19) 0.179(15) -0.009(14) -0.09(2) -0.18(3)
O50A 0.082(6) 0.239(13) 0.145(9) -0.046(9) -0.030(6) -0.053(7)
C50A 0.122(9) 0.188(11) 0.069(6) -0.006(7) 0.002(6) -0.056(6)
C51A 0.107(7) 0.221(12) 0.104(9) -0.029(9) -0.022(7) -0.026(7)
O51A 0.119(7) 0.286(12) 0.107(8) -0.028(8) -0.022(7) -0.004(7)
C52A 0.122(8) 0.252(12) 0.100(7) -0.058(8) -0.024(7) -0.039(8)
C53A 0.090(7) 0.255(12) 0.137(8) -0.065(9) 0.021(7) -0.033(7)
O50B 0.082(6) 0.239(13) 0.145(9) -0.046(9) -0.030(6) -0.053(7)
C50B 0.122(9) 0.188(11) 0.069(6) -0.006(7) 0.002(6) -0.056(6)
C51B 0.107(7) 0.221(12) 0.104(9) -0.029(9) -0.022(7) -0.026(7)
O51B 0.119(7) 0.286(12) 0.107(8) -0.028(8) -0.022(7) -0.004(7)
C52B 0.122(8) 0.252(12) 0.100(7) -0.058(8) -0.024(7) -0.039(8)
C53B 0.090(7) 0.255(12) 0.137(8) -0.065(9) 0.021(7) -0.033(7)
O60A 0.123(8) 0.098(7) 0.099(4) 0.021(4) 0.001(4) -0.032(6)
C60A 0.077(6) 0.072(5) 0.087(5) 0.005(4) 0.013(4) -0.014(5)
C61A 0.127(10) 0.104(7) 0.079(5) 0.018(5) -0.001(7) -0.066(8)
O61A 0.175(10) 0.147(9) 0.133(7) 0.017(6) 0.010(7) -0.106(8)
C62A 0.176(10) 0.115(9) 0.099(7) 0.027(6) -0.032(6) -0.087(8)
C63A 0.160(11) 0.111(6) 0.091(5) 0.039(5) -0.060(7) -0.068(7)
O60B 0.123(8) 0.098(7) 0.099(4) 0.021(4) 0.001(4) -0.032(6)
C60B 0.077(6) 0.072(5) 0.087(5) 0.005(4) 0.013(4) -0.014(5)
C61B 0.127(10) 0.104(7) 0.079(5) 0.018(5) -0.001(7) -0.066(8)
O61B 0.175(10) 0.147(9) 0.133(7) 0.017(6) 0.010(7) -0.106(8)
C62B 0.176(10) 0.115(9) 0.099(7) 0.027(6) -0.032(6) -0.087(8)
C63B 0.160(11) 0.111(6) 0.091(5) 0.039(5) -0.060(7) -0.068(7)
C70A 0.266(15) 0.19(2) 0.100(6) -0.031(8) -0.071(8) -0.083(13)
C71A 0.154(12) 0.060(6) 0.211(10) -0.039(6) -0.094(9) 0.023(7)
C70B 0.266(15) 0.19(2) 0.100(6) -0.031(8) -0.071(8) -0.083(13)
C71B 0.154(12) 0.060(6) 0.211(10) -0.039(6) -0.094(9) 0.023(7)
O70 0.146(10) 0.157(11) 0.124(7) 0.000 0.000 -0.070(8)
O71 0.52(4) 0.097(8) 0.139(10) 0.000 0.000 0.003(13)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
C2 C1 C2 2_575 . 103.0(4) y
C2 C1 C2 2_575 3_465 112.82(19) y
C2 C1 C2 . 3_465 112.82(19) y
C2 C1 C2 2_575 4_665 112.82(19) y
C2 C1 C2 . 4_665 112.8(2) y
C2 C1 C2 3_465 4_665 103.0(4) y
C9 N1 C5 . . 127.4(4) y
C9 N1 H1A . . 116.3 ?
C5 N1 H1A . . 116.3 ?
C7 C2 C3 . . 116.1(5) y
C7 C2 C1 . . 124.5(5) y
C3 C2 C1 . . 119.4(4) y
C10 N2 C9 . . 113.1(5) y
C4 C3 C2 . . 123.1(5) y
C4 C3 H3 . . 118.5 ?
C2 C3 H3 . . 118.5 ?
C9 N3 C11 . . 114.1(5) y
C3 C4 C5 . . 119.3(5) y
C3 C4 H4 . . 120.3 ?
C5 C4 H4 . . 120.3 ?
C11 N4 C10 . . 112.5(5) y
C6 C5 C4 . . 119.0(5) y
C6 C5 N1 . . 124.0(5) y
C4 C5 N1 . . 116.9(5) y
C11 N5 C16 . . 125.3(6) y
C11 N5 H5A . . 117.4 ?
C16 N5 H5A . . 117.4 ?
C5 C6 C7 . . 119.7(5) y
C5 C6 H6 . . 120.2 ?
C7 C6 H6 . . 120.2 ?
C10 N6 C12 . . 124.4(5) y
C10 N6 H6A . . 117.8 ?
C12 N6 H6A . . 117.8 ?
C2 C7 C6 . . 122.7(5) y
C2 C7 H7 . . 118.6 ?
C6 C7 H7 . . 118.6 ?
N3 C9 N1 . . 120.8(5) y
N3 C9 N2 . . 126.0(5) y
N1 C9 N2 . . 113.1(4) y
N2 C10 N6 . . 117.6(5) y
N2 C10 N4 . . 126.9(5) y
N6 C10 N4 . . 115.4(5) y
N4 C11 N3 . . 127.2(5) y
N4 C11 N5 . . 115.5(5) y
N3 C11 N5 . . 117.3(6) y
N6 C12 C13 . . 112.6(7) y
N6 C12 H12A . . 109.1 ?
C13 C12 H12A . . 109.1 ?
N6 C12 H12B . . 109.1 ?
C13 C12 H12B . . 109.1 ?
H12A C12 H12B . . 107.8 ?
C14 C13 C12 . . 116.6(9) y
C14 C13 H13A . . 108.1 ?
C12 C13 H13A . . 108.1 ?
C14 C13 H13B . . 108.1 ?
C12 C13 H13B . . 108.1 ?
H13A C13 H13B . . 107.3 ?
C13 C14 C15 . . 109.8(1) y
C13 C14 H14A . . 109.7 ?
C15 C14 H14A . . 109.7 ?
C13 C14 H14B . . 109.7 ?
C15 C14 H14B . . 109.7 ?
H14A C14 H14B . . 108.2 ?
C14 C15 H15A . . 109.5 ?
C14 C15 H15B . . 109.5 ?
H15A C15 H15B . . 109.5 ?
C14 C15 H15C . . 109.5 ?
H15A C15 H15C . . 109.5 ?
H15B C15 H15C . . 109.5 ?
N5 C16 C17A . . 108.70(12) y
N5 C16 C17 . . 112.1(9) y
C17A C16 C17 . . 57.20(16) y
N5 C16 H16A . . 109.2 ?
C17A C16 H16A . . 56.2 ?
C17 C16 H16A . . 109.2 ?
N5 C16 H16B . . 109.2 ?
C17A C16 H16B . . 142.1 ?
C17 C16 H16B . . 109.2 ?
H16A C16 H16B . . 107.9 ?
C18 C17A C16 . . 117.40(19) y
C18 C17A H17A . . 107.9 ?
C16 C17A H17A . . 107.9 ?
C18 C17A H17B . . 107.9 ?
C16 C17A H17B . . 107.9 ?
H17A C17A H17B . . 107.2 ?
C18 C17 C16 . . 108.70(11) y
C18 C17 H17A . . 110 ?
C16 C17 H17A . . 110 ?
C18 C17 H17B . . 110 ?
C16 C17 H17B . . 110 ?
H17A C17 H17B . . 108.3 ?
C17A C18 C17 . . 60.20(15) y
C17A C18 C19 . . 147.90(12) y
C17 C18 C19 . . 109.7(8) y
C17A C18 H18A . . 102.2 ?
C17 C18 H18A . . 109.7 ?
C19 C18 H18A . . 109.7 ?
C17A C18 H18B . . 55.4 ?
C17 C18 H18B . . 109.7 ?
C19 C18 H18B . . 109.7 ?
H18A C18 H18B . . 108.2 ?
C18 C19 H19A . . 109.5 ?
C18 C19 H19B . . 109.5 ?
H19A C19 H19B . . 109.5 ?
C18 C19 H19C . . 109.5 ?
H19A C19 H19C . . 109.5 ?
H19B C19 H19C . . 109.5 ?
C50A O50A C53A . . 102.7(5) y
O50A C50A C51A . . 110.90(12) y
O50A C50A H50A . . 109.4 ?
C51A C50A H50A . . 109.4 ?
O50A C50A H50B . . 109.5 ?
C51A C50A H50B . . 109.5 ?
H50A C50A H50B . . 108 ?
O51A C51A C50A . . 105.20(13) y
O51A C51A H51A . . 110.7 ?
C50A C51A H51A . . 110.7 ?
O51A C51A H51B . . 110.7 ?
C50A C51A H51B . . 110.7 ?
H51A C51A H51B . . 108.8 ?
C51A O51A C52A . . 102.7(5) y
O51A C52A C53A . . 96.60(12) y
O51A C52A H52A . . 112.4 ?
C53A C52A H52A . . 112.4 ?
O51A C52A H52B . . 112.4 ?
C53A C52A H52B . . 112.4 ?
H52A C52A H52B . . 110 ?
O50A C53A C52A . . 117.10(15) y
O50A C53A H53A . . 108 ?
C52A C53A H53A . . 108 ?
O50A C53A H53B . . 108 ?
C52A C53A H53B . . 108 ?
H53A C53A H53B . . 107.3 ?
C53B O50B C50B . . 102.4(5) y
O50B C50B C51B . . 105.70(19) y
O50B C50B H50A . . 110.6 ?
C51B C50B H50A . . 110.6 ?
O50B C50B H50B . . 110.6 ?
C51B C50B H50B . . 110.6 ?
H50A C50B H50B . . 108.7 ?
O51B C51B C50B . . 103(2) y
O51B C51B H51C . . 111.1 ?
C50B C51B H51C . . 111.1 ?
O51B C51B H51D . . 111.1 ?
C50B C51B H51D . . 111.1 ?
H51C C51B H51D . . 109.1 ?
C52B O51B C51B . . 102.1(5) y
O51B C52B C53B . . 94(2) y
O51B C52B H52C . . 112.9 ?
C53B C52B H52C . . 112.9 ?
O51B C52B H52D . . 112.9 ?
C53B C52B H52D . . 112.9 ?
H52C C52B H52D . . 110.3 ?
O50B C53B C52B . . 117(2) y
O50B C53B H53C . . 108.1 ?
C52B C53B H53C . . 108.1 ?
O50B C53B H53D . . 108.1 ?
C52B C53B H53D . . 108.1 ?
H53C C53B H53D . . 107.3 ?
C63A O60A C60A . . 103.4(5) y
O60A C60A C61A . . 119.1(1) y
O60A C60A H60A . . 107.5 ?
C61A C60A H60A . . 107.5 ?
O60A C60A H60B . . 107.5 ?
C61A C60A H60B . . 107.5 ?
H60A C60A H60B . . 107 ?
O61A C61A C60A . . 112.50(12) y
O61A C61A H61A . . 109.1 ?
C60A C61A H61A . . 109.1 ?
O61A C61A H61B . . 109.1 ?
C60A C61A H61B . . 109.1 ?
H61A C61A H61B . . 107.8 ?
C61A O61A C62A . . 103.2(5) y
O61A C62A C63A . . 123.90(11) y
O61A C62A H62A . . 106.4 ?
C63A C62A H62A . . 106.4 ?
O61A C62A H62B . . 106.3 ?
C63A C62A H62B . . 106.4 ?
H62A C62A H62B . . 106.4 ?
O60A C63A C62A . . 105.30(13) y
O60A C63A H63A . . 110.7 ?
C62A C63A H63A . . 110.7 ?
O60A C63A H63B . . 110.7 ?
C62A C63A H63B . . 110.7 ?
H63A C63A H63B . . 108.8 ?
C63B O60B C60B . . 101.7(5) y
O60B C60B C61B . . 102.50(11) y
O60B C60B H60C . . 111.3 ?
C61B C60B H60C . . 111.3 ?
O60B C60B H60D . . 111.3 ?
C61B C60B H60D . . 111.3 ?
H60C C60B H60D . . 109.2 ?
O61B C61B C60B . . 108.20(13) y
O61B C61B H61C . . 110.1 ?
C60B C61B H61C . . 110.1 ?
O61B C61B H61D . . 110.1 ?
C60B C61B H61D . . 110.1 ?
H61C C61B H61D . . 108.4 ?
C62B O61B C61B . . 102.7(5) y
O61B C62B C63B . . 112.70(15) y
O61B C62B H62C . . 109 ?
C63B C62B H62C . . 109 ?
O61B C62B H62D . . 109.1 ?
C63B C62B H62D . . 109 ?
H62C C62B H62D . . 107.8 ?
O60B C63B C62B . . 98.70(11) y
O60B C63B H63C . . 112 ?
C62B C63B H63C . . 112 ?
O60B C63B H63D . . 112 ?
C62B C63B H63D . . 112 ?
H63C C63B H63D . . 109.7 ?
O70 C70A C71A . . 102.20(11) y
O70 C70A H70A . . 111.3 ?
C71A C70A H70A . . 111.3 ?
O70 C70A H70B . . 111.3 ?
C71A C70A H70B . . 111.3 ?
H70A C70A H70B . . 109.2 ?
O71 C71A C70A . . 100.10(12) y
O71 C71A H71A . . 111.8 ?
C70A C71A H71A . . 111.8 ?
O71 C71A H71B . . 111.8 ?
C70A C71A H71B . . 111.8 ?
H71A C71A H71B . . 109.5 ?
O70 C70B C71B . . 105(3) y
O70 C70B H70C . . 110.8 ?
C71B C70B H70C . . 110.8 ?
O70 C70B H70D . . 110.8 ?
C71B C70B H70D . . 110.8 ?
H70C C70B H70D . . 108.9 ?
O71 C71B C70B . . 98(4) y
O71 C71B H71C . . 112.1 ?
C70B C71B H71C . . 112.1 ?
O71 C71B H71D . . 112.1 ?
C70B C71B H71D . . 112.1 ?
H71C C71B H71D . . 109.8 ?
C70A O70 C70A . 2_765 107.80(17) y
C70A O70 C70B . . 42(3) y
C70A O70 C70B 2_765 . 92(3) y
C70A O70 C70B . 2_765 92(3) y
C70A O70 C70B 2_765 2_765 42(3) y
C70B O70 C70B . 2_765 106(5) y
C71A O71 C71A 2_765 . 110.60(13) y
C71A O71 C71B 2_765 2_765 45(2) y
C71A O71 C71B . 2_765 95.30(18) y
C71A O71 C71B 2_765 . 95.30(18) y
C71A O71 C71B . . 45(2) y
C71B O71 C71B 2_765 . 114(4) y
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
C1 C2 2_575 1.554(6) y
C1 C2 . 1.554(6) y
C1 C2 3_465 1.554(6) y
C1 C2 4_665 1.554(6) y
N1 C9 . 1.361(7) y
N1 C5 . 1.417(7) y
N1 H1a . 0.87 ?
C2 C7 . 1.358(8) y
C2 C3 . 1.395(8) y
N2 C10 . 1.326(7) y
N2 C9 . 1.368(7) y
C3 C4 . 1.370(8) y
C3 H3 . 0.94 ?
N3 C9 . 1.318(8) y
N3 C11 . 1.339(8) y
C4 C5 . 1.390(8) y
C4 H4 . 0.94 ?
N4 C11 . 1.330(8) y
N4 C10 . 1.362(8) y
C5 C6 . 1.375(8) y
N5 C11 . 1.352(8) y
N5 C16 . 1.454(10) y
N5 H5a . 0.87 ?
C6 C7 . 1.397(9) y
C6 H6 . 0.94 ?
N6 C10 . 1.356(8) y
N6 C12 . 1.469(8) y
N6 H6a . 0.87 ?
C7 H7 . 0.94 ?
C12 C13 . 1.485(11) y
C12 H12a . 0.98 ?
C12 H12b . 0.98 ?
C13 C14 . 1.443(15) y
C13 H13a . 0.98 ?
C13 H13b . 0.98 ?
C14 C15 . 1.577(18) y
C14 H14a . 0.98 ?
C14 H14b . 0.98 ?
C15 H15a . 0.97 ?
C15 H15b . 0.97 ?
C15 H15c . 0.97 ?
C16 C17a . 1.46(2) y
C16 C17 . 1.58(2) y
C16 H16a . 0.98 ?
C16 H16b . 0.98 ?
C17a C18 . 1.44(3) y
C17a H17a . 0.98 ?
C17a H17b . 0.98 ?
C17 C18 . 1.47(3) y
C17 H17a . 0.98 ?
C17 H17b . 0.98 ?
C18 C19 . 1.5617 y
C18 H18a . 0.98 ?
C18 H18b . 0.98 ?
C19 H19a . 0.97 ?
C19 H19b . 0.97 ?
C19 H19c . 0.97 ?
O50a C50a . 1.378(5) y
O50a C53a . 1.379(5) y
C50a C51a . 1.497(5) y
C50a H50a . 0.98 ?
C50a H50b . 0.98 ?
C51a O51a . 1.377(5) y
C51a H51a . 0.98 ?
C51a H51b . 0.98 ?
O51a C52a . 1.379(5) y
C52a C53a . 1.501(5) y
C52a H52a . 0.98 ?
C52a H52b . 0.98 ?
C53a H53a . 0.98 ?
C53a H53b . 0.98 ?
O50b C53b . 1.379(5) y
O50b C50b . 1.380(5) y
C50b C51b . 1.502(5) y
C50b H50a . 0.98 ?
C50b H50b . 0.98 ?
C51b O51b . 1.383(5) y
C51b H51c . 0.98 ?
C51b H51d . 0.98 ?
O51b C52b . 1.380(5) y
C52b C53b . 1.501(5) y
C52b H52c . 0.98 ?
C52b H52d . 0.98 ?
C53b H53c . 0.98 ?
C53b H53d . 0.98 ?
O60a C63a . 1.375(5) y
O60a C60a . 1.375(5) y
C60a C61a . 1.491(5) y
C60a H60a . 0.98 ?
C60a H60b . 0.98 ?
C61a O61a . 1.373(5) y
C61a H61a . 0.98 ?
C61a H61b . 0.98 ?
O61a C62a . 1.379(5) y
C62a C63a . 1.498(5) y
C62a H62a . 0.98 ?
C62a H62b . 0.98 ?
C63a H63a . 0.98 ?
C63a H63b . 0.98 ?
O60b C63b . 1.383(5) y
O60b C60b . 1.386(5) y
C60b C61b . 1.499(5) y
C60b H60c . 0.98 ?
C60b H60d . 0.98 ?
C61b O61b . 1.385(5) y
C61b H61c . 0.98 ?
C61b H61d . 0.98 ?
O61b C62b . 1.377(5) y
C62b C63b . 1.502(5) y
C62b H62c . 0.98 ?
C62b H62d . 0.98 ?
C63b H63c . 0.98 ?
C63b H63d . 0.98 ?
C70a O70 . 1.450(4) y
C70a C71a . 1.521(5) y
C70a H70a . 0.98 ?
C70a H70b . 0.98 ?
C71a O71 . 1.449(4) y
C71a H71a . 0.98 ?
C71a H71b . 0.98 ?
C70b O70 . 1.450(4) y
C70b C71b . 1.528(5) y
C70b H70c . 0.98 ?
C70b H70d . 0.98 ?
C71b O71 . 1.452(4) y
C71b H71c . 0.98 ?
C71b H71d . 0.98 ?
O70 C70a 2_765 1.450(4) y
O70 C70b 2_765 1.450(4) y
O71 C71a 2_765 1.449(4) y
O71 C71b 2_765 1.452(4) y
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A N2 0.87 2.27 3.131(6) 170 2_675
N5 H5A N4 0.87 2.19 3.042(8) 164.5 2_665
N6 H6A O50B 0.87 2.11 2.89(2) 148.1 8_645
N6 H6A O50A 0.87 2.2 3.043(13) 161.9 8_645
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_4
_geom_torsion
_geom_torsion_publ_flag
C2 C1 C2 C7 2_575 . 119.0(6) y
C2 C1 C2 C7 3_465 . -2.9(5) y
C2 C1 C2 C7 4_665 . -119.1(6) y
C2 C1 C2 C3 2_575 . -61.9(4) y
C2 C1 C2 C3 3_465 . 176.2(5) y
C2 C1 C2 C3 4_665 . 60.0(3) y
C7 C2 C3 C4 . . -1.5(8) y
C1 C2 C3 C4 . . 179.2(4) y
C2 C3 C4 C5 . . 0.2(8) y
C3 C4 C5 C6 . . -0.3(8) y
C3 C4 C5 N1 . . 177.4(5) y
C9 N1 C5 C6 . . -24.3(8) y
C9 N1 C5 C4 . . 158.1(5) y
C4 C5 C6 C7 . . 1.7(8) y
N1 C5 C6 C7 . . -175.8(5) y
C3 C2 C7 C6 . . 3.0(9) y
C1 C2 C7 C6 . . -177.8(5) y
C5 C6 C7 C2 . . -3.2(9) y
C11 N3 C9 N1 . . -177.7(5) y
C11 N3 C9 N2 . . 2.6(9) y
C5 N1 C9 N3 . . -8.7(9) y
C5 N1 C9 N2 . . 171.0(5) y
C10 N2 C9 N3 . . -3.6(8) y
C10 N2 C9 N1 . . 176.7(5) y
C9 N2 C10 N6 . . -175.0(6) y
C9 N2 C10 N4 . . -0.1(8) y
C12 N6 C10 N2 . . 7.0(1) y
C12 N6 C10 N4 . . -168.6(6) y
C11 N4 C10 N2 . . 4.1(9) y
C11 N4 C10 N6 . . 179.1(6) y
C10 N4 C11 N3 . . -5.4(9) y
C10 N4 C11 N5 . . 173.9(6) y
C9 N3 C11 N4 . . 2.4(9) y
C9 N3 C11 N5 . . -176.9(6) y
C16 N5 C11 N4 . . -177.1(7) y
C16 N5 C11 N3 . . 2.30(11) y
C10 N6 C12 C13 . . 122.7(8) y
N6 C12 C13 C14 . . 179.1(9) y
C12 C13 C14 C15 . . 68.30(13) y
C11 N5 C16 C17A . . 87.90(16) y
C11 N5 C16 C17 . . 149.30(11) y
N5 C16 C17A C18 . . 72(2) y
C17 C16 C17A C18 . . -33.20(19) y
N5 C16 C17 C18 . . -68.60(14) y
C17A C16 C17 C18 . . 30.00(15) y
C16 C17A C18 C17 . . 34.60(18) y
C16 C17A C18 C19 . . 114.10(17) y
C16 C17 C18 C17A . . -29.50(15) y
C16 C17 C18 C19 . . -175.9(7) y
C53A O50A C50A C51A . . -52.40(18) y
O50A C50A C51A O51A . . 65.90(15) y
C50A C51A O51A C52A . . -77.90(16) y
C51A O51A C52A C53A . . 74.30(15) y
C50A O50A C53A C52A . . 60(2) y
O51A C52A C53A O50A . . -71.50(17) y
C53B O50B C50B C51B . . 58(3) y
O50B C50B C51B O51B . . -72(3) y
C50B C51B O51B C52B . . 84(2) y
C51B O51B C52B C53B . . -75(2) y
C50B O50B C53B C52B . . -64(3) y
O51B C52B C53B O50B . . 71(3) y
C63A O60A C60A C61A . . -44(2) y
O60A C60A C61A O61A . . -20(2) y
C60A C61A O61A C62A . . 53(2) y
C61A O61A C62A C63A . . -30(3) y
C60A O60A C63A C62A . . 64.30(18) y
O61A C62A C63A O60A . . -31(3) y
C63B O60B C60B C61B . . 78.80(14) y
O60B C60B C61B O61B . . -71.40(17) y
C60B C61B O61B C62B . . 60.50(19) y
C61B O61B C62B C63B . . -63(2) y
C60B O60B C63B C62B . . -75.20(16) y
O61B C62B C63B O60B . . 71.40(19) y
O70 C70A C71A O71 . . -83.00(14) y
O70 C70B C71B O71 . . -82(5) y
C71A C70A O70 C70A . 2_765 38.6(7) y
C71A C70A O70 C70B . . 111(5) y
C71A C70A O70 C70B . 2_765 -1(2) y
C71B C70B O70 C70A . . -35.10(18) y
C71B C70B O70 C70A . 2_765 80(4) y
C71B C70B O70 C70B . 2_765 39(2) y
C70A C71A O71 C71A . 2_765 37.6(6) y
C70A C71A O71 C71B . 2_765 81(2) y
C70A C71A O71 C71B . . -39(3) y
C70B C71B O71 C71A . 2_765 -6(3) y
C70B C71B O71 C71A . . 108(4) y
C70B C71B O71 C71B . 2_765 36.00(18) y
|
1501600.cif | #------------------------------------------------------------------------------
#$Date: 2019-10-10 08:26:25 +0300 (Thu, 10 Oct 2019) $
#$Revision: 219237 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/50/16/1501600.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_1501600
loop_
_publ_author_name
'Lalibert\'e, Dominic'
'Maris, Thierry'
'Sirois, Ariane'
'Wuest, James D.'
_publ_section_title
;
Molecular Tectonics. Dendritic Construction of Porous Hydrogen-Bonded
Networks
;
_journal_coden_ASTM ORLEF7
_journal_issue 25
_journal_name_full 'Organic Letters'
_journal_page_first 4787
_journal_page_last 4790
_journal_paper_doi 10.1021/ol035712j
_journal_volume 5
_journal_year 2003
_chemical_compound_source 'Synthesized by the authors. See text'
_chemical_formula_moiety 'C64 H64 N30 O7, 4(C2 H6 S O), 16(C4 H8 O2)'
_chemical_formula_sum 'C136 H216 N30 O43 S4'
_chemical_formula_weight 3087.63
_space_group_IT_number 13
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2yc'
_symmetry_space_group_name_H-M 'P 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 90.759(3)
_cell_angle_gamma 90.00
_cell_formula_units_Z 2
_cell_length_a 19.7580(12)
_cell_length_b 10.8646(7)
_cell_length_c 36.649(2)
_cell_measurement_reflns_used 14567
_cell_measurement_temperature 223(2)
_cell_measurement_theta_max 58.31
_cell_measurement_theta_min 2.24
_cell_volume 7866.5(8)
_computing_cell_refinement 'SMART (Bruker, 1999)'
_computing_data_collection 'SMART (Bruker, 1999)'
_computing_data_reduction 'SAINT (Bruker, 1999)'
_computing_molecular_graphics 'XP (Bruker, 1999)'
_computing_publication_material 'UdMX (local program)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 223(2)
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.893
_diffrn_measured_fraction_theta_max 0.893
_diffrn_measurement_device_type 'Bruker AXS Smart 2K/Platform'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'Sealed Tube'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.052
_diffrn_reflns_av_sigmaI/netI 0.0697
_diffrn_reflns_limit_h_max 21
_diffrn_reflns_limit_h_min -22
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_l_max 41
_diffrn_reflns_limit_l_min -40
_diffrn_reflns_number 63526
_diffrn_reflns_theta_full 62.36
_diffrn_reflns_theta_max 62.36
_diffrn_reflns_theta_min 2.24
_diffrn_standards_decay_% 0.26
_diffrn_standards_number 303
_exptl_absorpt_coefficient_mu 1.284
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_correction_T_min 0.6600
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Sadabs (Sheldrick,1996)'
_exptl_crystal_colour Colourless
_exptl_crystal_density_diffrn 1.304
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 3300
_exptl_crystal_size_max 0.22
_exptl_crystal_size_mid 0.12
_exptl_crystal_size_min 0.10
_refine_diff_density_max 0.681
_refine_diff_density_min -0.566
_refine_diff_density_rms 0.054
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.041
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 581
_refine_ls_number_reflns 11176
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.041
_refine_ls_R_factor_all 0.1337
_refine_ls_R_factor_gt 0.0970
_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^)+(0.1150P)^2^+2.5400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2195
_refine_ls_wR_factor_ref 0.2326
_reflns_number_gt 6356
_reflns_number_total 11176
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file deposit.cif
_cod_data_source_block jiw669
_cod_depositor_comments
;
Updated bibliographic information.
Antanas Vaitkus,
2019-10-10
;
_cod_original_sg_symbol_H-M P2/c
_cod_database_code 1501600
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.38552(16) -0.2123(3) 0.23221(7) 0.0369(8) Uani 1 1 d . . .
O1 O 0.36046(12) -0.0531(2) 0.18809(5) 0.0492(6) Uani 1 1 d . . .
O2 O 0.37230(12) -0.16142(18) 0.29573(5) 0.0476(6) Uani 1 1 d . . .
O3 O 0.31675(12) -0.3706(2) 0.20496(6) 0.0529(6) Uani 1 1 d . . .
O4 O 0.5000 -0.2378(3) 0.2500 0.0519(9) Uani 1 2 d S . .
C10 C 0.40378(18) -0.1572(3) 0.19530(8) 0.0416(8) Uani 1 1 d . . .
H10A H 0.4512 -0.1310 0.1956 0.050 Uiso 1 1 calc R . .
H10B H 0.3978 -0.2191 0.1761 0.050 Uiso 1 1 calc R . .
N10 N 0.41220(16) 0.1848(2) 0.03121(6) 0.0498(8) Uani 1 1 d . . .
C11 C 0.37229(18) 0.0130(3) 0.15699(8) 0.0434(9) Uani 1 1 d . . .
N11 N 0.38928(17) 0.3603(2) 0.06777(7) 0.0564(9) Uani 1 1 d . . .
C12 C 0.41627(18) -0.0228(3) 0.12982(8) 0.0433(9) Uani 1 1 d . . .
H12 H 0.4413 -0.0961 0.1321 0.052 Uiso 1 1 calc . . .
N12 N 0.41689(17) 0.3859(2) 0.00512(7) 0.0582(9) Uani 1 1 d . . .
C13 C 0.42296(18) 0.0509(3) 0.09914(8) 0.0439(9) Uani 1 1 d . . .
H13 H 0.4519 0.0251 0.0805 0.053 Uiso 1 1 calc . . .
N13 N 0.3968(2) 0.5513(3) 0.04188(8) 0.0822(12) Uani 1 1 d . . .
H13A H 0.4043 0.5991 0.0233 0.099 Uiso 1 1 calc . . .
H13B H 0.3866 0.5829 0.0629 0.099 Uiso 1 1 calc . . .
C14 C 0.38850(18) 0.1610(3) 0.09502(8) 0.0429(9) Uani 1 1 d . . .
N14 N 0.43175(18) 0.2126(2) -0.02987(7) 0.0614(9) Uani 1 1 d . . .
H14A H 0.4370 0.2594 -0.0489 0.074 Uiso 1 1 calc . . .
H14B H 0.4341 0.1330 -0.0321 0.074 Uiso 1 1 calc . . .
C15 C 0.3448(2) 0.1961(3) 0.12336(9) 0.0558(10) Uani 1 1 d . . .
H15 H 0.3206 0.2705 0.1215 0.067 Uiso 1 1 calc . . .
C16 C 0.3371(2) 0.1231(3) 0.15354(9) 0.0602(11) Uani 1 1 d . . .
H16 H 0.3077 0.1479 0.1721 0.072 Uiso 1 1 calc . . .
C17 C 0.39701(19) 0.2400(3) 0.06267(8) 0.0479(9) Uani 1 1 d . . .
C18 C 0.4201(2) 0.2634(3) 0.00300(8) 0.0505(10) Uani 1 1 d . . .
C19 C 0.4010(2) 0.4298(3) 0.03811(9) 0.0571(11) Uani 1 1 d . . .
C20 C 0.38507(18) -0.1080(3) 0.26038(7) 0.0419(8) Uani 1 1 d . . .
H20A H 0.4288 -0.0654 0.2607 0.050 Uiso 1 1 calc R . .
H20B H 0.3497 -0.0481 0.2541 0.050 Uiso 1 1 calc R . .
N20 N 0.41727(16) 0.2440(2) 0.41783(6) 0.0484(8) Uani 1 1 d . . .
C21 C 0.38151(17) -0.0882(3) 0.32544(8) 0.0405(8) Uani 1 1 d . . .
N21 N 0.40385(15) 0.0661(2) 0.45512(6) 0.0463(7) Uani 1 1 d . . .
C22 C 0.36059(19) -0.1336(3) 0.35829(8) 0.0488(9) Uani 1 1 d . . .
H22 H 0.3404 -0.2119 0.3592 0.059 Uiso 1 1 calc . . .
N22 N 0.41432(16) 0.2655(2) 0.48254(7) 0.0522(8) Uani 1 1 d . . .
C23 C 0.36850(19) -0.0672(3) 0.38984(8) 0.0472(9) Uani 1 1 d . . .
H23 H 0.3531 -0.1001 0.4120 0.057 Uiso 1 1 calc . . .
N23 N 0.40110(19) 0.0912(3) 0.51706(7) 0.0699(10) Uani 1 1 d . . .
H23A H 0.3955 0.0121 0.5191 0.084 Uiso 1 1 calc . . .
H23B H 0.4029 0.1372 0.5365 0.084 Uiso 1 1 calc . . .
C24 C 0.39906(18) 0.0489(3) 0.38963(8) 0.0415(9) Uani 1 1 d . . .
N24 N 0.43352(19) 0.4314(3) 0.44577(7) 0.0642(10) Uani 1 1 d . . .
H24A H 0.4360 0.4771 0.4652 0.077 Uiso 1 1 calc . . .
H24B H 0.4386 0.4643 0.4243 0.077 Uiso 1 1 calc . . .
C25 C 0.42004(19) 0.0944(3) 0.35618(8) 0.0465(9) Uani 1 1 d . . .
H25 H 0.4403 0.1726 0.3551 0.056 Uiso 1 1 calc . . .
C26 C 0.41166(19) 0.0270(3) 0.32435(8) 0.0499(9) Uani 1 1 d . . .
H26 H 0.4264 0.0593 0.3020 0.060 Uiso 1 1 calc . . .
C27 C 0.40742(18) 0.1247(3) 0.42291(8) 0.0436(9) Uani 1 1 d . . .
C28 C 0.4071(2) 0.1425(3) 0.48388(8) 0.0512(10) Uani 1 1 d . . .
C29 C 0.4218(2) 0.3107(3) 0.44879(8) 0.0512(10) Uani 1 1 d . . .
C30 C 0.31630(18) -0.2730(3) 0.23124(8) 0.0472(9) Uani 1 1 d . . .
H30A H 0.3057 -0.3059 0.2554 0.057 Uiso 1 1 calc R . .
H30B H 0.2816 -0.2123 0.2246 0.057 Uiso 1 1 calc R . .
N30 N 0.0287(2) -0.6230(4) 0.20124(13) 0.0973(13) Uani 1 1 d . . .
C31 C 0.2558(2) -0.4269(3) 0.19880(9) 0.0562(10) Uani 1 1 d . . .
N31 N -0.0483(3) -0.7219(5) 0.1597(2) 0.140(2) Uani 1 1 d . . .
C32 C 0.1981(2) -0.4045(4) 0.21772(11) 0.0693(12) Uani 1 1 d . . .
H32 H 0.1987 -0.3458 0.2366 0.083 Uiso 1 1 calc . . .
N32 N 0.0613(2) -0.6565(5) 0.13991(14) 0.1206(16) Uani 1 1 d . . .
C33 C 0.1390(2) -0.4664(4) 0.20966(13) 0.0802(13) Uani 1 1 d . . .
H33 H 0.0999 -0.4507 0.2233 0.096 Uiso 1 1 calc . . .
N33 N -0.0745(3) -0.6920(6) 0.22012(17) 0.143(2) Uani 1 1 d . . .
H33A H -0.0644 -0.6656 0.2419 0.171 Uiso 1 1 calc . . .
H33B H -0.1133 -0.7273 0.2159 0.171 Uiso 1 1 calc . . .
C34 C 0.1366(2) -0.5514(4) 0.18166(13) 0.0787(13) Uani 1 1 d . . .
N34 N -0.0133(4) -0.7558(7) 0.10139(19) 0.212(4) Uani 1 1 d . . .
H34A H -0.0521 -0.7908 0.0968 0.254 Uiso 1 1 calc . . .
H34B H 0.0168 -0.7502 0.0844 0.254 Uiso 1 1 calc . . .
C35 C 0.1944(3) -0.5746(5) 0.16303(12) 0.0865(15) Uani 1 1 d . . .
H35 H 0.1933 -0.6331 0.1441 0.104 Uiso 1 1 calc . . .
C36 C 0.2546(2) -0.5151(4) 0.17088(11) 0.0797(13) Uani 1 1 d . . .
H36 H 0.2940 -0.5333 0.1578 0.096 Uiso 1 1 calc . . .
C37 C 0.0708(3) -0.6142(5) 0.17464(17) 0.0927(15) Uani 1 1 d . . .
C38 C -0.0311(3) -0.6785(6) 0.1935(2) 0.115(2) Uani 1 1 d . . .
C39 C 0.0000(4) -0.7105(7) 0.1347(2) 0.138(2) Uani 1 1 d . . .
C40 C 0.44092(17) -0.3056(3) 0.24255(8) 0.0426(9) Uani 1 1 d . . .
H40A H 0.4277 -0.3528 0.2641 0.051 Uiso 1 1 calc R . .
H40B H 0.4484 -0.3630 0.2224 0.051 Uiso 1 1 calc R . .
O50 O -0.2077(2) -0.8119(5) 0.2120(2) 0.174(2) Uani 1 1 d . A 2
C51 C -0.2569(4) -0.7554(14) 0.2375(2) 0.222(6) Uani 1 1 d . A 2
H51A H -0.2362 -0.7475 0.2618 0.266 Uiso 1 1 calc R A 2
H51B H -0.2969 -0.8083 0.2395 0.266 Uiso 1 1 calc R A 2
C52 C -0.2779(5) -0.6292(11) 0.2235(3) 0.204(5) Uani 1 1 d . A 2
H52A H -0.3098 -0.5893 0.2399 0.245 Uiso 1 1 calc R A 2
H52B H -0.2386 -0.5756 0.2202 0.245 Uiso 1 1 calc R A 2
O53 O -0.3077(4) -0.6578(7) 0.1912(2) 0.205(3) Uani 1 1 d . A 2
C54 C -0.2376(5) -0.8198(10) 0.1787(3) 0.190(4) Uani 1 1 d . A 2
H54A H -0.2750 -0.8789 0.1796 0.228 Uiso 1 1 calc R A 2
H54B H -0.2048 -0.8502 0.1610 0.228 Uiso 1 1 calc R A 2
C55 C -0.2632(6) -0.7019(11) 0.1668(3) 0.211(5) Uani 1 1 d . A 2
H55A H -0.2255 -0.6439 0.1643 0.253 Uiso 1 1 calc R A 2
H55B H -0.2855 -0.7105 0.1429 0.253 Uiso 1 1 calc R A 2
S90 S 0.47636(13) -0.36988(19) 0.36146(6) 0.0699(9) Uiso 0.548(4) 1 d P B 6
O90 O 0.4582(3) -0.3584(5) 0.39994(16) 0.0829(17) Uiso 0.548(4) 1 d P B 6
C91 C 0.5468(2) -0.4561(4) 0.36012(13) 0.0255(14) Uiso 0.548(4) 1 d P B 6
H91A H 0.5852 -0.4077 0.3686 0.038 Uiso 1 1 calc R B 6
H91B H 0.5544 -0.4829 0.3353 0.038 Uiso 1 1 calc R B 6
H91C H 0.5416 -0.5274 0.3758 0.038 Uiso 1 1 calc R B 6
C92 C 0.4126(3) -0.4646(5) 0.34591(15) 0.0374(16) Uiso 0.548(4) 1 d P B 6
H92A H 0.3700 -0.4202 0.3460 0.056 Uiso 1 1 calc R B 6
H92B H 0.4094 -0.5360 0.3617 0.056 Uiso 1 1 calc R B 6
H92C H 0.4223 -0.4911 0.3213 0.056 Uiso 1 1 calc R B 6
S93 S 0.4310(3) -0.4017(5) 0.38299(15) 0.161(2) Uiso 0.452(4) 1 d P B 7
O94 O 0.5153(3) -0.5026(5) 0.32678(16) 0.072(2) Uiso 0.452(4) 1 d P B 7
C95 C 0.4501(5) -0.5448(8) 0.3357(2) 0.066(3) Uiso 0.452(4) 1 d P B 7
C96 C 0.5101(6) -0.3514(8) 0.3729(3) 0.061(2) Uiso 0.452(4) 1 d P B 7
S100 S 0.2757(3) 0.7360(7) 0.09500(15) 0.168(2) Uiso 0.606(11) 1 d P C 8
O100 O 0.3568(3) 0.7516(5) 0.08611(16) 0.0717(19) Uiso 0.606(11) 1 d P C 8
C101 C 0.2539(6) 0.8888(10) 0.0786(3) 0.138(4) Uiso 0.606(11) 1 d P C 8
H10C H 0.2617 0.9482 0.0980 0.207 Uiso 1 1 calc R C 8
H10D H 0.2066 0.8905 0.0712 0.207 Uiso 1 1 calc R C 8
H10E H 0.2819 0.9092 0.0580 0.207 Uiso 1 1 calc R C 8
C102 C 0.2477(8) 0.7192(14) 0.0488(4) 0.205(7) Uiso 0.606(11) 1 d P C 8
H10F H 0.2507 0.6334 0.0417 0.307 Uiso 1 1 calc R C 8
H10G H 0.2761 0.7685 0.0331 0.307 Uiso 1 1 calc R C 8
H10H H 0.2012 0.7467 0.0465 0.307 Uiso 1 1 calc R C 8
S103 S 0.2890(3) 0.8053(7) 0.08479(19) 0.150(4) Uiso 0.394(11) 1 d P C 9
O104 O 0.3429(5) 0.7144(9) 0.0995(3) 0.088(3) Uiso 0.394(11) 1 d P C 9
C105 C 0.2407(9) 0.6250(17) 0.0771(5) 0.144(7) Uiso 0.394(11) 1 d P C 9
C106 C 0.2819(6) 0.7656(11) 0.1096(3) 0.057(3) Uiso 0.394(11) 1 d P C 9
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 0.051(2) 0.0385(19) 0.0216(15) 0.0010(13) 0.0065(14) -0.0073(16)
O1 0.0690(17) 0.0522(14) 0.0266(11) 0.0123(10) 0.0074(11) 0.0103(12)
O2 0.0825(18) 0.0398(13) 0.0205(11) -0.0005(9) 0.0060(11) -0.0072(12)
O3 0.0555(17) 0.0606(15) 0.0428(13) -0.0206(12) 0.0107(11) -0.0162(13)
O4 0.065(2) 0.0320(18) 0.059(2) 0.000 -0.0119(18) 0.000
C10 0.063(2) 0.0365(19) 0.0256(16) 0.0055(14) 0.0024(15) 0.0027(17)
N10 0.092(2) 0.0315(15) 0.0255(14) 0.0003(12) 0.0015(14) 0.0046(15)
C11 0.068(3) 0.042(2) 0.0201(16) 0.0070(14) -0.0002(16) -0.0019(18)
N11 0.109(3) 0.0323(18) 0.0285(15) 0.0017(12) 0.0066(15) 0.0033(16)
C12 0.064(2) 0.037(2) 0.0291(17) 0.0034(14) -0.0009(17) 0.0053(17)
N12 0.115(3) 0.0301(18) 0.0296(15) 0.0057(12) 0.0063(16) 0.0034(16)
C13 0.064(2) 0.046(2) 0.0227(16) 0.0004(14) 0.0074(15) -0.0033(18)
N13 0.176(4) 0.0299(19) 0.0408(17) 0.0045(13) 0.018(2) 0.008(2)
C14 0.070(3) 0.0311(19) 0.0275(17) 0.0010(14) 0.0079(16) -0.0038(17)
N14 0.115(3) 0.0394(17) 0.0301(15) 0.0018(13) 0.0112(16) -0.0038(17)
C15 0.094(3) 0.040(2) 0.0341(19) 0.0052(16) 0.0049(19) 0.0204(19)
C16 0.091(3) 0.059(3) 0.0311(18) 0.0029(17) 0.0153(18) 0.017(2)
C17 0.078(3) 0.036(2) 0.0295(18) -0.0008(15) -0.0006(17) 0.0030(18)
C18 0.090(3) 0.036(2) 0.0251(18) 0.0023(15) 0.0001(17) -0.0021(18)
C19 0.100(3) 0.039(2) 0.032(2) 0.0041(16) 0.0015(19) 0.005(2)
C20 0.066(2) 0.0392(19) 0.0204(15) 0.0033(13) 0.0040(15) 0.0016(17)
N20 0.090(2) 0.0291(17) 0.0268(14) -0.0018(12) 0.0104(14) 0.0021(15)
C21 0.059(2) 0.035(2) 0.0272(17) -0.0046(14) -0.0028(15) 0.0037(17)
N21 0.083(2) 0.0335(15) 0.0221(14) -0.0037(12) 0.0060(13) -0.0001(14)
C22 0.082(3) 0.0343(19) 0.0304(18) 0.0039(15) 0.0018(17) -0.0081(18)
N22 0.101(3) 0.0273(17) 0.0287(15) -0.0032(12) 0.0077(15) -0.0021(15)
C23 0.075(3) 0.044(2) 0.0226(16) 0.0014(15) 0.0054(16) -0.0026(19)
N23 0.146(3) 0.0393(17) 0.0244(15) -0.0001(13) 0.0061(17) -0.0107(18)
C24 0.067(2) 0.033(2) 0.0252(16) -0.0010(14) 0.0026(16) 0.0044(17)
N24 0.134(3) 0.0293(18) 0.0300(15) 0.0005(12) 0.0112(16) -0.0046(17)
C25 0.074(3) 0.0336(19) 0.0324(18) 0.0001(15) 0.0094(17) -0.0049(17)
C26 0.079(3) 0.048(2) 0.0228(16) -0.0044(15) 0.0082(16) -0.0011(19)
C27 0.062(2) 0.037(2) 0.0324(18) 0.0000(15) 0.0066(16) 0.0067(17)
C28 0.091(3) 0.040(2) 0.0231(17) 0.0008(15) 0.0023(17) -0.0025(19)
C29 0.084(3) 0.043(2) 0.0267(18) 0.0006(16) 0.0052(17) 0.0022(19)
C30 0.059(3) 0.053(2) 0.0301(17) -0.0017(16) 0.0101(16) -0.0071(18)
N30 0.047(3) 0.106(3) 0.139(4) -0.006(3) 0.011(3) -0.018(2)
C31 0.057(3) 0.063(2) 0.049(2) -0.0020(19) 0.0071(19) -0.014(2)
N31 0.071(4) 0.160(5) 0.187(6) -0.026(4) -0.021(4) -0.040(3)
C32 0.063(3) 0.068(3) 0.077(3) -0.020(2) 0.015(2) -0.012(2)
N32 0.094(4) 0.144(4) 0.123(4) -0.016(3) -0.016(3) -0.047(3)
C33 0.056(3) 0.089(3) 0.096(3) -0.023(3) 0.014(2) -0.007(3)
N33 0.057(3) 0.193(5) 0.179(5) -0.023(4) 0.009(3) -0.036(3)
C34 0.064(3) 0.081(3) 0.091(3) -0.011(3) -0.008(3) -0.017(3)
N34 0.174(6) 0.294(9) 0.167(6) -0.069(6) -0.051(5) -0.106(6)
C35 0.074(3) 0.108(4) 0.078(3) -0.039(3) 0.017(3) -0.036(3)
C36 0.072(3) 0.099(3) 0.069(3) -0.036(3) 0.013(2) -0.030(3)
C37 0.061(4) 0.097(4) 0.120(4) -0.019(3) -0.002(3) -0.023(3)
C38 0.056(4) 0.119(5) 0.170(7) -0.017(4) -0.001(4) -0.018(3)
C39 0.080(5) 0.174(6) 0.162(7) -0.033(5) -0.011(5) -0.042(5)
C40 0.068(3) 0.0293(18) 0.0303(17) 0.0034(14) 0.0010(16) -0.0091(17)
O50 0.089(4) 0.182(5) 0.250(7) 0.039(5) -0.008(4) -0.026(3)
C51 0.086(6) 0.434(19) 0.146(7) 0.041(10) 0.032(5) 0.022(9)
C52 0.147(8) 0.251(12) 0.215(11) -0.126(9) -0.027(7) -0.043(8)
O53 0.207(7) 0.196(6) 0.213(7) -0.015(5) 0.001(6) 0.066(5)
C54 0.116(7) 0.225(11) 0.230(10) -0.103(9) -0.030(7) -0.010(6)
C55 0.246(13) 0.232(11) 0.156(8) 0.023(8) 0.033(8) 0.096(10)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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_3
_geom_angle
_geom_angle_publ_flag
C30 C1 C10 . 111.9(2) y
C30 C1 C20 . 108.9(3) y
C10 C1 C20 . 108.1(2) y
C30 C1 C40 . 111.0(3) y
C10 C1 C40 . 107.5(3) y
C20 C1 C40 . 109.4(2) y
C11 O1 C10 . 117.2(2) y
C21 O2 C20 . 117.4(2) y
C31 O3 C30 . 115.4(3) y
C40 O4 C40 2_655 116.7(3) y
O1 C10 C1 . 108.9(3) y
O1 C10 H10A . 109.9 ?
C1 C10 H10A . 109.9 ?
O1 C10 H10B . 109.9 ?
C1 C10 H10B . 109.9 ?
H10A C10 H10B . 108.3 ?
C17 N10 C18 . 113.9(3) y
O1 C11 C12 . 124.5(3) y
O1 C11 C16 . 115.9(3) y
C12 C11 C16 . 119.6(3) y
C17 N11 C19 . 114.6(3) y
C11 C12 C13 . 119.2(3) y
C11 C12 H12 . 120.4 ?
C13 C12 H12 . 120.4 ?
C18 N12 C19 . 114.8(3) y
C14 C13 C12 . 122.4(3) y
C14 C13 H13 . 118.8 ?
C12 C13 H13 . 118.8 ?
C19 N13 H13A . 120 ?
C19 N13 H13B . 120 ?
H13A N13 H13B . 120 ?
C13 C14 C15 . 117.3(3) y
C13 C14 C17 . 122.0(3) y
C15 C14 C17 . 120.7(3) y
C18 N14 H14A . 120 ?
C18 N14 H14B . 120 ?
H14A N14 H14B . 120 ?
C16 C15 C14 . 120.8(3) y
C16 C15 H15 . 119.6 ?
C14 C15 H15 . 119.6 ?
C15 C16 C11 . 120.8(3) y
C15 C16 H16 . 119.6 ?
C11 C16 H16 . 119.6 ?
N11 C17 N10 . 126.2(3) y
N11 C17 C14 . 116.4(3) y
N10 C17 C14 . 117.4(3) y
N12 C18 N14 . 118.0(3) y
N12 C18 N10 . 125.5(3) y
N14 C18 N10 . 116.6(3) y
N13 C19 N12 . 117.6(3) y
N13 C19 N11 . 117.5(3) y
N12 C19 N11 . 125.0(3) y
O2 C20 C1 . 108.0(2) y
O2 C20 H20A . 110.1 ?
C1 C20 H20A . 110.1 ?
O2 C20 H20B . 110.1 ?
C1 C20 H20B . 110.1 ?
H20A C20 H20B . 108.4 ?
C27 N20 C29 . 114.6(3) y
O2 C21 C22 . 117.0(3) y
O2 C21 C26 . 123.9(3) y
C22 C21 C26 . 119.0(3) y
C28 N21 C27 . 113.2(3) y
C21 C22 C23 . 121.3(3) y
C21 C22 H22 . 119.4 ?
C23 C22 H22 . 119.4 ?
C29 N22 C28 . 114.3(3) y
C22 C23 C24 . 121.0(3) y
C22 C23 H23 . 119.5 ?
C24 C23 H23 . 119.5 ?
C28 N23 H23A . 120 ?
C28 N23 H23B . 120 ?
H23A N23 H23B . 120 ?
C25 C24 C23 . 117.4(3) y
C25 C24 C27 . 119.9(3) y
C23 C24 C27 . 122.7(3) y
C29 N24 H24A . 120 ?
C29 N24 H24B . 120 ?
H24A N24 H24B . 120 ?
C26 C25 C24 . 121.4(3) y
C26 C25 H25 . 119.3 ?
C24 C25 H25 . 119.3 ?
C25 C26 C21 . 120.0(3) y
C25 C26 H26 . 120 ?
C21 C26 H26 . 120 ?
N20 C27 N21 . 126.6(3) y
N20 C27 C24 . 116.4(3) y
N21 C27 C24 . 117.0(3) y
N21 C28 N23 . 116.8(3) y
N21 C28 N22 . 126.1(3) y
N23 C28 N22 . 117.1(3) y
N24 C29 N22 . 117.2(3) y
N24 C29 N20 . 117.9(3) y
N22 C29 N20 . 124.9(3) y
O3 C30 C1 . 108.9(3) y
O3 C30 H30A . 109.9 ?
C1 C30 H30A . 109.9 ?
O3 C30 H30B . 109.9 ?
C1 C30 H30B . 109.9 ?
H30A C30 H30B . 108.3 ?
C37 N30 C38 . 116.3(5) y
C32 C31 O3 . 125.2(3) y
C32 C31 C36 . 119.1(4) y
O3 C31 C36 . 115.7(3) y
C39 N31 C38 . 114.7(5) y
C31 C32 C33 . 121.1(4) y
C31 C32 H32 . 119.5 ?
C33 C32 H32 . 119.5 ?
C39 N32 C37 . 112.9(6) y
C32 C33 C34 . 120.4(4) y
C32 C33 H33 . 119.8 ?
C34 C33 H33 . 119.8 ?
C38 N33 H33A . 120 ?
C38 N33 H33B . 120 ?
H33A N33 H33B . 120 ?
C35 C34 C33 . 118.4(4) y
C35 C34 C37 . 124.5(5) y
C33 C34 C37 . 117.1(5) y
C39 N34 H34A . 120 ?
C39 N34 H34B . 120 ?
H34A N34 H34B . 120 ?
C34 C35 C36 . 122.3(4) y
C34 C35 H35 . 118.8 ?
C36 C35 H35 . 118.8 ?
C35 C36 C31 . 118.6(4) y
C35 C36 H36 . 120.7 ?
C31 C36 H36 . 120.7 ?
N30 C37 N32 . 126.6(4) y
N30 C37 C34 . 118.2(5) y
N32 C37 C34 . 115.1(5) y
N33 C38 N30 . 118.1(7) y
N33 C38 N31 . 118.6(6) y
N30 C38 N31 . 123.4(7) y
N31 C39 N34 . 117.1(7) y
N31 C39 N32 . 126.0(7) y
N34 C39 N32 . 116.9(8) y
O4 C40 C1 . 106.9(2) y
O4 C40 H40A . 110.4 ?
C1 C40 H40A . 110.4 ?
O4 C40 H40B . 110.4 ?
C1 C40 H40B . 110.4 ?
H40A C40 H40B . 108.6 ?
C54 O50 C51 . 108.1(6) y
O50 C51 C52 . 109.6(8) y
O50 C51 H51A . 109.7 ?
C52 C51 H51A . 109.7 ?
O50 C51 H51B . 109.7 ?
C52 C51 H51B . 109.7 ?
H51A C51 H51B . 108.2 ?
O53 C52 C51 . 101.7(8) y
O53 C52 H52A . 111.4 ?
C51 C52 H52A . 111.4 ?
O53 C52 H52B . 111.4 ?
C51 C52 H52B . 111.4 ?
H52A C52 H52B . 109.3 ?
C52 O53 C55 . 112.4(9) y
O50 C54 C55 . 111.3(8) y
O50 C54 H54A . 109.4 ?
C55 C54 H54A . 109.4 ?
O50 C54 H54B . 109.4 ?
C55 C54 H54B . 109.4 ?
H54A C54 H54B . 108 ?
O53 C55 C54 . 110.1(9) y
O53 C55 H55A . 109.6 ?
C54 C55 H55A . 109.6 ?
O53 C55 H55B . 109.6 ?
C54 C55 H55B . 109.6 ?
H55A C55 H55B . 108.2 ?
O90 S90 C91 . 106.8(3) y
O90 S90 C92 . 100.5(3) y
C91 S90 C92 . 105.2(3) y
S90 C91 H91A . 109.5 ?
S90 C91 H91B . 109.5 ?
H91A C91 H91B . 109.5 ?
S90 C91 H91C . 109.5 ?
H91A C91 H91C . 109.5 ?
H91B C91 H91C . 109.5 ?
S90 C92 H92A . 109.5 ?
S90 C92 H92B . 109.5 ?
H92A C92 H92B . 109.5 ?
S90 C92 H92C . 109.5 ?
H92A C92 H92C . 109.5 ?
H92B C92 H92C . 109.5 ?
O100 S100 C102 . 96.4(6) y
O100 S100 C101 . 93.8(6) y
C102 S100 C101 . 73.2(6) y
S100 C101 H10C . 109.5 ?
S100 C101 H10D . 109.5 ?
H10C C101 H10D . 109.5 ?
S100 C101 H10E . 109.5 ?
H10C C101 H10E . 109.5 ?
H10D C101 H10E . 109.5 ?
S100 C102 H10F . 109.5 ?
S100 C102 H10G . 109.5 ?
H10F C102 H10G . 109.5 ?
S100 C102 H10H . 109.5 ?
H10F C102 H10H . 109.5 ?
H10G C102 H10H . 109.5 ?
C106 S103 O104 . 61.3(8) y
C106 S103 C105 . 70.8(1) y
O104 S103 C105 . 76.7(7) y
C106 O104 S103 . 40.3(6) y
S103 C106 O104 . 78.4(9) y
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
C1 C30 . 1.518(5) y
C1 C10 . 1.527(4) y
C1 C20 . 1.533(4) y
C1 C40 . 1.536(4) y
O1 C11 . 1.370(3) y
O1 C10 . 1.440(4) y
O2 C21 . 1.359(3) y
O2 C20 . 1.445(3) y
O3 C31 . 1.366(4) y
O3 C30 . 1.432(4) y
O4 C40 . 1.404(3) y
O4 C40 2_655 1.404(3) y
C10 H10a . 0.98 ?
C10 H10b . 0.98 ?
N10 C17 . 1.337(4) y
N10 C18 . 1.352(4) y
C11 C12 . 1.386(5) y
C11 C16 . 1.388(5) y
N11 C17 . 1.329(4) y
N11 C19 . 1.346(4) y
C12 C13 . 1.388(4) y
C12 H12 . 0.94 ?
N12 C18 . 1.334(4) y
N12 C19 . 1.341(4) y
C13 C14 . 1.383(4) y
C13 H13 . 0.94 ?
N13 C19 . 1.330(4) y
N13 H13a . 0.87 ?
N13 H13b . 0.87 ?
C14 C15 . 1.412(5) y
C14 C17 . 1.475(4) y
N14 C18 . 1.348(4) y
N14 H14a . 0.87 ?
N14 H14b . 0.87 ?
C15 C16 . 1.371(5) y
C15 H15 . 0.94 ?
C16 H16 . 0.94 ?
C20 H20a . 0.98 ?
C20 H20b . 0.98 ?
N20 C27 . 1.325(4) y
N20 C29 . 1.349(4) y
C21 C22 . 1.370(4) y
C21 C26 . 1.387(5) y
N21 C28 . 1.343(4) y
N21 C27 . 1.344(4) y
C22 C23 . 1.371(4) y
C22 H22 . 0.94 ?
N22 C29 . 1.341(4) y
N22 C28 . 1.345(4) y
C23 C24 . 1.398(4) y
C23 H23 . 0.94 ?
N23 C28 . 1.344(4) y
N23 H23a . 0.87 ?
N23 H23b . 0.87 ?
C24 C25 . 1.390(4) y
C24 C27 . 1.479(4) y
N24 C29 . 1.337(4) y
N24 H24a . 0.87 ?
N24 H24b . 0.87 ?
C25 C26 . 1.386(4) y
C25 H25 . 0.94 ?
C26 H26 . 0.94 ?
C30 H30a . 0.98 ?
C30 H30b . 0.98 ?
N30 C37 . 1.293(6) y
N30 C38 . 1.353(7) y
C31 C32 . 1.365(5) y
C31 C36 . 1.401(5) y
N31 C39 . 1.337(8) y
N31 C38 . 1.366(8) y
C32 C33 . 1.376(6) y
C32 H32 . 0.94 ?
N32 C39 . 1.356(8) y
N32 C37 . 1.364(7) y
C33 C34 . 1.381(6) y
C33 H33 . 0.94 ?
N33 C38 . 1.315(8) y
N33 H33a . 0.87 ?
N33 H33b . 0.87 ?
C34 C35 . 1.362(6) y
C34 C37 . 1.488(6) y
N34 C39 . 1.339(9) y
N34 H34a . 0.87 ?
N34 H34b . 0.87 ?
C35 C36 . 1.381(6) y
C35 H35 . 0.94 ?
C36 H36 . 0.94 ?
C40 H40a . 0.98 ?
C40 H40b . 0.98 ?
O50 C54 . 1.350(9) y
O50 C51 . 1.491(10) y
C51 C52 . 1.520(13) y
C51 H51a . 0.98 ?
C51 H51b . 0.98 ?
C52 O53 . 1.349(9) y
C52 H52a . 0.98 ?
C52 H52b . 0.98 ?
O53 C55 . 1.35(1) y
C54 C55 . 1.442(12) y
C54 H54a . 0.98 ?
C54 H54b . 0.98 ?
C55 H55a . 0.98 ?
C55 H55b . 0.98 ?
S90 O90 . 1.465(7) y
S90 C91 . 1.679(5) y
S90 C92 . 1.719(6) y
C91 H91a . 0.97 ?
C91 H91b . 0.97 ?
C91 H91c . 0.97 ?
C92 H92a . 0.97 ?
C92 H92b . 0.97 ?
C92 H92c . 0.97 ?
S93 C96 . 1.700(13) y
O94 C95 . 1.409(11) y
S100 O100 . 1.649(9) y
S100 C102 . 1.784(15) y
S100 C101 . 1.815(14) y
C101 H10c . 0.97 ?
C101 H10d . 0.97 ?
C101 H10e . 0.97 ?
C102 H10f . 0.97 ?
C102 H10g . 0.97 ?
C102 H10h . 0.97 ?
S103 C106 . 1.019(13) y
S103 O104 . 1.544(12) y
S103 C105 . 2.20(2) y
O104 C106 . 1.382(14) y
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N13 H13A N22 0.87 2.11 2.972(4) 171.6 4_565
N13 H13B O104 0.87 2.15 2.965(10) 156.3 .
N14 H14A O90 0.87 2.21 3.072(7) 172.5 4
N14 H14B N21 0.87 2.29 3.125(4) 160.7 4
N23 H23A N10 0.87 2.21 3.051(4) 162.8 4_556
N23 H23B O100 0.87 2.37 3.185(8) 155.1 4_566
N24 H24A N12 0.87 2.12 2.966(4) 162.9 4_566
N24 H24B O90 0.87 2.16 2.880(6) 139.7 1_565
N33 H33A N30 0.87 2.24 3.101(8) 171.4 2
N33 H33B O50 0.87 2.08 2.948(7) 173.8 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion
_geom_torsion_publ_flag
C11 O1 C10 C1 . 176.1(2) y
C30 C1 C10 O1 . 68.9(3) y
C20 C1 C10 O1 . -51.0(3) y
C40 C1 C10 O1 . -169.0(2) y
C10 O1 C11 C12 . 9.3(4) y
C10 O1 C11 C16 . -170.4(3) y
O1 C11 C12 C13 . 178.7(3) y
C16 C11 C12 C13 . -1.7(5) y
C11 C12 C13 C14 . 1.7(5) y
C12 C13 C14 C15 . -0.8(5) y
C12 C13 C14 C17 . 178.7(3) y
C13 C14 C15 C16 . -0.2(5) y
C17 C14 C15 C16 . -179.6(3) y
C14 C15 C16 C11 . 0.1(6) y
O1 C11 C16 C15 . -179.5(3) y
C12 C11 C16 C15 . 0.8(5) y
C19 N11 C17 N10 . -2.8(6) y
C19 N11 C17 C14 . 176.6(3) y
C18 N10 C17 N11 . 0.3(5) y
C18 N10 C17 C14 . -179.2(3) y
C13 C14 C17 N11 . -149.8(3) y
C15 C14 C17 N11 . 29.7(5) y
C13 C14 C17 N10 . 29.7(5) y
C15 C14 C17 N10 . -150.8(3) y
C19 N12 C18 N14 . 176.1(4) y
C19 N12 C18 N10 . -3.6(6) y
C17 N10 C18 N12 . 3.2(6) y
C17 N10 C18 N14 . -176.5(3) y
C18 N12 C19 N13 . -179.7(4) y
C18 N12 C19 N11 . 0.6(6) y
C17 N11 C19 N13 . -177.3(4) y
C17 N11 C19 N12 . 2.3(6) y
C21 O2 C20 C1 . 168.8(3) y
C30 C1 C20 O2 . 62.1(3) y
C10 C1 C20 O2 . -176.2(3) y
C40 C1 C20 O2 . -59.4(3) y
C20 O2 C21 C22 . 171.3(3) y
C20 O2 C21 C26 . -10.0(5) y
O2 C21 C22 C23 . 179.2(3) y
C26 C21 C22 C23 . 0.4(5) y
C21 C22 C23 C24 . -0.8(6) y
C22 C23 C24 C25 . 0.9(5) y
C22 C23 C24 C27 . 178.8(3) y
C23 C24 C25 C26 . -0.7(5) y
C27 C24 C25 C26 . -178.6(3) y
C24 C25 C26 C21 . 0.3(5) y
O2 C21 C26 C25 . -178.9(3) y
C22 C21 C26 C25 . -0.2(5) y
C29 N20 C27 N21 . -2.2(5) y
C29 N20 C27 C24 . 177.3(3) y
C28 N21 C27 N20 . 4.1(5) y
C28 N21 C27 C24 . -175.5(3) y
C25 C24 C27 N20 . 17.9(5) y
C23 C24 C27 N20 . -159.9(3) y
C25 C24 C27 N21 . -162.5(3) y
C23 C24 C27 N21 . 19.7(5) y
C27 N21 C28 N23 . 177.4(3) y
C27 N21 C28 N22 . -1.2(5) y
C29 N22 C28 N21 . -3.1(6) y
C29 N22 C28 N23 . 178.4(3) y
C28 N22 C29 N24 . -175.9(3) y
C28 N22 C29 N20 . 5.2(6) y
C27 N20 C29 N24 . 178.3(3) y
C27 N20 C29 N22 . -2.8(5) y
C31 O3 C30 C1 . -174.5(3) y
C10 C1 C30 O3 . 60.7(3) y
C20 C1 C30 O3 . -179.9(2) y
C40 C1 C30 O3 . -59.4(3) y
C30 O3 C31 C32 . -6.0(5) y
C30 O3 C31 C36 . 174.7(3) y
O3 C31 C32 C33 . -179.7(4) y
C36 C31 C32 C33 . -0.4(6) y
C31 C32 C33 C34 . -1.1(7) y
C32 C33 C34 C35 . 1.7(7) y
C32 C33 C34 C37 . -179.8(4) y
C33 C34 C35 C36 . -0.8(8) y
C37 C34 C35 C36 . -179.1(5) y
C34 C35 C36 C31 . -0.7(8) y
C32 C31 C36 C35 . 1.2(6) y
O3 C31 C36 C35 . -179.4(4) y
C38 N30 C37 N32 . -1.0(9) y
C38 N30 C37 C34 . 178.7(5) y
C39 N32 C37 N30 . 1.0(9) y
C39 N32 C37 C34 . -178.7(5) y
C35 C34 C37 N30 . 153.2(5) y
C33 C34 C37 N30 . -25.1(7) y
C35 C34 C37 N32 . -27.0(7) y
C33 C34 C37 N32 . 154.6(5) y
C37 N30 C38 N33 . 178.3(6) y
C37 N30 C38 N31 . -1.1(9) y
C39 N31 C38 N33 . -176.5(6) y
C39 N31 C38 N30 . 2.9(1) y
C38 N31 C39 N34 . 177.6(7) y
C38 N31 C39 N32 . -2.80(11) y
C37 N32 C39 N31 . 1.0(1) y
C37 N32 C39 N34 . -179.4(7) y
C40 O4 C40 C1 2_655 -175.3(3) y
C30 C1 C40 O4 . -168.3(2) y
C10 C1 C40 O4 . 69.1(3) y
C20 C1 C40 O4 . -48.1(3) y
C54 O50 C51 C52 . -58.6(1) y
O50 C51 C52 O53 . 62.0(1) y
C51 C52 O53 C55 . -67.20(11) y
C51 O50 C54 C55 . 54.20(11) y
C52 O53 C55 C54 . 67.10(13) y
O50 C54 C55 O53 . -58.00(12) y
C105 S103 O104 C106 . -75.2(1) y
C105 S103 C106 O104 . 85.0(8) y
|
1501601.cif | #------------------------------------------------------------------------------
#$Date: 2019-10-10 08:26:25 +0300 (Thu, 10 Oct 2019) $
#$Revision: 219237 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/50/16/1501601.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_1501601
loop_
_publ_author_name
'Lalibert\'e, Dominic'
'Maris, Thierry'
'Sirois, Ariane'
'Wuest, James D.'
_publ_section_title
;
Molecular Tectonics. Dendritic Construction of Porous Hydrogen-Bonded
Networks
;
_journal_coden_ASTM ORLEF7
_journal_issue 25
_journal_name_full 'Organic Letters'
_journal_page_first 4787
_journal_page_last 4790
_journal_paper_doi 10.1021/ol035712j
_journal_volume 5
_journal_year 2003
_chemical_compound_source 'Synthesized by the authors. See text'
_chemical_formula_moiety 'C52 H58 O19 S6, 2(C H4 O)'
_chemical_formula_sum 'C54 H66 O21 S6'
_chemical_formula_weight 1243.49
_space_group_IT_number 2
_symmetry_cell_setting triclinic
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 67.503(3)
_cell_angle_beta 67.112(4)
_cell_angle_gamma 88.948(4)
_cell_formula_units_Z 2
_cell_length_a 14.1959(19)
_cell_length_b 14.724(2)
_cell_length_c 17.312(2)
_cell_measurement_reflns_used 4220
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 64.89
_cell_measurement_theta_min 3.04
_cell_volume 3043.6(7)
_computing_cell_refinement 'SMART (Bruker, 1999)'
_computing_data_collection 'SMART (Bruker, 1999)'
_computing_data_reduction 'SAINT (Bruker, 1999)'
_computing_molecular_graphics 'XP (Bruker, 1999)'
_computing_publication_material 'UdMX (local program)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type 'Bruker AXS Smart 2K/Platform'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'Sealed Tube'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.032
_diffrn_reflns_av_sigmaI/netI 0.0459
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_l_max 21
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_number 36160
_diffrn_reflns_theta_full 69.86
_diffrn_reflns_theta_max 69.86
_diffrn_reflns_theta_min 3.03
_diffrn_standards_decay_% -0.14
_diffrn_standards_number 163
_exptl_absorpt_coefficient_mu 2.701
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_correction_T_min 0.6900
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Sadabs (Sheldrick,1996)'
_exptl_crystal_colour Colourless
_exptl_crystal_density_diffrn 1.357
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 1308
_exptl_crystal_size_max 0.80
_exptl_crystal_size_mid 0.50
_exptl_crystal_size_min 0.20
_refine_diff_density_max 0.450
_refine_diff_density_min -0.323
_refine_diff_density_rms 0.046
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.038
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 711
_refine_ls_number_reflns 11115
_refine_ls_number_restraints 3
_refine_ls_restrained_S_all 1.038
_refine_ls_R_factor_all 0.0929
_refine_ls_R_factor_gt 0.0561
_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^)+(0.0700P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1391
_refine_ls_wR_factor_ref 0.1519
_reflns_number_gt 6200
_reflns_number_total 11115
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file deposit.cif
_cod_data_source_block jiw578
_cod_depositor_comments
;
Updated bibliographic information.
Antanas Vaitkus,
2019-10-10
;
_cod_original_sg_symbol_H-M P-1
_cod_database_code 1501601
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
S1 S 0.24305(7) -0.27750(5) 1.03867(6) 0.0753(3) Uani 1 1 d . A 1
S2 S 0.33595(7) 0.03412(7) 1.11637(7) 0.0851(3) Uani 1 1 d . A 1
S3 S 0.09410(10) 0.00635(7) 0.80397(9) 0.1016(4) Uani 1 1 d . A 1
S4 S 0.62028(7) 0.32042(6) 0.53596(6) 0.0763(2) Uani 1 1 d . A 1
S5 S 0.62232(8) 0.58433(7) 0.65867(6) 0.0852(3) Uani 1 1 d . A 1
S6 S 0.14659(6) 0.34727(6) 0.91623(6) 0.0757(2) Uani 1 1 d . A 1
O1 O 0.34603(15) 0.18418(13) 0.81364(15) 0.0760(6) Uani 1 1 d . A 1
O10 O 0.15627(19) -0.33343(15) 1.12139(16) 0.0955(7) Uani 1 1 d . A 1
O11 O 0.34508(18) -0.28761(15) 1.03447(17) 0.0912(7) Uani 1 1 d . A 1
O12 O 0.22553(14) -0.16566(13) 1.01783(14) 0.0675(5) Uani 1 1 d . A 1
O20 O 0.27882(19) 0.11024(17) 1.13082(19) 0.1008(8) Uani 1 1 d . A 1
O21 O 0.4381(2) 0.0369(2) 1.1104(2) 0.1155(9) Uani 1 1 d . A 1
O22 O 0.34658(15) 0.03269(15) 1.02263(15) 0.0778(6) Uani 1 1 d . A 1
O30 O -0.0037(2) -0.02943(19) 0.8831(2) 0.1262(11) Uani 1 1 d . A 1
O31 O 0.1231(3) -0.0359(2) 0.7385(3) 0.1526(13) Uani 1 1 d . A 1
O32 O 0.18480(18) -0.00947(16) 0.83721(18) 0.0899(7) Uani 1 1 d . A 1
O40 O 0.72609(18) 0.31912(19) 0.52174(17) 0.0991(7) Uani 1 1 d . A 1
O41 O 0.59168(18) 0.38803(16) 0.46777(15) 0.0897(7) Uani 1 1 d . A 1
O42 O 0.56697(16) 0.33904(15) 0.62660(14) 0.0735(6) Uani 1 1 d . A 1
O50 O 0.6161(2) 0.67462(18) 0.59254(17) 0.1159(9) Uani 1 1 d . A 1
O51 O 0.7013(2) 0.52868(19) 0.63443(18) 0.1091(8) Uani 1 1 d . A 1
O52 O 0.51178(17) 0.51967(15) 0.69731(15) 0.0809(6) Uani 1 1 d . A 1
O60 O 0.11935(18) 0.24792(17) 0.93225(17) 0.0966(7) Uani 1 1 d . A 1
O61 O 0.10397(18) 0.42249(18) 0.86653(17) 0.0995(7) Uani 1 1 d . A 1
O62 O 0.26899(15) 0.37545(16) 0.86498(15) 0.0786(6) Uani 1 1 d . A 1
C1 C 0.4212(2) 0.35451(19) 0.74910(19) 0.0582(7) Uani 1 1 d . A 1
C2 C 0.4163(2) 0.2491(2) 0.8152(2) 0.0669(8) Uani 1 1 d . A 1
H2A H 0.4844 0.2293 0.7974 0.080 Uiso 1 1 calc R A 1
H2B H 0.3940 0.2460 0.8768 0.080 Uiso 1 1 calc R A 1
C3 C 0.3643(2) 0.08405(19) 0.8370(2) 0.0716(9) Uani 1 1 d . A 1
H3A H 0.4274 0.0782 0.8467 0.086 Uiso 1 1 calc R A 1
H3B H 0.3741 0.0661 0.7863 0.086 Uiso 1 1 calc R A 1
C4 C 0.2743(2) 0.01122(19) 0.9242(2) 0.0602(7) Uani 1 1 d . A 1
C10 C 0.2354(2) -0.2945(2) 0.9461(2) 0.0696(8) Uani 1 1 d . A 1
C11 C 0.3132(3) -0.3353(2) 0.8968(3) 0.0858(10) Uani 1 1 d . A 1
H11 H 0.3686 -0.3536 0.9123 0.103 Uiso 1 1 calc . B 1
C12 C 0.3056(3) -0.3479(3) 0.8233(3) 0.0914(11) Uani 1 1 d . A 1
H12 H 0.3562 -0.3765 0.7909 0.110 Uiso 1 1 calc . C 1
C13 C 0.2268(3) -0.3198(2) 0.7977(3) 0.0841(10) Uani 1 1 d . A 1
C14 C 0.1500(3) -0.2795(3) 0.8489(3) 0.0855(10) Uani 1 1 d . A 1
H14 H 0.0953 -0.2603 0.8326 0.103 Uiso 1 1 calc . D 1
C15 C 0.1536(2) -0.2677(2) 0.9221(3) 0.0761(9) Uani 1 1 d . A 1
H15 H 0.1011 -0.2417 0.9559 0.091 Uiso 1 1 calc . E 1
C16 C 0.2228(3) -0.3306(3) 0.7150(3) 0.1191(14) Uani 1 1 d . A 1
H16A H 0.1619 -0.3077 0.7076 0.179 Uiso 1 1 calc R A 1
H16B H 0.2210 -0.3993 0.7243 0.179 Uiso 1 1 calc R A 1
H16C H 0.2831 -0.2917 0.6609 0.179 Uiso 1 1 calc R A 1
C17 C 0.3079(2) -0.09009(18) 0.9386(2) 0.0644(8) Uani 1 1 d . A 1
H17A H 0.3222 -0.1028 0.8844 0.077 Uiso 1 1 calc R A 1
H17B H 0.3706 -0.0919 0.9488 0.077 Uiso 1 1 calc R A 1
C20 C 0.2631(3) -0.0802(3) 1.1987(3) 0.0919(11) Uani 1 1 d . A 1
C21 C 0.1679(5) -0.0848(4) 1.2638(4) 0.1371(17) Uani 1 1 d . A 1
H21 H 0.1395 -0.0272 1.2635 0.165 Uiso 1 1 calc . F 1
C22 C 0.1126(5) -0.1809(7) 1.3328(4) 0.171(2) Uani 1 1 d . A 1
H22 H 0.0491 -0.1865 1.3800 0.205 Uiso 1 1 calc . G 1
C23 C 0.1551(7) -0.2655(6) 1.3281(6) 0.166(3) Uani 1 1 d . A 1
C24 C 0.2465(7) -0.2568(5) 1.2635(6) 0.157(3) Uani 1 1 d . A 1
H24 H 0.2749 -0.3140 1.2627 0.188 Uiso 1 1 calc . H 1
C25 C 0.3011(4) -0.1670(4) 1.1977(4) 0.1231(16) Uani 1 1 d . A 1
H25 H 0.3645 -0.1639 1.1516 0.148 Uiso 1 1 calc . I 1
C26 C 0.0892(6) -0.3643(5) 1.4059(6) 0.274(5) Uani 1 1 d . A 1
H26A H 0.0243 -0.3514 1.4427 0.412 Uiso 1 1 calc R A 1
H26B H 0.1254 -0.3956 1.4435 0.412 Uiso 1 1 calc R A 1
H26C H 0.0769 -0.4076 1.3800 0.412 Uiso 1 1 calc R A 1
C27 C 0.2535(2) 0.0361(2) 1.0063(2) 0.0661(8) Uani 1 1 d . A 1
H27A H 0.2339 0.1019 0.9943 0.079 Uiso 1 1 calc R A 1
H27B H 0.1971 -0.0115 1.0601 0.079 Uiso 1 1 calc R A 1
C30 C 0.1090(3) 0.1359(2) 0.7481(2) 0.0767(9) Uani 1 1 d . A 1
C31 C 0.1878(3) 0.1856(4) 0.6635(3) 0.1144(14) Uani 1 1 d . A 1
H31 H 0.2326 0.1503 0.6345 0.137 Uiso 1 1 calc . J 1
C32 C 0.2006(4) 0.2866(4) 0.6216(3) 0.1197(15) Uani 1 1 d . A 1
H32 H 0.2543 0.3195 0.5639 0.144 Uiso 1 1 calc . K 1
C33 C 0.1367(4) 0.3410(3) 0.6625(3) 0.0949(11) Uani 1 1 d . A 1
C34 C 0.0595(3) 0.2909(3) 0.7463(3) 0.0950(11) Uani 1 1 d . A 1
H34 H 0.0147 0.3263 0.7750 0.114 Uiso 1 1 calc . L 1
C35 C 0.0454(3) 0.1890(3) 0.7902(2) 0.0834(10) Uani 1 1 d . A 1
H35 H -0.0075 0.1564 0.8484 0.100 Uiso 1 1 calc . M 1
C36 C 0.1540(4) 0.4529(3) 0.6156(3) 0.153(2) Uani 1 1 d . A 1
H36A H 0.2133 0.4746 0.5578 0.229 Uiso 1 1 calc R A 1
H36B H 0.1657 0.4805 0.6538 0.229 Uiso 1 1 calc R A 1
H36C H 0.0941 0.4748 0.6054 0.229 Uiso 1 1 calc R A 1
C37 C 0.1730(2) 0.0171(2) 0.9122(2) 0.0708(8) Uani 1 1 d . A 1
H37A H 0.1171 -0.0282 0.9682 0.085 Uiso 1 1 calc R A 1
H37B H 0.1563 0.0840 0.8992 0.085 Uiso 1 1 calc R A 1
C40 C 0.5624(3) 0.1998(2) 0.5691(2) 0.0760(9) Uani 1 1 d . A 1
C41 C 0.4872(3) 0.1844(3) 0.5443(3) 0.0879(10) Uani 1 1 d . A 1
H41 H 0.4661 0.2379 0.5080 0.105 Uiso 1 1 calc . N 1
C42 C 0.4406(3) 0.0852(4) 0.5743(3) 0.1066(13) Uani 1 1 d . A 1
H42 H 0.3899 0.0737 0.5562 0.128 Uiso 1 1 calc . O 1
C43 C 0.4696(4) 0.0075(3) 0.6291(3) 0.1106(15) Uani 1 1 d . A 1
C44 C 0.5481(5) 0.0257(3) 0.6518(3) 0.1245(16) Uani 1 1 d . A 1
H44 H 0.5703 -0.0276 0.6872 0.149 Uiso 1 1 calc . P 1
C45 C 0.5935(3) 0.1194(3) 0.6236(3) 0.1034(12) Uani 1 1 d . A 1
H45 H 0.6454 0.1301 0.6406 0.124 Uiso 1 1 calc . Q 1
C46 C 0.4131(4) -0.0961(3) 0.6621(4) 0.168(2) Uani 1 1 d . A 1
H46A H 0.3610 -0.0914 0.6388 0.253 Uiso 1 1 calc R A 1
H46B H 0.3810 -0.1260 0.7280 0.253 Uiso 1 1 calc R A 1
H46C H 0.4616 -0.1363 0.6402 0.253 Uiso 1 1 calc R A 1
C47 C 0.4633(2) 0.3626(2) 0.6501(2) 0.0632(7) Uani 1 1 d . A 1
H47A H 0.4200 0.3164 0.6455 0.076 Uiso 1 1 calc R A 1
H47B H 0.4637 0.4294 0.6086 0.076 Uiso 1 1 calc R A 1
C50 C 0.6202(2) 0.6025(2) 0.7529(2) 0.0686(8) Uani 1 1 d . A 1
C51 C 0.5899(3) 0.6882(3) 0.7641(3) 0.0873(10) Uani 1 1 d . A 1
H51 H 0.5728 0.7370 0.7205 0.105 Uiso 1 1 calc . R 1
C52 C 0.5853(3) 0.7004(3) 0.8389(3) 0.0955(11) Uani 1 1 d . A 1
H52 H 0.5647 0.7581 0.8458 0.115 Uiso 1 1 calc . S 1
C53 C 0.6096(3) 0.6313(3) 0.9045(2) 0.0814(10) Uani 1 1 d . A 1
C54 C 0.6424(3) 0.5481(3) 0.8915(3) 0.0931(11) Uani 1 1 d . A 1
H54 H 0.6611 0.5008 0.9348 0.112 Uiso 1 1 calc . T 1
C55 C 0.6483(3) 0.5329(2) 0.8173(3) 0.0838(10) Uani 1 1 d . A 1
H55 H 0.6712 0.4759 0.8099 0.101 Uiso 1 1 calc . U 1
C56 C 0.6000(3) 0.6456(4) 0.9891(3) 0.1230(15) Uani 1 1 d . A 1
H56A H 0.6219 0.5905 1.0267 0.184 Uiso 1 1 calc R A 1
H56B H 0.5293 0.6492 1.0232 0.184 Uiso 1 1 calc R A 1
H56C H 0.6429 0.7062 0.9710 0.184 Uiso 1 1 calc R A 1
C57 C 0.4962(3) 0.4196(2) 0.7597(2) 0.0740(9) Uani 1 1 d . A 1
H57A H 0.4676 0.4153 0.8220 0.089 Uiso 1 1 calc R A 1
H57B H 0.5620 0.3950 0.7480 0.089 Uiso 1 1 calc R A 1
C60 C 0.1272(2) 0.3540(2) 1.0200(2) 0.0714(9) Uani 1 1 d . A 1
C61 C 0.1275(3) 0.2712(3) 1.0914(3) 0.0915(11) Uani 1 1 d . A 1
H61 H 0.1398 0.2119 1.0845 0.110 Uiso 1 1 calc . V 1
C62 C 0.1096(3) 0.2760(3) 1.1735(3) 0.1038(13) Uani 1 1 d . A 1
H62 H 0.1106 0.2195 1.2217 0.125 Uiso 1 1 calc . W 1
C63 C 0.0900(3) 0.3633(3) 1.1863(3) 0.0961(11) Uani 1 1 d . A 1
C64 C 0.0892(3) 0.4455(3) 1.1128(3) 0.0916(11) Uani 1 1 d . A 1
H64 H 0.0755 0.5045 1.1198 0.110 Uiso 1 1 calc . X 1
C65 C 0.1080(3) 0.4424(2) 1.0303(3) 0.0827(10) Uani 1 1 d . A 1
H65 H 0.1079 0.4989 0.9816 0.099 Uiso 1 1 calc . y 1
C66 C 0.0706(4) 0.3698(4) 1.2761(3) 0.1454(18) Uani 1 1 d . A 1
H66A H 0.0757 0.3069 1.3187 0.218 Uiso 1 1 calc R A 1
H66B H 0.0026 0.3861 1.3010 0.218 Uiso 1 1 calc R A 1
H66C H 0.1212 0.4204 1.2658 0.218 Uiso 1 1 calc R A 1
C67 C 0.3140(2) 0.3845(2) 0.7706(2) 0.0685(8) Uani 1 1 d . A 1
H67A H 0.3187 0.4526 0.7290 0.082 Uiso 1 1 calc R A 1
H67B H 0.2705 0.3418 0.7627 0.082 Uiso 1 1 calc R A 1
O101 O 0.144(2) -0.0496(18) 0.5307(17) 0.696(13) Uiso 1 1 d D Z 2
H101 H 0.1707 -0.0744 0.4936 1.044 Uiso 1 1 calc . A 2
C102 C 0.041(2) -0.038(3) 0.541(3) 0.83(3) Uiso 1 1 d D Z 2
H10A H -0.0027 -0.0529 0.6043 1.245 Uiso 1 1 calc R Z 2
H10B H 0.0159 -0.0833 0.5227 1.245 Uiso 1 1 calc R Z 2
H10C H 0.0387 0.0288 0.5035 1.245 Uiso 1 1 calc R Z 2
O103 O 0.165(2) 0.116(2) 1.471(2) 0.799(19) Uiso 1 1 d D B 3
H103 H 0.2088 0.0952 1.4908 1.199 Uiso 1 1 calc . C 3
C104 C 0.181(3) 0.091(2) 1.395(2) 0.73(2) Uiso 1 1 d D B 3
H10D H 0.1882 0.0224 1.4115 1.102 Uiso 1 1 calc R B 3
H10E H 0.2432 0.1315 1.3437 1.102 Uiso 1 1 calc R B 3
H10F H 0.1233 0.1042 1.3790 1.102 Uiso 1 1 calc R B 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
S1 0.0808(6) 0.0445(4) 0.0867(6) -0.0210(4) -0.0263(5) 0.0056(4)
S2 0.0790(6) 0.0812(6) 0.1224(8) -0.0516(6) -0.0593(6) 0.0237(5)
S3 0.1236(9) 0.0707(6) 0.1429(10) -0.0415(7) -0.0893(8) 0.0190(6)
S4 0.0806(6) 0.0696(5) 0.0690(5) -0.0283(4) -0.0209(4) 0.0056(4)
S5 0.0917(7) 0.0750(6) 0.0738(6) -0.0235(5) -0.0245(5) -0.0206(5)
S6 0.0630(5) 0.0662(5) 0.0905(6) -0.0315(5) -0.0248(4) 0.0085(4)
O1 0.0684(14) 0.0444(11) 0.1089(17) -0.0193(11) -0.0420(12) 0.0034(9)
O10 0.1085(18) 0.0607(13) 0.0845(16) -0.0228(12) -0.0132(14) -0.0119(12)
O11 0.0933(17) 0.0637(13) 0.124(2) -0.0334(13) -0.0581(15) 0.0272(12)
O12 0.0635(13) 0.0472(10) 0.0804(14) -0.0225(10) -0.0219(10) 0.0059(9)
O20 0.114(2) 0.0835(16) 0.141(2) -0.0632(16) -0.0712(17) 0.0369(14)
O21 0.0887(19) 0.135(2) 0.169(3) -0.079(2) -0.0831(18) 0.0267(16)
O22 0.0592(13) 0.0895(15) 0.0984(17) -0.0464(13) -0.0385(12) 0.0169(11)
O30 0.097(2) 0.0912(19) 0.158(3) -0.0025(18) -0.067(2) -0.0245(15)
O31 0.246(4) 0.111(2) 0.213(3) -0.102(2) -0.171(3) 0.071(2)
O32 0.1047(18) 0.0756(15) 0.1215(19) -0.0550(15) -0.0648(15) 0.0341(13)
O40 0.0660(16) 0.1111(19) 0.1087(18) -0.0491(15) -0.0205(13) 0.0101(13)
O41 0.1112(18) 0.0731(14) 0.0699(15) -0.0189(12) -0.0326(13) 0.0102(13)
O42 0.0708(14) 0.0779(14) 0.0763(14) -0.0375(12) -0.0287(11) 0.0118(11)
O50 0.158(2) 0.0827(17) 0.0801(17) 0.0042(14) -0.0578(17) -0.0305(16)
O51 0.103(2) 0.0966(18) 0.114(2) -0.0503(16) -0.0229(16) -0.0072(15)
O52 0.0967(17) 0.0603(13) 0.0844(15) -0.0234(12) -0.0417(13) 0.0003(11)
O60 0.0972(17) 0.0722(15) 0.1080(19) -0.0401(14) -0.0263(14) -0.0056(12)
O61 0.0911(18) 0.0969(18) 0.1100(19) -0.0375(15) -0.0464(15) 0.0320(14)
O62 0.0643(14) 0.0922(16) 0.0782(15) -0.0417(13) -0.0213(11) 0.0050(11)
C1 0.0601(18) 0.0490(15) 0.0622(18) -0.0203(14) -0.0239(14) 0.0012(12)
C2 0.073(2) 0.0562(17) 0.074(2) -0.0233(16) -0.0359(16) 0.0069(15)
C3 0.067(2) 0.0446(15) 0.083(2) -0.0184(16) -0.0183(16) 0.0058(13)
C4 0.0612(19) 0.0414(14) 0.077(2) -0.0220(15) -0.0298(15) 0.0078(12)
C10 0.066(2) 0.0443(15) 0.083(2) -0.0247(15) -0.0159(17) 0.0023(13)
C11 0.073(2) 0.063(2) 0.099(3) -0.028(2) -0.018(2) 0.0167(16)
C12 0.086(3) 0.073(2) 0.093(3) -0.036(2) -0.013(2) 0.0164(19)
C13 0.091(3) 0.062(2) 0.083(3) -0.0307(19) -0.018(2) -0.0016(18)
C14 0.078(2) 0.072(2) 0.107(3) -0.040(2) -0.035(2) 0.0026(17)
C15 0.058(2) 0.067(2) 0.101(3) -0.0462(19) -0.0191(18) 0.0078(15)
C16 0.136(4) 0.113(3) 0.099(3) -0.049(3) -0.032(3) -0.007(3)
C17 0.0579(18) 0.0437(15) 0.079(2) -0.0199(15) -0.0213(15) 0.0050(13)
C20 0.092(3) 0.093(3) 0.114(3) -0.038(2) -0.069(3) 0.027(2)
C21 0.125(4) 0.121(4) 0.132(4) -0.018(3) -0.052(3) 0.019(3)
C22 0.123(5) 0.185(7) 0.145(5) -0.011(5) -0.051(4) -0.007(5)
C23 0.175(7) 0.125(5) 0.193(7) 0.009(5) -0.143(6) -0.004(6)
C24 0.181(6) 0.090(4) 0.239(8) -0.036(5) -0.157(6) 0.030(4)
C25 0.139(4) 0.088(3) 0.178(5) -0.047(3) -0.107(4) 0.038(3)
C26 0.243(8) 0.169(6) 0.308(9) 0.095(6) -0.196(7) -0.072(6)
C27 0.0561(19) 0.0560(17) 0.088(2) -0.0280(16) -0.0336(16) 0.0127(13)
C30 0.073(2) 0.076(2) 0.078(2) -0.0269(19) -0.0317(18) 0.0143(17)
C31 0.108(3) 0.119(4) 0.088(3) -0.044(3) -0.010(2) 0.030(3)
C32 0.111(3) 0.111(4) 0.072(3) -0.008(3) -0.001(2) -0.010(3)
C33 0.112(3) 0.076(3) 0.085(3) -0.010(2) -0.050(3) -0.001(2)
C34 0.102(3) 0.081(3) 0.091(3) -0.031(2) -0.034(2) 0.026(2)
C35 0.068(2) 0.081(2) 0.073(2) -0.0171(19) -0.0162(17) 0.0101(17)
C36 0.218(6) 0.075(3) 0.150(4) -0.002(3) -0.103(4) -0.005(3)
C37 0.067(2) 0.0586(18) 0.090(2) -0.0296(17) -0.0374(17) 0.0161(14)
C40 0.080(2) 0.071(2) 0.071(2) -0.0303(18) -0.0245(18) 0.0124(17)
C41 0.101(3) 0.077(2) 0.092(3) -0.041(2) -0.041(2) 0.018(2)
C42 0.106(3) 0.103(3) 0.117(3) -0.062(3) -0.034(3) 0.006(3)
C43 0.130(4) 0.066(3) 0.095(3) -0.037(2) -0.002(3) 0.002(3)
C44 0.157(5) 0.069(3) 0.118(4) -0.024(3) -0.042(3) 0.025(3)
C45 0.130(3) 0.076(3) 0.104(3) -0.032(2) -0.053(3) 0.028(2)
C46 0.195(5) 0.085(3) 0.155(5) -0.053(3) 0.002(4) -0.027(3)
C47 0.066(2) 0.0559(17) 0.069(2) -0.0245(15) -0.0312(15) 0.0079(14)
C50 0.067(2) 0.0618(18) 0.068(2) -0.0172(16) -0.0265(16) -0.0102(15)
C51 0.111(3) 0.072(2) 0.099(3) -0.034(2) -0.063(2) 0.023(2)
C52 0.101(3) 0.096(3) 0.120(3) -0.063(3) -0.058(3) 0.023(2)
C53 0.073(2) 0.092(3) 0.075(2) -0.026(2) -0.0344(18) -0.0130(19)
C54 0.115(3) 0.073(2) 0.096(3) -0.018(2) -0.064(2) 0.000(2)
C55 0.098(3) 0.062(2) 0.108(3) -0.033(2) -0.060(2) 0.0112(17)
C56 0.117(3) 0.161(4) 0.096(3) -0.060(3) -0.040(3) -0.028(3)
C57 0.091(2) 0.0609(19) 0.066(2) -0.0235(17) -0.0300(17) -0.0064(16)
C60 0.0542(19) 0.0617(19) 0.087(2) -0.0289(18) -0.0193(16) 0.0089(14)
C61 0.099(3) 0.073(2) 0.092(3) -0.033(2) -0.031(2) 0.0307(19)
C62 0.106(3) 0.096(3) 0.095(3) -0.032(3) -0.035(2) 0.033(2)
C63 0.077(3) 0.106(3) 0.101(3) -0.051(3) -0.025(2) 0.010(2)
C64 0.080(2) 0.079(3) 0.111(3) -0.050(3) -0.023(2) 0.0064(19)
C65 0.078(2) 0.0560(19) 0.100(3) -0.029(2) -0.026(2) 0.0066(16)
C66 0.141(4) 0.196(5) 0.117(4) -0.094(4) -0.041(3) 0.026(4)
C67 0.072(2) 0.0592(18) 0.070(2) -0.0229(16) -0.0280(16) 0.0095(15)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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_publ_flag
O10 S1 O11 119.61(15) y
O10 S1 O12 104.19(12) y
O11 S1 O12 109.52(12) y
O10 S1 C10 110.53(15) y
O11 S1 C10 108.83(15) y
O12 S1 C10 102.77(13) y
O21 S2 O20 119.80(16) y
O21 S2 O22 104.55(15) y
O20 S2 O22 108.80(14) y
O21 S2 C20 109.69(18) y
O20 S2 C20 108.71(19) y
O22 S2 C20 104.12(16) y
O31 S3 O30 121.0(2) y
O31 S3 O32 103.02(17) y
O30 S3 O32 109.07(16) y
O31 S3 C30 109.71(19) y
O30 S3 C30 109.58(18) y
O32 S3 C30 102.81(14) y
O41 S4 O40 121.21(15) y
O41 S4 O42 108.56(13) y
O40 S4 O42 104.59(13) y
O41 S4 C40 108.96(16) y
O40 S4 C40 109.01(16) y
O42 S4 C40 102.94(13) y
O51 S5 O50 120.92(18) y
O51 S5 O52 109.88(14) y
O50 S5 O52 102.69(15) y
O51 S5 C50 108.38(17) y
O50 S5 C50 110.00(17) y
O52 S5 C50 103.53(13) y
O61 S6 O60 118.64(16) y
O61 S6 O62 107.77(14) y
O60 S6 O62 108.54(13) y
O61 S6 C60 110.86(15) y
O60 S6 C60 109.58(15) y
O62 S6 C60 99.73(13) y
C2 O1 C3 115.8(2) y
C17 O12 S1 116.22(16) y
C27 O22 S2 117.21(19) y
C37 O32 S3 116.90(19) y
C47 O42 S4 117.93(17) y
C57 O52 S5 117.11(19) y
C67 O62 S6 115.47(18) y
C2 C1 C67 111.0(2) y
C2 C1 C47 110.6(2) y
C67 C1 C47 106.6(2) y
C2 C1 C57 104.8(2) y
C67 C1 C57 113.3(2) y
C47 C1 C57 110.6(2) y
O1 C2 C1 109.3(2) y
O1 C2 H2A 109.8 ?
C1 C2 H2A 109.8 ?
O1 C2 H2B 109.8 ?
C1 C2 H2B 109.8 ?
H2A C2 H2B 108.3 ?
O1 C3 C4 112.1(2) y
O1 C3 H3A 109.2 ?
C4 C3 H3A 109.2 ?
O1 C3 H3B 109.2 ?
C4 C3 H3B 109.2 ?
H3A C3 H3B 107.9 ?
C17 C4 C27 112.0(2) y
C17 C4 C37 112.2(2) y
C27 C4 C37 105.1(2) y
C17 C4 C3 104.5(2) y
C27 C4 C3 112.0(2) y
C37 C4 C3 111.2(2) y
C15 C10 C11 120.3(3) y
C15 C10 S1 120.6(2) y
C11 C10 S1 119.2(3) y
C10 C11 C12 118.1(3) y
C10 C11 H11 120.9 ?
C12 C11 H11 120.9 ?
C13 C12 C11 122.3(3) y
C13 C12 H12 118.9 ?
C11 C12 H12 118.9 ?
C12 C13 C14 118.0(4) y
C12 C13 C16 121.1(4) y
C14 C13 C16 120.8(4) y
C15 C14 C13 121.5(3) y
C15 C14 H14 119.3 ?
C13 C14 H14 119.3 ?
C14 C15 C10 119.8(3) y
C14 C15 H15 120.1 ?
C10 C15 H15 120.1 ?
C13 C16 H16A 109.5 ?
C13 C16 H16B 109.5 ?
H16A C16 H16B 109.5 ?
C13 C16 H16C 109.5 ?
H16A C16 H16C 109.5 ?
H16B C16 H16C 109.5 ?
O12 C17 C4 109.0(2) y
O12 C17 H17A 109.9 ?
C4 C17 H17A 109.9 ?
O12 C17 H17B 109.9 ?
C4 C17 H17B 109.9 ?
H17A C17 H17B 108.3 ?
C21 C20 C25 119.8(4) y
C21 C20 S2 120.3(4) y
C25 C20 S2 119.9(4) y
C20 C21 C22 118.2(5) y
C20 C21 H21 120.9 ?
C22 C21 H21 120.9 ?
C23 C22 C21 119.2(6) y
C23 C22 H22 120.4 ?
C21 C22 H22 120.4 ?
C24 C23 C22 120.0(7) y
C24 C23 C26 125.3(9) y
C22 C23 C26 114.6(9) y
C23 C24 C25 122.2(7) y
C23 C24 H24 118.9 ?
C25 C24 H24 118.9 ?
C24 C25 C20 120.5(5) y
C24 C25 H25 119.7 ?
C20 C25 H25 119.7 ?
C23 C26 H26A 109.5 ?
C23 C26 H26B 109.5 ?
H26A C26 H26B 109.5 ?
C23 C26 H26C 109.5 ?
H26A C26 H26C 109.5 ?
H26B C26 H26C 109.5 ?
O22 C27 C4 108.9(2) y
O22 C27 H27A 109.9 ?
C4 C27 H27A 109.9 ?
O22 C27 H27B 109.9 ?
C4 C27 H27B 109.9 ?
H27A C27 H27B 108.3 ?
C35 C30 C31 119.1(3) y
C35 C30 S3 120.5(3) y
C31 C30 S3 120.4(3) y
C32 C31 C30 120.0(4) y
C32 C31 H31 120 ?
C30 C31 H31 120 ?
C31 C32 C33 121.7(4) y
C31 C32 H32 119.2 ?
C33 C32 H32 119.2 ?
C34 C33 C32 117.6(4) y
C34 C33 C36 121.7(5) y
C32 C33 C36 120.6(4) y
C33 C34 C35 121.8(4) y
C33 C34 H34 119.1 ?
C35 C34 H34 119.1 ?
C30 C35 C34 119.8(3) y
C30 C35 H35 120.1 ?
C34 C35 H35 120.1 ?
C33 C36 H36A 109.5 ?
C33 C36 H36B 109.5 ?
H36A C36 H36B 109.5 ?
C33 C36 H36C 109.5 ?
H36A C36 H36C 109.5 ?
H36B C36 H36C 109.5 ?
O32 C37 C4 108.7(2) y
O32 C37 H37A 109.9 ?
C4 C37 H37A 109.9 ?
O32 C37 H37B 109.9 ?
C4 C37 H37B 109.9 ?
H37A C37 H37B 108.3 ?
C41 C40 C45 120.1(3) y
C41 C40 S4 120.9(3) y
C45 C40 S4 119.0(3) y
C40 C41 C42 119.2(4) y
C40 C41 H41 120.4 ?
C42 C41 H41 120.4 ?
C43 C42 C41 120.3(4) y
C43 C42 H42 119.8 ?
C41 C42 H42 119.8 ?
C42 C43 C44 119.0(4) y
C42 C43 C46 117.5(6) y
C44 C43 C46 123.5(5) y
C45 C44 C43 121.4(4) y
C45 C44 H44 119.3 ?
C43 C44 H44 119.3 ?
C44 C45 C40 119.9(4) y
C44 C45 H45 120 ?
C40 C45 H45 120 ?
C43 C46 H46A 109.5 ?
C43 C46 H46B 109.5 ?
H46A C46 H46B 109.5 ?
C43 C46 H46C 109.5 ?
H46A C46 H46C 109.5 ?
H46B C46 H46C 109.5 ?
O42 C47 C1 107.6(2) y
O42 C47 H47A 110.2 ?
C1 C47 H47A 110.2 ?
O42 C47 H47B 110.2 ?
C1 C47 H47B 110.2 ?
H47A C47 H47B 108.5 ?
C55 C50 C51 118.9(3) y
C55 C50 S5 121.3(3) y
C51 C50 S5 119.7(3) y
C52 C51 C50 119.4(3) y
C52 C51 H51 120.3 ?
C50 C51 H51 120.3 ?
C51 C52 C53 122.5(4) y
C51 C52 H52 118.7 ?
C53 C52 H52 118.7 ?
C52 C53 C54 117.7(4) y
C52 C53 C56 121.2(4) y
C54 C53 C56 121.2(4) y
C55 C54 C53 121.8(3) y
C55 C54 H54 119.1 ?
C53 C54 H54 119.1 ?
C54 C55 C50 119.6(3) y
C54 C55 H55 120.2 ?
C50 C55 H55 120.2 ?
C53 C56 H56A 109.5 ?
C53 C56 H56B 109.5 ?
H56A C56 H56B 109.5 ?
C53 C56 H56C 109.5 ?
H56A C56 H56C 109.5 ?
H56B C56 H56C 109.5 ?
O52 C57 C1 110.2(2) y
O52 C57 H57A 109.6 ?
C1 C57 H57A 109.6 ?
O52 C57 H57B 109.6 ?
C1 C57 H57B 109.6 ?
H57A C57 H57B 108.1 ?
C61 C60 C65 120.4(3) y
C61 C60 S6 119.7(3) y
C65 C60 S6 119.9(3) y
C60 C61 C62 119.6(3) y
C60 C61 H61 120.2 ?
C62 C61 H61 120.2 ?
C61 C62 C63 121.5(4) y
C61 C62 H62 119.2 ?
C63 C62 H62 119.2 ?
C64 C63 C62 117.3(4) y
C64 C63 C66 120.6(4) y
C62 C63 C66 122.1(4) y
C65 C64 C63 122.0(3) y
C65 C64 H64 119 ?
C63 C64 H64 119 ?
C64 C65 C60 119.2(3) y
C64 C65 H65 120.4 ?
C60 C65 H65 120.4 ?
C63 C66 H66A 109.5 ?
C63 C66 H66B 109.5 ?
H66A C66 H66B 109.5 ?
C63 C66 H66C 109.5 ?
H66A C66 H66C 109.5 ?
H66B C66 H66C 109.5 ?
O62 C67 C1 108.9(2) y
O62 C67 H67A 109.9 ?
C1 C67 H67A 109.9 ?
O62 C67 H67B 109.9 ?
C1 C67 H67B 109.9 ?
H67A C67 H67B 108.3 ?
C102 O101 H101 109.5 ?
O101 C102 H10A 109.5 ?
O101 C102 H10B 109.5 ?
H10A C102 H10B 109.5 ?
O101 C102 H10C 109.5 ?
H10A C102 H10C 109.5 ?
H10B C102 H10C 109.5 ?
C104 O103 H103 109.5 ?
O103 C104 H10D 109.5 ?
O103 C104 H10E 109.5 ?
H10D C104 H10E 109.5 ?
O103 C104 H10F 109.5 ?
H10D C104 H10F 109.5 ?
H10E C104 H10F 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
S1 O10 1.417(2) y
S1 O11 1.430(2) y
S1 O12 1.5824(18) y
S1 C10 1.757(3) y
S2 O21 1.413(2) y
S2 O20 1.414(2) y
S2 O22 1.579(2) y
S2 C20 1.737(4) y
S3 O31 1.416(3) y
S3 O30 1.441(3) y
S3 O32 1.583(2) y
S3 C30 1.750(3) y
S4 O41 1.417(2) y
S4 O40 1.425(2) y
S4 O42 1.584(2) y
S4 C40 1.751(3) y
S5 O51 1.403(3) y
S5 O50 1.412(2) y
S5 O52 1.602(2) y
S5 C50 1.739(3) y
S6 O61 1.409(2) y
S6 O60 1.412(2) y
S6 O62 1.589(2) y
S6 C60 1.750(3) y
O1 C2 1.409(3) y
O1 C3 1.420(3) y
O12 C17 1.456(3) y
O22 C27 1.450(3) y
O32 C37 1.443(4) y
O42 C47 1.441(3) y
O52 C57 1.413(3) y
O62 C67 1.455(3) y
C1 C2 1.518(4) y
C1 C67 1.520(4) y
C1 C47 1.535(4) y
C1 C57 1.552(4) y
C2 H2a 0.97 ?
C2 H2b 0.97 ?
C3 C4 1.540(4) y
C3 H3a 0.97 ?
C3 H3b 0.97 ?
C4 C17 1.515(3) y
C4 C27 1.520(4) y
C4 C37 1.527(4) y
C10 C15 1.382(4) y
C10 C11 1.394(4) y
C11 C12 1.397(5) y
C11 H11 0.93 ?
C12 C13 1.359(5) y
C12 H12 0.93 ?
C13 C14 1.398(5) y
C13 C16 1.521(5) y
C14 C15 1.364(5) y
C14 H14 0.93 ?
C15 H15 0.93 ?
C16 H16a 0.96 ?
C16 H16b 0.96 ?
C16 H16c 0.96 ?
C17 H17a 0.97 ?
C17 H17b 0.97 ?
C20 C21 1.365(6) y
C20 C25 1.381(5) y
C21 C22 1.436(8) y
C21 H21 0.93 ?
C22 C23 1.392(9) y
C22 H22 0.93 ?
C23 C24 1.311(9) y
C23 C26 1.542(8) y
C24 C25 1.358(8) y
C24 H24 0.93 ?
C25 H25 0.93 ?
C26 H26a 0.96 ?
C26 H26b 0.96 ?
C26 H26c 0.96 ?
C27 H27a 0.97 ?
C27 H27b 0.97 ?
C30 C35 1.363(5) y
C30 C31 1.366(5) y
C31 C32 1.362(6) y
C31 H31 0.93 ?
C32 C33 1.368(6) y
C32 H32 0.93 ?
C33 C34 1.350(5) y
C33 C36 1.506(5) y
C34 C35 1.374(5) y
C34 H34 0.93 ?
C35 H35 0.93 ?
C36 H36a 0.96 ?
C36 H36b 0.96 ?
C36 H36c 0.96 ?
C37 H37a 0.97 ?
C37 H37b 0.97 ?
C40 C41 1.347(4) y
C40 C45 1.391(5) y
C41 C42 1.425(5) y
C41 H41 0.93 ?
C42 C43 1.354(6) y
C42 H42 0.93 ?
C43 C44 1.378(6) y
C43 C46 1.524(5) y
C44 C45 1.353(6) y
C44 H44 0.93 ?
C45 H45 0.93 ?
C46 H46a 0.96 ?
C46 H46b 0.96 ?
C46 H46c 0.96 ?
C47 H47a 0.97 ?
C47 H47b 0.97 ?
C50 C55 1.382(4) y
C50 C51 1.385(4) y
C51 C52 1.351(5) y
C51 H51 0.93 ?
C52 C53 1.361(5) y
C52 H52 0.93 ?
C53 C54 1.369(5) y
C53 C56 1.512(5) y
C54 C55 1.359(5) y
C54 H54 0.93 ?
C55 H55 0.93 ?
C56 H56a 0.96 ?
C56 H56b 0.96 ?
C56 H56c 0.96 ?
C57 H57a 0.97 ?
C57 H57b 0.97 ?
C60 C61 1.366(4) y
C60 C65 1.389(4) y
C61 C62 1.373(5) y
C61 H61 0.93 ?
C62 C63 1.392(5) y
C62 H62 0.93 ?
C63 C64 1.384(5) y
C63 C66 1.511(5) y
C64 C65 1.365(5) y
C64 H64 0.93 ?
C65 H65 0.93 ?
C66 H66a 0.96 ?
C66 H66b 0.96 ?
C66 H66c 0.96 ?
C67 H67a 0.97 ?
C67 H67b 0.97 ?
O101 C102 1.427(5) y
O101 H101 0.82 ?
C102 H10a 0.96 ?
C102 H10b 0.96 ?
C102 H10c 0.96 ?
O103 C104 1.422(5) y
O103 H103 0.82 ?
C104 H10d 0.96 ?
C104 H10e 0.96 ?
C104 H10f 0.96 ?
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
O10 S1 O12 C17 176.0(2) y
O11 S1 O12 C17 46.9(2) y
C10 S1 O12 C17 -68.7(2) y
O21 S2 O22 C27 -176.2(2) y
O20 S2 O22 C27 -47.1(2) y
C20 S2 O22 C27 68.7(2) y
O31 S3 O32 C37 -173.9(2) y
O30 S3 O32 C37 -44.2(3) y
C30 S3 O32 C37 72.1(3) y
O41 S4 O42 C47 38.0(2) y
O40 S4 O42 C47 168.7(2) y
C40 S4 O42 C47 -77.4(2) y
O51 S5 O52 C57 44.0(3) y
O50 S5 O52 C57 173.9(2) y
C50 S5 O52 C57 -71.6(2) y
O61 S6 O62 C67 -60.0(2) y
O60 S6 O62 C67 69.7(2) y
C60 S6 O62 C67 -175.7(2) y
C3 O1 C2 C1 153.3(2) y
C67 C1 C2 O1 54.8(3) y
C47 C1 C2 O1 -63.2(3) y
C57 C1 C2 O1 177.5(2) y
C2 O1 C3 C4 117.4(3) y
O1 C3 C4 C17 -179.4(2) y
O1 C3 C4 C27 -58.0(3) y
O1 C3 C4 C37 59.3(3) y
O10 S1 C10 C15 60.9(3) y
O11 S1 C10 C15 -165.9(2) y
O12 S1 C10 C15 -49.8(3) y
O10 S1 C10 C11 -119.2(3) y
O11 S1 C10 C11 14.0(3) y
O12 S1 C10 C11 130.1(2) y
C15 C10 C11 C12 0.0(5) y
S1 C10 C11 C12 -179.9(2) y
C10 C11 C12 C13 1.5(5) y
C11 C12 C13 C14 -1.7(5) y
C11 C12 C13 C16 177.5(3) y
C12 C13 C14 C15 0.4(5) y
C16 C13 C14 C15 -178.8(3) y
C13 C14 C15 C10 1.0(5) y
C11 C10 C15 C14 -1.2(5) y
S1 C10 C15 C14 178.7(2) y
S1 O12 C17 C4 175.17(19) y
C27 C4 C17 O12 61.0(3) y
C37 C4 C17 O12 -56.9(3) y
C3 C4 C17 O12 -177.6(2) y
O21 S2 C20 C21 131.8(4) y
O20 S2 C20 C21 -0.9(4) y
O22 S2 C20 C21 -116.8(4) y
O21 S2 C20 C25 -49.1(4) y
O20 S2 C20 C25 178.2(3) y
O22 S2 C20 C25 62.3(3) y
C25 C20 C21 C22 3.5(7) y
S2 C20 C21 C22 -177.4(4) y
C20 C21 C22 C23 -3.4(9) y
C21 C22 C23 C24 2.8(1) y
C21 C22 C23 C26 179.7(5) y
C22 C23 C24 C25 -2.30(11) y
C26 C23 C24 C25 -178.9(5) y
C23 C24 C25 C20 2.5(9) y
C21 C20 C25 C24 -3.1(7) y
S2 C20 C25 C24 177.8(4) y
S2 O22 C27 C4 -167.63(17) y
C17 C4 C27 O22 58.1(3) y
C37 C4 C27 O22 -179.8(2) y
C3 C4 C27 O22 -58.9(3) y
O31 S3 C30 C35 148.4(3) y
O30 S3 C30 C35 13.4(4) y
O32 S3 C30 C35 -102.5(3) y
O31 S3 C30 C31 -34.7(4) y
O30 S3 C30 C31 -169.7(3) y
O32 S3 C30 C31 74.4(4) y
C35 C30 C31 C32 -1.2(7) y
S3 C30 C31 C32 -178.1(4) y
C30 C31 C32 C33 0.4(8) y
C31 C32 C33 C34 -0.1(7) y
C31 C32 C33 C36 178.6(4) y
C32 C33 C34 C35 0.6(6) y
C36 C33 C34 C35 -178.2(4) y
C31 C30 C35 C34 1.6(6) y
S3 C30 C35 C34 178.6(3) y
C33 C34 C35 C30 -1.4(6) y
S3 O32 C37 C4 -171.63(19) y
C17 C4 C37 O32 -55.9(3) y
C27 C4 C37 O32 -177.8(2) y
C3 C4 C37 O32 60.8(3) y
O41 S4 C40 C41 -12.4(3) y
O40 S4 C40 C41 -146.7(3) y
O42 S4 C40 C41 102.7(3) y
O41 S4 C40 C45 169.1(3) y
O40 S4 C40 C45 34.8(3) y
O42 S4 C40 C45 -75.8(3) y
C45 C40 C41 C42 -0.2(6) y
S4 C40 C41 C42 -178.7(3) y
C40 C41 C42 C43 1.7(6) y
C41 C42 C43 C44 -3.0(6) y
C41 C42 C43 C46 177.4(4) y
C42 C43 C44 C45 2.8(7) y
C46 C43 C44 C45 -177.6(4) y
C43 C44 C45 C40 -1.2(7) y
C41 C40 C45 C44 -0.1(6) y
S4 C40 C45 C44 178.4(3) y
S4 O42 C47 C1 167.87(17) y
C2 C1 C47 O42 -62.0(3) y
C67 C1 C47 O42 177.3(2) y
C57 C1 C47 O42 53.7(3) y
O51 S5 C50 C55 -31.1(3) y
O50 S5 C50 C55 -165.3(3) y
O52 S5 C50 C55 85.6(3) y
O51 S5 C50 C51 148.9(3) y
O50 S5 C50 C51 14.7(3) y
O52 S5 C50 C51 -94.5(3) y
C55 C50 C51 C52 -2.1(5) y
S5 C50 C51 C52 177.9(3) y
C50 C51 C52 C53 0.1(6) y
C51 C52 C53 C54 1.7(6) y
C51 C52 C53 C56 -177.8(4) y
C52 C53 C54 C55 -1.6(6) y
C56 C53 C54 C55 177.9(3) y
C53 C54 C55 C50 -0.4(6) y
C51 C50 C55 C54 2.2(5) y
S5 C50 C55 C54 -177.8(3) y
S5 O52 C57 C1 -148.5(2) y
C2 C1 C57 O52 176.8(2) y
C67 C1 C57 O52 -62.0(3) y
C47 C1 C57 O52 57.5(3) y
O61 S6 C60 C61 156.4(3) y
O60 S6 C60 C61 23.5(3) y
O62 S6 C60 C61 -90.2(3) y
O61 S6 C60 C65 -21.4(3) y
O60 S6 C60 C65 -154.2(2) y
O62 S6 C60 C65 92.0(3) y
C65 C60 C61 C62 -0.6(5) y
S6 C60 C61 C62 -178.3(3) y
C60 C61 C62 C63 0.6(6) y
C61 C62 C63 C64 0.0(6) y
C61 C62 C63 C66 -179.7(4) y
C62 C63 C64 C65 -0.8(6) y
C66 C63 C64 C65 179.0(4) y
C63 C64 C65 C60 0.8(6) y
C61 C60 C65 C64 -0.1(5) y
S6 C60 C65 C64 177.6(3) y
S6 O62 C67 C1 -148.91(19) y
C2 C1 C67 O62 57.8(3) y
C47 C1 C67 O62 178.4(2) y
C57 C1 C67 O62 -59.8(3) y
loop_
_cod_related_entry_id
_cod_related_entry_code
_cod_related_entry_database
1 21157397 ChemSpider
|
1501602.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/16/1501602.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_1501602
loop_
_publ_author_name
'Elliott, Emma-Claire'
'Bowkett, Elizabeth R.'
'Maggs, James L.'
'Bacsa, John'
'Park, B. Kevin'
'Regan, Sophie L.'
'O'Neill, Paul M'
'Stachulski, Andrew V.'
_publ_section_title
;
Convenient syntheses of benzo-fluorinated dibenz[b,f]azepines:
rearrangements of isatins, acridines, and indoles.
;
_journal_issue 20
_journal_name_full 'Organic letters'
_journal_page_first 5592
_journal_page_last 5595
_journal_paper_doi 10.1021/ol202318w
_journal_volume 13
_journal_year 2011
_chemical_formula_moiety 'C14 H10 F N'
_chemical_formula_sum 'C14 H10 F N'
_chemical_formula_weight 211.23
_chemical_name_common EB7721
_chemical_name_systematic
;
?
;
_space_group_IT_number 62
_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
_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 8.2094(19)
_cell_length_b 21.264(5)
_cell_length_c 5.9988(13)
_cell_measurement_reflns_used 488
_cell_measurement_temperature 218(2)
_cell_measurement_theta_max 24.2
_cell_measurement_theta_min 2.1
_cell_volume 1047.2(4)
_computing_cell_refinement 'IPDS (Stoe & Cie, 1996)'
_computing_data_collection 'IPDS (Stoe & Cie, 1996)'
_computing_data_reduction 'IPDS (Stoe & Cie, 1996)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 218(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type 'Stoe IPDS'
_diffrn_measurement_method '200\% f scan, \f-incr 2.0 \%, 100 exposures'
_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 0.0537
_diffrn_reflns_av_sigmaI/netI 0.0273
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 24
_diffrn_reflns_limit_k_min -24
_diffrn_reflns_limit_l_max 6
_diffrn_reflns_limit_l_min -6
_diffrn_reflns_number 5675
_diffrn_reflns_theta_full 24.15
_diffrn_reflns_theta_max 24.15
_diffrn_reflns_theta_min 3.53
_exptl_absorpt_coefficient_mu 0.091
_exptl_absorpt_correction_T_max 0.9910
_exptl_absorpt_correction_T_min 0.9559
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'SORTAV (R.H. Blessing, (1989)'
_exptl_crystal_colour brown
_exptl_crystal_density_diffrn 1.340
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 440
_exptl_crystal_size_max 0.50
_exptl_crystal_size_mid 0.30
_exptl_crystal_size_min 0.10
_refine_diff_density_max 0.106
_refine_diff_density_min -0.079
_refine_diff_density_rms 0.022
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.004
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 107
_refine_ls_number_reflns 842
_refine_ls_number_restraints 128
_refine_ls_restrained_S_all 0.956
_refine_ls_R_factor_all 0.0531
_refine_ls_R_factor_gt 0.0359
_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^)+(0.0592P)^2^+0.0559P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0923
_refine_ls_wR_factor_ref 0.0989
_reflns_number_gt 602
_reflns_number_total 842
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file ol202318w_si_002.cif
_cod_data_source_block eb7721
_cod_depositor_comments 'Adding full bibliography for 1501602.cif.'
_cod_original_sg_symbol_H-M Pnma
_cod_database_code 1501602
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, 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
N1 N 0.7087(2) 0.2604(2) 0.2191(3) 0.0492(11) Uani 0.50 1 d PDU A -1
C11 C 0.7580(3) 0.31787(14) 0.1191(5) 0.0425(6) Uani 0.50 1 d PDU A -1
C21 C 0.6976(3) 0.33475(18) -0.0917(5) 0.0402(7) Uani 0.50 1 d PDU A -1
C31 C 0.7351(4) 0.39540(19) -0.1642(6) 0.0522(7) Uani 0.50 1 d PDU A -1
H31 H 0.6987 0.4075 -0.3065 0.063 Uiso 0.50 1 calc PR A -1
C41 C 0.8201(4) 0.43808(19) -0.0439(6) 0.0608(8) Uani 0.50 1 d PDU A -1
H41 H 0.8357 0.4793 -0.0968 0.073 Uiso 0.50 1 calc PR A -1
C51 C 0.8810(5) 0.4199(2) 0.1522(7) 0.0612(7) Uani 0.50 1 d PDU A -1
H51 H 0.9468 0.4477 0.2341 0.073 Uiso 0.50 1 calc PR A -1
C61 C 0.8484(4) 0.3606(2) 0.2363(6) 0.0490(7) Uani 0.50 1 d PDU A -1
H61 H 0.8894 0.3494 0.3771 0.059 Uiso 0.50 1 calc PR A -1
C71 C 0.6016(4) 0.2922(2) -0.2292(5) 0.0496(10) Uani 0.50 1 d PDU A -1
H71 H 0.5362 0.3125 -0.3359 0.060 Uiso 0.50 1 calc PR A -1
C1 C 0.7424(4) 0.20057(18) 0.1237(5) 0.0425(6) Uani 0.50 1 d PDU A -1
C2 C 0.6795(3) 0.18606(18) -0.0897(5) 0.0402(7) Uani 0.50 1 d PDU A -1
C3 C 0.7051(4) 0.12467(19) -0.1668(6) 0.0522(7) Uani 0.50 1 d PDU A -1
H3 H 0.6595 0.1117 -0.3030 0.063 Uiso 0.50 1 calc PR A -1
C4 C 0.7971(5) 0.08331(19) -0.0431(6) 0.0608(8) Uani 0.50 1 d PDU A -1
C5 C 0.8575(5) 0.0977(2) 0.1742(7) 0.0612(7) Uani 0.50 1 d PDU A -1
H5 H 0.9129 0.0678 0.2612 0.073 Uiso 0.50 1 calc PR A -1
C6 C 0.8298(4) 0.1577(2) 0.2484(6) 0.0490(7) Uani 0.50 1 d PDU A -1
H6 H 0.8713 0.1700 0.3878 0.059 Uiso 0.50 1 calc PR A -1
C7 C 0.5898(3) 0.2297(2) -0.2307(4) 0.0496(10) Uani 0.50 1 d PDU A -1
H7 H 0.5162 0.2120 -0.3331 0.060 Uiso 0.50 1 calc PR A -1
F1 F 0.8312(3) 0.02008(10) -0.1164(4) 0.1162(8) Uani 0.50 1 d PU A -1
H1 H 0.7483(16) 0.2601(2) 0.3749(8) 0.072(7) Uiso 0.50 1 d PD B -1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
N1 0.0537(9) 0.064(3) 0.0300(8) -0.0065(13) 0.0026(7) 0.0064(13)
C11 0.0283(7) 0.0637(18) 0.0356(7) 0.0028(12) 0.0051(5) 0.0068(10)
C21 0.0270(7) 0.054(2) 0.0398(7) -0.0011(9) 0.0040(5) -0.0045(9)
C31 0.0387(11) 0.062(2) 0.0560(8) 0.0019(12) 0.0001(7) -0.0015(9)
C41 0.0653(11) 0.033(3) 0.0843(13) 0.0004(11) 0.0045(9) -0.0009(10)
C51 0.0545(11) 0.062(2) 0.0668(11) 0.0003(14) 0.0039(9) 0.0053(12)
C61 0.0387(8) 0.063(2) 0.0451(8) -0.0005(12) -0.0006(6) -0.0006(11)
C71 0.0315(6) 0.082(3) 0.0356(6) 0.0013(10) -0.0050(5) -0.0006(8)
C1 0.0283(7) 0.0637(18) 0.0356(7) 0.0028(12) 0.0051(5) 0.0068(10)
C2 0.0270(7) 0.054(2) 0.0398(7) -0.0011(9) 0.0040(5) -0.0045(9)
C3 0.0387(11) 0.062(2) 0.0560(8) 0.0019(12) 0.0001(7) -0.0015(9)
C4 0.0653(11) 0.033(3) 0.0843(13) 0.0004(11) 0.0045(9) -0.0009(10)
C5 0.0545(11) 0.062(2) 0.0668(11) 0.0003(14) 0.0039(9) 0.0053(12)
C6 0.0387(8) 0.063(2) 0.0451(8) -0.0005(12) -0.0006(6) -0.0006(11)
C7 0.0315(6) 0.082(3) 0.0356(6) 0.0013(10) -0.0050(5) -0.0006(8)
F1 0.150(2) 0.0800(14) 0.1189(17) -0.0176(13) -0.0122(15) -0.0238(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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
C1 N1 C11 123.0(2) yes
C11 N1 H1 108.1(5) no
C1 N1 H1 108.1(5) no
N1 C1 C6 118.3(3) yes
N1 C1 C2 119.2(3) yes
C2 C1 C6 122.4(3) no
C1 C2 C7 124.9(3) no
C3 C2 C7 118.6(3) no
C1 C2 C3 116.6(3) no
C2 C3 C4 120.0(3) no
F1 C4 C5 114.3(3) yes
F1 C4 C3 122.5(3) yes
C3 C4 C5 123.1(4) no
C4 C5 C6 116.0(4) no
C1 C6 C5 121.7(3) no
C2 C7 C71 126.5(3) no
N1 C11 C21 120.0(3) yes
N1 C11 C61 120.6(3) yes
C21 C11 C61 119.0(3) no
C11 C21 C31 116.0(3) no
C31 C21 C71 121.1(3) no
C11 C21 C71 122.8(3) no
C21 C31 C41 124.6(3) no
C31 C41 C51 118.0(4) no
C41 C51 C61 120.8(4) no
C11 C61 C51 121.5(3) no
C7 C71 C21 131.5(3) no
C2 C3 H3 120.00 no
C4 C3 H3 120.00 no
C4 C5 H5 122.00 no
C6 C5 H5 122.00 no
C1 C6 H6 119.00 no
C5 C6 H6 119.00 no
C2 C7 H7 117.00 no
C71 C7 H7 117.00 no
C21 C31 H31 118.00 no
C41 C31 H31 118.00 no
C31 C41 H41 121.00 no
C51 C41 H41 121.00 no
C41 C51 H51 120.00 no
C61 C51 H51 120.00 no
C11 C61 H61 119.00 no
C51 C61 H61 119.00 no
C7 C71 H71 114.00 no
C21 C71 H71 114.00 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
F1 C4 1.442(5) yes
N1 C1 1.422(5) yes
N1 C11 1.420(5) yes
N1 H1 0.990(7) no
C1 C6 1.380(5) no
C1 C2 1.414(4) no
C2 C7 1.456(5) no
C2 C3 1.401(5) no
C3 C4 1.376(5) no
C4 C5 1.428(6) no
C5 C6 1.370(6) no
C7 C71 1.333(6) no
C11 C61 1.368(5) no
C11 C21 1.405(4) no
C21 C31 1.395(5) no
C21 C71 1.456(5) no
C31 C41 1.353(5) no
C41 C51 1.335(6) no
C51 C61 1.384(6) no
C3 H3 0.9400 no
C5 H5 0.9400 no
C6 H6 0.9400 no
C7 H7 0.9400 no
C31 H31 0.9400 no
C41 H41 0.9400 no
C51 H51 0.9400 no
C61 H61 0.9400 no
C71 H71 0.9400 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
_geom_torsion_publ_flag
C11 N1 C1 C2 -60.9(4) no
C11 N1 C1 C6 122.0(3) no
C1 N1 C11 C21 62.4(3) no
C1 N1 C11 C61 -125.4(3) no
N1 C1 C2 C3 -174.8(3) no
N1 C1 C2 C7 4.4(4) no
C6 C1 C2 C3 2.3(5) no
C6 C1 C2 C7 -178.5(3) no
N1 C1 C6 C5 175.5(3) no
C2 C1 C6 C5 -1.6(5) no
C1 C2 C3 C4 -4.3(5) no
C7 C2 C3 C4 176.4(3) no
C1 C2 C7 C71 26.5(4) no
C3 C2 C7 C71 -154.3(3) no
C2 C3 C4 F1 -178.4(3) no
C2 C3 C4 C5 6.0(6) no
F1 C4 C5 C6 179.0(3) no
C3 C4 C5 C6 -5.0(6) no
C4 C5 C6 C1 2.7(6) no
C2 C7 C71 C21 -1.9(5) no
N1 C11 C21 C31 171.8(3) no
N1 C11 C21 C71 -8.3(4) no
C61 C11 C21 C31 -0.5(4) no
C61 C11 C21 C71 179.4(3) no
N1 C11 C61 C51 -172.1(3) no
C21 C11 C61 C51 0.2(5) no
C11 C21 C31 C41 -1.8(5) no
C71 C21 C31 C41 178.3(3) no
C11 C21 C71 C7 -22.2(5) no
C31 C21 C71 C7 157.7(3) no
C21 C31 C41 C51 4.3(5) no
C31 C41 C51 C61 -4.4(6) no
C41 C51 C61 C11 2.3(6) no
|
1501603.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/16/1501603.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_1501603
loop_
_publ_author_name
'Olivier Lebel'
'Thierry Maris'
'James D. Wuest'
_publ_section_title
;
Hydrogen-Bonded networks in crystals built from bis(biguanides) and their
salts
;
_journal_name_full 'Can J. Chem'
_journal_page_first 1426
_journal_page_last 1433
_journal_paper_doi 10.1139/v06-115
_journal_volume 84
_journal_year 2006
_chemical_formula_moiety 'C10 H18 N10, 0.5(H2 O), 0.5(H2 O), 2(Cl)'
_chemical_formula_sum 'C10 H20 Cl2 N10 O'
_chemical_formula_weight 367.26
_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 105.66(3)
_cell_angle_beta 95.65(3)
_cell_angle_gamma 102.12(2)
_cell_formula_units_Z 2
_cell_length_a 5.8749(8)
_cell_length_b 12.036(5)
_cell_length_c 13.084(5)
_cell_measurement_reflns_used 25
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 30.00
_cell_measurement_theta_min 15.00
_cell_volume 859.1(5)
_computing_cell_refinement 'CAD4 Program (Nonius 1989)'
_computing_data_collection 'CAD4 Program (Nonius 1989)'
_computing_data_reduction 'Local Program'
_computing_molecular_graphics 'SHELXTL (Bruker, 1997)'
_computing_publication_material 'UdMX (local program)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type Enraf-Nonius-CAD4
_diffrn_measurement_method \w/2\q
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'Sealed Tube'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.000
_diffrn_reflns_av_sigmaI/netI 0.0255
_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 15
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_number 6433
_diffrn_reflns_theta_full 70.01
_diffrn_reflns_theta_max 70.01
_diffrn_reflns_theta_min 3.56
_diffrn_standards_decay_% 0.00
_diffrn_standards_interval_time 60
_diffrn_standards_number 5
_exptl_absorpt_coefficient_mu 3.591
_exptl_absorpt_correction_T_max 0.6100
_exptl_absorpt_correction_T_min 0.4600
_exptl_absorpt_correction_type analytical
_exptl_absorpt_process_details 'Face indexing'
_exptl_crystal_colour Colourless
_exptl_crystal_density_diffrn 1.420
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 384
_exptl_crystal_size_max 0.25
_exptl_crystal_size_mid 0.25
_exptl_crystal_size_min 0.15
_refine_diff_density_max 0.323
_refine_diff_density_min -0.396
_refine_diff_density_rms 0.082
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.105
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 217
_refine_ls_number_reflns 3241
_refine_ls_number_restraints 3
_refine_ls_restrained_S_all 1.108
_refine_ls_R_factor_all 0.0463
_refine_ls_R_factor_gt 0.0456
_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^)+(0.0700P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1109
_refine_ls_wR_factor_ref 0.1110
_reflns_number_gt 2766
_reflns_number_total 3241
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file deposit.cif
_cod_data_source_block jiw811
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana
;
_cod_original_sg_symbol_H-M P-1
_cod_database_code 1501603
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
Cl1 Cl 0.03621(9) 0.30251(4) 0.26408(4) 0.03474(15) Uani 1 1 d . . .
Cl2 Cl 0.95448(9) 0.76876(5) 0.20941(4) 0.03589(15) Uani 1 1 d . . .
C1 C 0.6450(3) 0.90995(17) 0.66311(16) 0.0286(4) Uani 1 1 d . . .
H1 H 0.7797 0.9181 0.7110 0.034 Uiso 1 1 calc . . .
C2 C 0.6016(3) 0.82790(17) 0.56163(16) 0.0277(4) Uani 1 1 d . . .
H2 H 0.7072 0.7815 0.5414 0.033 Uiso 1 1 calc . . .
C3 C 0.3990(3) 0.81527(17) 0.49018(15) 0.0240(4) Uani 1 1 d . . .
C4 C 0.2454(4) 0.88652(19) 0.52152(16) 0.0301(4) Uani 1 1 d . . .
H4 H 0.1094 0.8782 0.4744 0.036 Uiso 1 1 calc . . .
C5 C 0.2928(4) 0.97039(18) 0.62292(16) 0.0297(4) Uani 1 1 d . . .
H5 H 0.1917 1.0196 0.6424 0.036 Uiso 1 1 calc . . .
C6 C 0.4890(3) 0.98006(17) 0.69374(16) 0.0274(4) Uani 1 1 d . . .
C10 C 0.4170(3) 1.06824(16) 0.87669(14) 0.0221(4) Uani 1 1 d . . .
N10 N 0.5470(3) 1.06681(15) 0.79823(13) 0.0279(4) Uani 1 1 d . . .
H10 H 0.6750 1.1220 0.8113 0.034 Uiso 1 1 calc . . .
C11 C 0.3738(3) 1.18642(16) 1.04412(15) 0.0253(4) Uani 1 1 d . . .
N11 N 0.2204(3) 0.98153(16) 0.85898(14) 0.0319(4) Uani 1 1 d . . .
H11A H 0.1410 0.9771 0.9102 0.038 Uiso 1 1 calc . . .
H11B H 0.1733 0.9302 0.7964 0.038 Uiso 1 1 calc . . .
N12 N 0.5081(3) 1.15297(15) 0.96998(12) 0.0280(4) Uani 1 1 d . . .
N13 N 0.1357(3) 1.17162(16) 1.02199(13) 0.0313(4) Uani 1 1 d . . .
H13A H 0.0591 1.1957 1.0729 0.038 Uiso 1 1 calc . . .
H13B H 0.0621 1.1382 0.9571 0.038 Uiso 1 1 calc . . .
N14 N 0.4774(3) 1.23818(17) 1.14510(13) 0.0334(4) Uani 1 1 d . . .
H14A H 0.6275 1.2497 1.1620 0.040 Uiso 1 1 calc . . .
H14B H 0.3948 1.2604 1.1940 0.040 Uiso 1 1 calc . . .
C20 C 0.4189(3) 0.63899(17) 0.33914(14) 0.0238(4) Uani 1 1 d . . .
N20 N 0.3399(3) 0.73683(15) 0.38507(13) 0.0290(4) Uani 1 1 d . . .
H20 H 0.2380 0.7529 0.3430 0.035 Uiso 1 1 calc . . .
C21 C 0.6747(3) 0.52037(16) 0.36249(15) 0.0258(4) Uani 1 1 d . . .
N21 N 0.3512(3) 0.59412(16) 0.23232(13) 0.0325(4) Uani 1 1 d . . .
H21A H 0.3869 0.5301 0.1979 0.039 Uiso 1 1 calc . . .
H21B H 0.2720 0.6293 0.1982 0.039 Uiso 1 1 calc . . .
N22 N 0.5397(3) 0.59481(15) 0.40118(12) 0.0284(4) Uani 1 1 d . . .
N23 N 0.7861(4) 0.52512(16) 0.27994(16) 0.0377(4) Uani 1 1 d . . .
H23A H 0.8719 0.4762 0.2591 0.045 Uiso 1 1 calc . . .
H23B H 0.7726 0.5771 0.2472 0.045 Uiso 1 1 calc . . .
N24 N 0.6989(4) 0.44015(16) 0.41057(15) 0.0375(4) Uani 1 1 d . . .
H24A H 0.7855 0.3921 0.3884 0.045 Uiso 1 1 calc . . .
H24B H 0.6281 0.4355 0.4643 0.045 Uiso 1 1 calc . . .
O1 O 0.3169(6) 0.4450(3) 0.0013(2) 0.0411(7) Uani 0.50 1 d P A 1
H1A H 0.2418 0.3839 -0.0561 0.250 Uiso 0.50 1 d PR A 1
H1B H 0.4533 0.4938 0.0005 0.250 Uiso 0.50 1 d PR A 1
O2 O 0.8391(7) 0.4232(3) 0.0128(3) 0.0472(8) Uani 0.50 1 d PD B 2
H2A H 0.7735 0.3470 -0.0229 0.250 Uiso 0.50 1 d PRD B 2
H2B H 0.9874 0.4347 -0.0004 0.250 Uiso 0.50 1 d PRD 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
Cl1 0.0330(3) 0.0333(3) 0.0345(3) -0.0018(2) 0.0064(2) 0.0161(2)
Cl2 0.0329(3) 0.0379(3) 0.0389(3) 0.0210(2) -0.0019(2) 0.0043(2)
C1 0.0250(9) 0.0278(9) 0.0306(10) 0.0055(8) 0.0021(8) 0.0068(8)
C2 0.0271(10) 0.0274(9) 0.0281(10) 0.0033(8) 0.0033(8) 0.0133(8)
C3 0.0232(9) 0.0256(9) 0.0255(9) 0.0080(7) 0.0072(7) 0.0088(7)
C4 0.0320(10) 0.0329(10) 0.0292(10) 0.0112(8) 0.0022(8) 0.0150(8)
C5 0.0308(10) 0.0328(10) 0.0284(10) 0.0082(8) 0.0091(8) 0.0132(8)
C6 0.0271(10) 0.0270(9) 0.0270(9) 0.0060(8) 0.0085(8) 0.0056(8)
C10 0.0236(9) 0.0258(9) 0.0178(8) 0.0067(7) 0.0024(7) 0.0080(7)
N10 0.0289(8) 0.0284(8) 0.0231(8) 0.0043(7) 0.0072(6) 0.0027(7)
C11 0.0231(9) 0.0229(9) 0.0295(10) 0.0067(7) 0.0047(7) 0.0061(7)
N11 0.0320(9) 0.0327(9) 0.0278(8) 0.0048(7) 0.0092(7) 0.0048(7)
N12 0.0265(8) 0.0318(9) 0.0206(8) 0.0010(6) 0.0037(6) 0.0054(7)
N13 0.0287(9) 0.0390(10) 0.0252(8) 0.0038(7) 0.0067(7) 0.0126(7)
N14 0.0325(9) 0.0427(10) 0.0223(8) 0.0022(7) 0.0058(7) 0.0126(8)
C20 0.0238(9) 0.0261(9) 0.0215(9) 0.0065(7) 0.0052(7) 0.0062(7)
N20 0.0352(9) 0.0285(8) 0.0248(8) 0.0061(7) -0.0002(7) 0.0161(7)
C21 0.0281(9) 0.0199(8) 0.0266(9) 0.0034(7) 0.0033(7) 0.0053(7)
N21 0.0401(10) 0.0306(9) 0.0245(8) 0.0036(7) 0.0022(7) 0.0115(7)
N22 0.0359(9) 0.0305(9) 0.0217(8) 0.0057(7) 0.0080(7) 0.0159(7)
N23 0.0489(11) 0.0332(9) 0.0421(10) 0.0160(8) 0.0256(9) 0.0196(8)
N24 0.0484(11) 0.0355(10) 0.0418(10) 0.0170(8) 0.0208(8) 0.0255(9)
O1 0.0511(19) 0.0408(17) 0.0352(16) 0.0173(14) 0.0057(14) 0.0124(15)
O2 0.059(2) 0.053(2) 0.0389(18) 0.0254(16) 0.0112(16) 0.0147(17)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 '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
C2 C1 C6 120.49(18)
C2 C1 H1 119.8
C6 C1 H1 119.8
C1 C2 C3 119.71(18)
C1 C2 H2 120.1
C3 C2 H2 120.1
C4 C3 C2 119.22(18)
C4 C3 N20 116.24(17)
C2 C3 N20 124.51(17)
C3 C4 C5 120.68(18)
C3 C4 H4 119.7
C5 C4 H4 119.7
C6 C5 C4 119.74(18)
C6 C5 H5 120.1
C4 C5 H5 120.1
C5 C6 C1 120.12(18)
C5 C6 N10 121.56(18)
C1 C6 N10 118.21(18)
N12 C10 N10 115.64(17)
N12 C10 N11 125.65(17)
N10 C10 N11 118.49(17)
C10 N10 C6 124.95(17)
C10 N10 H10 117.5
C6 N10 H10 117.5
N14 C11 N12 118.39(17)
N14 C11 N13 117.39(17)
N12 C11 N13 124.22(18)
C10 N11 H11A 120.0
C10 N11 H11B 120.0
H11A N11 H11B 120.0
C10 N12 C11 121.65(17)
C11 N13 H13A 120.0
C11 N13 H13B 120.0
H13A N13 H13B 120.0
C11 N14 H14A 120.0
C11 N14 H14B 120.0
H14A N14 H14B 120.0
N22 C20 N21 126.48(18)
N22 C20 N20 119.09(17)
N21 C20 N20 114.34(17)
C20 N20 C3 130.10(16)
C20 N20 H20 114.9
C3 N20 H20 114.9
N24 C21 N23 118.47(18)
N24 C21 N22 117.83(18)
N23 C21 N22 123.69(18)
C20 N21 H21A 120.0
C20 N21 H21B 120.0
H21A N21 H21B 120.0
C20 N22 C21 122.29(16)
C21 N23 H23A 120.0
C21 N23 H23B 120.0
H23A N23 H23B 120.0
C21 N24 H24A 120.0
C21 N24 H24B 120.0
H24A N24 H24B 120.0
H1A O1 H1B 122.2
H2A O2 H2B 104.1
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 C2 1.387(3)
C1 C6 1.388(3)
C1 H1 0.9300
C2 C3 1.393(3)
C2 H2 0.9300
C3 C4 1.388(3)
C3 N20 1.404(3)
C4 C5 1.394(3)
C4 H4 0.9300
C5 C6 1.370(3)
C5 H5 0.9300
C6 N10 1.436(3)
C10 N12 1.337(2)
C10 N10 1.337(2)
C10 N11 1.337(3)
N10 H10 0.8600
C11 N14 1.320(3)
C11 N12 1.341(2)
C11 N13 1.364(2)
N11 H11A 0.8600
N11 H11B 0.8600
N13 H13A 0.8600
N13 H13B 0.8600
N14 H14A 0.8600
N14 H14B 0.8600
C20 N22 1.313(2)
C20 N21 1.340(2)
C20 N20 1.366(2)
N20 H20 0.8600
C21 N24 1.310(3)
C21 N23 1.325(3)
C21 N22 1.349(2)
N21 H21A 0.8600
N21 H21B 0.8600
N23 H23A 0.8600
N23 H23B 0.8600
N24 H24A 0.8600
N24 H24B 0.8600
O1 H1A 0.8937
O1 H1B 0.8913
O2 H2A 0.8902
O2 H2B 0.8949
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N10 H10 Cl2 0.86 2.38 3.1992(19) 160.3 2_776
N11 H11B Cl1 0.86 2.67 3.307(2) 131.5 2_566
N11 H11A N13 0.86 2.41 2.843(3) 111.7 .
N11 H11A N13 0.86 2.56 3.282(3) 142.2 2_577
N13 H13A Cl1 0.86 2.52 3.304(2) 152.6 1_566
N13 H13B N11 0.86 2.39 2.843(3) 113.0 .
N13 H13B Cl2 0.86 2.71 3.313(2) 128.7 2_676
N14 H14A Cl1 0.86 2.49 3.328(2) 163.5 1_666
N14 H14B Cl1 0.86 2.47 3.2755(19) 155.6 1_566
N20 H20 Cl2 0.86 2.37 3.2209(19) 171.4 1_455
N21 H21A O1 0.86 2.46 3.033(4) 125.1 .
N21 H21B O2 0.86 2.64 3.227(4) 126.5 2_665
N21 H21B Cl2 0.86 2.75 3.493(2) 145.7 1_455
N23 H23A Cl1 0.86 2.49 3.285(2) 153.5 1_655
N23 H23B Cl2 0.86 2.53 3.294(2) 148.8 .
N24 H24B N22 0.86 2.18 3.033(3) 173.6 2_666
N24 H24A Cl1 0.86 2.48 3.280(2) 154.3 1_655
O1 H1A Cl2 0.89 2.32 3.216(4) 177.5 2_665
O1 H1B O1 0.89 1.40 2.285(7) 170.9 2_665
O2 H2A N12 0.89 2.49 3.289(4) 149.0 1_544
O2 H2B O2 0.89 1.86 2.470(7) 124.0 2_765
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
C6 C1 C2 C3 -0.4(3)
C1 C2 C3 C4 0.9(3)
C1 C2 C3 N20 178.75(18)
C2 C3 C4 C5 0.4(3)
N20 C3 C4 C5 -177.67(18)
C3 C4 C5 C6 -2.1(3)
C4 C5 C6 C1 2.6(3)
C4 C5 C6 N10 178.78(19)
C2 C1 C6 C5 -1.3(3)
C2 C1 C6 N10 -177.66(18)
N12 C10 N10 C6 176.64(17)
N11 C10 N10 C6 1.7(3)
C5 C6 N10 C10 64.8(3)
C1 C6 N10 C10 -119.0(2)
N10 C10 N12 C11 161.11(18)
N11 C10 N12 C11 -24.3(3)
N14 C11 N12 C10 157.59(18)
N13 C11 N12 C10 -23.1(3)
N22 C20 N20 C3 12.5(3)
N21 C20 N20 C3 -170.80(19)
C4 C3 N20 C20 -163.1(2)
C2 C3 N20 C20 18.9(3)
N21 C20 N22 C21 21.6(3)
N20 C20 N22 C21 -162.14(18)
N24 C21 N22 C20 -149.0(2)
N23 C21 N22 C20 32.0(3)
|
1501604.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/16/1501604.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_1501604
loop_
_publ_author_name
'Olivier Lebel'
'Thierry Maris'
'James D. Wuest'
_publ_section_title
;
Hydrogen-Bonded networks in crystals built from bis(biguanides) and their
salts
;
_journal_name_full 'Can J. Chem'
_journal_page_first 1426
_journal_page_last 1433
_journal_paper_doi 10.1139/v06-115
_journal_volume 84
_journal_year 2006
_chemical_compound_source 'Synthesized by the authors. See text'
_chemical_formula_moiety 'C10 H18 N10, 3(H2 O), 2(Cl)'
_chemical_formula_sum 'C10 H24 Cl2 N10 O3'
_chemical_formula_weight 403.29
_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 82.983(2)
_cell_angle_beta 71.193(2)
_cell_angle_gamma 73.759(2)
_cell_formula_units_Z 2
_cell_length_a 9.3537(3)
_cell_length_b 9.6015(3)
_cell_length_c 11.4402(4)
_cell_measurement_reflns_used 3859
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 70.00
_cell_measurement_theta_min 4.08
_cell_volume 933.19(5)
_computing_cell_refinement 'SMART (Bruker, 1999)'
_computing_data_collection 'SMART (Bruker, 1999)'
_computing_data_reduction 'SAINT (Bruker, 1999)'
_computing_molecular_graphics 'SHELXTL (Bruker, 1997)'
_computing_publication_material 'UdMX (local program)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type 'Bruker AXS Smart 2K/Platform'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'Sealed Tube'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.029
_diffrn_reflns_av_sigmaI/netI 0.0555
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 14
_diffrn_reflns_limit_l_min -12
_diffrn_reflns_number 4610
_diffrn_reflns_theta_full 70.00
_diffrn_reflns_theta_max 70.00
_diffrn_reflns_theta_min 4.08
_diffrn_standards_decay_% 0.91
_diffrn_standards_number 80
_exptl_absorpt_coefficient_mu 3.437
_exptl_absorpt_correction_T_max 0.4230
_exptl_absorpt_correction_T_min 0.1860
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Sadabs (Sheldrick,1996)'
_exptl_crystal_colour Colourless
_exptl_crystal_density_diffrn 1.435
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 424
_exptl_crystal_size_max 0.40
_exptl_crystal_size_mid 0.35
_exptl_crystal_size_min 0.25
_refine_diff_density_max 0.913
_refine_diff_density_min -0.626
_refine_diff_density_rms 0.139
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.058
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 226
_refine_ls_number_reflns 3017
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.058
_refine_ls_R_factor_all 0.0818
_refine_ls_R_factor_gt 0.0745
_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^)+(0.1841P)^2^+0.2654P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2142
_refine_ls_wR_factor_ref 0.2351
_reflns_number_gt 2583
_reflns_number_total 3545
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file deposit.cif
_cod_data_source_block jiw814
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana
;
_cod_original_sg_symbol_H-M P-1
_cod_database_code 1501604
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
C1 C 0.6877(4) 1.0347(4) 0.0834(3) 0.0151(8) Uani 1 1 d .
Cl1 Cl 0.30830(10) 0.30519(9) 0.06107(8) 0.0184(3) Uani 1 1 d .
Cl2 Cl 0.23365(11) 0.37996(9) 0.53283(8) 0.0216(3) Uani 1 1 d .
N1 N 0.7520(4) 1.0292(3) -0.0392(3) 0.0187(7) Uani 1 1 d .
H1A H 0.7299 0.9716 -0.0813 0.028 Uiso 1 1 calc .
H1B H 0.8165 1.0832 -0.0778 0.028 Uiso 1 1 calc .
C2 C 0.6404(4) 1.1806(4) 0.2476(3) 0.0154(8) Uani 1 1 d .
N2 N 0.5905(4) 0.9525(3) 0.1403(3) 0.0202(7) Uani 1 1 d .
H2A H 0.5691 0.8952 0.0973 0.030 Uiso 1 1 calc .
H2B H 0.5475 0.9553 0.2210 0.030 Uiso 1 1 calc .
C3 C 0.8598(4) 1.1413(4) 0.3316(3) 0.0166(8) Uani 1 1 d .
N3 N 0.7328(4) 1.1179(3) 0.1438(3) 0.0158(7) Uani 1 1 d .
C4 C 0.9480(4) 1.2261(4) 0.3516(3) 0.0175(8) Uani 1 1 d .
H4 H 0.9082 1.3284 0.3564 0.021 Uiso 1 1 calc .
N4 N 0.4843(4) 1.2321(4) 0.2748(3) 0.0207(7) Uani 1 1 d .
H4A H 0.4370 1.2251 0.2214 0.031 Uiso 1 1 calc .
H4B H 0.4296 1.2728 0.3459 0.031 Uiso 1 1 calc .
C5 C 1.0953(4) 1.1594(4) 0.3644(3) 0.0182(8) Uani 1 1 d .
H5 H 1.1548 1.2164 0.3803 0.022 Uiso 1 1 calc .
N5 N 0.7056(4) 1.2096(3) 0.3285(3) 0.0172(7) Uani 1 1 d .
H5A H 0.6481 1.2758 0.3833 0.021 Uiso 1 1 calc .
C6 C 1.1560(4) 1.0098(4) 0.3540(3) 0.0163(8) Uani 1 1 d .
H6 H 1.2571 0.9649 0.3615 0.020 Uiso 1 1 calc .
N6 N 1.1287(4) 0.7742(3) 0.3300(3) 0.0168(7) Uani 1 1 d .
H6A H 1.1804 0.7337 0.3827 0.020 Uiso 1 1 calc .
C7 C 1.0669(5) 0.9267(4) 0.3325(3) 0.0175(8) Uani 1 1 d .
N7 N 1.1549(4) 0.5444(3) 0.2782(3) 0.0192(7) Uani 1 1 d .
H7A H 1.1560 0.4828 0.2267 0.029 Uiso 1 1 calc .
H7B H 1.1803 0.5120 0.3461 0.029 Uiso 1 1 calc .
C8 C 0.9183(4) 0.9925(4) 0.3228(3) 0.0153(8) Uani 1 1 d .
H8 H 0.8570 0.9353 0.3100 0.018 Uiso 1 1 calc .
N8 N 1.0744(4) 0.7465(3) 0.1530(3) 0.0165(7) Uani 1 1 d .
C9 C 1.1149(4) 0.6861(4) 0.2535(3) 0.0160(8) Uani 1 1 d .
N9 N 0.8987(4) 0.6084(4) 0.1594(3) 0.0207(7) Uani 1 1 d .
H9A H 0.8778 0.5933 0.2399 0.031 Uiso 1 1 calc .
H9B H 0.8531 0.5719 0.1186 0.031 Uiso 1 1 calc .
C10 C 1.0000(4) 0.6872(4) 0.0988(3) 0.0160(8) Uani 1 1 d .
N10 N 1.0228(4) 0.7155(3) -0.0222(3) 0.0192(7) Uani 1 1 d .
H10A H 1.0846 0.7713 -0.0625 0.029 Uiso 1 1 calc .
H10B H 0.9760 0.6785 -0.0615 0.029 Uiso 1 1 calc .
O1 O 0.3839(3) 0.6383(3) 0.4369(3) 0.0274(7) Uani 1 1 d D
H1X H 0.362(6) 0.555(3) 0.469(3) 0.041 Uiso 1 1 d D
H1Y H 0.428(6) 0.627(5) 0.3561(10) 0.041 Uiso 1 1 d D
O2 O 0.5316(4) 0.8991(4) 0.4057(3) 0.0410(9) Uani 1 1 d D
H2X H 0.593(5) 0.810(2) 0.409(6) 0.061 Uiso 1 1 d D
H2Y H 0.591(5) 0.961(4) 0.395(6) 0.061 Uiso 1 1 d D
O3 O 0.5518(5) 0.5481(4) 0.1957(3) 0.0449(9) Uani 1 1 d D
H3X H 0.590(7) 0.599(5) 0.128(3) 0.067 Uiso 1 1 d D
H3Y H 0.516(7) 0.484(5) 0.172(5) 0.067 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
C1 0.0192(18) 0.0159(16) 0.0097(17) 0.0046(15) -0.0090(13) -0.0002(15)
Cl1 0.0232(6) 0.0204(5) 0.0130(5) 0.0001(4) -0.0075(4) -0.0056(4)
Cl2 0.0291(6) 0.0210(5) 0.0129(5) 0.0008(4) -0.0059(4) -0.0048(4)
N1 0.0270(17) 0.0213(15) 0.0087(15) -0.0011(13) -0.0050(12) -0.0079(14)
C2 0.0197(18) 0.0145(16) 0.0134(18) 0.0020(15) -0.0063(14) -0.0059(15)
N2 0.0297(18) 0.0201(15) 0.0114(16) -0.0026(13) -0.0052(13) -0.0078(14)
C3 0.0176(17) 0.0282(19) 0.0050(16) 0.0040(15) -0.0051(13) -0.0072(15)
N3 0.0228(16) 0.0165(14) 0.0089(15) 0.0020(13) -0.0058(12) -0.0062(13)
C4 0.0240(19) 0.0200(17) 0.0095(17) 0.0004(15) -0.0028(14) -0.0101(16)
N4 0.0188(16) 0.0301(17) 0.0146(16) -0.0051(15) -0.0066(12) -0.0050(14)
C5 0.0228(19) 0.0227(18) 0.0111(17) -0.0019(16) -0.0041(14) -0.0098(16)
N5 0.0188(16) 0.0196(15) 0.0109(15) -0.0081(13) -0.0045(12) 0.0021(13)
C6 0.0181(17) 0.0256(18) 0.0075(16) 0.0039(15) -0.0072(13) -0.0074(16)
N6 0.0219(16) 0.0202(15) 0.0111(16) 0.0021(13) -0.0099(12) -0.0054(13)
C7 0.0252(18) 0.0225(18) 0.0057(16) 0.0013(15) -0.0038(13) -0.0095(16)
N7 0.0302(17) 0.0170(14) 0.0123(16) -0.0015(13) -0.0110(13) -0.0034(13)
C8 0.0206(18) 0.0193(17) 0.0088(16) -0.0015(15) -0.0047(13) -0.0090(15)
N8 0.0245(16) 0.0188(15) 0.0076(15) 0.0002(13) -0.0069(12) -0.0056(13)
C9 0.0170(17) 0.0222(18) 0.0108(18) 0.0061(15) -0.0055(13) -0.0094(15)
N9 0.0266(17) 0.0252(16) 0.0144(16) 0.0011(14) -0.0096(13) -0.0102(14)
C10 0.0169(17) 0.0162(15) 0.0132(18) -0.0008(15) -0.0059(13) 0.0003(14)
N10 0.0261(17) 0.0259(16) 0.0097(15) -0.0005(14) -0.0072(12) -0.0112(15)
O1 0.0246(15) 0.0205(13) 0.0399(19) 0.0017(13) -0.0142(13) -0.0061(12)
O2 0.0345(18) 0.059(2) 0.0212(17) -0.0033(17) -0.0118(14) 0.0055(16)
O3 0.057(2) 0.0381(19) 0.0316(19) 0.0037(16) -0.0001(16) -0.0175(18)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
N2 C1 N1 119.3(3)
N2 C1 N3 123.2(3)
N1 C1 N3 117.4(3)
C1 N1 H1A 120.0
C1 N1 H1B 120.0
H1A N1 H1B 120.0
N3 C2 N4 124.8(3)
N3 C2 N5 118.7(3)
N4 C2 N5 116.1(3)
C1 N2 H2A 120.0
C1 N2 H2B 120.0
H2A N2 H2B 120.0
C8 C3 C4 120.5(3)
C8 C3 N5 120.9(3)
C4 C3 N5 118.5(3)
C2 N3 C1 122.4(3)
C3 C4 C5 119.4(3)
C3 C4 H4 120.3
C5 C4 H4 120.3
C2 N4 H4A 120.0
C2 N4 H4B 120.0
H4A N4 H4B 120.0
C6 C5 C4 120.5(3)
C6 C5 H5 119.8
C4 C5 H5 119.8
C2 N5 C3 124.8(3)
C2 N5 H5A 117.6
C3 N5 H5A 117.6
C5 C6 C7 119.4(3)
C5 C6 H6 120.3
C7 C6 H6 120.3
C9 N6 C7 125.4(3)
C9 N6 H6A 117.3
C7 N6 H6A 117.3
C8 C7 C6 120.2(3)
C8 C7 N6 122.0(3)
C6 C7 N6 117.6(3)
C9 N7 H7A 120.0
C9 N7 H7B 120.0
H7A N7 H7B 120.0
C3 C8 C7 120.0(3)
C3 C8 H8 120.0
C7 C8 H8 120.0
C10 N8 C9 122.6(3)
N7 C9 N8 124.7(4)
N7 C9 N6 117.2(3)
N8 C9 N6 117.9(3)
C10 N9 H9A 120.0
C10 N9 H9B 120.0
H9A N9 H9B 120.0
N8 C10 N10 117.1(3)
N8 C10 N9 124.0(3)
N10 C10 N9 118.8(3)
C10 N10 H10A 120.0
C10 N10 H10B 120.0
H10A N10 H10B 120.0
H1X O1 H1Y 107(4)
H2X O2 H2Y 107(4)
H3X O3 H3Y 107(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 N2 1.330(5)
C1 N1 1.337(5)
C1 N3 1.344(5)
N1 H1A 0.8800
N1 H1B 0.8800
C2 N3 1.320(5)
C2 N4 1.347(5)
C2 N5 1.353(5)
N2 H2A 0.8800
N2 H2B 0.8800
C3 C8 1.383(5)
C3 C4 1.392(5)
C3 N5 1.418(5)
C4 C5 1.394(6)
C4 H4 0.9500
N4 H4A 0.8800
N4 H4B 0.8800
C5 C6 1.393(5)
C5 H5 0.9500
N5 H5A 0.8800
C6 C7 1.394(5)
C6 H6 0.9500
N6 C9 1.346(5)
N6 C7 1.416(5)
N6 H6A 0.8800
C7 C8 1.391(5)
N7 C9 1.327(4)
N7 H7A 0.8800
N7 H7B 0.8800
C8 H8 0.9500
N8 C10 1.334(5)
N8 C9 1.341(5)
N9 C10 1.341(5)
N9 H9A 0.8800
N9 H9B 0.8800
C10 N10 1.336(5)
N10 H10A 0.8800
N10 H10B 0.8800
O1 H1X 0.89(3)
O1 H1Y 0.89(3)
O2 H2X 0.89(3)
O2 H2Y 0.89(3)
O3 H3X 0.89(3)
O3 H3Y 0.89(3)
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A Cl1 0.88 2.75 3.463(3) 138.8 2_665
N1 H1B N8 0.88 2.12 2.979(4) 166.6 2_775
N2 H2A Cl1 0.88 2.57 3.317(3) 143.9 2_665
N2 H2B O2 0.88 2.08 2.913(5) 156.6 .
N4 H4A Cl1 0.88 2.44 3.272(3) 157.5 1_565
N4 H4B Cl2 0.88 2.44 3.305(3) 168.6 1_565
N5 H5A O1 0.88 2.21 2.977(4) 145.5 2_676
N6 H6A O1 0.88 2.12 2.940(4) 154.9 1_655
N7 H7A Cl1 0.88 2.49 3.280(3) 149.1 1_655
N7 H7B Cl2 0.88 2.47 3.336(3) 168.8 1_655
N9 H9B Cl1 0.88 2.88 3.540(3) 132.9 2_665
N9 H9A Cl2 0.88 2.49 3.340(3) 163.6 2_666
N10 H10B Cl1 0.88 2.62 3.329(3) 138.6 2_665
N10 H10A N3 0.88 2.16 3.028(4) 169.0 2_775
O1 H1X Cl2 0.89(3) 2.25(2) 3.102(3) 161(5) .
O1 H1Y O3 0.89(3) 1.94(2) 2.803(5) 164(5) .
O2 H2X Cl2 0.89(3) 2.27(2) 3.121(4) 160(6) 2_666
O3 H3X Cl1 0.89(3) 2.26(2) 3.142(3) 170(5) 2_665
O3 H3Y N4 0.89(3) 2.60(4) 3.233(5) 128(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
N4 C2 N3 C1 -34.3(6)
N5 C2 N3 C1 152.8(3)
N2 C1 N3 C2 -33.0(5)
N1 C1 N3 C2 151.1(3)
C8 C3 C4 C5 -0.9(5)
N5 C3 C4 C5 175.2(3)
C3 C4 C5 C6 1.7(5)
N3 C2 N5 C3 -20.3(5)
N4 C2 N5 C3 166.1(3)
C8 C3 N5 C2 -45.1(5)
C4 C3 N5 C2 138.8(4)
C4 C5 C6 C7 -1.0(5)
C5 C6 C7 C8 -0.6(5)
C5 C6 C7 N6 -176.3(3)
C9 N6 C7 C8 41.9(5)
C9 N6 C7 C6 -142.5(4)
C4 C3 C8 C7 -0.7(5)
N5 C3 C8 C7 -176.6(3)
C6 C7 C8 C3 1.4(5)
N6 C7 C8 C3 176.9(3)
C10 N8 C9 N7 32.5(6)
C10 N8 C9 N6 -153.2(3)
C7 N6 C9 N7 -168.2(3)
C7 N6 C9 N8 17.2(5)
C9 N8 C10 N10 -152.2(4)
C9 N8 C10 N9 31.5(6)
|
1501605.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/16/1501605.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_1501605
loop_
_publ_author_name
'Olivier Lebel'
'Thierry Maris'
'James D. Wuest'
_publ_section_title
;
Hydrogen-Bonded networks in crystals built from bis(biguanides) and their
salts
;
_journal_name_full 'Can J. Chem'
_journal_page_first 1426
_journal_page_last 1433
_journal_paper_doi 10.1139/v06-115
_journal_volume 84
_journal_year 2006
_chemical_formula_moiety 'C10 H16 N10, H2 O'
_chemical_formula_sum 'C10 H18 N10 O'
_chemical_formula_weight 294.34
_chemical_name_systematic
;
?
;
_space_group_IT_number 2
_symmetry_cell_setting triclinic
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 88.090(7)
_cell_angle_beta 87.280(7)
_cell_angle_gamma 62.735(6)
_cell_formula_units_Z 6
_cell_length_a 10.0311(16)
_cell_length_b 10.8820(18)
_cell_length_c 21.127(3)
_cell_measurement_reflns_used 10825
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 58.01
_cell_measurement_theta_min 2.64
_cell_volume 2047.5(6)
_computing_cell_refinement 'SMART (Bruker, 1999)'
_computing_data_collection 'SMART (Bruker, 1999)'
_computing_data_reduction 'SAINT (Bruker, 1999)'
_computing_molecular_graphics 'SHELXTL (Bruker, 1997)'
_computing_publication_material 'UdMX (local program)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.929
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_device_type 'Bruker Smart 2000'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'X-ray Sealed Tube'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.070
_diffrn_reflns_av_sigmaI/netI 0.1616
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 23
_diffrn_reflns_limit_l_min -23
_diffrn_reflns_number 34030
_diffrn_reflns_theta_full 59.02
_diffrn_reflns_theta_max 58.01
_diffrn_reflns_theta_min 2.09
_diffrn_standards_decay_% 0.00
_diffrn_standards_interval_time 1440
_diffrn_standards_number 45
_exptl_absorpt_coefficient_mu 0.863
_exptl_absorpt_correction_T_max 0.9914
_exptl_absorpt_correction_T_min 0.8463
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Twinabs (Sheldrick, 2001)'
_exptl_crystal_colour Colorless
_exptl_crystal_density_diffrn 1.432
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 936
_exptl_crystal_size_max 0.20
_exptl_crystal_size_mid 0.07
_exptl_crystal_size_min 0.01
_refine_diff_density_max 0.318
_refine_diff_density_min -0.360
_refine_diff_density_rms 0.077
_refine_ls_extinction_coef 0.0005(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method SHELXL
_refine_ls_goodness_of_fit_ref 1.012
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 588
_refine_ls_number_reflns 6951
_refine_ls_number_restraints 514
_refine_ls_restrained_S_all 1.485
_refine_ls_R_factor_all 0.1294
_refine_ls_R_factor_gt 0.0600
_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^)+(0.0249P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0903
_refine_ls_wR_factor_ref 0.1012
_reflns_number_gt 3715
_reflns_number_total 6951
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file deposit.cif
_cod_data_source_block jiw845
_cod_original_sg_symbol_H-M P-1
_cod_database_code 1501605
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
C1 C 0.960(2) -0.3136(19) 0.5361(8) 0.023(5) Uani 1 1 d U
N1 N 0.9810(14) -0.4151(14) 0.5773(6) 0.027(4) Uani 1 1 d U
H1A H 1.0695 -0.4877 0.5795 0.033 Uiso 1 1 calc .
H1B H 0.9060 -0.4096 0.6025 0.033 Uiso 1 1 calc .
C2 C 1.0612(19) -0.2308(18) 0.4532(8) 0.023(5) Uani 1 1 d U
N2 N 0.8247(15) -0.2035(14) 0.5388(6) 0.027(4) Uani 1 1 d U
H2A H 0.7558 -0.2018 0.5666 0.032 Uiso 1 1 calc .
H2B H 0.8043 -0.1330 0.5127 0.032 Uiso 1 1 calc .
C3 C 0.9337(17) -0.0576(18) 0.3794(7) 0.020(4) Uani 1 1 d U
N3 N 1.0786(14) -0.3281(14) 0.4993(6) 0.019(4) Uani 1 1 d U
C4 C 0.9420(18) 0.0626(19) 0.3934(7) 0.028(5) Uani 1 1 d U
H4 H 0.9542 0.0800 0.4359 0.033 Uiso 1 1 calc .
N4 N 1.1937(14) -0.2280(14) 0.4379(6) 0.032(4) Uani 1 1 d U
H4A H 1.1969 -0.1697 0.4087 0.039 Uiso 1 1 calc .
H4B H 1.2757 -0.2844 0.4573 0.039 Uiso 1 1 calc .
C5 C 0.9329(17) 0.1567(17) 0.3467(8) 0.024(5) Uani 1 1 d U
H5 H 0.9397 0.2379 0.3571 0.029 Uiso 1 1 calc .
N5 N 0.9349(15) -0.1524(14) 0.4275(6) 0.023(4) Uani 1 1 d U
C6 C 0.9136(17) 0.1330(18) 0.2840(7) 0.021(4) Uani 1 1 d U
N6 N 0.9191(14) 0.2260(14) 0.2365(6) 0.022(4) Uani 1 1 d U
C7 C 0.9028(18) 0.0134(19) 0.2698(7) 0.026(5) Uani 1 1 d U
H7 H 0.8886 -0.0033 0.2274 0.031 Uiso 1 1 calc .
N7 N 0.6840(15) 0.2668(14) 0.1961(6) 0.031(4) Uani 1 1 d U
H7A H 0.6630 0.2233 0.2278 0.037 Uiso 1 1 calc .
H7B H 0.6204 0.3041 0.1654 0.037 Uiso 1 1 calc .
C8 C 0.9128(18) -0.0805(17) 0.3173(8) 0.024(5) Uani 1 1 d .
H8 H 0.9052 -0.1615 0.3073 0.028 Uiso 1 1 calc .
N8 N 0.8204(14) 0.3578(14) 0.1448(6) 0.022(4) Uani 1 1 d U
C9 C 0.816(2) 0.2764(17) 0.1943(8) 0.025(5) Uani 1 1 d .
N9 N 1.0848(15) 0.2720(15) 0.1444(6) 0.033(4) Uani 1 1 d U
H9A H 1.0957 0.2148 0.1764 0.040 Uiso 1 1 calc .
H9B H 1.1638 0.2761 0.1265 0.040 Uiso 1 1 calc .
C10 C 0.950(2) 0.3520(18) 0.1231(8) 0.023(5) Uani 1 1 d .
N10 N 0.9446(14) 0.4318(15) 0.0727(6) 0.030(4) Uani 1 1 d U
H10A H 1.0281 0.4288 0.0560 0.036 Uiso 1 1 calc .
H10B H 0.8579 0.4872 0.0564 0.036 Uiso 1 1 calc .
C11 C 0.4177(19) 1.3286(18) 0.3742(7) 0.022(5) Uani 1 1 d U
N11 N 0.3653(14) 1.4264(14) 0.4209(6) 0.031(4) Uani 1 1 d U
H11A H 0.2702 1.4637 0.4335 0.038 Uiso 1 1 calc .
H11B H 0.4269 1.4516 0.4382 0.038 Uiso 1 1 calc .
C12 C 0.369(2) 1.1980(17) 0.2998(7) 0.022(5) Uani 1 1 d U
N12 N 0.5638(14) 1.2777(13) 0.3582(6) 0.023(4) Uani 1 1 d U
H12A H 0.6040 1.2148 0.3286 0.028 Uiso 1 1 calc .
H12B H 0.6197 1.3072 0.3773 0.028 Uiso 1 1 calc .
C13 C 0.5189(17) 1.0539(18) 0.2176(8) 0.021(4) Uani 1 1 d U
N13 N 0.3211(14) 1.2939(14) 0.3495(6) 0.022(4) Uani 1 1 d U
C14 C 0.4757(17) 1.1048(17) 0.1569(8) 0.025(5) Uani 1 1 d U
H14 H 0.4304 1.2018 0.1492 0.030 Uiso 1 1 calc .
N14 N 0.2568(14) 1.1627(14) 0.2861(6) 0.031(4) Uani 1 1 d U
H14A H 0.2717 1.1042 0.2556 0.038 Uiso 1 1 calc .
H14B H 0.1708 1.1990 0.3079 0.038 Uiso 1 1 calc .
C15 C 0.4981(18) 1.0150(19) 0.1065(7) 0.027(5) Uani 1 1 d U
H15 H 0.4631 1.0530 0.0658 0.032 Uiso 1 1 calc .
N15 N 0.4986(14) 1.1465(13) 0.2685(6) 0.020(4) Uani 1 1 d U
C16 C 0.5696(17) 0.8731(18) 0.1146(8) 0.021(4) Uani 1 1 d U
N16 N 0.5883(14) 0.7781(14) 0.0640(6) 0.023(4) Uani 1 1 d U
C17 C 0.6135(17) 0.8219(17) 0.1747(8) 0.023(4) Uani 1 1 d U
H17 H 0.6592 0.7249 0.1822 0.027 Uiso 1 1 calc .
N17 N 0.7887(15) 0.8151(15) 0.0220(6) 0.033(4) Uani 1 1 d U
H17A H 0.7773 0.8740 0.0518 0.040 Uiso 1 1 calc .
H17B H 0.8598 0.7955 -0.0077 0.040 Uiso 1 1 calc .
C18 C 0.5917(17) 0.9115(18) 0.2250(7) 0.022(4) Uani 1 1 d U
H18 H 0.6282 0.8731 0.2654 0.026 Uiso 1 1 calc .
N18 N 0.7392(14) 0.6567(14) -0.0267(6) 0.021(4) Uani 1 1 d U
C19 C 0.6960(18) 0.7543(18) 0.0217(8) 0.024(5) Uani 1 1 d U
N19 N 0.4939(15) 0.6744(14) -0.0338(6) 0.027(4) Uani 1 1 d U
H19A H 0.4509 0.7493 -0.0107 0.032 Uiso 1 1 calc .
H19B H 0.4394 0.6385 -0.0490 0.032 Uiso 1 1 calc .
C20 C 0.643(2) 0.6147(18) -0.0461(7) 0.023(5) Uani 1 1 d U
N20 N 0.6989(14) 0.5053(15) -0.0862(6) 0.033(4) Uani 1 1 d U
H20A H 0.7946 0.4660 -0.0980 0.040 Uiso 1 1 calc .
H20B H 0.6392 0.4739 -0.1003 0.040 Uiso 1 1 calc .
C21 C 0.885(2) 0.3445(18) -0.2134(8) 0.027(5) Uani 1 1 d U
N21 N 0.8401(15) 0.4313(15) -0.2639(6) 0.034(4) Uani 1 1 d U
H21A H 0.7616 0.4412 -0.2846 0.041 Uiso 1 1 calc .
H21B H 0.8891 0.4780 -0.2761 0.041 Uiso 1 1 calc .
C22 C 0.850(2) 0.1903(18) -0.1457(8) 0.027(5) Uani 1 1 d U
N22 N 1.0049(15) 0.3395(14) -0.1849(6) 0.029(4) Uani 1 1 d U
H22A H 1.0400 0.2864 -0.1512 0.035 Uiso 1 1 calc .
H22B H 1.0481 0.3893 -0.2000 0.035 Uiso 1 1 calc .
C23 C 0.9752(18) 0.0815(19) -0.0550(8) 0.020(4) Uani 1 1 d U
N23 N 0.8093(14) 0.2786(14) -0.1975(6) 0.024(4) Uani 1 1 d U
C24 C 0.8973(17) 0.1381(17) 0.0028(8) 0.023(5) Uani 1 1 d U
H24 H 0.8284 0.2336 0.0048 0.028 Uiso 1 1 calc .
N24 N 0.7599(15) 0.1257(15) -0.1387(6) 0.034(4) Uani 1 1 d U
H24A H 0.7741 0.0657 -0.1076 0.041 Uiso 1 1 calc .
H24B H 0.6881 0.1445 -0.1654 0.041 Uiso 1 1 calc .
C25 C 0.9206(18) 0.0561(19) 0.0562(7) 0.023(5) Uani 1 1 d U
H25 H 0.8643 0.0946 0.0942 0.028 Uiso 1 1 calc .
N25 N 0.9580(15) 0.1682(14) -0.1083(6) 0.023(4) Uani 1 1 d U
C31 C 0.481(2) 0.6786(18) 0.2966(7) 0.023(5) Uani 1 1 d U
N31 N 0.4861(14) 0.5824(15) 0.2552(6) 0.033(4) Uani 1 1 d U
H31A H 0.5691 0.5046 0.2498 0.039 Uiso 1 1 calc .
H31B H 0.4064 0.5985 0.2339 0.039 Uiso 1 1 calc .
C32 C 0.603(2) 0.7393(18) 0.3740(8) 0.025(5) Uani 1 1 d U
N32 N 0.3534(14) 0.7977(14) 0.3003(6) 0.027(4) Uani 1 1 d U
H32A H 0.3467 0.8643 0.3247 0.033 Uiso 1 1 calc .
H32B H 0.2762 0.8091 0.2782 0.033 Uiso 1 1 calc .
C33 C 0.4969(17) 0.9148(18) 0.4509(7) 0.022(5) Uani 1 1 d U
N33 N 0.6056(15) 0.6479(14) 0.3273(6) 0.023(4) Uani 1 1 d U
C34 C 0.4413(17) 0.9084(17) 0.5113(8) 0.022(5) Uani 1 1 d U
H34 H 0.4000 0.8465 0.5202 0.027 Uiso 1 1 calc .
N34 N 0.7503(14) 0.7057(13) 0.3879(6) 0.025(4) Uani 1 1 d U
H34A H 0.7682 0.7495 0.4181 0.030 Uiso 1 1 calc .
H34B H 0.8256 0.6406 0.3665 0.030 Uiso 1 1 calc .
C35 C 0.4449(17) 0.9930(18) 0.5603(7) 0.025(5) Uani 1 1 d U
H35 H 0.4065 0.9860 0.6016 0.029 Uiso 1 1 calc .
N35 N 0.4824(14) 0.8329(14) 0.4019(6) 0.024(4) Uani 1 1 d U
O1 O 0.3496(11) 0.5582(13) 0.5604(5) 0.029(3) Uani 1 1 d D
H1X H 0.260(14) 0.59(3) 0.544(12) 0.250 Uiso 1 1 d D
H1Y H 0.35(3) 0.50(3) 0.593(9) 0.250 Uiso 1 1 d D
O2 O 0.8980(12) 0.4964(12) 0.2710(5) 0.028(3) Uani 1 1 d D
H2X H 0.91(3) 0.411(9) 0.271(15) 0.250 Uiso 1 1 d D
H2Y H 0.804(12) 0.55(2) 0.284(15) 0.250 Uiso 1 1 d D
O3 O 0.5550(12) 0.5416(12) 0.0999(5) 0.031(3) Uani 1 1 d D
H3X H 0.641(18) 0.48(2) 0.117(14) 0.250 Uiso 1 1 d D
H3Y H 0.54(3) 0.63(3) 0.087(15) 0.250 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
C1 0.025(11) 0.023(12) 0.020(11) -0.006(9) -0.008(9) -0.011(10)
N1 0.021(8) 0.031(9) 0.023(8) 0.009(7) -0.005(6) -0.006(7)
C2 0.025(11) 0.028(12) 0.019(11) -0.007(9) 0.007(9) -0.014(10)
N2 0.023(8) 0.030(9) 0.023(8) 0.007(6) 0.004(6) -0.010(7)
C3 0.016(10) 0.031(11) 0.011(10) 0.002(9) -0.001(8) -0.010(9)
N3 0.016(8) 0.028(8) 0.010(7) 0.001(7) 0.000(6) -0.008(7)
C4 0.032(11) 0.037(12) 0.014(10) 0.002(9) -0.001(8) -0.016(10)
N4 0.023(8) 0.036(9) 0.034(8) 0.013(7) -0.003(7) -0.011(7)
C5 0.023(10) 0.024(11) 0.027(10) -0.003(8) -0.003(9) -0.013(9)
N5 0.023(8) 0.026(9) 0.019(8) 0.005(7) -0.006(7) -0.010(7)
C6 0.016(10) 0.024(12) 0.016(10) 0.000(9) -0.007(8) -0.002(9)
N6 0.027(8) 0.025(9) 0.016(8) 0.002(7) -0.004(7) -0.013(7)
C7 0.034(12) 0.037(12) 0.008(10) -0.006(9) -0.003(8) -0.018(10)
N7 0.027(9) 0.041(10) 0.025(8) 0.015(7) -0.005(7) -0.016(8)
C8 0.029(12) 0.025(12) 0.017(11) -0.004(9) -0.002(9) -0.012(10)
N8 0.020(8) 0.033(9) 0.015(8) 0.008(7) 0.000(6) -0.015(7)
C9 0.029(13) 0.023(13) 0.015(11) -0.001(9) 0.002(10) -0.007(11)
N9 0.021(8) 0.045(10) 0.032(9) 0.015(7) -0.003(7) -0.015(8)
C10 0.023(12) 0.031(13) 0.009(11) -0.007(9) -0.002(9) -0.008(11)
N10 0.021(8) 0.042(9) 0.022(8) 0.014(7) -0.003(7) -0.011(7)
C11 0.024(11) 0.026(12) 0.014(10) 0.005(9) 0.001(9) -0.010(10)
N11 0.028(8) 0.035(9) 0.030(8) -0.010(7) 0.000(7) -0.013(7)
C12 0.029(11) 0.022(12) 0.013(10) 0.007(9) -0.010(9) -0.010(10)
N12 0.024(8) 0.028(8) 0.016(8) -0.005(6) -0.001(6) -0.009(7)
C13 0.017(10) 0.025(11) 0.022(10) 0.000(9) 0.005(8) -0.010(9)
N13 0.022(8) 0.030(9) 0.016(8) -0.002(7) -0.001(6) -0.013(7)
C14 0.018(10) 0.023(11) 0.028(11) 0.003(8) 0.001(9) -0.005(9)
N14 0.024(8) 0.042(9) 0.025(8) -0.009(7) 0.003(7) -0.013(7)
C15 0.025(11) 0.033(12) 0.016(10) 0.004(9) -0.006(8) -0.007(10)
N15 0.020(8) 0.022(8) 0.016(8) -0.005(6) 0.001(6) -0.007(7)
C16 0.012(10) 0.030(11) 0.022(10) -0.003(9) 0.003(8) -0.009(9)
N16 0.023(8) 0.026(9) 0.017(8) -0.004(7) 0.002(7) -0.010(7)
C17 0.026(11) 0.023(11) 0.020(10) 0.002(8) 0.002(8) -0.012(9)
N17 0.035(9) 0.041(9) 0.027(8) -0.014(7) 0.009(7) -0.020(8)
C18 0.018(11) 0.034(11) 0.009(9) 0.002(8) -0.003(8) -0.009(9)
N18 0.021(8) 0.026(9) 0.017(8) -0.003(7) -0.001(6) -0.011(7)
C19 0.014(10) 0.027(12) 0.025(11) 0.001(9) -0.008(9) -0.005(9)
N19 0.021(8) 0.030(8) 0.025(8) -0.008(6) -0.004(7) -0.008(7)
C20 0.027(12) 0.024(12) 0.011(10) 0.001(9) 0.000(9) -0.005(10)
N20 0.026(8) 0.044(10) 0.034(9) -0.014(8) 0.000(7) -0.019(7)
C21 0.032(12) 0.027(12) 0.018(11) -0.003(9) -0.002(9) -0.010(10)
N21 0.032(8) 0.043(9) 0.032(8) 0.010(7) -0.007(7) -0.021(7)
C22 0.030(12) 0.031(12) 0.026(11) -0.004(9) 0.010(9) -0.020(10)
N22 0.028(8) 0.035(9) 0.026(8) 0.008(7) -0.006(7) -0.018(7)
C23 0.017(10) 0.032(12) 0.019(10) 0.000(9) -0.006(8) -0.018(9)
N23 0.026(8) 0.031(9) 0.019(8) 0.009(7) -0.005(6) -0.016(7)
C24 0.023(11) 0.022(11) 0.025(10) 0.000(9) 0.001(9) -0.011(9)
N24 0.032(8) 0.044(9) 0.029(8) 0.016(7) -0.015(7) -0.020(7)
C25 0.018(11) 0.036(12) 0.015(10) 0.000(9) 0.002(8) -0.012(10)
N25 0.026(8) 0.033(9) 0.014(8) 0.006(7) -0.006(7) -0.016(7)
C31 0.030(12) 0.024(12) 0.008(10) -0.004(9) 0.005(9) -0.006(10)
N31 0.028(8) 0.034(9) 0.030(8) -0.009(7) -0.006(7) -0.008(7)
C32 0.026(11) 0.027(12) 0.022(11) 0.003(9) -0.009(9) -0.011(10)
N32 0.025(8) 0.034(9) 0.019(8) -0.002(7) -0.010(6) -0.009(7)
C33 0.017(10) 0.032(12) 0.012(10) -0.002(9) -0.002(8) -0.007(9)
N33 0.023(8) 0.025(8) 0.019(8) -0.003(6) -0.007(6) -0.008(7)
C34 0.021(10) 0.027(12) 0.021(10) 0.000(9) 0.000(8) -0.014(9)
N34 0.018(8) 0.028(9) 0.022(8) -0.008(6) -0.002(6) -0.004(7)
C35 0.021(10) 0.030(12) 0.016(10) 0.002(8) -0.002(8) -0.005(9)
N35 0.023(8) 0.032(9) 0.013(8) -0.007(7) 0.000(7) -0.009(7)
O1 0.028(8) 0.039(9) 0.021(8) -0.004(6) -0.002(6) -0.016(7)
O2 0.028(8) 0.040(9) 0.019(7) 0.002(6) -0.003(6) -0.017(7)
O3 0.027(8) 0.040(10) 0.026(8) 0.004(6) -0.011(6) -0.015(7)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
N1 C1 N3 117.1(16) . .
N1 C1 N2 115.8(15) . .
N3 C1 N2 127.0(17) . .
N5 C2 N4 124.7(17) . .
N5 C2 N3 123.8(16) . .
N4 C2 N3 111.5(16) . .
C8 C3 C4 118.9(16) . .
C8 C3 N5 119.0(16) . .
C4 C3 N5 121.9(15) . .
C1 N3 C2 119.5(15) . .
C5 C4 C3 121.2(16) . .
C4 C5 C6 119.9(16) . .
C2 N5 C3 117.8(14) . .
C7 C6 C5 119.1(15) . .
C7 C6 N6 122.6(15) . .
C5 C6 N6 118.0(16) . .
C9 N6 C6 119.9(14) . .
C8 C7 C6 120.2(15) . .
C7 C8 C3 120.6(16) . .
C10 N8 C9 121.1(15) . .
N6 C9 N8 122.7(16) . .
N6 C9 N7 126.2(16) . .
N8 C9 N7 110.8(15) . .
N9 C10 N8 127.1(16) . .
N9 C10 N10 115.8(16) . .
N8 C10 N10 117.1(15) . .
N13 C11 N12 126.4(16) . .
N13 C11 N11 117.9(15) . .
N12 C11 N11 115.7(16) . .
N15 C12 N14 122.0(15) . .
N15 C12 N13 127.4(15) . .
N14 C12 N13 110.6(15) . .
C18 C13 C14 116.7(16) . .
C18 C13 N15 122.6(15) . .
C14 C13 N15 120.6(16) . .
C11 N13 C12 119.7(14) . .
C13 C14 C15 121.0(16) . .
C16 C15 C14 121.6(15) . .
C12 N15 C13 117.0(14) . .
C17 C16 C15 117.5(15) . .
C17 C16 N16 119.6(16) . .
C15 C16 N16 122.7(15) . .
C19 N16 C16 117.2(15) . .
C16 C17 C18 120.8(16) . .
C13 C18 C17 122.1(15) . .
C20 N18 C19 120.1(14) . .
N16 C19 N17 123.6(17) . .
N16 C19 N18 125.0(16) . .
N17 C19 N18 111.3(15) . .
N18 C20 N19 126.8(16) . .
N18 C20 N20 116.9(16) . .
N19 C20 N20 116.2(16) . .
N23 C21 N22 127.9(17) . .
N23 C21 N21 117.5(17) . .
N22 C21 N21 114.7(17) . .
N25 C22 N24 123.7(17) . .
N25 C22 N23 126.0(16) . .
N24 C22 N23 110.3(16) . .
C25 C23 N25 120.8(16) 2_755 .
C25 C23 C24 118.7(15) 2_755 .
N25 C23 C24 120.1(16) . .
C21 N23 C22 119.5(15) . .
C25 C24 C23 120.6(15) . .
C24 C25 C23 120.6(15) . 2_755
C22 N25 C23 117.5(14) . .
N33 C31 N32 126.2(16) . .
N33 C31 N31 116.9(16) . .
N32 C31 N31 116.8(16) . .
N35 C32 N34 126.1(15) . .
N35 C32 N33 125.1(16) . .
N34 C32 N33 108.6(15) . .
C34 C33 C35 117.7(15) . 2_676
C34 C33 N35 118.9(16) . .
C35 C33 N35 123.3(15) 2_676 .
C31 N33 C32 119.0(15) . .
C33 C34 C35 121.1(15) . .
C33 C35 C34 121.2(15) 2_676 .
C32 N35 C33 119.1(14) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.328(19) .
C1 N3 1.335(18) .
C1 N2 1.340(19) .
C2 N5 1.293(18) .
C2 N4 1.367(17) .
C2 N3 1.37(2) .
C3 C8 1.39(2) .
C3 C4 1.39(2) .
C3 N5 1.420(19) .
C4 C5 1.37(2) .
C5 C6 1.40(2) .
C6 C7 1.40(2) .
C6 N6 1.418(19) .
N6 C9 1.306(19) .
C7 C8 1.38(2) .
N7 C9 1.369(19) .
N8 C10 1.330(18) .
N8 C9 1.361(19) .
N9 C10 1.322(19) .
C10 N10 1.338(19) .
C11 N13 1.324(18) .
C11 N12 1.338(17) .
C11 N11 1.375(18) .
C12 N15 1.310(17) .
C12 N14 1.391(18) .
C12 N13 1.409(18) .
C13 C18 1.38(2) .
C13 C14 1.39(2) .
C13 N15 1.441(18) .
C14 C15 1.41(2) .
C15 C16 1.38(2) .
C16 C17 1.38(2) .
C16 N16 1.458(19) .
N16 C19 1.304(18) .
C17 C18 1.41(2) .
N17 C19 1.366(19) .
N18 C20 1.327(19) .
N18 C19 1.403(19) .
N19 C20 1.347(18) .
C20 N20 1.364(18) .
C21 N23 1.292(19) .
C21 N22 1.346(19) .
C21 N21 1.350(19) .
C22 N25 1.297(19) .
C22 N24 1.376(18) .
C22 N23 1.38(2) .
C23 C25 1.38(2) 2_755
C23 N25 1.409(19) .
C23 C24 1.415(19) .
C24 C25 1.37(2) .
C25 C23 1.38(2) 2_755
C31 N33 1.330(19) .
C31 N32 1.343(18) .
C31 N31 1.369(19) .
C32 N35 1.300(18) .
C32 N34 1.395(18) .
C32 N33 1.415(19) .
C33 C34 1.381(19) .
C33 C35 1.38(2) 2_676
C33 N35 1.443(18) .
C34 C35 1.42(2) .
C35 C33 1.38(2) 2_676
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A N34 0.88 2.33 3.167(18) 158.0 2_756
N1 H1B N13 0.88 2.25 3.056(17) 153.1 2_666
N2 H2B N5 0.88 2.13 2.700(17) 121.7 .
N2 H2A N13 0.88 2.28 3.083(17) 151.9 2_666
N4 H4A N32 0.88 2.65 3.319(18) 133.2 1_645
N7 H7A N15 0.88 2.29 3.057(17) 145.7 1_545
N9 H9A N6 0.88 2.09 2.682(17) 123.9 .
N10 H10B N18 0.88 2.42 3.177(18) 144.1 .
N10 H10A N18 0.88 2.15 2.984(17) 158.6 2_765
N11 H11A N3 0.88 2.59 3.310(18) 139.2 1_475
N11 H11B O1 0.88 2.20 2.986(16) 149.0 2_676
N12 H12A N15 0.88 2.05 2.685(17) 128.5 .
N12 H12B O1 0.88 2.13 2.944(16) 152.8 2_676
N17 H17B N10 0.88 2.72 3.412(18) 136.9 2_765
N19 H19A N16 0.88 2.26 2.785(18) 117.9 .
N19 H19B O3 0.88 2.24 3.009(18) 145.2 2_665
N20 H20A N22 0.88 2.62 3.406(18) 149.3 .
N20 H20B O3 0.88 2.03 2.846(17) 153.6 2_665
N21 H21A N31 0.88 2.66 3.340(18) 135.3 2_665
N21 H21B O2 0.88 2.28 3.064(16) 147.7 2_765
N22 H22A N25 0.88 1.99 2.616(17) 126.7 .
N22 H22B O2 0.88 2.12 2.941(15) 154.7 2_765
N31 H31B N21 0.88 2.68 3.340(18) 132.5 2_665
N31 H31B N23 0.88 2.12 2.944(18) 155.5 2_665
N31 H31A N7 0.88 2.58 3.332(19) 144.0 .
N32 H32A N35 0.88 2.09 2.684(17) 124.0 .
N32 H32B N23 0.88 2.36 3.124(17) 146.1 2_665
N34 H34A N5 0.88 2.38 3.061(18) 134.5 1_565
N34 H34B O2 0.88 2.47 3.228(16) 144.9 .
N34 H34B N1 0.88 2.62 3.167(18) 121.3 2_756
O1 H1X N3 0.9(2) 1.9(2) 2.779(17) 171 1_465
O1 H1Y N33 0.9(2) 2.2(3) 3.112(17) 170 2_666
O2 H2X N6 0.9(2) 2.2(1) 2.966(17) 159 .
O2 H2Y N33 0.9(2) 2.0(2) 2.845(17) 169 .
O3 H3X N8 0.9(2) 1.8(3) 2.689(18) 175 .
O3 H3Y N16 0.9(2) 2.0(3) 2.816(18) 159 .
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_4
N1 C1 N3 C2 175.8(15) . .
N2 C1 N3 C2 -9(3) . .
N5 C2 N3 C1 -25(3) . .
N4 C2 N3 C1 155.6(14) . .
C8 C3 C4 C5 -1(3) . .
N5 C3 C4 C5 -176.6(15) . .
C3 C4 C5 C6 1(3) . .
N4 C2 N5 C3 1(2) . .
N3 C2 N5 C3 -178.9(16) . .
C8 C3 N5 C2 109.9(17) . .
C4 C3 N5 C2 -75(2) . .
C4 C5 C6 C7 0(2) . .
C4 C5 C6 N6 -174.1(15) . .
C7 C6 N6 C9 53(2) . .
C5 C6 N6 C9 -132.4(16) . .
C5 C6 C7 C8 -1(2) . .
N6 C6 C7 C8 173.6(15) . .
C6 C7 C8 C3 0(3) . .
C4 C3 C8 C7 1(3) . .
N5 C3 C8 C7 176.4(15) . .
C6 N6 C9 N8 -175.0(15) . .
C6 N6 C9 N7 11(3) . .
C10 N8 C9 N6 24(2) . .
C10 N8 C9 N7 -161.1(15) . .
C9 N8 C10 N9 0(3) . .
C9 N8 C10 N10 177.5(16) . .
N12 C11 N13 C12 -3(2) . .
N11 C11 N13 C12 177.6(14) . .
N15 C12 N13 C11 -8(2) . .
N14 C12 N13 C11 172.6(14) . .
C18 C13 C14 C15 3(2) . .
N15 C13 C14 C15 178.6(15) . .
C13 C14 C15 C16 -3(3) . .
N14 C12 N15 C13 2(2) . .
N13 C12 N15 C13 -177.5(15) . .
C18 C13 N15 C12 -97.6(18) . .
C14 C13 N15 C12 87.6(19) . .
C14 C15 C16 C17 2(2) . .
C14 C15 C16 N16 177.3(15) . .
C17 C16 N16 C19 -106.0(18) . .
C15 C16 N16 C19 79(2) . .
C15 C16 C17 C18 -3(2) . .
N16 C16 C17 C18 -177.6(14) . .
C14 C13 C18 C17 -4(2) . .
N15 C13 C18 C17 -178.8(15) . .
C16 C17 C18 C13 3(2) . .
C16 N16 C19 N17 -1(2) . .
C16 N16 C19 N18 173.7(14) . .
C20 N18 C19 N16 23(2) . .
C20 N18 C19 N17 -161.5(15) . .
C19 N18 C20 N19 14(2) . .
C19 N18 C20 N20 -170.4(15) . .
N22 C21 N23 C22 0(3) . .
N21 C21 N23 C22 -179.1(14) . .
N25 C22 N23 C21 2(3) . .
N24 C22 N23 C21 -177.1(15) . .
C25 C23 C24 C25 -3(3) 2_755 .
N25 C23 C24 C25 -175.8(14) . .
C23 C24 C25 C23 3(3) . 2_755
N24 C22 N25 C23 -5(3) . .
N23 C22 N25 C23 175.4(15) . .
C25 C23 N25 C22 98(2) 2_755 .
C24 C23 N25 C22 -89.0(19) . .
N32 C31 N33 C32 8(3) . .
N31 C31 N33 C32 -175.5(14) . .
N35 C32 N33 C31 19(2) . .
N34 C32 N33 C31 -165.3(14) . .
C35 C33 C34 C35 0(3) 2_676 .
N35 C33 C34 C35 -176.3(14) . .
C33 C34 C35 C33 0(3) . 2_676
N34 C32 N35 C33 2(3) . .
N33 C32 N35 C33 177.1(15) . .
C34 C33 N35 C32 -119.0(17) . .
C35 C33 N35 C32 65(2) 2_676 .
|
1501606.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/16/1501606.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_1501606
loop_
_publ_author_name
'Olivier Lebel'
'Thierry Maris'
'James D. Wuest'
_publ_section_title
;
Hydrogen-Bonded networks in crystals built from bis(biguanides) and their
salts
;
_journal_name_full 'Can J. Chem'
_journal_page_first 1426
_journal_page_last 1433
_journal_paper_doi 10.1139/v06-115
_journal_volume 84
_journal_year 2006
_chemical_formula_moiety 'C10 H18 N10, 0.5(C4 H8 O2), C O3, H2 O'
_chemical_formula_sum 'C13 H24 N10 O5'
_chemical_formula_weight 400.42
_chemical_name_systematic
;
?
;
_space_group_IT_number 2
_symmetry_cell_setting triclinic
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 77.297(2)
_cell_angle_beta 67.906(2)
_cell_angle_gamma 65.826(2)
_cell_formula_units_Z 2
_cell_length_a 9.9072(3)
_cell_length_b 10.1769(3)
_cell_length_c 11.0195(5)
_cell_measurement_reflns_used 2601
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 71.94
_cell_measurement_theta_min 4.34
_cell_volume 936.32(6)
_computing_cell_refinement 'SMART (Bruker, 1999)'
_computing_data_collection 'SMART (Bruker, 1999)'
_computing_data_reduction 'SAINT (Bruker, 1999)'
_computing_molecular_graphics 'SHELXTL (Bruker, 1997)'
_computing_publication_material 'UdMX (local program)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type 'Bruker AXS Smart 2K/Platform'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'Sealed Tube'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.029
_diffrn_reflns_av_sigmaI/netI 0.0604
_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 10733
_diffrn_reflns_theta_full 72.03
_diffrn_reflns_theta_max 72.03
_diffrn_reflns_theta_min 4.34
_diffrn_standards_decay_% -0.18
_diffrn_standards_number 42
_exptl_absorpt_coefficient_mu 0.947
_exptl_absorpt_correction_T_max 0.8710
_exptl_absorpt_correction_T_min 0.7976
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Sadabs (Sheldrick,1996)'
_exptl_crystal_colour Colourless
_exptl_crystal_density_diffrn 1.420
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 424
_exptl_crystal_size_max 0.25
_exptl_crystal_size_mid 0.20
_exptl_crystal_size_min 0.15
_refine_diff_density_max 0.397
_refine_diff_density_min -0.479
_refine_diff_density_rms 0.071
_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 259
_refine_ls_number_reflns 3526
_refine_ls_number_restraints 5
_refine_ls_restrained_S_all 0.942
_refine_ls_R_factor_all 0.0699
_refine_ls_R_factor_gt 0.0487
_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^)+(0.0825P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1277
_refine_ls_wR_factor_ref 0.1357
_reflns_number_gt 2403
_reflns_number_total 3557
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file deposit.cif
_cod_data_source_block jiw865
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana
;
_cod_original_sg_symbol_H-M P-1
_cod_database_code 1501606
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
N1 N 0.4531(2) -0.02620(19) 0.31111(18) 0.0166(4) Uani 1 1 d .
H1A H 0.5541 -0.0531 0.2960 0.020 Uiso 1 1 d R
N2 N 0.5053(2) -0.2390(2) 0.23522(18) 0.0203(4) Uani 1 1 d .
H2A H 0.4785 -0.3111 0.2341 0.024 Uiso 1 1 d R
H2B H 0.6016 -0.2424 0.1927 0.024 Uiso 1 1 d R
N3 N 0.2508(2) -0.1087(2) 0.36876(17) 0.0172(4) Uani 1 1 d .
N4 N 0.0633(2) -0.2086(2) 0.42485(19) 0.0210(5) Uani 1 1 d .
H4A H 0.0065 -0.2415 0.4034 0.025 Uiso 1 1 d R
H4B H 0.0486 -0.2048 0.5081 0.025 Uiso 1 1 d R
N5 N 0.1913(2) -0.1718(2) 0.20667(18) 0.0216(5) Uani 1 1 d .
H5A H 0.1332 -0.2051 0.1873 0.026 Uiso 1 1 d R
H5B H 0.2623 -0.1433 0.1434 0.026 Uiso 1 1 d R
N6 N 0.0347(2) 0.4276(2) 0.25650(19) 0.0202(4) Uani 1 1 d .
H6 H 0.0241 0.5187 0.2322 0.024 Uiso 1 1 d R
N7 N -0.1456(2) 0.4658(2) 0.15886(19) 0.0224(5) Uani 1 1 d .
H7A H -0.2161 0.4426 0.1473 0.027 Uiso 1 1 d R
H7B H -0.1305 0.5462 0.1200 0.027 Uiso 1 1 d R
N8 N -0.0739(2) 0.2545(2) 0.29951(18) 0.0182(4) Uani 1 1 d .
N9 N -0.1090(2) 0.1712(2) 0.13313(18) 0.0229(5) Uani 1 1 d .
H9A H -0.1409 0.1130 0.1119 0.027 Uiso 1 1 d R
H9B H -0.0670 0.2277 0.0717 0.027 Uiso 1 1 d R
N10 N -0.1880(2) 0.0871(2) 0.34815(18) 0.0199(4) Uani 1 1 d .
H10A H -0.1959 0.0839 0.4309 0.024 Uiso 1 1 d R
H10B H -0.2225 0.0327 0.3248 0.024 Uiso 1 1 d R
C1 C 0.2402(3) 0.1985(2) 0.2876(2) 0.0173(5) Uani 1 1 d .
H1 H 0.2209 0.1554 0.2307 0.021 Uiso 1 1 calc RD
C2 C 0.1518(3) 0.3424(2) 0.3150(2) 0.0181(5) Uani 1 1 d .
C3 C 0.1844(3) 0.4067(3) 0.3949(2) 0.0203(5) Uani 1 1 d .
H3 H 0.1262 0.5052 0.4123 0.024 Uiso 1 1 calc R
C4 C 0.3032(3) 0.3249(3) 0.4488(2) 0.0224(5) Uani 1 1 d .
H4 H 0.3259 0.3683 0.5030 0.027 Uiso 1 1 calc R
C5 C 0.3883(3) 0.1817(3) 0.4248(2) 0.0203(5) Uani 1 1 d .
H5 H 0.4681 0.1268 0.4632 0.024 Uiso 1 1 calc R
C6 C 0.3572(3) 0.1182(2) 0.3445(2) 0.0180(5) Uani 1 1 d .
C7 C 0.3995(3) -0.1242(2) 0.3014(2) 0.0169(5) Uani 1 1 d .
C8 C 0.1721(3) -0.1647(2) 0.3311(2) 0.0178(5) Uani 1 1 d .
C9 C -0.0614(3) 0.3789(3) 0.2355(2) 0.0180(5) Uani 1 1 d .
C10 C -0.1244(2) 0.1736(2) 0.2590(2) 0.0180(5) Uani 1 1 d .
O20 O 0.0237(2) 0.27989(18) 0.79412(19) 0.0331(5) Uani 1 1 d .
O21 O 0.23054(19) 0.07753(18) 0.78713(17) 0.0274(4) Uani 1 1 d .
O22 O 0.17412(19) 0.24634(17) 0.91489(16) 0.0237(4) Uani 1 1 d .
C20 C 0.1422(3) 0.2013(3) 0.8319(2) 0.0189(5) Uani 1 1 d .
O40 O 0.3532(2) -0.0047(2) 0.01592(19) 0.0358(5) Uani 1 1 d D
H40A H 0.289(3) 0.0498(14) -0.029(2) 0.043 Uiso 1 1 d D
H40B H 0.3741(3) 0.0554(11) 0.0457(10) 0.043 Uiso 1 1 d D
O30 O 0.56595(18) 0.49872(18) 0.09576(15) 0.0225(4) Uani 1 1 d .
C30 C 0.5164(3) 0.3849(3) 0.0952(2) 0.0228(5) Uani 1 1 d .
H30A H 0.4804 0.3434 0.1863 0.027 Uiso 1 1 calc R
H30B H 0.6059 0.3072 0.0434 0.027 Uiso 1 1 calc R
C31 C 0.6142(3) 0.5597(3) -0.0370(2) 0.0235(5) Uani 1 1 d .
H31A H 0.7053 0.4851 -0.0912 0.028 Uiso 1 1 calc R
H31B H 0.6466 0.6400 -0.0379 0.028 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
N1 0.0129(10) 0.0118(10) 0.0253(10) -0.0020(8) -0.0079(8) -0.0029(8)
N2 0.0169(10) 0.0153(10) 0.0286(11) -0.0047(9) -0.0054(8) -0.0059(9)
N3 0.0186(10) 0.0134(10) 0.0188(10) 0.0000(8) -0.0047(8) -0.0068(9)
N4 0.0219(11) 0.0199(11) 0.0234(10) -0.0001(9) -0.0066(8) -0.0110(9)
N5 0.0208(11) 0.0241(11) 0.0242(11) -0.0006(9) -0.0086(8) -0.0117(10)
N6 0.0193(10) 0.0100(10) 0.0310(11) 0.0025(8) -0.0099(8) -0.0054(9)
N7 0.0218(11) 0.0143(10) 0.0322(11) 0.0022(9) -0.0122(9) -0.0067(9)
N8 0.0155(10) 0.0135(10) 0.0248(10) -0.0006(8) -0.0064(8) -0.0051(9)
N9 0.0313(12) 0.0183(11) 0.0212(10) 0.0003(9) -0.0100(9) -0.0106(10)
N10 0.0227(11) 0.0192(11) 0.0223(10) -0.0014(8) -0.0073(8) -0.0118(9)
C1 0.0176(12) 0.0164(12) 0.0187(11) -0.0015(9) -0.0042(9) -0.0082(11)
C2 0.0164(12) 0.0162(12) 0.0204(12) 0.0006(10) -0.0050(9) -0.0064(11)
C3 0.0191(12) 0.0126(12) 0.0260(12) -0.0032(10) -0.0040(10) -0.0048(11)
C4 0.0252(13) 0.0203(13) 0.0231(12) -0.0057(10) -0.0081(10) -0.0073(11)
C5 0.0225(13) 0.0174(12) 0.0210(12) 0.0018(10) -0.0088(10) -0.0075(11)
C6 0.0184(12) 0.0141(12) 0.0198(11) 0.0011(9) -0.0036(9) -0.0076(11)
C7 0.0199(12) 0.0136(12) 0.0167(11) 0.0019(9) -0.0093(9) -0.0042(10)
C8 0.0160(12) 0.0085(11) 0.0241(12) -0.0021(9) -0.0064(9) 0.0006(10)
C9 0.0139(11) 0.0147(12) 0.0204(11) -0.0022(9) -0.0034(9) -0.0019(10)
C10 0.0112(11) 0.0132(12) 0.0257(12) -0.0031(10) -0.0070(9) 0.0012(10)
O20 0.0278(10) 0.0147(9) 0.0649(13) 0.0030(9) -0.0285(9) -0.0060(8)
O21 0.0220(9) 0.0208(9) 0.0415(11) -0.0129(8) -0.0090(8) -0.0055(8)
O22 0.0302(10) 0.0175(9) 0.0247(9) -0.0026(7) -0.0102(7) -0.0080(8)
C20 0.0187(12) 0.0151(12) 0.0230(12) -0.0001(10) -0.0040(9) -0.0093(11)
O40 0.0335(11) 0.0412(12) 0.0389(11) 0.0109(9) -0.0199(9) -0.0189(10)
O30 0.0264(9) 0.0234(9) 0.0206(8) 0.0007(7) -0.0082(7) -0.0124(8)
C30 0.0244(13) 0.0204(13) 0.0229(12) 0.0004(10) -0.0057(10) -0.0103(12)
C31 0.0267(14) 0.0227(13) 0.0222(12) 0.0020(10) -0.0063(10) -0.0133(12)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
C7 N1 C6 124.40(18) . .
C7 N1 H1A 117.8 . .
C6 N1 H1A 117.8 . .
C7 N2 H2A 120.0 . .
C7 N2 H2B 120.0 . .
H2A N2 H2B 120.0 . .
C7 N3 C8 121.79(19) . .
C8 N4 H4A 120.0 . .
C8 N4 H4B 120.0 . .
H4A N4 H4B 120.0 . .
C8 N5 H5A 120.1 . .
C8 N5 H5B 119.9 . .
H5A N5 H5B 120.0 . .
C9 N6 C2 124.53(19) . .
C9 N6 H6 117.7 . .
C2 N6 H6 117.7 . .
C9 N7 H7A 120.1 . .
C9 N7 H7B 120.0 . .
H7A N7 H7B 120.0 . .
C9 N8 C10 123.0(2) . .
C10 N9 H9A 120.0 . .
C10 N9 H9B 120.1 . .
H9A N9 H9B 120.0 . .
C10 N10 H10A 120.0 . .
C10 N10 H10B 120.0 . .
H10A N10 H10B 119.9 . .
C6 C1 C2 119.6(2) . .
C6 C1 H1 120.2 . .
C2 C1 H1 120.2 . .
C1 C2 C3 120.0(2) . .
C1 C2 N6 120.9(2) . .
C3 C2 N6 119.0(2) . .
C4 C3 C2 119.3(2) . .
C4 C3 H3 120.4 . .
C2 C3 H3 120.4 . .
C5 C4 C3 121.0(2) . .
C5 C4 H4 119.5 . .
C3 C4 H4 119.5 . .
C4 C5 C6 119.8(2) . .
C4 C5 H5 120.1 . .
C6 C5 H5 120.1 . .
C5 C6 C1 120.3(2) . .
C5 C6 N1 119.9(2) . .
C1 C6 N1 119.6(2) . .
N3 C7 N2 124.7(2) . .
N3 C7 N1 118.4(2) . .
N2 C7 N1 116.5(2) . .
N5 C8 N4 118.5(2) . .
N5 C8 N3 123.7(2) . .
N4 C8 N3 117.7(2) . .
N8 C9 N7 125.4(2) . .
N8 C9 N6 118.1(2) . .
N7 C9 N6 116.3(2) . .
N10 C10 N8 117.8(2) . .
N10 C10 N9 118.2(2) . .
N8 C10 N9 124.0(2) . .
O21 C20 O20 120.3(2) . .
O21 C20 O22 119.4(2) . .
O20 C20 O22 120.4(2) . .
H40A O40 H40B 105.7(8) . .
C30 O30 C31 108.52(17) . .
O30 C30 C31 110.87(19) . 2_665
O30 C30 H30A 109.5 . .
C31 C30 H30A 109.5 2_665 .
O30 C30 H30B 109.5 . .
C31 C30 H30B 109.5 2_665 .
H30A C30 H30B 108.1 . .
O30 C31 C30 111.05(18) . 2_665
O30 C31 H31A 109.4 . .
C30 C31 H31A 109.4 2_665 .
O30 C31 H31B 109.4 . .
C30 C31 H31B 109.4 2_665 .
H31A C31 H31B 108.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
N1 C7 1.346(3) .
N1 C6 1.424(3) .
N1 H1A 0.8799 .
N2 C7 1.338(3) .
N2 H2A 0.8802 .
N2 H2B 0.8801 .
N3 C7 1.336(3) .
N3 C8 1.348(3) .
N4 C8 1.335(3) .
N4 H4A 0.8799 .
N4 H4B 0.8796 .
N5 C8 1.326(3) .
N5 H5A 0.8806 .
N5 H5B 0.8798 .
N6 C9 1.345(3) .
N6 C2 1.416(3) .
N6 H6 0.8803 .
N7 C9 1.337(3) .
N7 H7A 0.8805 .
N7 H7B 0.8794 .
N8 C9 1.336(3) .
N8 C10 1.339(3) .
N9 C10 1.342(3) .
N9 H9A 0.8802 .
N9 H9B 0.8800 .
N10 C10 1.321(3) .
N10 H10A 0.8801 .
N10 H10B 0.8792 .
C1 C6 1.396(3) .
C1 C2 1.396(3) .
C1 H1 0.9500 .
C2 C3 1.396(3) .
C3 C4 1.391(3) .
C3 H3 0.9500 .
C4 C5 1.378(3) .
C4 H4 0.9500 .
C5 C6 1.385(3) .
C5 H5 0.9500 .
O20 C20 1.282(3) .
O21 C20 1.281(3) .
O22 C20 1.291(3) .
O30 C30 1.433(3) .
O30 C31 1.439(3) .
C30 C31 1.508(3) 2_665
C30 H30A 0.9900 .
C30 H30B 0.9900 .
C31 C30 1.508(3) 2_665
C31 H31A 0.9900 .
C31 H31B 0.9900 .
O40 H40A 0.88(1) .
O40 H40B 0.88(1) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A O21 0.88 1.91 2.761(2) 162.2 2_656
N2 H2A O30 0.88 2.40 3.105(2) 137.5 1_545
N2 H2B O22 0.88 2.08 2.956(2) 177.4 2_656
N4 H4A O20 0.88 2.44 3.153(3) 138.8 2_556
N4 H4B N8 0.88 2.15 3.005(3) 162.6 2_556
N5 H5A O20 0.88 1.92 2.772(2) 161.4 2_556
N5 H5B O40 0.88 2.00 2.830(3) 157.3 .
N6 H6 O20 0.88 1.89 2.759(3) 170.9 2_566
N7 H7A O30 0.88 2.25 3.061(2) 152.3 1_455
N7 H7B O22 0.88 1.95 2.788(3) 158.0 2_566
N9 H9A O21 0.88 2.35 3.058(3) 138.1 2_556
N9 H9B O22 0.88 2.42 3.179(3) 144.9 1_554
N9 H9B N7 0.88 2.51 2.933(3) 110.1 .
N10 H10A N3 0.88 2.11 2.982(3) 169.9 2_556
N10 H10B O21 0.88 1.88 2.713(2) 156.7 2_556
O40 H40A O22 0.88(1) 1.950(11) 2.727(2) 145.8(12) 1_554
O40 H40A O21 0.88(1) 2.243(13) 3.013(3) 145(2) 1_554
O40 H40B O40 0.88(1) 2.379(4) 2.835(4) 112.7(3) 2_655
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_4
C6 C1 C2 C3 2.3(3) .
C6 C1 C2 N6 178.6(2) .
C9 N6 C2 C1 38.4(3) .
C9 N6 C2 C3 -145.4(2) .
C1 C2 C3 C4 -1.4(3) .
N6 C2 C3 C4 -177.7(2) .
C2 C3 C4 C5 -0.2(3) .
C3 C4 C5 C6 0.9(3) .
C4 C5 C6 C1 0.1(3) .
C4 C5 C6 N1 175.0(2) .
C2 C1 C6 C5 -1.7(3) .
C2 C1 C6 N1 -176.63(19) .
C7 N1 C6 C5 141.6(2) .
C7 N1 C6 C1 -43.5(3) .
C8 N3 C7 N2 -32.1(3) .
C8 N3 C7 N1 155.4(2) .
C6 N1 C7 N3 -24.9(3) .
C6 N1 C7 N2 162.1(2) .
C7 N3 C8 N5 -35.6(3) .
C7 N3 C8 N4 147.8(2) .
C10 N8 C9 N7 26.5(3) .
C10 N8 C9 N6 -158.8(2) .
C2 N6 C9 N8 16.2(3) .
C2 N6 C9 N7 -168.5(2) .
C9 N8 C10 N10 -154.9(2) .
C9 N8 C10 N9 27.8(3) .
C31 O30 C30 C31 -57.8(3) 2_665
C30 O30 C31 C30 57.9(3) 2_665
|
1501607.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/16/1501607.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_1501607
loop_
_publ_author_name
'Olivier LeBel'
'Thierry Maris'
'Hugues Duval'
'James D. Wuest'
_publ_section_title
;
A practical guide to arylbiguanides --- Synthesis and structural
characterization
;
_journal_name_full 'Can. J. Chem.'
_journal_page_first 615
_journal_page_last 625
_journal_paper_doi 10.1139/v05-093
_journal_volume 83
_journal_year 2005
_chemical_compound_source 'Synthesized by the authors. See text'
_chemical_formula_moiety 'C14 H16 N5, Cl'
_chemical_formula_sum 'C14 H16 Cl N5'
_chemical_formula_weight 289.77
_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 95.79(2)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 9.627(5)
_cell_length_b 4.9751(5)
_cell_length_c 35.2533(5)
_cell_measurement_reflns_used 5926
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 6.54
_cell_measurement_theta_min 0.32
_cell_volume 1679.9(9)
_computing_cell_refinement 'SMART (Bruker, 1999)'
_computing_data_collection 'SMART (Bruker, 1999)'
_computing_data_reduction 'SAINT (Bruker, 1999)'
_computing_molecular_graphics 'SHELXTL (Bruker, 1997)'
_computing_publication_material 'UdMX (local program)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.935
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_device_type 'Bruker AXS Smart 2K/Platform'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'Sealed Tube'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.069
_diffrn_reflns_av_sigmaI/netI 0.0308
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 5
_diffrn_reflns_limit_k_min -5
_diffrn_reflns_limit_l_max 37
_diffrn_reflns_limit_l_min -40
_diffrn_reflns_number 15289
_diffrn_reflns_theta_full 66.39
_diffrn_reflns_theta_max 66.39
_diffrn_reflns_theta_min 2.52
_diffrn_standards_decay_% -0.09
_diffrn_standards_number 119
_exptl_absorpt_coefficient_mu 1.994
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_correction_T_min 0.0200
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Sadabs (Sheldrick,1996)'
_exptl_crystal_colour Colourless
_exptl_crystal_density_diffrn 1.146
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 608
_exptl_crystal_size_max 0.35
_exptl_crystal_size_mid 0.08
_exptl_crystal_size_min 0.08
_refine_diff_density_max 0.352
_refine_diff_density_min -0.201
_refine_diff_density_rms 0.045
_refine_ls_extinction_coef 0.0026(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 1.066
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 216
_refine_ls_number_reflns 2754
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.066
_refine_ls_R_factor_all 0.0652
_refine_ls_R_factor_gt 0.0563
_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^)+(0.1271P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1784
_refine_ls_wR_factor_ref 0.1869
_reflns_number_gt 2025
_reflns_number_total 2754
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file deposit.cif
_cod_data_source_block jiw794
_cod_original_sg_symbol_H-M P21/n
_cod_database_code 1501607
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
C1 C 0.5928(2) 0.4191(5) 0.18187(6) 0.0770(7) Uani 1 1 d .
Cl1 Cl 0.98304(5) 0.48975(14) 0.217648(15) 0.0925(4) Uani 1 1 d .
N1 N 0.46329(17) 0.3894(5) 0.16431(5) 0.0872(6) Uani 1 1 d .
C2 C 0.3474(2) 0.4359(5) 0.18197(6) 0.0811(7) Uani 1 1 d .
N2 N 0.2297(2) 0.4976(5) 0.15878(6) 0.0948(8) Uani 1 1 d .
C3 C 0.2180(2) 0.5239(5) 0.11655(6) 0.0843(8) Uani 1 1 d .
N3 N 0.69863(17) 0.2998(5) 0.16452(5) 0.0846(7) Uani 1 1 d .
C4 C 0.2996(3) 0.7127(7) 0.09812(8) 0.1028(8) Uani 1 1 d .
H4 H 0.3615 0.8247 0.1126 0.129(11) Uiso 1 1 d R
N4 N 0.6315(2) 0.5641(6) 0.21456(6) 0.0992(8) Uani 1 1 d .
C5 C 0.2855(3) 0.7331(9) 0.05737(8) 0.1216(11) Uani 1 1 d .
H5 H 0.3409 0.8549 0.0457 0.158(14) Uiso 1 1 d R
N5 N 0.3363(2) 0.4168(7) 0.22098(6) 0.0982(8) Uani 1 1 d .
C6 C 0.1914(4) 0.5742(9) 0.03441(9) 0.1201(11) Uani 1 1 d .
H6 H 0.1839 0.5877 0.0080 0.127(10) Uiso 1 1 d R
C7 C 0.1098(4) 0.3935(8) 0.05234(10) 0.1256(11) Uani 1 1 d .
H7 H 0.0447 0.2903 0.0375 0.160(14) Uiso 1 1 d R
C8 C 0.1224(3) 0.3641(8) 0.09372(8) 0.1090(9) Uani 1 1 d .
H8 H 0.0673 0.2397 0.1050 0.103(9) Uiso 1 1 d R
C9 C 0.6957(2) 0.1691(5) 0.12676(6) 0.0784(7) Uani 1 1 d .
C10 C 0.7953(3) -0.0331(6) 0.12231(9) 0.1040(9) Uani 1 1 d .
H10 H 0.8542 -0.0933 0.1431 0.090(7) Uiso 1 1 d R
C11 C 0.8033(4) -0.1495(8) 0.08466(11) 0.1329(12) Uani 1 1 d .
H11 H 0.8686 -0.2838 0.0818 0.155(13) Uiso 1 1 d R
C12 C 0.7164(5) -0.0654(8) 0.05197(11) 0.1211(11) Uani 1 1 d .
H12 H 0.7245 -0.1390 0.0280 0.130(10) Uiso 1 1 d R
C13 C 0.6199(3) 0.1318(7) 0.05685(8) 0.1094(9) Uani 1 1 d .
H13 H 0.5599 0.1878 0.0360 0.124(10) Uiso 1 1 d R
C14 C 0.6085(3) 0.2510(7) 0.09379(6) 0.0965(8) Uani 1 1 d .
H14 H 0.5428 0.3856 0.0960 0.114(9) Uiso 1 1 d R
H52 H 0.392(3) 0.328(5) 0.2343(7) 0.090(8) Uiso 1 1 d .
H51 H 0.262(4) 0.426(5) 0.2287(8) 0.098(8) Uiso 1 1 d .
H41 H 0.579(3) 0.647(5) 0.2255(7) 0.082(8) Uiso 1 1 d .
H42 H 0.720(4) 0.596(6) 0.2208(9) 0.116(9) Uiso 1 1 d .
H3 H 0.774(3) 0.320(5) 0.1765(7) 0.097(8) Uiso 1 1 d .
H2 H 0.164(5) 0.501(6) 0.1685(10) 0.117(11) 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
C1 0.0423(10) 0.1307(19) 0.0588(11) 0.0037(12) 0.0097(8) 0.0020(10)
Cl1 0.0415(4) 0.1629(8) 0.0739(5) -0.0011(3) 0.0090(3) -0.0103(3)
N1 0.0418(9) 0.1561(18) 0.0643(10) -0.0049(11) 0.0079(7) 0.0080(10)
C2 0.0436(11) 0.135(2) 0.0651(12) 0.0025(12) 0.0086(9) 0.0043(11)
N2 0.0413(10) 0.174(2) 0.0704(12) 0.0123(11) 0.0114(9) 0.0127(10)
C3 0.0480(12) 0.138(2) 0.0673(13) 0.0072(12) 0.0055(10) 0.0189(11)
N3 0.0376(9) 0.1453(19) 0.0712(11) -0.0086(11) 0.0074(8) 0.0004(10)
C4 0.0766(15) 0.141(2) 0.0896(16) 0.0157(16) 0.0035(13) 0.0037(16)
N4 0.0451(11) 0.179(2) 0.0749(13) -0.0257(13) 0.0140(10) -0.0027(13)
C5 0.098(2) 0.176(3) 0.0926(19) 0.037(2) 0.0131(17) 0.023(2)
N5 0.0434(10) 0.185(2) 0.0672(12) 0.0157(13) 0.0124(9) 0.0085(13)
C6 0.109(3) 0.175(3) 0.0776(18) 0.011(2) 0.0142(18) 0.049(2)
C7 0.108(2) 0.162(3) 0.100(2) -0.022(2) -0.0231(19) 0.020(2)
C8 0.0721(15) 0.155(3) 0.0975(18) 0.0072(18) -0.0021(14) -0.0008(17)
C9 0.0490(10) 0.1127(19) 0.0762(13) 0.0004(12) 0.0194(9) -0.0070(11)
C10 0.0836(19) 0.125(2) 0.106(2) 0.0140(16) 0.0227(17) 0.0209(15)
C11 0.149(3) 0.126(3) 0.132(3) -0.014(2) 0.052(3) 0.034(2)
C12 0.137(3) 0.133(2) 0.098(2) -0.027(2) 0.040(2) -0.005(2)
C13 0.098(2) 0.158(3) 0.0738(15) -0.0075(17) 0.0152(14) -0.009(2)
C14 0.0737(14) 0.143(2) 0.0737(14) -0.0087(14) 0.0098(11) 0.0145(15)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 '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_publ_flag
N1 C1 N3 116.26(19) y
N1 C1 N4 127.1(2) y
N3 C1 N4 116.6(2) y
C1 N1 C2 122.68(18) y
N1 C2 N2 115.9(2) y
N1 C2 N5 126.3(2) y
N2 C2 N5 117.7(2) y
C2 N2 C3 126.5(2) y
C2 N2 H2 115(3) ?
C3 N2 H2 118(3) ?
C8 C3 C4 118.1(2) y
C8 C3 N2 120.2(2) y
C4 C3 N2 121.7(2) y
C1 N3 C9 129.96(18) y
C1 N3 H3 112.30(19) ?
C9 N3 H3 117.50(19) ?
C3 C4 C5 120.2(3) y
C3 C4 H4 119.8 ?
C5 C4 H4 119.9 ?
C1 N4 H41 123.90(18) ?
C1 N4 H42 119(2) ?
H41 N4 H42 116(3) ?
C6 C5 C4 122.1(3) y
C6 C5 H5 118.7 ?
C4 C5 H5 119.2 ?
C2 N5 H52 119.70(18) ?
C2 N5 H51 120(2) ?
H52 N5 H51 114(3) ?
C7 C6 C5 117.8(3) y
C7 C6 H6 120.9 ?
C5 C6 H6 121.3 ?
C6 C7 C8 121.8(3) y
C6 C7 H7 118.8 ?
C8 C7 H7 119.4 ?
C3 C8 C7 120.0(3) y
C3 C8 H8 120 ?
C7 C8 H8 120 ?
C10 C9 C14 117.7(2) y
C10 C9 N3 117.5(2) y
C14 C9 N3 124.5(2) y
C9 C10 C11 118.9(3) y
C9 C10 H10 120.7 ?
C11 C10 H10 120.4 ?
C12 C11 C10 122.8(3) y
C12 C11 H11 118.4 ?
C10 C11 H11 118.8 ?
C13 C12 C11 117.4(3) y
C13 C12 H12 121 ?
C11 C12 H12 121.6 ?
C12 C13 C14 121.3(3) y
C12 C13 H13 119.2 ?
C14 C13 H13 119.4 ?
C9 C14 C13 121.8(3) y
C9 C14 H14 119.3 ?
C13 C14 H14 119 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
C1 N1 1.343(3) y
C1 N3 1.375(3) y
C1 N4 1.378(3) y
N1 C2 1.351(3) y
C2 N2 1.364(3) y
C2 N5 1.394(3) y
N2 C3 1.487(3) y
N2 H2 0.75(4) ?
C3 C8 1.406(4) y
C3 C4 1.423(4) y
N3 C9 1.479(3) y
N3 H3 0.81(3) ?
C4 C5 1.433(4) y
C4 H4 0.93 ?
N4 H41 0.78(3) ?
N4 H42 0.87(4) ?
C5 C6 1.397(5) y
C5 H5 0.93 ?
N5 H52 0.81(3) ?
N5 H51 0.79(3) ?
C6 C7 1.387(5) y
C6 H6 0.93 ?
C7 C8 1.459(4) y
C7 H7 0.93 ?
C8 H8 0.93 ?
C9 C10 1.410(4) y
C9 C14 1.423(3) y
C10 C11 1.457(5) y
C10 H10 0.93 ?
C11 C12 1.417(5) y
C11 H11 0.93 ?
C12 C13 1.374(5) y
C12 H12 0.93 ?
C13 C14 1.445(4) y
C13 H13 0.93 ?
C14 H14 0.93 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N5 H52 CL1 0.81(3) 2.59(3) 3.385(3) 166(2) 2_645
N5 H51 CL1 0.79(3) 2.69(4) 3.410(3) 152(3) 1_455
N4 H41 N5 0.78(3) 2.60(3) 2.966(4) 111(2) .
N4 H41 CL1 0.78(3) 2.75(2) 3.456(3) 153(2) 2_655
N4 H42 CL1 0.87(4) 2.60(4) 3.396(3) 152(3) .
N3 H3 CL1 0.81(3) 2.51(3) 3.296(2) 166(2) .
N2 H2 CL1 0.75(4) 2.58(4) 3.308(2) 165(4) 1_455
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
N3 C1 N1 C2 163.4(2) y
N4 C1 N1 C2 -19.2(4) y
C1 N1 C2 N2 156.1(3) y
C1 N1 C2 N5 -26.4(4) y
N1 C2 N2 C3 -1.4(4) y
N5 C2 N2 C3 -179.1(3) y
C2 N2 C3 C8 122.5(3) y
C2 N2 C3 C4 -58.9(4) y
N1 C1 N3 C9 8.3(4) y
N4 C1 N3 C9 -169.4(2) y
C8 C3 C4 C5 -1.3(4) y
N2 C3 C4 C5 -179.8(2) y
C3 C4 C5 C6 0.9(5) y
C4 C5 C6 C7 0.4(5) y
C5 C6 C7 C8 -1.2(5) y
C4 C3 C8 C7 0.4(4) y
N2 C3 C8 C7 179.0(2) y
C6 C7 C8 C3 0.8(5) y
C1 N3 C9 C10 -152.7(3) y
C1 N3 C9 C14 33.7(4) y
C14 C9 C10 C11 -0.7(4) y
N3 C9 C10 C11 -174.7(3) y
C9 C10 C11 C12 1.0(5) y
C10 C11 C12 C13 -1.0(6) y
C11 C12 C13 C14 0.7(5) y
C10 C9 C14 C13 0.3(4) y
N3 C9 C14 C13 174.0(2) y
C12 C13 C14 C9 -0.4(5) y
|
1501608.cif | #------------------------------------------------------------------------------
#$Date: 2017-10-13 02:32:00 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201954 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/50/16/1501608.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_1501608
loop_
_publ_author_name
'Olivier LeBel'
'Thierry Maris'
'Hugues Duval'
'James D. Wuest'
_publ_section_title
;
A practical guide to arylbiguanides --- Synthesis and structural
characterization
;
_journal_name_full 'Can. J. Chem.'
_journal_page_first 615
_journal_page_last 625
_journal_paper_doi 10.1139/v05-093
_journal_volume 83
_journal_year 2005
_chemical_compound_source 'Synthesized by the authors. See text'
_chemical_formula_moiety 'C14 H15 N5'
_chemical_formula_sum 'C14 H15 N5'
_chemical_formula_weight 253.31
_chemical_name_systematic
;
?
;
_space_group_IT_number 7
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall 'P -2yc'
_symmetry_space_group_name_H-M 'P 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 99.588(2)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 9.0317(3)
_cell_length_b 6.3945(2)
_cell_length_c 22.5874(8)
_cell_measurement_reflns_used 4072
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 71.97
_cell_measurement_theta_min 3.97
_cell_volume 1286.27(7)
_computing_cell_refinement 'SMART (Bruker, 1999)'
_computing_data_collection 'SMART (Bruker, 1999)'
_computing_data_reduction 'SAINT (Bruker, 1999)'
_computing_molecular_graphics 'SHELXTL (Bruker, 1997)'
_computing_publication_material 'UdMX (local program)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type 'Bruker Smart 2000'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'X-ray Sealed Tube'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.035
_diffrn_reflns_av_sigmaI/netI 0.1470
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 7
_diffrn_reflns_limit_k_min -7
_diffrn_reflns_limit_l_max 27
_diffrn_reflns_limit_l_min -27
_diffrn_reflns_number 7271
_diffrn_reflns_theta_full 71.96
_diffrn_reflns_theta_max 71.96
_diffrn_reflns_theta_min 3.97
_diffrn_standards_decay_% 0.23
_diffrn_standards_number 88
_exptl_absorpt_coefficient_mu 0.663
_exptl_absorpt_correction_T_max 0.980
_exptl_absorpt_correction_T_min 0.890
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Sadabs (Sheldrick,1996)'
_exptl_crystal_colour Colorless
_exptl_crystal_density_diffrn 1.308
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 536
_exptl_crystal_size_max 0.20
_exptl_crystal_size_mid 0.12
_exptl_crystal_size_min 0.03
_refine_diff_density_max 0.321
_refine_diff_density_min -0.327
_refine_diff_density_rms 0.081
_refine_ls_abs_structure_details 'friedel pairs merged'
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.024
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 343
_refine_ls_number_reflns 2530
_refine_ls_number_restraints 470
_refine_ls_restrained_S_all 0.951
_refine_ls_R_factor_all 0.0745
_refine_ls_R_factor_gt 0.0673
_refine_ls_shift/su_max 0.006
_refine_ls_shift/su_mean 0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0550P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1525
_refine_ls_wR_factor_ref 0.1551
_reflns_number_gt 1570
_reflns_number_total 2530
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file deposit.cif
_cod_data_source_block jiw810
_cod_original_sg_symbol_H-M Pc
_cod_database_code 1501608
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.2462(5) 1.0997(7) 0.5942(2) 0.0289(11) Uani 1 1 d U A 1
H1 H 0.1690 1.1806 0.5973 0.035 Uiso 1 1 calc . B 1
N2 N 0.1873(5) 0.9199(7) 0.6749(2) 0.0277(11) Uani 1 1 d U A 1
H2A H 0.2020 0.8204 0.7022 0.033 Uiso 1 1 calc . C 1
H2B H 0.1102 1.0050 0.6734 0.033 Uiso 1 1 calc . D 1
N3 N 0.3993(5) 0.8273(7) 0.6331(2) 0.0294(11) Uani 1 1 d U A 1
N4 N 0.5797(5) 0.5783(7) 0.6643(2) 0.0286(11) Uani 1 1 d U A 1
H4A H 0.6258 0.4862 0.6899 0.034 Uiso 1 1 calc . E 1
H4B H 0.6174 0.6113 0.6320 0.034 Uiso 1 1 calc . F 1
N5 N 0.3843(5) 0.6288(7) 0.7230(2) 0.0263(10) Uani 1 1 d U A 1
C1 C 0.3258(6) 1.1396(9) 0.5471(3) 0.0275(12) Uani 1 1 d U A 1
C2 C 0.3665(6) 0.9785(9) 0.5097(2) 0.0254(12) Uani 1 1 d U A 1
H2 H 0.3357 0.8382 0.5142 0.030 Uiso 1 1 calc . G 1
C3 C 0.4532(6) 1.0314(9) 0.4659(2) 0.0278(12) Uani 1 1 d U A 1
H3 H 0.4829 0.9236 0.4414 0.033 Uiso 1 1 calc . H 1
C4 C 0.4963(6) 1.2305(10) 0.4571(2) 0.0299(13) Uani 1 1 d U A 1
H4 H 0.5563 1.2610 0.4274 0.036 Uiso 1 1 calc . I 1
C5 C 0.4508(6) 1.3914(9) 0.4927(3) 0.0300(13) Uani 1 1 d U A 1
H5 H 0.4774 1.5322 0.4860 0.036 Uiso 1 1 calc . J 1
C6 C 0.3690(6) 1.3470(9) 0.5365(3) 0.0276(13) Uani 1 1 d U A 1
H6 H 0.3404 1.4573 0.5603 0.033 Uiso 1 1 calc . K 1
C7 C 0.2810(6) 0.9413(9) 0.6362(2) 0.0266(12) Uani 1 1 d U A 1
C8 C 0.4444(6) 0.6740(8) 0.6751(2) 0.0255(12) Uani 1 1 d U A 1
C9 C 0.4642(7) 0.4857(8) 0.7643(2) 0.0247(12) Uani 1 1 d U A 1
C10 C 0.5920(6) 0.5408(9) 0.8040(2) 0.0256(12) Uani 1 1 d U A 1
H10 H 0.6288 0.6802 0.8047 0.031 Uiso 1 1 calc . L 1
C11 C 0.6662(6) 0.3924(9) 0.8426(3) 0.0273(12) Uani 1 1 d U A 1
H11 H 0.7530 0.4322 0.8701 0.033 Uiso 1 1 calc . M 1
C12 C 0.6171(6) 0.1886(9) 0.8420(2) 0.0255(12) Uani 1 1 d U A 1
H12 H 0.6723 0.0876 0.8675 0.031 Uiso 1 1 calc . N 1
C13 C 0.4883(6) 0.1322(9) 0.8044(2) 0.0266(12) Uani 1 1 d U A 1
H13 H 0.4530 -0.0077 0.8045 0.032 Uiso 1 1 calc . O 1
C14 C 0.4080(6) 0.2806(9) 0.7657(3) 0.0300(13) Uani 1 1 d U A 1
H14 H 0.3167 0.2428 0.7407 0.036 Uiso 1 1 calc . P 1
N21 N 0.7941(5) -0.0685(7) 0.70783(19) 0.0245(10) Uani 1 1 d U A 1
H21A H 0.7120 -0.1440 0.7060 0.029 Uiso 1 1 calc . R 1
N22 N 0.6655(5) 0.1088(7) 0.6280(2) 0.0265(11) Uani 1 1 d U A 1
H22A H 0.6577 0.2070 0.6004 0.032 Uiso 1 1 calc . S 1
H22B H 0.5888 0.0258 0.6302 0.032 Uiso 1 1 calc . T 1
N23 N 0.9171(5) 0.1988(7) 0.66855(19) 0.0228(10) Uani 1 1 d U A 1
N24 N 1.0649(5) 0.4462(7) 0.6387(2) 0.0266(11) Uani 1 1 d U A 1
H24A H 1.0909 0.5412 0.6142 0.032 Uiso 1 1 calc . U 1
H24B H 1.1280 0.4099 0.6710 0.032 Uiso 1 1 calc . V 1
N25 N 0.8262(5) 0.3983(7) 0.5801(2) 0.0256(10) Uani 1 1 d U A 1
C21 C 0.9150(6) -0.1179(8) 0.7532(2) 0.0232(12) Uani 1 1 d U A 1
C22 C 0.9871(6) 0.0368(9) 0.7919(2) 0.0247(12) Uani 1 1 d U A 1
H22 H 0.9524 0.1773 0.7890 0.030 Uiso 1 1 calc . W 1
C23 C 1.1118(6) -0.0206(9) 0.8351(2) 0.0263(12) Uani 1 1 d U A 1
H23 H 1.1676 0.0843 0.8589 0.032 Uiso 1 1 calc . X 1
C24 C 1.1546(6) -0.2319(9) 0.8433(3) 0.0271(12) Uani 1 1 d U A 1
H24 H 1.2390 -0.2705 0.8722 0.032 Uiso 1 1 calc . y 1
C25 C 1.0713(6) -0.3814(9) 0.8085(2) 0.0223(11) Uani 1 1 d U A 1
H25 H 1.0952 -0.5249 0.8156 0.027 Uiso 1 1 calc . Z 1
C26 C 0.9565(6) -0.3291(8) 0.7645(2) 0.0227(12) Uani 1 1 d U A 1
H26 H 0.9029 -0.4361 0.7408 0.027 Uiso 1 1 calc . A 1
C27 C 0.7930(6) 0.0858(8) 0.6665(2) 0.0221(11) Uani 1 1 d U A 1
C28 C 0.9253(6) 0.3543(8) 0.6264(3) 0.0250(12) Uani 1 1 d U A 1
C29 C 0.8710(6) 0.5517(9) 0.5404(2) 0.0228(11) Uani 1 1 d U A 1
C30 C 0.9699(6) 0.5019(9) 0.5020(2) 0.0246(12) Uani 1 1 d U A 1
H30 H 1.0115 0.3654 0.5026 0.030 Uiso 1 1 calc . B 1
C31 C 1.0077(6) 0.6479(9) 0.4633(3) 0.0289(12) Uani 1 1 d U A 1
H31 H 1.0711 0.6104 0.4354 0.035 Uiso 1 1 calc . C 1
C32 C 0.9538(6) 0.8532(9) 0.4642(2) 0.0239(12) Uani 1 1 d U A 1
H32 H 0.9875 0.9582 0.4398 0.029 Uiso 1 1 calc . D 1
C33 C 0.8490(6) 0.9015(9) 0.5020(2) 0.0251(12) Uani 1 1 d U A 1
H33 H 0.8077 1.0382 0.5016 0.030 Uiso 1 1 calc . E 1
C34 C 0.8064(7) 0.7517(9) 0.5393(3) 0.0314(13) Uani 1 1 d U A 1
H34 H 0.7341 0.7830 0.5641 0.038 Uiso 1 1 calc . F 1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
N1 0.025(2) 0.031(2) 0.029(2) 0.0032(18) -0.0006(19) -0.0030(19)
N2 0.025(2) 0.029(2) 0.027(2) 0.0027(19) -0.0019(19) -0.0035(18)
N3 0.025(2) 0.028(2) 0.033(2) 0.0075(18) -0.0018(19) 0.0033(18)
N4 0.028(2) 0.031(2) 0.025(2) -0.0023(18) -0.0017(19) -0.0013(19)
N5 0.024(2) 0.026(2) 0.029(2) 0.0042(18) 0.0032(19) -0.0049(18)
C1 0.025(2) 0.029(2) 0.028(2) 0.003(2) 0.004(2) -0.004(2)
C2 0.023(2) 0.026(3) 0.026(2) 0.005(2) 0.001(2) 0.004(2)
C3 0.032(3) 0.027(3) 0.024(2) -0.001(2) 0.002(2) 0.008(2)
C4 0.030(3) 0.033(3) 0.026(3) 0.008(2) 0.003(2) 0.001(2)
C5 0.027(3) 0.029(3) 0.033(3) 0.001(2) 0.002(2) 0.005(2)
C6 0.028(3) 0.024(2) 0.029(3) 0.001(2) 0.002(2) 0.004(2)
C7 0.023(2) 0.028(3) 0.027(2) 0.009(2) 0.002(2) -0.002(2)
C8 0.024(2) 0.025(2) 0.026(2) -0.0015(19) -0.001(2) -0.002(2)
C9 0.030(2) 0.023(2) 0.020(2) 0.0046(19) 0.001(2) 0.002(2)
C10 0.024(2) 0.026(3) 0.024(2) -0.002(2) -0.002(2) -0.003(2)
C11 0.027(2) 0.025(2) 0.028(2) 0.001(2) -0.001(2) 0.002(2)
C12 0.025(2) 0.025(2) 0.025(3) 0.005(2) 0.000(2) 0.006(2)
C13 0.026(3) 0.029(3) 0.025(3) 0.005(2) 0.007(2) 0.007(2)
C14 0.031(3) 0.030(3) 0.026(3) 0.003(2) -0.002(2) -0.005(2)
N21 0.026(2) 0.023(2) 0.024(2) 0.0001(17) 0.0036(18) -0.0003(17)
N22 0.026(2) 0.024(2) 0.029(2) 0.0042(18) 0.0019(19) -0.0042(18)
N23 0.024(2) 0.023(2) 0.018(2) 0.0006(17) -0.0062(17) -0.0009(17)
N24 0.023(2) 0.028(2) 0.027(2) 0.0020(18) -0.0004(19) -0.0014(18)
N25 0.024(2) 0.025(2) 0.027(2) 0.0055(18) 0.0040(19) 0.0048(18)
C21 0.024(2) 0.021(2) 0.023(2) 0.0052(19) 0.001(2) -0.0030(19)
C22 0.017(2) 0.029(3) 0.026(2) -0.005(2) -0.003(2) -0.002(2)
C23 0.024(2) 0.027(3) 0.026(2) 0.003(2) 0.001(2) -0.002(2)
C24 0.026(3) 0.028(3) 0.026(3) 0.008(2) 0.001(2) 0.006(2)
C25 0.021(2) 0.023(2) 0.023(2) 0.0040(19) 0.006(2) 0.0001(19)
C26 0.017(2) 0.025(2) 0.027(2) 0.001(2) 0.003(2) -0.002(2)
C27 0.026(2) 0.019(2) 0.022(2) -0.0018(18) 0.006(2) -0.0015(19)
C28 0.027(2) 0.024(2) 0.024(2) 0.0017(19) 0.006(2) -0.0046(19)
C29 0.023(2) 0.028(2) 0.017(2) 0.0007(19) 0.0021(19) -0.001(2)
C30 0.026(2) 0.021(2) 0.026(2) 0.001(2) 0.002(2) 0.005(2)
C31 0.031(3) 0.028(3) 0.025(2) -0.001(2) -0.002(2) 0.002(2)
C32 0.020(2) 0.027(3) 0.025(2) 0.0045(19) 0.004(2) -0.007(2)
C33 0.030(3) 0.024(3) 0.020(2) 0.0032(19) 0.000(2) 0.000(2)
C34 0.033(3) 0.033(3) 0.028(3) -0.003(2) 0.003(2) 0.004(2)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
C7 N1 C1 124.4(5) y
C7 N1 H1 117.8 ?
C1 N1 H1 117.8 ?
C7 N2 H2A 120 ?
C7 N2 H2B 120 ?
H2A N2 H2B 120 ?
C7 N3 C8 120.8(5) y
C8 N4 H4A 120 ?
C8 N4 H4B 120 ?
H4A N4 H4B 120 ?
C8 N5 C9 116.6(5) y
N1 C1 C6 119.4(5) y
N1 C1 C2 122.4(5) y
C6 C1 C2 118.2(5) y
C3 C2 C1 118.4(5) y
C3 C2 H2 120.8 ?
C1 C2 H2 120.8 ?
C4 C3 C2 122.5(5) y
C4 C3 H3 118.7 ?
C2 C3 H3 118.7 ?
C3 C4 C5 119.0(5) y
C3 C4 H4 120.5 ?
C5 C4 H4 120.5 ?
C6 C5 C4 120.5(5) y
C6 C5 H5 119.7 ?
C4 C5 H5 119.7 ?
C5 C6 C1 121.3(5) y
C5 C6 H6 119.4 ?
C1 C6 H6 119.4 ?
N3 C7 N2 126.7(5) y
N3 C7 N1 117.7(5) y
N2 C7 N1 115.5(5) y
N5 C8 N3 127.2(5) y
N5 C8 N4 121.9(5) y
N3 C8 N4 110.6(5) y
C10 C9 C14 119.1(5) y
C10 C9 N5 122.7(5) y
C14 C9 N5 118.1(5) y
C11 C10 C9 119.8(5) y
C11 C10 H10 120.1 ?
C9 C10 H10 120.1 ?
C12 C11 C10 121.5(5) y
C12 C11 H11 119.3 ?
C10 C11 H11 119.3 ?
C13 C12 C11 119.6(5) y
C13 C12 H12 120.2 ?
C11 C12 H12 120.2 ?
C12 C13 C14 120.3(5) y
C12 C13 H13 119.9 ?
C14 C13 H13 119.9 ?
C13 C14 C9 119.5(5) y
C13 C14 H14 120.3 ?
C9 C14 H14 120.3 ?
C27 N21 C21 125.6(5) y
C27 N21 H21A 117.2 ?
C21 N21 H21A 117.2 ?
C27 N22 H22A 120 ?
C27 N22 H22B 120 ?
H22A N22 H22B 120 ?
C27 N23 C28 120.5(4) y
C28 N24 H24A 120 ?
C28 N24 H24B 120 ?
H24A N24 H24B 120 ?
C28 N25 C29 115.3(5) y
N21 C21 C22 121.3(5) y
N21 C21 C26 119.9(5) y
C22 C21 C26 118.6(5) y
C21 C22 C23 118.7(5) y
C21 C22 H22 120.7 ?
C23 C22 H22 120.6 ?
C24 C23 C22 120.7(5) y
C24 C23 H23 119.6 ?
C22 C23 H23 119.6 ?
C25 C24 C23 118.6(5) y
C25 C24 H24 120.7 ?
C23 C24 H24 120.7 ?
C26 C25 C24 121.7(5) y
C26 C25 H25 119.2 ?
C24 C25 H25 119.2 ?
C25 C26 C21 121.2(5) y
C25 C26 H26 119.4 ?
C21 C26 H26 119.4 ?
N23 C27 N22 126.6(5) y
N23 C27 N21 117.5(5) y
N22 C27 N21 115.9(5) y
N25 C28 N24 124.0(5) y
N25 C28 N23 127.1(5) y
N24 C28 N23 108.6(5) y
C30 C29 C34 120.6(5) y
C30 C29 N25 121.0(5) y
C34 C29 N25 118.3(5) y
C31 C30 C29 120.2(5) y
C31 C30 H30 119.9 ?
C29 C30 H30 119.9 ?
C30 C31 C32 120.6(5) y
C30 C31 H31 119.7 ?
C32 C31 H31 119.7 ?
C31 C32 C33 118.9(5) y
C31 C32 H32 120.5 ?
C33 C32 H32 120.5 ?
C34 C33 C32 120.2(5) y
C34 C33 H33 119.9 ?
C32 C33 H33 119.9 ?
C33 C34 C29 119.2(5) y
C33 C34 H34 120.4 ?
C29 C34 H34 120.4 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
N1 C7 1.388(7) y
N1 C1 1.402(7) y
N1 H1 0.88 ?
N2 C7 1.322(7) y
N2 H2a 0.8801 ?
N2 H2b 0.88 ?
N3 C7 1.305(7) y
N3 C8 1.377(6) y
N4 C8 1.424(7) y
N4 H4a 0.8801 ?
N4 H4b 0.8799 ?
N5 C8 1.320(7) y
N5 C9 1.416(7) y
C1 C6 1.415(8) y
C1 C2 1.419(8) y
C2 C3 1.402(7) y
C2 H2 0.95 ?
C3 C4 1.356(8) y
C3 H3 0.9499 ?
C4 C5 1.408(8) y
C4 H4 0.9499 ?
C5 C6 1.359(8) y
C5 H5 0.95 ?
C6 H6 0.9501 ?
C9 C10 1.385(8) y
C9 C14 1.408(8) y
C10 C11 1.384(8) y
C10 H10 0.95 ?
C11 C12 1.376(8) y
C11 H11 0.9501 ?
C12 C13 1.369(8) y
C12 H12 0.9501 ?
C13 C14 1.407(7) y
C13 H13 0.95 ?
C14 H14 0.9499 ?
N21 C27 1.357(6) y
N21 C21 1.403(7) y
N21 H21a 0.88 ?
N22 C27 1.331(6) y
N22 H22a 0.8799 ?
N22 H22b 0.88 ?
N23 C27 1.328(7) y
N23 C28 1.387(6) y
N24 C28 1.376(7) y
N24 H24a 0.8799 ?
N24 H24b 0.8801 ?
N25 C28 1.289(7) y
N25 C29 1.433(7) y
C21 C22 1.406(7) y
C21 C26 1.413(7) y
C22 C23 1.410(7) y
C22 H22 0.95 ?
C23 C24 1.409(8) y
C23 H23 0.9501 ?
C24 C25 1.378(8) y
C24 H24 0.9501 ?
C25 C26 1.353(7) y
C25 H25 0.95 ?
C26 H26 0.9499 ?
C29 C30 1.381(7) y
C29 C34 1.404(8) y
C30 C31 1.360(8) y
C30 H30 0.95 ?
C31 C32 1.401(8) y
C31 H31 0.9499 ?
C32 C33 1.410(7) y
C32 H32 0.9499 ?
C33 C34 1.373(8) y
C33 H33 0.95 ?
C34 H34 0.9501 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H2A N5 0.88 2.04 2.677(6) 128.0 .
N2 H2B N23 0.88 2.13 3.007(6) 177.3 1_465
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
C7 N1 C1 C6 -132.5(6) y
C7 N1 C1 C2 46.8(8) y
N1 C1 C2 C3 -176.5(5) y
C6 C1 C2 C3 2.9(8) y
C1 C2 C3 C4 -1.6(9) y
C2 C3 C4 C5 -0.9(9) y
C3 C4 C5 C6 2.2(9) y
C4 C5 C6 C1 -0.8(9) y
N1 C1 C6 C5 177.7(5) y
C2 C1 C6 C5 -1.7(8) y
C8 N3 C7 N2 -4.5(9) y
C8 N3 C7 N1 176.9(4) y
C1 N1 C7 N3 2.9(8) y
C1 N1 C7 N2 -175.9(5) y
C9 N5 C8 N3 -170.7(5) y
C9 N5 C8 N4 2.2(7) y
C7 N3 C8 N5 -3.4(8) y
C7 N3 C8 N4 -177.0(5) y
C8 N5 C9 C10 76.2(7) y
C8 N5 C9 C14 -105.4(6) y
C14 C9 C10 C11 2.7(9) y
N5 C9 C10 C11 -179.0(5) y
C9 C10 C11 C12 1.0(9) y
C10 C11 C12 C13 -3.0(9) y
C11 C12 C13 C14 1.3(8) y
C12 C13 C14 C9 2.3(8) y
C10 C9 C14 C13 -4.3(9) y
N5 C9 C14 C13 177.3(5) y
C27 N21 C21 C22 51.1(7) y
C27 N21 C21 C26 -135.2(5) y
N21 C21 C22 C23 -177.4(5) y
C26 C21 C22 C23 8.8(8) y
C21 C22 C23 C24 -6.1(8) y
C22 C23 C24 C25 -0.4(8) y
C23 C24 C25 C26 4.2(8) y
C24 C25 C26 C21 -1.4(8) y
N21 C21 C26 C25 -179.1(5) y
C22 C21 C26 C25 -5.3(8) y
C28 N23 C27 N22 -2.7(8) y
C28 N23 C27 N21 177.8(5) y
C21 N21 C27 N23 0.7(7) y
C21 N21 C27 N22 -178.8(5) y
C29 N25 C28 N24 0.7(8) y
C29 N25 C28 N23 -173.3(5) y
C27 N23 C28 N25 -5.2(8) y
C27 N23 C28 N24 -179.9(5) y
C28 N25 C29 C30 75.4(7) y
C28 N25 C29 C34 -107.6(6) y
C34 C29 C30 C31 1.1(9) y
N25 C29 C30 C31 178.1(5) y
C29 C30 C31 C32 3.6(9) y
C30 C31 C32 C33 -5.8(9) y
C31 C32 C33 C34 3.2(8) y
C32 C33 C34 C29 1.4(9) y
C30 C29 C34 C33 -3.6(9) y
N25 C29 C34 C33 179.3(5) y
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 14594618
|
1501609.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/16/1501609.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_1501609
loop_
_publ_author_name
'Dominic Lalibert\'e'
'Thierry Maris'
'James D. Wuest'
_publ_section_title
;
Molecular tectonics - Use of urethanes and ureas derived from
tetraphenylmethane and tetraphenylsilane to build porous chiral
hydrogenbonded networks
;
_journal_name_full 'Can. J. Chem.'
_journal_page_first 386
_journal_page_last 398
_journal_paper_doi 10.1139/v03-208
_journal_volume 82
_journal_year 2004
_chemical_compound_source 'Synthesized by the authors. See text'
_chemical_formula_sum 'C29 H16 N4 S4'
_chemical_formula_weight 548.70
_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 95.89
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 11.6490(1)
_cell_length_b 11.4547(1)
_cell_length_c 20.5132(1)
_cell_measurement_reflns_used 20454
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 72.83
_cell_measurement_theta_min 2.17
_cell_volume 2722.74(4)
_computing_cell_refinement 'SMART (Bruker, 1999)'
_computing_data_collection 'SAINT (Bruker, 1999)'
_computing_data_reduction 'SAINT (Bruker, 1999)'
_computing_molecular_graphics 'XP (Bruker, 1999)'
_computing_publication_material 'UdMX (local program)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type 'Bruker Smart 2K'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'Sealed Tube'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.026
_diffrn_reflns_av_sigmaI/netI 0.0182
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 25
_diffrn_reflns_limit_l_min -25
_diffrn_reflns_number 33047
_diffrn_reflns_theta_full 72.91
_diffrn_reflns_theta_max 72.91
_diffrn_reflns_theta_min 4.19
_diffrn_standards_decay_% -0.11
_diffrn_standards_number 236
_exptl_absorpt_coefficient_mu 3.407
_exptl_absorpt_correction_T_max 0.5900
_exptl_absorpt_correction_T_min 0.3600
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Sadabs (Sheldrick,1996)'
_exptl_crystal_colour Colourless
_exptl_crystal_density_diffrn 1.339
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 1128
_exptl_crystal_size_max 0.44
_exptl_crystal_size_mid 0.20
_exptl_crystal_size_min 0.16
_refine_diff_density_max 0.963
_refine_diff_density_min -0.517
_refine_diff_density_rms 0.052
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.056
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 341
_refine_ls_number_reflns 5381
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.056
_refine_ls_R_factor_all 0.0711
_refine_ls_R_factor_gt 0.0609
_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^)+(0.0970P)^2^+1.3029P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1727
_refine_ls_wR_factor_ref 0.1810
_reflns_number_gt 4354
_reflns_number_total 5381
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file deposit.cif
_cod_data_source_block jiw336
_cod_original_cell_volume 2722.75(4)
_cod_original_sg_symbol_H-M P21/n
_cod_database_code 1501609
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3824(2) 0.4585(2) 0.20543(11) 0.0445(5) Uani 1 1 d . . .
C10 C 0.4410(2) 0.5504(2) 0.16452(12) 0.0502(6) Uani 1 1 d . . .
C11 C 0.3905(3) 0.6600(2) 0.15570(13) 0.0577(7) Uani 1 1 d . . .
H11 H 0.3216 0.6752 0.1734 0.069 Uiso 1 1 calc . . .
C12 C 0.4401(3) 0.7468(2) 0.12130(15) 0.0681(8) Uani 1 1 d . . .
H12 H 0.4048 0.8194 0.1159 0.082 Uiso 1 1 calc . . .
C13 C 0.5410(3) 0.7258(3) 0.09521(16) 0.0726(9) Uani 1 1 d . . .
C14 C 0.5939(3) 0.6197(3) 0.1044(2) 0.0862(11) Uani 1 1 d . . .
H14 H 0.6631 0.6057 0.0868 0.103 Uiso 1 1 calc . . .
C15 C 0.5450(3) 0.5329(3) 0.13962(18) 0.0707(8) Uani 1 1 d . . .
H15 H 0.5830 0.4619 0.1466 0.085 Uiso 1 1 calc . . .
N16 N 0.5913(3) 0.8123(3) 0.05968(17) 0.0988(11) Uani 1 1 d . . .
C17 C 0.6274(3) 0.8971(3) 0.03949(14) 0.0632(7) Uani 1 1 d . . .
S18 S 0.67897(8) 1.01007(7) 0.01083(4) 0.0734(3) Uani 1 1 d . . .
C20 C 0.2550(2) 0.4388(2) 0.17882(12) 0.0466(5) Uani 1 1 d . . .
C21 C 0.2102(3) 0.4742(3) 0.11680(14) 0.0625(7) Uani 1 1 d . . .
H21 H 0.2567 0.5154 0.0906 0.075 Uiso 1 1 calc . . .
C22 C 0.0976(3) 0.4492(3) 0.09318(15) 0.0737(9) Uani 1 1 d . . .
H22 H 0.0691 0.4735 0.0514 0.088 Uiso 1 1 calc . . .
C23 C 0.0275(3) 0.3885(3) 0.13130(17) 0.0665(8) Uani 1 1 d . . .
C24 C 0.0707(2) 0.3499(2) 0.19248(16) 0.0601(7) Uani 1 1 d . . .
H24 H 0.0243 0.3075 0.2182 0.072 Uiso 1 1 calc . . .
C25 C 0.1832(2) 0.3747(2) 0.21522(13) 0.0525(6) Uani 1 1 d . . .
H25 H 0.2121 0.3476 0.2564 0.063 Uiso 1 1 calc . . .
N26 N -0.0867(3) 0.3647(3) 0.10775(17) 0.0925(10) Uani 1 1 d . . .
C27 C -0.1700(3) 0.3545(3) 0.07390(15) 0.0634(7) Uani 1 1 d . . .
y8 S -0.28763(9) 0.33687(11) 0.03042(5) 0.0979(4) Uani 1 1 d . . .
C30 C 0.4369(2) 0.33562(19) 0.20265(11) 0.0426(5) Uani 1 1 d . . .
C31 C 0.4538(3) 0.2852(2) 0.14249(13) 0.0549(6) Uani 1 1 d . . .
H31 H 0.4316 0.3263 0.1042 0.066 Uiso 1 1 calc . . .
C32 C 0.5026(3) 0.1763(2) 0.13828(14) 0.0602(7) Uani 1 1 d . . .
H32 H 0.5139 0.1449 0.0976 0.072 Uiso 1 1 calc . . .
C33 C 0.5344(2) 0.1139(2) 0.19508(14) 0.0530(6) Uani 1 1 d . . .
C34 C 0.5116(3) 0.1580(2) 0.25485(13) 0.0542(6) Uani 1 1 d . . .
H34 H 0.5283 0.1141 0.2928 0.065 Uiso 1 1 calc . . .
C35 C 0.4633(2) 0.2683(2) 0.25810(12) 0.0496(6) Uani 1 1 d . . .
H35 H 0.4484 0.2978 0.2986 0.059 Uiso 1 1 calc . . .
N36 N 0.5899(3) 0.0062(2) 0.19183(14) 0.0706(7) Uani 1 1 d . . .
C37 C 0.6499(2) -0.0680(2) 0.21489(16) 0.0610(7) Uani 1 1 d . . .
S38 S 0.72828(8) -0.17215(8) 0.24068(6) 0.0919(3) Uani 1 1 d . . .
C40 C 0.3965(2) 0.50835(19) 0.27588(12) 0.0444(5) Uani 1 1 d . . .
C41 C 0.3072(2) 0.5533(2) 0.30743(12) 0.0509(6) Uani 1 1 d . . .
H41 H 0.2328 0.5530 0.2861 0.061 Uiso 1 1 calc . . .
C42 C 0.3259(3) 0.5989(2) 0.37006(13) 0.0584(7) Uani 1 1 d . . .
H42 H 0.2646 0.6288 0.3905 0.070 Uiso 1 1 calc . . .
C43 C 0.4353(3) 0.5999(2) 0.40191(13) 0.0586(7) Uani 1 1 d . A .
C44 C 0.5270(3) 0.5587(3) 0.37126(15) 0.0635(7) Uani 1 1 d . . .
H44 H 0.6014 0.5606 0.3926 0.076 Uiso 1 1 calc . . .
C45 C 0.5071(2) 0.5144(2) 0.30844(14) 0.0570(7) Uani 1 1 d . . .
H45 H 0.5692 0.4881 0.2874 0.068 Uiso 1 1 calc . . .
N46 N 0.4555(3) 0.6466(2) 0.46516(12) 0.0765(8) Uani 1 1 d . . .
C47A C 0.4339(4) 0.7012(3) 0.50954(17) 0.0647(9) Uani 0.848(2) 1 d P A 1
S48A S 0.40954(17) 0.77328(13) 0.57224(6) 0.1121(6) Uani 0.848(2) 1 d P A 1
C47B C 0.503(2) 0.683(2) 0.5066(11) 0.0647(9) Uani 0.152(2) 1 d P A 2
S48B S 0.5308(10) 0.7585(7) 0.5718(3) 0.1121(6) Uani 0.152(2) 1 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
C1 0.0519(13) 0.0376(12) 0.0432(12) 0.0003(9) 0.0018(10) 0.0012(10)
C10 0.0630(15) 0.0388(12) 0.0475(13) 0.0009(10) -0.0003(11) -0.0031(11)
C11 0.0800(19) 0.0407(13) 0.0513(14) 0.0002(11) 0.0010(13) 0.0005(12)
C12 0.103(2) 0.0404(14) 0.0578(16) 0.0038(12) -0.0074(16) -0.0038(14)
C13 0.095(2) 0.0571(18) 0.0649(18) 0.0133(14) 0.0028(16) -0.0202(16)
C14 0.086(2) 0.068(2) 0.108(3) 0.020(2) 0.029(2) -0.0122(18)
C15 0.0685(19) 0.0514(16) 0.094(2) 0.0159(16) 0.0184(17) -0.0013(13)
N16 0.129(3) 0.0715(19) 0.095(2) 0.0277(17) 0.007(2) -0.0357(19)
C17 0.0749(19) 0.0574(17) 0.0584(16) 0.0022(13) 0.0120(14) -0.0015(14)
S18 0.0845(6) 0.0586(5) 0.0795(5) 0.0152(4) 0.0204(4) -0.0088(4)
C20 0.0531(14) 0.0381(12) 0.0473(12) -0.0046(10) -0.0023(10) 0.0044(10)
C21 0.0699(18) 0.0671(18) 0.0479(14) 0.0021(13) -0.0061(13) -0.0028(14)
C22 0.080(2) 0.078(2) 0.0565(16) -0.0041(15) -0.0237(15) 0.0084(17)
C23 0.0550(16) 0.0581(17) 0.083(2) -0.0194(15) -0.0118(15) 0.0067(13)
C24 0.0562(15) 0.0476(14) 0.0757(18) -0.0068(13) 0.0026(13) 0.0002(11)
C25 0.0559(14) 0.0426(13) 0.0571(14) 0.0022(11) -0.0030(11) 0.0015(11)
N26 0.0640(17) 0.096(2) 0.110(2) -0.0281(19) -0.0260(16) 0.0063(15)
C27 0.0647(18) 0.0624(17) 0.0623(17) -0.0023(13) 0.0030(14) -0.0076(13)
y8 0.0723(6) 0.1277(9) 0.0880(6) -0.0008(6) -0.0190(5) -0.0268(5)
C30 0.0451(12) 0.0376(12) 0.0449(12) -0.0020(9) 0.0031(9) -0.0020(9)
C31 0.0701(17) 0.0496(14) 0.0456(13) 0.0017(11) 0.0093(12) 0.0053(12)
C32 0.0797(19) 0.0512(15) 0.0517(14) -0.0087(12) 0.0160(13) 0.0059(13)
C33 0.0544(14) 0.0382(13) 0.0666(16) -0.0053(11) 0.0070(12) -0.0001(10)
C34 0.0672(17) 0.0426(13) 0.0512(14) 0.0026(10) -0.0011(12) -0.0004(11)
C35 0.0629(15) 0.0418(13) 0.0433(12) -0.0025(10) 0.0023(10) 0.0025(11)
N36 0.0802(17) 0.0479(13) 0.0843(18) -0.0053(12) 0.0106(14) 0.0134(12)
C37 0.0565(16) 0.0496(15) 0.0785(19) -0.0095(14) 0.0143(14) -0.0034(12)
S38 0.0654(5) 0.0688(6) 0.1392(9) 0.0095(5) -0.0003(5) 0.0162(4)
C40 0.0548(13) 0.0329(11) 0.0445(12) -0.0006(9) -0.0002(10) 0.0023(9)
C41 0.0536(14) 0.0490(14) 0.0495(13) 0.0010(11) 0.0026(11) 0.0037(11)
C42 0.0721(18) 0.0541(15) 0.0504(14) -0.0015(12) 0.0131(13) 0.0028(13)
C43 0.086(2) 0.0439(14) 0.0443(13) -0.0013(11) -0.0014(13) -0.0016(13)
C44 0.0670(17) 0.0542(16) 0.0649(17) -0.0105(13) -0.0146(14) 0.0027(13)
C45 0.0546(15) 0.0506(15) 0.0641(16) -0.0142(12) -0.0023(12) 0.0056(11)
N46 0.113(2) 0.0662(16) 0.0488(13) -0.0114(12) -0.0003(14) -0.0077(15)
C47A 0.085(3) 0.0570(19) 0.0494(17) 0.0017(15) -0.0074(19) -0.006(2)
S48A 0.1764(15) 0.0990(9) 0.0602(6) -0.0251(6) 0.0088(7) 0.0081(9)
C47B 0.085(3) 0.0570(19) 0.0494(17) 0.0017(15) -0.0074(19) -0.006(2)
S48B 0.1764(15) 0.0990(9) 0.0602(6) -0.0251(6) 0.0088(7) 0.0081(9)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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_publ_flag
C20 C1 C40 113.0(2) y
C20 C1 C30 103.76(18) y
C40 C1 C30 111.45(19) y
C20 C1 C10 111.66(19) y
C40 C1 C10 104.16(19) y
C30 C1 C10 113.1(2) y
C15 C10 C11 117.4(2) y
C15 C10 C1 123.8(2) y
C11 C10 C1 118.7(2) y
C12 C11 C10 121.5(3) y
C12 C11 H11 119.2 ?
C10 C11 H11 119.2 ?
C13 C12 C11 119.9(3) y
C13 C12 H12 120.1 ?
C11 C12 H12 120.1 ?
C12 C13 C14 119.9(3) y
C12 C13 N16 120.4(3) y
C14 C13 N16 119.7(4) y
C13 C14 C15 120.4(3) y
C13 C14 H14 119.8 ?
C15 C14 H14 119.8 ?
C10 C15 C14 120.9(3) y
C10 C15 H15 119.5 ?
C14 C15 H15 119.5 ?
C17 N16 C13 167.3(4) y
N16 C17 S18 178.2(3) y
C21 C20 C25 117.2(2) y
C21 C20 C1 122.7(2) y
C25 C20 C1 119.8(2) y
C22 C21 C20 121.1(3) y
C22 C21 H21 119.4 ?
C20 C21 H21 119.4 ?
C23 C22 C21 120.2(3) y
C23 C22 H22 119.9 ?
C21 C22 H22 119.9 ?
C22 C23 C24 119.8(3) y
C22 C23 N26 120.2(3) y
C24 C23 N26 120.0(3) y
C25 C24 C23 119.3(3) y
C25 C24 H24 120.3 ?
C23 C24 H24 120.3 ?
C24 C25 C20 122.2(2) y
C24 C25 H25 118.9 ?
C20 C25 H25 118.9 ?
C27 N26 C23 162.4(4) y
N26 C27 y8 176.9(3) y
C35 C30 C31 117.2(2) y
C35 C30 C1 122.3(2) y
C31 C30 C1 120.3(2) y
C32 C31 C30 121.8(2) y
C32 C31 H31 119.1 ?
C30 C31 H31 119.1 ?
C31 C32 C33 119.4(2) y
C31 C32 H32 120.3 ?
C33 C32 H32 120.3 ?
C34 C33 C32 120.0(2) y
C34 C33 N36 119.9(3) y
C32 C33 N36 120.1(3) y
C33 C34 C35 119.5(2) y
C33 C34 H34 120.2 ?
C35 C34 H34 120.2 ?
C30 C35 C34 121.7(2) y
C30 C35 H35 119.2 ?
C34 C35 H35 119.2 ?
C37 N36 C33 152.0(3) y
N36 C37 S38 175.7(3) y
C41 C40 C45 117.5(2) y
C41 C40 C1 124.3(2) y
C45 C40 C1 118.1(2) y
C40 C41 C42 121.5(2) y
C40 C41 H41 119.3 ?
C42 C41 H41 119.3 ?
C43 C42 C41 119.7(3) y
C43 C42 H42 120.1 ?
C41 C42 H42 120.1 ?
C42 C43 C44 120.4(2) y
C42 C43 N46 120.3(3) y
C44 C43 N46 119.3(3) y
C43 C44 C45 119.2(3) y
C43 C44 H44 120.4 ?
C45 C44 H44 120.4 ?
C44 C45 C40 121.6(3) y
C44 C45 H45 119.2 ?
C40 C45 H45 119.2 ?
C47B N46 C47A 44.30(14) y
C47B N46 C43 157.80(15) y
C47A N46 C43 155.3(4) y
N46 C47A S48A 177.3(4) y
N46 C47B S48B 160(2) y
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
C1 C20 1.543(3) y
C1 C40 1.547(3) y
C1 C30 1.547(3) y
C1 C10 1.548(3) y
C10 C15 1.377(4) y
C10 C11 1.391(4) y
C11 C12 1.380(4) y
C11 H11 0.93 ?
C12 C13 1.361(5) y
C12 H12 0.93 ?
C13 C14 1.367(5) y
C13 N16 1.395(4) y
C14 C15 1.386(4) y
C14 H14 0.93 ?
C15 H15 0.93 ?
N16 C17 1.152(4) y
C17 S18 1.567(3) y
C20 C21 1.385(4) y
C20 C25 1.388(4) y
C21 C22 1.381(4) y
C21 H21 0.93 ?
C22 C23 1.376(5) y
C22 H22 0.93 ?
C23 C24 1.377(5) y
C23 N26 1.394(4) y
C24 C25 1.374(4) y
C24 H24 0.93 ?
C25 H25 0.93 ?
N26 C27 1.140(4) y
C27 y8 1.570(3) y
C30 C35 1.382(3) y
C30 C31 1.395(3) y
C31 C32 1.377(4) y
C31 H31 0.93 ?
C32 C33 1.385(4) y
C32 H32 0.93 ?
C33 C34 1.377(4) y
C33 N36 1.397(3) y
C34 C35 1.388(4) y
C34 H34 0.93 ?
C35 H35 0.93 ?
N36 C37 1.169(4) y
C37 S38 1.562(3) y
C40 C41 1.380(4) y
C40 C45 1.391(4) y
C41 C42 1.384(4) y
C41 H41 0.93 ?
C42 C43 1.371(4) y
C42 H42 0.93 ?
C43 C44 1.377(4) y
C43 N46 1.400(4) y
C44 C45 1.382(4) y
C44 H44 0.93 ?
C45 H45 0.93 ?
N46 C47b 1.05(2) y
N46 C47a 1.154(5) y
C47a S48a 1.578(4) y
C47b S48b 1.60(2) y
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
C20 C1 C10 C15 -129.6(3) y
C40 C1 C10 C15 108.2(3) y
C30 C1 C10 C15 -13.0(4) y
C20 C1 C10 C11 54.8(3) y
C40 C1 C10 C11 -67.5(3) y
C30 C1 C10 C11 171.4(2) y
C15 C10 C11 C12 2.3(4) y
C1 C10 C11 C12 178.2(3) y
C10 C11 C12 C13 -0.1(5) y
C11 C12 C13 C14 -1.4(5) y
C11 C12 C13 N16 179.2(3) y
C12 C13 C14 C15 0.5(6) y
N16 C13 C14 C15 179.9(4) y
C11 C10 C15 C14 -3.2(5) y
C1 C10 C15 C14 -178.8(3) y
C13 C14 C15 C10 1.8(6) y
C12 C13 N16 C17 43(2) y
C14 C13 N16 C17 -136.80(18) y
C13 N16 C17 S18 157(11) y
C40 C1 C20 C21 133.5(3) y
C30 C1 C20 C21 -105.7(3) y
C10 C1 C20 C21 16.5(3) y
C40 C1 C20 C25 -52.2(3) y
C30 C1 C20 C25 68.6(3) y
C10 C1 C20 C25 -169.2(2) y
C25 C20 C21 C22 1.8(4) y
C1 C20 C21 C22 176.2(3) y
C20 C21 C22 C23 0.2(5) y
C21 C22 C23 C24 -1.7(5) y
C21 C22 C23 N26 179.1(3) y
C22 C23 C24 C25 1.3(4) y
N26 C23 C24 C25 -179.6(3) y
C23 C24 C25 C20 0.7(4) y
C21 C20 C25 C24 -2.2(4) y
C1 C20 C25 C24 -176.8(2) y
C22 C23 N26 C27 12.40(13) y
C24 C23 N26 C27 -166.70(11) y
C23 N26 C27 y8 171(5) y
C20 C1 C30 C35 -104.6(3) y
C40 C1 C30 C35 17.2(3) y
C10 C1 C30 C35 134.2(2) y
C20 C1 C30 C31 70.8(3) y
C40 C1 C30 C31 -167.3(2) y
C10 C1 C30 C31 -50.4(3) y
C35 C30 C31 C32 -4.6(4) y
C1 C30 C31 C32 179.7(3) y
C30 C31 C32 C33 0.9(5) y
C31 C32 C33 C34 3.6(4) y
C31 C32 C33 N36 -176.4(3) y
C32 C33 C34 C35 -4.2(4) y
N36 C33 C34 C35 175.8(3) y
C31 C30 C35 C34 4.0(4) y
C1 C30 C35 C34 179.6(2) y
C33 C34 C35 C30 0.3(4) y
C34 C33 N36 C37 -24.1(8) y
C32 C33 N36 C37 155.9(6) y
C33 N36 C37 S38 179(100) y
C20 C1 C40 C41 -12.5(3) y
C30 C1 C40 C41 -128.9(2) y
C10 C1 C40 C41 108.8(3) y
C20 C1 C40 C45 171.2(2) y
C30 C1 C40 C45 54.8(3) y
C10 C1 C40 C45 -67.4(3) y
C45 C40 C41 C42 -2.3(4) y
C1 C40 C41 C42 -178.6(2) y
C40 C41 C42 C43 0.0(4) y
C41 C42 C43 C44 1.7(4) y
C41 C42 C43 N46 179.6(3) y
C42 C43 C44 C45 -1.1(4) y
N46 C43 C44 C45 -179.0(3) y
C43 C44 C45 C40 -1.3(5) y
C41 C40 C45 C44 3.0(4) y
C1 C40 C45 C44 179.5(3) y
C42 C43 N46 C47B -160(3) y
C44 C43 N46 C47B 18(3) y
C42 C43 N46 C47A -17.2(9) y
C44 C43 N46 C47A 160.7(7) y
C47B N46 C47A S48A -29(8) y
C43 N46 C47A S48A 170(8) y
C47A N46 C47B S48B -9(4) y
C43 N46 C47B S48B 150(4) y
|
1501610.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/16/1501610.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_1501610
loop_
_publ_author_name
'Dominic Lalibert\'e'
'Thierry Maris'
'James D. Wuest'
_publ_section_title
;
Molecular tectonics - Use of urethanes and ureas derived from
tetraphenylmethane and tetraphenylsilane to build porous chiral
hydrogenbonded networks
;
_journal_name_full 'Can. J. Chem.'
_journal_page_first 386
_journal_page_last 398
_journal_paper_doi 10.1139/v03-208
_journal_volume 82
_journal_year 2004
_chemical_compound_source 'Synthesized by the authors. See text'
_chemical_formula_sum 'C45 H56 N4 O10'
_chemical_formula_weight 812.94
_chemical_name_systematic
;
?
;
_space_group_IT_number 82
_symmetry_cell_setting tetragonal
_symmetry_space_group_name_Hall 'I -4'
_symmetry_space_group_name_H-M 'I -4'
_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 24.9135(8)
_cell_length_b 24.9135(8)
_cell_length_c 7.1597(2)
_cell_measurement_reflns_used 7090
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 57.07
_cell_measurement_theta_min 2.51
_cell_volume 4443.9(2)
_computing_cell_refinement 'SMART (Bruker, 1999)'
_computing_data_collection 'SAINT (Bruker, 1999)'
_computing_data_reduction 'SAINT (Bruker, 1999)'
_computing_molecular_graphics 'XP (Bruker, 1999)'
_computing_publication_material 'UdMX (local program)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.712
_diffrn_measured_fraction_theta_max 0.712
_diffrn_measurement_device_type 'Bruker AXS Smart 2K/Platform'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'Sealed Tube'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.029
_diffrn_reflns_av_sigmaI/netI 0.0774
_diffrn_reflns_limit_h_max 20
_diffrn_reflns_limit_h_min -31
_diffrn_reflns_limit_k_max 20
_diffrn_reflns_limit_k_min -19
_diffrn_reflns_limit_l_max 5
_diffrn_reflns_limit_l_min -8
_diffrn_reflns_number 10595
_diffrn_reflns_theta_full 73.68
_diffrn_reflns_theta_max 73.68
_diffrn_reflns_theta_min 2.51
_diffrn_standards_decay_% 0.00
_diffrn_standards_interval_time 4500
_diffrn_standards_number 5
_exptl_absorpt_coefficient_mu 0.703
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_correction_T_min 0.6800
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Sadabs (Sheldrick,1996)'
_exptl_crystal_colour Colourless
_exptl_crystal_density_diffrn 1.215
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 1736
_exptl_crystal_size_max 0.35
_exptl_crystal_size_mid 0.13
_exptl_crystal_size_min 0.10
_refine_diff_density_max 0.316
_refine_diff_density_min -0.154
_refine_diff_density_rms 0.042
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack 0.0(4)
_refine_ls_extinction_coef 0.00031(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 1.008
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 268
_refine_ls_number_reflns 2750
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.008
_refine_ls_R_factor_all 0.1304
_refine_ls_R_factor_gt 0.0688
_refine_ls_shift/su_max 0.456
_refine_ls_shift/su_mean 0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0985P)^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 0.1795
_reflns_number_gt 1449
_reflns_number_total 2750
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file deposit.cif
_cod_data_source_block jiw365
_cod_original_sg_symbol_H-M I-4
_cod_database_code 1501610
loop_
_symmetry_equiv_pos_as_xyz
'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'
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
C1 C 0.5000 0.5000 1.5000 0.048(3) Uani 1 4 d S
C2 C 0.4941(2) 0.4507(2) 1.3701(6) 0.0503(14) Uani 1 1 d .
C3 C 0.5279(2) 0.4070(3) 1.3742(7) 0.0639(16) Uani 1 1 d .
H3 H 0.5548 0.4055 1.4642 0.077 Uiso 1 1 calc .
C4 C 0.5229(2) 0.3656(2) 1.2484(9) 0.0651(15) Uani 1 1 d .
H4 H 0.5467 0.3369 1.2540 0.078 Uiso 1 1 calc .
C5 C 0.4833(2) 0.3657(2) 1.1147(8) 0.0571(14) Uani 1 1 d .
C6 C 0.4493(2) 0.4096(3) 1.1095(7) 0.0644(16) Uani 1 1 d .
H6 H 0.4225 0.4112 1.0193 0.077 Uiso 1 1 calc .
C7 C 0.4544(2) 0.4501(2) 1.2334(8) 0.0598(15) Uani 1 1 d .
H7 H 0.4305 0.4787 1.2272 0.072 Uiso 1 1 calc .
N8 N 0.4816(2) 0.32179(18) 0.9900(7) 0.0823(15) Uani 1 1 d .
H8 H 0.5039 0.2964 1.0142 0.099 Uiso 1 1 calc R
C9 C 0.4507(4) 0.3138(3) 0.8406(10) 0.089(2) Uani 1 1 d .
O10 O 0.4112(2) 0.3404(2) 0.8020(7) 0.131(2) Uani 1 1 d .
O11 O 0.46809(18) 0.27230(19) 0.7400(7) 0.1162(16) Uani 1 1 d .
C12 C 0.4412(4) 0.2620(3) 0.5670(12) 0.148(3) Uani 1 1 d .
H12A H 0.4051 0.2493 0.5914 0.178 Uiso 1 1 calc R
H12B H 0.4387 0.2949 0.4953 0.178 Uiso 1 1 calc R
C13 C 0.4700(4) 0.2226(4) 0.4629(12) 0.173(4) Uani 1 1 d .
H13A H 0.4512 0.2151 0.3488 0.259 Uiso 1 1 calc R
H13B H 0.4729 0.1903 0.5352 0.259 Uiso 1 1 calc R
H13C H 0.5052 0.2359 0.4344 0.259 Uiso 1 1 calc R
C21 C 1.0000 0.5000 -0.2500 0.054(3) Uani 1 4 d S
C22 C 0.9538(2) 0.5176(2) -0.1245(7) 0.0567(14) Uani 1 1 d .
C23 C 0.9020(3) 0.5011(2) -0.1428(8) 0.0820(19) Uani 1 1 d .
H23 H 0.8944 0.4751 -0.2325 0.098 Uiso 1 1 calc .
C24 C 0.8596(2) 0.5204(3) -0.0360(11) 0.0876(19) Uani 1 1 d .
H24 H 0.8250 0.5078 -0.0569 0.105 Uiso 1 1 calc .
C25 C 0.8687(3) 0.5577(2) 0.0990(9) 0.0718(17) Uani 1 1 d .
C26 C 0.9223(3) 0.5725(2) 0.1313(8) 0.0689(16) Uani 1 1 d .
H26 H 0.9305 0.5963 0.2274 0.083 Uiso 1 1 calc .
C27 C 0.9621(2) 0.5526(2) 0.0238(9) 0.0695(17) Uani 1 1 d .
H27 H 0.9972 0.5628 0.0506 0.083 Uiso 1 1 calc .
N28 N 0.8274(3) 0.58140(18) 0.2052(7) 0.0945(17) Uani 1 1 d .
H28 H 0.8363 0.5945 0.3119 0.113 Uiso 1 1 calc R
C29 C 0.7750(4) 0.5857(3) 0.1561(15) 0.101(2) Uani 1 1 d .
O30 O 0.75515(18) 0.5690(2) 0.0141(8) 0.1058(16) Uani 1 1 d .
O31 O 0.7475(2) 0.61062(19) 0.2916(9) 0.132(2) Uani 1 1 d .
C32 C 0.6896(3) 0.6149(4) 0.2562(18) 0.190(5) Uani 1 1 d .
H32A H 0.6829 0.6314 0.1358 0.229 Uiso 1 1 calc R
H32B H 0.6729 0.5797 0.2583 0.229 Uiso 1 1 calc R
C33 C 0.6694(4) 0.6477(4) 0.404(2) 0.217(6) Uani 1 1 d .
H33A H 0.6313 0.6520 0.3897 0.326 Uiso 1 1 calc R
H33B H 0.6865 0.6822 0.3997 0.326 Uiso 1 1 calc R
H33C H 0.6769 0.6309 0.5218 0.326 Uiso 1 1 calc R
O40 O 0.3602(2) 0.1515(4) 0.0121(11) 0.189(3) Uani 1 1 d .
C41 C 0.3332(6) 0.1427(5) 0.1946(17) 0.207(5) Uani 1 1 d .
H41A H 0.3059 0.1151 0.1827 0.311 Uiso 1 1 calc R
H41B H 0.3591 0.1311 0.2874 0.311 Uiso 1 1 calc R
C42 C 0.3101(8) 0.1906(10) 0.248(3) 0.329(14) Uani 1 1 d .
H42A H 0.3303 0.2073 0.3481 0.493 Uiso 1 1 calc R
H42B H 0.2734 0.1852 0.2890 0.493 Uiso 1 1 calc R
C43 C 0.3121(16) 0.2238(12) 0.074(6) 0.54(4) Uani 1 1 d .
H43A H 0.2794 0.2197 0.0020 0.814 Uiso 1 1 calc R
H43B H 0.3169 0.2615 0.1042 0.814 Uiso 1 1 calc R
C44 C 0.3549(10) 0.2046(8) -0.021(5) 0.42(2) Uani 1 1 d .
H44A H 0.3501 0.2108 -0.1534 0.627 Uiso 1 1 calc R
H44B H 0.3872 0.2233 0.0187 0.627 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
C1 0.058(4) 0.058(4) 0.026(5) 0.000 0.000 0.000
C2 0.072(4) 0.049(4) 0.029(3) 0.000(3) 0.007(3) 0.003(3)
C3 0.078(4) 0.062(4) 0.051(3) -0.010(3) -0.013(3) -0.003(4)
C4 0.072(4) 0.056(4) 0.067(4) -0.006(4) -0.011(4) 0.017(3)
C5 0.072(4) 0.061(4) 0.039(3) -0.013(3) 0.001(3) 0.002(4)
C6 0.062(4) 0.085(4) 0.047(3) -0.006(4) -0.008(3) 0.000(4)
C7 0.071(4) 0.074(4) 0.034(3) -0.007(3) -0.007(3) 0.005(3)
N8 0.118(4) 0.070(3) 0.059(3) -0.017(3) -0.023(3) 0.014(3)
C9 0.127(7) 0.075(6) 0.064(5) -0.011(4) -0.021(5) 0.003(5)
O10 0.150(5) 0.132(4) 0.112(4) -0.043(3) -0.056(3) 0.037(4)
O11 0.154(4) 0.095(3) 0.100(4) -0.062(3) -0.033(3) 0.020(3)
C12 0.181(8) 0.144(7) 0.119(6) -0.088(6) -0.046(6) 0.033(6)
C13 0.275(11) 0.154(7) 0.088(5) -0.057(6) -0.020(6) 0.007(7)
C21 0.060(4) 0.060(4) 0.042(6) 0.000 0.000 0.000
C22 0.047(5) 0.069(4) 0.054(4) 0.006(3) -0.007(3) -0.003(3)
C23 0.076(5) 0.091(4) 0.079(4) -0.034(4) 0.001(4) -0.012(4)
C24 0.058(5) 0.105(5) 0.100(5) -0.038(5) 0.000(4) -0.004(4)
C25 0.085(6) 0.075(4) 0.056(4) 0.003(4) 0.011(4) 0.002(4)
C26 0.066(5) 0.082(4) 0.059(4) -0.008(3) -0.001(4) -0.007(4)
C27 0.055(4) 0.088(4) 0.066(4) -0.008(4) 0.000(4) 0.000(3)
N28 0.078(5) 0.125(4) 0.080(4) -0.032(3) 0.021(4) -0.008(3)
C29 0.061(6) 0.120(6) 0.123(7) -0.021(6) 0.024(6) -0.025(5)
O30 0.074(3) 0.129(4) 0.114(4) -0.013(3) 0.002(3) -0.013(3)
O31 0.111(5) 0.134(4) 0.151(5) -0.044(4) 0.049(4) 0.008(3)
C32 0.047(5) 0.230(10) 0.295(13) -0.104(11) 0.062(7) 0.027(5)
C33 0.131(7) 0.142(7) 0.380(18) -0.049(11) 0.068(11) 0.016(6)
O40 0.179(6) 0.226(8) 0.162(7) -0.071(6) 0.020(5) -0.013(5)
C41 0.296(14) 0.227(13) 0.098(7) -0.001(8) 0.022(9) 0.007(11)
C42 0.30(2) 0.42(3) 0.27(2) -0.22(2) 0.036(17) 0.093(19)
C43 0.76(7) 0.34(3) 0.53(6) -0.06(4) -0.40(6) 0.19(4)
C44 0.61(5) 0.154(14) 0.49(4) 0.08(2) 0.10(4) -0.12(2)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
C2 C1 C2 3_568 . 111.20(18) y
C2 C1 C2 3_568 2_665 111.20(18) y
C2 C1 C2 . 2_665 106.1(3) y
C2 C1 C2 3_568 4_658 106.1(3) y
C2 C1 C2 . 4_658 111.20(18) y
C2 C1 C2 2_665 4_658 111.20(18) y
C3 C2 C7 . . 116.1(4) y
C3 C2 C1 . . 123.9(5) y
C7 C2 C1 . . 119.9(5) y
C4 C3 C2 . . 121.6(5) y
C4 C3 H3 . . 119.2 ?
C2 C3 H3 . . 119.2 ?
C5 C4 C3 . . 121.3(5) y
C5 C4 H4 . . 119.3 ?
C3 C4 H4 . . 119.3 ?
C4 C5 C6 . . 117.4(5) y
C4 C5 N8 . . 117.4(5) y
C6 C5 N8 . . 125.2(6) y
C7 C6 C5 . . 121.0(5) y
C7 C6 H6 . . 119.5 ?
C5 C6 H6 . . 119.5 ?
C6 C7 C2 . . 122.6(5) y
C6 C7 H7 . . 118.7 ?
C2 C7 H7 . . 118.7 ?
C9 N8 C5 . . 129.8(6) y
C9 N8 H8 . . 115.1 ?
C5 N8 H8 . . 115.1 ?
O10 C9 O11 . . 124.2(7) y
O10 C9 N8 . . 124.5(7) y
O11 C9 N8 . . 111.3(7) y
C9 O11 C12 . . 117.0(6) y
C13 C12 O11 . . 109.9(7) y
C13 C12 H12A . . 109.7 ?
O11 C12 H12A . . 109.7 ?
C13 C12 H12B . . 109.7 ?
O11 C12 H12B . . 109.7 ?
H12A C12 H12B . . 108.2 ?
C12 C13 H13A . . 109.5 ?
C12 C13 H13B . . 109.5 ?
H13A C13 H13B . . 109.5 ?
C12 C13 H13C . . 109.5 ?
H13A C13 H13C . . 109.5 ?
H13B C13 H13C . . 109.5 ?
C22 C21 C22 8_644 . 110.3(2) y
C22 C21 C22 8_644 2_765 110.3(2) y
C22 C21 C22 . 2_765 107.8(4) y
C22 C21 C22 8_644 7_564 107.8(4) y
C22 C21 C22 . 7_564 110.3(2) y
C22 C21 C22 2_765 7_564 110.3(2) y
C23 C22 C27 . . 113.9(5) y
C23 C22 C21 . . 124.9(5) y
C27 C22 C21 . . 121.2(5) y
C22 C23 C24 . . 124.2(5) y
C22 C23 H23 . . 117.9 ?
C24 C23 H23 . . 117.9 ?
C25 C24 C23 . . 120.1(5) y
C25 C24 H24 . . 119.9 ?
C23 C24 H24 . . 119.9 ?
C24 C25 C26 . . 117.1(6) y
C24 C25 N28 . . 123.3(7) y
C26 C25 N28 . . 119.6(6) y
C27 C26 C25 . . 120.4(6) y
C27 C26 H26 . . 119.8 ?
C25 C26 H26 . . 119.8 ?
C26 C27 C22 . . 123.9(5) y
C26 C27 H27 . . 118.1 ?
C22 C27 H27 . . 118.1 ?
C29 N28 C25 . . 126.5(6) y
C29 N28 H28 . . 116.7 ?
C25 N28 H28 . . 116.7 ?
O30 C29 O31 . . 124.1(8) y
O30 C29 N28 . . 126.0(8) y
O31 C29 N28 . . 109.9(9) y
C29 O31 C32 . . 114.2(8) y
C33 C32 O31 . . 105.0(9) y
C33 C32 H32A . . 110.7 ?
O31 C32 H32A . . 110.7 ?
C33 C32 H32B . . 110.7 ?
O31 C32 H32B . . 110.7 ?
H32A C32 H32B . . 108.8 ?
C32 C33 H33A . . 109.5 ?
C32 C33 H33B . . 109.5 ?
H33A C33 H33B . . 109.5 ?
C32 C33 H33C . . 109.5 ?
H33A C33 H33C . . 109.5 ?
H33B C33 H33C . . 109.5 ?
C44 O40 C41 . . 104.70(15) y
C42 C41 O40 . . 107.70(13) y
C42 C41 H41A . . 110.2 ?
O40 C41 H41A . . 110.2 ?
C42 C41 H41B . . 110.2 ?
O40 C41 H41B . . 110.2 ?
H41A C41 H41B . . 108.5 ?
C41 C42 C43 . . 103.60(18) y
C41 C42 H42A . . 111 ?
C43 C42 H42A . . 111 ?
C41 C42 H42B . . 111 ?
C43 C42 H42B . . 111 ?
H42A C42 H42B . . 109 ?
C44 C43 C42 . . 104(2) y
C44 C43 H43A . . 110.9 ?
C42 C43 H43A . . 110.9 ?
C44 C43 H43B . . 110.9 ?
C42 C43 H43B . . 110.9 ?
H43A C43 H43B . . 108.9 ?
O40 C44 C43 . . 110(2) y
O40 C44 H44A . . 109.7 ?
C43 C44 H44A . . 109.7 ?
O40 C44 H44B . . 109.7 ?
C43 C44 H44B . . 109.7 ?
H44A C44 H44B . . 108.2 ?
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
C1 C2 3_568 1.547(5) y
C1 C2 . 1.547(5) y
C1 C2 2_665 1.547(5) y
C1 C2 4_658 1.547(5) y
C2 C3 . 1.376(7) y
C2 C7 . 1.392(6) y
C3 C4 . 1.375(7) y
C3 H3 . 0.93 ?
C4 C5 . 1.375(7) y
C4 H4 . 0.93 ?
C5 C6 . 1.383(7) y
C5 N8 . 1.413(6) y
C6 C7 . 1.349(7) y
C6 H6 . 0.93 ?
C7 H7 . 0.93 ?
N8 C9 . 1.332(8) y
N8 H8 . 0.86 ?
C9 O10 . 1.218(7) y
C9 O11 . 1.332(7) y
O11 C12 . 1.431(8) y
C12 C13 . 1.426(10) y
C12 H12a . 0.97 ?
C12 H12b . 0.97 ?
C13 H13a . 0.96 ?
C13 H13b . 0.96 ?
C13 H13c . 0.96 ?
C21 C22 8_644 1.525(5) y
C21 C22 . 1.525(5) y
C21 C22 2_765 1.525(5) y
C21 C22 7_564 1.525(5) y
C22 C23 . 1.361(7) y
C22 C27 . 1.389(7) y
C23 C24 . 1.389(8) y
C23 H23 . 0.93 ?
C24 C25 . 1.359(7) y
C24 H24 . 0.93 ?
C25 C26 . 1.406(8) y
C25 N28 . 1.410(7) y
C26 C27 . 1.350(7) y
C26 H26 . 0.93 ?
C27 H27 . 0.93 ?
N28 C29 . 1.356(9) y
N28 H28 . 0.86 ?
C29 O30 . 1.204(8) y
C29 O31 . 1.341(8) y
O31 C32 . 1.468(9) y
C32 C33 . 1.429(15) y
C32 H32a . 0.97 ?
C32 H32b . 0.97 ?
C33 H33a . 0.96 ?
C33 H33b . 0.96 ?
C33 H33c . 0.96 ?
O40 C44 . 1.350(18) y
O40 C41 . 1.486(13) y
C41 C42 . 1.379(18) y
C41 H41a . 0.97 ?
C41 H41b . 0.97 ?
C42 C43 . 1.50(4) y
C42 H42a . 0.97 ?
C42 H42b . 0.97 ?
C43 C44 . 1.35(5) y
C43 H43a . 0.97 ?
C43 H43b . 0.97 ?
C44 H44a . 0.97 ?
C44 H44b . 0.97 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N8 H8 O30 0.86 2.08 2.902(6) 159.9 3_566
N28 H28 O40 0.86 2.1 2.924(8) 159.2 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_site_symmetry_1
_geom_torsion
_geom_torsion_publ_flag
C2 C1 C2 C3 3_568 -116.5(5) y
C2 C1 C2 C3 2_665 122.5(5) y
C2 C1 C2 C3 4_658 1.5(5) y
C2 C1 C2 C7 3_568 66.6(3) y
C2 C1 C2 C7 2_665 -54.4(3) y
C2 C1 C2 C7 4_658 -175.4(4) y
C7 C2 C3 C4 . 0.9(7) y
C1 C2 C3 C4 . -176.2(4) y
C2 C3 C4 C5 . -1.0(7) y
C3 C4 C5 C6 . 1.1(7) y
C3 C4 C5 N8 . 179.2(5) y
C4 C5 C6 C7 . -1.2(7) y
N8 C5 C6 C7 . -179.1(5) y
C5 C6 C7 C2 . 1.1(7) y
C3 C2 C7 C6 . -0.9(7) y
C1 C2 C7 C6 . 176.2(4) y
C4 C5 N8 C9 . -174.2(5) y
C6 C5 N8 C9 . 3.8(9) y
C5 N8 C9 O10 . -12.8(1) y
C5 N8 C9 O11 . 168.2(5) y
O10 C9 O11 C12 . 6.1(1) y
N8 C9 O11 C12 . -174.9(6) y
C9 O11 C12 C13 . 170.2(7) y
C22 C21 C22 C23 8_644 -10.3(5) y
C22 C21 C22 C23 2_765 -130.8(6) y
C22 C21 C22 C23 7_564 108.6(6) y
C22 C21 C22 C27 8_644 168.9(4) y
C22 C21 C22 C27 2_765 48.4(4) y
C22 C21 C22 C27 7_564 -72.1(3) y
C27 C22 C23 C24 . 5.6(8) y
C21 C22 C23 C24 . -175.1(5) y
C22 C23 C24 C25 . -1.1(9) y
C23 C24 C25 C26 . -3.8(8) y
C23 C24 C25 N28 . 176.2(5) y
C24 C25 C26 C27 . 3.8(8) y
N28 C25 C26 C27 . -176.2(5) y
C25 C26 C27 C22 . 1.1(8) y
C23 C22 C27 C26 . -5.6(7) y
C21 C22 C27 C26 . 175.1(5) y
C24 C25 N28 C29 . -23.0(9) y
C26 C25 N28 C29 . 156.9(6) y
C25 N28 C29 O30 . 1.2(1) y
C25 N28 C29 O31 . -180.0(5) y
O30 C29 O31 C32 . 1.80(11) y
N28 C29 O31 C32 . -177.0(7) y
C29 O31 C32 C33 . -173.4(8) y
C44 O40 C41 C42 . 4.90(18) y
O40 C41 C42 C43 . 14(3) y
C41 C42 C43 C44 . -28(4) y
C41 O40 C44 C43 . -24(3) y
C42 C43 C44 O40 . 33(4) y
|
1501611.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/16/1501611.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_1501611
loop_
_publ_author_name
'Dominic Lalibert\'e'
'Thierry Maris'
'James D. Wuest'
_publ_section_title
;
Molecular tectonics - Use of urethanes and ureas derived from
tetraphenylmethane and tetraphenylsilane to build porous chiral
hydrogenbonded networks
;
_journal_name_full 'Can. J. Chem.'
_journal_page_first 386
_journal_page_last 398
_journal_paper_doi 10.1139/v03-208
_journal_volume 82
_journal_year 2004
_chemical_compound_source 'Synthesized by the authors. See text'
_chemical_formula_sum 'C44 H56 N4 O12 Si'
_chemical_formula_weight 861.02
_chemical_name_systematic
;
?
;
_space_group_IT_number 86
_symmetry_cell_setting tetragonal
_symmetry_space_group_name_Hall '-P 4bc'
_symmetry_space_group_name_H-M 'P 42/n :2'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 2
_cell_length_a 17.7781(2)
_cell_length_b 17.7781(2)
_cell_length_c 7.19040(10)
_cell_measurement_reflns_used 9912
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 72.26
_cell_measurement_theta_min 2.49
_cell_volume 2272.60(5)
_computing_cell_refinement 'SMART (Bruker, 1999)'
_computing_data_collection 'SAINT (Bruker, 1999)'
_computing_data_reduction 'SAINT (Bruker, 1999)'
_computing_molecular_graphics 'XP (Bruker, 1999)'
_computing_publication_material 'UdMX (local program)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type 'Bruker AXS Smart 2K/Platform'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'Sealed Tube'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.025
_diffrn_reflns_av_sigmaI/netI 0.0194
_diffrn_reflns_limit_h_max 21
_diffrn_reflns_limit_h_min -19
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -22
_diffrn_reflns_limit_l_max 8
_diffrn_reflns_limit_l_min -8
_diffrn_reflns_number 15976
_diffrn_reflns_theta_full 72.89
_diffrn_reflns_theta_max 72.89
_diffrn_reflns_theta_min 3.52
_diffrn_standards_decay_% 0.00
_diffrn_standards_number 5
_exptl_absorpt_coefficient_mu 0.995
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_correction_T_min 0.7800
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Sadabs (Sheldrick,1996)'
_exptl_crystal_colour Colourless
_exptl_crystal_density_diffrn 1.258
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 916
_exptl_crystal_size_max 0.40
_exptl_crystal_size_mid 0.16
_exptl_crystal_size_min 0.14
_refine_diff_density_max 0.364
_refine_diff_density_min -0.162
_refine_diff_density_rms 0.067
_refine_ls_extinction_coef 0.0000(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 1.023
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 139
_refine_ls_number_reflns 2240
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.023
_refine_ls_R_factor_all 0.0879
_refine_ls_R_factor_gt 0.0724
_refine_ls_shift/su_max 3.990
_refine_ls_shift/su_mean 0.029
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1542P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2024
_refine_ls_wR_factor_ref 0.2160
_reflns_number_gt 1627
_reflns_number_total 2240
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file deposit.cif
_cod_data_source_block jiw371
_cod_original_sg_symbol_H-M P42/n
_cod_database_code 1501611
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y, x+1/2, z+1/2'
'y+1/2, -x, z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y, -x-1/2, -z-1/2'
'-y-1/2, x, -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
Si1 Si 0.2500 0.2500 1.2500 0.0522(4) Uani 1 4 d S
C2 C 0.25498(11) 0.33434(12) 1.0953(3) 0.0534(6) Uani 1 1 d .
C3 C 0.31634(12) 0.38327(13) 1.0861(3) 0.0612(6) Uani 1 1 d .
H3 H 0.3557 0.3773 1.1699 0.073 Uiso 1 1 calc .
C4 C 0.32006(13) 0.44029(13) 0.9561(4) 0.0638(6) Uani 1 1 d .
H4 H 0.3615 0.4722 0.9546 0.077 Uiso 1 1 calc .
C5 C 0.26310(12) 0.45061(12) 0.8282(3) 0.0559(6) Uani 1 1 d .
C6 C 0.20068(13) 0.40420(14) 0.8362(4) 0.0659(7) Uani 1 1 d .
H6 H 0.1611 0.4111 0.7535 0.079 Uiso 1 1 calc .
C7 C 0.19745(13) 0.34796(13) 0.9666(4) 0.0643(6) Uani 1 1 d .
H7 H 0.1550 0.3174 0.9697 0.077 Uiso 1 1 calc .
N8 N 0.27326(11) 0.50568(12) 0.6895(3) 0.0695(6) Uani 1 1 d .
H8 H 0.3166 0.5271 0.6854 0.083 Uiso 1 1 calc .
C9 C 0.22219(16) 0.52855(16) 0.5621(4) 0.0768(8) Uani 1 1 d .
O10 O 0.15698(12) 0.51303(14) 0.5551(4) 0.1106(8) Uani 1 1 d .
O11 O 0.25706(11) 0.57425(13) 0.4380(3) 0.0995(8) Uani 1 1 d .
C12 C 0.2115(2) 0.5999(3) 0.2835(6) 0.149(2) Uani 1 1 d .
H12A H 0.1870 0.5572 0.2257 0.179 Uiso 1 1 calc R
H12B H 0.1728 0.6337 0.3290 0.179 Uiso 1 1 calc R
C13 C 0.2559(3) 0.6375(3) 0.1507(7) 0.158(2) Uani 1 1 d .
H13A H 0.2249 0.6526 0.0479 0.236 Uiso 1 1 calc R
H13B H 0.2948 0.6044 0.1071 0.236 Uiso 1 1 calc R
H13C H 0.2784 0.6812 0.2064 0.236 Uiso 1 1 calc R
O20 O 0.47941(12) 0.93381(10) 0.0936(3) 0.0874(7) Uani 1 1 d .
C21 C 0.4846(3) 1.00338(19) 0.1854(5) 0.1116(12) Uani 1 1 d .
H21A H 0.5012 0.9949 0.3122 0.134 Uiso 1 1 calc R
H21B H 0.4351 1.0261 0.1906 0.134 Uiso 1 1 calc R
C22 C 0.4641(3) 0.9449(2) -0.0962(5) 0.1150(13) Uani 1 1 d .
H22A H 0.4132 0.9638 -0.1093 0.138 Uiso 1 1 calc R
H22B H 0.4666 0.8967 -0.1596 0.138 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
Si1 0.0547(5) 0.0547(5) 0.0473(7) 0.000 0.000 0.000
C2 0.0557(11) 0.0582(12) 0.0464(13) -0.0051(10) 0.0002(10) -0.0014(8)
C3 0.0595(12) 0.0670(13) 0.0571(15) 0.0042(11) -0.0107(11) -0.0051(9)
C4 0.0622(13) 0.0674(14) 0.0617(15) 0.0038(12) -0.0058(11) -0.0114(10)
C5 0.0634(13) 0.0600(12) 0.0443(13) 0.0011(10) 0.0021(10) 0.0041(9)
C6 0.0627(14) 0.0800(16) 0.0550(15) 0.0062(12) -0.0114(11) -0.0037(11)
C7 0.0624(13) 0.0724(14) 0.0582(15) 0.0062(12) -0.0087(11) -0.0144(10)
N8 0.0699(12) 0.0766(13) 0.0621(13) 0.0189(10) -0.0033(10) -0.0040(9)
C9 0.0702(16) 0.0968(19) 0.0635(17) 0.0212(14) 0.0028(13) 0.0072(13)
O10 0.0724(13) 0.157(2) 0.1025(17) 0.0559(16) -0.0051(12) 0.0045(12)
O11 0.0916(14) 0.1238(17) 0.0832(15) 0.0495(13) -0.0045(11) 0.0004(11)
C12 0.105(3) 0.229(5) 0.113(3) 0.104(4) -0.016(2) 0.005(3)
C13 0.194(5) 0.167(4) 0.112(3) 0.063(3) -0.010(3) 0.012(4)
O20 0.1205(15) 0.0671(11) 0.0747(14) 0.0017(10) -0.0070(12) 0.0057(10)
C21 0.184(4) 0.0764(19) 0.074(2) -0.0109(17) 0.020(2) -0.006(2)
C22 0.168(4) 0.081(2) 0.096(3) -0.0011(19) -0.042(2) -0.016(2)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 '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
C2 SI1 C2 7_568 2 110.75(7) y
C2 SI1 C2 7_568 . 110.75(7) y
C2 SI1 C2 2 . 106.94(13) y
C2 SI1 C2 7_568 8_658 106.94(13) y
C2 SI1 C2 2 8_658 110.75(7) y
C2 SI1 C2 . 8_658 110.75(7) y
C3 C2 C7 . . 115.6(2) y
C3 C2 SI1 . . 124.37(16) y
C7 C2 SI1 . . 119.83(16) y
C4 C3 C2 . . 121.8(2) y
C4 C3 H3 . . 119.1 ?
C2 C3 H3 . . 119.1 ?
C5 C4 C3 . . 120.9(2) y
C5 C4 H4 . . 119.5 ?
C3 C4 H4 . . 119.5 ?
C4 C5 C6 . . 118.8(2) y
C4 C5 N8 . . 118.0(2) y
C6 C5 N8 . . 123.1(2) y
C7 C6 C5 . . 119.8(2) y
C7 C6 H6 . . 120.1 ?
C5 C6 H6 . . 120.1 ?
C6 C7 C2 . . 123.2(2) y
C6 C7 H7 . . 118.4 ?
C2 C7 H7 . . 118.4 ?
C9 N8 C5 . . 127.0(2) y
C9 N8 H8 . . 116.5 ?
C5 N8 H8 . . 116.5 ?
O10 C9 N8 . . 127.7(3) y
O10 C9 O11 . . 123.7(2) y
N8 C9 O11 . . 108.6(2) y
C9 O11 C12 . . 116.0(3) y
C13 C12 O11 . . 110.9(3) y
C13 C12 H12A . . 109.5 ?
O11 C12 H12A . . 109.5 ?
C13 C12 H12B . . 109.5 ?
O11 C12 H12B . . 109.5 ?
H12A C12 H12B . . 108 ?
C12 C13 H13A . . 109.5 ?
C12 C13 H13B . . 109.5 ?
H13A C13 H13B . . 109.5 ?
C12 C13 H13C . . 109.5 ?
H13A C13 H13C . . 109.5 ?
H13B C13 H13C . . 109.5 ?
C21 O20 C22 . . 110.3(2) y
O20 C21 C22 . 5_675 113.2(3) y
O20 C21 H21A . . 108.9 ?
C22 C21 H21A 5_675 . 108.9 ?
O20 C21 H21B . . 108.9 ?
C22 C21 H21B 5_675 . 108.9 ?
H21A C21 H21B . . 107.8 ?
O20 C22 C21 . 5_675 113.4(3) y
O20 C22 H22A . . 108.9 ?
C21 C22 H22A 5_675 . 108.9 ?
O20 C22 H22B . . 108.9 ?
C21 C22 H22B 5_675 . 108.9 ?
H22A C22 H22B . . 107.7 ?
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
Si1 C2 7_568 1.869(2) y
Si1 C2 2 1.869(2) y
Si1 C2 . 1.869(2) y
Si1 C2 8_658 1.869(2) y
C2 C3 . 1.397(3) y
C2 C7 . 1.400(3) y
C3 C4 . 1.381(3) y
C3 H3 . 0.93 ?
C4 C5 . 1.380(3) y
C4 H4 . 0.93 ?
C5 C6 . 1.384(3) y
C5 N8 . 1.409(3) y
C6 C7 . 1.372(3) y
C6 H6 . 0.93 ?
C7 H7 . 0.93 ?
N8 C9 . 1.352(3) y
N8 H8 . 0.86 ?
C9 O10 . 1.193(3) y
C9 O11 . 1.357(3) y
O11 C12 . 1.448(4) y
C12 C13 . 1.408(6) y
C12 H12a . 0.97 ?
C12 H12b . 0.97 ?
C13 H13a . 0.96 ?
C13 H13b . 0.96 ?
C13 H13c . 0.96 ?
O20 C21 . 1.405(4) y
O20 C22 . 1.406(4) y
C21 C22 5_675 1.446(5) y
C21 H21a . 0.97 ?
C21 H21b . 0.97 ?
C22 C21 5_675 1.446(5) y
C22 H22a . 0.97 ?
C22 H22b . 0.97 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N8 H8 O20 0.86 2.19 2.948(3) 147.2 4_465
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_4
_geom_torsion
_geom_torsion_publ_flag
C2 SI1 C2 C3 7_568 . 4.93(19) y
C2 SI1 C2 C3 2 . -115.8(2) y
C2 SI1 C2 C3 8_658 . 123.4(2) y
C2 SI1 C2 C7 7_568 . 179.2(2) y
C2 SI1 C2 C7 2 . 58.46(17) y
C2 SI1 C2 C7 8_658 . -62.30(15) y
C7 C2 C3 C4 . . -1.1(3) y
SI1 C2 C3 C4 . . 173.40(19) y
C2 C3 C4 C5 . . -0.6(4) y
C3 C4 C5 C6 . . 2.1(4) y
C3 C4 C5 N8 . . -174.7(2) y
C4 C5 C6 C7 . . -1.8(4) y
N8 C5 C6 C7 . . 174.9(2) y
C5 C6 C7 C2 . . 0.0(4) y
C3 C2 C7 C6 . . 1.4(4) y
SI1 C2 C7 C6 . . -173.3(2) y
C4 C5 N8 C9 . . -174.1(3) y
C6 C5 N8 C9 . . 9.2(4) y
C5 N8 C9 O10 . . 9.0(5) y
C5 N8 C9 O11 . . -171.4(2) y
O10 C9 O11 C12 . . -4.5(5) y
N8 C9 O11 C12 . . 175.9(3) y
C9 O11 C12 C13 . . -171.4(4) y
C22 O20 C21 C22 . 5_675 -51.8(5) y
C21 O20 C22 C21 . 5_675 51.9(5) y
|
1501612.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/16/1501612.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_1501612
loop_
_publ_author_name
'Dominic Lalibert\'e'
'Thierry Maris'
'James D. Wuest'
_publ_section_title
;
Molecular tectonics - Use of urethanes and ureas derived from
tetraphenylmethane and tetraphenylsilane to build porous chiral
hydrogenbonded networks
;
_journal_name_full 'Can. J. Chem.'
_journal_page_first 386
_journal_page_last 398
_journal_paper_doi 10.1139/v03-208
_journal_volume 82
_journal_year 2004
_chemical_compound_source 'Synthesized by the authors. See text'
_chemical_formula_sum 'C47 H64 N8 O8'
_chemical_formula_weight 869.06
_chemical_name_systematic
;
?
;
_space_group_IT_number 80
_symmetry_cell_setting tetragonal
_symmetry_space_group_name_Hall 'I 4bw'
_symmetry_space_group_name_H-M 'I 41'
_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 17.2392(3)
_cell_length_b 17.2392(3)
_cell_length_c 17.3495(3)
_cell_measurement_reflns_used 16283
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 73.02
_cell_measurement_theta_min 3.61
_cell_volume 5156.10(16)
_computing_cell_refinement 'SMART (Bruker, 1999)'
_computing_data_collection 'SAINT (Bruker, 1999)'
_computing_data_reduction 'SAINT (Bruker, 1999)'
_computing_molecular_graphics 'XP (Bruker, 1999)'
_computing_publication_material 'UdMX (local program)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type 'Bruker AXS Smart 2K/Platform'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'Sealed Tube'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.037
_diffrn_reflns_av_sigmaI/netI 0.0281
_diffrn_reflns_limit_h_max 21
_diffrn_reflns_limit_h_min -21
_diffrn_reflns_limit_k_max 21
_diffrn_reflns_limit_k_min -21
_diffrn_reflns_limit_l_max 21
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 31370
_diffrn_reflns_theta_full 73.14
_diffrn_reflns_theta_max 73.14
_diffrn_reflns_theta_min 3.61
_diffrn_standards_decay_% 0.50
_diffrn_standards_number 214
_exptl_absorpt_coefficient_mu 0.627
_exptl_absorpt_correction_T_max 0.8100
_exptl_absorpt_correction_T_min 0.5800
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Sadabs (Sheldrick,1996)'
_exptl_crystal_colour Colourless
_exptl_crystal_density_diffrn 1.120
_exptl_crystal_description block
_exptl_crystal_F_000 1864
_exptl_crystal_size_max 0.90
_exptl_crystal_size_mid 0.70
_exptl_crystal_size_min 0.50
_refine_diff_density_max 0.489
_refine_diff_density_min -0.413
_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 -0.2(7)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.265
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 259
_refine_ls_number_reflns 4741
_refine_ls_number_restraints 37
_refine_ls_restrained_S_all 1.272
_refine_ls_R_factor_all 0.1357
_refine_ls_R_factor_gt 0.1089
_refine_ls_shift/su_max 0.023
_refine_ls_shift/su_mean 0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1750P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2813
_refine_ls_wR_factor_ref 0.3059
_reflns_number_gt 3218
_reflns_number_total 4741
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file deposit.cif
_cod_data_source_block jiw374
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana
;
_cod_original_sg_symbol_H-M I41
_cod_database_code 1501612
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-y, x+1/2, z+1/4'
'y+1/2, -x, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1, z+1'
'-y+1/2, x+1, z+3/4'
'y+1, -x+1/2, z+5/4'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.0000 0.5000 0.1019(4) 0.0491(9) Uani 1 2 d S . .
C11 C 0.0592(2) 0.4593(2) 0.0514(2) 0.0476(9) Uani 1 1 d . . .
C12 C 0.1383(3) 0.4514(3) 0.0700(3) 0.0689(12) Uani 1 1 d . . .
H12 H 0.1555 0.4744 0.1154 0.083 Uiso 1 1 calc . . .
C13 C 0.1916(3) 0.4126(3) 0.0266(3) 0.0719(13) Uani 1 1 d . . .
H13 H 0.2436 0.4116 0.0407 0.086 Uiso 1 1 calc . . .
C14 C 0.1661(3) 0.3743(3) -0.0393(2) 0.0680(12) Uani 1 1 d . . .
C15 C 0.0907(3) 0.3792(3) -0.0598(2) 0.0675(12) Uani 1 1 d . . .
H15 H 0.0737 0.3538 -0.1039 0.081 Uiso 1 1 calc . . .
C16 C 0.0376(2) 0.4221(3) -0.0157(2) 0.0612(10) Uani 1 1 d . . .
H16 H -0.0137 0.4254 -0.0321 0.073 Uiso 1 1 calc . . .
N17 N 0.2199(2) 0.3362(2) -0.0884(2) 0.0734(11) Uani 1 1 d . A .
H17 H 0.2110 0.3395 -0.1370 0.088 Uiso 1 1 calc . . .
C18 C 0.2812(4) 0.2968(3) -0.0683(3) 0.0805(15) Uani 1 1 d . . .
O18 O 0.3045(3) 0.2897(3) -0.0018(2) 0.1153(15) Uani 1 1 d . A .
C31 C -0.0425(2) 0.4377(2) 0.1546(2) 0.0515(9) Uani 1 1 d . . .
C32 C -0.0806(3) 0.4617(2) 0.2224(2) 0.0682(12) Uani 1 1 d . . .
H32 H -0.0792 0.5137 0.2367 0.082 Uiso 1 1 calc . . .
C33 C -0.1190(3) 0.4106(3) 0.2668(3) 0.0679(12) Uani 1 1 d . . .
H33 H -0.1426 0.4279 0.3118 0.082 Uiso 1 1 calc . . .
C34 C -0.1244(2) 0.3325(2) 0.2471(2) 0.0547(10) Uani 1 1 d . . .
C35 C -0.0869(3) 0.3104(3) 0.1816(3) 0.0710(13) Uani 1 1 d . . .
H35 H -0.0892 0.2585 0.1670 0.085 Uiso 1 1 calc . . .
C36 C -0.0451(2) 0.3618(2) 0.1355(2) 0.0578(10) Uani 1 1 d . . .
H36 H -0.0192 0.3439 0.0920 0.069 Uiso 1 1 calc . . .
N37 N -0.1652(2) 0.2831(2) 0.2972(2) 0.0702(11) Uani 1 1 d . B .
H37 H -0.1657 0.2956 0.3452 0.084 Uiso 1 1 calc . . .
C38 C -0.2049(3) 0.2161(3) 0.2767(3) 0.0802(15) Uani 1 1 d . . .
O38 O -0.2080(2) 0.1942(2) 0.20996(19) 0.0997(13) Uani 1 1 d . B .
N19 N 0.3345(5) 0.2699(5) -0.1252(5) 0.043(3) Uiso 0.312(12) 1 d PD A 1
H19 H 0.3216 0.2786 -0.1722 0.051 Uiso 0.31 1 calc P A 1
C20 C 0.4054(7) 0.2310(9) -0.1144(10) 0.081(5) Uiso 0.312(12) 1 d PD A 1
H20 H 0.4352 0.2411 -0.1615 0.097 Uiso 0.312(12) 1 calc PR A 1
C21 C 0.449(3) 0.274(3) -0.050(3) 0.39(5) Uiso 0.312(12) 1 d PD A 1
H21A H 0.4886 0.2415 -0.0269 0.470 Uiso 0.312(12) 1 calc PR A 1
H21B H 0.4139 0.2918 -0.0102 0.470 Uiso 0.312(12) 1 calc PR A 1
C22 C 0.487(4) 0.344(3) -0.092(6) 0.39(5) Uiso 0.312(12) 1 d PD A 1
H22A H 0.5420 0.3375 -0.0930 0.591 Uiso 0.312(12) 1 calc PR A 1
H22B H 0.4740 0.3910 -0.0653 0.591 Uiso 0.312(12) 1 calc PR A 1
H22C H 0.4674 0.3465 -0.1438 0.591 Uiso 0.312(12) 1 calc PR A 1
C23 C 0.417(5) 0.1441(16) -0.098(6) 0.40(5) Uiso 0.312(12) 1 d PD A 1
H23A H 0.3690 0.1215 -0.0819 0.599 Uiso 0.312(12) 1 calc PR A 1
H23B H 0.4551 0.1378 -0.0580 0.599 Uiso 0.312(12) 1 calc PR A 1
H23C H 0.4350 0.1186 -0.1440 0.599 Uiso 0.312(12) 1 calc PR A 1
N192 N 0.3010(6) 0.2433(6) -0.1251(6) 0.123(3) Uiso 0.688(12) 1 d PD A 2
H192 H 0.2741 0.2411 -0.1668 0.147 Uiso 0.69 1 calc P A 2
C202 C 0.3640(6) 0.1931(5) -0.1154(7) 0.114(3) Uiso 0.688(12) 1 d PD A 2
H202 H 0.3884 0.2128 -0.0683 0.137 Uiso 0.688(12) 1 calc PR A 2
C212 C 0.4266(12) 0.2091(12) -0.1773(11) 0.294(13) Uiso 0.688(12) 1 d PD A 2
H21C H 0.4635 0.1668 -0.1804 0.352 Uiso 0.688(12) 1 calc PR A 2
H21D H 0.4034 0.2171 -0.2276 0.352 Uiso 0.688(12) 1 calc PR A 2
C222 C 0.4658(7) 0.2842(7) -0.1474(9) 0.156(5) Uiso 0.688(12) 1 d PD A 2
H22D H 0.5072 0.2985 -0.1815 0.234 Uiso 0.688(12) 1 calc PR A 2
H22E H 0.4862 0.2753 -0.0967 0.234 Uiso 0.688(12) 1 calc PR A 2
H22F H 0.4282 0.3252 -0.1455 0.234 Uiso 0.688(12) 1 calc PR A 2
C232 C 0.367(3) 0.1050(8) -0.104(4) 0.45(3) Uiso 0.688(12) 1 d PD A 2
H23D H 0.3288 0.0896 -0.0671 0.676 Uiso 0.688(12) 1 calc PR A 2
H23E H 0.4178 0.0907 -0.0853 0.676 Uiso 0.688(12) 1 calc PR A 2
H23F H 0.3576 0.0795 -0.1521 0.676 Uiso 0.688(12) 1 calc PR A 2
N39 N -0.2473(5) 0.1854(4) 0.3356(4) 0.045(2) Uiso 0.432(14) 1 d PD B 3
H39 H -0.2497 0.2097 0.3789 0.055 Uiso 0.43 1 calc P B 3
C40 C -0.2872(6) 0.1147(4) 0.3270(5) 0.058(3) Uiso 0.432(14) 1 d PD B 3
H40 H -0.3152 0.1195 0.2780 0.070 Uiso 0.432(14) 1 calc PR B 3
C41 C -0.3497(8) 0.1232(8) 0.3895(8) 0.116(6) Uiso 0.432(14) 1 d PD B 3
H41A H -0.3251 0.1252 0.4398 0.139 Uiso 0.432(14) 1 calc PR B 3
H41B H -0.3835 0.0782 0.3885 0.139 Uiso 0.432(14) 1 calc PR B 3
C42 C -0.3986(10) 0.1972(9) 0.3776(12) 0.122(6) Uiso 0.432(14) 1 d PD B 3
H42A H -0.4354 0.2021 0.4188 0.183 Uiso 0.432(14) 1 calc PR B 3
H42B H -0.4256 0.1939 0.3293 0.183 Uiso 0.432(14) 1 calc PR B 3
H42C H -0.3651 0.2417 0.3771 0.183 Uiso 0.432(14) 1 calc PR B 3
C43 C -0.2439(9) 0.0374(7) 0.3213(10) 0.120(6) Uiso 0.432(14) 1 d PD B 3
H43A H -0.2099 0.0383 0.2775 0.180 Uiso 0.432(14) 1 calc PR B 3
H43B H -0.2806 -0.0041 0.3157 0.180 Uiso 0.432(14) 1 calc PR B 3
H43C H -0.2139 0.0295 0.3673 0.180 Uiso 0.432(14) 1 calc PR B 3
N392 N -0.2145(6) 0.1718(4) 0.3408(4) 0.069(2) Uiso 0.568(14) 1 d PD B 4
H392 H -0.1957 0.1873 0.3840 0.082 Uiso 0.57 1 calc P B 4
C402 C -0.2536(10) 0.1032(5) 0.3374(9) 0.126(5) Uiso 0.568(14) 1 d PD B 4
H402 H -0.2587 0.0859 0.2838 0.152 Uiso 0.568(14) 1 calc PR B 4
C412 C -0.3343(12) 0.113(2) 0.374(2) 0.37(3) Uiso 0.568(14) 1 d PD B 4
H41C H -0.3264 0.1282 0.4276 0.446 Uiso 0.568(14) 1 calc PR B 4
H41D H -0.3593 0.0631 0.3745 0.446 Uiso 0.568(14) 1 calc PR B 4
C422 C -0.3920(11) 0.1718(13) 0.3390(14) 0.175(7) Uiso 0.568(14) 1 d PD B 4
H42D H -0.4422 0.1644 0.3618 0.262 Uiso 0.568(14) 1 calc PR B 4
H42E H -0.3953 0.1635 0.2844 0.262 Uiso 0.568(14) 1 calc PR B 4
H42F H -0.3744 0.2237 0.3489 0.262 Uiso 0.568(14) 1 calc PR B 4
C432 C -0.2065(15) 0.0431(15) 0.3851(19) 0.273(14) Uiso 0.568(14) 1 d PD B 4
H43D H -0.1535 0.0431 0.3681 0.410 Uiso 0.568(14) 1 calc PR B 4
H43E H -0.2283 -0.0077 0.3779 0.410 Uiso 0.568(14) 1 calc PR B 4
H43F H -0.2086 0.0567 0.4387 0.410 Uiso 0.568(14) 1 calc PR B 4
O70 O 0.4882(16) 0.4477(17) 0.820(2) 0.500 Uiso 1 1 d D C 5
C71 C 0.465(2) 0.466(3) 0.743(3) 0.500 Uiso 1 1 d D . 5
O72 O 0.529(2) 0.455(2) 0.7034(18) 0.500 Uiso 1 1 d D . 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_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.062(3) 0.052(3) 0.0340(18) 0.000 0.000 -0.006(3)
C11 0.0453(19) 0.059(2) 0.0382(18) 0.0095(16) 0.0040(15) -0.0096(17)
C12 0.068(3) 0.088(3) 0.050(3) -0.010(2) -0.011(2) 0.000(2)
C13 0.059(2) 0.086(3) 0.070(3) -0.014(3) -0.017(2) 0.017(2)
C14 0.098(3) 0.068(3) 0.038(2) -0.006(2) -0.005(2) -0.006(2)
C15 0.072(3) 0.102(3) 0.0284(19) -0.024(2) 0.0035(18) -0.018(2)
C16 0.059(2) 0.074(3) 0.051(3) -0.005(2) -0.0026(19) -0.0117(19)
N17 0.089(3) 0.092(3) 0.040(2) 0.0003(18) 0.0148(18) 0.024(2)
C18 0.102(4) 0.097(4) 0.043(3) -0.001(2) 0.001(2) 0.025(3)
O18 0.131(3) 0.154(4) 0.061(2) -0.010(2) -0.008(2) 0.074(3)
C31 0.055(2) 0.065(2) 0.0341(18) 0.0019(17) 0.0094(16) -0.0063(18)
C32 0.116(4) 0.055(2) 0.034(2) -0.0038(18) 0.020(2) -0.005(2)
C33 0.078(3) 0.072(3) 0.053(3) -0.011(2) 0.013(2) -0.013(2)
C34 0.079(3) 0.0455(18) 0.0400(19) 0.0168(16) 0.0067(19) -0.0119(17)
C35 0.107(3) 0.060(2) 0.046(2) 0.000(2) 0.022(2) -0.009(2)
C36 0.072(3) 0.059(2) 0.043(2) -0.0038(17) 0.0228(19) -0.0064(19)
N37 0.095(3) 0.077(2) 0.039(2) -0.0012(17) 0.0215(18) -0.014(2)
C38 0.107(4) 0.078(3) 0.056(3) 0.014(2) 0.026(3) -0.030(3)
O38 0.143(3) 0.117(3) 0.0399(18) -0.0047(19) 0.0124(19) -0.056(2)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
C11 C1 C11 6_454 . 109.5(5) y
C11 C1 C31 6_454 6_454 109.3(2) y
C11 C1 C31 . 6_454 109.6(2) y
C11 C1 C31 6_454 . 109.6(2) y
C11 C1 C31 . . 109.3(2) y
C31 C1 C31 6_454 . 109.7(5) y
C16 C11 C12 . . 114.2(4) y
C16 C11 C1 . . 121.3(3) y
C12 C11 C1 . . 124.3(4) y
C13 C12 C11 . . 124.9(4) y
C13 C12 H12 . . 117.5 ?
C11 C12 H12 . . 117.5 ?
C12 C13 C14 . . 118.3(4) y
C12 C13 H13 . . 120.8 ?
C14 C13 H13 . . 120.9 ?
C15 C14 C13 . . 119.4(4) y
C15 C14 N17 . . 120.0(4) y
C13 C14 N17 . . 120.4(4) y
C14 C15 C16 . . 121.2(4) y
C14 C15 H15 . . 119.4 ?
C16 C15 H15 . . 119.4 ?
C11 C16 C15 . . 121.8(4) y
C11 C16 H16 . . 119.1 ?
C15 C16 H16 . . 119.1 ?
C18 N17 C14 . . 127.6(4) y
C18 N17 H17 . . 116.2 ?
C14 N17 H17 . . 116.2 ?
O18 C18 N17 . . 124.6(5) y
O18 C18 N192 . . 121.3(6) y
N17 C18 N192 . . 110.8(6) y
O18 C18 N19 . . 114.0(6) y
N17 C18 N19 . . 120.5(5) y
N192 C18 N19 . . 30.3(4) y
C36 C31 C32 . . 118.2(3) y
C36 C31 C1 . . 122.0(3) y
C32 C31 C1 . . 119.8(3) y
C33 C32 C31 . . 121.1(4) y
C33 C32 H32 . . 119.5 ?
C31 C32 H32 . . 119.5 ?
C32 C33 C34 . . 121.7(4) y
C32 C33 H33 . . 119.1 ?
C34 C33 H33 . . 119.1 ?
C35 C34 C33 . . 116.3(3) y
C35 C34 N37 . . 125.8(3) y
C33 C34 N37 . . 117.8(4) y
C34 C35 C36 . . 123.1(4) y
C34 C35 H35 . . 118.4 ?
C36 C35 H35 . . 118.4 ?
C31 C36 C35 . . 119.5(4) y
C31 C36 H36 . . 120.2 ?
C35 C36 H36 . . 120.2 ?
C38 N37 C34 . . 126.2(4) y
C38 N37 H37 . . 116.9 ?
C34 N37 H37 . . 116.9 ?
O38 C38 N392 . . 126.7(5) y
O38 C38 N39 . . 124.7(5) y
N392 C38 N39 . . 26.3(3) y
O38 C38 N37 . . 121.5(4) y
N392 C38 N37 . . 108.5(5) y
N39 C38 N37 . . 113.2(5) y
C20 N19 C18 . . 128.6(1) y
C20 N19 H19 . . 115.7 ?
C18 N19 H19 . . 115.7 ?
N19 C20 C23 . . 127(3) y
N19 C20 C21 . . 107(2) y
C23 C20 C21 . . 106(3) y
N19 C20 H20 . . 105 ?
C23 C20 H20 . . 105 ?
C21 C20 H20 . . 105 ?
C20 C21 C22 . . 103.9(8) y
C20 C21 H21A . . 111 ?
C22 C21 H21A . . 111 ?
C20 C21 H21B . . 111 ?
C22 C21 H21B . . 111 ?
H21A C21 H21B . . 109 ?
C21 C22 H22A . . 109.5 ?
C21 C22 H22B . . 109.5 ?
H22A C22 H22B . . 109.5 ?
C21 C22 H22C . . 109.5 ?
H22A C22 H22C . . 109.5 ?
H22B C22 H22C . . 109.5 ?
C20 C23 H23A . . 109.4 ?
C20 C23 H23B . . 109.5 ?
H23A C23 H23B . . 109.5 ?
C20 C23 H23C . . 109.5 ?
H23A C23 H23C . . 109.5 ?
H23B C23 H23C . . 109.5 ?
C18 N192 C202 . . 121.0(8) y
C18 N192 H192 . . 119.5 ?
C202 N192 H192 . . 119.5 ?
N192 C202 C232 . . 131(2) y
N192 C202 C212 . . 110.40(13) y
C232 C202 C212 . . 104(2) y
N192 C202 H202 . . 102.6 ?
C232 C202 H202 . . 102.6 ?
C212 C202 H202 . . 102.6 ?
C222 C212 C202 . . 102.7(7) y
C222 C212 H21C . . 111.2 ?
C202 C212 H21C . . 111.2 ?
C222 C212 H21D . . 111.2 ?
C202 C212 H21D . . 111.2 ?
H21C C212 H21D . . 109.1 ?
C212 C222 H22D . . 109.5 ?
C212 C222 H22E . . 109.5 ?
H22D C222 H22E . . 109.5 ?
C212 C222 H22F . . 109.5 ?
H22D C222 H22F . . 109.5 ?
H22E C222 H22F . . 109.5 ?
C202 C232 H23D . . 109.5 ?
C202 C232 H23E . . 109.5 ?
H23D C232 H23E . . 109.5 ?
C202 C232 H23F . . 109.5 ?
H23D C232 H23F . . 109.5 ?
H23E C232 H23F . . 109.5 ?
C38 N39 C40 . . 121.2(6) y
C38 N39 H39 . . 119.4 ?
C40 N39 H39 . . 119.4 ?
N39 C40 C43 . . 121.5(1) y
N39 C40 C41 . . 100.6(8) y
C43 C40 C41 . . 118.0(9) y
N39 C40 H40 . . 105 ?
C43 C40 H40 . . 105 ?
C41 C40 H40 . . 105 ?
C40 C41 C42 . . 111.50(11) y
C40 C41 H41A . . 109.3 ?
C42 C41 H41A . . 109.3 ?
C40 C41 H41B . . 109.3 ?
C42 C41 H41B . . 109.3 ?
H41A C41 H41B . . 108 ?
C41 C42 H42A . . 109.5 ?
C41 C42 H42B . . 109.5 ?
H42A C42 H42B . . 109.5 ?
C41 C42 H42C . . 109.5 ?
H42A C42 H42C . . 109.5 ?
H42B C42 H42C . . 109.5 ?
C40 C43 H43A . . 109.5 ?
C40 C43 H43B . . 109.5 ?
H43A C43 H43B . . 109.5 ?
C40 C43 H43C . . 109.5 ?
H43A C43 H43C . . 109.5 ?
H43B C43 H43C . . 109.5 ?
C38 N392 C402 . . 120.9(9) y
C38 N392 H392 . . 119.6 ?
C402 N392 H392 . . 119.6 ?
N392 C402 C412 . . 109.20(18) y
N392 C402 C432 . . 107.30(15) y
C412 C402 C432 . . 109.20(15) y
N392 C402 H402 . . 110.4 ?
C412 C402 H402 . . 110.4 ?
C432 C402 H402 . . 110.4 ?
C402 C412 C422 . . 119.60(18) y
C402 C412 H41C . . 107.4 ?
C422 C412 H41C . . 107.4 ?
C402 C412 H41D . . 107.4 ?
C422 C412 H41D . . 107.4 ?
H41C C412 H41D . . 107 ?
C412 C422 H42D . . 109.5 ?
C412 C422 H42E . . 109.5 ?
H42D C422 H42E . . 109.5 ?
C412 C422 H42F . . 109.5 ?
H42D C422 H42F . . 109.5 ?
H42E C422 H42F . . 109.5 ?
C402 C432 H43D . . 109.5 ?
C402 C432 H43E . . 109.5 ?
H43D C432 H43E . . 109.5 ?
C402 C432 H43F . . 109.5 ?
H43D C432 H43F . . 109.5 ?
H43E C432 H43F . . 109.5 ?
O72 C71 O70 . . 104(3) y
O72 C71 O72 . 6_554 80(3) y
O70 C71 O72 . 6_554 127(4) y
O72 C71 C71 . 6_554 60(2) y
O70 C71 C71 . 6_554 88(3) y
O72 C71 C71 6_554 6_554 48(2) y
C71 O72 C71 . 6_554 72(4) y
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
C1 C11 6_454 1.517(5) y
C1 C11 . 1.517(5) y
C1 C31 6_454 1.589(5) y
C1 C31 . 1.589(5) y
C11 C16 . 1.380(5) y
C11 C12 . 1.408(6) y
C12 C13 . 1.364(6) y
C12 H12 . 0.9301 ?
C13 C14 . 1.391(6) y
C13 H13 . 0.93 ?
C14 C15 . 1.349(6) y
C14 N17 . 1.420(6) y
C15 C16 . 1.404(6) y
C15 H15 . 0.9299 ?
C16 H16 . 0.93 ?
N17 C18 . 1.304(6) y
N17 H17 . 0.8599 ?
C18 O18 . 1.228(6) y
C18 N192 . 1.391(10) y
C18 N19 . 1.425(10) y
C31 C36 . 1.352(6) y
C31 C32 . 1.410(5) y
C32 C33 . 1.344(6) y
C32 H32 . 0.93 ?
C33 C34 . 1.393(5) y
C33 H33 . 0.93 ?
C34 C35 . 1.362(6) y
C34 N37 . 1.405(5) y
C35 C36 . 1.394(6) y
C35 H35 . 0.93 ?
C36 H36 . 0.9299 ?
N37 C38 . 1.389(6) y
N37 H37 . 0.8601 ?
C38 O38 . 1.219(6) y
C38 N392 . 1.359(8) y
C38 N39 . 1.364(8) y
N19 C20 . 1.407(8) y
N19 H19 . 0.8599 ?
C20 C23 . 1.538(8) y
C20 C21 . 1.543(9) y
C20 H20 . 0.98 ?
C21 C22 . 1.543(9) y
C21 H21a . 0.97 ?
C21 H21b . 0.97 ?
C22 H22a . 0.96 ?
C22 H22b . 0.96 ?
C22 H22c . 0.96 ?
C23 H23a . 0.96 ?
C23 H23b . 0.96 ?
C23 H23c . 0.96 ?
N192 C202 . 1.398(11) y
N192 H192 . 0.8599 ?
C202 C232 . 1.534(8) y
C202 C212 . 1.549(8) y
C202 H202 . 0.98 ?
C212 C222 . 1.548(8) y
C212 H21c . 0.97 ?
C212 H21d . 0.97 ?
C222 H22d . 0.96 ?
C222 H22e . 0.96 ?
C222 H22f . 0.96 ?
C232 H23d . 0.96 ?
C232 H23e . 0.96 ?
C232 H23f . 0.96 ?
N39 C40 . 1.408(7) y
N39 H39 . 0.8601 ?
C40 C43 . 1.531(8) y
C40 C41 . 1.536(8) y
C40 H40 . 0.98 ?
C41 C42 . 1.543(8) y
C41 H41a . 0.97 ?
C41 H41b . 0.97 ?
C42 H42a . 0.96 ?
C42 H42b . 0.96 ?
C42 H42c . 0.96 ?
C43 H43a . 0.96 ?
C43 H43b . 0.96 ?
C43 H43c . 0.96 ?
N392 C402 . 1.363(10) y
N392 H392 . 0.8601 ?
C402 C412 . 1.540(8) y
C402 C432 . 1.555(8) y
C402 H402 . 0.98 ?
C412 C422 . 1.540(8) y
C412 H41c . 0.97 ?
C412 H41d . 0.97 ?
C422 H42d . 0.96 ?
C422 H42e . 0.96 ?
C422 H42f . 0.96 ?
C432 H43d . 0.96 ?
C432 H43e . 0.96 ?
C432 H43f . 0.96 ?
O70 C71 . 1.421(9) y
C71 O72 . 1.307(9) y
C71 O72 6_554 1.53(4) y
C71 C71 6_554 1.68(9) y
O72 C71 6_554 1.53(4) y
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N17 H17 O18 0.86 2.08 2.893(5) 157.1 7_544
N37 H37 O38 0.86 2.05 2.872(5) 159.1 3
N19 H19 O18 0.86 2.41 3.126(10) 141.6 7_544
N192 H192 O18 0.86 2.14 2.898(10) 146.6 7_544
N392 H392 O38 0.86 2.24 2.948(8) 140.2 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_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C11 C1 C11 C16 6_454 . -38.9(3) y
C31 C1 C11 C16 6_454 . -158.7(4) y
C31 C1 C11 C16 . . 81.1(5) y
C11 C1 C11 C12 6_454 . 145.4(4) y
C31 C1 C11 C12 6_454 . 25.6(5) y
C31 C1 C11 C12 . . -94.6(4) y
C16 C11 C12 C13 . . 1.5(7) y
C1 C11 C12 C13 . . 177.5(4) y
C11 C12 C13 C14 . . -3.3(8) y
C12 C13 C14 C15 . . 2.5(7) y
C12 C13 C14 N17 . . 177.0(4) y
C13 C14 C15 C16 . . -0.2(7) y
N17 C14 C15 C16 . . -174.6(4) y
C12 C11 C16 C15 . . 1.0(6) y
C1 C11 C16 C15 . . -175.1(4) y
C14 C15 C16 C11 . . -1.7(7) y
C15 C14 N17 C18 . . -147.4(5) y
C13 C14 N17 C18 . . 38.2(7) y
C14 N17 C18 O18 . . -4.0(1) y
C14 N17 C18 N192 . . 155.6(7) y
C14 N17 C18 N19 . . -172.4(6) y
C11 C1 C31 C36 6_454 . 97.7(4) y
C11 C1 C31 C36 . . -22.2(5) y
C31 C1 C31 C36 6_454 . -142.3(4) y
C11 C1 C31 C32 6_454 . -80.6(5) y
C11 C1 C31 C32 . . 159.5(4) y
C31 C1 C31 C32 6_454 . 39.4(3) y
C36 C31 C32 C33 . . -0.5(7) y
C1 C31 C32 C33 . . 177.9(4) y
C31 C32 C33 C34 . . -1.4(8) y
C32 C33 C34 C35 . . 1.7(7) y
C32 C33 C34 N37 . . 179.5(5) y
C33 C34 C35 C36 . . -0.2(7) y
N37 C34 C35 C36 . . -177.8(4) y
C32 C31 C36 C35 . . 1.9(7) y
C1 C31 C36 C35 . . -176.4(4) y
C34 C35 C36 C31 . . -1.7(7) y
C35 C34 N37 C38 . . -31.4(7) y
C33 C34 N37 C38 . . 151.0(5) y
C34 N37 C38 O38 . . -0.6(8) y
C34 N37 C38 N392 . . 160.2(6) y
C34 N37 C38 N39 . . -172.1(6) y
O18 C18 N19 C20 . . 6.20(14) y
N17 C18 N19 C20 . . 175.80(11) y
N192 C18 N19 C20 . . -105.10(15) y
C18 N19 C20 C23 . . 81(5) y
C18 N19 C20 C21 . . -46(3) y
N19 C20 C21 C22 . . -81(5) y
C23 C20 C21 C22 . . 141(6) y
O18 C18 N192 C202 . . -18.10(14) y
N17 C18 N192 C202 . . -178.5(8) y
N19 C18 N192 C202 . . 66.40(11) y
C18 N192 C202 C232 . . 111(3) y
C18 N192 C202 C212 . . -117.10(11) y
N192 C202 C212 C222 . . 76.40(17) y
C232 C202 C212 C222 . . -139(3) y
O38 C38 N39 C40 . . 13.10(12) y
N392 C38 N39 C40 . . -90.90(12) y
N37 C38 N39 C40 . . -175.8(7) y
C38 N39 C40 C43 . . 70.60(13) y
C38 N39 C40 C41 . . -156.8(1) y
N39 C40 C41 C42 . . 56.70(15) y
C43 C40 C41 C42 . . -168.80(14) y
O38 C38 N392 C402 . . -22.10(12) y
N39 C38 N392 C402 . . 73.20(11) y
N37 C38 N392 C402 . . 178.3(8) y
C38 N392 C402 C412 . . -105.40(17) y
C38 N392 C402 C432 . . 136.40(16) y
N392 C402 C412 C422 . . 62(4) y
C432 C402 C412 C422 . . 178(3) y
O70 C71 O72 C71 . 6_554 -79(3) y
O72 C71 O72 C71 6_554 6_554 47(3) y
|
1501613.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/16/1501613.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_1501613
loop_
_publ_author_name
'Dominic Lalibert\'e'
'Thierry Maris'
'James D. Wuest'
_publ_section_title
;
Molecular tectonics - Use of urethanes and ureas derived from
tetraphenylmethane and tetraphenylsilane to build porous chiral
hydrogenbonded networks
;
_journal_name_full 'Can. J. Chem.'
_journal_page_first 386
_journal_page_last 398
_journal_paper_doi 10.1139/v03-208
_journal_volume 82
_journal_year 2004
_chemical_compound_source 'Synthesized by the authors. See text'
_chemical_formula_sum 'C55 H80 N4 O8'
_chemical_formula_weight 925.23
_chemical_name_systematic
;
?
;
_space_group_IT_number 80
_symmetry_cell_setting tetragonal
_symmetry_space_group_name_Hall 'I 4bw'
_symmetry_space_group_name_H-M 'I 41'
_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 17.7201(6)
_cell_length_b 17.7201(6)
_cell_length_c 16.0845(7)
_cell_measurement_reflns_used 4677
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 71.09
_cell_measurement_theta_min 3.53
_cell_volume 5050.6(3)
_computing_cell_refinement 'SMART (Bruker, 1999)'
_computing_data_collection 'SMART (Bruker, 1999)'
_computing_data_reduction 'SAINT (Bruker, 1999)'
_computing_molecular_graphics 'SHELXTL (Bruker, 1997)'
_computing_publication_material 'UdMX (local program)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type 'Bruker AXS Smart 2K/Platform'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'Sealed Tube'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.065
_diffrn_reflns_av_sigmaI/netI 0.1005
_diffrn_reflns_limit_h_max 21
_diffrn_reflns_limit_h_min -21
_diffrn_reflns_limit_k_max 21
_diffrn_reflns_limit_k_min -21
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -20
_diffrn_reflns_number 16858
_diffrn_reflns_theta_full 73.85
_diffrn_reflns_theta_max 73.85
_diffrn_reflns_theta_min 3.53
_diffrn_standards_decay_% -1.79
_diffrn_standards_number 142
_exptl_absorpt_coefficient_mu 0.643
_exptl_absorpt_correction_T_max 0.8300
_exptl_absorpt_correction_T_min 0.3100
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Sadabs (Sheldrick,1996)'
_exptl_crystal_colour Colourless
_exptl_crystal_density_diffrn 1.217
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 2008
_exptl_crystal_size_max 0.50
_exptl_crystal_size_mid 0.30
_exptl_crystal_size_min 0.30
_refine_diff_density_max 0.223
_refine_diff_density_min -0.290
_refine_diff_density_rms 0.055
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack 0.1(18)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.038
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 267
_refine_ls_number_reflns 4837
_refine_ls_number_restraints 12
_refine_ls_restrained_S_all 1.040
_refine_ls_R_factor_all 0.1946
_refine_ls_R_factor_gt 0.1022
_refine_ls_shift/su_max 1.093
_refine_ls_shift/su_mean 0.057
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1250P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2493
_refine_ls_wR_factor_ref 0.2888
_reflns_number_gt 1859
_reflns_number_total 4837
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file deposit.cif
_cod_data_source_block jiw377
_cod_original_sg_symbol_H-M I41
_cod_database_code 1501613
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-y, x+1/2, z+1/4'
'y+1/2, -x, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1, z+1'
'-y+1/2, x+1, z+3/4'
'y+1, -x+1/2, z+5/4'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
C1 C 0.0000 0.5000 0.23756(15) 0.0619(5) Uani 1 2 d S
C11 C 0.06197(7) 0.53753(7) 0.18495(8) 0.0597(4) Uani 1 1 d .
C12 C 0.13589(7) 0.54089(7) 0.20704(8) 0.0662(5) Uani 1 1 d .
H12 H 0.1508 0.5162 0.2554 0.079 Uiso 1 1 calc .
C13 C 0.19205(8) 0.58016(9) 0.16036(10) 0.0911(6) Uani 1 1 d .
H13 H 0.2414 0.5826 0.1798 0.109 Uiso 1 1 calc .
C14 C 0.17289(7) 0.61457(8) 0.08615(8) 0.0708(5) Uani 1 1 d .
C15 C 0.09643(8) 0.61134(8) 0.06170(8) 0.0725(5) Uani 1 1 d .
H15 H 0.0815 0.6353 0.0129 0.087 Uiso 1 1 calc .
C16 C 0.04375(7) 0.57374(7) 0.10815(9) 0.0749(5) Uani 1 1 d .
H16 H -0.0057 0.5717 0.0890 0.090 Uiso 1 1 calc .
N17 N 0.22150(7) 0.65040(7) 0.03312(8) 0.0956(5) Uani 1 1 d .
H17 H 0.2075 0.6571 -0.0175 0.115 Uiso 1 1 calc .
C18 C 0.29044(11) 0.67593(9) 0.05595(10) 0.1148(7) Uani 1 1 d .
O18 O 0.32422(6) 0.66481(7) 0.12083(7) 0.1334(5) Uani 1 1 d .
O19 O 0.31949(7) 0.71331(9) -0.00934(9) 0.1739(6) Uani 1 1 d .
C20 C 0.39873(19) 0.75719(15) 0.01419(15) 0.3083(3) Uani 1 1 d DU
H20 H 0.4146 0.7710 0.0705 0.370 Uiso 1 1 calc .
C21 C 0.4437(2) 0.70792(15) -0.0451(2) 0.4316(4) Uani 1 1 d DU
H21A H 0.4859 0.7373 -0.0658 0.518 Uiso 1 1 calc R
H21B H 0.4118 0.6960 -0.0923 0.518 Uiso 1 1 calc R
C22 C 0.4754(2) 0.63187(19) -0.0089(3) 0.4657(9) Uani 1 1 d DU
H22A H 0.5092 0.6094 -0.0484 0.698 Uiso 1 1 calc R
H22B H 0.4344 0.5979 0.0020 0.698 Uiso 1 1 calc R
H22C H 0.5021 0.6419 0.0419 0.698 Uiso 1 1 calc R
C23 C 0.3862(2) 0.81319(17) -0.0574(2) 0.3518(5) Uani 1 1 d DU
H23A H 0.3525 0.8524 -0.0396 0.528 Uiso 1 1 calc R
H23B H 0.3646 0.7872 -0.1041 0.528 Uiso 1 1 calc R
H23C H 0.4337 0.8350 -0.0734 0.528 Uiso 1 1 calc R
C31 C -0.03720(7) 0.56057(7) 0.29465(8) 0.0633(5) Uani 1 1 d .
C32 C -0.07288(7) 0.54214(7) 0.36638(9) 0.0736(5) Uani 1 1 d .
H32 H -0.0724 0.4922 0.3841 0.088 Uiso 1 1 calc .
C33 C -0.11020(8) 0.59574(8) 0.41425(9) 0.0814(5) Uani 1 1 d .
H33 H -0.1331 0.5817 0.4639 0.098 Uiso 1 1 calc .
C34 C -0.11301(7) 0.66780(7) 0.38857(9) 0.0716(5) Uani 1 1 d .
C35 C -0.07633(8) 0.68821(7) 0.31685(8) 0.0739(5) Uani 1 1 d .
H35 H -0.0766 0.7382 0.2994 0.089 Uiso 1 1 calc .
C36 C -0.04042(7) 0.63623(8) 0.27257(10) 0.0808(5) Uani 1 1 d .
H36 H -0.0161 0.6513 0.2241 0.097 Uiso 1 1 calc .
N37 N -0.15486(7) 0.72167(6) 0.44025(7) 0.0846(4) Uani 1 1 d .
H37 H -0.1652 0.7065 0.4898 0.102 Uiso 1 1 calc .
C38 C -0.17869(9) 0.78932(8) 0.42188(9) 0.0898(6) Uani 1 1 d .
O38 O -0.16959(6) 0.82142(5) 0.35780(7) 0.1063(4) Uani 1 1 d .
O39 O -0.21845(7) 0.81794(6) 0.48487(7) 0.1189(5) Uani 1 1 d .
C40 C -0.26446(10) 0.88448(8) 0.47040(10) 0.1337(7) Uani 1 1 d D
H40 H -0.2865 0.8805 0.4147 0.160 Uiso 1 1 calc .
C41 C -0.32826(10) 0.88069(10) 0.53370(16) 0.1990(11) Uani 1 1 d D
H41A H -0.3604 0.9247 0.5279 0.239 Uiso 1 1 calc R
H41B H -0.3075 0.8807 0.5895 0.239 Uiso 1 1 calc R
C42 C -0.37510(12) 0.80887(11) 0.5202(2) 0.2106(13) Uani 1 1 d D
H42A H -0.4140 0.8061 0.5616 0.316 Uiso 1 1 calc R
H42B H -0.3430 0.7654 0.5246 0.316 Uiso 1 1 calc R
H42C H -0.3976 0.8102 0.4659 0.316 Uiso 1 1 calc R
C43 C -0.21792(14) 0.95533(10) 0.47367(19) 0.2182(14) Uani 1 1 d D
H43A H -0.1803 0.9539 0.4307 0.327 Uiso 1 1 calc R
H43B H -0.1937 0.9590 0.5269 0.327 Uiso 1 1 calc R
H43C H -0.2500 0.9983 0.4654 0.327 Uiso 1 1 calc R
C101 C 0.5000 0.0000 0.1124(14) 0.779(13) Uiso 1 2 d S
C102 C 0.5000 0.0000 0.3520(13) 0.716(12) Uiso 1 2 d S
C103 C 0.5000 0.0000 0.1999(19) 0.920(18) Uiso 1 2 d S
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0664(10) 0.0446(10) 0.0746(10) 0.000 0.000 0.0142(12)
C11 0.0588(7) 0.0503(7) 0.0700(8) -0.0069(7) 0.0092(7) 0.0080(7)
C12 0.0535(7) 0.0752(9) 0.0700(8) -0.0003(8) 0.0022(7) -0.0022(7)
C13 0.0677(9) 0.0989(11) 0.1067(11) 0.0152(10) -0.0080(9) 0.0009(9)
C14 0.0692(9) 0.0713(8) 0.0718(9) -0.0119(8) -0.0008(8) -0.0099(8)
C15 0.0746(9) 0.0769(9) 0.0661(9) 0.0047(8) 0.0041(8) 0.0204(7)
C16 0.0634(8) 0.0700(9) 0.0914(10) -0.0076(8) -0.0083(9) 0.0047(7)
N17 0.0827(8) 0.1033(8) 0.1010(9) 0.0143(8) 0.0202(8) -0.0394(7)
C18 0.1354(14) 0.1093(12) 0.0996(12) 0.0377(10) 0.0109(11) -0.0265(11)
O18 0.1101(8) 0.1992(11) 0.0908(7) 0.0042(8) -0.0144(7) -0.0605(8)
O19 0.1518(10) 0.2289(11) 0.1409(10) 0.0441(9) 0.0216(8) -0.1107(8)
C20 0.3067(8) 0.3664(4) 0.2518(5) 0.0466(3) 0.0445(5) -0.1129(3)
C21 0.4036(9) 0.4183(3) 0.4730(9) -0.0353(3) 0.0223(5) 0.0304(3)
C22 0.3740(11) 0.6168(3) 0.406(2) 0.0520(5) -0.0365(12) 0.1307(4)
C23 0.4102(14) 0.3553(4) 0.2899(6) 0.0328(4) -0.0445(15) -0.0468(4)
C31 0.0571(8) 0.0526(8) 0.0802(9) 0.0131(7) 0.0091(8) 0.0080(7)
C32 0.0806(9) 0.0502(8) 0.0899(10) -0.0047(8) 0.0222(9) -0.0072(7)
C33 0.0737(9) 0.0728(9) 0.0976(11) -0.0014(9) 0.0224(9) 0.0110(8)
C34 0.0631(8) 0.0589(8) 0.0927(11) -0.0121(8) 0.0211(8) 0.0036(7)
C35 0.0882(10) 0.0554(8) 0.0782(9) 0.0022(8) 0.0185(8) 0.0220(8)
C36 0.0766(9) 0.0748(10) 0.0910(10) 0.0146(9) 0.0283(9) 0.0138(8)
N37 0.1045(9) 0.0780(7) 0.0712(8) 0.0132(7) 0.0049(7) 0.0096(7)
C38 0.1196(12) 0.0677(9) 0.0821(10) -0.0118(9) -0.0173(10) 0.0316(9)
O38 0.1206(7) 0.0829(7) 0.1154(8) -0.0040(7) 0.0199(7) 0.0431(6)
O39 0.1543(9) 0.1157(8) 0.0868(7) 0.0001(7) 0.0166(7) 0.0585(7)
C40 0.1840(15) 0.1001(11) 0.1170(12) 0.0047(11) 0.0579(12) 0.0819(10)
C41 0.1593(16) 0.1431(15) 0.295(2) -0.0646(17) 0.0663(17) 0.0744(12)
C42 0.1428(18) 0.1671(19) 0.322(3) -0.005(2) 0.073(2) 0.0445(16)
C43 0.284(3) 0.1111(15) 0.260(3) -0.0315(19) 0.068(3) 0.0282(19)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
C11 C1 C11 6_454 . 113.22(18) y
C11 C1 C31 6_454 . 108.66(6) y
C11 C1 C31 . . 109.17(6) y
C11 C1 C31 6_454 6_454 109.17(6) y
C11 C1 C31 . 6_454 108.66(6) y
C31 C1 C31 . 6_454 107.81(17) y
C12 C11 C16 . . 115.11(11) y
C12 C11 C1 . . 124.30(12) y
C16 C11 C1 . . 120.57(12) y
C11 C12 C13 . . 123.76(13) y
C11 C12 H12 . . 118.1 ?
C13 C12 H12 . . 118.1 ?
C14 C13 C12 . . 119.86(13) y
C14 C13 H13 . . 120.1 ?
C12 C13 H13 . . 120.1 ?
N17 C14 C13 . . 126.02(12) y
N17 C14 C15 . . 116.69(12) y
C13 C14 C15 . . 117.27(12) y
C16 C15 C14 . . 121.47(12) y
C16 C15 H15 . . 119.3 ?
C14 C15 H15 . . 119.3 ?
C15 C16 C11 . . 122.44(12) y
C15 C16 H16 . . 118.8 ?
C11 C16 H16 . . 118.8 ?
C18 N17 C14 . . 123.65(13) y
C18 N17 H17 . . 118.2 ?
C14 N17 H17 . . 118.2 ?
O18 C18 O19 . . 124.09(18) y
O18 C18 N17 . . 128.41(16) y
O19 C18 N17 . . 107.37(14) y
C18 O19 C20 . . 112.28(15) y
C21 C20 C23 . . 88.6(2) y
C21 C20 O19 . . 91.8(2) y
C23 C20 O19 . . 90.5(2) y
C21 C20 H20 . . 125 ?
C23 C20 H20 . . 125.1 ?
O19 C20 H20 . . 125 ?
C20 C21 C22 . . 116.6(3) y
C20 C21 H21A . . 108.1 ?
C22 C21 H21A . . 108.1 ?
C20 C21 H21B . . 108.1 ?
C22 C21 H21B . . 108.2 ?
H21A C21 H21B . . 107.3 ?
C21 C22 H22A . . 109.4 ?
C21 C22 H22B . . 109.4 ?
H22A C22 H22B . . 109.5 ?
C21 C22 H22C . . 109.5 ?
H22A C22 H22C . . 109.5 ?
H22B C22 H22C . . 109.5 ?
C20 C23 H23A . . 109.4 ?
C20 C23 H23B . . 109.5 ?
H23A C23 H23B . . 109.5 ?
C20 C23 H23C . . 109.5 ?
H23A C23 H23C . . 109.5 ?
H23B C23 H23C . . 109.5 ?
C32 C31 C36 . . 115.55(12) y
C32 C31 C1 . . 122.20(12) y
C36 C31 C1 . . 122.12(12) y
C31 C32 C33 . . 121.92(12) y
C31 C32 H32 . . 119 ?
C33 C32 H32 . . 119 ?
C34 C33 C32 . . 119.80(13) y
C34 C33 H33 . . 120.1 ?
C32 C33 H33 . . 120.1 ?
C33 C34 C35 . . 119.43(13) y
C33 C34 N37 . . 117.59(12) y
C35 C34 N37 . . 122.97(12) y
C36 C35 C34 . . 119.69(13) y
C36 C35 H35 . . 120.2 ?
C34 C35 H35 . . 120.1 ?
C35 C36 C31 . . 123.56(14) y
C35 C36 H36 . . 118.2 ?
C31 C36 H36 . . 118.2 ?
C38 N37 C34 . . 129.27(12) y
C38 N37 H37 . . 115.4 ?
C34 N37 H37 . . 115.4 ?
O38 C38 N37 . . 126.33(14) y
O38 C38 O39 . . 123.26(14) y
N37 C38 O39 . . 110.37(13) y
C38 O39 C40 . . 118.90(12) y
O39 C40 C43 . . 111.38(15) y
O39 C40 C41 . . 105.89(13) y
C43 C40 C41 . . 114.88(16) y
O39 C40 H40 . . 108.1 ?
C43 C40 H40 . . 108.2 ?
C41 C40 H40 . . 108.2 ?
C40 C41 C42 . . 110.07(18) y
C40 C41 H41A . . 109.6 ?
C42 C41 H41A . . 109.6 ?
C40 C41 H41B . . 109.6 ?
C42 C41 H41B . . 109.7 ?
H41A C41 H41B . . 108.2 ?
C41 C42 H42A . . 109.5 ?
C41 C42 H42B . . 109.5 ?
H42A C42 H42B . . 109.5 ?
C41 C42 H42C . . 109.5 ?
H42A C42 H42C . . 109.5 ?
H42B C42 H42C . . 109.5 ?
C40 C43 H43A . . 109.5 ?
C40 C43 H43B . . 109.5 ?
H43A C43 H43B . . 109.5 ?
C40 C43 H43C . . 109.5 ?
H43A C43 H43C . . 109.5 ?
H43B C43 H43C . . 109.5 ?
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
C1 C11 6_454 1.5376(18) y
C1 C11 . 1.5376(18) y
C1 C31 . 1.5588(19) y
C1 C31 6_454 1.5588(19) y
C11 C12 . 1.3584(17) y
C11 C16 . 1.4289(19) y
C12 C13 . 1.428(2) y
C12 H12 . 0.93 ?
C13 C14 . 1.383(2) y
C13 H13 . 0.9299 ?
C14 N17 . 1.3685(18) y
C14 C15 . 1.4120(18) y
C15 C16 . 1.3687(19) y
C15 H15 . 0.9301 ?
C16 H16 . 0.9299 ?
N17 C18 . 1.353(2) y
N17 H17 . 0.86 ?
C18 O18 . 1.219(2) y
C18 O19 . 1.344(2) y
O19 C20 . 1.649(3) y
C20 C21 . 1.519(4) y
C20 C23 . 1.537(4) y
C20 H20 . 0.9796 ?
C21 C22 . 1.572(4) y
C21 H21a . 0.97 ?
C21 H21b . 0.97 ?
C22 H22a . 0.96 ?
C22 H22b . 0.96 ?
C22 H22c . 0.96 ?
C23 H23a . 0.96 ?
C23 H23b . 0.96 ?
C23 H23c . 0.96 ?
C31 C32 . 1.3556(19) y
C31 C36 . 1.3881(19) y
C32 C33 . 1.3900(19) y
C32 H32 . 0.93 ?
C33 C34 . 1.3429(19) y
C33 H33 . 0.93 ?
C34 C35 . 1.3725(19) y
C34 N37 . 1.4670(17) y
C35 C36 . 1.327(2) y
C35 H35 . 0.9302 ?
C36 H36 . 0.93 ?
N37 C38 . 1.3049(18) y
N37 H37 . 0.86 ?
C38 O38 . 1.1882(18) y
C38 O39 . 1.3342(18) y
O39 C40 . 1.4523(19) y
C40 C43 . 1.503(3) y
C40 C41 . 1.523(3) y
C40 H40 . 0.98 ?
C41 C42 . 1.535(3) y
C41 H41a . 0.97 ?
C41 H41b . 0.97 ?
C42 H42a . 0.96 ?
C42 H42b . 0.96 ?
C42 H42c . 0.96 ?
C43 H43a . 0.96 ?
C43 H43b . 0.96 ?
C43 H43c . 0.96 ?
C101 C103 . 1.41(4) y
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N17 H17 O18 0.86 1.98 2.8328(17) 173.9 4_464
N37 H37 O38 0.86 2.02 2.8794(16) 174.5 8_354
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
_geom_torsion_publ_flag
C11 C1 C11 C12 6_454 -146.00(14) y
C31 C1 C11 C12 . 92.81(14) y
C31 C1 C11 C12 6_454 -24.52(18) y
C11 C1 C11 C16 6_454 35.59(9) y
C31 C1 C11 C16 . -85.60(16) y
C31 C1 C11 C16 6_454 157.07(12) y
C16 C11 C12 C13 . 2.76(19) y
C1 C11 C12 C13 . -175.73(12) y
C11 C12 C13 C14 . -3.0(2) y
C12 C13 C14 N17 . -176.23(13) y
C12 C13 C14 C15 . 2.4(2) y
N17 C14 C15 C16 . 176.83(13) y
C13 C14 C15 C16 . -2.0(2) y
C14 C15 C16 C11 . 1.9(2) y
C12 C11 C16 C15 . -2.19(19) y
C1 C11 C16 C15 . 176.36(12) y
C13 C14 N17 C18 . -19.6(2) y
C15 C14 N17 C18 . 161.74(14) y
C14 N17 C18 O18 . 9.2(3) y
C14 N17 C18 O19 . -174.89(14) y
O18 C18 O19 C20 . -11.6(3) y
N17 C18 O19 C20 . 172.33(15) y
C18 O19 C20 C21 . 115.37(19) y
C18 O19 C20 C23 . -155.98(19) y
C23 C20 C21 C22 . -178.7(3) y
O19 C20 C21 C22 . -88.2(3) y
C11 C1 C31 C32 6_454 79.98(17) y
C11 C1 C31 C32 . -156.10(13) y
C31 C1 C31 C32 6_454 -38.22(10) y
C11 C1 C31 C36 6_454 -95.54(14) y
C11 C1 C31 C36 . 28.39(18) y
C31 C1 C31 C36 6_454 146.26(14) y
C36 C31 C32 C33 . 0.1(2) y
C1 C31 C32 C33 . -175.70(12) y
C31 C32 C33 C34 . 1.6(2) y
C32 C33 C34 C35 . -2.6(2) y
C32 C33 C34 N37 . 178.36(12) y
C33 C34 C35 C36 . 1.9(2) y
N37 C34 C35 C36 . -179.08(13) y
C34 C35 C36 C31 . -0.2(2) y
C32 C31 C36 C35 . -0.8(2) y
C1 C31 C36 C35 . 175.01(13) y
C33 C34 N37 C38 . -164.76(15) y
C35 C34 N37 C38 . 16.2(2) y
C34 N37 C38 O38 . -1.2(3) y
C34 N37 C38 O39 . 176.31(13) y
O38 C38 O39 C40 . 11.8(2) y
N37 C38 O39 C40 . -165.79(13) y
C38 O39 C40 C43 . -81.4(2) y
C38 O39 C40 C41 . 153.05(14) y
O39 C40 C41 C42 . -60.8(2) y
C43 C40 C41 C42 . 175.86(19) y
|
1501614.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/16/1501614.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_1501614
loop_
_publ_author_name
'Dominic Lalibert\'e'
'Thierry Maris'
'James D. Wuest'
_publ_section_title
;
Molecular tectonics - Use of urethanes and ureas derived from
tetraphenylmethane and tetraphenylsilane to build porous chiral
hydrogenbonded networks
;
_journal_name_full 'Can. J. Chem.'
_journal_page_first 386
_journal_page_last 398
_journal_paper_doi 10.1139/v03-208
_journal_volume 82
_journal_year 2004
_chemical_compound_source 'Synthesized by the authors. See text'
_chemical_formula_sum 'C53 H80 N8 O16 y'
_chemical_formula_weight 1174.15
_chemical_name_systematic
;
?
;
_space_group_IT_number 114
_symmetry_cell_setting tetragonal
_symmetry_space_group_name_Hall 'P -4 2n'
_symmetry_space_group_name_H-M 'P -4 21 c'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 17.281(2)
_cell_length_b 17.281(2)
_cell_length_c 20.591(2)
_cell_measurement_reflns_used 4821
_cell_measurement_temperature 223(2)
_cell_measurement_theta_max 47.60
_cell_measurement_theta_min 3.62
_cell_volume 6149.2(12)
_computing_cell_refinement 'SMART (Bruker, 1999)'
_computing_data_collection 'SAINT (Bruker, 1999)'
_computing_data_reduction 'SAINT (Bruker, 1999)'
_computing_molecular_graphics 'XP (Bruker, 1999)'
_computing_publication_material 'UdMX (local program)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 223(2)
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type 'Bruker AXS Smart 2K/Platform'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'Sealed Tube'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.022
_diffrn_reflns_av_sigmaI/netI 0.0380
_diffrn_reflns_limit_h_max 19
_diffrn_reflns_limit_h_min -19
_diffrn_reflns_limit_k_max 19
_diffrn_reflns_limit_k_min -19
_diffrn_reflns_limit_l_max 21
_diffrn_reflns_limit_l_min -23
_diffrn_reflns_number 31830
_diffrn_reflns_theta_full 61.88
_diffrn_reflns_theta_max 61.88
_diffrn_reflns_theta_min 3.34
_diffrn_standards_decay_% -5.91
_diffrn_standards_number 12
_exptl_absorpt_coefficient_mu 1.366
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_correction_T_min 0.7900
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Sadabs (Sheldrick,1996)'
_exptl_crystal_colour Colourless
_exptl_crystal_density_diffrn 1.242
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 2456
_exptl_crystal_size_max 0.20
_exptl_crystal_size_mid 0.15
_exptl_crystal_size_min 0.12
_refine_diff_density_max 0.310
_refine_diff_density_min -0.227
_refine_diff_density_rms 0.065
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack 0.14(10)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.249
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 347
_refine_ls_number_reflns 4715
_refine_ls_number_restraints 105
_refine_ls_restrained_S_all 1.280
_refine_ls_R_factor_all 0.1589
_refine_ls_R_factor_gt 0.0989
_refine_ls_shift/su_max 0.149
_refine_ls_shift/su_mean 0.032
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1200P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2505
_refine_ls_wR_factor_ref 0.2721
_reflns_number_gt 2226
_reflns_number_total 4715
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file deposit.cif
_cod_data_source_block jiw642
_cod_original_cell_volume 6148.8(12)
_cod_original_sg_symbol_H-M P-421c
_cod_database_code 1501614
loop_
_symmetry_equiv_pos_as_xyz
'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'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 1.0000 0.0000 0.0000 0.091(3) Uani 1 4 d S . .
C2 C 1.0290(3) 0.0646(3) 0.0463(3) 0.0864(16) Uani 1 1 d . . .
C3 C 1.1060(3) 0.0914(4) 0.0480(4) 0.101(2) Uani 1 1 d . . .
H3 H 1.1419 0.0722 0.0178 0.121 Uiso 1 1 calc . . .
C4 C 1.1291(3) 0.1449(4) 0.0928(4) 0.0971(19) Uani 1 1 d . . .
H4 H 1.1805 0.1625 0.0918 0.117 Uiso 1 1 calc . . .
C5 C 1.0806(3) 0.1735(4) 0.1388(4) 0.0951(18) Uani 1 1 d . . .
C6 C 1.0031(3) 0.1482(4) 0.1381(3) 0.0969(17) Uani 1 1 d . . .
H6 H 0.9678 0.1680 0.1685 0.116 Uiso 1 1 calc . . .
C7 C 0.9793(3) 0.0951(3) 0.0935(3) 0.0896(17) Uani 1 1 d . . .
H7 H 0.9275 0.0783 0.0945 0.108 Uiso 1 1 calc . . .
C8 C 1.1713(4) 0.2520(4) 0.2049(4) 0.115(2) Uani 1 1 d . . .
N8 N 1.0987(3) 0.2271(3) 0.1877(3) 0.1032(16) Uani 1 1 d . . .
H8 H 1.0600 0.2464 0.2094 0.124 Uiso 1 1 calc . . .
N9 N 1.1702(3) 0.3025(4) 0.2547(3) 0.132(2) Uani 1 1 d . . .
H9A H 1.2133 0.3213 0.2697 0.159 Uiso 1 1 calc . . .
H9B H 1.1263 0.3164 0.2718 0.159 Uiso 1 1 calc . . .
O9 O 1.2303(2) 0.2299(3) 0.1785(3) 0.1349(18) Uani 1 1 d . . .
C10 C 1.0000 0.0000 0.5000 0.123(5) Uani 1 4 d S . .
C11 C 0.9694(3) 0.0627(3) 0.4532(4) 0.101(2) Uani 1 1 d . . .
C12 C 1.0193(3) 0.1034(4) 0.4146(4) 0.106(2) Uani 1 1 d . . .
H12 H 1.0724 0.0923 0.4179 0.127 Uiso 1 1 calc . . .
C13 C 0.9966(3) 0.1595(4) 0.3714(3) 0.0994(18) Uani 1 1 d . . .
H13 H 1.0338 0.1848 0.3457 0.119 Uiso 1 1 calc . . .
C14 C 0.9204(4) 0.1787(3) 0.3656(4) 0.0993(19) Uani 1 1 d . . .
C15 C 0.8665(3) 0.1359(4) 0.4038(4) 0.103(2) Uani 1 1 d . . .
H15 H 0.8133 0.1466 0.4007 0.123 Uiso 1 1 calc . . .
C16 C 0.8915(3) 0.0807(4) 0.4438(4) 0.112(2) Uani 1 1 d . . .
H16 H 0.8545 0.0522 0.4671 0.135 Uiso 1 1 calc . . .
C17 C 0.9251(4) 0.2875(4) 0.2875(3) 0.1005(19) Uani 1 1 d . . .
N18 N 0.8881(3) 0.2346(3) 0.3248(3) 0.1061(17) Uani 1 1 d . . .
H18 H 0.8378 0.2355 0.3230 0.127 Uiso 1 1 calc . . .
N19 N 0.8807(3) 0.3352(4) 0.2557(4) 0.155(3) Uani 1 1 d . . .
H19A H 0.9010 0.3696 0.2300 0.186 Uiso 1 1 calc . . .
H19B H 0.8307 0.3326 0.2601 0.186 Uiso 1 1 calc . . .
O19 O 0.9966(2) 0.2903(3) 0.2819(2) 0.1161(14) Uani 1 1 d . . .
y0A S 1.3040(4) 0.4605(5) 0.2445(5) 0.219(2) Uani 0.547(6) 1 d PU . 1
O20 O 1.3132(4) 0.3885(5) 0.2900(4) 0.199(3) Uani 1 1 d U A 1
C21 C 1.1077(7) 0.0060(6) 0.2600(5) 0.215(5) Uani 1 1 d U . 1
H21A H 1.1100 0.0469 0.2922 0.322 Uiso 1 1 calc R . 1
H21B H 1.0683 -0.0312 0.2723 0.322 Uiso 1 1 calc R . 1
H21C H 1.0950 0.0279 0.2180 0.322 Uiso 1 1 calc R . 1
C22 C 0.7641(10) -0.0373(9) 0.2243(8) 0.283(7) Uani 1 1 d U . 1
H22A H 0.7385 -0.0666 0.2582 0.424 Uiso 1 1 calc R . 1
H22B H 0.8036 -0.0691 0.2041 0.424 Uiso 1 1 calc R . 1
H22C H 0.7264 -0.0218 0.1919 0.424 Uiso 1 1 calc R . 1
y0B S 0.8247(5) 0.0360(6) 0.2027(6) 0.219(2) Uani 0.453(6) 1 d P . 2
O50 O 0.9331(11) 0.5392(12) 0.1856(11) 0.247(7) Uiso 0.50 1 d PD B 1
C51 C 0.963(2) 0.5912(14) 0.1399(18) 0.303(17) Uiso 0.50 1 d PD . 1
H51A H 0.9546 0.6463 0.1486 0.364 Uiso 0.50 1 calc PR . 1
H51B H 0.9566 0.5773 0.0941 0.364 Uiso 0.50 1 calc PR . 1
C52 C 0.9472(13) 0.4595(12) 0.1876(14) 0.182(8) Uiso 0.50 1 d PD . 1
H52A H 0.8999 0.4341 0.1721 0.218 Uiso 0.50 1 calc PR . 1
H52B H 0.9526 0.4455 0.2335 0.218 Uiso 0.50 1 calc PR . 1
O50' O 0.9456(15) 0.4963(19) 0.1308(13) 0.296(10) Uiso 0.50 1 d P . 2
C51' C 1.0396(13) 0.5663(13) 0.1448(12) 0.161(6) Uiso 0.50 1 d P . 2
C52' C 1.0422(18) 0.4860(19) 0.2410(14) 0.245(12) Uiso 0.50 1 d P . 2
C30 C 0.275(2) 0.2325(14) 0.3852(15) 0.246(16) Uiso 0.42(3) 1 d PD C 3
H30A H 0.2300 0.2652 0.3932 0.296 Uiso 0.33 1 calc PR C 3
H30B H 0.3009 0.2523 0.3461 0.296 Uiso 0.33 1 calc PR C 3
C31 C 0.3263(19) 0.2411(17) 0.4375(15) 0.201(13) Uiso 0.42(3) 1 d PD C 3
H31A H 0.3786 0.2312 0.4210 0.242 Uiso 0.33 1 calc PR C 3
H31B H 0.3247 0.2956 0.4506 0.242 Uiso 0.33 1 calc PR C 3
C32 C 0.317(2) 0.197(2) 0.4938(13) 0.25(2) Uiso 0.42(3) 1 d PD C 3
H32A H 0.2765 0.2184 0.5215 0.295 Uiso 0.33 1 calc PR C 3
H32B H 0.3657 0.1952 0.5187 0.295 Uiso 0.33 1 calc PR C 3
C33 C 0.297(2) 0.123(2) 0.472(2) 0.83(16) Uiso 0.42(3) 1 d PD C 3
H33A H 0.2871 0.0877 0.5078 0.995 Uiso 0.33 1 calc PR C 3
H33B H 0.3378 0.1012 0.4439 0.995 Uiso 0.33 1 calc PR C 3
C34 C 0.2298(13) 0.1380(16) 0.4361(10) 0.160(11) Uiso 0.42(3) 1 d PD C 3
H34A H 0.1965 0.0921 0.4362 0.192 Uiso 0.33 1 calc PR C 3
H34B H 0.2011 0.1807 0.4561 0.192 Uiso 0.33 1 calc PR C 3
C35 C 0.2498(15) 0.1573(15) 0.3725(9) 0.161(11) Uiso 0.42(3) 1 d PD C 3
H35A H 0.2052 0.1563 0.3431 0.193 Uiso 0.33 1 calc PR C 3
H35B H 0.2911 0.1242 0.3553 0.193 Uiso 0.33 1 calc PR C 3
C30' C 0.2402(10) 0.1881(11) 0.4004(9) 0.151(8) Uiso 0.58(3) 1 d PD C 4
H30C H 0.2011 0.2009 0.4332 0.181 Uiso 0.33 1 calc PR C 4
H30D H 0.2208 0.2032 0.3575 0.181 Uiso 0.33 1 calc PR C 4
C31' C 0.312(2) 0.225(2) 0.414(2) 0.38(3) Uiso 0.58(3) 1 d PD C 4
H31C H 0.3485 0.2121 0.3794 0.461 Uiso 0.33 1 calc PR C 4
H31D H 0.3041 0.2811 0.4129 0.461 Uiso 0.33 1 calc PR C 4
C32' C 0.3473(16) 0.2083(14) 0.4715(15) 0.217(11) Uiso 0.58(3) 1 d PD C 4
H32C H 0.3241 0.2398 0.5059 0.260 Uiso 0.33 1 calc PR C 4
H32D H 0.4022 0.2222 0.4686 0.260 Uiso 0.33 1 calc PR C 4
C33' C 0.3413(15) 0.1317(16) 0.4881(12) 0.260(13) Uiso 0.58(3) 1 d PD C 4
H33C H 0.3411 0.1275 0.5355 0.312 Uiso 0.33 1 calc PR C 4
H33D H 0.3873 0.1045 0.4722 0.312 Uiso 0.33 1 calc PR C 4
C34' C 0.2758(13) 0.0944(13) 0.4640(10) 0.200(10) Uiso 0.58(3) 1 d PD C 4
H34C H 0.2831 0.0385 0.4687 0.240 Uiso 0.33 1 calc PR C 4
H34D H 0.2314 0.1091 0.4908 0.240 Uiso 0.33 1 calc PR C 4
C35' C 0.2589(13) 0.1095(11) 0.4022(11) 0.195(10) Uiso 0.58(3) 1 d PD C 4
H35C H 0.2151 0.0780 0.3877 0.234 Uiso 0.33 1 calc PR C 4
H35D H 0.3035 0.0986 0.3742 0.234 Uiso 0.33 1 calc PR C 4
C40 C 1.1310(18) 0.3572(18) 0.0179(17) 0.240(12) Uiso 0.481(15) 1 d PD D 5
H40A H 1.1805 0.3456 -0.0031 0.288 Uiso 0.481(15) 1 calc PR D 5
H40B H 1.1369 0.3491 0.0647 0.288 Uiso 0.481(15) 1 calc PR D 5
C41 C 1.0743(19) 0.3089(15) -0.0061(15) 0.241(13) Uiso 0.481(15) 1 d PD D 5
H41A H 1.1004 0.2591 -0.0117 0.289 Uiso 0.481(15) 1 calc PR D 5
H41B H 1.0388 0.3018 0.0306 0.289 Uiso 0.481(15) 1 calc PR D 5
C42 C 1.028(2) 0.3146(18) -0.0579(16) 0.276(16) Uiso 0.481(15) 1 d PD D 5
H42A H 0.9737 0.3054 -0.0456 0.331 Uiso 0.481(15) 1 calc PR D 5
H42B H 1.0425 0.2769 -0.0912 0.331 Uiso 0.481(15) 1 calc PR D 5
C43 C 1.038(3) 0.391(2) -0.0811(17) 0.36(2) Uiso 0.481(15) 1 d PD D 5
H43A H 1.0859 0.3974 -0.1055 0.437 Uiso 0.481(15) 1 calc PR D 5
H43B H 0.9938 0.4083 -0.1077 0.437 Uiso 0.481(15) 1 calc PR D 5
C44 C 1.040(2) 0.4286(17) -0.0215(18) 0.285(17) Uiso 0.481(15) 1 d PD D 5
H44A H 1.0192 0.4810 -0.0270 0.342 Uiso 0.481(15) 1 calc PR D 5
H44B H 1.0057 0.4011 0.0087 0.342 Uiso 0.481(15) 1 calc PR D 5
C45 C 1.110(3) 0.4340(18) 0.006(3) 0.48(5) Uiso 0.481(15) 1 d PD D 5
H45A H 1.1085 0.4639 0.0462 0.572 Uiso 0.481(15) 1 calc PR D 5
H45B H 1.1473 0.4586 -0.0239 0.572 Uiso 0.481(15) 1 calc PR D 5
C40' C 1.173(3) 0.343(2) -0.0230(19) 0.33(2) Uiso 0.519(15) 1 d PD D 6
H40C H 1.1664 0.3097 0.0154 0.402 Uiso 0.519(15) 1 calc PR D 6
H40D H 1.2234 0.3301 -0.0425 0.402 Uiso 0.519(15) 1 calc PR D 6
C41' C 1.115(3) 0.3269(17) -0.0675(19) 0.34(2) Uiso 0.519(15) 1 d PD D 6
H41C H 1.1280 0.2770 -0.0873 0.404 Uiso 0.519(15) 1 calc PR D 6
H41D H 1.0678 0.3180 -0.0419 0.404 Uiso 0.519(15) 1 calc PR D 6
C42' C 1.0936(17) 0.3738(16) -0.1171(13) 0.231(12) Uiso 0.519(15) 1 d PD D 6
H42C H 1.0463 0.3553 -0.1384 0.277 Uiso 0.519(15) 1 calc PR D 6
H42D H 1.1349 0.3785 -0.1495 0.277 Uiso 0.519(15) 1 calc PR D 6
C43' C 1.0809(18) 0.4443(16) -0.0847(16) 0.271(15) Uiso 0.519(15) 1 d PD D 6
H43C H 1.0654 0.4854 -0.1148 0.325 Uiso 0.519(15) 1 calc PR D 6
H43D H 1.0420 0.4392 -0.0504 0.325 Uiso 0.519(15) 1 calc PR D 6
C44' C 1.1538(19) 0.4570(15) -0.0597(16) 0.290(17) Uiso 0.519(15) 1 d PD D 6
H44C H 1.1917 0.4430 -0.0931 0.348 Uiso 0.519(15) 1 calc PR D 6
H44D H 1.1593 0.5126 -0.0516 0.348 Uiso 0.519(15) 1 calc PR D 6
C45' C 1.173(3) 0.419(2) -0.0043(16) 0.33(2) Uiso 0.519(15) 1 d PD D 6
H45C H 1.1346 0.4283 0.0299 0.401 Uiso 0.519(15) 1 calc PR D 6
H45D H 1.2241 0.4351 0.0114 0.401 Uiso 0.519(15) 1 calc PR D 6
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 0.078(4) 0.078(4) 0.118(9) 0.000 0.000 0.000
C2 0.075(4) 0.074(4) 0.110(4) 0.004(3) -0.013(4) 0.009(3)
C3 0.051(3) 0.106(4) 0.146(5) 0.011(4) 0.019(4) 0.002(3)
C4 0.054(3) 0.094(4) 0.144(5) -0.028(4) -0.006(4) -0.017(3)
C5 0.050(3) 0.091(4) 0.145(5) -0.021(4) 0.006(4) -0.011(3)
C6 0.061(3) 0.104(4) 0.126(5) -0.019(4) 0.007(4) 0.006(3)
C7 0.063(3) 0.085(4) 0.120(5) -0.007(4) 0.006(4) -0.006(3)
C8 0.064(4) 0.118(5) 0.162(7) -0.017(5) -0.005(5) -0.014(4)
N8 0.059(3) 0.100(4) 0.150(4) -0.014(4) 0.011(3) -0.010(2)
N9 0.074(3) 0.172(5) 0.151(5) -0.058(5) -0.015(3) -0.009(3)
O9 0.059(2) 0.150(4) 0.195(5) -0.060(4) 0.020(3) -0.010(3)
C10 0.062(4) 0.062(4) 0.243(16) 0.000 0.000 0.000
C11 0.049(3) 0.073(4) 0.182(6) -0.001(4) 0.008(4) 0.001(3)
C12 0.047(3) 0.093(4) 0.179(6) -0.012(5) 0.002(4) 0.011(3)
C13 0.060(4) 0.082(4) 0.156(5) 0.009(4) 0.008(4) 0.014(3)
C14 0.069(4) 0.077(4) 0.152(6) -0.008(4) -0.009(4) 0.000(3)
C15 0.062(3) 0.093(4) 0.154(6) -0.002(5) 0.010(4) -0.008(3)
C16 0.069(4) 0.074(4) 0.193(7) 0.031(4) 0.014(4) 0.001(3)
C17 0.070(4) 0.110(5) 0.121(5) -0.019(4) 0.009(4) 0.016(4)
N18 0.056(3) 0.097(3) 0.165(5) 0.025(4) 0.010(3) 0.003(3)
N19 0.066(3) 0.158(5) 0.242(8) 0.076(6) 0.002(4) 0.011(4)
O19 0.067(3) 0.138(3) 0.143(3) -0.004(3) 0.016(3) -0.015(2)
y0A 0.209(3) 0.208(3) 0.241(5) 0.003(4) 0.003(3) -0.017(3)
O20 0.192(4) 0.183(4) 0.222(5) -0.004(4) -0.012(4) -0.008(4)
C21 0.205(6) 0.218(6) 0.221(6) 0.005(5) 0.010(5) 0.019(5)
C22 0.272(8) 0.282(8) 0.295(8) -0.003(5) 0.015(5) -0.014(5)
y0B 0.209(3) 0.208(3) 0.241(5) 0.003(4) 0.003(3) -0.017(3)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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
C2 C1 C2 . 4_645 112.2(2) y
C2 C1 C2 . 2_755 104.1(4) y
C2 C1 C2 4_645 2_755 112.2(2) y
C2 C1 C2 . 3_665 112.2(2) y
C2 C1 C2 4_645 3_665 104.1(4) y
C2 C1 C2 2_755 3_665 112.2(2) y
C7 C2 C3 . . 116.0(5) y
C7 C2 C1 . . 120.0(5) y
C3 C2 C1 . . 123.8(6) y
C4 C3 C2 . . 121.0(6) y
C4 C3 H3 . . 119.5 ?
C2 C3 H3 . . 119.5 ?
C5 C4 C3 . . 122.5(5) y
C5 C4 H4 . . 118.8 ?
C3 C4 H4 . . 118.7 ?
C4 C5 N8 . . 127.2(5) y
C4 C5 C6 . . 117.8(6) y
N8 C5 C6 . . 115.0(6) y
C7 C6 C5 . . 120.3(6) y
C7 C6 H6 . . 119.9 ?
C5 C6 H6 . . 119.9 ?
C6 C7 C2 . . 122.4(5) y
C6 C7 H7 . . 118.8 ?
C2 C7 H7 . . 118.8 ?
O9 C8 N9 . . 123.8(6) y
O9 C8 N8 . . 123.5(8) y
N9 C8 N8 . . 112.7(7) y
C8 N8 C5 . . 126.5(6) y
C8 N8 H8 . . 116.8 ?
C5 N8 H8 . . 116.7 ?
C8 N9 H9A . . 120 ?
C8 N9 H9B . . 120 ?
H9A N9 H9B . . 120 ?
C11 C10 C11 4_646 3_666 102.7(5) y
C11 C10 C11 4_646 . 113.0(3) y
C11 C10 C11 3_666 . 113.0(3) y
C11 C10 C11 4_646 2_755 113.0(3) y
C11 C10 C11 3_666 2_755 113.0(3) y
C11 C10 C11 . 2_755 102.7(5) y
C12 C11 C16 . . 114.3(6) y
C12 C11 C10 . . 120.6(5) y
C16 C11 C10 . . 125.0(6) y
C11 C12 C13 . . 124.1(5) y
C11 C12 H12 . . 118 ?
C13 C12 H12 . . 118 ?
C14 C13 C12 . . 120.3(6) y
C14 C13 H13 . . 119.8 ?
C12 C13 H13 . . 119.9 ?
C13 C14 N18 . . 127.3(6) y
C13 C14 C15 . . 117.2(6) y
N18 C14 C15 . . 115.5(5) y
C16 C15 C14 . . 120.0(6) y
C16 C15 H15 . . 120 ?
C14 C15 H15 . . 120 ?
C15 C16 C11 . . 124.0(6) y
C15 C16 H16 . . 118 ?
C11 C16 H16 . . 118 ?
O19 C17 N19 . . 121.0(7) y
O19 C17 N18 . . 123.3(7) y
N19 C17 N18 . . 115.7(6) y
C17 N18 C14 . . 128.3(5) y
C17 N18 H18 . . 115.8 ?
C14 N18 H18 . . 115.8 ?
C17 N19 H19A . . 120 ?
C17 N19 H19B . . 120 ?
H19A N19 H19B . . 120 ?
O20 y0A C22 . 6 117.0(8) y
O20 y0A C21 . 5_755 107.8(7) y
C22 y0A C21 6 5_755 91.4(8) y
y0A C21 H21A 5_745 . 109.5 ?
y0A C21 H21B 5_745 . 109.5 ?
H21A C21 H21B . . 109.5 ?
y0A C21 H21C 5_745 . 109.5 ?
H21A C21 H21C . . 109.5 ?
H21B C21 H21C . . 109.5 ?
y0A C22 H22A 6_455 . 109.5 ?
y0A C22 H22B 6_455 . 109.5 ?
H22A C22 H22B . . 109.5 ?
y0A C22 H22C 6_455 . 109.4 ?
H22A C22 H22C . . 109.5 ?
H22B C22 H22C . . 109.5 ?
C52 O50 C51 . . 125.9(7) y
O50 C51 C52 . 2_765 71.40(16) y
O50 C51 H51A . . 116.3 ?
C52 C51 H51A 2_765 . 116.4 ?
O50 C51 H51B . . 116.5 ?
C52 C51 H51B 2_765 . 116.5 ?
H51A C51 H51B . . 113.4 ?
O50 C52 C51 . 2_765 123(2) y
O50 C52 H52A . . 106.5 ?
C51 C52 H52A 2_765 . 106.5 ?
O50 C52 H52B . . 106.8 ?
C51 C52 H52B 2_765 . 106.7 ?
H52A C52 H52B . . 106.5 ?
C35 C30 C31 . . 116(2) y
C35 C30 H30A . . 108.3 ?
C31 C30 H30A . . 108.4 ?
C35 C30 H30B . . 108.1 ?
C31 C30 H30B . . 108.1 ?
H30A C30 H30B . . 107.4 ?
C32 C31 C30 . . 121(2) y
C32 C31 H31A . . 107.1 ?
C30 C31 H31A . . 107.3 ?
C32 C31 H31B . . 107.1 ?
C30 C31 H31B . . 107 ?
H31A C31 H31B . . 106.8 ?
C31 C32 C33 . . 105(2) y
C31 C32 H32A . . 110.8 ?
C33 C32 H32A . . 110.9 ?
C31 C32 H32B . . 110.8 ?
C33 C32 H32B . . 110.8 ?
H32A C32 H32B . . 108.9 ?
C32 C33 C34 . . 102(2) y
C32 C33 H33A . . 111.3 ?
C34 C33 H33A . . 111.3 ?
C32 C33 H33B . . 111.4 ?
C34 C33 H33B . . 111.4 ?
H33A C33 H33B . . 109.2 ?
C35 C34 C33 . . 109(3) y
C35 C34 H34A . . 109.9 ?
C33 C34 H34A . . 109.8 ?
C35 C34 H34B . . 109.8 ?
C33 C34 H34B . . 109.9 ?
H34A C34 H34B . . 108.3 ?
C34 C35 C30 . . 97.20(18) y
C34 C35 H35A . . 112.3 ?
C30 C35 H35A . . 112.3 ?
C34 C35 H35B . . 112.2 ?
C30 C35 H35B . . 112.4 ?
H35A C35 H35B . . 109.9 ?
C35' C30' C31' . . 103.00(19) y
C35' C30' H30C . . 111.2 ?
C31' C30' H30C . . 111.1 ?
C35' C30' H30D . . 111.2 ?
C31' C30' H30D . . 111.1 ?
H30C C30' H30D . . 109.1 ?
C32' C31' C30' . . 118(2) y
C32' C31' H31C . . 107.8 ?
C30' C31' H31C . . 107.8 ?
C32' C31' H31D . . 107.8 ?
C30' C31' H31D . . 107.8 ?
H31C C31' H31D . . 107.1 ?
C31' C32' C33' . . 113(2) y
C31' C32' H32C . . 109.1 ?
C33' C32' H32C . . 109 ?
C31' C32' H32D . . 109 ?
C33' C32' H32D . . 109 ?
H32C C32' H32D . . 107.8 ?
C32' C33' C34' . . 115(2) y
C32' C33' H33C . . 108.6 ?
C34' C33' H33C . . 108.6 ?
C32' C33' H33D . . 108.6 ?
C34' C33' H33D . . 108.5 ?
H33C C33' H33D . . 107.5 ?
C35' C34' C33' . . 115.40(19) y
C35' C34' H34C . . 108.4 ?
C33' C34' H34C . . 108.4 ?
C35' C34' H34D . . 108.5 ?
C33' C34' H34D . . 108.4 ?
H34C C34' H34D . . 107.5 ?
C34' C35' C30' . . 105.40(17) y
C34' C35' H35C . . 110.6 ?
C30' C35' H35C . . 110.6 ?
C34' C35' H35D . . 110.7 ?
C30' C35' H35D . . 110.7 ?
H35C C35' H35D . . 108.8 ?
C41 C40 C45 . . 109(2) y
C41 C40 H40A . . 109.7 ?
C45 C40 H40A . . 109.9 ?
C41 C40 H40B . . 109.8 ?
C45 C40 H40B . . 109.8 ?
H40A C40 H40B . . 108.3 ?
C42 C41 C40 . . 132(2) y
C42 C41 H41A . . 104.3 ?
C40 C41 H41A . . 104.4 ?
C42 C41 H41B . . 104.2 ?
C40 C41 H41B . . 104.2 ?
H41A C41 H41B . . 105.6 ?
C41 C42 C43 . . 105(2) y
C41 C42 H42A . . 110.7 ?
C43 C42 H42A . . 110.6 ?
C41 C42 H42B . . 110.7 ?
C43 C42 H42B . . 110.7 ?
H42A C42 H42B . . 108.8 ?
C44 C43 C42 . . 98(2) y
C44 C43 H43A . . 112.2 ?
C42 C43 H43A . . 112.1 ?
C44 C43 H43B . . 112.1 ?
C42 C43 H43B . . 112.2 ?
H43A C43 H43B . . 109.8 ?
C45 C44 C43 . . 115(3) y
C45 C44 H44A . . 108.4 ?
C43 C44 H44A . . 108.5 ?
C45 C44 H44B . . 108.4 ?
C43 C44 H44B . . 108.5 ?
H44A C44 H44B . . 107.5 ?
C44 C45 C40 . . 104(2) y
C44 C45 H45A . . 111.1 ?
C40 C45 H45A . . 111 ?
C44 C45 H45B . . 110.9 ?
C40 C45 H45B . . 110.9 ?
H45A C45 H45B . . 109 ?
C45' C40' C41' . . 112(2) y
C45' C40' H40C . . 109.4 ?
C41' C40' H40C . . 109.4 ?
C45' C40' H40D . . 109.1 ?
C41' C40' H40D . . 109.2 ?
H40C C40' H40D . . 108 ?
C42' C41' C40' . . 125(3) y
C42' C41' H41C . . 106 ?
C40' C41' H41C . . 106 ?
C42' C41' H41D . . 106.2 ?
C40' C41' H41D . . 105.9 ?
H41C C41' H41D . . 106.3 ?
C41' C42' C43' . . 102(2) y
C41' C42' H42C . . 111.3 ?
C43' C42' H42C . . 111.4 ?
C41' C42' H42D . . 111.6 ?
C43' C42' H42D . . 111.4 ?
H42C C42' H42D . . 109.3 ?
C44' C43' C42' . . 100(2) y
C44' C43' H43C . . 111.8 ?
C42' C43' H43C . . 111.8 ?
C44' C43' H43D . . 111.7 ?
C42' C43' H43D . . 111.8 ?
H43C C43' H43D . . 109.5 ?
C45' C44' C43' . . 117(3) y
C45' C44' H44C . . 107.9 ?
C43' C44' H44C . . 107.9 ?
C45' C44' H44D . . 108 ?
C43' C44' H44D . . 107.9 ?
H44C C44' H44D . . 107.2 ?
C44' C45' C40' . . 103(2) y
C44' C45' H45C . . 111.1 ?
C40' C45' H45C . . 111 ?
C44' C45' H45D . . 111.1 ?
C40' C45' H45D . . 111.3 ?
H45C C45' H45D . . 109.1 ?
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
C1 C2 . 1.551(6) y
C1 C2 4_645 1.551(6) y
C1 C2 2_755 1.551(6) y
C1 C2 3_665 1.551(6) y
C2 C7 . 1.400(7) y
C2 C3 . 1.409(8) y
C3 C4 . 1.366(8) y
C3 H3 . 0.9397 ?
C4 C5 . 1.357(8) y
C4 H4 . 0.9401 ?
C5 N8 . 1.404(7) y
C5 C6 . 1.409(8) y
C6 C7 . 1.361(8) y
C6 H6 . 0.9399 ?
C7 H7 . 0.9398 ?
C8 O9 . 1.218(8) y
C8 N9 . 1.346(9) y
C8 N8 . 1.374(8) y
N8 H8 . 0.8698 ?
N9 H9a . 0.8698 ?
N9 H9b . 0.8701 ?
C10 C11 4_646 1.543(6) y
C10 C11 3_666 1.543(6) y
C10 C11 . 1.543(6) y
C10 C11 2_755 1.543(6) y
C11 C12 . 1.367(8) y
C11 C16 . 1.395(8) y
C12 C13 . 1.373(9) y
C12 H12 . 0.9402 ?
C13 C14 . 1.363(8) y
C13 H13 . 0.9402 ?
C14 N18 . 1.397(8) y
C14 C15 . 1.426(8) y
C15 C16 . 1.332(8) y
C15 H15 . 0.9402 ?
C16 H16 . 0.9402 ?
C17 O19 . 1.243(7) y
C17 N19 . 1.303(8) y
C17 N18 . 1.354(8) y
N18 H18 . 0.87 ?
N19 H19a . 0.8698 ?
N19 H19b . 0.8701 ?
y0a O20 . 1.567(11) y
y0a C22 6 1.628(16) y
y0a C21 5_755 1.718(12) y
C21 y0a 5_745 1.718(12) y
C21 H21a . 0.97 ?
C21 H21b . 0.97 ?
C21 H21c . 0.97 ?
C22 y0a 6_455 1.628(16) y
C22 H22a . 0.97 ?
C22 H22b . 0.97 ?
C22 H22c . 0.97 ?
O50 C52 . 1.399(5) y
O50 C51 . 1.403(5) y
C51 C52 2_765 2.03(4) y
C51 H51a . 0.98 ?
C51 H51b . 0.98 ?
C52 C51 2_765 2.03(4) y
C52 H52a . 0.98 ?
C52 H52b . 0.98 ?
O50' C51' 2_765 1.15(3) y
C51' O50' 2_765 1.15(3) y
C52' C52' 2_765 1.54(6) y
C30 C35 . 1.399(5) y
C30 C31 . 1.399(5) y
C30 H30a . 0.98 ?
C30 H30b . 0.98 ?
C31 C32 . 1.397(5) y
C31 H31a . 0.98 ?
C31 H31b . 0.98 ?
C32 C33 . 1.400(5) y
C32 H32a . 0.98 ?
C32 H32b . 0.98 ?
C33 C34 . 1.400(5) y
C33 H33a . 0.98 ?
C33 H33b . 0.98 ?
C34 C35 . 1.396(5) y
C34 H34a . 0.98 ?
C34 H34b . 0.98 ?
C35 H35a . 0.98 ?
C35 H35b . 0.98 ?
C30' C35' . 1.398(16) y
C30' C31' . 1.431(19) y
C30' H30c . 0.98 ?
C30' H30d . 0.98 ?
C31' C32' . 1.353(18) y
C31' H31c . 0.98 ?
C31' H31d . 0.98 ?
C32' C33' . 1.371(18) y
C32' H32c . 0.98 ?
C32' H32d . 0.98 ?
C33' C34' . 1.393(18) y
C33' H33c . 0.98 ?
C33' H33d . 0.98 ?
C34' C35' . 1.330(16) y
C34' H34c . 0.98 ?
C34' H34d . 0.98 ?
C35' H35c . 0.98 ?
C35' H35d . 0.98 ?
C40 C41 . 1.378(17) y
C40 C45 . 1.396(19) y
C40 H40a . 0.98 ?
C40 H40b . 0.98 ?
C41 C42 . 1.340(18) y
C41 H41a . 0.98 ?
C41 H41b . 0.98 ?
C42 C43 . 1.418(19) y
C42 H42a . 0.98 ?
C42 H42b . 0.98 ?
C43 C44 . 1.389(19) y
C43 H43a . 0.98 ?
C43 H43b . 0.98 ?
C44 C45 . 1.346(19) y
C44 H44a . 0.98 ?
C44 H44b . 0.98 ?
C45 H45a . 0.98 ?
C45 H45b . 0.98 ?
C40' C45' . 1.376(19) y
C40' C41' . 1.392(18) y
C40' H40c . 0.98 ?
C40' H40d . 0.98 ?
C41' C42' . 1.355(19) y
C41' H41c . 0.98 ?
C41' H41d . 0.98 ?
C42' C43' . 1.406(18) y
C42' H42c . 0.98 ?
C42' H42d . 0.98 ?
C43' C44' . 1.378(18) y
C43' H43c . 0.98 ?
C43' H43d . 0.98 ?
C44' C45' . 1.357(18) y
C44' H44c . 0.98 ?
C44' H44d . 0.98 ?
C45' H45c . 0.98 ?
C45' H45d . 0.98 ?
|
1501615.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/16/1501615.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_1501615
loop_
_publ_author_name
'Fedor Valach'
'Miroslav Tokar\<c\'ik'
'Thierry Maris'
'David J. Watkin'
'Keith Prout'
_publ_section_title
;
Bond-valence approach to the copper-copper and copper-oxygen bonding in
binuclear copper(II) complexes: Structure of
tetrakis(2-fluorobenzoato-O,O')-bis (2-fluorobenzoate-O) dicopper(II)
;
_journal_issue 1
_journal_name_full
;
Zeitschrift f\"ur Kristallographie - Crystalline Materials
;
_journal_page_first 56
_journal_page_last 60
_journal_paper_doi 10.1524/zkri.2000.215.1.56
_journal_volume 215
_journal_year 2000
_chemical_formula_moiety ' C21 H13 Cu1 O6 F3 '
_chemical_formula_sum 'C21 H13 Cu F3 O6'
_chemical_formula_weight 481.86
_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 90.00(2)
_cell_angle_beta 91.62(4)
_cell_angle_gamma 90.00(3)
_cell_formula_units_Z 4
_cell_length_a 10.633(3)
_cell_length_b 12.528(3)
_cell_length_c 14.729(3)
_cell_measurement_reflns_used 25
_cell_measurement_temperature 293
_cell_measurement_theta_max 26
_cell_measurement_theta_min 5
_cell_volume 1961.3(8)
_computing_cell_refinement 'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_collection 'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_reduction
;
RC93 (Watkin, D.J., Prout, C.K., Lilley, P.M.deQ. 1994)
;
_computing_molecular_graphics
;
CAMERON (Watkin, Prout & Pearce, 1996)
;
_computing_publication_material
;
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)
;
_computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)'
_diffrn_ambient_temperature 293
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device ' Enraf-nonius CAD4 '
_diffrn_measurement_method \w/2\q
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type 'Cu K\a'
_diffrn_radiation_wavelength 1.54180
_diffrn_reflns_av_R_equivalents 0.03
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_number 4038
_diffrn_reflns_theta_max 75.00
_diffrn_reflns_theta_min 0.00
_diffrn_standards_decay_% 3.94
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_standards_number 2
_exptl_absorpt_coefficient_mu 2.14
_exptl_absorpt_correction_T_max 0.90
_exptl_absorpt_correction_T_min 0.59
_exptl_absorpt_correction_type psi-scan
_exptl_absorpt_process_details '\y scan,(North et al, 1968)'
_exptl_crystal_colour ' colourless '
_exptl_crystal_density_diffrn 1.63
_exptl_crystal_description ' block '
_exptl_crystal_F_000 967.17
_exptl_crystal_size_max 0.20
_exptl_crystal_size_mid 0.10
_exptl_crystal_size_min 0.05
_refine_diff_density_max 0.64
_refine_diff_density_min -0.48
_refine_ls_extinction_coef 62.4(62)
_refine_ls_extinction_method
'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_obs 1.0574
_refine_ls_hydrogen_treatment noref
_refine_ls_matrix_type full
_refine_ls_number_parameters 281
_refine_ls_number_reflns 3204
_refine_ls_R_factor_obs 0.0448
_refine_ls_shift/su_max 0.001140
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Chebychev polynomial with 3 parameters (Carruthers & Watkin, 1979)
3.49 1.84 2.72
;
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_obs 0.0539
_reflns_limit_h_max 13
_reflns_limit_h_min -13
_reflns_limit_k_max 15
_reflns_limit_k_min 0
_reflns_limit_l_max 18
_reflns_limit_l_min 0
_reflns_number_observed 3204
_reflns_number_total 4038
_reflns_observed_criterion >3.00\s(I)
_cod_data_source_file deposit.cif
_cod_data_source_block CRYSTALS_cif
_cod_original_cell_volume 1961.2
_cod_original_sg_symbol_H-M 'P 1 21/n 1 '
_cod_original_formula_sum ' C21 H13 Cu1 O6 F3 '
_cod_database_code 1501615
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_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 0.0335(2) 0.03139(19) 0.0369(2) -0.00485(12) 0.00474(12) 0.00202(11)
O1 0.0399(8) 0.0353(9) 0.053(1) -0.0056(7) 0.0120(7) -0.0038(7)
O2 0.0364(8) 0.0371(9) 0.0697(11) -0.0103(8) 0.0132(8) -0.0043(7)
C3 0.034(1) 0.0378(11) 0.035(1) -0.0030(8) 0.0008(8) 0.0001(9)
C4 0.034(1) 0.0401(11) 0.0398(11) -0.0007(9) 0.0032(8) -0.0027(8)
C5 0.0458(13) 0.0445(14) 0.0708(17) 0.0044(12) 0.0150(12) -0.0055(11)
C6 0.0636(19) 0.0556(18) 0.124(3) 0.0103(19) 0.036(2) -0.0136(16)
C7 0.0532(17) 0.074(2) 0.116(3) 0.010(2) 0.0374(19) -0.0126(16)
C8 0.0403(14) 0.0687(19) 0.0772(19) -0.0064(15) 0.0181(13) 0.0007(13)
C9 0.0376(12) 0.0484(13) 0.0475(12) -0.004(1) 0.0040(9) -0.001(1)
F10 0.0449(8) 0.0435(8) 0.0840(12) -0.0041(7) 0.0095(8) 0.0042(6)
O11 0.056(1) 0.0528(11) 0.0377(8) -0.0036(7) 0.0006(7) 0.0089(8)
O12 0.0631(11) 0.050(1) 0.0420(9) -0.0047(8) -0.0050(8) 0.0105(9)
C13 0.033(1) 0.0503(13) 0.0394(11) 0.001(1) 0.0062(8) 0.002(1)
C14 0.033(1) 0.0553(14) 0.0403(11) -0.000(1) 0.0026(8) 0.002(1)
C15 0.0653(17) 0.0592(16) 0.0503(15) -0.0058(13) -0.0069(12) 0.0090(14)
C16 0.102(3) 0.074(2) 0.0556(18) -0.0144(17) -0.0226(17) 0.008(2)
C17 0.103(3) 0.092(3) 0.0501(17) 0.0036(17) -0.0248(18) -0.006(2)
C18 0.109(3) 0.070(2) 0.0549(17) 0.0145(16) -0.0128(17) -0.004(2)
C19 0.0717(18) 0.0543(16) 0.0482(14) 0.0031(13) -0.0042(13) -0.0102(14)
F20 0.176(3) 0.0560(11) 0.0715(13) 0.004(1) -0.0264(15) -0.0223(14)
O21 0.050(1) 0.0346(8) 0.0696(12) -0.0118(8) 0.0178(8) -0.0022(7)
O22 0.0669(14) 0.041(1) 0.144(2) -0.0310(13) 0.0503(15) -0.013(1)
C23 0.0462(12) 0.0314(11) 0.0455(11) 0.0002(9) 0.0093(9) -0.0007(9)
C24 0.0508(13) 0.0310(11) 0.0408(11) -0.0007(9) 0.0036(9) 0.0008(9)
C25 0.0605(16) 0.0412(13) 0.0537(14) -0.0063(11) 0.0112(12) -0.0069(11)
C26 0.084(2) 0.0437(15) 0.0611(17) -0.0043(13) 0.0035(15) -0.0153(14)
C27 0.095(2) 0.0350(13) 0.0569(16) -0.0100(12) -0.0091(15) 0.0079(14)
C28 0.077(2) 0.0422(14) 0.0590(16) -0.0095(12) 0.0010(14) 0.0175(14)
C29 0.0539(15) 0.0405(13) 0.0569(15) -0.0032(11) 0.0073(11) 0.0061(11)
F30 0.0654(12) 0.0634(11) 0.1250(19) -0.0178(11) 0.0446(12) -0.0021(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_occupancy
_atom_site_thermal_displace_type
Cu1 0.48277(3) 0.10019(2) 0.52026(2) 0.0339 1.0000 Uani
O1 0.31142(15) 0.05343(13) 0.55536(12) 0.0426 1.0000 Uani
O2 0.34424(16) -0.11656(13) 0.51981(14) 0.0475 1.0000 Uani
C3 0.2777(2) -0.04318(18) 0.55071(14) 0.0356 1.0000 Uani
C4 0.1522(2) -0.07510(19) 0.58413(16) 0.0378 1.0000 Uani
C5 0.1288(3) -0.1840(2) 0.5947(2) 0.0535 1.0000 Uani
C6 0.0137(3) -0.2204(3) 0.6243(3) 0.0804 1.0000 Uani
C7 -0.0798(3) -0.1472(3) 0.6451(3) 0.0804 1.0000 Uani
C8 -0.0583(3) -0.0402(3) 0.6359(2) 0.0617 1.0000 Uani
C9 0.0562(2) -0.0057(2) 0.60575(17) 0.0444 1.0000 Uani
F10 0.07046(15) 0.09985(12) 0.59495(13) 0.0573 1.0000 Uani
O11 0.42011(18) 0.11661(15) 0.39444(12) 0.0489 1.0000 Uani
O12 0.45416(19) -0.05440(16) 0.35940(12) 0.0519 1.0000 Uani
C13 0.4192(2) 0.0389(2) 0.34065(15) 0.0407 1.0000 Uani
C14 0.3721(2) 0.0568(2) 0.24492(17) 0.0429 1.0000 Uani
C15 0.3463(3) -0.0315(3) 0.1900(2) 0.0584 1.0000 Uani
C16 0.3077(4) -0.0200(3) 0.0999(2) 0.0774 1.0000 Uani
C17 0.2922(4) 0.0803(4) 0.0632(2) 0.0821 1.0000 Uani
C18 0.3134(4) 0.1700(3) 0.1167(2) 0.0782 1.0000 Uani
C19 0.3538(3) 0.1566(2) 0.2059(2) 0.0582 1.0000 Uani
F20 0.3712(3) 0.24469(17) 0.25450(16) 0.1018 1.0000 Uani
O21 0.44521(18) 0.26365(14) 0.56538(14) 0.0510 1.0000 Uani
O22 0.2531(2) 0.24870(17) 0.6168(2) 0.0830 1.0000 Uani
C23 0.3561(2) 0.30146(19) 0.60220(16) 0.0409 1.0000 Uani
C24 0.3540(2) 0.41381(18) 0.63451(17) 0.0408 1.0000 Uani
C25 0.4563(3) 0.4787(2) 0.61417(19) 0.0516 1.0000 Uani
C26 0.4595(4) 0.5848(2) 0.6392(2) 0.0627 1.0000 Uani
C27 0.3600(4) 0.6282(2) 0.6862(2) 0.0626 1.0000 Uani
C28 0.2597(3) 0.5660(2) 0.7077(2) 0.0594 1.0000 Uani
C29 0.2584(3) 0.4601(2) 0.68231(19) 0.0503 1.0000 Uani
F30 0.1600(2) 0.40157(16) 0.70892(19) 0.0838 1.0000 Uani
H51 0.1962 -0.2367 0.5809 0.0527 1.0000 Uiso
H61 -0.0020 -0.2986 0.6305 0.0757 1.0000 Uiso
H71 -0.1627 -0.1733 0.6667 0.0761 1.0000 Uiso
H81 -0.1248 0.0127 0.6516 0.0600 1.0000 Uiso
H151 0.3549 -0.1048 0.2163 0.0579 1.0000 Uiso
H161 0.2926 -0.0845 0.0613 0.0745 1.0000 Uiso
H171 0.2642 0.0889 -0.0017 0.0774 1.0000 Uiso
H181 0.3004 0.2428 0.0907 0.0748 1.0000 Uiso
H251 0.5283 0.4478 0.5806 0.0513 1.0000 Uiso
H261 0.5329 0.6305 0.6233 0.0607 1.0000 Uiso
H271 0.3617 0.7051 0.7044 0.0577 1.0000 Uiso
H281 0.1880 0.5968 0.7413 0.0581 1.0000 Uiso
H22 0.2522 0.1805 0.5854 0.0500 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 ' 0.0170 0.0090 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
'O ' 0.0470 0.0320 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
'F ' 0.0690 0.0530 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476
0.2776 International_Tables_Vol_IV_Table_2.2B
'Cu ' -2.0190 0.5890 13.3380 3.5828 7.1676 0.2470 5.6158 11.3966 1.6735
64.8126 1.1910 International_Tables_Vol_IV_Table_2.2B
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cu1 2_656 Cu1 O1 . 84.95(5) yes
Cu1 2_656 Cu1 O2 2_656 83.83(5) yes
O1 . Cu1 O2 2_656 168.78(7) yes
Cu1 2_656 Cu1 O11 . 86.04(5) yes
O1 . Cu1 O11 . 89.28(8) yes
O2 2_656 Cu1 O11 . 90.06(8) yes
Cu1 2_656 Cu1 O12 2_656 83.04(6) yes
O1 . Cu1 O12 2_656 88.36(8) yes
O2 2_656 Cu1 O12 2_656 90.17(9) yes
O11 . Cu1 O12 2_656 168.98(8) yes
Cu1 2_656 Cu1 O21 . 174.80(5) yes
O1 . Cu1 O21 . 91.16(7) yes
O2 2_656 Cu1 O21 . 100.03(7) yes
O11 . Cu1 O21 . 97.38(8) yes
O12 2_656 Cu1 O21 . 93.43(8) yes
Cu1 . O1 C3 . 121.78(15) yes
Cu1 2_656 O2 C3 . 125.25(15) yes
O1 . C3 O2 . 124.1(2) yes
O1 . C3 C4 . 119.6(2) yes
O2 . C3 C4 . 116.3(2) yes
C3 . C4 C5 . 117.6(2) yes
C3 . C4 C9 . 125.5(2) yes
C5 . C4 C9 . 116.9(2) yes
C4 . C5 C6 . 121.2(3) yes
C4 . C5 H51 . 119.5(2) no
C6 . C5 H51 . 119.3(3) no
C5 . C6 C7 . 119.6(3) yes
C5 . C6 H61 . 120.2(3) no
C7 . C6 H61 . 120.2(3) no
C6 . C7 C8 . 120.1(3) yes
C6 . C7 H71 . 119.8(4) no
C8 . C7 H71 . 120.1(4) no
C7 . C8 C9 . 119.4(3) yes
C7 . C8 H81 . 120.3(3) no
C9 . C8 H81 . 120.3(3) no
C4 . C9 C8 . 122.8(3) yes
C4 . C9 F10 . 120.3(2) yes
C8 . C9 F10 . 116.8(2) yes
Cu1 . O11 C13 . 120.74(16) yes
Cu1 2_656 O12 C13 . 124.22(17) yes
O11 . C13 O12 . 125.9(2) yes
O11 . C13 C14 . 118.3(2) yes
O12 . C13 C14 . 115.8(2) yes
C13 . C14 C15 . 118.9(3) yes
C13 . C14 C19 . 124.3(2) yes
C15 . C14 C19 . 116.9(2) yes
C14 . C15 C16 . 121.5(3) yes
C14 . C15 H151 . 119.3(3) no
C16 . C15 H151 . 119.2(3) no
C15 . C16 C17 . 120.0(3) yes
C15 . C16 H161 . 119.9(4) no
C17 . C16 H161 . 120.0(3) no
C16 . C17 C18 . 120.0(3) yes
C16 . C17 H171 . 120.2(4) no
C18 . C17 H171 . 119.8(4) no
C17 . C18 C19 . 118.9(3) yes
C17 . C18 H181 . 120.2(3) no
C19 . C18 H181 . 120.9(4) no
C14 . C19 C18 . 122.7(3) yes
C14 . C19 F20 . 120.8(2) yes
C18 . C19 F20 . 116.5(3) yes
Cu1 . O21 C23 . 131.10(16) yes
C23 . O22 H22 . 111.4(2) no
O21 . C23 O22 . 123.5(2) yes
O21 . C23 C24 . 122.5(2) yes
O22 . C23 C24 . 114.0(2) yes
C23 . C24 C25 . 117.6(2) yes
C23 . C24 C29 . 125.4(2) yes
C25 . C24 C29 . 117.0(2) yes
C24 . C25 C26 . 121.1(3) yes
C24 . C25 H251 . 119.5(3) no
C26 . C25 H251 . 119.4(3) no
C25 . C26 C27 . 119.8(3) yes
C25 . C26 H261 . 120.1(3) no
C27 . C26 H261 . 120.1(3) no
C26 . C27 C28 . 120.2(3) yes
C26 . C27 H271 . 120.1(4) no
C28 . C27 H271 . 119.8(3) no
C27 . C28 C29 . 119.2(3) yes
C27 . C28 H281 . 120.5(3) no
C29 . C28 H281 . 120.3(3) no
C24 . C29 C28 . 122.7(3) yes
C24 . C29 F30 . 120.6(2) yes
C28 . C29 F30 . 116.6(3) yes
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
Cu1 Cu1 2_656 2.6087(6) yes
Cu1 O1 . 1.9957(16) yes
Cu1 O2 2_656 1.9583(17) yes
Cu1 O11 . 1.9624(18) yes
Cu1 O12 2_656 1.9629(18) yes
Cu1 O21 . 2.1931(17) yes
O1 C3 . 1.264(3) yes
O2 C3 . 1.253(3) yes
C3 C4 . 1.490(3) yes
C4 C5 . 1.396(4) yes
C4 C9 . 1.385(3) yes
C5 C6 . 1.388(4) yes
C5 H51 . 1.000(3) no
C6 C7 . 1.392(5) yes
C6 H61 . 0.999(3) no
C7 C8 . 1.368(6) yes
C7 H71 . 1.000(3) no
C8 C9 . 1.377(4) yes
C8 H81 . 1.001(3) no
C9 F10 . 1.341(3) yes
O11 C13 . 1.255(3) yes
O12 C13 . 1.255(3) yes
C13 C14 . 1.500(3) yes
C14 C15 . 1.393(4) yes
C14 C19 . 1.387(4) yes
C15 C16 . 1.385(4) yes
C15 H151 . 1.000(3) no
C16 C17 . 1.376(6) yes
C16 H161 . 0.999(4) no
C17 C18 . 1.388(6) yes
C17 H171 . 0.998(3) no
C18 C19 . 1.381(4) yes
C18 H181 . 0.997(4) no
C19 F20 . 1.325(4) yes
O21 C23 . 1.202(3) yes
O22 C23 . 1.303(3) yes
O22 H22 . 0.971(2) no
C23 C24 . 1.486(3) yes
C24 C25 . 1.397(4) yes
C24 C29 . 1.381(4) yes
C25 C26 . 1.380(4) yes
C25 H251 . 1.001(3) no
C26 C27 . 1.391(5) yes
C26 H261 . 1.001(3) no
C27 C28 . 1.364(5) yes
C27 H271 . 1.000(3) no
C28 C29 . 1.378(4) yes
C28 H281 . 0.998(3) no
C29 F30 . 1.345(3) yes
loop_
_refln_index_h
_refln_index_k
_refln_index_l
_refln_F_meas
_refln_F_calc
_refln_F_sigma
2 0 0 73.67 73.81 0.34
4 0 0 13.87 17.94 0.22
6 0 0 54.49 57.84 0.66
8 0 0 8.73 8.96 0.44
10 0 0 32.56 31.93 0.48
12 0 0 11.24 10.61 0.45
1 1 0 92.55 81.95 0.29
2 1 0 102.22 102.27 0.37
3 1 0 62.71 60.44 0.44
4 1 0 10.23 8.49 0.28
5 1 0 102.54 108.67 0.57
6 1 0 15.91 17.31 0.29
7 1 0 40.04 41.76 0.54
8 1 0 26.89 25.77 0.39
9 1 0 29.11 28.12 0.43
10 1 0 29.37 28.69 0.40
11 1 0 21.54 21.28 0.44
12 1 0 12.96 12.72 0.46
13 1 0 -2.19 0.00 3.09
0 2 0 157.32 167.66 0.29
1 2 0 38.05 38.28 0.37
2 2 0 23.52 23.12 0.35
3 2 0 81.43 79.49 0.47
4 2 0 36.59 38.88 0.39
5 2 0 112.81 117.59 0.59
6 2 0 9.56 11.27 0.37
7 2 0 18.43 18.75 0.30
8 2 0 22.23 22.58 0.37
9 2 0 7.50 7.28 0.60
10 2 0 1.35 0.00 5.18
11 2 0 27.25 27.53 0.45
12 2 0 -2.11 0.00 4.33
13 2 0 15.99 15.75 0.41
1 3 0 3.62 3.70 0.56
2 3 0 80.24 76.86 0.47
3 3 0 67.46 61.20 0.55
4 3 0 13.35 7.20 0.26
5 3 0 26.41 26.73 0.38
6 3 0 7.09 9.50 0.40
7 3 0 9.47 11.18 0.43
8 3 0 10.91 12.39 0.46
9 3 0 5.07 0.00 1.71
10 3 0 27.30 27.15 0.44
11 3 0 2.04 0.00 3.61
12 3 0 29.70 29.70 0.51
13 3 0 -1.16 0.00 5.65
0 4 0 62.94 63.35 0.43
1 4 0 9.68 11.64 0.24
2 4 0 72.23 72.28 0.52
3 4 0 56.60 51.97 0.60
4 4 0 24.99 19.23 0.37
5 4 0 51.35 52.93 0.67
6 4 0 63.75 65.94 0.74
7 4 0 9.56 11.27 0.47
8 4 0 18.89 20.31 0.38
9 4 0 5.21 3.64 0.87
10 4 0 15.25 14.67 0.44
11 4 0 20.99 21.57 0.39
12 4 0 14.63 14.47 0.43
1 5 0 126.22 131.53 0.51
2 5 0 68.23 60.09 0.61
3 5 0 78.79 68.64 0.67
4 5 0 8.46 8.15 0.38
5 5 0 58.22 61.73 0.71
6 5 0 14.00 14.21 0.33
7 5 0 47.33 48.79 0.59
8 5 0 2.46 0.00 4.20
9 5 0 12.00 12.58 0.50
10 5 0 5.94 5.99 0.78
11 5 0 -2.74 0.00 2.88
12 5 0 1.50 0.00 3.24
0 6 0 176.33 183.24 0.56
1 6 0 30.02 30.63 0.44
2 6 0 45.14 46.07 0.65
3 6 0 48.85 49.57 0.64
4 6 0 55.18 57.54 0.70
5 6 0 55.81 56.43 0.76
6 6 0 28.11 29.67 0.41
7 6 0 12.49 13.89 0.48
8 6 0 18.18 18.83 0.42
9 6 0 23.47 24.36 0.40
10 6 0 -1.65 0.00 5.35
11 6 0 10.67 10.24 0.44
12 6 0 8.41 8.07 0.52
1 7 0 11.58 12.64 0.29
2 7 0 18.77 15.40 0.30
3 7 0 23.95 23.17 0.39
4 7 0 46.90 48.47 0.54
5 7 0 12.73 13.27 0.40
6 7 0 44.85 45.95 0.62
7 7 0 13.52 14.95 0.48
8 7 0 18.16 15.96 0.46
9 7 0 8.60 9.58 0.65
10 7 0 25.01 26.12 0.38
11 7 0 4.36 0.00 1.42
0 8 0 26.70 28.68 0.39
1 8 0 5.76 0.00 1.16
2 8 0 42.36 42.80 0.55
3 8 0 3.60 0.00 0.98
4 8 0 7.57 6.95 0.51
5 8 0 66.49 67.58 0.87
6 8 0 4.13 0.00 2.19
7 8 0 14.17 13.05 0.48
8 8 0 -6.23 0.00 2.16
9 8 0 16.93 17.77 0.45
10 8 0 2.04 0.00 3.93
11 8 0 22.47 22.70 0.36
1 9 0 16.00 14.82 0.33
2 9 0 9.25 9.95 0.42
3 9 0 27.61 26.73 0.40
4 9 0 24.33 24.28 0.39
5 9 0 21.21 21.45 0.44
6 9 0 9.01 9.92 0.53
7 9 0 32.70 33.68 0.47
8 9 0 19.15 19.35 0.45
9 9 0 14.27 15.16 0.45
10 9 0 16.16 16.15 0.42
0 10 0 27.29 25.84 0.39
1 10 0 16.02 15.68 0.38
2 10 0 66.42 64.56 0.89
3 10 0 18.50 19.17 0.42
4 10 0 14.84 14.92 0.43
5 10 0 17.89 17.77 0.45
6 10 0 40.05 41.04 0.61
7 10 0 14.88 14.64 0.47
8 10 0 12.01 12.05 0.50
9 10 0 6.15 5.22 0.76
10 10 0 4.34 0.00 1.46
1 11 0 11.66 11.01 0.52
2 11 0 22.80 22.22 0.43
3 11 0 41.34 40.67 0.62
4 11 0 35.77 35.23 0.61
5 11 0 25.63 25.71 0.42
6 11 0 19.56 18.72 0.43
7 11 0 16.98 16.98 0.42
8 11 0 2.07 0.00 2.86
9 11 0 10.38 9.29 0.51
0 12 0 8.30 9.50 0.62
1 12 0 19.42 19.84 0.43
2 12 0 9.71 9.61 0.59
3 12 0 17.18 17.70 0.46
4 12 0 8.49 7.85 0.70
5 12 0 34.53 34.59 0.57
6 12 0 5.06 0.00 0.90
7 12 0 14.70 14.70 0.43
8 12 0 -1.99 0.00 3.17
1 13 0 25.61 25.49 0.43
2 13 0 7.72 8.13 0.74
3 13 0 8.87 9.18 0.60
4 13 0 14.66 15.67 0.49
5 13 0 11.03 10.44 0.46
6 13 0 11.80 12.00 0.49
7 13 0 -2.41 0.00 2.20
0 14 0 37.71 37.18 0.57
1 14 0 -2.82 0.00 3.44
2 14 0 12.56 11.93 0.47
3 14 0 1.39 0.00 4.66
4 14 0 14.53 14.78 0.43
5 14 0 5.95 6.64 0.66
6 14 0 4.35 0.00 0.96
1 15 0 18.60 19.72 0.39
2 15 0 -1.62 0.00 4.35
3 15 0 1.62 0.00 2.30
-13 0 1 1.48 0.00 4.21
-11 0 1 11.51 10.13 0.48
-9 0 1 11.75 11.88 0.52
-7 0 1 28.38 27.85 0.38
-5 0 1 55.20 55.29 0.59
-3 0 1 163.85 177.54 0.43
-1 0 1 85.72 92.65 0.27
1 0 1 173.82 169.70 0.24
3 0 1 32.21 34.18 0.41
5 0 1 99.56 104.24 0.57
7 0 1 48.57 51.76 0.68
9 0 1 48.50 47.83 0.64
11 0 1 -3.51 0.00 2.36
13 0 1 5.97 6.38 0.62
-13 1 1 7.94 8.20 0.50
-12 1 1 -1.72 0.00 4.45
-11 1 1 1.71 0.00 4.49
-10 1 1 14.66 14.42 0.43
-9 1 1 11.62 11.47 0.52
-8 1 1 -0.72 0.00 11.69
-7 1 1 16.60 17.29 0.33
-6 1 1 19.01 19.65 0.30
-5 1 1 99.83 102.62 0.58
-4 1 1 73.67 79.06 0.52
-3 1 1 115.17 125.09 0.44
-2 1 1 227.42 234.42 0.37
-1 1 1 13.06 10.26 0.20
0 1 1 169.16 153.06 0.25
1 1 1 31.58 32.84 0.33
2 1 1 4.45 9.50 0.69
3 1 1 11.87 13.52 0.23
4 1 1 8.64 7.72 0.30
5 1 1 52.70 57.30 0.58
6 1 1 19.92 21.11 0.30
7 1 1 14.08 14.26 0.37
8 1 1 6.41 4.72 0.61
9 1 1 6.46 6.16 0.69
10 1 1 8.47 7.16 0.64
11 1 1 6.66 7.17 0.81
12 1 1 19.78 20.40 0.39
13 1 1 10.82 9.37 0.42
-13 2 1 3.28 0.00 1.24
-12 2 1 27.54 26.38 0.40
-11 2 1 11.10 10.71 0.60
-10 2 1 39.35 38.41 0.58
-9 2 1 24.26 25.72 0.39
-8 2 1 26.76 27.38 0.44
-7 2 1 10.03 10.43 0.45
-6 2 1 18.73 18.84 0.29
-5 2 1 56.27 58.11 0.62
-4 2 1 99.85 101.37 0.55
-3 2 1 63.53 61.80 0.48
-2 2 1 23.02 25.98 0.34
-1 2 1 33.24 29.20 0.39
0 2 1 90.47 91.78 0.32
1 2 1 55.39 58.75 0.34
2 2 1 44.66 44.35 0.45
3 2 1 1.56 0.00 3.69
4 2 1 40.00 41.01 0.54
5 2 1 37.62 39.74 0.43
6 2 1 32.98 35.29 0.51
7 2 1 18.76 18.77 0.34
8 2 1 35.57 34.94 0.55
9 2 1 23.09 22.43 0.39
10 2 1 20.34 21.38 0.44
11 2 1 5.73 0.00 1.26
12 2 1 31.73 30.86 0.48
13 2 1 1.19 0.00 4.98
-13 3 1 14.68 14.76 0.40
-12 3 1 7.59 6.83 0.58
-11 3 1 28.00 28.01 0.43
-10 3 1 9.20 9.33 0.49
-9 3 1 1.84 0.00 3.69
-8 3 1 20.88 21.20 0.34
-7 3 1 46.78 47.57 0.56
-6 3 1 5.90 5.21 0.49
-5 3 1 46.38 48.12 0.64
-4 3 1 5.42 3.11 0.49
-3 3 1 80.47 77.56 0.53
-2 3 1 52.27 48.86 0.48
-1 3 1 46.11 43.63 0.43
0 3 1 28.16 29.30 0.36
1 3 1 9.00 8.59 0.24
2 3 1 35.80 32.34 0.51
3 3 1 75.26 67.36 0.57
4 3 1 36.89 36.13 0.41
5 3 1 12.47 15.57 0.30
6 3 1 29.38 31.66 0.43
7 3 1 24.24 24.76 0.31
8 3 1 20.67 22.14 0.34
9 3 1 6.98 6.62 0.65
10 3 1 4.51 0.00 0.99
11 3 1 24.11 24.14 0.41
12 3 1 7.83 6.61 0.63
13 3 1 19.96 20.26 0.36
-12 4 1 16.06 15.38 0.41
-11 4 1 8.18 8.61 0.58
-10 4 1 7.20 6.54 0.60
-9 4 1 10.51 11.75 0.58
-8 4 1 20.81 21.95 0.35
-7 4 1 42.31 42.63 0.58
-6 4 1 25.49 26.31 0.39
-5 4 1 105.34 109.58 0.66
-4 4 1 8.87 8.41 0.34
-3 4 1 18.42 19.83 0.28
-2 4 1 56.77 56.85 0.52
-1 4 1 54.42 50.87 0.47
0 4 1 43.93 44.13 0.45
1 4 1 97.46 107.22 0.44
2 4 1 10.78 11.00 0.29
3 4 1 88.97 86.56 0.55
4 4 1 35.67 31.90 0.45
5 4 1 5.21 0.78 0.49
6 4 1 1.31 0.00 5.09
7 4 1 60.83 66.61 0.81
8 4 1 33.25 33.70 0.47
9 4 1 19.96 18.87 0.41
10 4 1 -4.27 0.00 2.05
11 4 1 9.02 9.26 0.56
12 4 1 17.02 16.52 0.41
-12 5 1 8.20 7.96 0.53
-11 5 1 9.75 10.62 0.52
-10 5 1 1.45 0.00 6.18
-9 5 1 16.08 16.80 0.44
-8 5 1 4.96 0.00 0.93
-7 5 1 9.06 10.02 0.45
-6 5 1 40.13 43.65 0.56
-5 5 1 16.65 17.41 0.29
-4 5 1 69.70 66.01 0.72
-3 5 1 1.66 0.00 2.66
-2 5 1 74.44 74.79 0.57
-1 5 1 86.12 83.09 0.52
0 5 1 124.58 131.16 0.50
1 5 1 14.66 15.26 0.21
2 5 1 115.76 112.24 0.59
3 5 1 6.69 7.02 0.40
4 5 1 22.17 20.89 0.35
5 5 1 39.78 40.07 0.51
6 5 1 44.26 44.97 0.56
7 5 1 7.70 7.68 0.52
8 5 1 27.98 28.96 0.37
9 5 1 17.77 17.83 0.42
10 5 1 10.73 10.92 0.56
11 5 1 -4.41 0.00 1.95
12 5 1 14.76 15.22 0.41
-12 6 1 2.36 0.00 2.06
-11 6 1 10.86 11.23 0.43
-10 6 1 20.37 19.96 0.44
-9 6 1 3.18 0.00 2.46
-8 6 1 22.97 22.89 0.41
-7 6 1 7.58 7.48 0.58
-6 6 1 18.91 20.62 0.34
-5 6 1 37.01 38.02 0.55
-4 6 1 50.36 51.57 0.71
-3 6 1 72.77 64.91 0.74
-2 6 1 15.09 17.73 0.28
-1 6 1 47.21 49.13 0.59
0 6 1 33.62 29.93 0.42
1 6 1 149.19 145.08 0.59
2 6 1 32.46 29.53 0.46
3 6 1 34.51 36.12 0.47
4 6 1 45.43 45.93 0.50
5 6 1 45.82 46.84 0.55
6 6 1 41.24 40.78 0.62
7 6 1 31.79 34.87 0.49
8 6 1 2.13 0.00 4.42
9 6 1 12.89 14.37 0.46
10 6 1 23.28 24.29 0.43
11 6 1 3.34 0.00 1.98
12 6 1 6.82 7.51 0.60
-11 7 1 21.29 21.51 0.39
-10 7 1 12.62 12.47 0.45
-9 7 1 34.33 36.10 0.52
-8 7 1 4.32 0.00 2.20
-7 7 1 13.87 15.37 0.44
-6 7 1 18.59 18.86 0.38
-5 7 1 63.30 64.29 0.81
-4 7 1 37.86 37.76 0.54
-3 7 1 59.63 61.77 0.75
-2 7 1 26.79 28.40 0.43
-1 7 1 34.11 34.00 0.48
0 7 1 21.59 20.38 0.31
1 7 1 61.36 58.73 0.66
2 7 1 1.19 0.00 4.05
3 7 1 12.04 11.12 0.37
4 7 1 4.85 6.71 0.69
5 7 1 49.17 48.64 0.59
6 7 1 24.73 25.43 0.37
7 7 1 8.57 7.27 0.58
8 7 1 3.90 0.00 1.17
9 7 1 9.76 8.98 0.57
10 7 1 4.98 0.00 0.90
11 7 1 13.24 13.40 0.43
-11 8 1 1.20 0.00 3.48
-10 8 1 28.41 28.64 0.49
-9 8 1 2.32 0.00 2.03
-8 8 1 18.73 17.42 0.43
-7 8 1 11.60 10.73 0.54
-6 8 1 6.03 5.84 0.75
-5 8 1 13.46 13.56 0.42
-4 8 1 43.81 45.16 0.59
-3 8 1 3.17 0.00 2.01
-2 8 1 18.67 17.68 0.31
-1 8 1 36.33 35.45 0.52
0 8 1 13.09 11.40 0.32
1 8 1 18.02 20.50 0.33
2 8 1 20.34 19.62 0.32
3 8 1 22.96 21.39 0.36
4 8 1 0.30 0.00 26.08
5 8 1 18.68 18.02 0.39
6 8 1 55.45 55.55 0.65
7 8 1 29.46 30.63 0.48
8 8 1 23.72 25.13 0.40
9 8 1 2.73 0.00 2.68
10 8 1 24.93 25.84 0.37
11 8 1 1.52 0.00 3.13
-10 9 1 1.85 0.00 3.44
-9 9 1 19.79 18.34 0.43
-8 9 1 11.45 12.05 0.53
-7 9 1 31.31 31.90 0.46
-6 9 1 32.69 31.95 0.48
-5 9 1 17.60 17.63 0.44
-4 9 1 48.96 50.09 0.63
-3 9 1 7.43 7.56 0.56
-2 9 1 50.37 47.54 0.60
-1 9 1 10.78 9.62 0.42
0 9 1 40.28 40.28 0.59
1 9 1 11.57 12.32 0.45
2 9 1 50.32 51.05 0.60
3 9 1 25.40 25.28 0.38
4 9 1 13.98 12.93 0.43
5 9 1 4.37 0.00 1.08
6 9 1 12.18 13.67 0.46
7 9 1 8.99 8.04 0.53
8 9 1 25.24 26.32 0.45
9 9 1 6.92 6.90 0.66
10 9 1 13.61 13.96 0.43
-10 10 1 2.58 0.00 1.80
-9 10 1 7.14 7.18 0.68
-8 10 1 -3.16 0.00 2.91
-7 10 1 22.37 23.04 0.44
-6 10 1 18.39 18.40 0.42
-5 10 1 36.24 36.07 0.54
-4 10 1 25.16 25.65 0.38
-3 10 1 10.55 10.04 0.59
-2 10 1 26.80 26.62 0.44
-1 10 1 14.64 13.84 0.42
0 10 1 9.33 8.07 0.49
1 10 1 50.00 50.56 0.63
2 10 1 14.69 13.80 0.41
3 10 1 79.60 78.48 0.91
4 10 1 22.24 20.95 0.44
5 10 1 8.72 9.31 0.56
6 10 1 20.48 20.91 0.41
7 10 1 48.77 49.58 0.65
8 10 1 14.04 14.53 0.51
9 10 1 15.00 15.03 0.42
10 10 1 2.06 0.00 3.01
-9 11 1 12.42 12.68 0.43
-8 11 1 8.30 8.27 0.66
-7 11 1 19.79 19.38 0.42
-6 11 1 12.68 13.30 0.55
-5 11 1 19.04 19.02 0.40
-4 11 1 17.05 17.06 0.47
-3 11 1 14.39 15.55 0.46
-2 11 1 38.85 38.38 0.55
-1 11 1 9.47 9.10 0.64
0 11 1 21.28 19.91 0.44
1 11 1 3.39 0.00 2.89
2 11 1 43.49 41.89 0.68
3 11 1 22.17 22.47 0.45
4 11 1 23.51 22.52 0.42
5 11 1 4.43 0.00 1.11
6 11 1 6.96 5.18 0.73
7 11 1 1.73 0.00 5.42
8 11 1 16.70 16.23 0.45
9 11 1 1.73 0.00 3.03
-8 12 1 9.53 10.79 0.52
-7 12 1 -3.45 0.00 2.49
-6 12 1 11.96 13.45 0.47
-5 12 1 8.29 8.92 0.70
-4 12 1 18.54 18.82 0.47
-3 12 1 13.74 13.19 0.46
-2 12 1 13.49 13.95 0.48
-1 12 1 2.08 0.00 4.51
0 12 1 -4.61 0.00 2.32
1 12 1 -3.75 0.00 3.29
2 12 1 6.03 6.58 0.81
3 12 1 39.04 38.76 0.61
4 12 1 22.42 23.21 0.46
5 12 1 15.85 15.41 0.46
6 12 1 11.69 10.40 0.48
7 12 1 9.36 9.85 0.57
8 12 1 7.16 7.65 0.61
-7 13 1 13.97 14.60 0.40
-6 13 1 -3.99 0.00 2.12
-5 13 1 18.73 19.22 0.38
-4 13 1 5.76 7.12 0.82
-3 13 1 13.67 13.49 0.48
-2 13 1 8.66 8.00 0.66
-1 13 1 9.11 8.06 0.65
0 13 1 26.78 26.34 0.44
1 13 1 8.42 8.69 0.70
2 13 1 10.45 10.85 0.55
3 13 1 10.14 10.38 0.53
4 13 1 3.42 0.00 2.32
5 13 1 19.57 19.28 0.39
6 13 1 5.98 6.31 0.81
7 13 1 5.77 5.73 0.86
-5 14 1 11.84 12.36 0.44
-4 14 1 0.38 0.00 23.51
-3 14 1 20.83 20.61 0.41
-2 14 1 3.09 0.00 1.39
-1 14 1 23.95 22.94 0.38
0 14 1 5.16 0.00 0.89
1 14 1 22.48 22.76 0.41
2 14 1 2.45 0.00 2.85
3 14 1 12.15 11.22 0.47
4 14 1 2.93 0.00 2.35
5 14 1 20.37 20.39 0.35
-3 15 1 -0.99 0.00 6.21
-2 15 1 15.27 16.00 0.39
-1 15 1 3.99 0.00 1.04
0 15 1 17.05 17.39 0.39
1 15 1 5.63 4.36 0.77
2 15 1 17.74 17.72 0.37
3 15 1 6.89 6.11 0.64
-12 0 2 2.41 0.00 3.21
-10 0 2 3.53 0.00 1.32
-8 0 2 13.59 16.19 0.39
-6 0 2 20.67 22.90 0.35
-4 0 2 198.96 215.13 0.52
-2 0 2 34.07 39.70 0.42
0 0 2 87.70 85.96 0.30
2 0 2 163.15 167.14 0.35
4 0 2 30.10 35.06 0.38
6 0 2 77.02 77.53 0.66
8 0 2 19.76 18.75 0.33
10 0 2 40.25 39.10 0.60
12 0 2 7.26 7.52 0.65
-13 1 2 -2.98 0.00 2.28
-12 1 2 12.67 12.42 0.45
-11 1 2 1.14 0.00 5.55
-10 1 2 -1.30 0.00 5.24
-9 1 2 33.49 31.28 0.51
-8 1 2 23.36 23.77 0.38
-7 1 2 6.37 7.24 0.53
-6 1 2 45.05 46.29 0.50
-5 1 2 135.17 137.57 0.61
-4 1 2 59.67 64.44 0.54
-3 1 2 127.16 134.50 0.46
-2 1 2 38.76 42.49 0.42
-1 1 2 37.20 37.66 0.37
0 1 2 48.36 46.55 0.34
1 1 2 74.80 76.96 0.33
2 1 2 77.83 70.38 0.41
3 1 2 11.68 10.04 0.23
4 1 2 6.91 6.23 0.36
5 1 2 50.28 56.32 0.59
6 1 2 42.91 42.65 0.49
7 1 2 28.00 29.02 0.44
8 1 2 25.20 25.37 0.38
9 1 2 24.25 24.03 0.37
10 1 2 22.69 22.24 0.40
11 1 2 20.55 20.23 0.44
12 1 2 14.14 12.90 0.40
13 1 2 1.86 0.00 2.54
-13 2 2 13.48 13.74 0.41
-12 2 2 7.97 8.02 0.57
-11 2 2 24.93 24.68 0.42
-10 2 2 1.28 0.00 2.59
-9 2 2 19.07 18.73 0.40
-8 2 2 4.19 3.49 0.70
-7 2 2 74.74 78.20 0.79
-6 2 2 24.90 24.04 0.33
-5 2 2 114.31 114.56 0.65
-4 2 2 71.40 71.94 0.57
-3 2 2 5.09 6.35 0.49
-2 2 2 24.08 23.18 0.38
-1 2 2 41.35 37.61 0.43
0 2 2 27.83 30.54 0.30
1 2 2 78.04 80.37 0.36
2 2 2 -3.42 0.00 1.54
3 2 2 8.40 10.56 0.27
4 2 2 34.92 39.12 0.51
5 2 2 7.67 9.89 0.36
6 2 2 37.26 36.90 0.47
7 2 2 21.07 19.78 0.31
8 2 2 -1.61 0.00 2.42
9 2 2 8.42 8.22 0.53
10 2 2 29.12 29.08 0.46
11 2 2 25.60 25.07 0.39
12 2 2 7.92 8.71 0.67
13 2 2 24.35 24.22 0.34
-13 3 2 0.45 0.00 11.30
-12 3 2 21.81 22.04 0.39
-11 3 2 -5.33 0.00 1.86
-10 3 2 33.73 33.13 0.53
-9 3 2 10.08 10.34 0.56
-8 3 2 45.10 43.10 0.63
-7 3 2 23.08 22.35 0.33
-6 3 2 81.89 83.73 0.72
-5 3 2 27.76 25.02 0.37
-4 3 2 7.72 11.11 0.38
-3 3 2 35.97 36.01 0.41
-2 3 2 95.26 93.91 0.49
-1 3 2 54.85 53.30 0.46
0 3 2 13.49 13.22 0.25
1 3 2 32.26 33.82 0.44
2 3 2 4.46 3.76 0.41
3 3 2 39.87 42.70 0.48
4 3 2 20.49 21.61 0.30
5 3 2 25.79 29.80 0.37
6 3 2 4.11 5.13 0.69
7 3 2 21.76 22.52 0.31
8 3 2 32.31 32.37 0.49
9 3 2 11.66 11.83 0.52
10 3 2 9.66 9.53 0.60
11 3 2 8.21 7.57 0.59
12 3 2 26.45 26.36 0.40
-12 4 2 -0.92 0.00 7.82
-11 4 2 6.55 6.94 0.71
-10 4 2 1.28 0.00 3.38
-9 4 2 -2.23 0.00 1.81
-8 4 2 17.07 17.76 0.44
-7 4 2 49.46 48.99 0.59
-6 4 2 45.30 45.94 0.54
-5 4 2 38.18 35.38 0.52
-4 4 2 51.44 49.48 0.68
-3 4 2 62.34 60.71 0.60
-2 4 2 98.25 94.90 0.54
-1 4 2 45.91 44.94 0.51
0 4 2 82.41 87.26 0.47
1 4 2 30.52 31.51 0.35
2 4 2 47.01 49.57 0.50
3 4 2 3.47 2.10 0.47
4 4 2 23.37 26.85 0.32
5 4 2 16.93 17.19 0.29
6 4 2 25.99 26.33 0.39
7 4 2 25.73 26.69 0.38
8 4 2 39.81 42.13 0.62
9 4 2 22.59 23.40 0.40
10 4 2 20.76 21.17 0.41
11 4 2 13.75 13.39 0.47
12 4 2 16.15 16.07 0.41
-12 5 2 0.52 0.00 11.24
-11 5 2 6.47 5.26 0.65
-10 5 2 15.85 16.26 0.52
-9 5 2 13.99 15.15 0.43
-8 5 2 16.87 17.63 0.46
-7 5 2 29.97 29.85 0.47
-6 5 2 2.20 0.00 1.65
-5 5 2 29.44 30.54 0.45
-4 5 2 2.84 0.00 1.07
-3 5 2 66.56 62.86 0.63
-2 5 2 8.93 6.75 0.31
-1 5 2 131.52 128.94 0.55
0 5 2 57.18 54.35 0.53
1 5 2 80.61 85.37 0.53
2 5 2 7.40 9.05 0.32
3 5 2 67.33 74.56 0.59
4 5 2 23.91 24.07 0.33
5 5 2 67.95 71.65 0.71
6 5 2 35.39 35.98 0.55
7 5 2 40.75 43.18 0.58
8 5 2 16.76 18.22 0.43
9 5 2 19.86 19.94 0.40
10 5 2 2.17 0.00 2.88
11 5 2 6.72 6.07 0.67
12 5 2 3.03 0.00 1.71
-12 6 2 -2.45 0.00 2.54
-11 6 2 10.81 11.30 0.46
-10 6 2 -2.97 0.00 2.71
-9 6 2 22.39 22.55 0.42
-8 6 2 2.49 0.00 3.73
-7 6 2 17.47 17.29 0.42
-6 6 2 17.35 18.69 0.38
-5 6 2 43.04 43.98 0.55
-4 6 2 56.35 53.48 0.79
-3 6 2 16.23 17.33 0.29
-2 6 2 91.36 89.47 0.65
-1 6 2 -2.10 0.00 3.85
0 6 2 63.65 62.36 0.60
1 6 2 20.15 15.93 0.28
2 6 2 37.75 41.45 0.46
3 6 2 41.99 41.87 0.48
4 6 2 62.59 64.19 0.71
5 6 2 33.04 30.84 0.49
6 6 2 38.59 39.94 0.63
7 6 2 9.08 9.15 0.47
8 6 2 10.02 10.70 0.59
9 6 2 4.28 0.00 1.83
10 6 2 19.68 20.67 0.44
11 6 2 14.31 14.36 0.44
12 6 2 9.93 9.65 0.51
-11 7 2 -2.36 0.00 3.17
-10 7 2 21.83 22.45 0.41
-9 7 2 17.49 17.31 0.52
-8 7 2 18.69 19.77 0.41
-7 7 2 3.02 0.00 1.51
-6 7 2 21.15 21.18 0.33
-5 7 2 28.88 30.41 0.44
-4 7 2 42.82 39.62 0.63
-3 7 2 30.00 28.94 0.41
-2 7 2 13.56 12.33 0.29
-1 7 2 1.90 0.00 4.27
0 7 2 41.20 40.00 0.49
1 7 2 8.83 6.23 0.40
2 7 2 4.53 6.13 0.62
3 7 2 16.65 17.43 0.31
4 7 2 17.38 18.77 0.33
5 7 2 30.34 29.05 0.44
6 7 2 48.28 45.04 0.68
7 7 2 3.48 0.00 1.30
8 7 2 10.94 11.51 0.55
9 7 2 -3.84 0.00 2.65
10 7 2 24.38 24.86 0.39
11 7 2 9.28 9.02 0.53
-11 8 2 17.01 17.74 0.36
-10 8 2 9.83 9.36 0.53
-9 8 2 31.55 31.67 0.52
-8 8 2 0.00 0.00 0.00
-7 8 2 29.47 33.01 0.46
-6 8 2 7.88 7.60 0.56
-5 8 2 52.83 55.17 0.60
-4 8 2 17.93 18.12 0.36
-3 8 2 40.19 38.20 0.61
-2 8 2 33.08 33.53 0.46
-1 8 2 8.40 8.93 0.39
0 8 2 22.18 21.85 0.39
1 8 2 11.98 10.60 0.37
2 8 2 33.17 31.13 0.55
3 8 2 8.17 7.53 0.45
4 8 2 34.38 34.66 0.51
5 8 2 10.57 10.55 0.43
6 8 2 10.98 8.48 0.47
7 8 2 8.07 8.56 0.58
8 8 2 15.62 15.75 0.46
9 8 2 2.55 0.00 3.70
10 8 2 -0.89 0.00 8.02
11 8 2 14.34 14.51 0.38
-10 9 2 19.62 18.38 0.41
-9 9 2 6.72 6.71 0.67
-8 9 2 4.48 0.00 0.84
-7 9 2 31.32 33.30 0.46
-6 9 2 15.17 14.96 0.39
-5 9 2 15.09 14.72 0.49
-4 9 2 29.51 29.96 0.44
-3 9 2 20.17 19.88 0.38
-2 9 2 33.87 33.43 0.51
-1 9 2 54.00 53.94 0.59
0 9 2 21.27 21.84 0.37
1 9 2 30.92 29.96 0.43
2 9 2 14.20 14.18 0.39
3 9 2 42.87 40.65 0.62
4 9 2 16.31 15.74 0.38
5 9 2 47.94 49.24 0.66
6 9 2 -5.30 0.00 2.65
7 9 2 42.23 40.39 0.69
8 9 2 17.67 17.40 0.45
9 9 2 14.23 14.03 0.43
10 9 2 9.88 10.62 0.50
-10 10 2 7.98 7.02 0.62
-9 10 2 7.82 7.98 0.58
-8 10 2 10.64 10.59 0.48
-7 10 2 -2.75 0.00 3.21
-6 10 2 22.86 23.34 0.37
-5 10 2 2.98 0.00 1.49
-4 10 2 21.50 22.62 0.42
-3 10 2 -4.90 0.00 2.14
-2 10 2 65.02 61.64 0.91
-1 10 2 30.14 30.60 0.46
0 10 2 64.92 63.56 0.91
1 10 2 16.95 16.53 0.37
2 10 2 36.09 34.69 0.53
3 10 2 16.88 15.82 0.49
4 10 2 20.17 20.43 0.42
5 10 2 -5.58 0.00 2.17
6 10 2 16.35 14.81 0.41
7 10 2 13.86 13.69 0.56
8 10 2 34.46 34.56 0.59
9 10 2 -3.07 0.00 2.31
10 10 2 9.66 9.98 0.49
-9 11 2 8.36 8.94 0.56
-8 11 2 14.52 15.67 0.43
-7 11 2 12.38 13.34 0.42
-6 11 2 3.15 0.00 1.58
-5 11 2 8.15 9.48 0.51
-4 11 2 8.64 9.84 0.69
-3 11 2 15.74 16.60 0.39
-2 11 2 19.78 18.90 0.42
-1 11 2 25.33 23.66 0.40
0 11 2 16.35 13.05 0.41
1 11 2 37.75 35.64 0.54
2 11 2 -4.92 0.00 2.81
3 11 2 61.20 58.59 0.68
4 11 2 5.57 6.68 0.93
5 11 2 36.38 35.10 0.50
6 11 2 8.78 8.46 0.68
7 11 2 13.42 13.68 0.49
8 11 2 5.29 0.00 0.94
9 11 2 6.71 6.74 0.56
-8 12 2 4.07 0.00 0.89
-7 12 2 12.96 14.16 0.42
-6 12 2 8.24 8.58 0.48
-5 12 2 18.39 19.79 0.39
-4 12 2 -1.63 0.00 6.52
-3 12 2 26.16 26.98 0.39
-2 12 2 17.71 17.49 0.45
-1 12 2 -4.06 0.00 2.44
0 12 2 4.10 0.00 1.23
1 12 2 23.70 23.18 0.43
2 12 2 13.39 12.57 0.51
3 12 2 0.00 0.00 0.00
4 12 2 23.44 22.38 0.47
5 12 2 13.55 12.25 0.51
6 12 2 4.37 0.00 1.09
7 12 2 2.37 0.00 3.56
8 12 2 2.28 0.00 3.71
-7 13 2 3.51 0.00 1.21
-6 13 2 7.77 8.35 0.54
-5 13 2 9.83 9.24 0.46
-4 13 2 20.68 21.38 0.41
-3 13 2 6.56 5.79 0.73
-2 13 2 7.21 7.96 0.72
-1 13 2 18.31 18.76 0.47
0 13 2 20.56 20.30 0.43
1 13 2 13.40 13.11 0.56
2 13 2 4.83 0.00 0.91
3 13 2 -5.76 0.00 2.16
4 13 2 5.66 2.78 0.87
5 13 2 -3.54 0.00 3.83
6 13 2 11.04 9.54 0.53
7 13 2 3.68 0.00 1.23
-5 14 2 -1.51 0.00 2.26
-4 14 2 18.27 19.72 0.40
-3 14 2 6.15 5.75 0.70
-2 14 2 20.14 20.21 0.38
-1 14 2 3.29 0.00 1.32
0 14 2 20.90 20.48 0.38
1 14 2 5.25 5.44 0.66
2 14 2 15.16 14.50 0.43
3 14 2 -5.40 0.00 1.98
4 14 2 15.29 13.74 0.43
5 14 2 3.76 0.00 1.03
-3 15 2 15.86 17.83 0.41
-2 15 2 4.35 0.00 0.82
-1 15 2 10.68 9.37 0.43
0 15 2 3.16 0.00 1.13
1 15 2 15.52 15.50 0.41
2 15 2 -1.60 0.00 2.40
3 15 2 16.76 16.73 0.42
-13 0 3 11.58 11.22 0.45
-11 0 3 8.13 8.75 0.65
-9 0 3 35.06 35.54 0.53
-7 0 3 32.60 35.40 0.48
-5 0 3 90.83 86.63 0.63
-3 0 3 74.48 74.55 0.48
-1 0 3 20.43 23.21 0.33
1 0 3 207.07 206.54 0.40
3 0 3 104.78 114.22 0.43
5 0 3 73.59 77.82 0.60
7 0 3 72.87 72.96 0.77
9 0 3 49.94 47.13 0.63
11 0 3 13.68 13.84 0.46
13 0 3 -2.15 0.00 3.11
-13 1 3 7.37 6.97 0.59
-12 1 3 9.48 8.59 0.48
-11 1 3 18.39 18.15 0.43
-10 1 3 19.70 22.41 0.39
-9 1 3 20.42 21.12 0.38
-8 1 3 50.02 50.53 0.63
-7 1 3 77.13 79.97 0.80
-6 1 3 105.31 107.66 0.71
-5 1 3 43.06 42.50 0.56
-4 1 3 85.29 87.44 0.56
-3 1 3 3.66 0.00 0.65
-2 1 3 14.56 20.38 0.22
-1 1 3 83.57 83.70 0.41
0 1 3 180.77 163.63 0.39
1 1 3 134.45 141.54 0.39
2 1 3 105.65 104.56 0.46
3 1 3 44.39 48.75 0.48
4 1 3 2.66 0.00 2.26
5 1 3 20.10 18.04 0.29
6 1 3 79.40 79.21 0.69
7 1 3 13.89 12.70 0.37
8 1 3 46.15 45.65 0.60
9 1 3 19.51 17.45 0.40
10 1 3 21.42 21.48 0.41
11 1 3 30.85 30.09 0.48
12 1 3 16.29 15.28 0.46
13 1 3 8.57 8.30 0.54
-13 2 3 -2.42 0.00 2.19
-12 2 3 21.10 20.75 0.41
-11 2 3 6.67 6.14 0.76
-10 2 3 35.53 34.91 0.54
-9 2 3 13.51 11.86 0.46
-8 2 3 23.34 22.56 0.38
-7 2 3 2.74 0.00 2.74
-6 2 3 67.02 69.66 0.75
-5 2 3 41.83 38.62 0.47
-4 2 3 102.92 102.19 0.59
-3 2 3 40.57 38.60 0.54
-2 2 3 57.80 55.84 0.49
-1 2 3 40.09 42.82 0.47
0 2 3 29.57 20.76 0.33
1 2 3 59.04 60.91 0.43
2 2 3 64.45 67.47 0.43
3 2 3 21.33 22.39 0.31
4 2 3 14.82 15.02 0.22
5 2 3 11.21 13.72 0.31
6 2 3 29.44 30.02 0.41
7 2 3 33.29 35.16 0.54
8 2 3 26.33 26.18 0.40
9 2 3 -3.57 0.00 2.60
10 2 3 13.71 13.78 0.46
11 2 3 7.57 5.84 0.63
12 2 3 19.03 18.56 0.39
-12 3 3 3.22 0.00 1.84
-11 3 3 37.57 36.96 0.61
-10 3 3 -1.38 0.00 6.68
-9 3 3 36.28 35.40 0.54
-8 3 3 3.03 0.00 3.03
-7 3 3 69.22 72.01 0.82
-6 3 3 20.24 21.22 0.35
-5 3 3 103.04 105.48 0.70
-4 3 3 38.45 36.08 0.46
-3 3 3 24.90 21.43 0.36
-2 3 3 85.04 83.04 0.52
-1 3 3 60.26 56.42 0.49
0 3 3 48.21 47.66 0.47
1 3 3 17.60 15.89 0.27
2 3 3 16.74 18.91 0.26
3 3 3 -1.82 0.00 3.64
4 3 3 7.09 9.99 0.35
5 3 3 4.93 5.27 0.62
6 3 3 40.78 41.98 0.53
7 3 3 12.89 11.68 0.37
8 3 3 13.81 14.93 0.39
9 3 3 24.91 25.36 0.42
10 3 3 -2.51 0.00 3.55
11 3 3 26.94 27.10 0.40
12 3 3 2.70 0.00 2.21
-12 4 3 8.99 9.09 0.56
-11 4 3 -1.48 0.00 6.86
-10 4 3 26.40 26.45 0.43
-9 4 3 5.52 6.90 0.88
-8 4 3 22.57 23.84 0.41
-7 4 3 26.67 28.44 0.40
-6 4 3 57.39 56.83 0.84
-5 4 3 62.97 57.01 0.76
-4 4 3 38.95 39.89 0.49
-3 4 3 48.06 48.15 0.62
-2 4 3 33.41 31.78 0.41
-1 4 3 129.04 129.35 0.53
0 4 3 74.37 73.60 0.51
1 4 3 6.87 5.94 0.36
2 4 3 48.76 51.06 0.53
3 4 3 23.21 27.00 0.34
4 4 3 47.91 49.54 0.64
5 4 3 23.51 28.98 0.33
6 4 3 10.22 10.33 0.42
7 4 3 39.70 41.31 0.58
8 4 3 22.70 22.98 0.37
9 4 3 17.12 18.37 0.44
10 4 3 10.09 10.47 0.56
11 4 3 16.91 16.06 0.45
12 4 3 16.34 15.16 0.38
-12 5 3 2.66 0.00 1.37
-11 5 3 4.38 0.00 0.92
-10 5 3 17.64 18.54 0.46
-9 5 3 20.64 22.00 0.43
-8 5 3 7.05 6.89 0.66
-7 5 3 15.08 15.75 0.38
-6 5 3 51.30 53.48 0.58
-5 5 3 18.31 14.80 0.33
-4 5 3 41.78 42.95 0.52
-3 5 3 14.31 15.05 0.30
-2 5 3 91.97 91.10 0.61
-1 5 3 49.60 44.80 0.59
0 5 3 129.44 125.59 0.56
1 5 3 119.05 114.16 0.56
2 5 3 70.81 71.32 0.58
3 5 3 31.39 33.48 0.45
4 5 3 44.38 45.85 0.52
5 5 3 7.61 8.09 0.51
6 5 3 65.74 68.87 0.79
7 5 3 17.48 17.76 0.39
8 5 3 44.59 45.89 0.62
9 5 3 10.17 10.49 0.59
10 5 3 22.18 21.99 0.41
11 5 3 5.91 5.88 0.73
12 5 3 14.50 13.51 0.37
-12 6 3 11.69 11.49 0.42
-11 6 3 7.76 7.61 0.56
-10 6 3 4.38 0.00 1.86
-9 6 3 -0.96 0.00 8.93
-8 6 3 7.02 5.53 0.66
-7 6 3 16.68 16.27 0.44
-6 6 3 20.12 21.78 0.33
-5 6 3 24.07 22.13 0.40
-4 6 3 52.17 47.27 0.57
-3 6 3 35.66 32.94 0.52
-2 6 3 15.24 14.73 0.29
-1 6 3 3.10 0.00 0.77
0 6 3 37.47 39.24 0.44
1 6 3 74.11 75.39 0.62
2 6 3 43.02 42.98 0.47
3 6 3 69.81 75.48 0.68
4 6 3 -3.63 0.00 2.12
5 6 3 48.79 48.12 0.59
6 6 3 6.88 6.98 0.57
7 6 3 36.75 37.40 0.52
8 6 3 9.93 8.31 0.45
9 6 3 18.09 18.08 0.40
10 6 3 18.54 18.85 0.45
11 6 3 11.36 11.69 0.52
12 6 3 9.20 9.15 0.51
-11 7 3 18.19 19.31 0.39
-10 7 3 -0.72 0.00 14.11
-9 7 3 27.85 28.52 0.42
-8 7 3 15.87 17.11 0.47
-7 7 3 32.82 37.47 0.56
-6 7 3 11.47 12.25 0.50
-5 7 3 76.05 79.51 0.82
-4 7 3 11.50 11.30 0.51
-3 7 3 36.69 35.59 0.56
-2 7 3 20.71 20.95 0.30
-1 7 3 21.95 16.11 0.31
0 7 3 17.40 17.72 0.32
1 7 3 -3.88 0.00 1.70
2 7 3 11.36 11.20 0.35
3 7 3 7.49 8.90 0.43
4 7 3 20.86 19.02 0.35
5 7 3 18.77 17.66 0.38
6 7 3 17.38 17.98 0.42
7 7 3 4.67 0.64 0.67
8 7 3 6.71 6.52 0.67
9 7 3 5.60 0.00 1.34
10 7 3 6.83 6.51 0.61
11 7 3 13.53 13.84 0.41
-11 8 3 6.16 4.70 0.59
-10 8 3 21.27 19.75 0.43
-9 8 3 -2.05 0.00 4.05
-8 8 3 8.31 9.04 0.66
-7 8 3 2.44 0.00 4.89
-6 8 3 -2.43 0.00 3.65
-5 8 3 33.71 35.37 0.50
-4 8 3 38.31 34.46 0.52
-3 8 3 22.57 21.76 0.37
-2 8 3 31.54 32.55 0.46
-1 8 3 36.15 35.56 0.54
0 8 3 19.97 20.50 0.34
1 8 3 31.42 30.48 0.44
2 8 3 43.19 40.42 0.56
3 8 3 22.45 23.79 0.35
4 8 3 2.91 0.00 2.91
5 8 3 49.37 48.34 0.64
6 8 3 11.87 11.20 0.58
7 8 3 15.04 14.79 0.42
8 8 3 13.94 13.31 0.51
9 8 3 -3.54 0.00 2.67
10 8 3 10.28 10.89 0.53
11 8 3 5.16 3.97 0.79
-10 9 3 8.64 9.02 0.55
-9 9 3 16.93 16.76 0.41
-8 9 3 3.48 0.00 1.05
-7 9 3 29.43 31.71 0.38
-6 9 3 38.35 41.92 0.54
-5 9 3 44.77 47.24 0.63
-4 9 3 21.24 19.59 0.46
-3 9 3 9.13 8.75 0.51
-2 9 3 79.67 79.49 0.86
-1 9 3 13.12 13.35 0.42
0 9 3 41.32 40.28 0.60
1 9 3 19.73 19.41 0.35
2 9 3 25.88 24.97 0.39
3 9 3 14.63 14.26 0.41
4 9 3 5.37 6.30 0.89
5 9 3 28.36 26.51 0.42
6 9 3 20.48 19.49 0.43
7 9 3 12.85 14.60 0.47
8 9 3 18.12 18.55 0.43
9 9 3 -1.65 0.00 3.76
10 9 3 10.91 10.89 0.46
-10 10 3 4.28 0.00 1.58
-9 10 3 -5.63 0.00 1.63
-8 10 3 -2.44 0.00 3.65
-7 10 3 11.40 12.56 0.54
-6 10 3 10.64 11.17 0.52
-5 10 3 8.38 10.32 0.70
-4 10 3 3.00 0.00 3.00
-3 10 3 19.92 19.58 0.41
-2 10 3 49.53 49.19 0.66
-1 10 3 60.33 59.31 0.65
0 10 3 14.21 13.23 0.44
1 10 3 30.61 28.95 0.47
2 10 3 1.80 0.00 2.70
3 10 3 68.12 64.41 0.96
4 10 3 15.74 14.88 0.44
5 10 3 43.99 42.94 0.71
6 10 3 1.84 0.00 5.51
7 10 3 28.39 27.42 0.47
8 10 3 12.60 12.82 0.43
9 10 3 14.99 16.26 0.41
-9 11 3 9.98 9.73 0.54
-8 11 3 -4.56 0.00 1.63
-7 11 3 8.46 10.19 0.59
-6 11 3 6.93 7.06 0.69
-5 11 3 23.84 24.73 0.40
-4 11 3 3.81 0.00 1.14
-3 11 3 13.50 13.22 0.48
-2 11 3 77.78 75.52 0.94
-1 11 3 21.74 22.50 0.46
0 11 3 37.62 37.65 0.58
1 11 3 8.48 8.37 0.61
2 11 3 16.83 15.70 0.51
3 11 3 17.08 16.37 0.51
4 11 3 36.57 35.87 0.56
5 11 3 5.69 5.76 0.85
6 11 3 23.79 22.41 0.44
7 11 3 2.74 0.00 1.83
8 11 3 6.31 6.48 0.66
9 11 3 -0.36 0.00 18.60
-8 12 3 8.42 9.58 0.57
-7 12 3 4.35 0.00 0.84
-6 12 3 14.98 16.37 0.38
-5 12 3 16.88 16.71 0.41
-4 12 3 31.95 34.10 0.52
-3 12 3 6.25 6.53 0.89
-2 12 3 6.12 7.70 0.76
-1 12 3 5.96 3.83 0.81
0 12 3 8.51 8.07 0.58
1 12 3 16.01 15.86 0.42
2 12 3 14.78 14.17 0.45
3 12 3 30.20 28.26 0.43
4 12 3 4.94 0.00 0.93
5 12 3 9.86 9.83 0.55
6 12 3 13.85 13.36 0.49
7 12 3 2.69 0.00 1.68
8 12 3 9.17 9.11 0.51
-7 13 3 13.41 14.43 0.42
-6 13 3 -4.43 0.00 1.77
-5 13 3 16.44 17.83 0.41
-4 13 3 11.20 11.02 0.45
-3 13 3 14.94 16.33 0.46
-2 13 3 1.61 0.00 5.64
-1 13 3 -6.02 0.00 1.85
0 13 3 16.25 15.73 0.44
1 13 3 17.05 17.06 0.51
2 13 3 -4.10 0.00 2.73
3 13 3 3.64 0.00 2.91
4 13 3 6.68 6.42 0.70
5 13 3 4.65 0.00 1.06
6 13 3 16.75 16.61 0.41
7 13 3 -3.65 0.00 2.25
-5 14 3 5.96 7.16 0.61
-4 14 3 -2.61 0.00 2.61
-3 14 3 8.05 8.96 0.60
-2 14 3 7.41 7.22 0.64
-1 14 3 12.30 12.26 0.50
0 14 3 6.61 5.65 0.66
1 14 3 25.10 24.49 0.39
2 14 3 2.87 0.00 3.23
3 14 3 7.29 6.24 0.63
4 14 3 -3.03 0.00 2.78
5 14 3 22.59 22.01 0.39
-3 15 3 -2.67 0.00 2.34
-2 15 3 12.97 13.98 0.38
-1 15 3 4.17 0.00 0.89
0 15 3 16.82 16.21 0.36
1 15 3 -1.14 0.00 3.43
2 15 3 14.75 14.08 0.40
3 15 3 5.79 3.18 0.74
-12 0 4 13.94 15.12 0.43
-10 0 4 16.63 18.44 0.46
-8 0 4 36.66 35.82 0.54
-6 0 4 40.19 40.06 0.53
-4 0 4 45.90 48.45 0.59
-2 0 4 29.81 32.13 0.37
0 0 4 125.19 116.38 0.43
2 0 4 33.74 31.54 0.39
4 0 4 1.50 0.00 1.50
6 0 4 145.16 145.67 0.70
8 0 4 68.02 66.15 0.85
10 0 4 36.54 34.12 0.53
12 0 4 19.18 19.01 0.42
-13 1 4 -0.64 0.00 6.78
-12 1 4 13.99 14.40 0.42
-11 1 4 8.54 8.27 0.59
-10 1 4 13.47 14.37 0.51
-9 1 4 12.07 11.66 0.52
-8 1 4 -2.17 0.00 3.55
-7 1 4 22.80 20.60 0.34
-6 1 4 17.74 19.43 0.30
-5 1 4 -3.10 0.00 2.38
-4 1 4 104.54 106.32 0.59
-3 1 4 25.32 28.41 0.42
-2 1 4 34.52 38.87 0.44
-1 1 4 10.92 10.73 0.25
0 1 4 81.06 77.32 0.46
1 1 4 297.37 272.15 0.46
2 1 4 57.46 56.14 0.51
3 1 4 17.81 22.04 0.32
4 1 4 16.07 15.09 0.22
5 1 4 72.78 74.96 0.63
6 1 4 29.34 28.34 0.43
7 1 4 72.11 72.79 0.79
8 1 4 13.54 13.24 0.41
9 1 4 9.03 8.85 0.59
10 1 4 7.69 7.51 0.66
11 1 4 1.33 0.00 4.98
12 1 4 11.09 11.28 0.49
-12 2 4 7.89 8.12 0.61
-11 2 4 43.06 43.69 0.58
-10 2 4 7.35 6.85 0.61
-9 2 4 74.71 73.71 0.93
-8 2 4 51.42 51.62 0.66
-7 2 4 44.54 46.48 0.63
-6 2 4 14.66 13.94 0.39
-5 2 4 52.34 56.20 0.69
-4 2 4 79.74 80.29 0.62
-3 2 4 29.94 33.41 0.42
-2 2 4 64.73 63.48 0.53
-1 2 4 32.05 28.09 0.37
0 2 4 17.66 16.16 0.30
1 2 4 17.15 14.97 0.26
2 2 4 53.84 51.56 0.53
3 2 4 44.12 49.51 0.57
4 2 4 3.46 0.00 0.69
5 2 4 43.92 43.59 0.63
6 2 4 39.24 40.25 0.52
7 2 4 5.15 4.42 0.70
8 2 4 24.63 25.57 0.38
9 2 4 30.69 30.16 0.46
10 2 4 17.23 15.96 0.41
11 2 4 18.14 17.68 0.40
12 2 4 11.96 11.94 0.44
-12 3 4 21.47 21.22 0.38
-11 3 4 3.71 0.00 1.24
-10 3 4 55.64 55.82 0.63
-9 3 4 -1.41 0.00 6.28
-8 3 4 25.32 26.32 0.37
-7 3 4 29.06 28.88 0.41
-6 3 4 76.87 76.05 0.80
-5 3 4 44.28 41.31 0.53
-4 3 4 121.68 118.59 0.66
-3 3 4 32.74 28.29 0.45
-2 3 4 40.84 42.26 0.58
-1 3 4 75.00 70.54 0.52
0 3 4 25.06 24.21 0.41
1 3 4 10.54 11.87 0.28
2 3 4 43.51 47.70 0.55
3 3 4 18.94 17.00 0.25
4 3 4 25.67 25.58 0.44
5 3 4 14.50 14.54 0.28
6 3 4 42.38 45.56 0.53
7 3 4 31.21 31.07 0.48
8 3 4 22.48 21.69 0.37
9 3 4 16.53 16.54 0.46
10 3 4 5.61 0.00 1.66
11 3 4 10.71 10.11 0.51
12 3 4 14.36 14.16 0.42
-12 4 4 5.81 5.52 0.68
-11 4 4 24.66 23.98 0.39
-10 4 4 17.16 18.71 0.47
-9 4 4 17.71 17.26 0.46
-8 4 4 1.77 0.00 6.20
-7 4 4 36.90 37.45 0.49
-6 4 4 54.15 55.00 0.60
-5 4 4 40.22 41.58 0.55
-4 4 4 118.51 116.85 0.69
-3 4 4 28.24 26.03 0.40
-2 4 4 76.95 72.88 0.60
-1 4 4 58.28 53.88 0.57
0 4 4 96.08 91.44 0.55
1 4 4 10.35 11.97 0.28
2 4 4 1.55 0.00 3.49
3 4 4 5.32 3.26 0.56
4 4 4 52.67 57.04 0.63
5 4 4 7.88 6.33 0.46
6 4 4 48.74 51.37 0.55
7 4 4 2.31 0.00 3.47
8 4 4 36.06 37.30 0.53
9 4 4 20.39 21.73 0.44
10 4 4 11.66 11.62 0.58
11 4 4 6.99 6.13 0.73
12 4 4 10.80 10.47 0.46
-12 5 4 -2.67 0.00 2.45
-11 5 4 10.61 11.25 0.45
-10 5 4 -5.39 0.00 1.93
-9 5 4 13.00 13.33 0.49
-8 5 4 5.58 7.32 0.84
-7 5 4 2.95 0.00 0.98
-6 5 4 2.41 0.00 4.22
-5 5 4 63.53 61.97 0.82
-4 5 4 8.06 7.33 0.39
-3 5 4 8.00 4.02 0.46
-2 5 4 55.38 50.40 0.64
-1 5 4 18.24 20.58 0.29
0 5 4 47.12 43.90 0.61
1 5 4 120.31 121.42 0.59
2 5 4 28.74 29.04 0.45
3 5 4 44.48 47.72 0.48
4 5 4 9.43 10.70 0.43
5 5 4 50.82 57.48 0.73
6 5 4 4.44 0.00 0.83
7 5 4 59.13 62.95 0.87
8 5 4 20.64 20.66 0.44
9 5 4 28.73 28.60 0.45
10 5 4 -0.53 0.00 15.44
11 5 4 11.41 11.13 0.48
12 5 4 -2.27 0.00 2.26
-12 6 4 8.34 7.77 0.51
-11 6 4 5.91 6.57 0.69
-10 6 4 -2.84 0.00 3.80
-9 6 4 16.48 15.66 0.45
-8 6 4 -3.50 0.00 3.06
-7 6 4 10.37 10.07 0.58
-6 6 4 25.68 23.81 0.37
-5 6 4 45.76 45.18 0.63
-4 6 4 11.41 12.34 0.41
-3 6 4 32.33 33.13 0.55
-2 6 4 5.50 4.45 0.52
-1 6 4 64.14 58.02 0.67
0 6 4 69.09 70.82 0.66
1 6 4 40.70 38.69 0.47
2 6 4 62.50 63.26 0.68
3 6 4 84.47 84.30 0.71
4 6 4 18.85 18.35 0.30
5 6 4 2.18 0.00 3.81
6 6 4 49.49 50.74 0.61
7 6 4 3.50 0.00 3.06
8 6 4 27.73 27.76 0.39
9 6 4 8.27 8.56 0.68
10 6 4 19.65 19.74 0.41
11 6 4 16.34 16.55 0.43
-11 7 4 3.62 0.00 1.03
-10 7 4 22.51 21.35 0.41
-9 7 4 3.29 0.00 1.23
-8 7 4 25.95 26.86 0.40
-7 7 4 12.57 15.07 0.48
-6 7 4 10.79 12.56 0.54
-5 7 4 12.86 12.71 0.51
-4 7 4 78.85 77.60 0.82
-3 7 4 6.38 5.86 0.56
-2 7 4 39.47 42.22 0.55
-1 7 4 2.87 0.00 1.08
0 7 4 40.55 40.19 0.52
1 7 4 62.44 58.12 0.73
2 7 4 25.14 25.89 0.38
3 7 4 17.10 15.94 0.34
4 7 4 15.26 14.77 0.34
5 7 4 15.34 16.23 0.35
6 7 4 23.82 25.44 0.38
7 7 4 28.09 27.68 0.45
8 7 4 3.00 0.00 3.00
9 7 4 9.54 11.63 0.63
10 7 4 15.39 14.87 0.40
11 7 4 -0.23 0.00 28.48
-11 8 4 12.49 12.89 0.46
-10 8 4 6.32 6.86 0.83
-9 8 4 31.55 32.24 0.46
-8 8 4 5.67 5.04 0.94
-7 8 4 30.17 30.90 0.49
-6 8 4 40.97 44.20 0.65
-5 8 4 36.53 34.75 0.47
-4 8 4 16.71 15.92 0.38
-3 8 4 35.09 36.47 0.50
-2 8 4 26.94 24.83 0.37
-1 8 4 8.66 7.65 0.42
0 8 4 27.36 27.40 0.44
1 8 4 4.44 0.00 0.83
2 8 4 13.68 14.75 0.37
3 8 4 19.27 18.85 0.35
4 8 4 6.46 5.57 0.69
5 8 4 16.45 16.48 0.49
6 8 4 27.80 28.73 0.40
7 8 4 6.40 4.66 0.74
8 8 4 21.28 20.98 0.46
9 8 4 -1.19 0.00 8.17
10 8 4 1.12 0.00 6.59
11 8 4 12.83 12.37 0.42
-10 9 4 13.75 12.87 0.40
-9 9 4 11.17 10.25 0.44
-8 9 4 12.00 13.20 0.48
-7 9 4 6.81 6.88 0.60
-6 9 4 29.54 31.20 0.40
-5 9 4 44.78 47.32 0.63
-4 9 4 67.17 65.37 0.93
-3 9 4 21.75 22.43 0.34
-2 9 4 7.18 7.30 0.60
-1 9 4 73.01 70.10 0.85
0 9 4 6.08 6.68 0.70
1 9 4 43.28 41.55 0.64
2 9 4 15.56 14.92 0.38
3 9 4 52.56 52.40 0.65
4 9 4 1.81 0.00 2.72
5 9 4 16.77 15.87 0.51
6 9 4 30.44 29.77 0.48
7 9 4 23.45 23.71 0.44
8 9 4 3.15 0.00 1.18
9 9 4 7.89 7.50 0.58
10 9 4 -1.23 0.00 5.05
-9 10 4 -4.63 0.00 2.31
-8 10 4 6.11 7.70 0.76
-7 10 4 6.31 5.98 0.74
-6 10 4 23.18 24.92 0.41
-5 10 4 13.79 14.59 0.42
-4 10 4 52.41 52.38 0.65
-3 10 4 2.56 0.00 1.92
-2 10 4 32.82 33.22 0.48
-1 10 4 31.26 29.81 0.46
0 10 4 24.22 23.18 0.40
1 10 4 -3.61 0.00 1.36
2 10 4 27.64 27.72 0.42
3 10 4 14.87 15.24 0.46
4 10 4 41.98 40.19 0.66
5 10 4 13.87 13.19 0.50
6 10 4 10.73 10.94 0.61
7 10 4 8.35 8.29 0.62
8 10 4 23.94 22.98 0.38
9 10 4 2.28 0.00 2.68
-9 11 4 10.78 10.74 0.49
-8 11 4 4.98 8.08 0.83
-7 11 4 3.06 0.00 2.44
-6 11 4 20.48 22.86 0.39
-5 11 4 9.29 8.35 0.56
-4 11 4 6.03 5.17 0.75
-3 11 4 1.78 0.00 6.24
-2 11 4 3.13 0.00 2.61
-1 11 4 41.94 39.76 0.67
0 11 4 4.10 0.00 1.23
1 11 4 37.75 36.37 0.54
2 11 4 36.79 35.63 0.56
3 11 4 41.87 39.52 0.70
4 11 4 7.76 7.35 0.65
5 11 4 17.49 16.22 0.45
6 11 4 -1.68 0.00 5.89
7 11 4 20.46 19.39 0.35
8 11 4 3.25 0.00 2.79
-8 12 4 1.31 0.00 5.24
-7 12 4 14.54 16.43 0.41
-6 12 4 -1.89 0.00 1.89
-5 12 4 13.07 14.24 0.41
-4 12 4 -3.84 0.00 2.88
-3 12 4 22.14 22.03 0.45
-2 12 4 20.69 21.52 0.44
-1 12 4 10.48 10.14 0.45
0 12 4 2.53 0.00 4.43
1 12 4 20.23 19.36 0.40
2 12 4 12.76 11.95 0.50
3 12 4 17.53 17.10 0.53
4 12 4 9.65 9.72 0.60
5 12 4 -1.60 0.00 5.60
6 12 4 -1.47 0.00 6.63
7 12 4 2.71 0.00 1.62
-6 13 4 9.31 9.17 0.45
-5 13 4 -2.17 0.00 3.99
-4 13 4 22.41 23.47 0.34
-3 13 4 -2.59 0.00 3.45
-2 13 4 21.33 20.65 0.40
-1 13 4 6.09 6.84 0.87
0 13 4 8.90 8.79 0.61
1 13 4 8.59 8.48 0.64
2 13 4 20.38 20.05 0.39
3 13 4 0.00 0.00 0.00
4 13 4 6.78 6.66 0.65
5 13 4 15.29 16.13 0.47
6 13 4 9.27 7.61 0.53
-5 14 4 5.33 5.77 0.69
-4 14 4 7.13 7.06 0.52
-3 14 4 8.28 8.12 0.54
-2 14 4 11.10 11.18 0.47
-1 14 4 5.59 6.37 0.87
0 14 4 16.15 15.12 0.44
1 14 4 2.45 0.00 1.64
2 14 4 22.07 21.69 0.43
3 14 4 1.30 0.00 3.24
4 14 4 8.28 9.00 0.58
5 14 4 2.00 0.00 3.50
-2 15 4 -3.53 0.00 2.04
-1 15 4 19.01 19.30 0.33
0 15 4 2.68 0.00 2.68
1 15 4 15.57 15.31 0.41
2 15 4 2.46 0.00 3.07
-11 0 5 5.99 7.52 0.60
-9 0 5 36.94 34.39 0.55
-7 0 5 37.24 37.24 0.63
-5 0 5 6.04 6.49 0.48
-3 0 5 6.94 8.58 0.37
-1 0 5 44.93 47.56 0.51
1 0 5 121.97 121.61 0.53
3 0 5 76.67 93.31 0.53
5 0 5 107.67 111.21 0.63
7 0 5 59.65 60.03 0.82
9 0 5 15.79 14.28 0.42
11 0 5 10.54 10.33 0.51
-12 1 5 13.88 12.82 0.44
-11 1 5 29.53 29.00 0.44
-10 1 5 11.89 12.13 0.50
-9 1 5 16.90 15.38 0.49
-8 1 5 -4.41 0.00 2.58
-7 1 5 30.50 30.99 0.48
-6 1 5 5.20 6.61 0.68
-5 1 5 16.12 15.99 0.30
-4 1 5 64.59 67.82 0.64
-3 1 5 40.54 45.13 0.60
-2 1 5 7.82 7.95 0.36
-1 1 5 30.13 31.63 0.39
0 1 5 46.41 42.92 0.52
1 1 5 43.02 40.04 0.54
2 1 5 96.55 106.91 0.52
3 1 5 54.26 67.50 0.55
4 1 5 72.26 74.82 0.57
5 1 5 26.97 25.85 0.40
6 1 5 95.82 97.69 0.73
7 1 5 23.96 22.84 0.34
8 1 5 39.56 38.18 0.61
9 1 5 9.95 10.35 0.59
10 1 5 31.65 30.53 0.48
11 1 5 13.02 12.32 0.46
12 1 5 6.99 6.62 0.60
-12 2 5 21.44 22.49 0.37
-11 2 5 5.96 6.08 0.77
-10 2 5 33.62 33.89 0.50
-9 2 5 5.44 2.17 0.91
-8 2 5 30.98 32.11 0.49
-7 2 5 24.49 22.50 0.36
-6 2 5 51.60 51.53 0.58
-5 2 5 2.86 0.00 2.50
-4 2 5 67.07 71.77 0.66
-3 2 5 18.82 19.18 0.27
-2 2 5 80.97 81.48 0.57
-1 2 5 23.83 24.83 0.34
0 2 5 36.64 35.53 0.39
1 2 5 70.64 67.94 0.57
2 2 5 20.59 20.97 0.33
3 2 5 22.67 25.11 0.36
4 2 5 14.70 14.33 0.28
5 2 5 14.65 15.13 0.28
6 2 5 24.20 25.85 0.38
7 2 5 -4.48 0.00 1.96
8 2 5 17.97 17.27 0.39
9 2 5 2.78 0.00 3.17
10 2 5 -2.16 0.00 3.99
11 2 5 -2.91 0.00 2.51
12 2 5 4.03 0.00 0.99
-12 3 5 -0.90 0.00 6.69
-11 3 5 32.84 33.70 0.48
-10 3 5 14.41 14.61 0.51
-9 3 5 56.86 57.32 0.67
-8 3 5 11.31 12.24 0.57
-7 3 5 59.43 57.07 0.63
-6 3 5 36.28 35.00 0.61
-5 3 5 57.39 57.28 0.75
-4 3 5 47.89 47.72 0.70
-3 3 5 25.91 26.82 0.34
-2 3 5 14.49 14.41 0.24
-1 3 5 39.07 38.77 0.43
0 3 5 12.91 12.74 0.28
1 3 5 24.46 28.77 0.43
2 3 5 13.69 12.48 0.26
3 3 5 48.52 52.41 0.57
4 3 5 18.65 20.23 0.28
5 3 5 13.48 13.96 0.33
6 3 5 -4.45 0.00 1.98
7 3 5 2.29 0.00 4.01
8 3 5 20.03 19.62 0.37
9 3 5 17.40 16.97 0.43
10 3 5 -4.06 0.00 2.29
11 3 5 4.93 4.00 0.82
12 3 5 4.42 0.00 0.88
-12 4 5 12.25 12.88 0.40
-11 4 5 4.98 5.06 0.79
-10 4 5 17.26 18.03 0.49
-9 4 5 8.71 8.59 0.64
-8 4 5 14.85 14.44 0.43
-7 4 5 21.03 21.06 0.39
-6 4 5 26.04 25.30 0.37
-5 4 5 30.91 31.68 0.46
-4 4 5 48.02 47.63 0.51
-3 4 5 35.98 36.78 0.49
-2 4 5 45.01 45.19 0.65
-1 4 5 40.48 35.62 0.45
0 4 5 17.87 18.53 0.27
1 4 5 67.56 73.13 0.59
2 4 5 7.38 3.63 0.42
3 4 5 51.26 51.08 0.65
4 4 5 16.55 17.28 0.31
5 4 5 29.33 32.38 0.44
6 4 5 10.00 9.98 0.48
7 4 5 35.88 36.65 0.62
8 4 5 12.98 13.16 0.46
9 4 5 21.92 22.12 0.40
10 4 5 5.72 4.83 0.77
11 4 5 10.48 9.10 0.48
12 4 5 -3.36 0.00 1.82
-12 5 5 8.00 8.25 0.53
-11 5 5 10.35 10.90 0.55
-10 5 5 -4.33 0.00 2.59
-9 5 5 11.35 11.35 0.53
-8 5 5 3.54 0.00 1.33
-7 5 5 -3.18 0.00 3.18
-6 5 5 28.24 28.69 0.43
-5 5 5 27.36 27.05 0.42
-4 5 5 46.15 45.75 0.56
-3 5 5 33.42 31.07 0.54
-2 5 5 31.53 29.86 0.52
-1 5 5 6.20 5.60 0.54
0 5 5 14.42 15.19 0.28
1 5 5 24.95 24.63 0.38
2 5 5 87.14 85.12 0.68
3 5 5 19.92 18.14 0.29
4 5 5 73.59 76.25 0.71
5 5 5 19.97 20.91 0.34
6 5 5 51.73 53.27 0.58
7 5 5 7.49 6.73 0.59
8 5 5 52.53 52.83 0.67
9 5 5 13.27 14.03 0.43
10 5 5 18.20 18.20 0.43
11 5 5 19.53 18.87 0.40
-11 6 5 -4.25 0.00 2.04
-10 6 5 18.35 18.04 0.43
-9 6 5 4.14 0.00 1.03
-8 6 5 20.98 22.45 0.43
-7 6 5 1.74 0.00 2.61
-6 6 5 13.78 13.26 0.48
-5 6 5 4.42 0.00 0.95
-4 6 5 17.71 18.42 0.35
-3 6 5 30.01 30.40 0.45
-2 6 5 28.97 29.93 0.43
-1 6 5 54.61 54.55 0.71
0 6 5 21.98 21.99 0.34
1 6 5 20.45 21.96 0.28
2 6 5 37.30 39.24 0.50
3 6 5 45.69 46.43 0.53
4 6 5 20.42 19.41 0.33
5 6 5 49.79 51.49 0.58
6 6 5 10.98 11.39 0.39
7 6 5 46.47 46.19 0.67
8 6 5 8.60 8.39 0.54
9 6 5 14.57 14.77 0.47
10 6 5 9.93 10.18 0.53
11 6 5 9.03 8.11 0.54
-11 7 5 13.18 12.88 0.42
-10 7 5 2.20 0.00 2.92
-9 7 5 27.23 26.56 0.45
-8 7 5 -5.07 0.00 1.97
-7 7 5 37.15 38.40 0.53
-6 7 5 16.73 16.73 0.54
-5 7 5 25.15 24.19 0.41
-4 7 5 10.92 10.02 0.51
-3 7 5 60.27 63.37 0.82
-2 7 5 25.36 24.54 0.33
-1 7 5 21.99 21.15 0.35
0 7 5 2.56 0.00 3.42
1 7 5 66.08 62.83 0.76
2 7 5 24.27 24.99 0.34
3 7 5 66.86 65.07 0.83
4 7 5 4.72 0.00 0.89
5 7 5 20.67 19.00 0.34
6 7 5 19.27 19.73 0.40
7 7 5 24.03 22.04 0.40
8 7 5 7.87 8.22 0.56
9 7 5 8.06 9.06 0.66
10 7 5 2.83 0.00 1.42
11 7 5 25.00 25.29 0.37
-10 8 5 20.89 21.68 0.38
-9 8 5 7.73 7.65 0.58
-8 8 5 39.27 41.13 0.59
-7 8 5 16.85 14.85 0.43
-6 8 5 45.39 44.89 0.71
-5 8 5 20.54 20.23 0.42
-4 8 5 29.59 30.96 0.45
-3 8 5 6.05 7.12 0.70
-2 8 5 43.02 45.02 0.59
-1 8 5 34.19 34.51 0.49
0 8 5 6.60 7.45 0.58
1 8 5 1.62 0.00 1.62
2 8 5 2.34 0.00 4.68
3 8 5 14.44 13.41 0.40
4 8 5 13.25 12.35 0.47
5 8 5 11.21 10.78 0.55
6 8 5 9.97 10.99 0.48
7 8 5 12.78 13.21 0.49
8 8 5 9.59 9.65 0.56
9 8 5 6.32 5.65 0.71
10 8 5 4.82 0.00 1.34
-10 9 5 11.06 10.28 0.41
-9 9 5 17.70 18.15 0.42
-8 9 5 5.53 3.69 0.79
-7 9 5 19.98 20.68 0.39
-6 9 5 33.50 34.17 0.51
-5 9 5 23.06 23.51 0.43
-4 9 5 20.28 21.26 0.38
-3 9 5 24.44 24.66 0.37
-2 9 5 9.74 8.96 0.46
-1 9 5 37.51 38.79 0.51
0 9 5 34.07 35.10 0.52
1 9 5 12.80 11.59 0.47
2 9 5 12.38 12.54 0.38
3 9 5 3.12 0.00 1.56
4 9 5 31.98 29.87 0.48
5 9 5 8.32 7.24 0.62
6 9 5 14.82 15.35 0.43
7 9 5 7.01 6.95 0.82
8 9 5 35.50 34.39 0.49
9 9 5 4.26 0.00 1.03
10 9 5 6.68 7.08 0.68
-9 10 5 12.67 12.66 0.43
-8 10 5 6.56 6.26 0.66
-7 10 5 10.05 10.73 0.55
-6 10 5 12.12 13.76 0.53
-5 10 5 30.29 29.70 0.45
-4 10 5 9.47 9.29 0.51
-3 10 5 37.27 37.25 0.55
-2 10 5 15.04 15.64 0.42
-1 10 5 47.43 45.67 0.64
0 10 5 6.99 5.71 0.70
1 10 5 37.57 36.72 0.57
2 10 5 8.00 9.27 0.63
3 10 5 36.96 35.68 0.56
4 10 5 3.22 0.00 1.61
5 10 5 15.56 15.19 0.54
6 10 5 4.52 0.00 0.97
7 10 5 8.56 8.02 0.57
8 10 5 8.76 8.84 0.64
9 10 5 16.06 17.57 0.38
-8 11 5 -2.24 0.00 3.07
-7 11 5 2.93 0.00 2.64
-6 11 5 12.53 13.79 0.43
-5 11 5 11.92 12.40 0.52
-4 11 5 2.95 0.00 3.93
-3 11 5 5.55 3.65 0.83
-2 11 5 8.39 8.46 0.57
-1 11 5 7.24 6.86 0.68
0 11 5 23.56 23.90 0.42
1 11 5 12.95 12.38 0.52
2 11 5 18.13 16.55 0.46
3 11 5 20.10 18.58 0.42
4 11 5 38.09 36.32 0.68
5 11 5 14.11 15.18 0.53
6 11 5 18.01 16.76 0.40
7 11 5 5.68 5.25 0.84
8 11 5 23.27 22.26 0.34
-7 12 5 -3.62 0.00 1.98
-6 12 5 12.42 13.40 0.46
-5 12 5 2.46 0.00 3.27
-4 12 5 20.54 20.50 0.41
-3 12 5 6.51 6.04 0.81
-2 12 5 33.65 33.80 0.52
-1 12 5 24.97 24.15 0.42
0 12 5 27.90 27.12 0.44
1 12 5 7.45 7.29 0.83
2 12 5 14.69 13.70 0.52
3 12 5 2.96 0.00 1.48
4 12 5 3.29 0.00 1.65
5 12 5 3.07 0.00 1.54
6 12 5 1.97 0.00 2.47
7 12 5 -2.52 0.00 3.03
-6 13 5 5.76 6.58 0.63
-5 13 5 -3.57 0.00 2.38
-4 13 5 7.15 5.98 0.62
-3 13 5 27.62 27.38 0.41
-2 13 5 3.04 0.00 1.52
-1 13 5 21.22 20.61 0.41
0 13 5 7.31 6.84 0.70
1 13 5 10.93 10.52 0.58
2 13 5 18.05 17.19 0.41
3 13 5 17.15 16.56 0.40
4 13 5 1.99 0.00 1.99
5 13 5 11.16 10.31 0.50
6 13 5 16.10 15.38 0.44
-4 14 5 6.96 9.13 0.62
-3 14 5 -3.48 0.00 2.32
-2 14 5 12.43 12.83 0.45
-1 14 5 8.47 8.99 0.62
0 14 5 7.51 7.19 0.61
1 14 5 17.04 16.48 0.42
2 14 5 5.96 4.38 0.71
3 14 5 16.38 16.47 0.40
4 14 5 5.51 5.29 0.74
-1 15 5 2.18 0.00 3.26
0 15 5 14.79 14.40 0.40
1 15 5 1.68 0.00 3.92
-12 0 6 -1.65 0.00 4.54
-10 0 6 8.12 9.08 0.71
-8 0 6 13.60 14.73 0.49
-6 0 6 5.75 7.00 0.66
-4 0 6 36.05 36.74 0.50
-2 0 6 8.80 14.17 0.30
0 0 6 37.80 36.58 0.41
2 0 6 124.46 130.69 0.58
4 0 6 84.85 98.02 0.61
6 0 6 72.16 73.25 0.76
8 0 6 39.10 38.16 0.52
10 0 6 26.71 23.94 0.41
12 0 6 17.52 16.19 0.36
-12 1 6 15.60 15.39 0.39
-11 1 6 12.21 11.30 0.45
-10 1 6 22.11 22.59 0.47
-9 1 6 21.78 20.67 0.39
-8 1 6 -1.76 0.00 5.96
-7 1 6 10.72 10.50 0.42
-6 1 6 49.44 50.28 0.58
-5 1 6 10.69 11.05 0.40
-4 1 6 42.28 43.35 0.49
-3 1 6 8.90 13.21 0.35
-2 1 6 8.73 9.61 0.35
-1 1 6 28.75 32.77 0.42
0 1 6 41.38 43.21 0.59
1 1 6 129.76 119.85 0.60
2 1 6 152.76 155.77 0.57
3 1 6 110.09 121.86 0.61
4 1 6 8.23 7.28 0.36
5 1 6 30.59 33.26 0.49
6 1 6 12.38 10.80 0.36
7 1 6 61.71 59.14 0.85
8 1 6 3.20 0.00 2.98
9 1 6 8.11 8.46 0.63
10 1 6 3.92 0.00 1.14
11 1 6 15.09 14.31 0.40
12 1 6 8.21 8.69 0.56
-12 2 6 -3.80 0.00 1.56
-11 2 6 25.96 26.76 0.38
-10 2 6 12.01 10.89 0.55
-9 2 6 36.36 34.99 0.51
-8 2 6 24.34 23.38 0.42
-7 2 6 55.97 53.20 0.65
-6 2 6 17.85 17.53 0.38
-5 2 6 42.27 44.45 0.56
-4 2 6 31.55 30.09 0.52
-3 2 6 14.89 15.73 0.28
-2 2 6 10.12 8.91 0.29
-1 2 6 56.76 57.07 0.61
0 2 6 65.70 65.43 0.59
1 2 6 83.95 80.42 0.62
2 2 6 49.42 50.64 0.59
3 2 6 1.19 0.00 5.95
4 2 6 13.89 15.42 0.28
5 2 6 13.27 15.81 0.35
6 2 6 13.82 15.81 0.33
7 2 6 6.88 7.14 0.57
8 2 6 8.76 7.99 0.51
9 2 6 12.70 12.33 0.45
10 2 6 -3.39 0.00 2.40
11 2 6 7.63 6.36 0.54
12 2 6 6.08 5.36 0.65
-12 3 6 18.36 18.44 0.34
-11 3 6 -3.21 0.00 1.97
-10 3 6 27.70 27.58 0.40
-9 3 6 6.55 0.00 1.58
-8 3 6 20.58 20.53 0.43
-7 3 6 31.60 31.89 0.51
-6 3 6 55.96 54.85 0.60
-5 3 6 26.75 25.70 0.36
-4 3 6 84.62 82.35 0.73
-3 3 6 14.63 13.76 0.31
-2 3 6 22.08 26.50 0.33
-1 3 6 18.02 18.66 0.25
0 3 6 61.59 64.56 0.62
1 3 6 7.77 5.85 0.44
2 3 6 18.99 16.63 0.30
3 3 6 6.99 6.04 0.44
4 3 6 4.35 5.03 0.59
5 3 6 19.38 22.06 0.31
6 3 6 -5.77 0.00 1.44
7 3 6 11.71 10.91 0.47
8 3 6 -3.00 0.00 3.50
9 3 6 17.74 16.83 0.41
10 3 6 4.28 0.00 1.15
11 3 6 2.08 0.00 3.68
12 3 6 4.91 0.00 0.93
-12 4 6 9.86 9.58 0.47
-11 4 6 21.93 21.37 0.35
-10 4 6 13.92 13.69 0.46
-9 4 6 11.49 10.93 0.53
-8 4 6 5.91 6.38 0.89
-7 4 6 27.52 29.17 0.49
-6 4 6 34.87 34.62 0.50
-5 4 6 55.33 52.71 0.81
-4 4 6 12.69 12.05 0.35
-3 4 6 5.97 3.77 0.50
-2 4 6 20.85 20.68 0.30
-1 4 6 4.67 5.66 0.54
0 4 6 86.98 86.03 0.65
1 4 6 82.12 72.85 0.69
2 4 6 58.33 54.35 0.70
3 4 6 5.21 5.58 0.49
4 4 6 33.50 37.86 0.51
5 4 6 8.41 8.32 0.39
6 4 6 42.18 46.30 0.58
7 4 6 6.58 5.00 0.66
8 4 6 29.84 28.16 0.41
9 4 6 6.01 0.00 1.44
10 4 6 9.28 10.21 0.64
11 4 6 4.24 0.00 1.60
-11 5 6 8.05 6.84 0.64
-10 5 6 -3.22 0.00 2.50
-9 5 6 7.73 7.12 0.75
-8 5 6 32.17 33.08 0.49
-7 5 6 3.21 0.00 3.21
-6 5 6 14.49 14.59 0.42
-5 5 6 10.73 10.79 0.51
-4 5 6 6.44 6.86 0.57
-3 5 6 21.84 21.21 0.30
-2 5 6 14.63 13.91 0.35
-1 5 6 18.84 22.28 0.30
0 5 6 13.83 11.07 0.33
1 5 6 52.16 49.87 0.69
2 5 6 29.47 27.60 0.46
3 5 6 60.78 62.50 0.70
4 5 6 5.09 2.67 0.64
5 5 6 59.26 63.65 0.80
6 5 6 16.28 16.10 0.34
7 5 6 40.90 41.10 0.67
8 5 6 3.52 0.00 1.32
9 5 6 20.01 20.30 0.47
10 5 6 10.25 9.59 0.52
11 5 6 20.97 20.04 0.38
-11 6 6 12.42 12.80 0.48
-10 6 6 3.40 0.00 1.22
-9 6 6 22.13 22.18 0.43
-8 6 6 11.85 12.46 0.50
-7 6 6 14.76 12.91 0.48
-6 6 6 7.33 7.98 0.65
-5 6 6 16.97 18.28 0.43
-4 6 6 9.82 10.54 0.41
-3 6 6 24.14 22.79 0.36
-2 6 6 26.78 27.24 0.38
-1 6 6 50.93 47.53 0.53
0 6 6 2.50 0.00 1.25
1 6 6 55.56 55.66 0.74
2 6 6 46.26 44.36 0.56
3 6 6 49.51 46.09 0.57
4 6 6 55.65 58.67 0.81
5 6 6 7.72 6.66 0.53
6 6 6 58.82 59.38 0.63
7 6 6 2.50 0.00 5.63
8 6 6 13.72 13.73 0.44
9 6 6 8.58 9.39 0.65
10 6 6 13.20 11.65 0.43
11 6 6 15.71 16.27 0.38
-11 7 6 7.48 6.86 0.61
-10 7 6 24.69 24.71 0.39
-9 7 6 4.57 0.00 1.81
-8 7 6 27.95 30.33 0.44
-7 7 6 10.05 9.76 0.54
-6 7 6 39.02 39.22 0.61
-5 7 6 2.49 0.00 1.87
-4 7 6 50.60 50.61 0.63
-3 7 6 2.85 0.00 2.85
-2 7 6 56.83 58.17 0.83
-1 7 6 15.11 15.49 0.32
0 7 6 38.71 38.87 0.56
1 7 6 27.31 26.95 0.45
2 7 6 52.36 51.11 0.59
3 7 6 9.77 9.62 0.43
4 7 6 22.56 21.40 0.37
5 7 6 -1.72 0.00 6.02
6 7 6 4.34 0.00 1.09
7 7 6 20.42 20.58 0.46
8 7 6 13.22 12.56 0.43
9 7 6 -1.72 0.00 4.24
10 7 6 6.68 7.43 0.73
-10 8 6 3.69 0.00 2.07
-9 8 6 31.51 31.84 0.51
-8 8 6 7.29 7.38 0.66
-7 8 6 27.27 29.46 0.41
-6 8 6 34.09 35.09 0.61
-5 8 6 25.20 26.13 0.38
-4 8 6 26.38 26.92 0.41
-3 8 6 2.43 0.00 3.64
-2 8 6 19.66 20.39 0.36
-1 8 6 42.40 42.09 0.61
0 8 6 2.86 0.00 3.82
1 8 6 37.63 36.87 0.63
2 8 6 -1.71 0.00 1.71
3 8 6 20.89 19.93 0.38
4 8 6 -3.01 0.00 4.51
5 8 6 12.77 11.94 0.49
6 8 6 21.02 20.54 0.46
7 8 6 3.50 0.00 3.50
8 8 6 26.56 27.62 0.43
9 8 6 12.03 12.66 0.47
10 8 6 -4.09 0.00 1.91
-10 9 6 5.76 4.88 0.68
-9 9 6 9.12 9.36 0.54
-8 9 6 22.12 22.98 0.36
-7 9 6 11.83 13.04 0.52
-6 9 6 30.07 31.58 0.46
-5 9 6 20.42 20.95 0.40
-4 9 6 44.63 45.24 0.63
-3 9 6 26.19 26.06 0.41
-2 9 6 20.63 21.41 0.37
-1 9 6 43.77 43.22 0.66
0 9 6 21.59 20.85 0.43
1 9 6 23.45 23.69 0.40
2 9 6 3.12 0.00 3.12
3 9 6 18.73 16.92 0.45
4 9 6 3.21 0.00 1.60
5 9 6 24.46 25.38 0.39
6 9 6 7.01 5.97 0.66
7 9 6 7.40 6.54 0.74
8 9 6 0.00 0.00 0.00
9 9 6 13.93 13.69 0.43
-9 10 6 5.83 4.65 0.69
-8 10 6 11.17 11.64 0.42
-7 10 6 -4.71 0.00 1.71
-6 10 6 17.57 17.85 0.44
-5 10 6 -3.82 0.00 2.67
-4 10 6 -4.25 0.00 2.48
-3 10 6 7.70 7.22 0.61
-2 10 6 23.07 23.78 0.41
-1 10 6 5.69 4.56 0.85
0 10 6 20.83 21.47 0.39
1 10 6 2.58 0.00 1.94
2 10 6 7.11 5.82 0.71
3 10 6 8.83 8.75 0.58
4 10 6 43.71 41.22 0.69
5 10 6 14.67 14.71 0.51
6 10 6 33.36 32.92 0.54
7 10 6 5.62 4.94 0.80
8 10 6 18.37 18.12 0.41
9 10 6 2.55 0.00 2.11
-8 11 6 11.47 11.21 0.38
-7 11 6 4.30 0.00 0.90
-6 11 6 8.41 8.11 0.47
-5 11 6 -5.40 0.00 1.80
-4 11 6 29.08 31.12 0.42
-3 11 6 -4.53 0.00 2.27
-2 11 6 16.40 16.73 0.47
-1 11 6 32.15 31.09 0.50
0 11 6 12.36 11.05 0.53
1 11 6 18.07 18.49 0.45
2 11 6 -4.02 0.00 1.21
3 11 6 10.09 8.91 0.63
4 11 6 13.55 12.97 0.56
5 11 6 15.63 14.15 0.53
6 11 6 13.70 14.24 0.48
7 11 6 12.19 12.90 0.48
8 11 6 1.04 0.00 7.30
-7 12 6 13.99 14.67 0.36
-6 12 6 -2.40 0.00 3.00
-5 12 6 12.67 12.97 0.44
-4 12 6 5.90 6.85 0.74
-3 12 6 29.29 29.21 0.43
-2 12 6 14.23 14.03 0.47
-1 12 6 31.27 29.52 0.45
0 12 6 12.16 12.99 0.48
1 12 6 27.26 26.72 0.43
2 12 6 7.72 6.87 0.74
3 12 6 20.59 19.84 0.46
4 12 6 16.56 15.23 0.44
5 12 6 -2.90 0.00 3.62
6 12 6 6.20 6.64 0.74
7 12 6 2.49 0.00 2.70
-6 13 6 13.86 14.96 0.40
-5 13 6 7.08 6.74 0.60
-4 13 6 12.46 13.87 0.44
-3 13 6 -1.37 0.00 6.17
-2 13 6 24.43 24.44 0.38
-1 13 6 3.34 0.00 2.67
0 13 6 15.12 13.87 0.46
1 13 6 14.87 15.01 0.46
2 13 6 8.66 8.08 0.64
3 13 6 6.98 5.52 0.73
4 13 6 6.85 6.36 0.63
5 13 6 9.82 9.63 0.48
-4 14 6 7.13 6.82 0.55
-3 14 6 6.47 7.77 0.61
-2 14 6 5.65 4.97 0.74
-1 14 6 9.70 10.37 0.55
0 14 6 10.58 10.10 0.45
1 14 6 5.29 5.16 0.74
2 14 6 11.89 12.07 0.42
3 14 6 1.11 0.00 7.19
4 14 6 13.17 12.34 0.42
-11 0 7 24.56 24.81 0.36
-9 0 7 13.54 14.05 0.49
-7 0 7 29.31 30.31 0.43
-5 0 7 22.03 23.05 0.39
-3 0 7 7.54 8.08 0.47
-1 0 7 47.05 48.22 0.65
1 0 7 142.99 138.41 0.60
3 0 7 2.28 0.00 3.42
5 0 7 29.32 35.07 0.53
7 0 7 54.91 54.57 0.61
9 0 7 10.73 11.19 0.52
11 0 7 21.64 20.14 0.39
-12 1 7 3.65 0.00 1.53
-11 1 7 20.17 20.17 0.38
-10 1 7 17.67 16.46 0.49
-9 1 7 18.62 17.55 0.45
-8 1 7 16.98 16.25 0.45
-7 1 7 25.16 25.26 0.38
-6 1 7 18.69 17.50 0.38
-5 1 7 14.38 15.33 0.34
-4 1 7 4.45 1.34 0.70
-3 1 7 38.83 36.78 0.49
-2 1 7 38.77 35.45 0.47
-1 1 7 50.89 51.77 0.64
0 1 7 95.34 88.81 0.65
1 1 7 36.54 38.97 0.45
2 1 7 113.71 112.85 0.63
3 1 7 49.75 50.47 0.69
4 1 7 43.26 50.08 0.50
5 1 7 12.63 13.38 0.35
6 1 7 46.34 46.31 0.56
7 1 7 -2.05 0.00 4.06
8 1 7 31.21 30.04 0.43
9 1 7 4.49 0.00 1.48
10 1 7 15.00 13.83 0.47
11 1 7 1.81 0.00 4.38
12 1 7 10.03 8.74 0.52
-12 2 7 12.73 12.65 0.37
-11 2 7 11.76 10.34 0.42
-10 2 7 35.46 34.31 0.53
-9 2 7 30.55 30.21 0.46
-8 2 7 28.49 27.28 0.43
-7 2 7 21.49 21.29 0.39
-6 2 7 69.82 70.08 0.86
-5 2 7 2.75 0.00 3.21
-4 2 7 65.06 66.38 0.76
-3 2 7 76.11 73.67 0.70
-2 2 7 20.05 21.09 0.31
-1 2 7 44.15 43.41 0.65
0 2 7 93.78 86.04 0.66
1 2 7 96.09 93.76 0.63
2 2 7 81.93 83.32 0.64
3 2 7 23.59 23.84 0.36
4 2 7 18.88 19.12 0.29
5 2 7 7.83 8.45 0.40
6 2 7 12.89 13.11 0.38
7 2 7 -4.07 0.00 2.72
8 2 7 22.03 21.73 0.40
9 2 7 2.52 0.00 3.54
10 2 7 7.32 6.91 0.69
11 2 7 9.81 9.11 0.50
12 2 7 9.86 10.14 0.49
-12 3 7 1.90 0.00 3.26
-11 3 7 23.29 22.84 0.40
-10 3 7 -2.58 0.00 3.26
-9 3 7 40.20 38.32 0.61
-8 3 7 -3.74 0.00 3.27
-7 3 7 21.04 21.62 0.40
-6 3 7 35.49 35.14 0.55
-5 3 7 56.96 57.17 0.83
-4 3 7 3.04 0.00 2.28
-3 3 7 87.53 86.84 0.73
-2 3 7 20.73 18.89 0.32
-1 3 7 69.79 67.97 0.68
0 3 7 25.23 21.84 0.45
1 3 7 48.60 46.47 0.73
2 3 7 19.35 20.27 0.31
3 3 7 52.91 56.99 0.68
4 3 7 10.14 9.99 0.39
5 3 7 6.72 6.93 0.50
6 3 7 10.94 11.17 0.48
7 3 7 10.85 9.79 0.53
8 3 7 13.29 12.07 0.45
9 3 7 5.05 0.00 1.56
10 3 7 -3.94 0.00 2.42
11 3 7 1.80 0.00 3.62
-11 4 7 9.36 8.43 0.54
-10 4 7 16.62 16.58 0.42
-9 4 7 28.08 29.25 0.43
-8 4 7 9.46 9.94 0.55
-7 4 7 3.67 0.00 3.67
-6 4 7 34.66 34.93 0.53
-5 4 7 12.00 10.96 0.46
-4 4 7 42.62 43.88 0.58
-3 4 7 14.61 11.76 0.38
-2 4 7 13.72 14.68 0.37
-1 4 7 62.56 60.62 0.71
0 4 7 12.11 13.05 0.39
1 4 7 94.65 82.05 0.75
2 4 7 61.68 63.70 0.69
3 4 7 41.09 43.02 0.50
4 4 7 2.08 0.00 1.56
5 4 7 43.52 46.17 0.56
6 4 7 16.74 17.40 0.41
7 4 7 39.17 39.97 0.54
8 4 7 22.33 21.24 0.41
9 4 7 16.06 16.51 0.51
10 4 7 7.53 6.93 0.56
11 4 7 3.12 0.00 2.15
-11 5 7 7.27 7.65 0.57
-10 5 7 3.49 0.00 0.87
-9 5 7 -2.84 0.00 3.79
-8 5 7 0.00 0.00 0.00
-7 5 7 4.08 0.00 0.82
-6 5 7 15.20 13.99 0.42
-5 5 7 9.37 9.26 0.47
-4 5 7 1.63 0.00 2.44
-3 5 7 59.39 56.06 0.80
-2 5 7 9.40 7.61 0.36
-1 5 7 8.44 6.51 0.38
0 5 7 30.96 33.13 0.54
1 5 7 2.16 0.00 4.32
2 5 7 29.26 32.08 0.46
3 5 7 5.54 2.85 0.59
4 5 7 58.11 61.85 0.79
5 5 7 6.92 7.73 0.58
6 5 7 37.89 38.03 0.50
7 5 7 37.44 36.31 0.54
8 5 7 29.76 28.90 0.41
9 5 7 1.96 0.00 3.74
10 5 7 15.45 15.58 0.43
11 5 7 -2.35 0.00 3.07
-11 6 7 10.94 10.65 0.43
-10 6 7 18.52 19.58 0.37
-9 6 7 16.86 17.26 0.45
-8 6 7 19.56 19.44 0.42
-7 6 7 0.00 0.00 0.00
-6 6 7 7.41 7.92 0.65
-5 6 7 16.28 16.29 0.38
-4 6 7 56.69 55.01 0.61
-3 6 7 29.02 26.12 0.41
-2 6 7 20.95 21.53 0.36
-1 6 7 32.74 32.38 0.48
0 6 7 7.49 7.80 0.47
1 6 7 60.53 55.46 0.82
2 6 7 13.15 12.33 0.40
3 6 7 47.48 48.42 0.57
4 6 7 25.03 26.08 0.37
5 6 7 27.87 27.47 0.42
6 6 7 25.80 25.36 0.42
7 6 7 26.93 26.28 0.46
8 6 7 8.89 8.74 0.66
9 6 7 17.62 18.01 0.43
10 6 7 4.84 0.00 0.96
11 6 7 11.18 10.80 0.48
-10 7 7 11.39 11.24 0.47
-9 7 7 22.12 22.61 0.40
-8 7 7 8.37 9.16 0.62
-7 7 7 9.74 8.74 0.54
-6 7 7 1.79 0.00 6.27
-5 7 7 11.96 11.36 0.53
-4 7 7 37.46 37.98 0.53
-3 7 7 35.36 33.54 0.53
-2 7 7 3.32 0.00 1.24
-1 7 7 58.17 59.12 0.84
0 7 7 5.60 5.60 0.70
1 7 7 74.94 72.04 0.83
2 7 7 33.83 31.33 0.51
3 7 7 60.03 60.34 0.85
4 7 7 18.16 18.07 0.40
5 7 7 4.65 0.00 1.00
6 7 7 20.01 20.00 0.40
7 7 7 13.92 15.00 0.44
8 7 7 11.17 10.22 0.49
9 7 7 3.19 0.00 2.55
10 7 7 10.47 11.55 0.49
-10 8 7 17.97 18.26 0.35
-9 8 7 -3.95 0.00 2.46
-8 8 7 30.10 33.47 0.41
-7 8 7 2.46 0.00 1.84
-6 8 7 47.51 48.92 0.67
-5 8 7 43.35 44.02 0.65
-4 8 7 68.85 70.63 0.91
-3 8 7 25.23 24.37 0.36
-2 8 7 24.00 22.36 0.37
-1 8 7 7.24 7.63 0.60
0 8 7 35.93 34.60 0.65
1 8 7 -2.98 0.00 3.48
2 8 7 16.58 16.31 0.38
3 8 7 20.15 21.20 0.41
4 8 7 -1.77 0.00 5.30
5 8 7 3.98 0.00 0.80
6 8 7 15.09 14.99 0.41
7 8 7 -1.70 0.00 5.94
8 8 7 8.54 9.22 0.55
9 8 7 11.52 11.24 0.51
10 8 7 -4.06 0.00 1.79
-9 9 7 15.75 15.56 0.40
-8 9 7 4.05 0.00 0.90
-7 9 7 4.70 0.00 1.04
-6 9 7 14.93 15.96 0.48
-5 9 7 8.45 8.79 0.53
-4 9 7 13.48 13.99 0.46
-3 9 7 33.35 32.33 0.47
-2 9 7 7.29 6.80 0.64
-1 9 7 24.71 24.52 0.38
0 9 7 29.57 28.01 0.48
1 9 7 15.24 14.00 0.42
2 9 7 19.85 18.67 0.42
3 9 7 32.61 31.61 0.52
4 9 7 41.30 40.72 0.65
5 9 7 21.24 20.57 0.44
6 9 7 38.68 36.45 0.53
7 9 7 11.78 10.89 0.54
8 9 7 18.24 17.18 0.42
9 9 7 4.10 0.00 1.68
-9 10 7 11.00 10.31 0.45
-8 10 7 -2.34 0.00 3.51
-7 10 7 0.00 0.00 0.00
-6 10 7 -4.35 0.00 2.18
-5 10 7 6.90 6.99 0.58
-4 10 7 4.16 0.00 1.04
-3 10 7 8.70 9.65 0.52
-2 10 7 20.43 21.16 0.38
-1 10 7 49.78 47.52 0.65
0 10 7 -2.56 0.00 4.48
1 10 7 17.64 16.90 0.47
2 10 7 8.73 10.18 0.76
3 10 7 9.08 9.58 0.73
4 10 7 -3.00 0.00 3.00
5 10 7 29.97 28.51 0.42
6 10 7 3.55 0.00 2.84
7 10 7 14.28 14.28 0.42
8 10 7 1.67 0.00 4.59
-8 11 7 7.65 7.70 0.57
-7 11 7 9.11 10.03 0.44
-6 11 7 8.92 9.50 0.51
-5 11 7 20.05 20.51 0.38
-4 11 7 1.59 0.00 6.34
-3 11 7 29.01 28.97 0.47
-2 11 7 18.26 19.48 0.48
-1 11 7 2.47 0.00 5.55
0 11 7 7.06 7.52 0.66
1 11 7 16.48 15.22 0.47
2 11 7 14.55 14.07 0.53
3 11 7 12.86 11.59 0.57
4 11 7 29.02 27.35 0.47
5 11 7 10.70 10.38 0.55
6 11 7 17.82 18.37 0.43
7 11 7 7.09 6.81 0.69
-7 12 7 -1.27 0.00 4.78
-6 12 7 18.59 20.52 0.36
-5 12 7 10.54 10.84 0.46
-4 12 7 23.16 23.69 0.34
-3 12 7 9.62 10.47 0.59
-2 12 7 21.84 23.23 0.39
-1 12 7 20.05 20.26 0.45
0 12 7 18.11 16.65 0.44
1 12 7 3.26 0.00 1.63
2 12 7 23.97 23.53 0.38
3 12 7 -5.17 0.00 2.12
4 12 7 5.46 4.51 0.78
5 12 7 3.69 0.00 1.15
6 12 7 2.51 0.00 2.76
-5 13 7 11.82 12.99 0.38
-4 13 7 -2.61 0.00 3.14
-3 13 7 14.38 15.28 0.40
-2 13 7 5.23 5.17 0.87
-1 13 7 17.81 17.03 0.38
0 13 7 6.21 6.36 0.82
1 13 7 19.13 17.95 0.37
2 13 7 12.33 12.12 0.55
3 13 7 9.14 9.34 0.57
4 13 7 2.91 0.00 2.67
5 13 7 7.27 5.67 0.58
-3 14 7 7.55 7.42 0.62
-2 14 7 14.02 14.63 0.40
-1 14 7 7.25 7.17 0.52
0 14 7 6.04 5.19 0.65
1 14 7 14.84 14.13 0.39
2 14 7 2.84 0.00 2.43
3 14 7 10.61 10.62 0.48
-12 0 8 1.32 0.00 5.27
-10 0 8 9.80 9.85 0.53
-8 0 8 11.84 11.52 0.58
-6 0 8 14.29 14.69 0.43
-4 0 8 3.09 0.00 3.09
-2 0 8 38.47 37.50 0.51
0 0 8 69.58 70.45 0.65
2 0 8 145.11 145.39 0.69
4 0 8 38.57 42.34 0.54
6 0 8 32.89 36.25 0.49
8 0 8 31.20 30.52 0.46
10 0 8 12.87 12.46 0.48
-12 1 8 2.44 0.00 1.98
-11 1 8 16.43 15.99 0.45
-10 1 8 31.38 30.40 0.48
-9 1 8 5.19 0.00 0.92
-8 1 8 28.36 27.06 0.45
-7 1 8 5.01 0.00 1.00
-6 1 8 8.56 9.41 0.54
-5 1 8 2.63 0.00 3.18
-4 1 8 23.38 24.11 0.36
-3 1 8 64.96 64.74 0.74
-2 1 8 56.41 60.09 0.71
-1 1 8 21.71 20.00 0.29
0 1 8 12.77 11.79 0.33
1 1 8 4.58 6.65 0.57
2 1 8 9.80 10.46 0.38
3 1 8 6.69 7.19 0.56
4 1 8 31.44 35.19 0.47
5 1 8 8.35 8.67 0.42
6 1 8 23.55 23.91 0.32
7 1 8 29.08 29.74 0.48
8 1 8 4.34 0.00 2.25
9 1 8 27.40 25.71 0.41
10 1 8 -3.46 0.00 2.34
11 1 8 19.55 19.01 0.37
-12 2 8 8.32 8.83 0.51
-11 2 8 20.91 19.79 0.41
-10 2 8 12.66 12.13 0.49
-9 2 8 22.20 21.74 0.42
-8 2 8 30.11 31.00 0.52
-7 2 8 0.00 0.00 0.00
-6 2 8 14.69 13.82 0.43
-5 2 8 56.72 54.70 0.59
-4 2 8 3.52 0.00 1.06
-3 2 8 116.38 117.07 0.75
-2 2 8 68.50 63.50 0.72
-1 2 8 75.05 72.35 0.72
0 2 8 13.88 13.86 0.32
1 2 8 76.55 76.82 0.69
2 2 8 85.70 83.09 0.71
3 2 8 67.61 72.06 0.72
4 2 8 6.28 5.53 0.52
5 2 8 4.08 0.00 0.87
6 2 8 4.33 0.00 0.93
7 2 8 4.81 0.00 0.90
8 2 8 4.52 0.00 0.97
9 2 8 -0.98 0.00 9.57
10 2 8 -2.84 0.00 3.21
11 2 8 3.98 0.00 0.87
-11 3 8 1.76 0.00 3.49
-10 3 8 23.62 23.17 0.40
-9 3 8 13.79 14.04 0.54
-8 3 8 43.25 40.05 0.71
-7 3 8 24.38 22.64 0.43
-6 3 8 30.79 31.72 0.47
-5 3 8 8.31 7.31 0.52
-4 3 8 77.26 77.52 0.82
-3 3 8 18.56 19.54 0.32
-2 3 8 41.44 41.44 0.55
-1 3 8 25.48 24.61 0.39
0 3 8 56.72 52.15 0.76
1 3 8 43.34 43.77 0.51
2 3 8 33.99 34.66 0.53
3 3 8 16.96 17.83 0.31
4 3 8 27.58 29.28 0.41
5 3 8 22.62 23.44 0.33
6 3 8 28.87 29.14 0.44
7 3 8 9.47 7.59 0.47
8 3 8 8.93 9.23 0.66
9 3 8 -0.20 0.00 49.60
10 3 8 7.71 7.79 0.58
11 3 8 -3.42 0.00 2.09
-11 4 8 6.55 7.29 0.61
-10 4 8 3.60 0.00 1.20
-9 4 8 26.64 26.77 0.43
-8 4 8 23.69 23.45 0.42
-7 4 8 -5.23 0.00 1.96
-6 4 8 6.23 5.09 0.78
-5 4 8 20.44 21.11 0.37
-4 4 8 8.58 7.92 0.48
-3 4 8 59.50 58.79 0.82
-2 4 8 23.13 22.40 0.35
-1 4 8 47.52 47.55 0.54
0 4 8 23.77 22.47 0.37
1 4 8 46.67 47.20 0.53
2 4 8 70.80 72.46 0.74
3 4 8 35.85 36.35 0.57
4 4 8 48.24 48.60 0.58
5 4 8 23.16 25.01 0.35
6 4 8 25.62 27.39 0.40
7 4 8 11.32 11.49 0.54
8 4 8 19.26 18.56 0.38
9 4 8 13.93 13.76 0.46
10 4 8 9.49 8.67 0.48
11 4 8 3.08 0.00 1.20
-11 5 8 10.18 11.00 0.44
-10 5 8 5.27 6.02 0.70
-9 5 8 11.85 10.33 0.45
-8 5 8 0.00 0.00 0.00
-7 5 8 4.83 0.00 1.03
-6 5 8 6.99 6.34 0.70
-5 5 8 3.93 0.00 1.18
-4 5 8 18.75 17.82 0.38
-3 5 8 19.29 19.45 0.35
-2 5 8 19.02 17.22 0.33
-1 5 8 26.37 23.29 0.37
0 5 8 21.69 20.96 0.38
1 5 8 63.08 60.84 0.82
2 5 8 16.13 16.49 0.36
3 5 8 37.67 37.58 0.59
4 5 8 3.26 0.00 1.22
5 5 8 26.89 25.92 0.43
6 5 8 40.47 40.34 0.65
7 5 8 35.21 34.99 0.57
8 5 8 0.00 0.00 0.00
9 5 8 13.37 13.14 0.44
10 5 8 12.34 13.50 0.47
11 5 8 13.98 12.94 0.42
-11 6 8 18.51 18.44 0.36
-10 6 8 4.05 0.00 1.58
-9 6 8 14.00 13.54 0.48
-8 6 8 -3.95 0.00 2.77
-7 6 8 10.69 11.43 0.59
-6 6 8 1.80 0.00 2.70
-5 6 8 13.96 14.02 0.46
-4 6 8 6.29 6.78 0.73
-3 6 8 47.77 45.48 0.63
-2 6 8 13.04 13.25 0.42
-1 6 8 15.19 15.75 0.35
0 6 8 24.75 25.22 0.37
1 6 8 44.56 40.63 0.60
2 6 8 55.99 56.10 0.83
3 6 8 20.73 21.48 0.33
4 6 8 -3.40 0.00 2.97
5 6 8 17.09 18.14 0.44
6 6 8 26.33 25.77 0.42
7 6 8 21.12 20.00 0.43
8 6 8 39.71 38.34 0.65
9 6 8 16.24 16.18 0.42
10 6 8 7.05 6.82 0.59
-10 7 8 17.46 17.84 0.36
-9 7 8 5.30 4.38 0.73
-8 7 8 20.90 20.28 0.46
-7 7 8 5.40 5.26 0.81
-6 7 8 26.19 25.57 0.42
-5 7 8 15.80 17.14 0.51
-4 7 8 35.69 35.95 0.53
-3 7 8 27.36 28.05 0.44
-2 7 8 53.64 53.72 0.63
-1 7 8 2.93 0.00 2.93
0 7 8 31.44 30.00 0.45
1 7 8 19.69 18.51 0.39
2 7 8 28.31 28.22 0.40
3 7 8 2.98 0.00 3.48
4 7 8 13.33 14.53 0.46
5 7 8 3.97 0.00 3.18
6 7 8 11.86 10.37 0.53
7 7 8 -1.70 0.00 2.56
8 7 8 6.85 6.74 0.72
9 7 8 -0.96 0.00 3.34
10 7 8 0.85 0.00 8.12
-10 8 8 5.71 5.74 0.76
-9 8 8 20.21 19.05 0.39
-8 8 8 2.92 0.00 2.92
-7 8 8 23.50 23.19 0.40
-6 8 8 -4.15 0.00 2.42
-5 8 8 27.77 27.62 0.44
-4 8 8 -3.54 0.00 3.09
-3 8 8 58.51 58.35 0.64
-2 8 8 26.94 27.57 0.46
-1 8 8 36.75 36.15 0.54
0 8 8 23.62 23.18 0.39
1 8 8 48.52 45.39 0.67
2 8 8 4.05 0.00 1.22
3 8 8 13.57 13.14 0.46
4 8 8 29.65 28.33 0.43
5 8 8 4.33 0.00 1.08
6 8 8 3.45 0.00 3.45
7 8 8 8.45 7.32 0.63
8 8 8 1.44 0.00 6.49
9 8 8 5.20 6.38 0.80
-9 9 8 12.92 14.13 0.39
-8 9 8 13.66 14.89 0.41
-7 9 8 12.74 12.79 0.42
-6 9 8 9.75 9.70 0.51
-5 9 8 15.53 15.07 0.45
-4 9 8 13.48 13.72 0.44
-3 9 8 16.25 16.10 0.47
-2 9 8 14.57 14.61 0.43
-1 9 8 7.55 7.05 0.63
0 9 8 28.42 27.04 0.45
1 9 8 32.74 32.71 0.50
2 9 8 16.93 16.12 0.49
3 9 8 24.62 23.78 0.38
4 9 8 7.65 7.94 0.60
5 9 8 13.47 12.87 0.54
6 9 8 3.65 0.00 3.29
7 9 8 13.96 13.99 0.48
8 9 8 7.38 5.77 0.65
9 9 8 15.08 15.69 0.40
-8 10 8 13.95 14.24 0.36
-7 10 8 -2.55 0.00 3.19
-6 10 8 -1.43 0.00 5.73
-5 10 8 4.66 0.00 1.04
-4 10 8 -2.84 0.00 3.79
-3 10 8 9.44 10.02 0.61
-2 10 8 7.36 8.08 0.61
-1 10 8 9.18 8.89 0.51
0 10 8 31.29 30.30 0.51
1 10 8 3.59 0.00 1.35
2 10 8 30.03 29.03 0.42
3 10 8 6.36 4.04 0.73
4 10 8 36.92 36.62 0.68
5 10 8 7.14 8.65 0.71
6 10 8 25.00 23.31 0.40
7 10 8 6.49 6.41 0.65
8 10 8 14.98 14.90 0.43
-7 11 8 6.75 7.80 0.56
-6 11 8 12.80 12.99 0.42
-5 11 8 8.12 8.60 0.48
-4 11 8 26.39 26.73 0.39
-3 11 8 -3.88 0.00 2.26
-2 11 8 24.01 24.34 0.39
-1 11 8 2.38 0.00 4.75
0 11 8 -4.17 0.00 2.78
1 11 8 5.90 5.16 0.74
2 11 8 7.71 6.82 0.55
3 11 8 14.50 14.37 0.46
4 11 8 3.04 0.00 3.81
5 11 8 22.24 21.76 0.36
6 11 8 7.30 5.36 0.55
7 11 8 9.05 8.70 0.54
-6 12 8 2.60 0.00 2.78
-5 12 8 15.30 16.30 0.41
-4 12 8 2.93 0.00 1.46
-3 12 8 17.22 16.51 0.40
-2 12 8 17.31 16.42 0.38
-1 12 8 21.40 21.94 0.38
0 12 8 13.50 12.61 0.44
1 12 8 19.98 19.48 0.41
2 12 8 2.13 0.00 2.13
3 12 8 18.21 17.64 0.39
4 12 8 9.09 9.39 0.57
5 12 8 7.61 6.25 0.54
6 12 8 -2.90 0.00 1.45
-4 13 8 7.52 7.57 0.51
-3 13 8 -3.07 0.00 2.41
-2 13 8 18.64 20.12 0.37
-1 13 8 -3.86 0.00 2.14
0 13 8 11.86 11.47 0.51
1 13 8 12.83 13.26 0.46
2 13 8 6.56 7.54 0.73
3 13 8 9.00 8.69 0.52
4 13 8 4.98 0.00 0.87
-1 14 8 10.70 11.35 0.49
0 14 8 10.04 9.89 0.49
1 14 8 2.58 0.00 1.66
-11 0 9 23.79 23.22 0.35
-9 0 9 11.91 11.75 0.50
-7 0 9 3.21 0.00 1.61
-5 0 9 4.27 0.00 1.07
-3 0 9 61.34 59.61 0.81
-1 0 9 19.65 24.04 0.36
1 0 9 21.77 21.57 0.33
3 0 9 16.01 14.37 0.38
5 0 9 7.49 9.00 0.53
7 0 9 50.71 52.11 0.61
9 0 9 22.01 20.89 0.42
11 0 9 19.97 19.17 0.34
-11 1 9 9.91 9.68 0.48
-10 1 9 10.94 10.17 0.51
-9 1 9 19.11 17.95 0.46
-8 1 9 4.07 0.00 2.22
-7 1 9 6.70 1.84 0.77
-6 1 9 24.66 24.38 0.40
-5 1 9 32.85 32.91 0.46
-4 1 9 10.52 9.24 0.46
-3 1 9 46.74 48.22 0.58
-2 1 9 13.04 12.74 0.36
-1 1 9 39.60 40.01 0.51
0 1 9 2.65 0.00 1.14
1 1 9 24.35 24.83 0.36
2 1 9 78.25 75.69 0.76
3 1 9 36.53 37.13 0.58
4 1 9 7.50 8.49 0.52
5 1 9 14.34 14.91 0.38
6 1 9 13.97 15.94 0.45
7 1 9 2.93 0.00 2.58
8 1 9 21.41 20.50 0.39
9 1 9 1.72 0.00 5.09
10 1 9 5.67 0.00 1.18
11 1 9 -1.84 0.00 4.28
-11 2 9 10.20 10.41 0.48
-10 2 9 20.39 19.33 0.37
-9 2 9 -3.59 0.00 3.21
-8 2 9 24.65 24.12 0.40
-7 2 9 1.86 0.00 2.80
-6 2 9 55.42 52.85 0.67
-5 2 9 15.82 14.14 0.39
-4 2 9 71.12 72.01 0.84
-3 2 9 21.64 21.85 0.35
-2 2 9 54.72 54.05 0.57
-1 2 9 0.00 0.00 0.00
0 2 9 45.34 46.76 0.52
1 2 9 11.28 11.24 0.38
2 2 9 62.71 60.86 0.77
3 2 9 27.69 28.31 0.39
4 2 9 32.87 35.08 0.50
5 2 9 10.49 11.24 0.51
6 2 9 9.88 12.42 0.58
7 2 9 18.88 20.75 0.39
8 2 9 15.96 16.19 0.44
9 2 9 3.98 0.00 1.95
10 2 9 -2.52 0.00 3.38
11 2 9 7.87 7.20 0.51
-11 3 9 13.83 12.78 0.39
-10 3 9 -1.42 0.00 6.13
-9 3 9 9.47 10.00 0.57
-8 3 9 9.86 9.47 0.66
-7 3 9 32.40 30.62 0.43
-6 3 9 -1.84 0.00 2.76
-5 3 9 46.21 45.12 0.68
-4 3 9 4.15 0.00 1.04
-3 3 9 83.30 81.76 0.83
-2 3 9 10.70 10.38 0.47
-1 3 9 83.30 78.95 0.82
0 3 9 28.68 28.73 0.45
1 3 9 77.16 77.56 0.75
2 3 9 38.22 37.48 0.55
3 3 9 19.47 18.33 0.32
4 3 9 24.36 24.54 0.32
5 3 9 -2.36 0.00 1.77
6 3 9 9.12 8.30 0.65
7 3 9 3.47 0.00 1.30
8 3 9 8.40 8.73 0.67
9 3 9 3.79 0.00 1.26
10 3 9 12.33 12.80 0.52
11 3 9 3.41 0.00 1.21
-11 4 9 6.69 6.74 0.53
-10 4 9 20.12 19.27 0.42
-9 4 9 16.09 16.28 0.47
-8 4 9 8.80 8.44 0.70
-7 4 9 31.60 30.86 0.43
-6 4 9 25.48 23.90 0.39
-5 4 9 3.57 0.00 3.12
-4 4 9 30.53 31.05 0.49
-3 4 9 2.36 0.00 4.71
-2 4 9 39.86 38.14 0.59
-1 4 9 25.61 23.06 0.38
0 4 9 22.39 22.82 0.31
1 4 9 50.75 50.89 0.56
2 4 9 41.49 39.48 0.59
3 4 9 50.03 48.86 0.59
4 4 9 54.47 55.12 0.60
5 4 9 29.14 28.83 0.40
6 4 9 1.75 0.00 7.87
7 4 9 7.18 7.09 0.63
8 4 9 3.71 0.00 1.11
9 4 9 21.21 19.89 0.40
10 4 9 2.92 0.00 2.09
-11 5 9 -2.64 0.00 2.64
-10 5 9 5.71 5.56 0.80
-9 5 9 4.10 0.00 1.02
-8 5 9 10.75 9.70 0.54
-7 5 9 9.53 8.47 0.51
-6 5 9 17.96 17.64 0.46
-5 5 9 1.80 0.00 7.19
-4 5 9 11.38 11.15 0.41
-3 5 9 6.63 5.04 0.66
-2 5 9 12.96 12.94 0.43
-1 5 9 14.01 11.65 0.44
0 5 9 44.41 41.18 0.62
1 5 9 12.45 14.64 0.41
2 5 9 27.41 25.31 0.43
3 5 9 35.90 36.44 0.50
4 5 9 27.54 27.36 0.42
5 5 9 16.64 15.82 0.46
6 5 9 28.10 28.86 0.39
7 5 9 9.65 9.25 0.62
8 5 9 13.62 13.44 0.49
9 5 9 4.89 0.00 0.85
10 5 9 14.50 14.44 0.42
-10 6 9 6.16 5.94 0.62
-9 6 9 3.26 0.00 1.30
-8 6 9 14.94 14.75 0.43
-7 6 9 -4.91 0.00 2.46
-6 6 9 16.38 16.12 0.49
-5 6 9 10.65 10.35 0.61
-4 6 9 30.51 30.71 0.42
-3 6 9 5.25 2.67 0.58
-2 6 9 42.39 40.21 0.63
-1 6 9 19.55 19.78 0.37
0 6 9 18.57 17.36 0.42
1 6 9 6.82 5.54 0.60
2 6 9 10.19 9.49 0.41
3 6 9 -4.19 0.00 2.45
4 6 9 7.61 7.07 0.60
5 6 9 28.78 29.63 0.43
6 6 9 8.45 8.68 0.55
7 6 9 19.11 18.38 0.45
8 6 9 2.71 0.00 3.62
9 6 9 14.25 14.49 0.44
10 6 9 11.53 11.75 0.51
-10 7 9 1.62 0.00 3.15
-9 7 9 20.31 19.96 0.41
-8 7 9 -6.09 0.00 1.52
-7 7 9 20.80 20.05 0.39
-6 7 9 7.11 7.51 0.63
-5 7 9 27.32 28.12 0.40
-4 7 9 9.43 9.25 0.67
-3 7 9 24.59 24.29 0.38
-2 7 9 27.56 28.18 0.39
-1 7 9 60.84 59.93 0.90
0 7 9 -3.11 0.00 1.55
1 7 9 14.61 14.89 0.44
2 7 9 6.24 6.02 0.72
3 7 9 -2.48 0.00 3.72
4 7 9 5.87 4.75 0.80
5 7 9 17.95 16.94 0.44
6 7 9 11.20 10.66 0.53
7 7 9 14.77 13.90 0.45
8 7 9 -6.06 0.00 1.60
9 7 9 13.16 13.16 0.44
-9 8 9 8.97 5.99 0.49
-8 8 9 15.87 16.79 0.45
-7 8 9 -1.51 0.00 2.26
-6 8 9 29.02 28.80 0.45
-5 8 9 6.60 8.36 0.66
-4 8 9 33.51 34.45 0.46
-3 8 9 -5.29 0.00 1.76
-2 8 9 44.76 44.33 0.66
-1 8 9 2.50 0.00 2.50
0 8 9 40.10 41.23 0.67
1 8 9 24.73 24.59 0.40
2 8 9 18.48 18.06 0.42
3 8 9 1.77 0.00 2.65
4 8 9 15.92 15.34 0.39
5 8 9 7.12 7.28 0.84
6 8 9 11.21 11.39 0.49
7 8 9 -2.65 0.00 3.53
8 8 9 -2.29 0.00 3.43
9 8 9 10.56 11.88 0.52
-8 9 9 14.13 15.96 0.36
-7 9 9 11.85 12.27 0.46
-6 9 9 10.65 10.38 0.52
-5 9 9 14.49 14.50 0.44
-4 9 9 -2.37 0.00 4.14
-3 9 9 21.02 22.13 0.42
-2 9 9 -1.74 0.00 2.61
-1 9 9 21.76 21.11 0.43
0 9 9 42.58 42.59 0.67
1 9 9 18.87 20.21 0.43
2 9 9 27.91 26.98 0.44
3 9 9 2.45 0.00 1.23
4 9 9 25.42 24.01 0.45
5 9 9 13.57 13.80 0.49
6 9 9 15.16 14.72 0.46
7 9 9 -5.66 0.00 1.66
8 9 9 7.24 7.45 0.60
-8 10 9 -1.26 0.00 2.52
-7 10 9 7.69 8.26 0.60
-6 10 9 1.88 0.00 1.88
-5 10 9 2.92 0.00 2.92
-4 10 9 11.24 12.19 0.54
-3 10 9 14.19 15.42 0.47
-2 10 9 -1.68 0.00 5.03
-1 10 9 10.82 10.59 0.54
0 10 9 16.64 16.71 0.45
1 10 9 29.97 29.64 0.40
2 10 9 8.05 8.47 0.73
3 10 9 13.45 13.15 0.50
4 10 9 8.51 8.57 0.59
5 10 9 27.10 26.42 0.37
6 10 9 14.16 13.70 0.46
7 10 9 15.11 14.78 0.39
-7 11 9 15.13 15.62 0.36
-6 11 9 9.61 9.79 0.47
-5 11 9 9.16 9.35 0.54
-4 11 9 7.53 6.27 0.52
-3 11 9 26.83 27.96 0.37
-2 11 9 1.55 0.00 6.20
-1 11 9 25.26 25.43 0.40
0 11 9 12.59 13.11 0.52
1 11 9 6.44 7.20 0.81
2 11 9 6.83 6.53 0.72
3 11 9 8.40 8.69 0.52
4 11 9 19.45 18.87 0.41
5 11 9 1.29 0.00 3.23
6 11 9 8.33 8.51 0.52
-5 12 9 -4.68 0.00 1.40
-4 12 9 8.86 8.56 0.55
-3 12 9 6.43 5.13 0.64
-2 12 9 20.09 18.82 0.37
-1 12 9 4.86 4.37 0.81
0 12 9 13.93 13.37 0.44
1 12 9 2.83 0.00 3.19
2 12 9 14.70 14.58 0.44
3 12 9 -4.84 0.00 1.56
4 12 9 14.54 14.88 0.42
5 12 9 9.99 9.72 0.50
-3 13 9 8.99 9.67 0.51
-2 13 9 5.15 5.11 0.82
-1 13 9 16.60 17.94 0.40
0 13 9 -2.03 0.00 2.03
1 13 9 8.75 7.89 0.46
2 13 9 8.60 7.65 0.50
3 13 9 10.99 11.53 0.49
-10 0 10 31.11 30.64 0.46
-8 0 10 11.77 11.27 0.53
-6 0 10 3.21 0.00 4.28
-4 0 10 18.72 19.60 0.41
-2 0 10 23.10 21.16 0.37
0 0 10 36.28 34.87 0.56
2 0 10 27.73 25.99 0.37
4 0 10 12.57 12.47 0.47
6 0 10 22.24 22.94 0.40
8 0 10 31.22 32.05 0.54
10 0 10 6.61 6.79 0.68
-11 1 10 6.65 7.55 0.56
-10 1 10 11.89 11.19 0.43
-9 1 10 18.27 17.84 0.43
-8 1 10 23.32 23.16 0.40
-7 1 10 15.38 15.08 0.44
-6 1 10 25.08 24.34 0.41
-5 1 10 9.70 9.11 0.51
-4 1 10 26.39 25.04 0.38
-3 1 10 10.05 8.37 0.43
-2 1 10 12.91 12.38 0.41
-1 1 10 3.28 0.00 1.09
0 1 10 27.83 27.08 0.43
1 1 10 13.63 13.13 0.36
2 1 10 16.47 16.72 0.39
3 1 10 10.16 10.54 0.48
4 1 10 5.67 5.77 0.78
5 1 10 14.53 15.56 0.48
6 1 10 17.15 18.39 0.44
7 1 10 22.63 23.09 0.38
8 1 10 8.48 7.97 0.61
9 1 10 12.10 10.95 0.48
10 1 10 -2.45 0.00 2.81
-11 2 10 14.17 13.35 0.41
-10 2 10 10.85 9.75 0.49
-9 2 10 17.61 16.48 0.43
-8 2 10 20.53 19.62 0.45
-7 2 10 10.60 10.29 0.64
-6 2 10 11.79 11.54 0.59
-5 2 10 66.76 64.57 0.95
-4 2 10 20.55 21.42 0.38
-3 2 10 78.91 76.30 0.87
-2 2 10 -1.69 0.00 5.91
-1 2 10 46.82 48.49 0.57
0 2 10 -2.19 0.00 3.84
1 2 10 53.80 54.05 0.57
2 2 10 20.07 20.89 0.32
3 2 10 49.20 50.89 0.61
4 2 10 22.72 23.56 0.38
5 2 10 7.08 8.41 0.63
6 2 10 5.21 4.09 0.87
7 2 10 7.65 7.92 0.57
8 2 10 6.29 6.52 0.84
9 2 10 8.14 8.53 0.60
10 2 10 -2.11 0.00 3.82
-11 3 10 2.54 0.00 2.22
-10 3 10 16.44 15.55 0.40
-9 3 10 13.23 13.71 0.45
-8 3 10 18.76 17.42 0.47
-7 3 10 35.48 34.86 0.56
-6 3 10 64.87 62.69 0.98
-5 3 10 2.58 0.00 4.51
-4 3 10 57.90 58.86 0.65
-3 3 10 6.43 5.60 0.69
-2 3 10 59.28 56.31 0.89
-1 3 10 14.99 14.42 0.33
0 3 10 53.83 54.31 0.58
1 3 10 41.51 39.49 0.58
2 3 10 67.40 66.48 0.82
3 3 10 18.37 18.95 0.38
4 3 10 9.78 11.39 0.44
5 3 10 3.00 0.00 1.50
6 3 10 18.59 18.42 0.41
7 3 10 4.20 0.00 1.05
8 3 10 13.48 11.97 0.48
9 3 10 7.67 7.14 0.54
10 3 10 2.97 0.00 2.16
-10 4 10 11.13 10.50 0.48
-9 4 10 15.59 15.61 0.42
-8 4 10 25.93 24.63 0.43
-7 4 10 -3.11 0.00 4.14
-6 4 10 11.46 11.92 0.59
-5 4 10 25.71 26.15 0.39
-4 4 10 17.55 18.56 0.45
-3 4 10 41.69 40.73 0.62
-2 4 10 4.67 0.00 1.00
-1 4 10 24.18 22.05 0.39
0 4 10 43.03 41.82 0.60
1 4 10 38.52 41.22 0.62
2 4 10 37.85 37.75 0.62
3 4 10 35.15 36.15 0.53
4 4 10 2.98 0.00 3.48
5 4 10 7.43 7.41 0.62
6 4 10 14.67 14.23 0.42
7 4 10 11.82 12.50 0.49
8 4 10 25.03 24.87 0.40
9 4 10 -2.95 0.00 1.32
10 4 10 13.13 12.89 0.41
-10 5 10 6.00 4.14 0.63
-9 5 10 17.06 17.99 0.40
-8 5 10 -2.25 0.00 5.07
-7 5 10 4.26 0.00 1.07
-6 5 10 9.86 10.13 0.49
-5 5 10 7.89 8.32 0.62
-4 5 10 3.11 0.00 3.11
-3 5 10 -1.77 0.00 6.20
-2 5 10 27.31 26.21 0.39
-1 5 10 37.54 33.75 0.55
0 5 10 -3.69 0.00 2.58
1 5 10 20.72 20.04 0.34
2 5 10 38.84 38.45 0.63
3 5 10 24.67 25.04 0.42
4 5 10 19.37 18.75 0.39
5 5 10 7.06 7.65 0.66
6 5 10 8.73 9.24 0.70
7 5 10 23.40 23.22 0.42
8 5 10 -3.42 0.00 1.37
9 5 10 17.70 17.87 0.41
10 5 10 5.72 6.61 0.77
-10 6 10 10.17 10.35 0.46
-9 6 10 10.55 10.78 0.50
-8 6 10 12.88 12.70 0.43
-7 6 10 16.73 15.77 0.41
-6 6 10 9.05 9.47 0.50
-5 6 10 13.35 12.37 0.48
-4 6 10 8.22 7.76 0.59
-3 6 10 44.41 43.55 0.68
-2 6 10 -3.54 0.00 3.09
-1 6 10 33.94 32.97 0.50
0 6 10 20.16 18.12 0.41
1 6 10 16.03 16.01 0.46
2 6 10 11.96 12.61 0.50
3 6 10 -4.94 0.00 1.85
4 6 10 23.19 22.35 0.40
5 6 10 26.66 26.96 0.41
6 6 10 2.97 0.00 3.47
7 6 10 5.82 6.90 0.90
8 6 10 21.23 20.73 0.40
9 6 10 6.95 6.71 0.67
-9 7 10 4.08 0.00 1.05
-8 7 10 17.71 17.09 0.36
-7 7 10 1.54 0.00 2.31
-6 7 10 20.88 20.84 0.46
-5 7 10 16.98 16.71 0.44
-4 7 10 41.10 41.70 0.53
-3 7 10 17.91 17.26 0.44
-2 7 10 4.34 0.00 1.08
-1 7 10 -2.57 0.00 5.15
0 7 10 21.77 20.87 0.38
1 7 10 23.18 22.82 0.39
2 7 10 30.76 30.73 0.50
3 7 10 22.94 22.11 0.40
4 7 10 28.62 28.94 0.48
5 7 10 9.44 10.16 0.63
6 7 10 13.71 12.80 0.50
7 7 10 -4.82 0.00 2.17
8 7 10 16.71 16.19 0.48
9 7 10 -1.62 0.00 3.91
-9 8 10 5.92 4.88 0.73
-8 8 10 9.18 9.31 0.54
-7 8 10 15.21 15.86 0.38
-6 8 10 6.49 7.31 0.54
-5 8 10 40.38 41.93 0.62
-4 8 10 8.96 10.01 0.48
-3 8 10 58.92 58.84 0.64
-2 8 10 22.46 22.48 0.41
-1 8 10 31.50 31.57 0.49
0 8 10 25.43 25.03 0.38
1 8 10 26.64 26.09 0.40
2 8 10 -3.49 0.00 3.05
3 8 10 25.26 25.67 0.42
4 8 10 11.30 10.19 0.51
5 8 10 10.66 10.38 0.51
6 8 10 6.74 6.58 0.71
7 8 10 7.77 6.43 0.63
8 8 10 5.55 6.07 0.84
-8 9 10 10.26 10.30 0.46
-7 9 10 11.74 12.96 0.45
-6 9 10 3.09 0.00 2.78
-5 9 10 2.12 0.00 3.72
-4 9 10 -3.55 0.00 3.20
-3 9 10 9.63 9.17 0.57
-2 9 10 20.00 20.72 0.43
-1 9 10 10.87 10.76 0.54
0 9 10 23.59 23.58 0.39
1 9 10 20.19 20.19 0.45
2 9 10 3.38 0.00 3.38
3 9 10 8.95 9.02 0.62
4 9 10 9.51 9.64 0.54
5 9 10 18.14 17.67 0.45
6 9 10 18.98 18.16 0.36
7 9 10 13.08 12.67 0.45
-7 10 10 -3.52 0.00 2.05
-6 10 10 9.96 10.87 0.51
-5 10 10 2.69 0.00 2.69
-4 10 10 12.49 13.32 0.42
-3 10 10 3.43 0.00 2.74
-2 10 10 -3.55 0.00 2.49
-1 10 10 1.63 0.00 5.70
0 10 10 36.28 36.04 0.52
1 10 10 -2.83 0.00 3.30
2 10 10 23.62 24.25 0.42
3 10 10 5.73 5.71 0.82
4 10 10 7.14 7.49 0.60
5 10 10 3.03 0.00 1.21
6 10 10 12.62 12.21 0.46
7 10 10 2.12 0.00 2.96
-6 11 10 10.57 10.49 0.50
-5 11 10 0.00 0.00 0.00
-4 11 10 14.62 15.25 0.44
-3 11 10 4.74 5.43 0.79
-2 11 10 18.31 18.74 0.39
-1 11 10 10.33 10.29 0.53
0 11 10 8.46 8.13 0.53
1 11 10 -1.47 0.00 2.93
2 11 10 11.70 12.47 0.42
3 11 10 1.90 0.00 3.81
4 11 10 7.93 7.98 0.59
5 11 10 15.80 16.34 0.40
-4 12 10 0.00 0.00 0.00
-3 12 10 11.58 12.92 0.39
-2 12 10 6.32 7.13 0.70
-1 12 10 12.57 11.46 0.44
0 12 10 1.28 0.00 3.20
1 12 10 15.91 16.32 0.44
2 12 10 4.17 0.00 0.87
3 12 10 9.57 10.25 0.45
4 12 10 -0.99 0.00 6.93
-2 13 10 7.72 8.64 0.54
-1 13 10 1.95 0.00 3.66
0 13 10 16.03 17.31 0.40
1 13 10 1.95 0.00 3.66
-9 0 11 27.74 26.47 0.44
-7 0 11 8.05 7.30 0.60
-5 0 11 25.90 25.71 0.40
-3 0 11 11.22 9.94 0.40
-1 0 11 36.83 37.02 0.63
1 0 11 8.66 8.41 0.48
3 0 11 39.48 41.01 0.65
5 0 11 16.09 15.28 0.50
7 0 11 17.28 17.12 0.48
9 0 11 30.89 30.29 0.46
-10 1 11 17.73 16.91 0.39
-9 1 11 20.96 21.21 0.42
-8 1 11 16.62 16.12 0.51
-7 1 11 24.00 22.76 0.40
-6 1 11 -3.96 0.00 3.07
-5 1 11 37.14 36.05 0.56
-4 1 11 24.34 23.05 0.41
-3 1 11 33.40 33.11 0.52
-2 1 11 18.13 17.77 0.39
-1 1 11 13.22 14.74 0.42
0 1 11 3.10 0.00 3.13
1 1 11 23.99 21.17 0.35
2 1 11 22.49 21.45 0.38
3 1 11 22.98 23.67 0.37
4 1 11 1.22 0.00 3.90
5 1 11 0.31 0.00 15.76
6 1 11 8.96 8.06 0.61
7 1 11 12.59 12.47 0.54
8 1 11 16.47 16.89 0.49
9 1 11 13.04 13.23 0.44
10 1 11 11.08 11.44 0.46
-10 2 11 19.44 19.81 0.37
-9 2 11 -1.04 0.00 6.31
-8 2 11 25.51 24.66 0.43
-7 2 11 12.62 12.99 0.50
-6 2 11 6.42 6.60 0.80
-5 2 11 36.75 35.10 0.57
-4 2 11 54.29 52.08 0.68
-3 2 11 15.82 15.48 0.42
-2 2 11 60.60 63.06 0.86
-1 2 11 18.34 18.17 0.38
0 2 11 32.57 32.26 0.50
1 2 11 14.76 14.81 0.37
2 2 11 18.82 18.02 0.38
3 2 11 27.31 27.14 0.44
4 2 11 38.84 41.32 0.67
5 2 11 13.55 13.72 0.46
6 2 11 15.89 15.82 0.47
7 2 11 9.44 9.43 0.59
8 2 11 11.38 10.99 0.52
9 2 11 10.33 9.59 0.52
10 2 11 2.85 0.00 2.15
-10 3 11 5.83 5.89 0.63
-9 3 11 18.14 16.81 0.38
-8 3 11 15.04 14.42 0.51
-7 3 11 7.01 5.24 0.66
-6 3 11 18.99 17.94 0.44
-5 3 11 60.95 58.55 0.67
-4 3 11 3.64 0.00 1.37
-3 3 11 63.72 62.97 0.94
-2 3 11 5.41 2.27 0.90
-1 3 11 40.17 39.53 0.59
0 3 11 28.49 28.80 0.39
1 3 11 29.96 28.80 0.42
2 3 11 9.48 9.41 0.46
3 3 11 41.54 40.70 0.65
4 3 11 12.03 12.00 0.51
5 3 11 4.30 0.00 1.08
6 3 11 14.29 14.90 0.53
7 3 11 9.92 10.28 0.55
8 3 11 3.02 0.00 1.51
9 3 11 12.53 12.83 0.47
10 3 11 4.93 0.00 0.89
-10 4 11 9.98 9.69 0.42
-9 4 11 11.00 10.80 0.48
-8 4 11 28.08 29.16 0.42
-7 4 11 23.57 22.32 0.43
-6 4 11 12.21 11.34 0.53
-5 4 11 7.75 6.14 0.65
-4 4 11 12.71 13.77 0.52
-3 4 11 4.91 0.00 1.05
-2 4 11 23.63 22.10 0.43
-1 4 11 12.00 11.47 0.36
0 4 11 46.03 45.71 0.62
1 4 11 14.36 13.94 0.40
2 4 11 4.21 0.00 1.05
3 4 11 12.58 11.37 0.48
4 4 11 12.26 13.35 0.50
5 4 11 13.36 13.75 0.46
6 4 11 13.75 12.89 0.43
7 4 11 17.90 17.18 0.44
8 4 11 6.39 6.56 0.67
9 4 11 13.19 12.99 0.47
-10 5 11 21.24 21.90 0.33
-9 5 11 7.40 7.52 0.61
-8 5 11 30.19 31.43 0.49
-7 5 11 1.64 0.00 7.36
-6 5 11 9.25 9.19 0.50
-5 5 11 3.58 0.00 1.34
-4 5 11 -4.77 0.00 2.39
-3 5 11 16.31 16.27 0.40
-2 5 11 18.20 16.88 0.50
-1 5 11 27.35 26.83 0.43
0 5 11 36.14 34.19 0.53
1 5 11 10.43 10.90 0.56
2 5 11 23.82 24.01 0.38
3 5 11 12.96 12.94 0.47
4 5 11 -3.03 0.00 3.54
5 5 11 14.04 13.37 0.43
6 5 11 23.99 23.30 0.41
7 5 11 5.89 5.56 0.84
8 5 11 24.08 23.88 0.37
9 5 11 3.34 0.00 1.85
-9 6 11 11.80 12.06 0.42
-8 6 11 8.64 7.49 0.51
-7 6 11 3.76 0.00 2.82
-6 6 11 15.87 15.29 0.44
-5 6 11 -1.73 0.00 2.60
-4 6 11 23.40 24.36 0.40
-3 6 11 10.25 10.36 0.62
-2 6 11 21.38 20.19 0.41
-1 6 11 29.07 29.20 0.42
0 6 11 4.88 0.00 0.92
1 6 11 11.71 11.57 0.51
2 6 11 30.03 29.40 0.45
3 6 11 6.54 2.87 0.70
4 6 11 27.95 27.37 0.43
5 6 11 5.38 3.20 0.81
6 6 11 22.93 22.00 0.46
7 6 11 7.46 7.66 0.60
8 6 11 5.82 4.87 0.87
9 6 11 15.75 16.02 0.44
-9 7 11 8.32 8.81 0.54
-8 7 11 3.75 0.00 1.13
-7 7 11 22.98 22.77 0.39
-6 7 11 4.65 0.00 1.03
-5 7 11 42.41 42.83 0.60
-4 7 11 27.14 26.89 0.43
-3 7 11 46.95 47.89 0.64
-2 7 11 17.89 18.27 0.43
-1 7 11 -3.13 0.00 3.13
0 7 11 5.96 5.26 0.74
1 7 11 28.95 29.58 0.46
2 7 11 13.16 12.71 0.45
3 7 11 12.89 13.21 0.46
4 7 11 3.38 0.00 1.27
5 7 11 16.59 17.08 0.48
6 7 11 12.16 12.10 0.48
7 7 11 13.93 13.42 0.48
8 7 11 9.38 9.10 0.50
-8 8 11 9.77 9.47 0.42
-7 8 11 7.48 5.78 0.62
-6 8 11 11.98 11.51 0.42
-5 8 11 8.49 6.77 0.55
-4 8 11 23.33 22.45 0.39
-3 8 11 3.32 0.00 1.25
-2 8 11 21.85 23.25 0.39
-1 8 11 8.18 8.35 0.56
0 8 11 32.63 32.16 0.47
1 8 11 16.34 16.64 0.43
2 8 11 34.06 33.96 0.54
3 8 11 -2.34 0.00 4.10
4 8 11 27.29 28.02 0.47
5 8 11 -4.32 0.00 2.16
6 8 11 19.88 20.09 0.40
7 8 11 11.92 11.64 0.44
8 8 11 6.47 5.06 0.67
-7 9 11 12.29 13.30 0.41
-6 9 11 12.86 14.30 0.42
-5 9 11 16.54 16.98 0.40
-4 9 11 14.40 15.14 0.45
-3 9 11 21.84 23.03 0.39
-2 9 11 4.81 4.31 0.80
-1 9 11 9.29 8.18 0.58
0 9 11 20.59 19.33 0.40
1 9 11 18.41 19.26 0.42
2 9 11 14.35 14.28 0.44
3 9 11 5.58 6.33 0.86
4 9 11 3.31 0.00 2.65
5 9 11 5.15 4.43 0.74
6 9 11 6.04 5.73 0.75
7 9 11 7.43 7.08 0.61
-6 10 11 7.21 7.15 0.54
-5 10 11 8.19 8.30 0.53
-4 10 11 -4.58 0.00 1.91
-3 10 11 9.86 9.61 0.50
-2 10 11 -2.55 0.00 2.98
-1 10 11 3.38 0.00 2.71
0 10 11 3.02 0.00 3.02
1 10 11 10.77 10.64 0.51
2 10 11 -2.90 0.00 3.26
3 10 11 3.40 0.00 1.42
4 10 11 6.10 6.16 0.69
5 10 11 14.70 13.80 0.43
6 10 11 1.40 0.00 4.90
-5 11 11 10.02 10.89 0.53
-4 11 11 1.58 0.00 4.35
-3 11 11 14.32 14.45 0.42
-2 11 11 -4.08 0.00 2.04
-1 11 11 22.48 22.91 0.40
0 11 11 25.24 25.20 0.38
1 11 11 6.44 6.93 0.67
2 11 11 3.34 0.00 1.19
3 11 11 9.51 10.23 0.45
4 11 11 0.00 0.00 0.00
-3 12 11 3.03 0.00 1.21
-2 12 11 13.06 12.64 0.37
-1 12 11 10.53 10.90 0.45
0 12 11 7.46 6.81 0.58
1 12 11 7.63 7.18 0.52
2 12 11 15.08 14.88 0.41
3 12 11 -4.08 0.00 1.53
-10 0 12 16.95 17.35 0.33
-8 0 12 28.75 27.23 0.38
-6 0 12 10.24 10.90 0.64
-4 0 12 15.36 14.01 0.46
-2 0 12 6.86 5.81 0.69
0 0 12 9.04 8.25 0.50
2 0 12 14.91 14.05 0.42
4 0 12 18.28 18.69 0.44
6 0 12 -3.85 0.00 3.08
8 0 12 30.96 30.92 0.42
-10 1 12 7.36 7.83 0.54
-9 1 12 14.65 13.48 0.41
-8 1 12 15.05 14.43 0.47
-7 1 12 28.43 27.42 0.41
-6 1 12 6.83 0.00 1.82
-5 1 12 26.96 25.78 0.45
-4 1 12 29.14 28.07 0.43
-3 1 12 21.19 20.54 0.45
-2 1 12 29.21 28.07 0.46
-1 1 12 -4.66 0.00 2.47
0 1 12 13.97 14.55 0.44
1 1 12 6.20 5.86 0.74
2 1 12 11.80 12.13 0.53
3 1 12 42.47 40.75 0.68
4 1 12 19.20 19.57 0.42
5 1 12 7.70 5.89 0.63
6 1 12 13.58 14.32 0.55
7 1 12 23.27 23.85 0.43
8 1 12 9.72 9.87 0.50
9 1 12 14.10 13.93 0.44
-10 2 12 1.64 0.00 3.19
-8 2 12 -3.36 0.00 2.69
-7 2 12 29.73 28.66 0.43
-6 2 12 11.33 9.41 0.42
-5 2 12 35.08 33.55 0.49
-4 2 12 19.79 19.94 0.44
-3 2 12 45.67 44.88 0.65
-2 2 12 1.74 0.00 2.61
-1 2 12 16.25 15.96 0.46
0 2 12 8.48 9.72 0.53
1 2 12 20.90 21.43 0.43
2 2 12 3.50 0.00 1.31
3 2 12 24.72 22.87 0.38
4 2 12 8.49 7.57 0.55
5 2 12 18.13 17.64 0.42
6 2 12 9.37 8.38 0.60
7 2 12 25.01 25.70 0.45
8 2 12 8.44 8.07 0.59
9 2 12 14.11 13.49 0.44
-10 3 12 11.21 11.81 0.43
-8 3 12 11.80 12.19 0.45
-7 3 12 4.33 0.00 0.93
-6 3 12 8.98 8.71 0.69
-5 3 12 6.85 6.57 0.73
-4 3 12 47.20 44.26 0.70
-3 3 12 18.33 16.74 0.48
-2 3 12 54.21 54.36 0.64
-1 3 12 12.54 13.08 0.48
0 3 12 19.43 18.25 0.39
1 3 12 9.20 9.04 0.49
2 3 12 44.57 46.02 0.65
3 3 12 -2.48 0.00 4.35
4 3 12 43.07 42.00 0.64
5 3 12 8.46 9.49 0.71
6 3 12 -1.66 0.00 2.50
7 3 12 2.19 0.00 4.38
8 3 12 12.51 11.93 0.53
9 3 12 7.27 7.65 0.61
-8 4 12 19.38 20.39 0.39
-7 4 12 12.91 13.00 0.48
-6 4 12 19.99 18.59 0.44
-5 4 12 4.00 0.00 1.20
-4 4 12 12.13 10.49 0.54
-3 4 12 34.61 32.26 0.52
-2 4 12 0.00 0.00 0.00
-1 4 12 13.27 13.07 0.46
0 4 12 2.46 0.00 5.53
1 4 12 5.75 5.29 0.78
2 4 12 3.48 0.00 3.04
3 4 12 9.58 9.08 0.48
4 4 12 18.34 17.40 0.41
5 4 12 10.07 9.61 0.58
6 4 12 8.47 8.57 0.63
7 4 12 15.71 14.75 0.43
8 4 12 13.97 13.57 0.49
9 4 12 7.45 7.97 0.66
-9 5 12 15.76 14.90 0.36
-8 5 12 6.00 5.37 0.68
-7 5 12 15.40 15.43 0.43
-6 5 12 12.41 12.21 0.54
-5 5 12 7.34 7.43 0.61
-4 5 12 0.00 0.00 0.00
-3 5 12 13.22 12.11 0.55
-2 5 12 17.81 16.41 0.52
-1 5 12 6.25 6.73 0.72
0 5 12 2.45 0.00 3.68
1 5 12 6.00 3.88 0.75
2 5 12 20.90 21.56 0.43
3 5 12 5.46 4.92 0.82
4 5 12 -2.96 0.00 2.96
5 5 12 13.61 13.04 0.51
6 5 12 6.48 6.11 0.76
7 5 12 17.11 17.72 0.42
8 5 12 7.86 7.02 0.57
-8 6 12 14.49 13.92 0.36
-7 6 12 19.66 20.51 0.38
-6 6 12 3.08 0.00 1.54
-5 6 12 21.68 21.23 0.44
-4 6 12 21.11 21.11 0.48
-3 6 12 3.65 0.00 1.37
-2 6 12 12.14 11.29 0.55
-1 6 12 22.46 23.09 0.39
0 6 12 5.16 4.46 0.86
1 6 12 19.82 20.38 0.44
2 6 12 3.40 0.00 3.40
3 6 12 15.24 14.94 0.47
4 6 12 -5.25 0.00 2.36
5 6 12 22.80 22.57 0.45
6 6 12 7.74 9.13 0.72
7 6 12 13.29 13.21 0.47
8 6 12 8.33 9.20 0.66
-8 7 12 18.54 19.63 0.32
-7 7 12 3.89 0.00 0.97
-6 7 12 24.44 24.23 0.37
-5 7 12 16.83 17.43 0.42
-4 7 12 17.29 18.25 0.45
-3 7 12 13.78 15.25 0.50
-2 7 12 28.61 27.19 0.37
-1 7 12 7.10 7.29 0.59
0 7 12 16.59 18.57 0.42
1 7 12 7.09 7.95 0.59
2 7 12 28.45 28.00 0.39
3 7 12 11.19 11.13 0.48
4 7 12 25.69 25.42 0.39
5 7 12 -3.68 0.00 3.07
6 7 12 18.58 18.16 0.41
7 7 12 5.73 6.35 0.75
-7 8 12 14.68 15.98 0.38
-6 8 12 2.52 0.00 1.57
-5 8 12 16.83 17.40 0.40
-4 8 12 23.28 24.61 0.38
-3 8 12 25.00 25.06 0.39
-2 8 12 4.29 0.00 1.23
-1 8 12 27.08 27.28 0.45
0 8 12 9.37 9.01 0.55
1 8 12 22.37 23.89 0.40
2 8 12 3.16 0.00 1.18
3 8 12 21.23 20.39 0.39
4 8 12 6.22 6.18 0.69
5 8 12 23.01 22.99 0.37
6 8 12 -6.91 0.00 1.29
7 8 12 12.12 13.38 0.50
-6 9 12 12.13 12.51 0.38
-5 9 12 2.47 0.00 1.54
-4 9 12 3.54 0.00 1.01
-3 9 12 2.46 0.00 3.69
-2 9 12 18.90 19.11 0.41
-1 9 12 -5.86 0.00 1.76
0 9 12 17.18 17.73 0.39
1 9 12 12.91 11.99 0.43
2 9 12 18.61 19.45 0.40
3 9 12 4.43 4.65 0.66
4 9 12 7.07 6.41 0.61
5 9 12 14.06 14.00 0.40
6 9 12 12.57 12.77 0.50
-5 10 12 -4.64 0.00 1.62
-4 10 12 7.36 6.90 0.55
-3 10 12 8.61 9.54 0.55
-2 10 12 7.94 8.04 0.55
-1 10 12 5.54 5.48 0.65
0 10 12 4.30 0.00 0.86
1 10 12 9.35 8.21 0.48
2 10 12 3.18 0.00 1.32
3 10 12 3.87 0.00 1.16
4 10 12 5.25 4.81 0.72
5 10 12 -2.38 0.00 2.57
-4 11 12 8.69 7.97 0.54
-3 11 12 -1.04 0.00 3.11
-2 11 12 11.02 11.75 0.45
-1 11 12 11.42 11.27 0.40
0 11 12 9.06 8.94 0.51
1 11 12 4.92 5.27 0.78
2 11 12 14.27 14.22 0.37
3 11 12 -2.43 0.00 2.83
-9 0 13 24.93 26.73 0.33
-7 0 13 23.09 20.83 0.37
-5 0 13 16.52 17.12 0.50
-3 0 13 14.61 13.70 0.45
-1 0 13 -2.54 0.00 3.18
1 0 13 5.38 3.63 0.90
3 0 13 22.05 19.34 0.44
5 0 13 12.68 13.16 0.59
7 0 13 15.44 15.97 0.48
9 0 13 10.02 10.41 0.58
-9 1 13 5.70 6.44 0.70
-8 1 13 22.31 21.91 0.38
-7 1 13 22.36 21.77 0.41
-6 1 13 9.07 8.59 0.65
-5 1 13 21.46 21.02 0.44
-4 1 13 18.51 18.32 0.43
-3 1 13 15.65 14.97 0.42
-2 1 13 8.18 7.59 0.60
-1 1 13 8.94 9.00 0.55
0 1 13 12.31 13.06 0.52
1 1 13 7.62 8.07 0.63
2 1 13 12.87 12.48 0.50
3 1 13 14.85 13.79 0.54
4 1 13 1.33 0.00 2.67
5 1 13 22.81 22.27 0.45
6 1 13 14.35 14.32 0.55
7 1 13 11.15 11.18 0.48
8 1 13 16.47 16.66 0.42
9 1 13 3.98 0.00 2.63
-9 2 13 8.24 7.96 0.55
-8 2 13 12.00 11.56 0.44
-7 2 13 11.82 12.06 0.49
-6 2 13 19.55 18.30 0.43
-5 2 13 33.72 31.06 0.47
-4 2 13 23.21 23.05 0.44
-3 2 13 13.55 14.13 0.47
-2 2 13 30.09 28.06 0.47
-1 2 13 3.05 0.00 4.07
0 2 13 25.16 24.58 0.37
1 2 13 9.01 10.60 0.69
2 2 13 30.26 29.77 0.46
3 2 13 15.52 14.75 0.39
4 2 13 31.66 31.93 0.56
5 2 13 11.35 10.86 0.49
6 2 13 19.93 19.54 0.43
7 2 13 7.02 6.42 0.73
8 2 13 7.51 7.93 0.71
9 2 13 -5.61 0.00 1.36
-9 3 13 8.31 9.33 0.47
-8 3 13 4.39 0.00 0.91
-7 3 13 5.53 4.57 0.79
-6 3 13 10.08 9.73 0.53
-5 3 13 36.12 34.02 0.55
-4 3 13 2.59 0.00 3.88
-3 3 13 26.82 26.95 0.46
-2 3 13 14.01 14.62 0.44
-1 3 13 15.10 13.85 0.41
0 3 13 -4.98 0.00 2.18
1 3 13 30.20 29.62 0.46
2 3 13 3.01 0.00 1.51
3 3 13 34.73 35.98 0.51
4 3 13 6.56 6.81 0.66
5 3 13 29.80 30.45 0.49
6 3 13 13.23 13.38 0.54
7 3 13 15.44 15.40 0.50
8 3 13 0.00 0.00 0.00
-9 4 13 6.46 6.29 0.61
-8 4 13 4.10 0.00 0.85
-7 4 13 10.32 9.79 0.48
-6 4 13 14.25 14.51 0.43
-5 4 13 2.40 0.00 4.20
-4 4 13 16.94 15.98 0.49
-3 4 13 7.28 8.22 0.61
-2 4 13 8.29 8.45 0.54
-1 4 13 27.33 28.32 0.44
0 4 13 10.84 10.02 0.56
1 4 13 -4.89 0.00 2.14
2 4 13 18.08 17.98 0.41
3 4 13 9.25 7.70 0.46
4 4 13 6.18 5.32 0.88
5 4 13 3.90 0.00 1.30
6 4 13 10.30 10.97 0.54
7 4 13 11.07 11.39 0.56
8 4 13 8.51 9.53 0.58
-8 5 13 18.02 18.87 0.32
-7 5 13 3.45 0.00 2.71
-6 5 13 12.77 12.31 0.43
-5 5 13 10.95 10.65 0.48
-4 5 13 5.90 5.74 0.81
-3 5 13 0.00 0.00 0.00
-2 5 13 17.04 17.21 0.42
-1 5 13 23.85 24.82 0.37
0 5 13 10.93 9.78 0.53
1 5 13 -2.94 0.00 3.92
2 5 13 12.56 12.32 0.45
3 5 13 -2.84 0.00 1.42
4 5 13 -4.23 0.00 2.12
5 5 13 3.42 0.00 1.03
6 5 13 14.05 13.28 0.43
7 5 13 -3.93 0.00 2.36
8 5 13 12.29 14.25 0.56
-8 6 13 16.86 17.69 0.35
-7 6 13 13.58 13.53 0.41
-6 6 13 12.39 11.80 0.38
-5 6 13 15.89 16.29 0.43
-4 6 13 2.25 0.00 3.93
-3 6 13 6.80 7.34 0.85
-2 6 13 7.49 6.96 0.71
-1 6 13 0.00 0.00 0.00
0 6 13 27.10 28.11 0.41
1 6 13 12.43 12.13 0.44
2 6 13 18.92 19.91 0.42
3 6 13 4.75 4.37 0.79
4 6 13 11.32 10.89 0.51
5 6 13 7.76 7.43 0.67
6 6 13 10.22 9.91 0.59
7 6 13 6.71 9.47 0.75
-7 7 13 14.91 15.04 0.35
-6 7 13 14.67 15.29 0.41
-5 7 13 17.71 18.14 0.38
-4 7 13 18.90 18.88 0.40
-3 7 13 32.81 34.36 0.49
-2 7 13 3.95 0.00 1.32
-1 7 13 18.05 17.71 0.41
0 7 13 1.58 0.00 2.38
1 7 13 14.51 15.71 0.43
2 7 13 -2.68 0.00 1.34
3 7 13 30.14 29.64 0.48
4 7 13 6.97 7.00 0.58
5 7 13 21.57 21.37 0.41
6 7 13 7.93 9.35 0.60
7 7 13 4.64 0.00 0.97
-6 8 13 7.56 7.95 0.44
-5 8 13 2.74 0.00 2.20
-4 8 13 15.62 16.11 0.40
-3 8 13 0.00 0.00 0.00
-2 8 13 21.26 21.63 0.41
-1 8 13 -5.10 0.00 1.70
0 8 13 21.47 21.93 0.36
1 8 13 -1.47 0.00 2.21
2 8 13 24.41 24.65 0.38
3 8 13 6.62 5.25 0.58
4 8 13 20.41 19.89 0.41
5 8 13 3.51 0.00 1.17
6 8 13 13.22 14.22 0.48
-5 9 13 11.30 10.76 0.39
-4 9 13 0.00 0.00 0.00
-3 9 13 -1.26 0.00 3.15
-2 9 13 7.78 8.30 0.56
-1 9 13 13.82 14.61 0.39
0 9 13 8.21 7.98 0.56
1 9 13 22.81 22.72 0.35
2 9 13 -3.17 0.00 2.38
3 9 13 12.20 13.43 0.49
4 9 13 -1.94 0.00 1.62
5 9 13 3.76 0.00 1.00
-4 10 13 5.18 4.34 0.72
-3 10 13 5.25 5.48 0.66
-2 10 13 1.58 0.00 3.95
-1 10 13 15.59 15.22 0.39
0 10 13 -2.62 0.00 1.57
1 10 13 3.83 0.00 0.87
2 10 13 6.16 6.67 0.60
3 10 13 -3.53 0.00 1.91
-1 11 13 9.93 9.85 0.46
0 11 13 4.24 0.00 0.91
1 11 13 11.57 11.36 0.38
-8 0 14 26.88 28.41 0.40
-6 0 14 4.15 0.00 1.19
-4 0 14 10.65 10.80 0.55
-2 0 14 15.44 16.45 0.42
0 0 14 16.64 16.95 0.48
2 0 14 22.38 20.69 0.41
4 0 14 20.79 20.79 0.47
6 0 14 5.22 5.41 0.80
8 0 14 7.18 8.12 0.60
-8 1 14 7.56 8.11 0.53
-7 1 14 19.73 19.21 0.39
-6 1 14 9.95 8.16 0.56
-5 1 14 8.56 8.06 0.61
-4 1 14 16.99 17.13 0.47
-3 1 14 14.78 13.85 0.47
-2 1 14 14.84 14.56 0.53
-1 1 14 8.94 7.47 0.54
0 1 14 7.24 6.49 0.68
1 1 14 2.80 0.00 2.62
2 1 14 28.87 28.14 0.48
3 1 14 19.74 19.35 0.45
4 1 14 24.27 24.40 0.45
5 1 14 6.27 5.40 0.79
6 1 14 6.38 5.48 0.74
7 1 14 2.69 0.00 3.28
8 1 14 7.01 7.23 0.67
-8 2 14 3.68 0.00 1.00
-7 2 14 14.25 14.31 0.44
-6 2 14 7.85 6.84 0.60
-5 2 14 22.27 21.06 0.44
-4 2 14 11.73 10.35 0.48
-3 2 14 15.36 16.04 0.49
-2 2 14 -1.74 0.00 2.61
-1 2 14 18.97 18.88 0.40
0 2 14 -3.01 0.00 1.51
1 2 14 23.10 21.31 0.39
2 2 14 8.58 9.08 0.69
3 2 14 40.07 39.86 0.66
4 2 14 -5.08 0.00 2.29
5 2 14 15.92 15.03 0.44
6 2 14 0.00 0.00 0.00
7 2 14 18.57 17.83 0.45
8 2 14 5.69 5.47 0.78
-8 3 14 10.71 10.98 0.40
-7 3 14 8.47 8.91 0.48
-6 3 14 5.47 0.00 0.98
-5 3 14 -5.94 0.00 2.06
-4 3 14 11.87 10.97 0.57
-3 3 14 18.14 17.67 0.47
-2 3 14 27.23 26.86 0.43
-1 3 14 10.82 10.42 0.54
0 3 14 22.72 21.70 0.39
1 3 14 1.70 0.00 7.65
2 3 14 27.02 26.91 0.42
3 3 14 10.20 10.10 0.52
4 3 14 40.59 42.69 0.60
5 3 14 -3.31 0.00 3.31
6 3 14 17.81 17.31 0.41
7 3 14 9.02 9.72 0.62
-8 4 14 7.58 7.99 0.52
-7 4 14 14.65 15.80 0.44
-6 4 14 11.59 12.75 0.50
-5 4 14 28.40 26.39 0.41
-4 4 14 14.62 12.56 0.50
-3 4 14 5.41 0.00 0.98
-2 4 14 15.49 16.70 0.44
-1 4 14 12.12 12.31 0.46
0 4 14 5.01 4.18 0.84
1 4 14 14.08 13.48 0.49
2 4 14 5.42 5.20 0.74
3 4 14 19.75 19.88 0.44
4 4 14 -2.13 0.00 4.80
5 4 14 3.49 0.00 1.16
6 4 14 11.98 12.27 0.49
7 4 14 13.72 15.74 0.49
-7 5 14 17.85 18.34 0.36
-6 5 14 -3.85 0.00 2.35
-5 5 14 4.55 0.00 0.91
-4 5 14 3.90 0.00 1.30
-3 5 14 16.12 16.40 0.45
-2 5 14 6.15 6.25 0.62
-1 5 14 25.61 27.31 0.40
0 5 14 5.12 0.00 1.02
1 5 14 3.93 0.00 0.98
2 5 14 0.00 0.00 0.00
3 5 14 3.03 0.00 2.65
4 5 14 6.46 7.40 0.65
5 5 14 5.21 4.37 0.87
6 5 14 -5.23 0.00 1.65
7 5 14 5.86 6.20 0.75
-7 6 14 4.49 0.00 0.88
-6 6 14 4.77 0.00 0.84
-5 6 14 8.35 8.54 0.63
-4 6 14 11.64 11.98 0.45
-3 6 14 19.55 19.75 0.39
-2 6 14 3.37 0.00 2.70
-1 6 14 1.53 0.00 5.37
0 6 14 9.62 9.85 0.49
1 6 14 21.24 22.11 0.38
2 6 14 2.11 0.00 5.28
3 6 14 15.01 14.89 0.41
4 6 14 10.76 10.53 0.43
5 6 14 10.04 10.97 0.54
6 6 14 4.71 0.00 0.87
-6 7 14 10.63 10.65 0.38
-5 7 14 2.89 0.00 2.41
-4 7 14 20.88 21.37 0.40
-3 7 14 11.10 10.30 0.43
-2 7 14 26.49 27.69 0.37
-1 7 14 7.96 9.28 0.51
0 7 14 21.09 21.23 0.39
1 7 14 6.71 6.47 0.61
2 7 14 23.05 22.59 0.34
3 7 14 2.98 0.00 1.19
4 7 14 14.23 13.88 0.43
5 7 14 1.57 0.00 2.36
6 7 14 6.59 8.31 0.70
-5 8 14 6.53 7.37 0.54
-4 8 14 4.30 0.00 0.92
-3 8 14 9.43 9.92 0.48
-2 8 14 9.51 9.99 0.51
-1 8 14 9.77 10.17 0.44
0 8 14 9.78 11.55 0.44
1 8 14 26.78 26.40 0.41
2 8 14 -2.19 0.00 3.64
3 8 14 17.06 17.98 0.42
4 8 14 6.94 6.94 0.59
5 8 14 9.43 10.60 0.54
-4 9 14 14.03 14.05 0.42
-3 9 14 9.26 8.80 0.46
-2 9 14 10.58 10.90 0.47
-1 9 14 11.81 12.54 0.39
0 9 14 9.40 8.68 0.50
1 9 14 6.24 6.24 0.62
2 9 14 15.38 15.39 0.35
3 9 14 3.17 0.00 0.95
-2 10 14 16.91 18.32 0.34
-1 10 14 0.93 0.00 6.53
0 10 14 6.11 7.34 0.65
1 10 14 3.66 0.00 1.03
-7 0 15 18.59 17.81 0.38
-5 0 15 4.82 0.00 0.88
-3 0 15 16.89 16.29 0.47
-1 0 15 9.71 10.27 0.61
1 0 15 -4.75 0.00 2.38
3 0 15 8.98 8.25 0.56
5 0 15 2.77 0.00 3.46
7 0 15 2.47 0.00 2.88
-8 1 15 17.00 16.82 0.36
-7 1 15 4.21 0.00 1.01
-6 1 15 5.14 0.00 1.34
-5 1 15 -2.48 0.00 3.40
-4 1 15 11.40 11.51 0.53
-3 1 15 7.54 7.47 0.70
-2 1 15 16.38 15.71 0.51
-1 1 15 13.92 13.13 0.52
0 1 15 19.32 19.69 0.45
1 1 15 24.49 24.62 0.40
2 1 15 -4.20 0.00 2.42
3 1 15 11.36 11.05 0.55
4 1 15 4.17 0.00 1.74
5 1 15 10.46 10.75 0.55
6 1 15 1.26 0.00 5.10
7 1 15 6.20 7.54 0.77
-7 2 15 -3.30 0.00 2.20
-6 2 15 1.36 0.00 6.12
-5 2 15 8.23 9.56 0.61
-4 2 15 23.51 22.27 0.39
-3 2 15 10.74 10.39 0.48
-2 2 15 19.88 18.85 0.41
-1 2 15 3.70 0.00 1.48
0 2 15 25.33 24.93 0.43
1 2 15 5.63 3.12 0.70
2 2 15 33.09 31.49 0.50
3 2 15 3.42 0.00 2.74
4 2 15 29.96 31.07 0.49
5 2 15 5.79 6.41 0.76
6 2 15 7.97 8.12 0.61
7 2 15 -3.06 0.00 2.30
-7 3 15 10.56 10.87 0.40
-6 3 15 9.06 8.40 0.57
-5 3 15 7.19 7.24 0.51
-4 3 15 2.95 0.00 2.95
-3 3 15 14.03 13.42 0.52
-2 3 15 7.81 6.95 0.65
-1 3 15 19.86 20.84 0.39
0 3 15 8.30 9.04 0.61
1 3 15 26.51 25.62 0.38
2 3 15 -4.09 0.00 2.92
3 3 15 22.99 23.96 0.38
4 3 15 -3.41 0.00 1.99
5 3 15 29.33 30.59 0.42
6 3 15 -1.59 0.00 5.58
7 3 15 9.76 13.33 0.67
-7 4 15 11.05 12.09 0.43
-6 4 15 5.16 5.12 0.81
-5 4 15 21.55 20.86 0.43
-4 4 15 13.11 12.88 0.45
-3 4 15 13.07 13.12 0.42
-2 4 15 9.76 10.21 0.48
-1 4 15 16.99 17.09 0.42
0 4 15 16.30 16.39 0.44
1 4 15 -3.05 0.00 2.67
2 4 15 15.87 17.28 0.42
3 4 15 -2.46 0.00 1.64
4 4 15 18.54 19.37 0.38
5 4 15 8.53 10.31 0.61
6 4 15 2.58 0.00 3.22
-6 5 15 11.75 12.08 0.37
-5 5 15 5.05 0.00 0.89
-4 5 15 9.25 8.98 0.47
-3 5 15 -5.07 0.00 1.95
-2 5 15 8.17 7.88 0.51
-1 5 15 -3.27 0.00 2.95
0 5 15 19.61 20.11 0.38
1 5 15 2.05 0.00 3.58
2 5 15 -2.44 0.00 3.25
3 5 15 3.00 0.00 2.70
4 5 15 -2.17 0.00 1.81
5 5 15 3.19 0.00 1.20
6 5 15 -3.26 0.00 1.90
-6 6 15 12.21 11.97 0.39
-5 6 15 9.98 10.68 0.47
-4 6 15 11.24 11.09 0.46
-3 6 15 17.99 18.62 0.37
-2 6 15 14.45 14.13 0.37
-1 6 15 6.40 7.71 0.73
0 6 15 3.35 0.00 0.84
1 6 15 7.41 7.02 0.49
2 6 15 14.72 15.10 0.41
3 6 15 4.32 0.00 0.90
4 6 15 -1.62 0.00 4.46
5 6 15 2.46 0.00 2.67
-5 7 15 7.33 6.74 0.52
-4 7 15 7.73 8.41 0.51
-3 7 15 12.08 12.63 0.40
-2 7 15 3.86 0.00 1.16
-1 7 15 18.93 19.49 0.37
0 7 15 -4.16 0.00 2.08
1 7 15 20.46 20.18 0.37
2 7 15 4.31 0.00 0.83
3 7 15 15.54 16.32 0.40
4 7 15 2.84 0.00 1.24
-4 8 15 10.63 10.40 0.38
-3 8 15 2.46 0.00 2.46
-2 8 15 20.28 20.57 0.34
-1 8 15 3.12 0.00 2.34
0 8 15 12.32 12.65 0.40
1 8 15 -3.61 0.00 1.97
2 8 15 17.13 17.37 0.35
3 8 15 2.67 0.00 1.33
-1 9 15 8.76 7.95 0.52
0 9 15 7.91 9.23 0.53
-6 0 16 11.08 10.35 0.41
-4 0 16 21.13 21.45 0.39
-2 0 16 23.09 23.07 0.39
0 0 16 1.56 0.00 3.11
2 0 16 9.76 9.74 0.55
4 0 16 8.89 9.48 0.56
6 0 16 -2.84 0.00 2.36
-6 1 16 7.99 7.66 0.49
-5 1 16 3.57 0.00 1.05
-4 1 16 8.62 8.31 0.53
-3 1 16 20.60 21.50 0.40
-2 1 16 15.27 15.00 0.44
-1 1 16 5.33 4.41 0.89
0 1 16 13.01 12.81 0.46
1 1 16 12.25 11.68 0.47
2 1 16 13.91 13.68 0.46
3 1 16 4.89 0.00 1.35
4 1 16 10.79 9.98 0.53
5 1 16 2.55 0.00 1.52
6 1 16 -3.38 0.00 2.08
-6 2 16 -3.93 0.00 1.70
-5 2 16 -2.37 0.00 2.96
-4 2 16 12.21 11.32 0.42
-3 2 16 15.48 15.79 0.44
-2 2 16 8.80 9.60 0.61
-1 2 16 31.85 30.99 0.42
0 2 16 -4.71 0.00 2.12
1 2 16 22.88 23.14 0.37
2 2 16 9.42 10.95 0.52
3 2 16 22.07 23.30 0.40
4 2 16 -3.88 0.00 1.94
5 2 16 16.53 20.06 0.43
6 2 16 -2.70 0.00 2.25
-6 3 16 2.80 0.00 2.45
-5 3 16 6.17 6.93 0.72
-4 3 16 2.51 0.00 3.44
-3 3 16 3.57 0.00 1.02
-2 3 16 18.23 17.81 0.38
-1 3 16 10.95 10.58 0.47
0 3 16 17.30 18.09 0.41
1 3 16 5.60 6.46 0.70
2 3 16 20.71 20.99 0.35
3 3 16 2.21 0.00 2.21
4 3 16 20.61 21.35 0.40
5 3 16 1.47 0.00 2.21
-6 4 16 9.45 10.48 0.48
-5 4 16 4.31 0.00 0.76
-4 4 16 11.55 10.77 0.42
-3 4 16 11.29 11.69 0.51
-2 4 16 17.16 17.61 0.37
-1 4 16 10.77 10.59 0.43
0 4 16 11.92 11.71 0.46
1 4 16 17.66 18.11 0.40
2 4 16 -3.14 0.00 2.62
3 4 16 16.82 17.07 0.39
4 4 16 -2.47 0.00 2.72
5 4 16 10.10 14.10 0.64
-5 5 16 13.23 13.79 0.40
-4 5 16 -3.57 0.00 1.79
-3 5 16 8.28 8.73 0.51
-2 5 16 3.06 0.00 2.55
-1 5 16 10.51 10.90 0.46
0 5 16 -3.80 0.00 1.90
1 5 16 7.76 7.81 0.60
2 5 16 4.64 4.31 0.77
3 5 16 -5.49 0.00 1.26
4 5 16 5.60 5.00 0.63
-4 6 16 12.23 13.05 0.40
-3 6 16 7.64 7.11 0.51
-2 6 16 11.23 11.17 0.46
-1 6 16 8.07 7.12 0.50
0 6 16 -3.29 0.00 2.26
1 6 16 6.64 6.09 0.59
2 6 16 4.35 0.00 0.82
3 6 16 9.99 11.10 0.45
-3 7 16 11.57 11.24 0.42
-2 7 16 18.44 18.99 0.37
-1 7 16 0.00 0.00 0.00
0 7 16 15.62 16.03 0.34
1 7 16 4.69 3.89 0.64
2 7 16 8.59 10.79 0.56
-5 0 17 14.07 13.97 0.39
-3 0 17 20.13 21.65 0.40
-1 0 17 8.09 6.85 0.53
1 0 17 7.50 7.25 0.57
3 0 17 7.63 7.61 0.61
-5 1 17 3.66 0.00 1.03
-4 1 17 20.08 19.92 0.34
-3 1 17 13.81 14.07 0.41
-2 1 17 15.61 15.34 0.41
-1 1 17 13.63 12.66 0.43
0 1 17 14.30 13.66 0.42
1 1 17 8.25 8.27 0.60
2 1 17 9.64 10.38 0.55
3 1 17 9.86 10.52 0.53
4 1 17 6.26 8.13 0.65
-5 2 17 7.59 7.16 0.53
-4 2 17 11.08 12.39 0.44
-3 2 17 6.30 7.21 0.73
-2 2 17 16.54 17.50 0.40
-1 2 17 6.05 6.83 0.66
0 2 17 18.54 17.66 0.39
1 2 17 5.69 5.48 0.68
2 2 17 19.19 19.33 0.40
3 2 17 1.87 0.00 1.87
4 2 17 7.45 9.78 0.61
-4 3 17 1.97 0.00 1.48
-3 3 17 5.68 5.90 0.63
-2 3 17 -2.02 0.00 1.68
-1 3 17 20.23 20.02 0.36
0 3 17 2.43 0.00 2.74
1 3 17 20.76 19.63 0.37
2 3 17 5.90 6.10 0.63
3 3 17 11.20 11.73 0.42
4 3 17 1.78 0.00 3.57
-4 4 17 11.70 12.39 0.41
-3 4 17 15.62 15.42 0.33
-2 4 17 9.58 9.77 0.43
-1 4 17 13.61 14.78 0.42
0 4 17 1.13 0.00 5.67
1 4 17 1.10 0.00 3.30
2 4 17 14.72 15.85 0.40
3 4 17 2.83 0.00 2.20
-3 5 17 0.89 0.00 6.68
-2 5 17 4.25 0.00 0.90
-1 5 17 5.61 5.82 0.56
0 5 17 7.16 8.35 0.52
1 5 17 -3.75 0.00 1.74
2 5 17 7.89 8.79 0.56
-1 6 17 10.10 11.74 0.46
0 6 17 5.88 7.02 0.68
-2 0 18 21.68 22.77 0.37
0 0 18 10.38 11.32 0.40
2 0 18 2.45 0.00 2.45
-3 1 18 18.66 19.67 0.35
-2 1 18 7.74 8.41 0.57
-1 1 18 7.35 7.78 0.55
0 1 18 8.41 8.31 0.49
1 1 18 6.44 6.26 0.67
2 1 18 5.69 5.03 0.66
-2 2 18 11.06 11.06 0.42
-1 2 18 15.98 16.35 0.38
0 2 18 4.85 3.52 0.78
1 2 18 9.05 9.30 0.49
-1 3 18 -3.45 0.00 1.03
0 3 18 14.92 16.54 0.41
1 3 18 1.94 0.00 2.91
|
1501616.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/16/1501616.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_1501616
loop_
_publ_author_name
'Eric Gagnon'
'Thierry Maris'
'Kenneth E. Maly'
'James D. Wuest'
_publ_section_title
;
The potential of intermolecular N/O interactions of nitro groups in
crystal engineering, as revealed by structures of
hexakis(4-nitrophenyl)benzene
;
_journal_name_full Tetrahedron
_journal_page_first 6603
_journal_page_last 6613
_journal_paper_doi 10.1016/j.tet.2007.03.101
_journal_volume 63
_journal_year 2007
_chemical_compound_source 'Synthesized by the authors. See text'
_chemical_formula_moiety 'C42 H24 N6 O12 7(C6 H6)'
_chemical_formula_sum 'C84 H66 N6 O12'
_chemical_formula_weight 1351.43
_chemical_name_systematic
;
?
;
_space_group_IT_number 2
_symmetry_cell_setting triclinic
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 84.436(5)
_cell_angle_beta 83.004(5)
_cell_angle_gamma 68.693(5)
_cell_formula_units_Z 2
_cell_length_a 11.1911(9)
_cell_length_b 13.9932(11)
_cell_length_c 24.378(2)
_cell_measurement_reflns_used 8790
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 68.81
_cell_measurement_theta_min 3.40
_cell_volume 3524.4(5)
_computing_cell_refinement 'SMART (Bruker, 2003)'
_computing_data_collection 'SMART (Bruker, 2003)'
_computing_data_reduction 'SAINT (Bruker, 2004)'
_computing_molecular_graphics 'SHELXTL (Bruker, 1997)'
_computing_publication_material 'UdMX (local program)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.903
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_device_type 'Bruker Smart 6000'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator 'Montel 200 optics'
_diffrn_radiation_source 'Rotating Anode'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.069
_diffrn_reflns_av_sigmaI/netI 0.1064
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_l_max 29
_diffrn_reflns_limit_l_min -29
_diffrn_reflns_number 46735
_diffrn_reflns_theta_full 68.47
_diffrn_reflns_theta_max 68.47
_diffrn_reflns_theta_min 1.83
_diffrn_standards_decay_% 0.40
_diffrn_standards_interval_time 1440
_diffrn_standards_number 1
_exptl_absorpt_coefficient_mu 0.697
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_correction_T_min 0.6000
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Sadabs (Sheldrick,1996)'
_exptl_crystal_colour Colorless
_exptl_crystal_density_diffrn 1.273
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 1416
_exptl_crystal_size_max 0.22
_exptl_crystal_size_mid 0.18
_exptl_crystal_size_min 0.12
_refine_diff_density_max 0.262
_refine_diff_density_min -0.273
_refine_diff_density_rms 0.064
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.051
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 919
_refine_ls_number_reflns 11726
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.051
_refine_ls_R_factor_all 0.0734
_refine_ls_R_factor_gt 0.0650
_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^)+(0.0450P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1447
_refine_ls_wR_factor_ref 0.1465
_reflns_number_gt 6567
_reflns_number_total 11726
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file deposit.cif
_cod_data_source_block jw1105
_cod_original_cell_volume 3524.5(5)
_cod_original_sg_symbol_H-M P-1
_cod_database_code 1501616
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
N1 N 1.1940(2) -0.24375(17) 0.67801(10) 0.0579(6) Uani 1 1 d .
N2 N 1.0978(2) -0.1186(2) 0.95191(11) 0.0719(7) Uani 1 1 d .
N3 N 0.62217(19) 0.37431(18) 1.03339(9) 0.0557(5) Uani 1 1 d .
N4 N 0.3018(2) 0.74227(19) 0.81811(10) 0.0677(7) Uani 1 1 d .
N5 N 0.4090(2) 0.60699(16) 0.54336(9) 0.0536(5) Uani 1 1 d .
N6 N 0.8696(2) 0.12101(16) 0.46626(8) 0.0502(5) Uani 1 1 d .
O1 O 1.15313(19) -0.30478(16) 0.66264(10) 0.0796(6) Uani 1 1 d .
O2 O 1.31057(16) -0.26213(14) 0.68142(8) 0.0624(5) Uani 1 1 d .
O3 O 1.0873(2) -0.20132(19) 0.95687(10) 0.0959(8) Uani 1 1 d .
O4 O 1.1684(2) -0.09274(19) 0.97705(10) 0.0912(7) Uani 1 1 d .
O5 O 0.58019(19) 0.31945(16) 1.06697(8) 0.0710(5) Uani 1 1 d .
O6 O 0.6404(2) 0.44833(16) 1.04605(8) 0.0746(6) Uani 1 1 d .
O7 O 0.1910(2) 0.75235(18) 0.83307(11) 0.0952(8) Uani 1 1 d .
O8 O 0.3414(2) 0.81294(15) 0.81169(9) 0.0779(6) Uani 1 1 d .
O9 O 0.28842(17) 0.62840(14) 0.54453(8) 0.0672(5) Uani 1 1 d .
O10 O 0.47016(17) 0.64364(14) 0.50735(8) 0.0671(5) Uani 1 1 d .
O11 O 0.97924(18) 0.10742(15) 0.44244(8) 0.0668(5) Uani 1 1 d .
O12 O 0.78091(18) 0.11661(15) 0.44261(7) 0.0647(5) Uani 1 1 d .
C1 C 0.83573(19) 0.14944(17) 0.73556(9) 0.0371(5) Uani 1 1 d .
C2 C 0.8073(2) 0.17694(17) 0.79203(9) 0.0406(5) Uani 1 1 d .
C3 C 0.71995(19) 0.27475(17) 0.80503(9) 0.0374(5) Uani 1 1 d .
C4 C 0.6562(2) 0.34415(18) 0.76384(10) 0.0426(5) Uani 1 1 d .
C5 C 0.6833(2) 0.31714(17) 0.70742(9) 0.0434(6) Uani 1 1 d .
C6 C 0.7706(2) 0.21918(17) 0.69411(9) 0.0399(5) Uani 1 1 d .
C7 C 0.9268(2) 0.04591(18) 0.72148(9) 0.0413(5) Uani 1 1 d .
C8 C 1.0580(2) 0.02076(18) 0.72801(10) 0.0466(6) Uani 1 1 d .
H8 H 1.0860 0.0693 0.7420 0.056 Uiso 1 1 calc R
C9 C 1.1479(2) -0.07591(19) 0.71392(11) 0.0523(7) Uani 1 1 d .
H9 H 1.2367 -0.0940 0.7184 0.063 Uiso 1 1 calc R
C10 C 1.1038(2) -0.14240(18) 0.69370(9) 0.0440(6) Uani 1 1 d .
C11 C 0.9724(2) -0.12034(18) 0.68724(10) 0.0456(6) Uani 1 1 d .
H11 H 0.9442 -0.1694 0.6739 0.055 Uiso 1 1 calc R
C12 C 0.8871(2) -0.02473(18) 0.70108(9) 0.0439(5) Uani 1 1 d .
H12 H 0.7985 -0.0071 0.6964 0.053 Uiso 1 1 calc R
C13 C 0.8744(2) 0.10101(19) 0.83547(10) 0.0481(6) Uani 1 1 d .
C14 C 0.9649(2) 0.1226(2) 0.86615(10) 0.0535(6) Uani 1 1 d .
H14 H 0.9756 0.1872 0.8603 0.064 Uiso 1 1 calc R
C15 C 1.0335(2) 0.0513(2) 0.90291(12) 0.0625(7) Uani 1 1 d .
H15 H 1.0933 0.0656 0.9223 0.075 Uiso 1 1 calc R
C16 C 1.0171(2) -0.0414(2) 0.91234(10) 0.0554(7) Uani 1 1 d .
C17 C 0.9298(2) -0.0654(2) 0.88434(11) 0.0574(7) Uani 1 1 d .
H17 H 0.9195 -0.1301 0.8912 0.069 Uiso 1 1 calc R
C18 C 0.8598(2) 0.00664(18) 0.84681(9) 0.0464(6) Uani 1 1 d .
H18 H 0.7997 -0.0087 0.8281 0.056 Uiso 1 1 calc R
C19 C 0.6917(2) 0.30265(19) 0.86484(10) 0.0506(6) Uani 1 1 d .
C20 C 0.7178(2) 0.38564(19) 0.88076(10) 0.0493(6) Uani 1 1 d .
H20 H 0.7512 0.4258 0.8541 0.059 Uiso 1 1 calc R
C21 C 0.6935(2) 0.4098(2) 0.93777(10) 0.0507(6) Uani 1 1 d .
H21 H 0.7111 0.4659 0.9492 0.061 Uiso 1 1 calc R
C22 C 0.6454(2) 0.35200(18) 0.97514(10) 0.0449(6) Uani 1 1 d .
C23 C 0.6179(2) 0.26971(18) 0.96022(10) 0.0471(6) Uani 1 1 d .
H23 H 0.5839 0.2305 0.9873 0.057 Uiso 1 1 calc R
C24 C 0.6413(2) 0.24483(18) 0.90402(10) 0.0484(6) Uani 1 1 d .
H24 H 0.6226 0.1888 0.8931 0.058 Uiso 1 1 calc R
C25 C 0.5675(2) 0.44748(17) 0.77687(9) 0.0396(5) Uani 1 1 d .
C26 C 0.4464(2) 0.45807(19) 0.80832(10) 0.0471(6) Uani 1 1 d .
H26 H 0.4257 0.3989 0.8206 0.057 Uiso 1 1 calc R
C27 C 0.3595(2) 0.5557(2) 0.82065(11) 0.0532(6) Uani 1 1 d .
H27 H 0.2788 0.5640 0.8411 0.064 Uiso 1 1 calc R
C28 C 0.3926(2) 0.63888(19) 0.80287(10) 0.0493(6) Uani 1 1 d .
C29 C 0.5117(2) 0.63279(19) 0.77177(11) 0.0512(6) Uani 1 1 d .
H29 H 0.5323 0.6923 0.7603 0.061 Uiso 1 1 calc R
C30 C 0.5954(2) 0.53508(18) 0.75939(11) 0.0534(6) Uani 1 1 d .
H30 H 0.6749 0.5277 0.7381 0.064 Uiso 1 1 calc R
C31 C 0.6137(2) 0.39010(17) 0.66385(10) 0.0429(5) Uani 1 1 d .
C32 C 0.4779(2) 0.42026(18) 0.66514(10) 0.0470(6) Uani 1 1 d .
H32 H 0.4328 0.3908 0.6931 0.056 Uiso 1 1 calc R
C33 C 0.4103(2) 0.49186(17) 0.62641(10) 0.0473(6) Uani 1 1 d .
H33 H 0.3191 0.5137 0.6281 0.057 Uiso 1 1 calc R
C34 C 0.4795(2) 0.53146(17) 0.58460(10) 0.0447(6) Uani 1 1 d .
C35 C 0.61289(19) 0.50207(17) 0.58130(10) 0.0432(6) Uani 1 1 d .
H35 H 0.6580 0.5297 0.5524 0.052 Uiso 1 1 calc R
C36 C 0.6774(2) 0.43267(17) 0.62060(9) 0.0444(6) Uani 1 1 d .
H36 H 0.7685 0.4124 0.6187 0.053 Uiso 1 1 calc R
C37 C 0.7957(2) 0.18907(17) 0.63506(9) 0.0403(5) Uani 1 1 d .
C38 C 0.6993(2) 0.17676(17) 0.60810(9) 0.0434(5) Uani 1 1 d .
H38 H 0.6179 0.1836 0.6274 0.052 Uiso 1 1 calc R
C39 C 0.7250(2) 0.15409(16) 0.55194(9) 0.0412(5) Uani 1 1 d .
H39 H 0.6606 0.1467 0.5325 0.049 Uiso 1 1 calc R
C40 C 0.8477(2) 0.14248(17) 0.52502(10) 0.0423(5) Uani 1 1 d .
C41 C 0.9415(2) 0.15458(17) 0.55047(10) 0.0469(6) Uani 1 1 d .
H41 H 1.0226 0.1474 0.5307 0.056 Uiso 1 1 calc R
C42 C 0.9181(2) 0.17774(17) 0.60623(9) 0.0409(5) Uani 1 1 d .
H42 H 0.9835 0.1858 0.6247 0.049 Uiso 1 1 calc R
C50 C 0.7334(3) 0.9126(3) 0.39811(13) 0.0712(8) Uani 1 1 d .
H50 H 0.7702 0.9644 0.3899 0.085 Uiso 1 1 calc R
C51 C 0.6770(3) 0.8983(3) 0.45193(14) 0.0772(9) Uani 1 1 d .
H51 H 0.6729 0.9424 0.4799 0.093 Uiso 1 1 calc R
C52 C 0.6274(3) 0.8201(2) 0.46404(14) 0.0730(9) Uani 1 1 d .
H52 H 0.5914 0.8096 0.5005 0.088 Uiso 1 1 calc R
C53 C 0.6305(2) 0.7585(2) 0.42350(13) 0.0671(8) Uani 1 1 d .
H53 H 0.5971 0.7049 0.4322 0.081 Uiso 1 1 calc R
C54 C 0.6807(3) 0.7721(3) 0.37043(14) 0.0744(9) Uani 1 1 d .
H54 H 0.6798 0.7297 0.3424 0.089 Uiso 1 1 calc R
C55 C 0.7339(3) 0.8498(3) 0.35790(14) 0.0748(9) Uani 1 1 d .
H55 H 0.7703 0.8588 0.3214 0.090 Uiso 1 1 calc R
C60 C 0.9466(2) 0.6920(2) 0.04961(12) 0.0655(8) Uani 1 1 d .
H60 H 1.0204 0.7105 0.0492 0.079 Uiso 1 1 calc R
C61 C 0.9555(3) 0.5927(2) 0.06271(12) 0.0648(8) Uani 1 1 d .
H61 H 1.0365 0.5418 0.0696 0.078 Uiso 1 1 calc R
C62 C 0.8452(2) 0.5652(2) 0.06604(12) 0.0646(8) Uani 1 1 d .
H62 H 0.8526 0.4955 0.0736 0.077 Uiso 1 1 calc R
C63 C 0.7287(2) 0.6386(2) 0.05841(13) 0.0688(8) Uani 1 1 d .
H63 H 0.6528 0.6220 0.0631 0.083 Uiso 1 1 calc R
C64 C 0.7228(3) 0.7373(2) 0.04376(12) 0.0653(8) Uani 1 1 d .
H64 H 0.6418 0.7891 0.0379 0.078 Uiso 1 1 calc R
C65 C 0.8340(3) 0.7635(3) 0.03727(12) 0.0686(8) Uani 1 1 d .
H65 H 0.8294 0.8309 0.0243 0.082 Uiso 1 1 calc R
C70 C 0.5805(2) 0.9915(2) 0.23456(11) 0.0571(7) Uani 1 1 d .
H70 H 0.5724 1.0510 0.2526 0.069 Uiso 1 1 calc R
C71 C 0.4969(2) 0.9326(2) 0.25415(12) 0.0557(7) Uani 1 1 d .
H71 H 0.4371 0.9533 0.2858 0.067 Uiso 1 1 calc R
C72 C 0.5028(2) 0.8555(2) 0.23002(11) 0.0586(7) Uani 1 1 d .
H72 H 0.4405 0.8237 0.2392 0.070 Uiso 1 1 calc R
C73 C 0.6006(2) 0.8195(2) 0.19070(11) 0.0568(7) Uani 1 1 d .
H73 H 0.6200 0.7539 0.1767 0.068 Uiso 1 1 calc R
C74 C 0.6744(2) 0.8817(2) 0.17049(12) 0.0611(7) Uani 1 1 d .
H74 H 0.7331 0.8606 0.1386 0.073 Uiso 1 1 calc R
C75 C 0.6685(2) 0.9610(2) 0.19101(12) 0.0597(7) Uani 1 1 d .
H75 H 0.7228 0.9981 0.1768 0.072 Uiso 1 1 calc R
C80 C 0.9358(2) 0.6464(2) 0.22586(11) 0.0540(7) Uani 1 1 d .
H80 H 0.9352 0.6952 0.1959 0.065 Uiso 1 1 calc R
C81 C 1.0010(2) 0.6428(2) 0.27190(11) 0.0543(7) Uani 1 1 d .
H81 H 1.0445 0.6895 0.2734 0.065 Uiso 1 1 calc R
C82 C 1.0021(2) 0.5709(2) 0.31541(11) 0.0543(7) Uani 1 1 d .
H82 H 1.0473 0.5676 0.3465 0.065 Uiso 1 1 calc R
C83 C 0.9368(2) 0.5033(2) 0.31362(12) 0.0567(7) Uani 1 1 d .
H83 H 0.9365 0.4548 0.3437 0.068 Uiso 1 1 calc R
C84 C 0.8721(2) 0.5071(2) 0.26786(11) 0.0558(7) Uani 1 1 d .
H84 H 0.8281 0.4608 0.2665 0.067 Uiso 1 1 calc R
C85 C 0.8720(2) 0.5785(2) 0.22419(11) 0.0549(7) Uani 1 1 d .
H85 H 0.8278 0.5809 0.1929 0.066 Uiso 1 1 calc R
C90 C 0.2619(2) 0.2961(2) 0.38449(12) 0.0653(8) Uani 1 1 d .
H90 H 0.2156 0.3681 0.3836 0.078 Uiso 1 1 calc R
C91 C 0.1935(3) 0.2291(2) 0.40077(12) 0.0644(8) Uani 1 1 d .
H91 H 0.1036 0.2546 0.4115 0.077 Uiso 1 1 calc R
C92 C 0.2637(2) 0.1240(2) 0.40039(12) 0.0638(8) Uani 1 1 d .
H92 H 0.2212 0.0762 0.4101 0.077 Uiso 1 1 calc R
C93 C 0.3955(2) 0.0891(2) 0.38584(11) 0.0601(7) Uani 1 1 d .
H93 H 0.4426 0.0173 0.3863 0.072 Uiso 1 1 calc R
C94 C 0.4602(3) 0.1572(2) 0.37062(13) 0.0688(8) Uani 1 1 d .
H94 H 0.5505 0.1321 0.3607 0.083 Uiso 1 1 calc R
C95 C 0.3916(3) 0.2617(2) 0.37003(12) 0.0667(8) Uani 1 1 d .
H95 H 0.4343 0.3092 0.3597 0.080 Uiso 1 1 calc R
C100 C 0.1168(6) 0.2785(4) 0.1970(2) 0.157(2) Uani 1 1 d .
H100 H 0.0574 0.2765 0.2281 0.189 Uiso 1 1 calc R
C101 C 0.0733(3) 0.3200(3) 0.14589(15) 0.0793(9) Uani 1 1 d .
H101 H -0.0165 0.3464 0.1420 0.095 Uiso 1 1 calc R
C102 C 0.1589(3) 0.3234(2) 0.10073(14) 0.0736(9) Uani 1 1 d .
H102 H 0.1275 0.3523 0.0661 0.088 Uiso 1 1 calc R
C103 C 0.2917(3) 0.2847(2) 0.10540(14) 0.0764(9) Uani 1 1 d .
H103 H 0.3507 0.2871 0.0743 0.092 Uiso 1 1 calc R
C104 C 0.3360(3) 0.2422(2) 0.15683(13) 0.0720(8) Uani 1 1 d .
H104 H 0.4260 0.2150 0.1605 0.086 Uiso 1 1 calc R
C105 C 0.2505(3) 0.2394(3) 0.20214(15) 0.0763(9) Uani 1 1 d .
H105 H 0.2816 0.2110 0.2369 0.092 Uiso 1 1 calc R
C110 C 0.9458(2) 0.4247(2) 0.49935(12) 0.0618(7) Uani 1 1 d .
H110 H 0.9074 0.3741 0.5003 0.074 Uiso 1 1 calc R
C111 C 0.8896(2) 0.5209(2) 0.47257(12) 0.0587(7) Uani 1 1 d .
H111 H 0.8166 0.5348 0.4527 0.070 Uiso 1 1 calc R
C112 C 0.9423(2) 0.5967(2) 0.47546(12) 0.0596(7) Uani 1 1 d .
H112 H 0.9006 0.6639 0.4599 0.072 Uiso 1 1 calc R
C113 C 0.6165(2) 0.0126(2) -0.01934(12) 0.0600(7) Uani 1 1 d .
H113 H 0.6948 0.0228 -0.0324 0.072 Uiso 1 1 calc R
C114 C 0.5645(2) 0.0345(2) 0.03619(12) 0.0617(7) Uani 1 1 d .
H114 H 0.6079 0.0563 0.0608 0.074 Uiso 1 1 calc R
C115 C 0.4406(2) 0.0218(2) 0.05367(13) 0.0632(7) Uani 1 1 d .
H115 H 0.4007 0.0382 0.0899 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
N1 0.0730(13) 0.0387(12) 0.0559(15) -0.0032(12) -0.0036(12) -0.0133(13)
N2 0.0826(15) 0.0601(17) 0.0629(17) 0.0177(15) -0.0018(14) -0.0202(15)
N3 0.0674(12) 0.0473(13) 0.0493(14) -0.0038(13) -0.0024(11) -0.0175(12)
N4 0.0842(15) 0.0452(14) 0.0615(17) 0.0058(13) 0.0010(13) -0.0133(15)
N5 0.0704(11) 0.0409(12) 0.0492(13) 0.0114(11) -0.0125(11) -0.0209(12)
N6 0.0671(12) 0.0429(12) 0.0329(12) 0.0025(11) -0.0044(10) -0.0116(12)
O1 0.0874(12) 0.0568(13) 0.0941(17) -0.0223(13) -0.0033(12) -0.0222(12)
O2 0.0630(9) 0.0516(11) 0.0655(13) -0.0015(10) -0.0099(10) -0.0112(10)
O3 0.0926(14) 0.0827(16) 0.099(2) 0.0367(15) -0.0174(14) -0.0235(14)
O4 0.0933(15) 0.0940(18) 0.0730(16) 0.0123(14) -0.0231(13) -0.0171(15)
O5 0.0962(13) 0.0701(13) 0.0486(12) -0.0040(11) -0.0010(10) -0.0334(12)
O6 0.1066(14) 0.0620(13) 0.0632(14) -0.0131(12) -0.0096(11) -0.0364(13)
O7 0.0892(14) 0.0735(15) 0.106(2) 0.0033(14) 0.0119(14) -0.0183(14)
O8 0.1021(14) 0.0461(12) 0.0786(16) -0.0038(11) -0.0129(12) -0.0168(12)
O9 0.0701(10) 0.0600(12) 0.0662(13) 0.0190(11) -0.0155(10) -0.0197(11)
O10 0.0752(10) 0.0625(12) 0.0574(12) 0.0238(10) -0.0055(10) -0.0240(11)
O11 0.0769(11) 0.0694(13) 0.0489(11) -0.0125(11) 0.0089(10) -0.0221(11)
O12 0.0877(12) 0.0650(13) 0.0414(11) -0.0086(10) -0.0032(10) -0.0266(12)
C1 0.0520(10) 0.0317(12) 0.0277(11) 0.0024(11) 0.0047(10) -0.0187(11)
C2 0.0585(12) 0.0269(12) 0.0310(12) -0.0025(11) -0.0008(10) -0.0098(11)
C3 0.0534(11) 0.0294(12) 0.0285(12) 0.0002(11) -0.0027(10) -0.0145(11)
C4 0.0595(12) 0.0340(13) 0.0354(13) 0.0008(12) -0.0078(11) -0.0175(12)
C5 0.0582(12) 0.0337(13) 0.0340(13) 0.0044(12) 0.0058(11) -0.0161(12)
C6 0.0532(11) 0.0291(12) 0.0313(12) 0.0013(11) 0.0052(10) -0.0113(11)
C7 0.0531(11) 0.0356(13) 0.0280(11) 0.0020(11) 0.0007(10) -0.0097(12)
C8 0.0605(12) 0.0312(12) 0.0465(15) 0.0031(12) -0.0029(12) -0.0164(12)
C9 0.0611(13) 0.0398(14) 0.0495(16) 0.0084(13) 0.0012(12) -0.0147(13)
C10 0.0636(13) 0.0340(13) 0.0326(13) 0.0016(12) -0.0044(11) -0.0162(13)
C11 0.0572(12) 0.0344(13) 0.0431(14) 0.0023(12) -0.0033(11) -0.0152(12)
C12 0.0541(12) 0.0349(13) 0.0399(13) -0.0032(12) -0.0048(11) -0.0119(12)
C13 0.0577(12) 0.0429(14) 0.0328(13) 0.0068(12) -0.0054(11) -0.0070(12)
C14 0.0670(14) 0.0484(15) 0.0356(14) -0.0006(13) -0.0037(12) -0.0098(14)
C15 0.0671(14) 0.0544(17) 0.0566(18) 0.0053(15) -0.0052(14) -0.0127(15)
C16 0.0641(14) 0.0522(16) 0.0365(14) 0.0036(14) -0.0031(12) -0.0071(14)
C17 0.0692(14) 0.0443(15) 0.0446(15) 0.0130(13) 0.0062(13) -0.0108(14)
C18 0.0557(12) 0.0403(13) 0.0355(13) 0.0040(12) 0.0030(11) -0.0118(12)
C19 0.0635(13) 0.0353(13) 0.0400(14) -0.0024(13) -0.0042(12) -0.0024(12)
C20 0.0742(14) 0.0435(14) 0.0275(12) -0.0001(12) -0.0080(12) -0.0170(13)
C21 0.0654(13) 0.0412(14) 0.0398(14) -0.0021(13) -0.0100(12) -0.0106(13)
C22 0.0610(12) 0.0369(13) 0.0274(12) -0.0030(12) -0.0002(11) -0.0071(12)
C23 0.0653(13) 0.0361(13) 0.0306(13) 0.0067(12) -0.0079(11) -0.0081(12)
C24 0.0697(14) 0.0336(13) 0.0323(13) 0.0007(12) 0.0005(12) -0.0091(12)
C25 0.0595(12) 0.0322(12) 0.0272(11) 0.0012(11) -0.0069(10) -0.0162(12)
C26 0.0596(13) 0.0366(13) 0.0423(14) 0.0020(12) -0.0104(11) -0.0129(12)
C27 0.0627(13) 0.0485(15) 0.0460(15) 0.0004(14) 0.0004(12) -0.0196(14)
C28 0.0623(13) 0.0394(14) 0.0397(14) 0.0048(13) -0.0073(12) -0.0115(13)
C29 0.0630(13) 0.0367(14) 0.0546(16) -0.0041(13) 0.0005(12) -0.0199(13)
C30 0.0703(14) 0.0355(13) 0.0472(15) 0.0029(13) -0.0019(12) -0.0127(13)
C31 0.0594(12) 0.0281(12) 0.0440(14) -0.0044(12) 0.0013(11) -0.0203(12)
C32 0.0590(12) 0.0354(13) 0.0467(15) 0.0017(12) 0.0005(12) -0.0197(12)
C33 0.0657(13) 0.0302(12) 0.0424(14) 0.0014(12) -0.0102(12) -0.0121(12)
C34 0.0662(13) 0.0294(12) 0.0402(14) -0.0025(12) -0.0032(11) -0.0192(12)
C35 0.0528(11) 0.0347(13) 0.0429(14) 0.0007(12) -0.0005(11) -0.0185(12)
C36 0.0593(12) 0.0344(13) 0.0340(13) 0.0006(12) -0.0002(11) -0.0121(12)
C37 0.0534(11) 0.0304(12) 0.0311(12) 0.0012(11) -0.0045(10) -0.0084(11)
C38 0.0644(13) 0.0285(12) 0.0283(12) 0.0010(11) -0.0005(11) -0.0076(12)
C39 0.0661(13) 0.0277(11) 0.0267(12) 0.0054(11) -0.0055(11) -0.0144(12)
C40 0.0596(12) 0.0298(12) 0.0318(12) -0.0006(11) -0.0039(11) -0.0098(12)
C41 0.0605(12) 0.0341(13) 0.0360(13) -0.0031(12) 0.0038(12) -0.0069(12)
C42 0.0595(11) 0.0283(12) 0.0344(12) -0.0028(11) -0.0012(11) -0.0158(11)
C50 0.0693(16) 0.069(2) 0.071(2) -0.0047(19) -0.0053(16) -0.0202(17)
C51 0.0753(17) 0.077(2) 0.079(2) -0.002(2) -0.0071(17) -0.0275(18)
C52 0.0711(16) 0.075(2) 0.074(2) 0.000(2) -0.0106(16) -0.0264(18)
C53 0.0690(15) 0.0635(19) 0.069(2) -0.0040(18) -0.0070(15) -0.0239(16)
C54 0.0758(17) 0.078(2) 0.070(2) -0.0026(19) -0.0044(16) -0.0297(18)
C55 0.0750(17) 0.077(2) 0.073(2) -0.008(2) -0.0030(16) -0.0277(18)
C60 0.0659(15) 0.0619(19) 0.069(2) -0.0028(17) -0.0070(15) -0.0226(16)
C61 0.0699(16) 0.0622(19) 0.0635(19) -0.0046(17) -0.0094(15) -0.0235(16)
C62 0.0650(16) 0.0668(19) 0.0597(18) -0.0021(16) -0.0041(14) -0.0218(16)
C63 0.0684(16) 0.069(2) 0.068(2) -0.0055(18) -0.0033(15) -0.0237(17)
C64 0.0643(15) 0.0626(19) 0.0673(19) -0.0014(17) -0.0090(14) -0.0202(15)
C65 0.0699(17) 0.073(2) 0.0633(19) -0.0010(17) -0.0038(15) -0.0270(17)
C70 0.0557(13) 0.0626(18) 0.0526(16) -0.0008(15) -0.0059(13) -0.0209(14)
C71 0.0554(13) 0.0548(17) 0.0576(17) -0.0040(15) -0.0060(12) -0.0198(14)
C72 0.0615(14) 0.0558(17) 0.0570(17) -0.0021(16) -0.0030(13) -0.0202(15)
C73 0.0529(12) 0.0615(18) 0.0550(16) -0.0034(15) -0.0055(12) -0.0189(14)
C74 0.0604(14) 0.0667(19) 0.0569(17) -0.0034(16) -0.0063(13) -0.0230(15)
C75 0.0614(13) 0.0615(19) 0.0610(18) -0.0001(16) -0.0113(14) -0.0266(15)
C80 0.0577(13) 0.0545(16) 0.0514(16) -0.0048(14) -0.0042(12) -0.0216(14)
C81 0.0506(11) 0.0552(17) 0.0570(17) -0.0073(15) -0.0004(12) -0.0192(13)
C82 0.0525(12) 0.0524(16) 0.0563(16) -0.0005(14) -0.0063(12) -0.0168(13)
C83 0.0564(13) 0.0563(16) 0.0582(17) 0.0004(15) -0.0048(13) -0.0222(14)
C84 0.0519(12) 0.0585(17) 0.0554(16) -0.0004(15) -0.0062(12) -0.0180(13)
C85 0.0541(12) 0.0592(17) 0.0507(16) -0.0027(15) -0.0053(12) -0.0194(14)
C90 0.0626(14) 0.068(2) 0.0643(19) 0.0011(17) -0.0087(14) -0.0222(16)
C91 0.0652(15) 0.0617(18) 0.068(2) -0.0020(17) -0.0064(14) -0.0254(16)
C92 0.0594(14) 0.0624(19) 0.069(2) -0.0082(17) -0.0016(14) -0.0209(15)
C93 0.0587(13) 0.0632(18) 0.0588(17) -0.0051(16) -0.0033(13) -0.0225(15)
C94 0.0689(16) 0.069(2) 0.070(2) -0.0034(18) -0.0086(15) -0.0250(17)
C95 0.0657(15) 0.066(2) 0.069(2) -0.0019(17) -0.0098(14) -0.0242(17)
C100 0.166(5) 0.153(5) 0.145(5) 0.007(4) 0.002(4) -0.056(4)
C101 0.0737(17) 0.084(2) 0.076(2) -0.011(2) -0.0046(18) -0.0222(19)
C102 0.0729(16) 0.073(2) 0.075(2) -0.0052(19) -0.0074(16) -0.0256(18)
C103 0.0764(17) 0.076(2) 0.078(2) -0.0042(19) -0.0098(17) -0.0271(18)
C104 0.0698(16) 0.069(2) 0.076(2) -0.0037(19) -0.0066(17) -0.0232(17)
C105 0.0765(17) 0.074(2) 0.078(2) -0.0046(19) -0.0075(17) -0.0265(19)
C110 0.0632(14) 0.0627(18) 0.0625(18) -0.0055(16) -0.0054(14) -0.0255(15)
C111 0.0598(13) 0.0609(18) 0.0553(16) 0.0007(15) -0.0071(12) -0.0219(14)
C112 0.0597(13) 0.0578(17) 0.0608(18) 0.0001(15) -0.0093(13) -0.0200(14)
C113 0.0617(12) 0.0589(18) 0.0596(17) -0.0058(16) -0.0031(13) -0.0218(14)
C114 0.0585(14) 0.0623(18) 0.0631(18) -0.0035(16) -0.0062(14) -0.0199(15)
C115 0.0630(14) 0.0620(18) 0.0651(18) -0.0040(16) -0.0087(14) -0.0219(15)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 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_site_symmetry_1
_geom_angle
_geom_angle_publ_flag
O1 N1 O2 . 123.4(2) y
O1 N1 C10 . 119.5(2) y
O2 N1 C10 . 117.0(2) y
O3 N2 O4 . 125.2(3) y
O3 N2 C16 . 116.9(3) y
O4 N2 C16 . 117.9(3) y
O6 N3 O5 . 123.1(2) y
O6 N3 C22 . 117.7(2) y
O5 N3 C22 . 119.1(2) y
O7 N4 O8 . 123.7(3) y
O7 N4 C28 . 118.3(3) y
O8 N4 C28 . 117.9(2) y
O10 N5 O9 . 122.9(2) y
O10 N5 C34 . 118.52(19) y
O9 N5 C34 . 118.54(19) y
O12 N6 O11 . 122.8(2) y
O12 N6 C40 . 119.4(2) y
O11 N6 C40 . 117.7(2) y
C6 C1 C2 . 119.4(2) y
C6 C1 C7 . 120.29(19) y
C2 C1 C7 . 120.18(19) y
C3 C2 C1 . 119.80(19) y
C3 C2 C13 . 121.5(2) y
C1 C2 C13 . 118.6(2) y
C4 C3 C2 . 120.7(2) y
C4 C3 C19 . 120.2(2) y
C2 C3 C19 . 119.05(19) y
C3 C4 C5 . 119.9(2) y
C3 C4 C25 . 121.0(2) y
C5 C4 C25 . 119.00(19) y
C6 C5 C4 . 119.7(2) y
C6 C5 C31 . 120.4(2) y
C4 C5 C31 . 119.8(2) y
C1 C6 C5 . 120.4(2) y
C1 C6 C37 . 119.73(19) y
C5 C6 C37 . 119.84(19) y
C12 C7 C8 . 119.4(2) y
C12 C7 C1 . 121.96(19) y
C8 C7 C1 . 118.6(2) y
C7 C8 C9 . 120.3(2) y
C7 C8 H8 . 119.8 ?
C9 C8 H8 . 119.8 ?
C10 C9 C8 . 117.8(2) y
C10 C9 H9 . 121.1 ?
C8 C9 H9 . 121.1 ?
C9 C10 C11 . 123.4(2) y
C9 C10 N1 . 119.9(2) y
C11 C10 N1 . 116.7(2) y
C12 C11 C10 . 117.2(2) y
C12 C11 H11 . 121.4 ?
C10 C11 H11 . 121.4 ?
C7 C12 C11 . 121.8(2) y
C7 C12 H12 . 119.1 ?
C11 C12 H12 . 119.1 ?
C18 C13 C14 . 117.4(2) y
C18 C13 C2 . 122.8(2) y
C14 C13 C2 . 119.7(2) y
C15 C14 C13 . 120.4(3) y
C15 C14 H14 . 119.8 ?
C13 C14 H14 . 119.8 ?
C14 C15 C16 . 120.2(3) y
C14 C15 H15 . 119.9 ?
C16 C15 H15 . 119.9 ?
C15 C16 C17 . 121.5(3) y
C15 C16 N2 . 118.2(2) y
C17 C16 N2 . 120.3(3) y
C18 C17 C16 . 118.7(2) y
C18 C17 H17 . 120.7 ?
C16 C17 H17 . 120.7 ?
C17 C18 C13 . 121.8(2) y
C17 C18 H18 . 119.1 ?
C13 C18 H18 . 119.1 ?
C24 C19 C20 . 120.1(2) y
C24 C19 C3 . 120.0(2) y
C20 C19 C3 . 119.9(2) y
C19 C20 C21 . 119.4(2) y
C19 C20 H20 . 120.3 ?
C21 C20 H20 . 120.3 ?
C22 C21 C20 . 119.4(2) y
C22 C21 H21 . 120.3 ?
C20 C21 H21 . 120.3 ?
C21 C22 C23 . 122.2(2) y
C21 C22 N3 . 120.2(2) y
C23 C22 N3 . 117.6(2) y
C22 C23 C24 . 119.1(2) y
C22 C23 H23 . 120.5 ?
C24 C23 H23 . 120.5 ?
C19 C24 C23 . 119.8(2) y
C19 C24 H24 . 120.1 ?
C23 C24 H24 . 120.1 ?
C30 C25 C26 . 119.1(2) y
C30 C25 C4 . 122.4(2) y
C26 C25 C4 . 118.5(2) y
C27 C26 C25 . 119.6(2) y
C27 C26 H26 . 120.2 ?
C25 C26 H26 . 120.2 ?
C28 C27 C26 . 118.8(2) y
C28 C27 H27 . 120.6 ?
C26 C27 H27 . 120.6 ?
C27 C28 C29 . 124.0(2) y
C27 C28 N4 . 118.4(2) y
C29 C28 N4 . 117.6(2) y
C30 C29 C28 . 116.1(2) y
C30 C29 H29 . 122 ?
C28 C29 H29 . 122 ?
C29 C30 C25 . 122.5(2) y
C29 C30 H30 . 118.8 ?
C25 C30 H30 . 118.8 ?
C36 C31 C32 . 117.7(2) y
C36 C31 C5 . 122.3(2) y
C32 C31 C5 . 120.04(19) y
C33 C32 C31 . 121.0(2) y
C33 C32 H32 . 119.5 ?
C31 C32 H32 . 119.5 ?
C32 C33 C34 . 118.3(2) y
C32 C33 H33 . 120.8 ?
C34 C33 H33 . 120.8 ?
C35 C34 C33 . 122.2(2) y
C35 C34 N5 . 118.97(19) y
C33 C34 N5 . 118.8(2) y
C36 C35 C34 . 118.4(2) y
C36 C35 H35 . 120.8 ?
C34 C35 H35 . 120.8 ?
C35 C36 C31 . 122.3(2) y
C35 C36 H36 . 118.9 ?
C31 C36 H36 . 118.9 ?
C38 C37 C42 . 120.4(2) y
C38 C37 C6 . 120.9(2) y
C42 C37 C6 . 118.6(2) y
C37 C38 C39 . 118.9(2) y
C37 C38 H38 . 120.6 ?
C39 C38 H38 . 120.6 ?
C40 C39 C38 . 119.0(2) y
C40 C39 H39 . 120.5 ?
C38 C39 H39 . 120.5 ?
C41 C40 C39 . 122.8(2) y
C41 C40 N6 . 119.9(2) y
C39 C40 N6 . 117.2(2) y
C40 C41 C42 . 119.4(2) y
C40 C41 H41 . 120.3 ?
C42 C41 H41 . 120.3 ?
C41 C42 C37 . 119.6(2) y
C41 C42 H42 . 120.2 ?
C37 C42 H42 . 120.2 ?
C55 C50 C51 . 118.5(3) y
C55 C50 H50 . 120.8 ?
C51 C50 H50 . 120.8 ?
C52 C51 C50 . 120.3(3) y
C52 C51 H51 . 119.8 ?
C50 C51 H51 . 119.8 ?
C53 C52 C51 . 119.8(3) y
C53 C52 H52 . 120.1 ?
C51 C52 H52 . 120.1 ?
C52 C53 C54 . 121.6(3) y
C52 C53 H53 . 119.2 ?
C54 C53 H53 . 119.2 ?
C53 C54 C55 . 119.2(3) y
C53 C54 H54 . 120.4 ?
C55 C54 H54 . 120.4 ?
C50 C55 C54 . 120.6(3) y
C50 C55 H55 . 119.7 ?
C54 C55 H55 . 119.7 ?
C65 C60 C61 . 120.2(3) y
C65 C60 H60 . 119.9 ?
C61 C60 H60 . 119.9 ?
C60 C61 C62 . 120.5(3) y
C60 C61 H61 . 119.8 ?
C62 C61 H61 . 119.8 ?
C63 C62 C61 . 119.8(3) y
C63 C62 H62 . 120.1 ?
C61 C62 H62 . 120.1 ?
C62 C63 C64 . 118.6(3) y
C62 C63 H63 . 120.7 ?
C64 C63 H63 . 120.7 ?
C63 C64 C65 . 121.5(3) y
C63 C64 H64 . 119.2 ?
C65 C64 H64 . 119.2 ?
C60 C65 C64 . 119.0(3) y
C60 C65 H65 . 120.5 ?
C64 C65 H65 . 120.5 ?
C75 C70 C71 . 119.9(3) y
C75 C70 H70 . 120.1 ?
C71 C70 H70 . 120.1 ?
C72 C71 C70 . 121.4(3) y
C72 C71 H71 . 119.3 ?
C70 C71 H71 . 119.3 ?
C71 C72 C73 . 117.6(3) y
C71 C72 H72 . 121.2 ?
C73 C72 H72 . 121.2 ?
C72 C73 C74 . 118.6(3) y
C72 C73 H73 . 120.7 ?
C74 C73 H73 . 120.7 ?
C75 C74 C73 . 125.4(3) y
C75 C74 H74 . 117.3 ?
C73 C74 H74 . 117.3 ?
C74 C75 C70 . 116.0(3) y
C74 C75 H75 . 122 ?
C70 C75 H75 . 122 ?
C85 C80 C81 . 119.8(2) y
C85 C80 H80 . 120.1 ?
C81 C80 H80 . 120.1 ?
C82 C81 C80 . 119.7(2) y
C82 C81 H81 . 120.1 ?
C80 C81 H81 . 120.1 ?
C81 C82 C83 . 120.2(2) y
C81 C82 H82 . 119.9 ?
C83 C82 H82 . 119.9 ?
C84 C83 C82 . 120.0(2) y
C84 C83 H83 . 120 ?
C82 C83 H83 . 120 ?
C85 C84 C83 . 119.9(2) y
C85 C84 H84 . 120.1 ?
C83 C84 H84 . 120.1 ?
C80 C85 C84 . 120.5(2) y
C80 C85 H85 . 119.7 ?
C84 C85 H85 . 119.7 ?
C95 C90 C91 . 122.7(3) y
C95 C90 H90 . 118.6 ?
C91 C90 H90 . 118.6 ?
C92 C91 C90 . 117.2(3) y
C92 C91 H91 . 121.4 ?
C90 C91 H91 . 121.4 ?
C93 C92 C91 . 120.0(3) y
C93 C92 H92 . 120 ?
C91 C92 H92 . 120 ?
C92 C93 C94 . 121.3(3) y
C92 C93 H93 . 119.3 ?
C94 C93 H93 . 119.3 ?
C95 C94 C93 . 119.3(3) y
C95 C94 H94 . 120.3 ?
C93 C94 H94 . 120.3 ?
C90 C95 C94 . 119.4(3) y
C90 C95 H95 . 120.3 ?
C94 C95 H95 . 120.3 ?
C101 C100 C105 . 119.0(5) y
C101 C100 H100 . 120.5 ?
C105 C100 H100 . 120.5 ?
C102 C101 C100 . 120.8(4) y
C102 C101 H101 . 119.6 ?
C100 C101 H101 . 119.6 ?
C101 C102 C103 . 120.6(3) y
C101 C102 H102 . 119.7 ?
C103 C102 H102 . 119.7 ?
C102 C103 C104 . 118.8(3) y
C102 C103 H103 . 120.6 ?
C104 C103 H103 . 120.6 ?
C105 C104 C103 . 120.7(3) y
C105 C104 H104 . 119.7 ?
C103 C104 H104 . 119.7 ?
C104 C105 C100 . 120.2(4) y
C104 C105 H105 . 119.9 ?
C100 C105 H105 . 119.9 ?
C112 C110 C111 2_766 119.7(3) y
C112 C110 H110 2_766 120.1 ?
C111 C110 H110 . 120.1 ?
C110 C111 C112 . 119.0(3) y
C110 C111 H111 . 120.5 ?
C112 C111 H111 . 120.5 ?
C110 C112 C111 2_766 121.1(3) y
C110 C112 H112 2_766 119.5 ?
C111 C112 H112 . 119.5 ?
C115 C113 C114 2_655 122.3(2) y
C115 C113 H113 2_655 118.9 ?
C114 C113 H113 . 118.9 ?
C113 C114 C115 . 116.8(2) y
C113 C114 H114 . 121.6 ?
C115 C114 H114 . 121.6 ?
C113 C115 C114 2_655 120.8(3) y
C113 C115 H115 2_655 119.6 ?
C114 C115 H115 . 119.6 ?
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
N1 O1 . 1.211(3) y
N1 O2 . 1.247(3) y
N1 C10 . 1.465(3) y
N2 O3 . 1.199(3) y
N2 O4 . 1.225(3) y
N2 C16 . 1.488(3) y
N3 O6 . 1.200(3) y
N3 O5 . 1.236(3) y
N3 C22 . 1.456(3) y
N4 O7 . 1.210(3) y
N4 O8 . 1.213(3) y
N4 C28 . 1.486(3) y
N5 O10 . 1.235(2) y
N5 O9 . 1.269(2) y
N5 C34 . 1.460(3) y
N6 O12 . 1.230(3) y
N6 O11 . 1.248(2) y
N6 C40 . 1.465(3) y
C1 C6 . 1.406(3) y
C1 C2 . 1.432(3) y
C1 C7 . 1.481(3) y
C2 C3 . 1.402(3) y
C2 C13 . 1.487(3) y
C3 C4 . 1.394(3) y
C3 C19 . 1.512(3) y
C4 C5 . 1.429(3) y
C4 C25 . 1.465(3) y
C5 C6 . 1.405(3) y
C5 C31 . 1.480(3) y
C6 C37 . 1.504(3) y
C7 C12 . 1.375(3) y
C7 C8 . 1.405(3) y
C8 C9 . 1.406(3) y
C8 H8 . 0.95 ?
C9 C10 . 1.354(3) y
C9 H9 . 0.95 ?
C10 C11 . 1.414(3) y
C11 C12 . 1.377(3) y
C11 H11 . 0.95 ?
C12 H12 . 0.95 ?
C13 C18 . 1.386(3) y
C13 C14 . 1.459(3) y
C14 C15 . 1.351(4) y
C14 H14 . 0.95 ?
C15 C16 . 1.369(4) y
C15 H15 . 0.95 ?
C16 C17 . 1.406(4) y
C17 C18 . 1.374(3) y
C17 H17 . 0.95 ?
C18 H18 . 0.95 ?
C19 C24 . 1.391(3) y
C19 C20 . 1.395(3) y
C20 C21 . 1.432(3) y
C20 H20 . 0.95 ?
C21 C22 . 1.352(3) y
C21 H21 . 0.95 ?
C22 C23 . 1.385(3) y
C23 C24 . 1.416(3) y
C23 H23 . 0.95 ?
C24 H24 . 0.95 ?
C25 C30 . 1.388(3) y
C25 C26 . 1.439(3) y
C26 C27 . 1.395(3) y
C26 H26 . 0.95 ?
C27 C28 . 1.362(3) y
C27 H27 . 0.95 ?
C28 C29 . 1.429(3) y
C29 C30 . 1.385(3) y
C29 H29 . 0.95 ?
C30 H30 . 0.95 ?
C31 C36 . 1.407(3) y
C31 C32 . 1.419(3) y
C32 C33 . 1.381(3) y
C32 H32 . 0.95 ?
C33 C34 . 1.398(3) y
C33 H33 . 0.95 ?
C34 C35 . 1.391(3) y
C35 C36 . 1.364(3) y
C35 H35 . 0.95 ?
C36 H36 . 0.95 ?
C37 C38 . 1.398(3) y
C37 C42 . 1.423(3) y
C38 C39 . 1.407(3) y
C38 H38 . 0.95 ?
C39 C40 . 1.407(3) y
C39 H39 . 0.95 ?
C40 C41 . 1.351(3) y
C41 C42 . 1.400(3) y
C41 H41 . 0.95 ?
C42 H42 . 0.95 ?
C50 C55 . 1.378(4) y
C50 C51 . 1.414(4) y
C50 H50 . 0.95 ?
C51 C52 . 1.390(4) y
C51 H51 . 0.95 ?
C52 C53 . 1.362(4) y
C52 H52 . 0.95 ?
C53 C54 . 1.370(4) y
C53 H53 . 0.95 ?
C54 C55 . 1.411(4) y
C54 H54 . 0.95 ?
C55 H55 . 0.95 ?
C60 C65 . 1.341(4) y
C60 C61 . 1.365(4) y
C60 H60 . 0.95 ?
C61 C62 . 1.412(3) y
C61 H61 . 0.95 ?
C62 C63 . 1.355(4) y
C62 H62 . 0.95 ?
C63 C64 . 1.373(4) y
C63 H63 . 0.95 ?
C64 C65 . 1.407(3) y
C64 H64 . 0.95 ?
C65 H65 . 0.95 ?
C70 C75 . 1.344(4) y
C70 C71 . 1.469(3) y
C70 H70 . 0.95 ?
C71 C72 . 1.256(4) y
C71 H71 . 0.95 ?
C72 C73 . 1.345(3) y
C72 H72 . 0.95 ?
C73 C74 . 1.422(3) y
C73 H73 . 0.95 ?
C74 C75 . 1.238(4) y
C74 H74 . 0.95 ?
C75 H75 . 0.95 ?
C80 C85 . 1.387(3) y
C80 C81 . 1.399(3) y
C80 H80 . 0.95 ?
C81 C82 . 1.388(3) y
C81 H81 . 0.95 ?
C82 C83 . 1.395(3) y
C82 H82 . 0.95 ?
C83 C84 . 1.388(3) y
C83 H83 . 0.95 ?
C84 C85 . 1.388(3) y
C84 H84 . 0.95 ?
C85 H85 . 0.95 ?
C90 C95 . 1.365(3) y
C90 C91 . 1.413(4) y
C90 H90 . 0.95 ?
C91 C92 . 1.393(4) y
C91 H91 . 0.95 ?
C92 C93 . 1.387(3) y
C92 H92 . 0.95 ?
C93 C94 . 1.391(4) y
C93 H93 . 0.95 ?
C94 C95 . 1.383(4) y
C94 H94 . 0.95 ?
C95 H95 . 0.95 ?
C100 C101 . 1.390(6) y
C100 C105 . 1.411(6) y
C100 H100 . 0.95 ?
C101 C102 . 1.377(4) y
C101 H101 . 0.95 ?
C102 C103 . 1.400(4) y
C102 H102 . 0.95 ?
C103 C104 . 1.402(4) y
C103 H103 . 0.95 ?
C104 C105 . 1.378(4) y
C104 H104 . 0.95 ?
C105 H105 . 0.95 ?
C110 C112 2_766 1.383(3) y
C110 C111 . 1.396(4) y
C110 H110 . 0.95 ?
C111 C112 . 1.398(4) y
C111 H111 . 0.95 ?
C112 C110 2_766 1.383(3) y
C112 H112 . 0.95 ?
C113 C115 2_655 1.331(4) y
C113 C114 . 1.423(4) y
C113 H113 . 0.95 ?
C114 C115 . 1.469(3) y
C114 H114 . 0.95 ?
C115 C113 2_655 1.331(4) y
C115 H115 . 0.95 ?
|
1501617.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/16/1501617.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_1501617
loop_
_publ_author_name
'Eric Gagnon'
'Thierry Maris'
'Kenneth E. Maly'
'James D. Wuest'
_publ_section_title
;
The potential of intermolecular N/O interactions of nitro groups in
crystal engineering, as revealed by structures of
hexakis(4-nitrophenyl)benzene
;
_journal_name_full Tetrahedron
_journal_page_first 6603
_journal_page_last 6613
_journal_paper_doi 10.1016/j.tet.2007.03.101
_journal_volume 63
_journal_year 2007
_chemical_formula_moiety 'C42 H24 N6 O12, 7(C4 H8 O2)'
_chemical_formula_sum 'C70 H80 N6 O26'
_chemical_formula_weight 1421.40
_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 105.10(3)
_cell_angle_beta 108.37(3)
_cell_angle_gamma 110.42(3)
_cell_formula_units_Z 1
_cell_length_a 11.533(2)
_cell_length_b 13.037(3)
_cell_length_c 14.014(3)
_cell_measurement_reflns_used 1100
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 66.62
_cell_measurement_theta_min 5.10
_cell_volume 1703.7(11)
_computing_cell_refinement 'SMART (Bruker, 2003)'
_computing_data_collection 'SMART (Bruker, 2003)'
_computing_data_reduction 'SAINT (Bruker, 2004)'
_computing_molecular_graphics 'SHELXTL (Bruker, 1997)'
_computing_publication_material 'UdMX (local program)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.875
_diffrn_measured_fraction_theta_max 0.875
_diffrn_measurement_device_type 'Bruker Microstar'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator 'Helios optics'
_diffrn_radiation_source 'Micro source'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.026
_diffrn_reflns_av_sigmaI/netI 0.0207
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_number 6484
_diffrn_reflns_theta_full 67.06
_diffrn_reflns_theta_max 66.71
_diffrn_reflns_theta_min 3.66
_diffrn_standards_decay_% 0.00
_diffrn_standards_number 5
_exptl_absorpt_coefficient_mu 0.897
_exptl_absorpt_correction_T_max 0.9200
_exptl_absorpt_correction_T_min 0.7100
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Sadabs (Sheldrick,1996)'
_exptl_crystal_colour Colorless
_exptl_crystal_density_diffrn 1.385
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 750
_exptl_crystal_size_max 0.20
_exptl_crystal_size_mid 0.08
_exptl_crystal_size_min 0.08
_refine_diff_density_max 0.251
_refine_diff_density_min -0.257
_refine_diff_density_rms 0.066
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.978
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 460
_refine_ls_number_reflns 5328
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.978
_refine_ls_R_factor_all 0.0602
_refine_ls_R_factor_gt 0.0567
_refine_ls_shift/su_max 0.004
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0719P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1321
_refine_ls_wR_factor_ref 0.1327
_reflns_number_gt 3740
_reflns_number_total 5328
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file deposit.cif
_cod_data_source_block jw1177
_cod_original_cell_volume 1703.7(10)
_cod_original_sg_symbol_H-M P-1
_cod_database_code 1501617
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
O10 O 0.10518(19) 0.20903(17) 0.54793(13) 0.0629(5) Uani 1 1 d .
O11 O 0.2144(2) 0.10811(19) 0.54967(16) 0.0786(7) Uani 1 1 d .
O20 O -0.5040(2) -0.36667(17) 0.37373(12) 0.0821(7) Uani 1 1 d .
O21 O -0.4081(2) -0.47485(18) 0.39048(14) 0.0994(9) Uani 1 1 d .
O30 O 0.69553(18) 0.55634(18) 1.18655(18) 0.0855(6) Uani 1 1 d .
O31 O 0.56526(19) 0.63684(15) 1.14825(16) 0.0685(5) Uani 1 1 d .
N10 N 0.14728(17) 0.14688(15) 0.58268(13) 0.0358(4) Uani 1 1 d .
N20 N -0.42380(18) -0.39116(16) 0.42824(13) 0.0398(4) Uani 1 1 d .
N30 N 0.58135(19) 0.55162(16) 1.15356(14) 0.0418(4) Uani 1 1 d .
C1 C 0.02449(19) 0.02910(17) 0.91751(14) 0.0309(4) Uani 1 1 d .
C2 C -0.08546(19) -0.07905(18) 0.88852(14) 0.0304(4) Uani 1 1 d .
C3 C 0.11293(19) 0.11036(17) 1.02841(14) 0.0311(4) Uani 1 1 d .
C10 C 0.1145(2) 0.11547(18) 0.66794(15) 0.0343(4) Uani 1 1 d .
C11 C 0.1701(2) 0.05272(19) 0.71144(15) 0.0370(5) Uani 1 1 d .
H11 H 0.2290 0.0290 0.6878 0.044 Uiso 1 1 calc R
C12 C 0.1378(2) 0.02384(18) 0.79268(15) 0.0347(4) Uani 1 1 d .
H12 H 0.1733 -0.0222 0.8230 0.042 Uiso 1 1 calc R
C13 C 0.05642(19) 0.06086(18) 0.82870(14) 0.0324(4) Uani 1 1 d .
C14 C 0.0054(2) 0.12668(19) 0.78469(16) 0.0404(5) Uani 1 1 d .
H14 H -0.0497 0.1543 0.8106 0.049 Uiso 1 1 calc R
C15 C 0.0336(2) 0.15399(19) 0.70140(15) 0.0392(5) Uani 1 1 d .
H15 H -0.0033 0.1984 0.6695 0.047 Uiso 1 1 calc R
C20 C -0.17954(19) -0.16591(17) 0.76933(14) 0.0299(4) Uani 1 1 d .
C21 C -0.2813(2) -0.14710(19) 0.70641(16) 0.0414(5) Uani 1 1 d .
H21 H -0.2964 -0.0827 0.7397 0.050 Uiso 1 1 calc R
C22 C -0.3631(2) -0.2217(2) 0.59382(16) 0.0429(5) Uani 1 1 d .
H22 H -0.4333 -0.2086 0.5498 0.051 Uiso 1 1 calc R
C23 C -0.3398(2) -0.31332(18) 0.54901(15) 0.0333(4) Uani 1 1 d .
C24 C -0.2396(2) -0.3351(2) 0.60905(16) 0.0413(5) Uani 1 1 d .
H24 H -0.2257 -0.4002 0.5755 0.050 Uiso 1 1 calc R
C25 C -0.1581(2) -0.25850(18) 0.72150(15) 0.0353(5) Uani 1 1 d .
H25 H -0.0870 -0.2711 0.7650 0.042 Uiso 1 1 calc R
C30 C 0.2334(2) 0.22506(18) 1.05863(14) 0.0323(4) Uani 1 1 d .
C31 C 0.3601(2) 0.2307(2) 1.08398(16) 0.0419(5) Uani 1 1 d .
H31 H 0.3704 0.1607 1.0805 0.050 Uiso 1 1 calc R
C32 C 0.4759(2) 0.3397(2) 1.11533(17) 0.0467(5) Uani 1 1 d .
H32 H 0.5648 0.3443 1.1351 0.056 Uiso 1 1 calc R
C33 C 0.4598(2) 0.4378(2) 1.11723(16) 0.0393(5) Uani 1 1 d .
C34 C 0.3346(2) 0.4342(2) 1.08947(17) 0.0426(5) Uani 1 1 d .
H34 H 0.3241 0.5034 1.0897 0.051 Uiso 1 1 calc R
C35 C 0.2224(2) 0.32716(19) 1.06080(16) 0.0402(5) Uani 1 1 d .
H35 H 0.1341 0.3239 1.0418 0.048 Uiso 1 1 calc R
O40 O 0.37169(19) 0.96719(16) 0.06921(16) 0.0683(5) Uani 1 1 d .
O43 O 0.30547(18) 0.73386(15) 0.05723(15) 0.0667(5) Uani 1 1 d .
C41 C 0.4650(3) 0.9148(3) 0.0721(2) 0.0696(8) Uani 1 1 d .
H41A H 0.4512 0.8755 -0.0042 0.084 Uiso 1 1 calc R
H41B H 0.5618 0.9801 0.1161 0.084 Uiso 1 1 calc R
C42 C 0.4439(3) 0.8290(3) 0.1182(2) 0.0651(7) Uani 1 1 d .
H42A H 0.4633 0.8689 0.1960 0.078 Uiso 1 1 calc R
H42B H 0.5089 0.7956 0.1174 0.078 Uiso 1 1 calc R
C44 C 0.2147(3) 0.7859(3) 0.0573(2) 0.0689(7) Uani 1 1 d .
H44A H 0.1175 0.7211 0.0161 0.083 Uiso 1 1 calc R
H44B H 0.2326 0.8275 0.1344 0.083 Uiso 1 1 calc R
C45 C 0.2330(3) 0.8699(3) 0.0082(2) 0.0616(7) Uani 1 1 d .
H45A H 0.1666 0.9019 0.0074 0.074 Uiso 1 1 calc R
H45B H 0.2141 0.8287 -0.0693 0.074 Uiso 1 1 calc R
O50 O 0.8312(2) 0.39670(19) 0.46528(17) 0.0839(6) Uani 1 1 d .
C51 C 0.6873(4) 0.3040(3) 0.4044(3) 0.0910(10) Uani 1 1 d .
H51A H 0.6256 0.3415 0.3946 0.109 Uiso 1 1 calc R
H51B H 0.6656 0.2548 0.4456 0.109 Uiso 1 1 calc R
C52 C 0.6660(3) 0.2280(3) 0.2962(3) 0.0849(9) Uani 1 1 d .
H52A H 0.5675 0.1664 0.2521 0.102 Uiso 1 1 calc R
H52B H 0.6884 0.2782 0.2560 0.102 Uiso 1 1 calc R
O53 O 0.7509(2) 0.1695(2) 0.30741(16) 0.1012(9) Uani 1 1 d .
C54 C 0.8928(3) 0.2600(3) 0.3682(2) 0.0722(8) Uani 1 1 d .
H54A H 0.9155 0.3084 0.3267 0.087 Uiso 1 1 calc R
H54B H 0.9533 0.2213 0.3780 0.087 Uiso 1 1 calc R
C55 C 0.9178(3) 0.3392(3) 0.4777(2) 0.0703(8) Uani 1 1 d .
H55A H 0.8980 0.2910 0.5201 0.084 Uiso 1 1 calc R
H55B H 1.0163 0.4013 0.5197 0.084 Uiso 1 1 calc R
O60 O 0.0939(3) 0.6669(2) 0.2159(2) 0.0944(8) Uani 1 1 d .
O63 O 0.0301(2) 0.43436(17) 0.20380(15) 0.0835(7) Uani 1 1 d .
C61 C -0.0403(3) 0.5712(3) 0.1492(3) 0.0791(9) Uani 1 1 d .
H61A H -0.0511 0.5329 0.0738 0.095 Uiso 1 1 calc R
H61B H -0.1082 0.6021 0.1438 0.095 Uiso 1 1 calc R
C62 C -0.0690(3) 0.4783(3) 0.1967(2) 0.0743(8) Uani 1 1 d .
H62A H -0.0616 0.5152 0.2711 0.089 Uiso 1 1 calc R
H62B H -0.1640 0.4109 0.1486 0.089 Uiso 1 1 calc R
C64 C 0.1665(3) 0.5297(3) 0.2704(2) 0.0641(7) Uani 1 1 d .
H64A H 0.2333 0.4978 0.2737 0.077 Uiso 1 1 calc R
H64B H 0.1793 0.5675 0.3466 0.077 Uiso 1 1 calc R
C65 C 0.1944(3) 0.6223(3) 0.2244(2) 0.0668(7) Uani 1 1 d .
H65A H 0.2891 0.6899 0.2733 0.080 Uiso 1 1 calc R
H65B H 0.1884 0.5862 0.1504 0.080 Uiso 1 1 calc R
O70 O 0.5485(2) -0.0092(2) 0.60213(14) 0.0835(7) Uani 1 1 d .
C71 C 0.6431(3) 0.0404(3) 0.5601(2) 0.0690(8) Uani 1 1 d .
H71A H 0.7209 0.0217 0.5832 0.083 Uiso 1 1 calc R
H71B H 0.6814 0.1291 0.5903 0.083 Uiso 1 1 calc R
C72 C 0.4337(3) 0.0136(3) 0.5660(2) 0.0629(7) Uani 1 1 d .
H72A H 0.4669 0.1016 0.5958 0.075 Uiso 1 1 calc R
H72B H 0.3692 -0.0214 0.5951 0.075 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
O10 0.0924(14) 0.0947(14) 0.0681(11) 0.0675(11) 0.0600(11) 0.0664(13)
O11 0.1209(17) 0.1260(18) 0.1015(14) 0.0944(14) 0.0979(14) 0.0965(17)
O20 0.1071(16) 0.0698(13) 0.0326(8) 0.0027(8) -0.0093(9) 0.0539(14)
O21 0.1173(18) 0.0818(16) 0.0474(10) -0.0198(9) -0.0076(10) 0.0679(16)
O30 0.0340(10) 0.0503(14) 0.1389(18) 0.0459(13) 0.0126(11) 0.0045(11)
O31 0.0678(13) 0.0356(11) 0.1146(15) 0.0421(11) 0.0502(12) 0.0207(12)
N10 0.0420(10) 0.0354(10) 0.0350(8) 0.0196(8) 0.0216(8) 0.0158(10)
N20 0.0406(10) 0.0311(10) 0.0347(9) 0.0093(8) 0.0155(8) 0.0080(10)
N30 0.0410(11) 0.0292(11) 0.0454(10) 0.0184(8) 0.0160(8) 0.0076(10)
C1 0.0331(11) 0.0321(12) 0.0313(9) 0.0140(8) 0.0149(8) 0.0182(11)
C2 0.0295(10) 0.0316(12) 0.0311(9) 0.0134(8) 0.0152(8) 0.0137(11)
C3 0.0334(11) 0.0327(12) 0.0299(9) 0.0129(8) 0.0141(8) 0.0185(11)
C10 0.0345(11) 0.0321(12) 0.0347(10) 0.0154(9) 0.0160(9) 0.0126(11)
C11 0.0381(11) 0.0402(13) 0.0344(10) 0.0169(9) 0.0185(9) 0.0171(12)
C12 0.0337(11) 0.0372(12) 0.0351(10) 0.0165(9) 0.0183(9) 0.0151(11)
C13 0.0315(10) 0.0335(12) 0.0307(9) 0.0119(8) 0.0143(8) 0.0146(11)
C14 0.0426(12) 0.0418(13) 0.0421(11) 0.0209(10) 0.0210(10) 0.0210(12)
C15 0.0404(12) 0.0399(13) 0.0387(11) 0.0202(10) 0.0178(9) 0.0175(12)
C20 0.0302(10) 0.0311(11) 0.0309(9) 0.0156(8) 0.0166(8) 0.0126(10)
C21 0.0406(13) 0.0416(14) 0.0421(11) 0.0142(10) 0.0147(9) 0.0251(13)
C22 0.0444(13) 0.0430(14) 0.0429(11) 0.0199(10) 0.0169(10) 0.0232(13)
C23 0.0327(11) 0.0362(12) 0.0317(9) 0.0168(9) 0.0172(8) 0.0124(11)
C24 0.0404(12) 0.0412(14) 0.0427(11) 0.0141(10) 0.0174(9) 0.0233(12)
C25 0.0366(12) 0.0333(12) 0.0375(10) 0.0148(9) 0.0162(9) 0.0184(11)
C30 0.0367(11) 0.0338(12) 0.0265(9) 0.0141(8) 0.0146(8) 0.0152(11)
C31 0.0394(13) 0.0384(14) 0.0489(12) 0.0187(10) 0.0190(10) 0.0196(13)
C32 0.0418(14) 0.0458(15) 0.0517(13) 0.0212(11) 0.0182(11) 0.0216(14)
C33 0.0420(12) 0.0418(14) 0.0377(10) 0.0197(10) 0.0199(9) 0.0193(13)
C34 0.0449(13) 0.0388(14) 0.0457(12) 0.0195(10) 0.0202(10) 0.0201(13)
C35 0.0406(13) 0.0351(13) 0.0450(11) 0.0176(10) 0.0175(10) 0.0189(12)
O40 0.0629(12) 0.0539(12) 0.1162(15) 0.0480(11) 0.0506(12) 0.0381(12)
O43 0.0510(11) 0.0408(11) 0.0952(13) 0.0207(9) 0.0266(10) 0.0192(11)
C41 0.0662(19) 0.069(2) 0.0688(17) 0.0279(16) 0.0276(15) 0.0295(19)
C42 0.0621(18) 0.070(2) 0.0634(16) 0.0269(15) 0.0265(14) 0.0329(18)
C44 0.0664(19) 0.068(2) 0.0729(18) 0.0308(16) 0.0299(15) 0.0318(19)
C45 0.0636(18) 0.0645(19) 0.0584(15) 0.0237(14) 0.0248(13) 0.0357(17)
O50 0.0971(17) 0.0811(16) 0.0887(14) 0.0243(12) 0.0411(12) 0.0664(16)
C51 0.089(3) 0.097(3) 0.096(2) 0.040(2) 0.045(2) 0.051(3)
C52 0.085(2) 0.083(3) 0.088(2) 0.0344(19) 0.0370(19) 0.044(2)
O53 0.0996(17) 0.1110(19) 0.0772(13) 0.0010(12) 0.0106(11) 0.0873(17)
C54 0.073(2) 0.070(2) 0.0746(18) 0.0296(16) 0.0343(16) 0.035(2)
C55 0.0722(19) 0.069(2) 0.0696(17) 0.0280(15) 0.0315(15) 0.0339(19)
O60 0.152(2) 0.1079(19) 0.1407(19) 0.0918(17) 0.1080(19) 0.114(2)
O63 0.0871(15) 0.0638(14) 0.0831(13) 0.0146(10) 0.0091(11) 0.0563(14)
C61 0.081(2) 0.081(3) 0.079(2) 0.0344(18) 0.0365(18) 0.040(2)
C62 0.074(2) 0.076(2) 0.0753(18) 0.0310(17) 0.0345(16) 0.038(2)
C64 0.0671(19) 0.0622(19) 0.0636(16) 0.0259(14) 0.0265(14) 0.0341(18)
C65 0.0705(19) 0.067(2) 0.0640(16) 0.0281(15) 0.0289(14) 0.0347(18)
O70 0.1140(16) 0.147(2) 0.0542(10) 0.0571(12) 0.0464(11) 0.1092(17)
C71 0.0692(19) 0.066(2) 0.0690(17) 0.0258(15) 0.0286(15) 0.0325(19)
C72 0.0658(17) 0.0642(19) 0.0630(15) 0.0274(14) 0.0297(13) 0.0336(17)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
O11 N10 O10 122.59(16) . .
O11 N10 C10 118.09(15) . .
O10 N10 C10 119.32(15) . .
O21 N20 O20 122.84(18) . .
O21 N20 C23 118.33(17) . .
O20 N20 C23 118.82(16) . .
O31 N30 O30 122.5(2) . .
O31 N30 C33 118.79(19) . .
O30 N30 C33 118.72(18) . .
C2 C1 C3 121.66(17) . .
C2 C1 C13 120.02(17) . .
C3 C1 C13 118.27(18) . .
C1 C2 C3 120.07(17) . 2_557
C1 C2 C20 121.31(16) . .
C3 C2 C20 118.61(18) 2_557 .
C1 C3 C2 118.26(19) . 2_557
C1 C3 C30 121.10(16) . .
C2 C3 C30 120.62(16) 2_557 .
C15 C10 C11 123.06(18) . .
C15 C10 N10 118.27(16) . .
C11 C10 N10 118.64(16) . .
C10 C11 C12 117.82(18) . .
C13 C12 C11 120.97(18) . .
C12 C13 C14 119.33(18) . .
C12 C13 C1 119.71(16) . .
C14 C13 C1 120.96(16) . .
C13 C14 C15 120.58(18) . .
C10 C15 C14 118.21(18) . .
C25 C20 C21 119.66(18) . .
C25 C20 C2 120.36(16) . .
C21 C20 C2 119.82(16) . .
C20 C21 C22 120.63(18) . .
C23 C22 C21 118.24(18) . .
C22 C23 C24 122.82(19) . .
C22 C23 N20 118.57(17) . .
C24 C23 N20 118.57(17) . .
C23 C24 C25 117.93(18) . .
C20 C25 C24 120.70(17) . .
C31 C30 C35 118.0(2) . .
C31 C30 C3 119.59(18) . .
C35 C30 C3 122.43(18) . .
C30 C31 C32 120.12(19) . .
C33 C32 C31 119.6(2) . .
C32 C33 C34 121.7(2) . .
C32 C33 N30 119.16(19) . .
C34 C33 N30 119.15(19) . .
C33 C34 C35 118.1(2) . .
C30 C35 C34 122.53(19) . .
C45 O40 C41 107.37(19) . .
C42 O43 C44 107.85(19) . .
C42 C41 O40 112.7(2) . .
C41 C42 O43 110.7(2) . .
C45 C44 O43 111.9(2) . .
C44 C45 O40 110.2(2) . .
C55 O50 C51 108.6(2) . .
O50 C51 C52 108.1(3) . .
O53 C52 C51 111.5(3) . .
C54 O53 C52 108.4(2) . .
O53 C54 C55 109.8(2) . .
O50 C55 C54 110.6(2) . .
C61 O60 C65 109.9(2) . .
C64 O63 C62 110.76(19) . .
O60 C61 C62 110.8(3) . .
O63 C62 C61 108.7(2) . .
O63 C64 C65 110.5(2) . .
O60 C65 C64 109.9(2) . .
C72 O70 C71 110.19(19) . .
O70 C71 C72 109.2(2) . 2_656
O70 C72 C71 111.3(2) . 2_656
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O10 N10 1.209(2) .
O11 N10 1.202(2) .
O20 N20 1.195(2) .
O21 N20 1.183(2) .
O30 N30 1.223(2) .
O31 N30 1.205(2) .
N10 C10 1.474(2) .
N20 C23 1.490(2) .
N30 C33 1.459(3) .
C1 C2 1.374(3) .
C1 C3 1.402(2) .
C1 C13 1.520(2) .
C2 C3 1.419(2) 2_557
C2 C20 1.505(3) .
C3 C2 1.419(2) 2_557
C3 C30 1.481(3) .
C10 C15 1.350(3) .
C10 C11 1.353(2) .
C11 C12 1.404(2) .
C12 C13 1.363(2) .
C13 C14 1.365(3) .
C14 C15 1.404(3) .
C20 C25 1.363(2) .
C20 C21 1.370(2) .
C21 C22 1.395(3) .
C22 C23 1.354(3) .
C23 C24 1.365(2) .
C24 C25 1.398(3) .
C30 C31 1.360(3) .
C30 C35 1.374(3) .
C31 C32 1.405(3) .
C32 C33 1.350(3) .
C33 C34 1.352(3) .
C34 C35 1.378(3) .
O40 C45 1.433(3) .
O40 C41 1.458(3) .
O43 C42 1.422(3) .
O43 C44 1.433(3) .
C41 C42 1.421(4) .
C44 C45 1.429(4) .
O50 C55 1.439(3) .
O50 C51 1.453(4) .
C51 C52 1.469(4) .
C52 O53 1.431(3) .
O53 C54 1.430(4) .
C54 C55 1.481(4) .
O60 C61 1.399(4) .
O60 C65 1.454(3) .
O63 C64 1.412(3) .
O63 C62 1.436(3) .
C61 C62 1.517(4) .
C64 C65 1.497(4) .
O70 C72 1.424(3) .
O70 C71 1.438(3) .
C71 C72 1.527(3) 2_656
C72 C71 1.527(3) 2_656
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C25 H25 O63 0.95 2.54 3.342(2) 142.8 2_556
C31 H31 O40 0.95 2.49 3.438(3) 173.9 1_546
C42 H42B O31 0.99 2.47 3.322(3) 143.3 1_554
C51 H51A O21 0.99 2.57 3.454(4) 149.0 1_665
C54 H54A O50 0.99 3.57 3.941(4) 104.7 2_766
C54 H54B O10 0.99 2.56 3.302(3) 132.1 1_655
C61 H61B O30 0.99 2.44 3.200(4) 133.5 1_454
C62 H62B O43 0.99 2.57 3.353(4) 136.2 2_565
C64 H64A O20 0.99 2.56 3.208(3) 122.8 1_665
|
1501618.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/16/1501618.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_1501618
loop_
_publ_author_name
'Eric Gagnon'
'Thierry Maris'
'Kenneth E. Maly'
'James D. Wuest'
_publ_section_title
;
The potential of intermolecular N/O interactions of nitro groups in
crystal engineering, as revealed by structures of
hexakis(4-nitrophenyl)benzene
;
_journal_name_full Tetrahedron
_journal_page_first 6603
_journal_page_last 6613
_journal_paper_doi 10.1016/j.tet.2007.03.101
_journal_volume 63
_journal_year 2007
_chemical_compound_source 'Synthesized by the authors. See text'
_chemical_formula_moiety 'C42 H24 N6 O12, 2(C2 H3 N)'
_chemical_formula_sum 'C46 H30 N8 O12'
_chemical_formula_weight 886.78
_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 102.048(11)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 11.237(2)
_cell_length_b 20.367(5)
_cell_length_c 19.002(4)
_cell_measurement_reflns_used 3395
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 58.98
_cell_measurement_theta_min 4.34
_cell_volume 4253.1(16)
_computing_cell_refinement 'SMART (Bruker, 2003)'
_computing_data_collection 'SMART (Bruker, 2003)'
_computing_data_reduction 'SAINT (Bruker, 2004)'
_computing_molecular_graphics 'SHELXTL (Bruker, 1997)'
_computing_publication_material 'UdMX (local program)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type 'Bruker Smart 6000'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator 'Montel 200 optics'
_diffrn_radiation_source 'Rotating Anode'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.090
_diffrn_reflns_av_sigmaI/netI 0.0734
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 24
_diffrn_reflns_limit_k_min -24
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_number 27798
_diffrn_reflns_theta_full 68.90
_diffrn_reflns_theta_max 68.90
_diffrn_reflns_theta_min 4.34
_diffrn_standards_decay_% 2.35
_diffrn_standards_interval_time 1440
_diffrn_standards_number 32
_exptl_absorpt_coefficient_mu 0.864
_exptl_absorpt_correction_T_max 0.95
_exptl_absorpt_correction_T_min 0.91
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Sadabs (Sheldrick,1996)'
_exptl_crystal_colour Colorless
_exptl_crystal_density_diffrn 1.385
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 1832
_exptl_crystal_size_max 0.12
_exptl_crystal_size_mid 0.11
_exptl_crystal_size_min 0.05
_refine_diff_density_max 0.245
_refine_diff_density_min -0.270
_refine_diff_density_rms 0.064
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.017
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 303
_refine_ls_number_reflns 3815
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.017
_refine_ls_R_factor_all 0.0652
_refine_ls_R_factor_gt 0.0568
_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^)+(0.0434P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1281
_refine_ls_wR_factor_ref 0.1292
_reflns_number_gt 2069
_reflns_number_total 3815
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file deposit.cif
_cod_data_source_block jw1118
_cod_original_cell_volume 4253.0(16)
_cod_original_sg_symbol_H-M C2/c
_cod_database_code 1501618
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
N1 N 0.5000 -0.34522(15) 0.7500 0.0513(8) Uani 1 2 d S
N2 N 0.5000 0.35306(15) 0.7500 0.0547(8) Uani 1 2 d S
N3 N 0.8068(2) 0.17848(12) 1.06002(13) 0.0596(7) Uani 1 1 d .
N4 N 0.8367(2) -0.18154(14) 1.04476(17) 0.0734(8) Uani 1 1 d .
O1 O 0.42596(17) -0.37455(8) 0.77838(11) 0.0640(6) Uani 1 1 d .
O2 O 0.59757(17) 0.38183(9) 0.75220(11) 0.0675(6) Uani 1 1 d .
O3 O 0.74627(18) 0.21676(9) 1.08623(10) 0.0652(6) Uani 1 1 d .
O4 O 0.91567(17) 0.16566(10) 1.08407(11) 0.0761(6) Uani 1 1 d .
O5 O 0.8174(3) -0.17051(12) 1.10404(14) 0.1067(9) Uani 1 1 d .
O6 O 0.9048(2) -0.22554(12) 1.02912(13) 0.0966(8) Uani 1 1 d .
C1 C 0.5000 -0.06511(17) 0.7500 0.0402(9) Uani 1 2 d S
C2 C 0.5683(2) -0.03058(12) 0.80916(13) 0.0405(6) Uani 1 1 d .
C3 C 0.5680(2) 0.03807(12) 0.80934(13) 0.0406(6) Uani 1 1 d .
C4 C 0.5000 0.07279(17) 0.7500 0.0419(9) Uani 1 2 d S
C5 C 0.5000 -0.13859(16) 0.7500 0.0403(9) Uani 1 2 d S
C6 C 0.4456(2) -0.17292(12) 0.79816(13) 0.0414(6) Uani 1 1 d .
H6 H 0.4088 -0.1496 0.8313 0.050 Uiso 1 1 calc R
C7 C 0.4447(2) -0.24095(12) 0.79814(13) 0.0454(7) Uani 1 1 d .
H7 H 0.4068 -0.2646 0.8306 0.054 Uiso 1 1 calc R
C8 C 0.5000 -0.27373(16) 0.7500 0.0427(9) Uani 1 2 d S
C9 C 0.5000 0.14592(16) 0.7500 0.0417(9) Uani 1 2 d S
C10 C 0.3926(2) 0.18046(12) 0.75141(13) 0.0474(7) Uani 1 1 d .
H10 H 0.3197 0.1571 0.7521 0.057 Uiso 1 1 calc R
C11 C 0.3925(2) 0.24867(12) 0.75187(13) 0.0467(7) Uani 1 1 d .
H11 H 0.3204 0.2724 0.7534 0.056 Uiso 1 1 calc R
C12 C 0.5000 0.28125(17) 0.7500 0.0460(9) Uani 1 2 d S
C13 C 0.6336(2) 0.07642(12) 0.87332(14) 0.0462(7) Uani 1 1 d .
C14 C 0.5670(2) 0.11571(13) 0.91126(14) 0.0517(7) Uani 1 1 d .
H14 H 0.4814 0.1190 0.8948 0.062 Uiso 1 1 calc R
C15 C 0.6217(2) 0.14973(13) 0.97177(14) 0.0525(7) Uani 1 1 d .
H15 H 0.5760 0.1760 0.9979 0.063 Uiso 1 1 calc R
C16 C 0.7470(2) 0.14379(12) 0.99285(14) 0.0486(7) Uani 1 1 d .
C17 C 0.8172(2) 0.10664(13) 0.95691(15) 0.0541(7) Uani 1 1 d .
H17 H 0.9029 0.1041 0.9733 0.065 Uiso 1 1 calc R
C18 C 0.7590(2) 0.07288(12) 0.89581(13) 0.0473(7) Uani 1 1 d .
H18 H 0.8052 0.0473 0.8694 0.057 Uiso 1 1 calc R
C19 C 0.6408(2) -0.06886(12) 0.87141(13) 0.0426(6) Uani 1 1 d .
C20 C 0.6150(2) -0.06292(12) 0.93943(14) 0.0490(7) Uani 1 1 d .
H20 H 0.5524 -0.0341 0.9469 0.059 Uiso 1 1 calc R
C21 C 0.6807(3) -0.09899(14) 0.99657(14) 0.0571(8) Uani 1 1 d .
H21 H 0.6654 -0.0943 1.0436 0.069 Uiso 1 1 calc R
C22 C 0.7696(2) -0.14215(13) 0.98321(17) 0.0581(8) Uani 1 1 d .
C23 C 0.7970(2) -0.14857(13) 0.91690(17) 0.0578(8) Uani 1 1 d .
H23 H 0.8589 -0.1779 0.9095 0.069 Uiso 1 1 calc R
C24 C 0.7324(2) -0.11137(11) 0.86043(14) 0.0458(7) Uani 1 1 d .
H24 H 0.7507 -0.1149 0.8140 0.055 Uiso 1 1 calc R
N30 N 0.3092(3) -0.03002(15) 0.87641(16) 0.0952(9) Uani 1 1 d .
C30 C 0.2097(3) -0.01483(15) 0.87269(18) 0.0733(9) Uani 1 1 d .
C31 C 0.0829(3) 0.00008(14) 0.8722(2) 0.0898(11) Uani 1 1 d .
H31A H 0.0303 -0.0305 0.8400 0.135 Uiso 1 1 calc R
H31B H 0.0647 0.0451 0.8552 0.135 Uiso 1 1 calc R
H31C H 0.0681 -0.0043 0.9210 0.135 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
N1 0.0449(19) 0.0400(19) 0.065(2) 0.000 0.0020(17) 0.000
N2 0.054(2) 0.0389(19) 0.072(2) 0.000 0.0143(18) 0.000
N3 0.0541(16) 0.0603(16) 0.0581(17) -0.0047(14) -0.0025(13) -0.0095(13)
N4 0.0681(19) 0.071(2) 0.067(2) 0.0209(18) -0.0181(17) -0.0111(15)
O1 0.0595(12) 0.0437(11) 0.0881(15) 0.0116(11) 0.0137(11) -0.0038(9)
O2 0.0631(13) 0.0477(11) 0.0939(15) -0.0006(11) 0.0215(12) -0.0111(10)
O3 0.0685(14) 0.0626(13) 0.0624(13) -0.0170(11) 0.0088(11) -0.0022(11)
O4 0.0482(12) 0.0932(16) 0.0759(15) -0.0129(12) -0.0123(11) -0.0095(11)
O5 0.139(2) 0.101(2) 0.0599(16) 0.0199(15) -0.0235(16) -0.0125(16)
O6 0.0763(17) 0.0827(18) 0.113(2) 0.0250(15) -0.0209(15) 0.0141(13)
C1 0.0337(19) 0.046(2) 0.040(2) 0.000 0.0046(17) 0.000
C2 0.0341(13) 0.0382(15) 0.0454(16) 0.0027(13) -0.0003(12) 0.0016(11)
C3 0.0361(14) 0.0387(15) 0.0437(16) -0.0020(13) 0.0010(12) -0.0025(11)
C4 0.0293(18) 0.043(2) 0.050(2) 0.000 -0.0013(17) 0.000
C5 0.0369(19) 0.037(2) 0.043(2) 0.000 -0.0019(17) 0.000
C6 0.0350(13) 0.0423(16) 0.0420(16) -0.0021(13) -0.0035(12) 0.0026(12)
C7 0.0334(14) 0.0469(16) 0.0507(16) 0.0032(14) -0.0032(12) 0.0005(12)
C8 0.035(2) 0.034(2) 0.053(2) 0.000 -0.0045(18) 0.000
C9 0.040(2) 0.040(2) 0.040(2) 0.000 -0.0029(17) 0.000
C10 0.0394(15) 0.0484(17) 0.0514(17) -0.0003(14) 0.0028(12) 0.0012(12)
C11 0.0377(14) 0.0433(16) 0.0556(17) -0.0034(14) 0.0016(12) 0.0018(12)
C12 0.048(2) 0.039(2) 0.049(2) 0.000 0.0069(18) 0.000
C13 0.0446(16) 0.0397(15) 0.0496(17) 0.0053(14) -0.0012(13) -0.0059(13)
C14 0.0499(17) 0.0524(17) 0.0474(17) -0.0024(15) -0.0020(14) -0.0016(13)
C15 0.0497(17) 0.0562(18) 0.0477(17) -0.0009(15) 0.0012(14) 0.0032(14)
C16 0.0524(17) 0.0419(16) 0.0475(17) -0.0015(14) 0.0011(14) -0.0108(14)
C17 0.0422(16) 0.0515(17) 0.0626(19) 0.0039(16) -0.0029(14) -0.0085(13)
C18 0.0435(15) 0.0422(15) 0.0520(17) 0.0037(14) 0.0000(13) -0.0057(12)
C19 0.0365(14) 0.0427(16) 0.0424(16) 0.0006(13) -0.0059(12) -0.0102(12)
C20 0.0389(15) 0.0549(18) 0.0483(17) 0.0023(15) -0.0019(13) -0.0054(13)
C21 0.0611(19) 0.0614(19) 0.0418(17) -0.0002(15) -0.0055(15) -0.0197(16)
C22 0.0447(17) 0.0497(18) 0.067(2) 0.0154(17) -0.0188(16) -0.0093(14)
C23 0.0359(15) 0.0584(19) 0.070(2) 0.0062(17) -0.0107(15) -0.0038(13)
C24 0.0362(14) 0.0433(16) 0.0536(17) 0.0035(14) -0.0005(13) -0.0010(12)
N30 0.072(2) 0.104(2) 0.108(2) -0.0131(18) 0.0150(18) 0.0027(17)
C30 0.067(2) 0.064(2) 0.089(3) -0.0177(18) 0.015(2) -0.0015(18)
C31 0.068(2) 0.061(2) 0.129(3) -0.001(2) -0.006(2) 0.0115(17)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 N1 O1 2_656 . 122.2(3) y
O1 N1 C8 2_656 . 118.91(16) y
O1 N1 C8 . . 118.91(16) y
O2 N2 O2 2_656 . 123.4(3) y
O2 N2 C12 2_656 . 118.29(16) y
O2 N2 C12 . . 118.29(16) y
O3 N3 O4 . . 125.5(2) y
O3 N3 C16 . . 117.8(2) y
O4 N3 C16 . . 116.7(2) y
O5 N4 O6 . . 126.1(3) y
O5 N4 C22 . . 118.1(3) y
O6 N4 C22 . . 115.7(3) y
C2 C1 C2 2_656 . 120.2(3) y
C2 C1 C5 2_656 . 119.92(15) y
C2 C1 C5 . . 119.92(15) y
C3 C2 C1 . . 120.0(2) y
C3 C2 C19 . . 121.1(2) y
C1 C2 C19 . . 118.9(2) y
C2 C3 C4 . . 120.0(2) y
C2 C3 C13 . . 121.4(2) y
C4 C3 C13 . . 118.5(2) y
C3 C4 C3 2_656 . 119.9(3) y
C3 C4 C9 2_656 . 120.04(15) y
C3 C4 C9 . . 120.04(15) y
C6 C5 C6 . 2_656 119.6(3) y
C6 C5 C1 . . 120.19(16) y
C6 C5 C1 2_656 . 120.19(16) y
C7 C6 C5 . . 120.5(3) y
C7 C6 H6 . . 119.8 ?
C5 C6 H6 . . 119.8 ?
C8 C7 C6 . . 118.7(3) y
C8 C7 H7 . . 120.7 ?
C6 C7 H7 . . 120.7 ?
C7 C8 C7 . 2_656 122.2(3) y
C7 C8 N1 . . 118.92(17) y
C7 C8 N1 2_656 . 118.92(17) y
C10 C9 C10 . 2_656 119.7(3) y
C10 C9 C4 . . 120.12(16) y
C10 C9 C4 2_656 . 120.13(16) y
C11 C10 C9 . . 120.3(2) y
C11 C10 H10 . . 119.9 ?
C9 C10 H10 . . 119.9 ?
C12 C11 C10 . . 118.5(3) y
C12 C11 H11 . . 120.8 ?
C10 C11 H11 . . 120.8 ?
C11 C12 C11 2_656 . 122.8(3) y
C11 C12 N2 2_656 . 118.62(17) y
C11 C12 N2 . . 118.62(17) y
C18 C13 C14 . . 119.4(2) y
C18 C13 C3 . . 121.2(2) y
C14 C13 C3 . . 119.4(2) y
C15 C14 C13 . . 121.8(3) y
C15 C14 H14 . . 119.1 ?
C13 C14 H14 . . 119.1 ?
C14 C15 C16 . . 116.6(3) y
C14 C15 H15 . . 121.7 ?
C16 C15 H15 . . 121.7 ?
C17 C16 C15 . . 124.0(2) y
C17 C16 N3 . . 118.9(2) y
C15 C16 N3 . . 117.1(3) y
C16 C17 C18 . . 118.0(2) y
C16 C17 H17 . . 121 ?
C18 C17 H17 . . 121 ?
C13 C18 C17 . . 120.2(3) y
C13 C18 H18 . . 119.9 ?
C17 C18 H18 . . 119.9 ?
C20 C19 C24 . . 119.9(2) y
C20 C19 C2 . . 120.2(2) y
C24 C19 C2 . . 120.0(2) y
C19 C20 C21 . . 120.1(2) y
C19 C20 H20 . . 119.9 ?
C21 C20 H20 . . 119.9 ?
C20 C21 C22 . . 118.4(3) y
C20 C21 H21 . . 120.8 ?
C22 C21 H21 . . 120.8 ?
C23 C22 C21 . . 122.5(3) y
C23 C22 N4 . . 120.0(3) y
C21 C22 N4 . . 117.5(3) y
C22 C23 C24 . . 118.6(3) y
C22 C23 H23 . . 120.7 ?
C24 C23 H23 . . 120.7 ?
C23 C24 C19 . . 120.4(3) y
C23 C24 H24 . . 119.8 ?
C19 C24 H24 . . 119.8 ?
N30 C30 C31 . . 175.2(4) y
C30 C31 H31A . . 109.5 ?
C30 C31 H31B . . 109.5 ?
H31A C31 H31B . . 109.5 ?
C30 C31 H31C . . 109.5 ?
H31A C31 H31C . . 109.5 ?
H31B C31 H31C . . 109.5 ?
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
N1 O1 2_656 1.236(2) y
N1 O1 . 1.236(2) y
N1 C8 . 1.456(4) y
N2 O2 2_656 1.236(2) y
N2 O2 . 1.236(2) y
N2 C12 . 1.463(4) y
N3 O3 . 1.208(3) y
N3 O4 . 1.241(3) y
N3 C16 . 1.491(3) y
N4 O5 . 1.212(4) y
N4 O6 . 1.253(3) y
N4 C22 . 1.487(4) y
C1 C2 2_656 1.410(3) y
C1 C2 . 1.410(3) y
C1 C5 . 1.497(4) y
C2 C3 . 1.398(3) y
C2 C19 . 1.506(3) y
C3 C4 . 1.413(3) y
C3 C13 . 1.502(3) y
C4 C3 2_656 1.413(3) y
C4 C9 . 1.489(5) y
C5 C6 . 1.391(3) y
C5 C6 2_656 1.391(3) y
C6 C7 . 1.385(3) y
C6 H6 . 0.95 ?
C7 C8 . 1.381(3) y
C7 H7 . 0.95 ?
C8 C7 2_656 1.381(3) y
C9 C10 . 1.402(3) y
C9 C10 2_656 1.402(3) y
C10 C11 . 1.389(3) y
C10 H10 . 0.95 ?
C11 C12 . 1.385(3) y
C11 H11 . 0.95 ?
C12 C11 2_656 1.385(3) y
C13 C18 . 1.386(3) y
C13 C14 . 1.395(3) y
C14 C15 . 1.373(3) y
C14 H14 . 0.95 ?
C15 C16 . 1.386(3) y
C15 H15 . 0.95 ?
C16 C17 . 1.373(4) y
C17 C18 . 1.390(3) y
C17 H17 . 0.95 ?
C18 H18 . 0.95 ?
C19 C20 . 1.388(3) y
C19 C24 . 1.393(3) y
C20 C21 . 1.389(3) y
C20 H20 . 0.95 ?
C21 C22 . 1.393(4) y
C21 H21 . 0.95 ?
C22 C23 . 1.364(4) y
C23 C24 . 1.388(3) y
C23 H23 . 0.95 ?
C24 H24 . 0.95 ?
N30 C30 . 1.148(4) y
C30 C31 . 1.455(4) y
C31 H31a . 0.98 ?
C31 H31b . 0.98 ?
C31 H31c . 0.98 ?
|
1501619.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/16/1501619.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_1501619
loop_
_publ_author_name
'Eric Gagnon'
'Thierry Maris'
'Kenneth E. Maly'
'James D. Wuest'
_publ_section_title
;
The potential of intermolecular N/O interactions of nitro groups in
crystal engineering, as revealed by structures of
hexakis(4-nitrophenyl)benzene
;
_journal_name_full Tetrahedron
_journal_page_first 6603
_journal_page_last 6613
_journal_paper_doi 10.1016/j.tet.2007.03.101
_journal_volume 63
_journal_year 2007
_chemical_compound_source 'Synthesized by the authors. See text'
_chemical_formula_moiety 'C42 H24 N6 O12, 2(C3 H6 O)'
_chemical_formula_sum 'C48 H36 N6 O14'
_chemical_formula_weight 920.83
_chemical_name_systematic
;
?
;
_space_group_IT_number 15
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-C 2yc'
_symmetry_space_group_name_H-M 'C 1 2/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 104.74(7)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 11.18(2)
_cell_length_b 20.59(3)
_cell_length_c 20.07(4)
_cell_measurement_reflns_used 6757
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 39.16
_cell_measurement_theta_min 18.04
_cell_volume 4468(14)
_computing_cell_refinement 'SMART (Bruker, 2003)'
_computing_data_collection 'SMART (Bruker, 2003)'
_computing_data_reduction 'SAINT (Bruker, 2004)'
_computing_molecular_graphics 'SHELXTL (Bruker, 1997)'
_computing_publication_material 'UdMX (local program)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type 'Bruker Smart 6000'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator 'Montel 200 optics'
_diffrn_radiation_source 'Rotating Anode'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.066
_diffrn_reflns_av_sigmaI/netI 0.0529
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 24
_diffrn_reflns_limit_k_min -24
_diffrn_reflns_limit_l_max 23
_diffrn_reflns_limit_l_min -23
_diffrn_reflns_number 28457
_diffrn_reflns_theta_full 67.48
_diffrn_reflns_theta_max 67.48
_diffrn_reflns_theta_min 4.29
_diffrn_standards_decay_% 6.78
_diffrn_standards_interval_time 1440
_diffrn_standards_number 35
_exptl_absorpt_coefficient_mu 0.862
_exptl_absorpt_correction_T_max 0.9300
_exptl_absorpt_correction_T_min 0.8500
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Sadabs (Sheldrick,1996)'
_exptl_crystal_colour Colorless
_exptl_crystal_density_diffrn 1.368
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 1912
_exptl_crystal_size_max 0.19
_exptl_crystal_size_mid 0.11
_exptl_crystal_size_min 0.11
_refine_diff_density_max 0.523
_refine_diff_density_min -0.264
_refine_diff_density_rms 0.066
_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 313
_refine_ls_number_reflns 3878
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.036
_refine_ls_R_factor_all 0.0630
_refine_ls_R_factor_gt 0.0542
_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^)+(0.0924P)^2^+3.8710P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1575
_refine_ls_wR_factor_ref 0.1670
_reflns_number_gt 3217
_reflns_number_total 3878
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file deposit.cif
_cod_data_source_block jw1127
_cod_original_sg_symbol_H-M C2/c
_cod_database_code 1501619
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
C1 C 1.0000 0.08386(13) 0.2500 0.0249(6) Uani 1 2 d S
C2 C 0.93354(17) 0.04986(10) 0.19084(10) 0.0249(4) Uani 1 1 d .
C3 C 0.93287(17) -0.01885(9) 0.19078(10) 0.0244(4) Uani 1 1 d .
C4 C 1.0000 -0.05330(13) 0.2500 0.0237(6) Uani 1 2 d S
C5 C 1.0000 0.15729(14) 0.2500 0.0260(6) Uani 1 2 d S
C6 C 0.88927(18) 0.19150(10) 0.24826(10) 0.0295(5) Uani 1 1 d .
H6 H 0.8152 0.1682 0.2465 0.035 Uiso 1 1 calc R
C7 C 0.88873(19) 0.25945(10) 0.24906(10) 0.0302(5) Uani 1 1 d .
H7 H 0.8157 0.2831 0.2490 0.036 Uiso 1 1 calc R
C8 C 1.0000 0.29139(14) 0.2500 0.0268(6) Uani 1 2 d S
N1 N 1.0000 0.36320(12) 0.2500 0.0331(6) Uani 1 2 d S
O1 O 1.09864(15) 0.39191(8) 0.25054(9) 0.0433(4) Uani 1 1 d .
C9 C 0.86804(18) 0.08727(10) 0.12739(10) 0.0273(5) Uani 1 1 d .
C10 C 0.9391(2) 0.12597(10) 0.09295(11) 0.0313(5) Uani 1 1 d .
H10 H 1.0256 0.1302 0.1121 0.038 Uiso 1 1 calc R
C11 C 0.8839(2) 0.15768(11) 0.03157(11) 0.0338(5) Uani 1 1 d .
H11 H 0.9312 0.1827 0.0077 0.041 Uiso 1 1 calc R
C12 C 0.7565(2) 0.15119(10) 0.00667(11) 0.0338(5) Uani 1 1 d .
C13 C 0.6813(2) 0.11671(11) 0.04026(11) 0.0354(5) Uani 1 1 d .
H13 H 0.5941 0.1155 0.0222 0.043 Uiso 1 1 calc R
C14 C 0.73849(19) 0.08372(10) 0.10169(11) 0.0319(5) Uani 1 1 d .
H14 H 0.6902 0.0594 0.1255 0.038 Uiso 1 1 calc R
N2 N 0.69714(18) 0.18165(10) -0.06151(10) 0.0398(5) Uani 1 1 d .
O2 O 0.76445(16) 0.21398(9) -0.08935(8) 0.0461(4) Uani 1 1 d .
O3 O 0.58408(16) 0.17223(10) -0.08586(9) 0.0541(5) Uani 1 1 d .
C15 C 0.86336(17) -0.05668(9) 0.12830(10) 0.0257(5) Uani 1 1 d .
C16 C 0.89905(19) -0.05241(10) 0.06558(10) 0.0295(5) Uani 1 1 d .
H16 H 0.9629 -0.0233 0.0618 0.035 Uiso 1 1 calc R
C17 C 0.8407(2) -0.09082(11) 0.00935(11) 0.0337(5) Uani 1 1 d .
H17 H 0.8640 -0.0881 -0.0329 0.040 Uiso 1 1 calc R
C18 C 0.74684(19) -0.13352(11) 0.01661(11) 0.0343(5) Uani 1 1 d .
C19 C 0.7067(2) -0.13814(11) 0.07710(12) 0.0359(5) Uani 1 1 d .
H19 H 0.6418 -0.1668 0.0802 0.043 Uiso 1 1 calc R
C20 C 0.76586(18) -0.09870(10) 0.13319(11) 0.0306(5) Uani 1 1 d .
H20 H 0.7400 -0.1004 0.1747 0.037 Uiso 1 1 calc R
N3 N 0.68883(19) -0.17691(10) -0.04216(11) 0.0434(5) Uani 1 1 d .
O4 O 0.72677(19) -0.17279(10) -0.09545(9) 0.0558(5) Uani 1 1 d .
O5 O 0.60756(18) -0.21561(10) -0.03412(11) 0.0609(6) Uani 1 1 d .
C21 C 1.0000 -0.12662(13) 0.2500 0.0247(6) Uani 1 2 d S
C22 C 1.05072(18) -0.16099(10) 0.20235(10) 0.0276(5) Uani 1 1 d .
H22 H 1.0852 -0.1377 0.1708 0.033 Uiso 1 1 calc R
C23 C 1.05025(18) -0.22880(10) 0.20148(10) 0.0288(5) Uani 1 1 d .
H23 H 1.0827 -0.2523 0.1693 0.035 Uiso 1 1 calc R
C24 C 1.0000 -0.26108(14) 0.2500 0.0292(6) Uani 1 2 d S
N4 N 1.0000 -0.33299(13) 0.2500 0.0359(6) Uani 1 2 d S
O6 O 1.04775(16) -0.36143(8) 0.20817(9) 0.0456(4) Uani 1 1 d .
C30 C 0.7966(2) 0.48764(11) 0.13306(12) 0.0372(5) Uani 1 1 d .
O30 O 0.71622(16) 0.44903(10) 0.10352(9) 0.0535(5) Uani 1 1 d .
C31 C 0.9172(2) 0.49744(13) 0.11155(14) 0.0459(6) Uani 1 1 d .
H31A H 0.9836 0.4728 0.1425 0.069 Uiso 1 1 calc R
H31B H 0.9385 0.5437 0.1141 0.069 Uiso 1 1 calc R
H31C H 0.9066 0.4821 0.0642 0.069 Uiso 1 1 calc R
C32 C 0.7785(2) 0.52877(12) 0.19186(13) 0.0420(6) Uani 1 1 d .
H32A H 0.7709 0.5745 0.1778 0.063 Uiso 1 1 calc R
H32B H 0.8497 0.5235 0.2317 0.063 Uiso 1 1 calc R
H32C H 0.7031 0.5150 0.2043 0.063 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
C1 0.0264(13) 0.0229(15) 0.0259(14) 0.000 0.0076(11) 0.000
C2 0.0275(10) 0.0259(11) 0.0225(10) 0.0013(8) 0.0086(8) 0.0018(8)
C3 0.0263(10) 0.0240(11) 0.0235(10) -0.0004(8) 0.0073(8) -0.0006(7)
C4 0.0268(13) 0.0241(15) 0.0215(14) 0.000 0.0086(11) 0.000
C5 0.0348(15) 0.0246(15) 0.0185(13) 0.000 0.0066(11) 0.000
C6 0.0308(11) 0.0294(11) 0.0281(11) -0.0003(8) 0.0070(9) -0.0015(8)
C7 0.0326(11) 0.0296(12) 0.0284(11) 0.0018(8) 0.0078(9) 0.0048(8)
C8 0.0354(15) 0.0261(15) 0.0184(13) 0.000 0.0057(11) 0.000
N1 0.0435(15) 0.0263(13) 0.0323(14) 0.000 0.0148(11) 0.000
O1 0.0480(9) 0.0295(9) 0.0567(11) -0.0022(7) 0.0214(8) -0.0087(7)
C9 0.0379(11) 0.0226(10) 0.0206(10) -0.0022(8) 0.0056(8) 0.0051(8)
C10 0.0399(11) 0.0274(11) 0.0267(11) -0.0011(8) 0.0088(9) 0.0030(9)
C11 0.0450(13) 0.0295(12) 0.0275(11) 0.0010(9) 0.0102(9) 0.0017(9)
C12 0.0457(13) 0.0284(12) 0.0284(11) 0.0005(9) 0.0112(10) 0.0058(9)
C13 0.0337(11) 0.0393(13) 0.0300(11) -0.0056(9) 0.0023(9) 0.0033(9)
C14 0.0364(11) 0.0293(12) 0.0282(11) -0.0007(8) 0.0049(9) 0.0020(9)
N2 0.0415(11) 0.0437(12) 0.0317(10) 0.0025(8) 0.0047(9) 0.0075(9)
O2 0.0546(10) 0.0476(11) 0.0366(9) 0.0134(8) 0.0125(8) 0.0014(8)
O3 0.0411(10) 0.0773(14) 0.0389(10) 0.0144(9) 0.0009(8) 0.0088(9)
C15 0.0288(10) 0.0222(10) 0.0239(10) -0.0004(7) 0.0025(8) 0.0049(8)
C16 0.0335(10) 0.0273(11) 0.0269(11) -0.0006(8) 0.0063(8) 0.0025(8)
C17 0.0389(12) 0.0362(12) 0.0242(10) -0.0022(9) 0.0045(9) 0.0080(9)
C18 0.0341(11) 0.0323(12) 0.0306(12) -0.0065(9) -0.0025(9) 0.0071(9)
C19 0.0326(11) 0.0300(12) 0.0412(13) -0.0013(9) 0.0023(10) -0.0013(9)
C20 0.0311(10) 0.0306(11) 0.0287(11) 0.0008(8) 0.0048(8) 0.0004(9)
N3 0.0466(12) 0.0389(12) 0.0394(12) -0.0083(9) 0.0011(9) 0.0021(9)
O4 0.0762(13) 0.0558(12) 0.0316(10) -0.0116(8) 0.0068(9) -0.0025(10)
O5 0.0533(11) 0.0596(13) 0.0638(13) -0.0218(10) 0.0041(9) -0.0170(10)
C21 0.0256(13) 0.0241(15) 0.0219(14) 0.000 0.0015(11) 0.000
C22 0.0287(10) 0.0268(11) 0.0252(10) 0.0011(8) 0.0032(8) 0.0010(8)
C23 0.0293(10) 0.0272(11) 0.0271(11) -0.0037(8) 0.0021(8) 0.0019(8)
C24 0.0269(14) 0.0209(15) 0.0350(16) 0.000 -0.0010(12) 0.000
N4 0.0356(14) 0.0262(14) 0.0433(16) 0.000 0.0052(12) 0.000
O6 0.0550(10) 0.0281(9) 0.0559(11) -0.0050(7) 0.0185(8) 0.0062(7)
C30 0.0392(12) 0.0363(13) 0.0349(12) -0.0015(9) 0.0072(10) 0.0037(10)
O30 0.0452(10) 0.0640(13) 0.0500(11) -0.0192(9) 0.0099(8) -0.0108(9)
C31 0.0423(13) 0.0496(15) 0.0478(14) -0.0110(11) 0.0154(11) -0.0040(11)
C32 0.0430(13) 0.0380(13) 0.0478(14) -0.0069(10) 0.0164(11) -0.0002(10)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
C2 C1 C2 . 2_755 120.7(3) y
C2 C1 C5 . . 119.65(14) y
C2 C1 C5 2_755 . 119.65(14) y
C3 C2 C1 . . 119.80(19) y
C3 C2 C9 . . 120.55(18) y
C1 C2 C9 . . 119.6(2) y
C2 C3 C4 . . 119.74(19) y
C2 C3 C15 . . 121.16(17) y
C4 C3 C15 . . 119.1(2) y
C3 C4 C3 . 2_755 120.2(3) y
C3 C4 C21 . . 119.90(13) y
C3 C4 C21 2_755 . 119.90(13) y
C6 C5 C6 2_755 . 120.4(3) y
C6 C5 C1 2_755 . 119.81(15) y
C6 C5 C1 . . 119.81(15) y
C7 C6 C5 . . 120.2(2) y
C7 C6 H6 . . 119.9 ?
C5 C6 H6 . . 119.9 ?
C6 C7 C8 . . 117.5(2) y
C6 C7 H7 . . 121.2 ?
C8 C7 H7 . . 121.2 ?
C7 C8 C7 2_755 . 124.1(3) y
C7 C8 N1 2_755 . 117.96(15) y
C7 C8 N1 . . 117.96(15) y
O1 N1 O1 . 2_755 123.5(3) y
O1 N1 C8 . . 118.25(14) y
O1 N1 C8 2_755 . 118.25(14) y
C14 C9 C10 . . 120.0(2) y
C14 C9 C2 . . 120.98(19) y
C10 C9 C2 . . 119.0(2) y
C11 C10 C9 . . 121.1(2) y
C11 C10 H10 . . 119.5 ?
C9 C10 H10 . . 119.5 ?
C12 C11 C10 . . 117.1(2) y
C12 C11 H11 . . 121.4 ?
C10 C11 H11 . . 121.4 ?
C11 C12 C13 . . 124.2(2) y
C11 C12 N2 . . 117.6(2) y
C13 C12 N2 . . 118.2(2) y
C12 C13 C14 . . 118.2(2) y
C12 C13 H13 . . 120.9 ?
C14 C13 H13 . . 120.9 ?
C13 C14 C9 . . 119.3(2) y
C13 C14 H14 . . 120.3 ?
C9 C14 H14 . . 120.3 ?
O2 N2 O3 . . 125.3(2) y
O2 N2 C12 . . 117.3(2) y
O3 N2 C12 . . 117.5(2) y
C20 C15 C16 . . 119.72(19) y
C20 C15 C3 . . 120.0(2) y
C16 C15 C3 . . 120.2(2) y
C17 C16 C15 . . 120.2(2) y
C17 C16 H16 . . 119.9 ?
C15 C16 H16 . . 119.9 ?
C16 C17 C18 . . 118.6(2) y
C16 C17 H17 . . 120.7 ?
C18 C17 H17 . . 120.7 ?
C19 C18 C17 . . 123.0(2) y
C19 C18 N3 . . 118.3(2) y
C17 C18 N3 . . 118.6(2) y
C18 C19 C20 . . 117.7(2) y
C18 C19 H19 . . 121.2 ?
C20 C19 H19 . . 121.2 ?
C19 C20 C15 . . 120.7(2) y
C19 C20 H20 . . 119.6 ?
C15 C20 H20 . . 119.6 ?
O5 N3 O4 . . 124.8(2) y
O5 N3 C18 . . 117.7(2) y
O4 N3 C18 . . 117.5(2) y
C22 C21 C22 . 2_755 120.2(3) y
C22 C21 C4 . . 119.92(14) y
C22 C21 C4 2_755 . 119.92(14) y
C23 C22 C21 . . 120.4(2) y
C23 C22 H22 . . 119.8 ?
C21 C22 H22 . . 119.8 ?
C22 C23 C24 . . 117.6(2) y
C22 C23 H23 . . 121.2 ?
C24 C23 H23 . . 121.2 ?
C23 C24 C23 . 2_755 123.7(3) y
C23 C24 N4 . . 118.16(14) y
C23 C24 N4 2_755 . 118.15(14) y
O6 N4 O6 . 2_755 124.1(3) y
O6 N4 C24 . . 117.96(14) y
O6 N4 C24 2_755 . 117.96(14) y
O30 C30 C32 . . 120.8(2) y
O30 C30 C31 . . 122.4(2) y
C32 C30 C31 . . 116.8(2) y
C30 C31 H31A . . 109.5 ?
C30 C31 H31B . . 109.5 ?
H31A C31 H31B . . 109.5 ?
C30 C31 H31C . . 109.5 ?
H31A C31 H31C . . 109.5 ?
H31B C31 H31C . . 109.5 ?
C30 C32 H32A . . 109.5 ?
C30 C32 H32B . . 109.5 ?
H32A C32 H32B . . 109.5 ?
C30 C32 H32C . . 109.5 ?
H32A C32 H32C . . 109.5 ?
H32B C32 H32C . . 109.5 ?
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
C1 C2 . 1.415(3) y
C1 C2 2_755 1.416(3) y
C1 C5 . 1.512(5) y
C2 C3 . 1.415(4) y
C2 C9 . 1.509(3) y
C3 C4 . 1.423(3) y
C3 C15 . 1.513(3) y
C4 C3 2_755 1.423(3) y
C4 C21 . 1.510(5) y
C5 C6 2_755 1.417(3) y
C5 C6 . 1.417(3) y
C6 C7 . 1.399(4) y
C6 H6 . 0.95 ?
C7 C8 . 1.403(3) y
C7 H7 . 0.95 ?
C8 C7 2_755 1.403(3) y
C8 N1 . 1.479(4) y
N1 O1 . 1.249(3) y
N1 O1 2_755 1.249(3) y
C9 C14 . 1.411(4) y
C9 C10 . 1.423(3) y
C10 C11 . 1.392(4) y
C10 H10 . 0.95 ?
C11 C12 . 1.391(4) y
C11 H11 . 0.95 ?
C12 C13 . 1.398(4) y
C12 N2 . 1.498(4) y
C13 C14 . 1.411(4) y
C13 H13 . 0.95 ?
C14 H14 . 0.95 ?
N2 O2 . 1.239(3) y
N2 O3 . 1.249(4) y
C15 C20 . 1.415(4) y
C15 C16 . 1.417(4) y
C16 C17 . 1.397(3) y
C16 H16 . 0.95 ?
C17 C18 . 1.405(4) y
C17 H17 . 0.95 ?
C18 C19 . 1.401(4) y
C18 N3 . 1.491(3) y
C19 C20 . 1.409(4) y
C19 H19 . 0.95 ?
C20 H20 . 0.95 ?
N3 O5 . 1.250(3) y
N3 O4 . 1.250(4) y
C21 C22 . 1.419(3) y
C21 C22 2_755 1.419(3) y
C22 C23 . 1.397(4) y
C22 H22 . 0.95 ?
C23 C24 . 1.409(3) y
C23 H23 . 0.95 ?
C24 C23 2_755 1.409(3) y
C24 N4 . 1.481(5) y
N4 O6 . 1.250(3) y
N4 O6 2_755 1.250(3) y
C30 O30 . 1.233(3) y
C30 C32 . 1.508(4) y
C30 C31 . 1.530(4) y
C31 H31a . 0.98 ?
C31 H31b . 0.98 ?
C31 H31c . 0.98 ?
C32 H32a . 0.98 ?
C32 H32b . 0.98 ?
C32 H32c . 0.98 ?
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_4
_geom_torsion
_geom_torsion_publ_flag
C2 C1 C2 C3 2_755 . 0.29(12) y
C5 C1 C2 C3 . . -179.71(12) y
C2 C1 C2 C9 2_755 . -177.35(19) y
C5 C1 C2 C9 . . 2.65(19) y
C1 C2 C3 C4 . . -0.6(2) y
C9 C2 C3 C4 . . 177.05(15) y
C1 C2 C3 C15 . . -179.67(15) y
C9 C2 C3 C15 . . -2.1(3) y
C2 C3 C4 C3 . 2_755 0.29(12) y
C15 C3 C4 C3 . 2_755 179.40(18) y
C2 C3 C4 C21 . . -179.71(12) y
C15 C3 C4 C21 . . -0.59(18) y
C2 C1 C5 C6 . 2_755 -112.59(16) y
C2 C1 C5 C6 2_755 2_755 67.41(16) y
C2 C1 C5 C6 . . 67.41(16) y
C2 C1 C5 C6 2_755 . -112.59(16) y
C6 C5 C6 C7 2_755 . -0.75(13) y
C1 C5 C6 C7 . . 179.25(13) y
C5 C6 C7 C8 . . 1.4(3) y
C6 C7 C8 C7 . 2_755 -0.72(13) y
C6 C7 C8 N1 . . 179.27(13) y
C7 C8 N1 O1 2_755 . 0.30(13) y
C7 C8 N1 O1 . . -179.70(13) y
C7 C8 N1 O1 2_755 2_755 -179.71(13) y
C7 C8 N1 O1 . 2_755 0.30(13) y
C3 C2 C9 C14 . . 64.4(3) y
C1 C2 C9 C14 . . -117.9(2) y
C3 C2 C9 C10 . . -114.9(2) y
C1 C2 C9 C10 . . 62.8(2) y
C14 C9 C10 C11 . . -3.9(3) y
C2 C9 C10 C11 . . 175.45(18) y
C9 C10 C11 C12 . . 1.6(3) y
C10 C11 C12 C13 . . 1.9(3) y
C10 C11 C12 N2 . . -176.30(18) y
C11 C12 C13 C14 . . -3.2(3) y
N2 C12 C13 C14 . . 175.05(18) y
C12 C13 C14 C9 . . 0.8(3) y
C10 C9 C14 C13 . . 2.6(3) y
C2 C9 C14 C13 . . -176.74(18) y
C11 C12 N2 O2 . . -4.2(3) y
C13 C12 N2 O2 . . 177.5(2) y
C11 C12 N2 O3 . . 175.5(2) y
C13 C12 N2 O3 . . -2.8(3) y
C2 C3 C15 C20 . . -118.8(2) y
C4 C3 C15 C20 . . 62.1(2) y
C2 C3 C15 C16 . . 64.0(3) y
C4 C3 C15 C16 . . -115.1(2) y
C20 C15 C16 C17 . . -1.8(3) y
C3 C15 C16 C17 . . 175.43(18) y
C15 C16 C17 C18 . . -0.2(3) y
C16 C17 C18 C19 . . 1.8(3) y
C16 C17 C18 N3 . . -176.99(18) y
C17 C18 C19 C20 . . -1.3(3) y
N3 C18 C19 C20 . . 177.47(19) y
C18 C19 C20 C15 . . -0.8(3) y
C16 C15 C20 C19 . . 2.3(3) y
C3 C15 C20 C19 . . -174.95(18) y
C19 C18 N3 O5 . . -0.5(3) y
C17 C18 N3 O5 . . 178.4(2) y
C19 C18 N3 O4 . . -179.1(2) y
C17 C18 N3 O4 . . -0.3(3) y
C3 C4 C21 C22 . . 62.5(2) y
C3 C4 C21 C22 2_755 . -117.5(2) y
C3 C4 C21 C22 . 2_755 -117.5(2) y
C3 C4 C21 C22 2_755 2_755 62.5(2) y
C22 C21 C22 C23 2_755 . 0.56(13) y
C4 C21 C22 C23 . . -179.44(13) y
C21 C22 C23 C24 . . -1.1(2) y
C22 C23 C24 C23 . 2_755 0.54(12) y
C22 C23 C24 N4 . . -179.46(12) y
C23 C24 N4 O6 . . 1.95(13) y
C23 C24 N4 O6 2_755 . -178.05(13) y
C23 C24 N4 O6 . 2_755 -178.05(13) y
C23 C24 N4 O6 2_755 2_755 1.95(13) y
|
1501620.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/16/1501620.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_1501620
loop_
_publ_author_name
'Eric Gagnon'
'Thierry Maris'
'Kenneth E. Maly'
'James D. Wuest'
_publ_section_title
;
The potential of intermolecular N/O interactions of nitro groups in
crystal engineering, as revealed by structures of
hexakis(4-nitrophenyl)benzene
;
_journal_name_full Tetrahedron
_journal_page_first 6603
_journal_page_last 6613
_journal_paper_doi 10.1016/j.tet.2007.03.101
_journal_volume 63
_journal_year 2007
_chemical_compound_source 'Synthesized by the authors. See text'
_chemical_formula_moiety 'C42 H24 N6 O12, 2(C2 H6 O)'
_chemical_formula_sum 'C46 H36 N6 O14'
_chemical_formula_weight 896.81
_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 98.039(6)
_cell_angle_gamma 90.00
_cell_formula_units_Z 2
_cell_length_a 10.7355(10)
_cell_length_b 13.9310(14)
_cell_length_c 14.1161(15)
_cell_measurement_reflns_used 4545
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 67.80
_cell_measurement_theta_min 4.48
_cell_volume 2090.4(4)
_computing_cell_refinement 'SMART (Bruker, 2003)'
_computing_data_collection 'SMART (Bruker, 2003)'
_computing_data_reduction 'SAINT (Bruker, 2004)'
_computing_molecular_graphics 'SHELXTL (Bruker, 1997)'
_computing_publication_material 'UdMX (local program)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type 'Bruker Smart 6000'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator 'Montel 200 optics'
_diffrn_radiation_source 'Rotating Anode'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.097
_diffrn_reflns_av_sigmaI/netI 0.1134
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_number 27886
_diffrn_reflns_theta_full 68.68
_diffrn_reflns_theta_max 68.68
_diffrn_reflns_theta_min 4.48
_diffrn_standards_decay_% 4.61
_diffrn_standards_interval_time 1440
_diffrn_standards_number 59
_exptl_absorpt_coefficient_mu 0.904
_exptl_absorpt_correction_T_max 0.9100
_exptl_absorpt_correction_T_min 0.7400
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Sadabs (Sheldrick,1996)'
_exptl_crystal_colour Colorless
_exptl_crystal_density_diffrn 1.425
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 932
_exptl_crystal_size_max 0.22
_exptl_crystal_size_mid 0.20
_exptl_crystal_size_min 0.11
_refine_diff_density_max 0.259
_refine_diff_density_min -0.249
_refine_diff_density_rms 0.068
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.832
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 299
_refine_ls_number_reflns 3774
_refine_ls_number_restraints 3
_refine_ls_restrained_S_all 0.832
_refine_ls_R_factor_all 0.0863
_refine_ls_R_factor_gt 0.0665
_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^)+(0.0110P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1376
_refine_ls_wR_factor_ref 0.1422
_reflns_number_gt 2110
_reflns_number_total 3774
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file deposit.cif
_cod_data_source_block jw1110
_cod_original_sg_symbol_H-M P21/n
_cod_database_code 1501620
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
C1 C -0.0080(3) -0.4024(2) 0.0248(2) 0.0319(8) Uani 1 1 d .
C2 C -0.0015(3) -0.4290(2) -0.0706(3) 0.0319(7) Uani 1 1 d .
C3 C 0.0056(3) -0.5267(2) -0.0940(2) 0.0327(7) Uani 1 1 d .
C10 C -0.0070(3) -0.2991(2) 0.0519(3) 0.0396(9) Uani 1 1 d .
C11 C 0.1043(3) -0.2481(2) 0.0605(3) 0.0431(9) Uani 1 1 d .
H11 H 0.1797 -0.2801 0.0511 0.052 Uiso 1 1 calc R
C12 C 0.1082(3) -0.1514(2) 0.0824(3) 0.0448(9) Uani 1 1 d .
H12 H 0.1850 -0.1168 0.0857 0.054 Uiso 1 1 calc R
C13 C -0.0006(3) -0.1053(3) 0.0994(3) 0.0432(9) Uani 1 1 d .
C14 C -0.1154(3) -0.1545(2) 0.0916(3) 0.0454(9) Uani 1 1 d .
H14 H -0.1895 -0.1233 0.1053 0.055 Uiso 1 1 calc R
C15 C -0.1181(3) -0.2503(2) 0.0634(3) 0.0457(9) Uani 1 1 d .
H15 H -0.1964 -0.2830 0.0517 0.055 Uiso 1 1 calc R
C20 C -0.0049(4) -0.3547(3) -0.1462(3) 0.0485(10) Uani 1 1 d .
C21 C 0.1001(3) -0.3343(2) -0.1892(3) 0.0407(8) Uani 1 1 d .
H21 H 0.1754 -0.3688 -0.1689 0.049 Uiso 1 1 calc R
C22 C 0.1009(3) -0.2656(3) -0.2606(3) 0.0442(9) Uani 1 1 d .
H22 H 0.1747 -0.2521 -0.2882 0.053 Uiso 1 1 calc R
C23 C -0.0116(3) -0.2178(2) -0.2897(3) 0.0420(9) Uani 1 1 d .
C24 C -0.1205(3) -0.2357(2) -0.2504(3) 0.0437(9) Uani 1 1 d .
H24 H -0.1963 -0.2022 -0.2717 0.052 Uiso 1 1 calc R
C25 C -0.1146(3) -0.3048(3) -0.1786(3) 0.0462(9) Uani 1 1 d .
H25 H -0.1884 -0.3183 -0.1509 0.055 Uiso 1 1 calc R
C30 C 0.0092(3) -0.5548(2) -0.1951(3) 0.0422(9) Uani 1 1 d .
C31 C 0.1185(3) -0.5789(2) -0.2307(3) 0.0454(9) Uani 1 1 d .
H31 H 0.1946 -0.5792 -0.1874 0.054 Uiso 1 1 calc R
C32 C 0.1250(3) -0.6024(2) -0.3243(3) 0.0420(9) Uani 1 1 d .
H32 H 0.2022 -0.6202 -0.3450 0.050 Uiso 1 1 calc R
C33 C 0.0132(3) -0.5988(2) -0.3875(3) 0.0425(9) Uani 1 1 d .
C34 C -0.1015(3) -0.5786(2) -0.3550(3) 0.0426(9) Uani 1 1 d .
H34 H -0.1781 -0.5819 -0.3975 0.051 Uiso 1 1 calc R
C35 C -0.1016(3) -0.5536(2) -0.2593(3) 0.0443(9) Uani 1 1 d .
H35 H -0.1782 -0.5356 -0.2378 0.053 Uiso 1 1 calc R
N10 N 0.0038(3) -0.0053(2) 0.1254(2) 0.0438(8) Uani 1 1 d .
N20 N -0.0176(3) -0.1451(2) -0.3642(2) 0.0426(8) Uani 1 1 d .
N30 N 0.0163(3) -0.6252(2) -0.4857(2) 0.0415(7) Uani 1 1 d .
O10 O -0.0914(2) 0.03018(17) 0.14924(17) 0.0423(6) Uani 1 1 d .
O11 O 0.0997(3) 0.0384(2) 0.1228(2) 0.0573(7) Uani 1 1 d .
O20 O 0.0806(3) -0.12926(18) -0.3976(2) 0.0546(7) Uani 1 1 d .
O21 O -0.1179(2) -0.10955(19) -0.3922(2) 0.0551(7) Uani 1 1 d .
O30 O 0.1122(2) -0.65822(17) -0.5103(2) 0.0519(7) Uani 1 1 d .
O31 O -0.0803(2) -0.61226(18) -0.5428(2) 0.0555(7) Uani 1 1 d .
O40 O 0.8612(3) 0.1799(2) 0.5766(2) 0.0703(9) Uani 1 1 d D
H40 H 0.8767 0.1549 0.5253 0.105 Uiso 1 1 calc .
C40 C 0.9312(4) 0.1314(3) 0.6558(3) 0.0716(13) Uani 1 1 d D
H40A H 0.8967 0.0659 0.6600 0.086 Uiso 1 1 calc R
H40B H 0.9201 0.1658 0.7153 0.086 Uiso 1 1 calc R
C41 C 1.0735(3) 0.1239(3) 0.6489(3) 0.0718(14) Uani 1 1 d D
H41A H 1.0903 0.0638 0.6168 0.108 Uiso 1 1 calc R
H41B H 1.1212 0.1246 0.7134 0.108 Uiso 1 1 calc R
H41C H 1.0992 0.1784 0.6123 0.108 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
C1 0.0317(16) 0.0299(15) 0.034(2) 0.0027(15) 0.0044(17) 0.0002(12)
C2 0.0299(15) 0.0321(16) 0.0336(19) -0.0052(14) 0.0041(16) -0.0027(12)
C3 0.0320(16) 0.0308(16) 0.0353(18) 0.0000(15) 0.0045(16) 0.0009(13)
C10 0.0361(17) 0.0386(18) 0.044(2) -0.0006(16) 0.0065(18) 0.0018(14)
C11 0.046(2) 0.043(2) 0.041(2) -0.0012(17) 0.0086(19) -0.0039(15)
C12 0.0423(19) 0.047(2) 0.046(2) -0.0031(18) 0.0074(19) -0.0021(15)
C13 0.0426(19) 0.048(2) 0.040(2) -0.0007(17) 0.0069(19) 0.0030(16)
C14 0.0419(19) 0.045(2) 0.050(3) 0.0008(18) 0.010(2) 0.0056(15)
C15 0.046(2) 0.045(2) 0.045(2) -0.0047(18) 0.007(2) -0.0025(16)
C20 0.052(2) 0.043(2) 0.050(2) -0.0007(19) 0.003(2) 0.0014(17)
C21 0.0420(18) 0.0397(19) 0.042(2) 0.0019(17) 0.0113(19) 0.0035(15)
C22 0.050(2) 0.048(2) 0.035(2) 0.0006(17) 0.008(2) 0.0065(16)
C23 0.0410(19) 0.0422(19) 0.043(2) 0.0011(17) 0.0057(19) -0.0028(15)
C24 0.045(2) 0.046(2) 0.040(2) 0.0008(17) 0.0026(19) -0.0043(15)
C25 0.0413(19) 0.050(2) 0.048(3) -0.0031(19) 0.008(2) -0.0037(16)
C30 0.046(2) 0.042(2) 0.038(2) -0.0005(17) 0.0057(19) -0.0018(15)
C31 0.047(2) 0.0407(19) 0.048(3) -0.0012(17) 0.006(2) 0.0030(15)
C32 0.045(2) 0.044(2) 0.036(2) -0.0028(17) 0.0041(19) 0.0014(15)
C33 0.044(2) 0.043(2) 0.041(2) -0.0009(17) 0.006(2) 0.0040(15)
C34 0.045(2) 0.043(2) 0.040(2) -0.0028(17) 0.007(2) 0.0017(16)
C35 0.0393(19) 0.046(2) 0.046(2) -0.0013(18) 0.001(2) -0.0021(15)
N10 0.0433(17) 0.0463(17) 0.042(2) -0.0012(14) 0.0059(16) -0.0021(14)
N20 0.0406(17) 0.0427(17) 0.044(2) -0.0013(14) 0.0059(17) -0.0002(13)
N30 0.0444(17) 0.0428(16) 0.0384(19) 0.0019(15) 0.0104(17) 0.0048(13)
O10 0.0405(13) 0.0434(13) 0.0422(15) -0.0013(12) 0.0036(12) 0.0034(11)
O11 0.0555(17) 0.0601(17) 0.0557(18) 0.0023(14) 0.0056(15) 0.0001(13)
O20 0.0586(17) 0.0503(15) 0.0562(19) 0.0034(14) 0.0128(15) 0.0036(12)
O21 0.0499(15) 0.0575(16) 0.0583(19) 0.0011(14) 0.0085(15) -0.0046(13)
O30 0.0593(17) 0.0497(16) 0.0468(17) 0.0023(13) 0.0080(15) -0.0008(13)
O31 0.0525(16) 0.0563(17) 0.0568(19) -0.0014(14) 0.0042(15) 0.0030(13)
O40 0.076(2) 0.0654(19) 0.070(2) 0.0012(17) 0.0118(18) -0.0005(16)
C40 0.075(3) 0.068(3) 0.071(3) 0.000(3) 0.010(3) -0.004(2)
C41 0.076(3) 0.061(3) 0.077(4) -0.005(3) 0.006(3) -0.004(2)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
_geom_angle_publ_flag
C3 C1 C2 3_545 119.2(3) y
C3 C1 C10 3_545 120.5(3) y
C2 C1 C10 . 120.1(3) y
C3 C2 C1 . 119.5(3) y
C3 C2 C20 . 120.2(3) y
C1 C2 C20 . 120.3(3) y
C1 C3 C2 3_545 121.3(3) y
C1 C3 C30 3_545 119.3(3) y
C2 C3 C30 . 119.4(3) y
C11 C10 C15 . 118.6(3) y
C11 C10 C1 . 119.7(3) y
C15 C10 C1 . 121.5(3) y
C10 C11 C12 . 121.4(3) y
C10 C11 H11 . 119.3 ?
C12 C11 H11 . 119.3 ?
C11 C12 C13 . 119.5(3) y
C11 C12 H12 . 120.3 ?
C13 C12 H12 . 120.3 ?
C12 C13 C14 . 120.9(3) y
C12 C13 N10 . 119.7(3) y
C14 C13 N10 . 119.4(3) y
C15 C14 C13 . 118.4(3) y
C15 C14 H14 . 120.8 ?
C13 C14 H14 . 120.8 ?
C14 C15 C10 . 120.9(3) y
C14 C15 H15 . 119.5 ?
C10 C15 H15 . 119.5 ?
C21 C20 C25 . 117.3(4) y
C21 C20 C2 . 121.3(3) y
C25 C20 C2 . 121.4(4) y
C20 C21 C22 . 123.2(3) y
C20 C21 H21 . 118.4 ?
C22 C21 H21 . 118.4 ?
C23 C22 C21 . 116.8(3) y
C23 C22 H22 . 121.6 ?
C21 C22 H22 . 121.6 ?
C24 C23 C22 . 122.8(4) y
C24 C23 N20 . 117.4(3) y
C22 C23 N20 . 119.7(3) y
C23 C24 C25 . 117.5(3) y
C23 C24 H24 . 121.3 ?
C25 C24 H24 . 121.3 ?
C20 C25 C24 . 122.4(4) y
C20 C25 H25 . 118.8 ?
C24 C25 H25 . 118.8 ?
C31 C30 C35 . 117.3(4) y
C31 C30 C3 . 123.5(3) y
C35 C30 C3 . 119.2(3) y
C32 C31 C30 . 124.7(4) y
C32 C31 H31 . 117.7 ?
C30 C31 H31 . 117.7 ?
C31 C32 C33 . 117.0(4) y
C31 C32 H32 . 121.5 ?
C33 C32 H32 . 121.5 ?
C32 C33 C34 . 120.9(4) y
C32 C33 N30 . 118.3(3) y
C34 C33 N30 . 120.5(3) y
C35 C34 C33 . 119.2(4) y
C35 C34 H34 . 120.4 ?
C33 C34 H34 . 120.4 ?
C30 C35 C34 . 120.7(4) y
C30 C35 H35 . 119.6 ?
C34 C35 H35 . 119.6 ?
O11 N10 O10 . 123.8(3) y
O11 N10 C13 . 118.7(3) y
O10 N10 C13 . 117.5(3) y
O21 N20 O20 . 125.1(3) y
O21 N20 C23 . 118.1(3) y
O20 N20 C23 . 116.6(3) y
O30 N30 O31 . 122.3(3) y
O30 N30 C33 . 120.3(3) y
O31 N30 C33 . 117.4(3) y
C40 O40 H40 . 109.5 ?
O40 C40 C41 . 113.6(3) y
O40 C40 H40A . 108.9 ?
C41 C40 H40A . 108.9 ?
O40 C40 H40B . 108.9 ?
C41 C40 H40B . 108.9 ?
H40A C40 H40B . 107.7 ?
C40 C41 H41A . 109.5 ?
C40 C41 H41B . 109.5 ?
H41A C41 H41B . 109.5 ?
C40 C41 H41C . 109.5 ?
H41A C41 H41C . 109.5 ?
H41B C41 H41C . 109.5 ?
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
C1 C3 3_545 1.387(4) y
C1 C2 . 1.407(5) y
C1 C10 . 1.488(4) y
C2 C3 . 1.406(4) y
C2 C20 . 1.483(5) y
C3 C1 3_545 1.387(4) y
C3 C30 . 1.486(5) y
C10 C11 . 1.381(5) y
C10 C15 . 1.402(5) y
C11 C12 . 1.381(5) y
C11 H11 . 0.95 ?
C12 C13 . 1.382(5) y
C12 H12 . 0.95 ?
C13 C14 . 1.402(5) y
C13 N10 . 1.440(4) y
C14 C15 . 1.391(4) y
C14 H14 . 0.95 ?
C15 H15 . 0.95 ?
C20 C21 . 1.382(5) y
C20 C25 . 1.389(5) y
C21 C22 . 1.391(5) y
C21 H21 . 0.95 ?
C22 C23 . 1.390(5) y
C22 H22 . 0.95 ?
C23 C24 . 1.385(5) y
C23 N20 . 1.455(5) y
C24 C25 . 1.393(5) y
C24 H24 . 0.95 ?
C25 H25 . 0.95 ?
C30 C31 . 1.381(5) y
C30 C35 . 1.391(5) y
C31 C32 . 1.371(5) y
C31 H31 . 0.95 ?
C32 C33 . 1.393(5) y
C32 H32 . 0.95 ?
C33 C34 . 1.401(5) y
C33 N30 . 1.438(5) y
C34 C35 . 1.395(5) y
C34 H34 . 0.95 ?
C35 H35 . 0.95 ?
N10 O11 . 1.202(4) y
N10 O10 . 1.223(4) y
N20 O21 . 1.201(4) y
N20 O20 . 1.233(4) y
N30 O30 . 1.222(4) y
N30 O31 . 1.234(4) y
O40 C40 . 1.427(4) y
O40 H40 . 0.84 ?
C40 C41 . 1.548(4) y
C40 H40a . 0.99 ?
C40 H40b . 0.99 ?
C41 H41a . 0.98 ?
C41 H41b . 0.98 ?
C41 H41c . 0.98 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O40 H40 O20 0.84 1.95 2.777(4) 166.1 3_655
|
1501621.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/16/1501621.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_1501621
loop_
_publ_author_name
'Eric Gagnon'
'Thierry Maris'
'Kenneth E. Maly'
'James D. Wuest'
_publ_section_title
;
The potential of intermolecular N/O interactions of nitro groups in
crystal engineering, as revealed by structures of
hexakis(4-nitrophenyl)benzene
;
_journal_name_full Tetrahedron
_journal_page_first 6603
_journal_page_last 6613
_journal_paper_doi 10.1016/j.tet.2007.03.101
_journal_volume 63
_journal_year 2007
_chemical_absolute_configuration rmad
_chemical_compound_source 'Synthesized by the authors. See text'
_chemical_formula_moiety 'C42 H24 N6 O12, 2(C3 H7 N O)'
_chemical_formula_sum 'C48 H38 N8 O14'
_chemical_formula_weight 950.859
_chemical_name_systematic
;
?
;
_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'
_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 116.183(6)
_cell_angle_gamma 90.00
_cell_formula_units_Z 2
_cell_length_a 11.6772(13)
_cell_length_b 17.9809(19)
_cell_length_c 11.9334(13)
_cell_measurement_reflns_used 7796
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 55.52
_cell_measurement_theta_min 4.22
_cell_volume 2248.5(4)
_computing_cell_refinement 'SMART (Bruker, 2003)'
_computing_data_collection 'SMART (Bruker, 2003)'
_computing_data_reduction 'SAINT (Bruker, 2004)'
_computing_molecular_graphics 'SHELXTL (Bruker, 1997)'
_computing_publication_material 'UdMX (local program)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.866
_diffrn_measured_fraction_theta_max 0.866
_diffrn_measurement_device_type 'Bruker Microstar'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator 'Helios optics'
_diffrn_radiation_source 'Micro source'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.040
_diffrn_reflns_av_sigmaI/netI 0.0617
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 19
_diffrn_reflns_limit_k_min -19
_diffrn_reflns_limit_l_max 11
_diffrn_reflns_limit_l_min -12
_diffrn_reflns_number 20684
_diffrn_reflns_theta_full 56.28
_diffrn_reflns_theta_max 56.28
_diffrn_reflns_theta_min 4.13
_diffrn_standards_decay_% 0.00
_diffrn_standards_number 5
_exptl_absorpt_coefficient_mu 0.888
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_correction_T_min 0.8600
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Sadabs (Sheldrick,1996)'
_exptl_crystal_colour Colorless
_exptl_crystal_density_diffrn 1.404
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 988
_exptl_crystal_size_max 0.08
_exptl_crystal_size_mid 0.08
_exptl_crystal_size_min 0.02
_refine_diff_density_max 0.309
_refine_diff_density_min -0.349
_refine_diff_density_rms 0.071
_refine_ls_abs_structure_Flack 0.2(4)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.154
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 631
_refine_ls_number_reflns 4938
_refine_ls_number_restraints 1
_refine_ls_restrained_S_all 1.154
_refine_ls_R_factor_all 0.0838
_refine_ls_R_factor_gt 0.0567
_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^)+(0.0356P)^2^+3.9503P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1329
_refine_ls_wR_factor_ref 0.1442
_reflns_number_gt 3946
_reflns_number_total 4938
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file deposit.cif
_cod_data_source_block jw1167
_cod_original_sg_symbol_H-M P21
_cod_database_code 1501621
loop_
_symmetry_equiv_pos_as_xyz
'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
O10 O 0.9020(5) -0.1929(3) 0.2641(5) 0.0541(17) Uani 1 1 d . . .
O11 O 0.9088(5) -0.1366(3) 0.1083(6) 0.0401(16) Uani 1 1 d . . .
O20 O 0.1213(7) -0.1908(4) -0.0522(7) 0.091(3) Uani 1 1 d . . .
O21 O 0.1215(6) -0.1445(3) -0.2181(7) 0.066(2) Uani 1 1 d . . .
O30 O -0.2047(5) 0.1835(4) -0.1979(6) 0.066(2) Uani 1 1 d . . .
O31 O -0.2235(5) 0.1329(4) -0.0430(6) 0.076(2) Uani 1 1 d . . .
O40 O 0.0967(5) 0.4436(3) 0.4037(7) 0.0533(19) Uani 1 1 d . . .
O41 O 0.0640(5) 0.4895(3) 0.2215(6) 0.0559(18) Uani 1 1 d . . .
O50 O 0.9031(5) 0.4727(3) 0.7262(6) 0.0547(18) Uani 1 1 d . . .
O51 O 0.8282(5) 0.5352(3) 0.5546(5) 0.0558(18) Uani 1 1 d . . .
O60 O 1.2340(5) 0.1306(3) 0.7137(6) 0.060(2) Uani 1 1 d . . .
O61 O 1.2497(5) 0.2107(3) 0.5861(6) 0.0535(18) Uani 1 1 d . . .
N10 N 0.8767(6) -0.1398(3) 0.1921(7) 0.0344(19) Uani 1 1 d . . .
N20 N 0.1502(6) -0.1420(4) -0.1069(9) 0.054(2) Uani 1 1 d . . .
N30 N -0.1587(6) 0.1585(4) -0.0925(7) 0.050(2) Uani 1 1 d . . .
N40 N 0.1152(6) 0.4450(4) 0.3082(8) 0.047(2) Uani 1 1 d . . .
N50 N 0.8426(6) 0.4773(4) 0.6107(7) 0.0427(19) Uani 1 1 d . . .
N60 N 1.1872(6) 0.1684(4) 0.6187(7) 0.044(2) Uani 1 1 d . . .
C1 C 0.5840(6) 0.1000(3) 0.2503(6) 0.0196(17) Uani 1 1 d . . .
C2 C 0.4488(6) 0.1006(3) 0.1844(6) 0.0205(18) Uani 1 1 d . . .
C3 C 0.3822(6) 0.1624(3) 0.1930(6) 0.0200(18) Uani 1 1 d . . .
C4 C 0.4445(6) 0.2226(3) 0.2690(6) 0.0197(18) Uani 1 1 d . . .
C5 C 0.5773(6) 0.2219(3) 0.3349(6) 0.0204(18) Uani 1 1 d . . .
C6 C 0.6472(5) 0.1602(3) 0.3258(6) 0.0213(18) Uani 1 1 d . . .
C10 C 0.6594(6) 0.0360(3) 0.2368(7) 0.0217(19) Uani 1 1 d . . .
C11 C 0.6905(6) -0.0250(3) 0.3123(7) 0.0278(19) Uani 1 1 d . . .
H11 H 0.6614 -0.0281 0.3750 0.033 Uiso 1 1 calc R . .
C12 C 0.7635(7) -0.0827(4) 0.3005(8) 0.037(2) Uani 1 1 d . . .
H12 H 0.7843 -0.1248 0.3541 0.044 Uiso 1 1 calc R . .
C13 C 0.8044(6) -0.0775(4) 0.2101(7) 0.0228(19) Uani 1 1 d . . .
C14 C 0.7752(6) -0.0171(4) 0.1305(7) 0.034(2) Uani 1 1 d . . .
H14 H 0.8031 -0.0144 0.0670 0.041 Uiso 1 1 calc R . .
C15 C 0.7034(7) 0.0390(4) 0.1475(8) 0.036(2) Uani 1 1 d . . .
H15 H 0.6836 0.0815 0.0950 0.043 Uiso 1 1 calc R . .
C20 C 0.3760(6) 0.0358(3) 0.1068(7) 0.0235(19) Uani 1 1 d . . .
C21 C 0.3241(6) -0.0153(4) 0.1590(7) 0.032(2) Uani 1 1 d . . .
H21 H 0.3414 -0.0108 0.2443 0.038 Uiso 1 1 calc R . .
C22 C 0.2478(7) -0.0725(4) 0.0881(8) 0.039(2) Uani 1 1 d . . .
H22 H 0.2112 -0.1071 0.1233 0.047 Uiso 1 1 calc R . .
C23 C 0.2258(6) -0.0783(4) -0.0345(8) 0.028(2) Uani 1 1 d . . .
C24 C 0.2727(6) -0.0290(4) -0.0899(7) 0.034(2) Uani 1 1 d . . .
H24 H 0.2538 -0.0336 -0.1756 0.041 Uiso 1 1 calc R . .
C25 C 0.3494(6) 0.0285(4) -0.0170(8) 0.035(2) Uani 1 1 d . . .
H25 H 0.3840 0.0634 -0.0536 0.042 Uiso 1 1 calc R . .
C30 C 0.2395(6) 0.1620(3) 0.1193(7) 0.0199(18) Uani 1 1 d . . .
C31 C 0.1829(6) 0.1814(3) -0.0054(7) 0.028(2) Uani 1 1 d . . .
H31 H 0.2356 0.1954 -0.0439 0.034 Uiso 1 1 calc R . .
C32 C 0.0541(6) 0.1811(4) -0.0749(7) 0.030(2) Uani 1 1 d . . .
H32 H 0.0163 0.1951 -0.1605 0.036 Uiso 1 1 calc R . .
C33 C -0.0199(6) 0.1599(4) -0.0164(7) 0.0275(19) Uani 1 1 d . . .
C34 C 0.0301(7) 0.1401(4) 0.1076(7) 0.032(2) Uani 1 1 d . . .
H34 H -0.0234 0.1256 0.1450 0.039 Uiso 1 1 calc R . .
C35 C 0.1631(6) 0.1422(3) 0.1766(6) 0.0249(19) Uani 1 1 d . . .
H35 H 0.2013 0.1301 0.2629 0.030 Uiso 1 1 calc R . .
C40 C 0.3654(6) 0.2843(3) 0.2827(8) 0.024(2) Uani 1 1 d . . .
C41 C 0.2987(6) 0.3326(3) 0.1833(7) 0.036(2) Uani 1 1 d . . .
H41 H 0.3095 0.3298 0.1091 0.043 Uiso 1 1 calc R . .
C42 C 0.2161(6) 0.3849(4) 0.1942(8) 0.033(2) Uani 1 1 d . . .
H42 H 0.1703 0.4181 0.1273 0.040 Uiso 1 1 calc R . .
C43 C 0.2014(6) 0.3881(3) 0.3020(8) 0.028(2) Uani 1 1 d . . .
C44 C 0.2668(6) 0.3414(3) 0.4009(8) 0.033(2) Uani 1 1 d . . .
H44 H 0.2556 0.3444 0.4749 0.040 Uiso 1 1 calc R . .
C45 C 0.3498(6) 0.2896(4) 0.3904(8) 0.030(2) Uani 1 1 d . . .
H45 H 0.3966 0.2574 0.4585 0.036 Uiso 1 1 calc R . .
C50 C 0.6491(6) 0.2876(3) 0.4105(7) 0.025(2) Uani 1 1 d . . .
C51 C 0.7069(6) 0.2856(4) 0.5400(7) 0.033(2) Uani 1 1 d . . .
H51 H 0.7009 0.2422 0.5826 0.039 Uiso 1 1 calc R . .
C52 C 0.7741(6) 0.3477(4) 0.6073(8) 0.038(2) Uani 1 1 d . . .
H52 H 0.8152 0.3470 0.6960 0.046 Uiso 1 1 calc R . .
C53 C 0.7794(6) 0.4103(3) 0.5420(8) 0.031(2) Uani 1 1 d . . .
C54 C 0.7269(7) 0.4126(4) 0.4159(8) 0.040(2) Uani 1 1 d . . .
H54 H 0.7356 0.4554 0.3737 0.048 Uiso 1 1 calc R . .
C55 C 0.6607(7) 0.3514(3) 0.3507(8) 0.039(2) Uani 1 1 d . . .
H55 H 0.6216 0.3528 0.2620 0.047 Uiso 1 1 calc R . .
C60 C 0.7887(6) 0.1600(3) 0.3989(7) 0.025(2) Uani 1 1 d . . .
C61 C 0.8456(6) 0.1192(3) 0.5077(7) 0.029(2) Uani 1 1 d . . .
H61 H 0.7944 0.0894 0.5336 0.035 Uiso 1 1 calc R . .
C62 C 0.9778(6) 0.1210(4) 0.5803(7) 0.034(2) Uani 1 1 d . . .
H62 H 1.0173 0.0920 0.6541 0.041 Uiso 1 1 calc R . .
C63 C 1.0481(6) 0.1654(4) 0.5425(7) 0.0242(19) Uani 1 1 d . . .
C64 C 0.9952(6) 0.2053(4) 0.4337(7) 0.030(2) Uani 1 1 d . . .
H64 H 1.0469 0.2345 0.4077 0.036 Uiso 1 1 calc R . .
C65 C 0.8656(6) 0.2020(4) 0.3633(7) 0.0265(19) Uani 1 1 d . . .
H65 H 0.8278 0.2294 0.2876 0.032 Uiso 1 1 calc R . .
O70 O 0.4895(5) 0.4782(3) 0.5443(7) 0.0524(17) Uani 1 1 d . A 1
N70 N 0.4840(6) 0.5365(3) 0.3720(7) 0.043(2) Uani 1 1 d . A 1
C70 C 0.4802(7) 0.4777(5) 0.4383(10) 0.040(2) Uani 1 1 d . A 1
H70 H 0.4692 0.4306 0.3990 0.048 Uiso 1 1 calc R A 1
C71 C 0.4755(8) 0.5300(5) 0.2472(8) 0.053(3) Uani 1 1 d . A 1
H71A H 0.4686 0.4774 0.2236 0.080 Uiso 1 1 calc R A 1
H71B H 0.5523 0.5513 0.2461 0.080 Uiso 1 1 calc R A 1
H71C H 0.4001 0.5568 0.1879 0.080 Uiso 1 1 calc R A 1
C72 C 0.5024(8) 0.6103(4) 0.4283(9) 0.064(3) Uani 1 1 d . A 1
H72A H 0.4927 0.6075 0.5057 0.096 Uiso 1 1 calc R A 1
H72B H 0.4386 0.6446 0.3700 0.096 Uiso 1 1 calc R A 1
H72C H 0.5881 0.6283 0.4470 0.096 Uiso 1 1 calc R A 1
O80 O 0.4761(5) 0.3539(3) 1.0484(7) 0.0498(18) Uani 1 1 d . B 1
N80 N 0.5108(6) 0.2918(3) 0.9008(7) 0.0388(19) Uani 1 1 d . B 1
C80 C 0.4903(7) 0.3522(4) 0.9539(10) 0.037(3) Uani 1 1 d . B 1
H80 H 0.4863 0.3984 0.9137 0.045 Uiso 1 1 calc R B 1
C81 C 0.5204(9) 0.2187(4) 0.9582(10) 0.078(4) Uani 1 1 d . B 1
H81A H 0.5195 0.2246 1.0394 0.117 Uiso 1 1 calc R B 1
H81B H 0.6002 0.1947 0.9697 0.117 Uiso 1 1 calc R B 1
H81C H 0.4479 0.1878 0.9038 0.117 Uiso 1 1 calc R B 1
C82 C 0.5259(7) 0.2931(4) 0.7874(9) 0.056(3) Uani 1 1 d . B 1
H82A H 0.5139 0.3440 0.7548 0.084 Uiso 1 1 calc R B 1
H82B H 0.4623 0.2603 0.7255 0.084 Uiso 1 1 calc R B 1
H82C H 0.6118 0.2758 0.8049 0.084 Uiso 1 1 calc R B 1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O10 0.087(4) 0.042(3) 0.048(4) 0.015(3) 0.044(4) 0.030(3)
O11 0.045(3) 0.042(3) 0.042(4) -0.007(3) 0.027(3) 0.006(2)
O20 0.113(6) 0.068(5) 0.101(6) -0.036(4) 0.056(5) -0.065(4)
O21 0.064(4) 0.056(4) 0.063(5) -0.035(4) 0.015(4) -0.004(3)
O30 0.029(3) 0.119(5) 0.040(4) 0.030(4) 0.007(3) 0.009(3)
O31 0.032(3) 0.134(6) 0.064(5) 0.041(4) 0.023(4) -0.006(3)
O40 0.055(4) 0.057(4) 0.048(5) -0.009(3) 0.023(4) 0.020(3)
O41 0.051(3) 0.042(3) 0.057(4) 0.007(3) 0.007(3) 0.028(3)
O50 0.053(3) 0.049(3) 0.047(4) -0.012(3) 0.008(3) -0.004(3)
O51 0.081(4) 0.030(3) 0.053(4) 0.001(3) 0.026(3) -0.015(3)
O60 0.030(3) 0.088(4) 0.050(4) 0.031(4) 0.008(3) 0.004(3)
O61 0.028(3) 0.061(4) 0.068(5) 0.013(3) 0.017(3) -0.007(3)
N10 0.036(4) 0.028(4) 0.037(5) -0.005(4) 0.014(4) 0.009(3)
N20 0.042(4) 0.036(4) 0.078(7) -0.023(5) 0.021(5) -0.004(3)
N30 0.030(4) 0.074(5) 0.042(5) 0.019(4) 0.014(4) 0.006(4)
N40 0.040(4) 0.043(4) 0.049(6) -0.020(4) 0.011(4) 0.004(3)
N50 0.038(4) 0.040(4) 0.044(5) -0.013(4) 0.013(4) -0.008(3)
N60 0.030(4) 0.042(4) 0.048(5) 0.002(4) 0.006(4) -0.002(3)
C1 0.030(4) 0.025(3) 0.010(4) 0.005(3) 0.014(3) -0.003(3)
C2 0.024(3) 0.019(3) 0.018(4) 0.001(3) 0.009(3) -0.001(3)
C3 0.024(3) 0.020(3) 0.016(4) 0.003(3) 0.010(3) 0.002(3)
C4 0.027(4) 0.016(3) 0.016(4) 0.001(3) 0.009(3) 0.002(3)
C5 0.028(4) 0.024(4) 0.011(4) 0.004(3) 0.011(3) -0.001(3)
C6 0.022(3) 0.020(3) 0.019(4) 0.003(3) 0.006(3) 0.003(3)
C10 0.020(3) 0.022(4) 0.021(5) -0.006(3) 0.008(3) 0.000(3)
C11 0.039(4) 0.030(4) 0.023(5) 0.000(3) 0.022(4) 0.004(3)
C12 0.042(4) 0.024(4) 0.036(6) 0.004(4) 0.011(4) 0.007(3)
C13 0.020(4) 0.028(4) 0.024(5) -0.001(3) 0.012(4) 0.005(3)
C14 0.045(4) 0.034(4) 0.041(5) 0.005(4) 0.035(4) 0.008(4)
C15 0.051(5) 0.027(4) 0.041(5) 0.009(4) 0.029(5) 0.017(4)
C20 0.020(3) 0.023(4) 0.026(5) 0.006(3) 0.009(3) 0.005(3)
C21 0.038(4) 0.030(4) 0.031(5) -0.002(4) 0.018(4) -0.002(3)
C22 0.043(4) 0.031(4) 0.054(6) 0.000(4) 0.031(4) -0.010(3)
C23 0.028(4) 0.028(4) 0.028(5) -0.011(4) 0.013(4) -0.006(3)
C24 0.045(4) 0.033(4) 0.024(5) -0.003(4) 0.015(4) 0.005(4)
C25 0.042(4) 0.021(4) 0.038(6) 0.002(4) 0.014(4) -0.001(3)
C30 0.031(4) 0.016(3) 0.022(5) -0.005(3) 0.021(4) 0.003(3)
C31 0.030(4) 0.035(4) 0.022(5) 0.002(3) 0.013(4) -0.004(3)
C32 0.027(4) 0.043(4) 0.018(5) 0.004(3) 0.008(4) 0.002(3)
C33 0.019(4) 0.037(4) 0.025(5) 0.004(4) 0.009(4) 0.000(3)
C34 0.034(4) 0.045(4) 0.031(5) 0.005(4) 0.027(4) 0.004(3)
C35 0.030(4) 0.037(4) 0.011(4) 0.004(3) 0.012(4) 0.007(3)
C40 0.020(3) 0.016(3) 0.034(5) -0.004(3) 0.011(4) -0.001(3)
C41 0.033(4) 0.027(4) 0.037(6) -0.002(4) 0.005(4) 0.004(3)
C42 0.029(4) 0.033(4) 0.038(6) 0.003(4) 0.015(4) 0.009(3)
C43 0.025(4) 0.023(4) 0.036(5) -0.005(3) 0.011(4) 0.008(3)
C44 0.030(4) 0.025(4) 0.043(6) -0.008(4) 0.014(4) -0.007(3)
C45 0.032(4) 0.024(4) 0.037(6) -0.005(3) 0.017(4) 0.003(3)
C50 0.020(3) 0.024(4) 0.034(5) -0.007(3) 0.014(4) 0.004(3)
C51 0.032(4) 0.035(4) 0.032(6) -0.009(4) 0.015(4) -0.003(3)
C52 0.032(4) 0.050(5) 0.033(5) -0.011(4) 0.014(4) 0.001(3)
C53 0.027(4) 0.017(4) 0.050(6) -0.002(4) 0.018(4) 0.000(3)
C54 0.044(5) 0.037(4) 0.041(6) 0.000(4) 0.020(4) -0.007(4)
C55 0.038(4) 0.024(4) 0.050(6) 0.005(4) 0.014(4) -0.001(3)
C60 0.025(4) 0.020(3) 0.027(5) -0.003(3) 0.007(4) -0.002(3)
C61 0.032(4) 0.027(4) 0.027(5) -0.001(3) 0.010(4) -0.003(3)
C62 0.033(4) 0.025(4) 0.034(5) 0.005(3) 0.004(4) -0.001(3)
C63 0.022(3) 0.028(4) 0.020(5) -0.001(3) 0.008(4) -0.001(3)
C64 0.029(4) 0.045(4) 0.022(5) 0.004(4) 0.017(4) -0.004(3)
C65 0.031(4) 0.040(4) 0.012(4) 0.005(3) 0.014(4) 0.008(3)
O70 0.057(4) 0.066(4) 0.048(4) -0.017(3) 0.035(4) -0.018(3)
N70 0.049(4) 0.019(3) 0.061(5) -0.009(3) 0.023(4) -0.009(3)
C70 0.038(4) 0.045(5) 0.046(7) -0.024(5) 0.026(5) -0.014(4)
C71 0.076(6) 0.053(5) 0.038(6) 0.004(4) 0.031(5) 0.003(4)
C72 0.065(6) 0.043(5) 0.085(8) -0.018(5) 0.034(6) -0.004(4)
O80 0.056(4) 0.064(4) 0.036(4) 0.008(3) 0.027(4) 0.001(3)
N80 0.045(4) 0.035(4) 0.042(5) 0.007(3) 0.024(4) -0.004(3)
C80 0.025(4) 0.028(5) 0.048(7) 0.001(5) 0.007(5) -0.004(3)
C81 0.088(7) 0.040(5) 0.126(11) 0.023(6) 0.066(7) 0.001(5)
C82 0.049(5) 0.045(5) 0.072(8) -0.014(5) 0.025(6) -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 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
O11 N10 O10 123.0(7) y
O11 N10 C13 119.3(7) y
O10 N10 C13 117.7(8) y
O21 N20 O20 123.0(8) y
O21 N20 C23 118.3(9) y
O20 N20 C23 118.6(9) y
O30 N30 O31 123.2(6) y
O30 N30 C33 119.9(8) y
O31 N30 C33 116.9(7) y
O41 N40 O40 124.3(7) y
O41 N40 C43 120.1(9) y
O40 N40 C43 115.7(8) y
O51 N50 O50 123.0(6) y
O51 N50 C53 119.1(7) y
O50 N50 C53 117.7(7) y
O60 N60 O61 123.5(6) y
O60 N60 C63 118.1(7) y
O61 N60 C63 118.3(6) y
C6 C1 C2 119.7(6) y
C6 C1 C10 119.8(5) y
C2 C1 C10 120.5(5) y
C3 C2 C1 119.2(5) y
C3 C2 C20 119.0(5) y
C1 C2 C20 121.7(6) y
C2 C3 C4 121.5(5) y
C2 C3 C30 117.8(5) y
C4 C3 C30 120.7(6) y
C5 C4 C3 119.3(6) y
C5 C4 C40 122.1(5) y
C3 C4 C40 118.5(5) y
C4 C5 C6 120.1(5) y
C4 C5 C50 121.3(5) y
C6 C5 C50 118.5(5) y
C1 C6 C5 120.1(5) y
C1 C6 C60 120.7(6) y
C5 C6 C60 119.1(5) y
C11 C10 C15 117.5(6) y
C11 C10 C1 123.0(8) y
C15 C10 C1 119.5(6) y
C10 C11 C12 122.1(8) y
C10 C11 H11 119 ?
C12 C11 H11 119 ?
C13 C12 C11 118.3(7) y
C13 C12 H12 120.9 ?
C11 C12 H12 120.9 ?
C12 C13 C14 122.1(7) y
C12 C13 N10 119.1(7) y
C14 C13 N10 118.7(8) y
C15 C14 C13 117.0(8) y
C15 C14 H14 121.5 ?
C13 C14 H14 121.5 ?
C10 C15 C14 122.9(7) y
C10 C15 H15 118.5 ?
C14 C15 H15 118.5 ?
C25 C20 C21 118.8(6) y
C25 C20 C2 122.4(6) y
C21 C20 C2 118.6(7) y
C22 C21 C20 120.7(8) y
C22 C21 H21 119.7 ?
C20 C21 H21 119.7 ?
C23 C22 C21 118.4(7) y
C23 C22 H22 120.8 ?
C21 C22 H22 120.8 ?
C24 C23 C22 122.9(7) y
C24 C23 N20 119.3(8) y
C22 C23 N20 117.8(8) y
C23 C24 C25 117.9(8) y
C23 C24 H24 121.1 ?
C25 C24 H24 121.1 ?
C20 C25 C24 121.3(7) y
C20 C25 H25 119.4 ?
C24 C25 H25 119.4 ?
C31 C30 C35 119.3(6) y
C31 C30 C3 120.6(7) y
C35 C30 C3 120.0(6) y
C32 C31 C30 122.1(8) y
C32 C31 H31 119 ?
C30 C31 H31 119 ?
C31 C32 C33 117.5(7) y
C31 C32 H32 121.2 ?
C33 C32 H32 121.2 ?
C34 C33 C32 123.4(6) y
C34 C33 N30 119.4(8) y
C32 C33 N30 117.2(7) y
C33 C34 C35 117.3(7) y
C33 C34 H34 121.4 ?
C35 C34 H34 121.4 ?
C30 C35 C34 120.3(6) y
C30 C35 H35 119.8 ?
C34 C35 H35 119.8 ?
C45 C40 C41 119.6(6) y
C45 C40 C4 119.6(6) y
C41 C40 C4 120.5(8) y
C42 C41 C40 119.4(8) y
C42 C41 H41 120.3 ?
C40 C41 H41 120.3 ?
C43 C42 C41 119.6(7) y
C43 C42 H42 120.2 ?
C41 C42 H42 120.2 ?
C42 C43 C44 121.8(7) y
C42 C43 N40 116.9(7) y
C44 C43 N40 121.3(9) y
C43 C44 C45 118.6(8) y
C43 C44 H44 120.7 ?
C45 C44 H44 120.7 ?
C40 C45 C44 121.0(7) y
C40 C45 H45 119.5 ?
C44 C45 H45 119.5 ?
C51 C50 C55 118.9(6) y
C51 C50 C5 121.2(6) y
C55 C50 C5 119.8(7) y
C50 C51 C52 119.6(7) y
C50 C51 H51 120.2 ?
C52 C51 H51 120.2 ?
C53 C52 C51 118.6(7) y
C53 C52 H52 120.7 ?
C51 C52 H52 120.7 ?
C54 C53 C52 122.7(6) y
C54 C53 N50 117.9(7) y
C52 C53 N50 119.4(7) y
C53 C54 C55 118.1(7) y
C53 C54 H54 120.9 ?
C55 C54 H54 120.9 ?
C54 C55 C50 121.9(8) y
C54 C55 H55 119 ?
C50 C55 H55 119 ?
C65 C60 C61 118.2(6) y
C65 C60 C6 121.6(6) y
C61 C60 C6 120.1(7) y
C60 C61 C62 120.8(7) y
C60 C61 H61 119.6 ?
C62 C61 H61 119.6 ?
C63 C62 C61 118.2(7) y
C63 C62 H62 120.9 ?
C61 C62 H62 120.9 ?
C62 C63 C64 122.5(6) y
C62 C63 N60 118.7(6) y
C64 C63 N60 118.7(7) y
C63 C64 C65 118.3(7) y
C63 C64 H64 120.9 ?
C65 C64 H64 120.9 ?
C64 C65 C60 121.9(7) y
C64 C65 H65 119 ?
C60 C65 H65 119 ?
C70 N70 C71 122.6(7) y
C70 N70 C72 119.0(8) y
C71 N70 C72 118.4(7) y
O70 C70 N70 126.8(8) y
O70 C70 H70 116.6 ?
N70 C70 H70 116.6 ?
N70 C71 H71A 109.5 ?
N70 C71 H71B 109.5 ?
H71A C71 H71B 109.5 ?
N70 C71 H71C 109.5 ?
H71A C71 H71C 109.5 ?
H71B C71 H71C 109.5 ?
N70 C72 H72A 109.5 ?
N70 C72 H72B 109.5 ?
H72A C72 H72B 109.5 ?
N70 C72 H72C 109.5 ?
H72A C72 H72C 109.5 ?
H72B C72 H72C 109.5 ?
C80 N80 C82 123.8(8) y
C80 N80 C81 120.2(9) y
C82 N80 C81 116.0(8) y
O80 C80 N80 126.3(8) y
O80 C80 H80 116.9 ?
N80 C80 H80 116.9 ?
N80 C81 H81A 109.5 ?
N80 C81 H81B 109.5 ?
H81A C81 H81B 109.5 ?
N80 C81 H81C 109.5 ?
H81A C81 H81C 109.5 ?
H81B C81 H81C 109.5 ?
N80 C82 H82A 109.5 ?
N80 C82 H82B 109.5 ?
H82A C82 H82B 109.5 ?
N80 C82 H82C 109.5 ?
H82A C82 H82C 109.5 ?
H82B C82 H82C 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
O10 N10 1.230(8) y
O11 N10 1.215(8) y
O20 N20 1.227(11) y
O21 N20 1.217(10) y
O30 N30 1.215(8) y
O31 N30 1.236(9) y
O40 N40 1.249(9) y
O41 N40 1.233(9) y
O50 N50 1.244(8) y
O51 N50 1.208(8) y
O60 N60 1.224(8) y
O61 N60 1.230(8) y
N10 C13 1.474(9) y
N20 C23 1.471(9) y
N30 C33 1.467(9) y
N40 C43 1.459(10) y
N50 C53 1.462(9) y
N60 C63 1.471(8) y
C1 C6 1.393(8) y
C1 C2 1.419(9) y
C1 C10 1.499(9) y
C2 C3 1.386(9) y
C2 C20 1.497(9) y
C3 C4 1.394(8) y
C3 C30 1.503(9) y
C4 C5 1.395(9) y
C4 C40 1.498(9) y
C5 C6 1.410(9) y
C5 C50 1.499(9) y
C6 C60 1.489(8) y
C10 C11 1.363(9) y
C10 C15 1.373(10) y
C11 C12 1.389(10) y
C11 H11 0.95 ?
C12 C13 1.362(10) y
C12 H12 0.95 ?
C13 C14 1.382(10) y
C14 C15 1.383(10) y
C14 H14 0.95 ?
C15 H15 0.95 ?
C20 C25 1.375(10) y
C20 C21 1.39(1) y
C21 C22 1.38(1) y
C21 H21 0.95 ?
C22 C23 1.374(11) y
C22 H22 0.95 ?
C23 C24 1.357(11) y
C24 C25 1.393(10) y
C24 H24 0.95 ?
C25 H25 0.95 ?
C30 C31 1.38(1) y
C30 C35 1.388(10) y
C31 C32 1.360(9) y
C31 H31 0.95 ?
C32 C33 1.384(11) y
C32 H32 0.95 ?
C33 C34 1.376(10) y
C34 C35 1.402(9) y
C34 H34 0.95 ?
C35 H35 0.95 ?
C40 C45 1.379(10) y
C40 C41 1.397(9) y
C41 C42 1.393(10) y
C41 H41 0.95 ?
C42 C43 1.373(11) y
C42 H42 0.95 ?
C43 C44 1.373(10) y
C44 C45 1.388(10) y
C44 H44 0.95 ?
C45 H45 0.95 ?
C50 C51 1.387(10) y
C50 C55 1.39(1) y
C51 C52 1.397(9) y
C51 H51 0.95 ?
C52 C53 1.386(11) y
C52 H52 0.95 ?
C53 C54 1.351(10) y
C54 C55 1.373(9) y
C54 H54 0.95 ?
C55 H55 0.95 ?
C60 C65 1.377(10) y
C60 C61 1.381(9) y
C61 C62 1.398(9) y
C61 H61 0.95 ?
C62 C63 1.357(10) y
C62 H62 0.95 ?
C63 C64 1.369(10) y
C64 C65 1.370(9) y
C64 H64 0.95 ?
C65 H65 0.95 ?
O70 C70 1.222(9) y
N70 C70 1.332(11) y
N70 C71 1.453(10) y
N70 C72 1.459(10) y
C70 H70 0.95 ?
C71 H71a 0.98 ?
C71 H71b 0.98 ?
C71 H71c 0.98 ?
C72 H72a 0.98 ?
C72 H72b 0.98 ?
C72 H72c 0.98 ?
O80 C80 1.21(1) y
N80 C80 1.332(11) y
N80 C82 1.439(11) y
N80 C81 1.464(10) y
C80 H80 0.95 ?
C81 H81a 0.98 ?
C81 H81b 0.98 ?
C81 H81c 0.98 ?
C82 H82a 0.98 ?
C82 H82b 0.98 ?
C82 H82c 0.98 ?
|
1501622.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/16/1501622.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_1501622
loop_
_publ_author_name
'Thierry Maris'
'Georges Bravic'
'Nguyen Ba Chan'
'Jean-Michel Leger'
'Jean-Claude Bissey'
'Antoine Villesuzanne'
'Ridha Zouari'
'Abdelaziz Daoud'
_publ_section_title
;
Structures and thermal behavior in the series of two-dimensional
molecular composites NH~3~-(CH~2~)~4~-NH~3~ MCl~4~ related to the nature
of the metal M. Part 1 : Crystal structure and phase transition in the
case M=Cu and Pd.
;
_journal_name_full 'J. Phys. Chem. Solids'
_journal_page_first 1963
_journal_page_last 1975
_journal_paper_doi 10.1016/S0022-3697(96)00045-5
_journal_volume 57
_journal_year 1996
_chemical_formula_moiety 'C4 H14 N2, Cl4 Pd'
_chemical_formula_sum 'C4 H14 Cl4 N2 Pd'
_chemical_formula_weight 338.37
_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 103.82(2)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 9.087(2)
_cell_length_b 7.699(2)
_cell_length_c 7.792(2)
_cell_measurement_temperature 293
_cell_volume 529.4(2)
_diffrn_ambient_temperature 293
_diffrn_measurement_device_type Nonius-CAD4
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_source 'Sealed Tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_exptl_absorpt_coefficient_mu 2.707
_exptl_crystal_F_000 332
_refine_ls_hydrogen_treatment constr
_refine_ls_R_factor_gt 0.0178
_refine_ls_structure_factor_coef F
_refine_ls_wR_factor_gt 0.0220
_cod_data_source_file deposit.cif
_cod_data_source_block 2C4PdCl4
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_original_formula_sum 'C4 H14 N2, Cl4 Pd'
_cod_database_code 1501622
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_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
N1 0.0258(8) 0.0378(10) 0.0461(10) 0.0013(7) 0.0126(7) 0.0037(8)
C1 0.0292(9) 0.0474(13) 0.0366(10) 0.0043(9) 0.0033(8) 0.0117(9)
C2 0.0295(9) 0.0270(9) 0.0382(10) 0.0026(8) 0.0133(8) -0.0004(8)
Pd1 0.0210(1) 0.0194(1) 0.0186(1) 0.0008(1) 0.0061(1) -0.0003(1)
Cl1 0.0357(2) 0.0290(2) 0.0266(2) -0.0034(2) 0.0104(2) -0.0080(2)
Cl2 0.0233(2) 0.0359(3) 0.0447(3) 0.0024(2) 0.0066(2) -0.0040(2)
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_thermal_displace_type
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
N1 N Uani 0.2219(2) -0.0385(3) 0.5700(3) 1.000 0.0359(5)
C1 C Uani 0.3614(2) 0.0627(3) 0.6455(3) 1.000 0.0385(6)
C2 C Uani 0.4618(2) 0.0829(3) 0.5173(3) 1.000 0.0307(5)
Pd1 Pd Uani 0.00000 0.00000 0.00000 1.000 0.0194(1)
Cl1 Cl Uani 0.03750(10) 0.19660(10) 0.22970(10) 1.000 0.0299(1)
Cl2 Cl Uani -0.25880(10) 0.04460(10) -0.04900(10) 1.000 0.0349(2)
H1 H Uiso 0.1547(2) -0.0500(3) 0.6667(3) 1.000 0.0500
H2 H Uiso 0.1568(2) 0.0274(3) 0.4542(3) 1.000 0.0500
H3 H Uiso 0.2526(2) -0.1664(3) 0.5336(3) 1.000 0.0500
H4 H Uiso 0.4251(2) -0.0039(3) 0.7617(3) 1.000 0.0500
H5 H Uiso 0.3292(2) 0.1899(3) 0.6822(3) 1.000 0.0500
H6 H Uiso 0.538(3) 0.171(3) 0.562(3) 1.000 0.0500
H7 H Uiso 0.402(3) 0.133(3) 0.409(3) 1.000 0.0500
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'
N N 0.0061 0.0033 ' 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
Cl2 Pd1 Cl2 180.00 . 3_555 yes
Cl1 Pd1 Cl2 89.23(4) 3_555 3_555 yes
Cl1 Pd1 Cl2 90.77(4) . 3_555 yes
Cl1 Pd1 Cl2 89.23(4) . . yes
Cl1 Pd1 Cl1 180.00 . 3_555 yes
Cl1 Pd1 Cl2 90.77(4) 3_555 . yes
C1 N1 H1 109.8(2) . . no
H1 N1 H3 109.4(3) . . no
H2 N1 H3 109.5(3) . . no
C1 N1 H3 109.5(2) . . no
H1 N1 H2 109.5(2) . . no
C1 N1 H2 109.3(2) . . no
N1 C1 C2 112.63(19) . . yes
C1 C2 C2 114.02(19) . 3_656 no
C2 C1 H4 108.4(2) . . no
N1 C1 H5 108.7(2) . . no
N1 C1 H4 108.6(2) . . no
C2 C1 H5 109.0(2) . . no
H4 C1 H5 109.5(3) . . no
C2 C2 H7 111.6(14) 3_656 . no
C1 C2 H6 109.0(14) . . no
C1 C2 H7 108.4(16) . . no
H6 C2 H7 104(2) . . no
C2 C2 H6 109.6(15) 3_656 . no
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 Cl1 2.3064(10) . yes
Pd1 Cl2 2.3163(11) . yes
Pd1 Cl1 2.3064(10) 3_555 yes
Pd1 Cl2 2.3163(11) 3_555 yes
N1 C1 1.485(3) . yes
N1 H1 1.081(3) . no
N1 H2 1.080(3) . no
N1 H3 1.080(3) . no
C1 C2 1.513(3) . no
C2 C2 1.508(3) 3_656 no
C1 H5 1.080(3) . no
C1 H4 1.081(3) . no
C2 H6 0.97(3) . no
C2 H7 0.97(2) . no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1 Cl1 1.081(3) 2.377(2) 3.351(2) 149.2(2) 3_556 yes
N1 H2 Cl1 1.080(3) 2.242(2) 3.316(3) 172.3(2) . yes
N1 H3 Cl2 1.080(3) 2.228(3) 3.235(3) 154.3(2) 2_545 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_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C2 -70.2(2) . 3_656 no
C1 C2 C2 C1 180.00(17) 3_656 3_656 no
|
1501623.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/16/1501623.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_1501623
loop_
_publ_author_name
'Thierry Maris'
'Georges Bravic'
'Nguyen Ba Chan'
'Jean-Michel Leger'
'Jean-Claude Bissey'
'Antoine Villesuzanne'
'Ridha Zouari'
'Abdelaziz Daoud'
_publ_section_title
;
Structures and thermal behavior in the series of two-dimensional
molecular composites NH~3~-(CH~2~)~4~-NH~3~ MCl~4~ related to the nature
of the metal M. Part 1 : Crystal structure and phase transition in the
case M=Cu and Pd.
;
_journal_name_full 'J. Phys. Chem. Solids'
_journal_page_first 1963
_journal_page_last 1975
_journal_paper_doi 10.1016/S0022-3697(96)00045-5
_journal_volume 57
_journal_year 1996
_chemical_compound_source 'see text'
_chemical_formula_moiety 'C4 H14 N2, Cl4 Cu'
_chemical_formula_sum 'C4 H14 Cl4 Cu N2'
_chemical_formula_weight 295.52
_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 93.46(4)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 10.419(3)
_cell_length_b 7.442(1)
_cell_length_c 7.225(5)
_cell_volume 559.2(4)
_diffrn_measurement_device_type 'Nonous CAD-4'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_source 'Sealed Tube'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_exptl_absorpt_coefficient_mu 2.856
_exptl_crystal_density_diffrn 1.755
_exptl_crystal_F_000 298
_refine_ls_hydrogen_treatment constr
_refine_ls_R_factor_gt 0.0420
_refine_ls_structure_factor_coef F
_refine_ls_wR_factor_gt 0.0812
_cod_data_source_file deposit.cif
_cod_data_source_block 2C4CuCl4_ht
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_original_formula_sum 'C4 H14 N2, Cl4 Cu'
_cod_database_code 1501623
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_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
N1 0.0212(15) 0.0374(19) 0.049(2) -0.0049(13) 0.0090(5) 0.0022(15)
C1 0.0224(18) 0.041(2) 0.064(3) -0.0046(19) -0.0016(18) -0.008(2)
C2 0.036(3) 0.045(3) 0.067(3) 0.005(2) 0.004(2) 0.011(2)
Cu1 0.0240(4) 0.0292(4) 0.0350(4) -0.0021(3) 0.0007(3) -0.0049(3)
Cl1 0.0381(5) 0.0304(4) 0.0358(5) 0.0005(4) 0.0031(4) -0.0051(4)
Cl2 0.0253(4) 0.0370(5) 0.0537(6) -0.0021(4) 0.0002(4) -0.0021(5)
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_thermal_displace_type
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
N1 N Uani 0.2009(3) -0.0261(5) 0.5132(6) 1.000 0.0356(10)
C1 C Uani 0.3279(4) 0.0560(7) 0.5598(8) 1.000 0.0426(13)
C2 C Uani 0.4364(5) -0.0427(7) 0.4724(8) 1.000 0.0493(17)
Cu1 Cu Uani 0.00000 0.00000 0.00000 1.000 0.0294(2)
Cl1 Cl Uani 0.02660(10) 0.21260(10) -0.22210(10) 1.000 0.0347(3)
Cl2 Cl Uani 0.21950(10) -0.0398(2) 0.0352(2) 1.000 0.0388(3)
H1 H Uiso 0.133(6) 0.043(8) 0.573(9) 1.000 0.0500
H2 H Uiso 0.183(7) -0.026(8) 0.375(11) 1.000 0.0500
H3 H Uiso 0.201(7) -0.153(9) 0.559(8) 1.000 0.0500
H4 H Uiso 0.344(6) 0.056(8) 0.698(10) 1.000 0.0500
H5 H Uiso 0.326(6) 0.184(9) 0.514(8) 1.000 0.0500
H6 H Uiso 0.439(6) -0.171(8) 0.502(7) 1.000 0.0500
H7 H Uiso 0.423(6) -0.040(7) 0.334(9) 1.000 0.0500
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'
Cu Cu 0.3201 1.2651 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1 Cu1 Cl1 91.99(5) 3_555 4_555 yes
Cl1 Cu1 Cl2 91.95(6) 4_555 3_555 yes
Cl1 Cu1 Cl2 89.72(6) 3_555 . yes
Cl1 Cu1 Cl2 90.28(6) . . yes
Cl1 Cu1 Cl1 91.99(5) . 2_544 yes
Cl1 Cu1 Cl1 180.00 . 3_555 yes
Cl1 Cu1 Cl2 89.72(6) . 3_555 yes
Cl1 Cu1 Cl1 88.01(5) . 4_555 yes
Cl1 Cu1 Cl2 91.95(6) 2_544 . yes
Cl1 Cu1 Cl1 88.01(5) 2_544 3_555 yes
Cl2 Cu1 Cl2 180.00 . 3_555 yes
Cl1 Cu1 Cl2 88.06(6) 4_555 . yes
Cl1 Cu1 Cl2 90.28(6) 3_555 3_555 yes
Cl1 Cu1 Cl2 88.06(6) 2_544 3_555 yes
Cl1 Cu1 Cl1 180.00 2_544 4_555 yes
Cu1 Cl1 Cu1 167.33(6) . 2_554 yes
C1 N1 H3 109(4) . . no
H1 N1 H2 110(5) . . no
C1 N1 H2 110(4) . . no
H2 N1 H3 109(5) . . no
C1 N1 H1 110(4) . . no
H1 N1 H3 109(5) . . no
N1 C1 C2 112.6(4) . . yes
C1 C2 C2 110.6(4) . 3_656 no
N1 C1 H5 108(4) . . no
C2 C1 H4 109(4) . . no
N1 C1 H4 109(4) . . no
H4 C1 H5 109(5) . . no
C2 C1 H5 109(4) . . no
C1 C2 H6 113(3) . . no
C1 C2 H7 110(3) . . no
C2 C2 H6 110(4) 3_656 . no
C2 C2 H7 109(4) 3_656 . no
H6 C2 H7 104(4) . . no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 Cl1 2.935(2) 4_555 yes
Cu1 Cl2 2.3049(19) . yes
Cu1 Cl1 2.935(2) 2_544 yes
Cu1 Cl1 2.2823(17) . yes
Cu1 Cl2 2.3049(19) 3_555 yes
Cu1 Cl1 2.2823(17) 3_555 yes
N1 C1 1.478(6) . yes
N1 H2 1.01(8) . no
N1 H3 1.00(7) . no
N1 H1 0.99(6) . no
C1 C2 1.517(7) . no
C2 C2 1.502(8) 3_656 no
C1 H4 1.00(7) . no
C1 H5 1.01(7) . no
C2 H7 1.00(7) . no
C2 H6 0.98(6) . no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1 Cl1 0.99(6) 2.28(6) 3.245(4) 163(5) 1_556 yes
N1 H2 Cl2 1.01(8) 2.51(8) 3.472(5) 161(6) . yes
N1 H2 Cl1 1.01(8) 2.76(7) 3.371(4) 120(5) 3_555 yes
N1 H3 Cl2 1.00(7) 2.30(7) 3.240(5) 156(5) 4_545 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_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C2 -178.6(4) . 3_656 no
C1 C2 C2 C1 180.0(5) 3_656 3_656 no
|
1501624.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/16/1501624.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_1501624
loop_
_publ_author_name
'Philippe Brunet'
'Eric Demers'
'Thierry Maris'
'Gary D. Enright'
'James D. Wuest'
_publ_section_title
;
Designing Permeable Molecular Crystals That React with External Agents To
Give Crystalline Products
;
_journal_name_full 'Angewandte Chemie International Edition'
_journal_page_first 5303
_journal_page_last 5306
_journal_paper_doi 10.1002/anie.200352252
_journal_volume 42
_journal_year 2003
_chemical_formula_sum 'C85 H116 N24 O12'
_chemical_formula_weight 1666.02
_chemical_name_systematic
;
?
;
_space_group_IT_number 88
_symmetry_cell_setting tetragonal
_symmetry_space_group_name_Hall '-I 4ad'
_symmetry_space_group_name_H-M 'I 41/a :2'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 23.0674(6)
_cell_length_b 23.0674(6)
_cell_length_c 16.1892(6)
_cell_measurement_temperature 173(2)
_cell_volume 8614.4(4)
_computing_cell_refinement 'Smart (Bruker, 1999)'
_computing_data_collection 'Smart (Bruker, 1999)'
_computing_data_reduction 'Saint (Bruker, 1999)'
_computing_molecular_graphics 'XP (Sheldrick, 1997)'
_computing_publication_material 'Platon (Spek, 1999)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type 'Bruker Smart 1K'
_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 0.0478
_diffrn_reflns_av_sigmaI/netI 0.0244
_diffrn_reflns_limit_h_max 23
_diffrn_reflns_limit_h_min -23
_diffrn_reflns_limit_k_max 23
_diffrn_reflns_limit_k_min -23
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_number 25463
_diffrn_reflns_theta_full 20.85
_diffrn_reflns_theta_max 20.85
_diffrn_reflns_theta_min 1.54
_exptl_absorpt_coefficient_mu 0.089
_exptl_crystal_density_diffrn 1.285
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 3560
_refine_diff_density_max 0.535
_refine_diff_density_min -0.415
_refine_diff_density_rms 0.077
_refine_ls_extinction_coef 0.0
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.076
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 273
_refine_ls_number_reflns 2269
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.076
_refine_ls_R_factor_all 0.0974
_refine_ls_R_factor_gt 0.0795
_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^)+(0.1694P)^2^+20.3528P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2306
_refine_ls_wR_factor_ref 0.2493
_reflns_number_gt 1759
_reflns_number_total 2269
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file deposit.cif
_cod_data_source_block jiw233
_cod_original_sg_symbol_H-M I41/a
_cod_database_code 1501624
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
O1 O 0.6015(3) 0.1955(2) 0.0203(4) 0.0979(18) Uani 1 1 d .
O2 O 0.5153(3) 0.1127(2) 0.0584(3) 0.0989(18) Uani 1 1 d .
O3 O 0.95339(16) 0.53437(15) 0.0295(2) 0.0539(11) Uani 1 1 d .
N1 N 0.62095(16) 0.40011(16) 0.1460(2) 0.0319(11) Uani 1 1 d .
H1 H 0.6172 0.4372 0.1577 0.038 Uiso 1 1 calc R
N2 N 0.65500(17) 0.33535(16) 0.0471(2) 0.0330(11) Uani 1 1 d .
N3 N 0.72411(16) 0.37131(17) -0.0506(2) 0.0313(11) Uani 1 1 d .
N4 N 0.68354(16) 0.43497(16) 0.0502(2) 0.0316(11) Uani 1 1 d .
N5 N 0.69416(18) 0.27571(17) -0.0502(2) 0.0402(12) Uani 1 1 d .
H5 H 0.6766 0.2475 -0.0236 0.048 Uiso 1 1 calc R
N6 N 0.74697(18) 0.46728(16) -0.0500(3) 0.0392(11) Uani 1 1 d .
H6 H 0.7704 0.4586 -0.0911 0.047 Uiso 1 1 calc R
C1 C 0.5000 0.2500 0.3750 0.023(2) Uani 1 4 d S
C2 C 0.53331(18) 0.29200(18) 0.3169(3) 0.0249(11) Uani 1 1 d .
C3 C 0.5677(2) 0.2683(2) 0.2550(3) 0.0313(12) Uani 1 1 d .
H3 H 0.5717 0.2274 0.2523 0.038 Uiso 1 1 calc R
C4 C 0.5964(2) 0.3019(2) 0.1973(3) 0.0318(12) Uani 1 1 d .
H4 H 0.6194 0.2841 0.1559 0.038 Uiso 1 1 calc R
C5 C 0.59138(19) 0.3617(2) 0.2002(3) 0.0283(12) Uani 1 1 d .
C6 C 0.5578(2) 0.3861(2) 0.2614(3) 0.0328(13) Uani 1 1 d .
H6A H 0.5544 0.4271 0.2645 0.039 Uiso 1 1 calc R
C7 C 0.5287(2) 0.3517(2) 0.3188(3) 0.0300(12) Uani 1 1 d .
H7 H 0.5054 0.3696 0.3599 0.036 Uiso 1 1 calc R
C8 C 0.6541(2) 0.3882(2) 0.0788(3) 0.0285(12) Uani 1 1 d .
C9 C 0.6916(2) 0.3294(2) -0.0180(3) 0.0311(12) Uani 1 1 d .
C10 C 0.7169(2) 0.4238(2) -0.0152(3) 0.0307(12) Uani 1 1 d .
C11 C 0.7241(3) 0.2618(2) -0.1257(4) 0.0506(15) Uani 1 1 d .
H11A H 0.7650 0.2742 -0.1205 0.061 Uiso 1 1 calc R
H11B H 0.7065 0.2843 -0.1714 0.061 Uiso 1 1 calc R
C12 C 0.7227(4) 0.1999(4) -0.1473(7) 0.115(3) Uani 1 1 d .
H12 H 0.7322 0.1918 -0.2032 0.137 Uiso 1 1 calc R
C13 C 0.7115(5) 0.1567(4) -0.1054(7) 0.127(3) Uani 1 1 d .
H13A H 0.7016 0.1609 -0.0488 0.152 Uiso 1 1 calc R
H13B H 0.7127 0.1193 -0.1298 0.152 Uiso 1 1 calc R
C14 C 0.7437(3) 0.5272(2) -0.0249(4) 0.0498(16) Uani 1 1 d .
H14A H 0.7099 0.5455 -0.0521 0.060 Uiso 1 1 calc R
H14B H 0.7373 0.5290 0.0355 0.060 Uiso 1 1 calc R
C15 C 0.7945(4) 0.5597(3) -0.0448(6) 0.105(3) Uani 1 1 d .
H15 H 0.8267 0.5431 -0.0170 0.126 Uiso 1 1 calc R
C16 C 0.8108(4) 0.6003(3) -0.0839(7) 0.121(4) Uani 1 1 d .
H16A H 0.7840 0.6222 -0.1158 0.145 Uiso 1 1 calc R
H16B H 0.8506 0.6108 -0.0832 0.145 Uiso 1 1 calc R
C20 C 0.6106(4) 0.1485(4) 0.0771(5) 0.095(3) Uani 1 1 d .
H20A H 0.6384 0.1609 0.1201 0.114 Uiso 1 1 calc R
H20B H 0.6279 0.1154 0.0471 0.114 Uiso 1 1 calc R
C21 C 0.5564(5) 0.1292(5) 0.1172(5) 0.123(4) Uani 1 1 d .
H21A H 0.5648 0.0960 0.1541 0.148 Uiso 1 1 calc R
H21B H 0.5406 0.1611 0.1514 0.148 Uiso 1 1 calc R
C22 C 0.5039(4) 0.1612(4) 0.0091(7) 0.110(3) Uani 1 1 d .
H22A H 0.4901 0.1933 0.0445 0.132 Uiso 1 1 calc R
H22B H 0.4727 0.1516 -0.0305 0.132 Uiso 1 1 calc R
C23 C 0.5549(3) 0.1802(4) -0.0365(5) 0.095(3) Uani 1 1 d .
H23A H 0.5448 0.2142 -0.0709 0.115 Uiso 1 1 calc R
H23B H 0.5680 0.1487 -0.0737 0.115 Uiso 1 1 calc R
C30 C 0.9508(3) 0.5064(3) -0.0477(4) 0.0619(17) Uani 1 1 d .
H30A H 0.9272 0.5300 -0.0862 0.074 Uiso 1 1 calc R
H30B H 0.9316 0.4683 -0.0412 0.074 Uiso 1 1 calc R
C31 C 0.9896(3) 0.5024(3) 0.0840(4) 0.0637(17) Uani 1 1 d .
H31A H 0.9717 0.4641 0.0952 0.076 Uiso 1 1 calc R
H31B H 0.9930 0.5233 0.1371 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
O1 0.116(4) 0.062(3) 0.116(4) 0.003(3) 0.014(4) -0.030(3)
O2 0.115(4) 0.083(4) 0.099(4) -0.014(3) 0.022(3) -0.035(3)
O3 0.057(3) 0.046(2) 0.059(3) -0.006(2) 0.000(2) 0.0045(19)
N1 0.041(2) 0.024(2) 0.031(2) 0.0009(18) 0.011(2) -0.0009(18)
N2 0.040(2) 0.032(3) 0.028(2) -0.0018(19) 0.009(2) -0.0035(19)
N3 0.032(2) 0.033(2) 0.029(2) 0.003(2) 0.0069(18) -0.0020(19)
N4 0.037(2) 0.030(2) 0.028(2) 0.0000(18) 0.009(2) -0.0040(19)
N5 0.057(3) 0.029(3) 0.035(2) -0.007(2) 0.019(2) -0.005(2)
N6 0.047(3) 0.029(2) 0.042(3) 0.002(2) 0.019(2) -0.003(2)
C1 0.024(3) 0.024(3) 0.021(5) 0.000 0.000 0.000
C2 0.024(2) 0.028(3) 0.023(3) 0.000(2) -0.002(2) 0.000(2)
C3 0.040(3) 0.024(3) 0.030(3) 0.000(2) 0.004(2) 0.003(2)
C4 0.038(3) 0.030(3) 0.027(3) 0.000(2) 0.011(2) 0.001(2)
C5 0.027(3) 0.035(3) 0.023(3) 0.001(2) 0.003(2) -0.002(2)
C6 0.043(3) 0.021(3) 0.035(3) -0.001(2) 0.005(2) 0.000(2)
C7 0.032(3) 0.032(3) 0.026(3) -0.001(2) 0.005(2) 0.001(2)
C8 0.032(3) 0.031(3) 0.022(3) 0.000(2) 0.002(2) 0.001(2)
C9 0.033(3) 0.037(3) 0.023(3) 0.002(2) 0.002(2) -0.001(2)
C10 0.029(3) 0.033(3) 0.030(3) 0.002(2) 0.002(2) 0.001(2)
C11 0.056(4) 0.038(3) 0.057(4) -0.013(3) 0.017(3) -0.002(3)
C12 0.132(8) 0.070(6) 0.142(8) 0.016(6) 0.081(7) -0.006(5)
C13 0.148(9) 0.081(6) 0.151(9) -0.005(7) -0.010(7) 0.014(6)
C14 0.057(4) 0.036(3) 0.056(4) 0.004(3) 0.025(3) -0.008(3)
C15 0.107(6) 0.049(5) 0.158(8) -0.024(5) 0.056(6) -0.017(4)
C16 0.108(7) 0.046(5) 0.207(10) 0.013(6) 0.081(7) -0.008(4)
C20 0.095(6) 0.098(6) 0.092(6) 0.005(5) -0.020(5) -0.032(5)
C21 0.151(9) 0.145(8) 0.074(6) -0.031(5) 0.011(6) -0.081(7)
C22 0.093(6) 0.069(5) 0.167(9) 0.025(6) 0.027(6) -0.009(5)
C23 0.083(6) 0.087(6) 0.116(7) 0.029(5) -0.013(5) -0.008(4)
C30 0.055(4) 0.073(4) 0.058(4) -0.005(3) -0.009(3) 0.007(3)
C31 0.061(4) 0.083(5) 0.047(4) 0.001(3) -0.004(3) 0.006(3)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
C20 O1 C23 109.1(5) . .
C21 O2 C22 107.4(7) . .
C30 O3 C31 109.8(4) . .
C8 N1 C5 129.8(4) . .
C8 N2 C9 113.8(4) . .
C9 N3 C10 114.5(4) . .
C10 N4 C8 114.0(4) . .
C9 N5 C11 123.7(4) . .
C10 N6 C14 124.9(4) . .
C2 C1 C2 105.5(3) 16_656 11_666
C2 C1 C2 111.50(16) 16_656 6_554
C2 C1 C2 111.50(16) 11_666 6_554
C2 C1 C2 111.50(16) 16_656 .
C2 C1 C2 111.50(16) 11_666 .
C2 C1 C2 105.5(3) 6_554 .
C7 C2 C3 116.8(4) . .
C7 C2 C1 124.8(4) . .
C3 C2 C1 118.3(3) . .
C4 C3 C2 122.7(4) . .
C3 C4 C5 119.7(4) . .
C6 C5 C4 118.6(4) . .
C6 C5 N1 117.4(4) . .
C4 C5 N1 124.0(4) . .
C5 C6 C7 121.2(4) . .
C2 C7 C6 121.0(4) . .
N2 C8 N4 126.3(4) . .
N2 C8 N1 120.4(4) . .
N4 C8 N1 113.3(4) . .
N3 C9 N5 119.3(4) . .
N3 C9 N2 125.7(4) . .
N5 C9 N2 115.0(4) . .
N4 C10 N6 119.1(4) . .
N4 C10 N3 125.5(4) . .
N6 C10 N3 115.5(4) . .
N5 C11 C12 114.1(5) . .
C13 C12 C11 131.2(10) . .
C15 C14 N6 113.4(5) . .
C16 C15 C14 142.4(11) . .
O1 C20 C21 112.6(8) . .
O2 C21 C20 110.9(6) . .
O2 C22 C23 112.3(7) . .
C22 C23 O1 110.4(7) . .
O3 C30 C31 111.6(5) . 9_765
O3 C31 C30 111.3(5) . 9_765
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O1 C20 1.438(10) .
O1 C23 1.459(10) .
O2 C21 1.397(10) .
O2 C22 1.398(10) .
O3 C30 1.408(7) .
O3 C31 1.422(7) .
N1 C8 1.358(6) .
N1 C5 1.421(6) .
N2 C8 1.323(6) .
N2 C9 1.356(6) .
N3 C9 1.333(6) .
N3 C10 1.349(6) .
N4 C10 1.335(6) .
N4 C8 1.356(6) .
N5 C9 1.345(6) .
N5 C11 1.440(6) .
N6 C10 1.342(6) .
N6 C14 1.443(6) .
C1 C2 1.554(4) 16_656
C1 C2 1.554(4) 11_666
C1 C2 1.554(4) 6_554
C1 C2 1.554(4) .
C2 C7 1.382(6) .
C2 C3 1.390(6) .
C3 C4 1.382(6) .
C4 C5 1.385(6) .
C5 C6 1.377(6) .
C6 C7 1.395(6) .
C11 C12 1.470(10) .
C12 C13 1.233(11) .
C14 C15 1.427(10) .
C15 C16 1.191(10) .
C20 C21 1.477(11) .
C22 C23 1.455(11) .
C30 C31 1.508(8) 9_765
C31 C30 1.508(8) 9_765
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1 N3 0.88 2.16 3.028(5) 170.0 8_454
N5 H5 O1 0.88 2.22 3.049(6) 156.2 .
N6 H6 N4 0.88 2.12 2.993(5) 171.1 7_544
|
1501625.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/16/1501625.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_1501625
loop_
_publ_author_name
'Philippe Brunet'
'Eric Demers'
'Thierry Maris'
'Gary D. Enright'
'James D. Wuest'
_publ_section_title
;
Designing Permeable Molecular Crystals That React with External Agents To
Give Crystalline Products
;
_journal_name_full 'Angewandte Chemie International Edition'
_journal_page_first 5303
_journal_page_last 5306
_journal_paper_doi 10.1002/anie.200352252
_journal_volume 42
_journal_year 2003
_chemical_formula_moiety '0.40 (C69 H100 N24 S8) 0.60(C61 H28 N24)'
_chemical_formula_sum 'C64.2 H80.8 N24 S3.2'
_chemical_name_systematic
;
?
;
_space_group_IT_number 88
_symmetry_cell_setting tetragonal
_symmetry_space_group_name_Hall '-I 4ad'
_symmetry_space_group_name_H-M 'I 41/a :2'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 20.988(2)
_cell_length_b 20.988(2)
_cell_length_c 16.816(3)
_cell_measurement_temperature 173(2)
_cell_volume 7407.4(17)
_computing_cell_refinement 'Smart (Bruker, 1999)'
_computing_data_collection 'Smart (Bruker, 1999)'
_computing_data_reduction 'Saint (Bruker, 1999)'
_computing_molecular_graphics 'XP (Sheldrick, 1997)'
_computing_publication_material 'Platon (Spek, 1999)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type 'Bruker Smart 1K'
_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 0.2328
_diffrn_reflns_av_sigmaI/netI 0.1244
_diffrn_reflns_limit_h_max 21
_diffrn_reflns_limit_h_min -21
_diffrn_reflns_limit_k_max 21
_diffrn_reflns_limit_k_min -21
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_number 17939
_diffrn_reflns_theta_full 20.99
_diffrn_reflns_theta_max 20.99
_diffrn_reflns_theta_min 1.55
_exptl_absorpt_coefficient_mu 0.301
_exptl_absorpt_correction_T_max 0.9763
_exptl_absorpt_correction_T_min 0.9422
_exptl_crystal_colour Colourless
_exptl_crystal_density_diffrn 1.365
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 3240
_exptl_crystal_size_max 0.20
_exptl_crystal_size_mid 0.15
_exptl_crystal_size_min 0.08
_refine_diff_density_max 0.620
_refine_diff_density_min -0.570
_refine_diff_density_rms 0.094
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.306
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 214
_refine_ls_number_reflns 1976
_refine_ls_number_restraints 45
_refine_ls_restrained_S_all 1.299
_refine_ls_R_factor_all 0.2324
_refine_ls_R_factor_gt 0.1210
_refine_ls_shift/su_max 0.524
_refine_ls_shift/su_mean 0.038
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1700P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.3330
_refine_ls_wR_factor_ref 0.3894
_reflns_number_gt 865
_reflns_number_total 1976
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file deposit.cif
_cod_data_source_block Jiw301
_cod_original_cell_volume 7407.6(16)
_cod_original_sg_symbol_H-M I41/a
_cod_database_code 1501625
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.0000 0.7500 -0.1250 0.053(2) Uani 1 4 d S . .
C2 C 0.04334(13) 0.71366(14) -0.06685(17) 0.0481(10) Uani 1 1 d . . .
C3 C 0.01798(14) 0.67317(15) -0.01194(16) 0.0567(11) Uani 1 1 d . . .
H3 H -0.0265 0.6649 -0.0141 0.068 Uiso 1 1 calc R . .
C4 C 0.05265(14) 0.64393(14) 0.04562(17) 0.0548(11) Uani 1 1 d . . .
H4 H 0.0325 0.6157 0.0819 0.066 Uiso 1 1 calc R . .
C5 C 0.11799(14) 0.65550(14) 0.05123(18) 0.0544(11) Uani 1 1 d . . .
C6 C 0.14540(15) 0.69572(16) -0.00338(18) 0.0672(12) Uani 1 1 d . . .
H6 H 0.1899 0.7040 -0.0015 0.081 Uiso 1 1 calc R . .
C7 C 0.10762(15) 0.72451(15) -0.06185(18) 0.0621(12) Uani 1 1 d . . .
H7 H 0.1271 0.7524 -0.0991 0.075 Uiso 1 1 calc R . .
N8 N 0.15705(11) 0.62935(13) 0.11070(13) 0.0602(9) Uani 1 1 d . . .
H8 H 0.1982 0.6320 0.1014 0.072 Uiso 1 1 calc . . .
C9 C 0.14114(15) 0.60055(14) 0.18036(17) 0.0541(11) Uani 1 1 d . . .
N10 N 0.08081(11) 0.60058(11) 0.20489(14) 0.0552(9) Uani 1 1 d . . .
C11 C 0.07291(14) 0.57071(14) 0.27516(18) 0.0561(11) Uani 1 1 d . . .
N12 N 0.11756(12) 0.54392(11) 0.31955(14) 0.0574(9) Uani 1 1 d . . .
C13 C 0.17669(15) 0.55018(15) 0.28893(19) 0.0608(11) Uani 1 1 d . . .
N14 N 0.19267(12) 0.57625(12) 0.22001(15) 0.0611(9) Uani 1 1 d . . .
N20 N 0.01347(13) 0.56882(14) 0.30154(15) 0.0782(10) Uani 1 1 d . . .
H20 H -0.0162 0.5845 0.2702 0.094 Uiso 1 1 calc . . .
C21 C -0.0065(2) 0.54376(18) 0.3760(2) 0.1098(18) Uani 1 1 d D . .
H21A H 0.0277 0.5161 0.3971 0.132 Uiso 1 1 calc R . .
H21B H -0.0445 0.5167 0.3672 0.132 Uiso 1 1 calc R . .
C22 C -0.0223(3) 0.5927(2) 0.4369(3) 0.1862(10) Uani 1 1 d DU . .
H22A H -0.0678 0.6034 0.4293 0.223 Uiso 1 1 calc R A 1
H22B H -0.0191 0.5712 0.4892 0.223 Uiso 0.3881(14) 1 calc PR B 1
C23 C 0.0121(2) 0.6542(2) 0.4448(4) 0.2397(11) Uani 1 1 d DU B 1
H23C H -0.0136 0.6859 0.4743 0.288 Uiso 1 1 calc R B 1
H23D H 0.0236 0.6718 0.3921 0.288 Uiso 1 1 calc R B 1
S24 S 0.08033(11) 0.63168(13) 0.49889(14) 0.0813(10) Uani 0.3881(14) 1 d PD B 1
C25 C 0.0550(7) 0.6305(8) 0.5998(4) 0.2147(12) Uani 0.3881(14) 1 d PDU B 1
H25D H 0.0905 0.6171 0.6338 0.322 Uiso 0.3881(14) 1 calc PR B 1
H25E H 0.0195 0.6005 0.6057 0.322 Uiso 0.3881(14) 1 calc PR B 1
H25F H 0.0410 0.6733 0.6154 0.322 Uiso 0.3881(14) 1 calc PR B 1
N30 N 0.22259(12) 0.52398(15) 0.33297(18) 0.0860(12) Uani 1 1 d D B 2
H30 H 0.2111 0.5056 0.3777 0.103 Uiso 1 1 calc . C 2
C31 C 0.28930(16) 0.52338(19) 0.3133(3) 0.131(2) Uani 1 1 d D B 2
H31C H 0.3099 0.5639 0.3290 0.158 Uiso 1 1 calc R B 2
H31D H 0.2956 0.5168 0.2555 0.158 Uiso 1 1 calc R B 2
C32 C 0.3167(2) 0.4671(2) 0.3612(4) 0.1862(10) Uani 1 1 d DU B 2
H32C H 0.3137 0.4771 0.4186 0.223 Uiso 1 1 calc R B 2
H32D H 0.2903 0.4288 0.3511 0.223 Uiso 0.3881(14) 1 calc PR B 2
C33 C 0.38474(13) 0.45228(15) 0.3410(2) 0.2397(11) Uani 1 1 d DU B 2
H33C H 0.3898 0.4485 0.2826 0.288 Uiso 1 1 calc R B 2
H33D H 0.3976 0.4114 0.3657 0.288 Uiso 1 1 calc R B 2
S34 S 0.43339(13) 0.51616(15) 0.3782(2) 0.1186(13) Uani 0.3881(14) 1 d PRD B 2
C35 C 0.39698(13) 0.57300(15) 0.4441(2) 0.2147(12) Uani 0.3881(14) 1 d PRDU B 2
H35D H 0.4286 0.6050 0.4598 0.322 Uiso 0.3881(14) 1 calc PR B 2
H35E H 0.3811 0.5510 0.4916 0.322 Uiso 0.3881(14) 1 calc PR B 2
H35F H 0.3614 0.5940 0.4169 0.322 Uiso 0.3881(14) 1 calc PR B 2
C352 C 0.0598(4) 0.6548(3) 0.5665(5) 0.191(3) Uiso 0.893(7) 1 d P D 3
C252 C 0.4127(4) 0.5222(4) 0.4763(6) 0.238(4) Uiso 0.893(7) 1 d P D 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
C1 0.060(2) 0.060(2) 0.039(4) 0.000 0.000 0.000
C2 0.0478(17) 0.0600(19) 0.0367(16) -0.0036(16) -0.0146(15) 0.0010(16)
C3 0.0514(18) 0.088(2) 0.0306(17) 0.0183(17) -0.0042(15) -0.0231(18)
C4 0.071(2) 0.067(2) 0.0264(17) 0.0041(17) -0.0067(16) -0.0235(17)
C5 0.0526(19) 0.069(2) 0.0418(19) 0.0052(17) 0.0031(17) -0.0004(18)
C6 0.053(2) 0.092(2) 0.056(2) 0.020(2) 0.0010(18) -0.0075(19)
C7 0.076(2) 0.075(2) 0.0361(18) 0.0159(17) 0.0037(18) 0.0078(19)
N8 0.0465(15) 0.101(2) 0.0329(14) 0.0248(14) -0.0008(13) 0.0011(15)
C9 0.077(2) 0.0477(18) 0.0378(18) -0.0037(17) -0.0020(17) -0.0040(18)
N10 0.0557(15) 0.0633(16) 0.0468(16) 0.0067(14) 0.0012(14) 0.0017(14)
C11 0.066(2) 0.0540(19) 0.048(2) 0.0034(17) 0.0059(18) 0.0034(17)
N12 0.0682(16) 0.0561(15) 0.0478(15) 0.0106(14) -0.0025(15) 0.0005(14)
C13 0.068(2) 0.064(2) 0.050(2) 0.0053(18) -0.0123(18) 0.0017(18)
N14 0.0593(16) 0.0849(18) 0.0390(15) 0.0187(14) 0.0021(13) -0.0043(16)
N20 0.0829(19) 0.103(2) 0.0490(17) 0.0293(16) 0.0214(16) 0.0077(18)
C21 0.125(3) 0.133(4) 0.071(3) 0.010(3) 0.024(3) 0.024(3)
C22 0.1843(17) 0.1871(17) 0.1873(18) 0.0010(14) 0.0120(14) 0.0046(14)
C23 0.2378(18) 0.2408(18) 0.2404(19) -0.0021(15) 0.0010(15) 0.0008(15)
S24 0.0748(16) 0.116(2) 0.0532(15) 0.0041(15) 0.0151(14) 0.0017(15)
C25 0.2152(19) 0.2140(19) 0.2150(19) 0.0003(16) -0.0012(16) -0.0008(16)
N30 0.0665(18) 0.123(2) 0.069(2) 0.0269(19) -0.0150(17) 0.0015(18)
C31 0.104(3) 0.175(4) 0.116(3) 0.075(3) -0.019(3) 0.004(3)
C32 0.1843(17) 0.1871(17) 0.1873(18) 0.0010(14) 0.0120(14) 0.0046(14)
C33 0.2378(18) 0.2408(18) 0.2404(19) -0.0021(15) 0.0010(15) 0.0008(15)
S34 0.101(2) 0.115(2) 0.140(3) 0.029(2) -0.001(2) -0.016(2)
C35 0.2152(19) 0.2140(19) 0.2150(19) 0.0003(16) -0.0012(16) -0.0008(16)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C2 113.85(11) 11_565 . y
C2 C1 C2 113.85(11) 11_565 6_464 y
C2 C1 C2 101.0(2) . 6_464 y
C2 C1 C2 101.0(2) 11_565 16_665 y
C2 C1 C2 113.85(11) . 16_665 y
C2 C1 C2 113.85(11) 6_464 16_665 y
C3 C2 C7 116.5(3) . . y
C3 C2 C1 120.6(2) . . y
C7 C2 C1 122.6(2) . . y
C4 C3 C2 123.7(3) . . y
C3 C4 C5 119.8(3) . . y
C6 C5 C4 118.2(3) . . y
C6 C5 N8 118.1(3) . . y
C4 C5 N8 123.6(3) . . y
C5 C6 C7 119.8(3) . . y
C2 C7 C6 121.9(3) . . y
C9 N8 C5 130.1(2) . . y
N10 C9 N8 120.0(3) . . y
N10 C9 N14 126.9(3) . . y
N8 C9 N14 113.0(3) . . y
C9 N10 C11 112.8(2) . . y
N20 C11 N12 117.7(3) . . y
N20 C11 N10 115.1(3) . . y
N12 C11 N10 127.2(3) . . y
C11 N12 C13 113.2(3) . . y
N14 C13 N30 118.2(3) . . y
N14 C13 N12 127.3(3) . . y
N30 C13 N12 114.3(3) . . y
C13 N14 C9 112.3(3) . . y
C11 N20 C21 125.8(3) . . y
N20 C21 C22 114.6(3) . . y
C23 C22 C21 123.7(5) . . y
C22 C23 S24 102.0(4) . . y
C23 S24 C25 104.7(5) . . y
C13 N30 C31 125.4(3) . . y
N30 C31 C32 104.4(3) . . y
C33 C32 C31 113.3(4) . . y
C32 C33 S34 107.9(2) . . y
C33 S34 C35 117.9 . . y
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.538(3) 11_565 y
C1 C2 1.538(3) . y
C1 C2 1.538(3) 6_464 y
C1 C2 1.538(3) 16_665 y
C2 C3 1.363(4) . y
C2 C7 1.371(4) . y
C3 C4 1.358(4) . y
C4 C5 1.396(4) . y
C5 C6 1.374(4) . y
C5 N8 1.405(4) . y
C6 C7 1.400(4) . y
N8 C9 1.360(4) . y
C9 N10 1.332(4) . y
C9 N14 1.369(4) . y
N10 C11 1.348(4) . y
C11 N20 1.324(4) . y
C11 N12 1.323(4) . y
N12 C13 1.350(4) . y
C13 N14 1.325(4) . y
C13 N30 1.334(4) . y
N20 C21 1.421(4) . y
C21 C22 1.487(6) . y
C22 C23 1.484(7) . y
C23 S24 1.761(6) . y
S24 C25 1.778(7) . y
N30 C31 1.439(4) . y
C31 C32 1.541(6) . y
C32 C33 1.502(5) . y
C33 S34 1.7980 . y
S34 C35 1.7990 . y
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N8 H8 N12 0.88 2.08 2.956(3) 174.2 4_454
N20 H20 S24 0.88 2.81 3.585(4) 147.8 11_566
N30 H30 N14 0.88 2.18 3.045(4) 166.5 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_publ_flag
C2 C1 C2 C3 -64.62(18) 11_565 y
C2 C1 C2 C3 57.8(2) 6_464 y
C2 C1 C2 C3 -179.7(3) 16_665 y
C2 C1 C2 C7 121.9(3) 11_565 y
C2 C1 C2 C7 -115.6(3) 6_464 y
C2 C1 C2 C7 6.8(3) 16_665 y
C7 C2 C3 C4 -0.1(5) . y
C1 C2 C3 C4 -174.0(2) . y
C2 C3 C4 C5 0.8(5) . y
C3 C4 C5 C6 -1.2(4) . y
C3 C4 C5 N8 177.4(3) . y
C4 C5 C6 C7 0.9(5) . y
N8 C5 C6 C7 -177.7(3) . y
C3 C2 C7 C6 -0.2(5) . y
C1 C2 C7 C6 173.6(3) . y
C5 C6 C7 C2 -0.3(5) . y
C6 C5 N8 C9 163.9(3) . y
C4 C5 N8 C9 -14.7(5) . y
C5 N8 C9 N10 -7.9(5) . y
C5 N8 C9 N14 174.8(3) . y
N8 C9 N10 C11 -179.4(3) . y
N14 C9 N10 C11 -2.6(4) . y
C9 N10 C11 N20 -179.2(3) . y
C9 N10 C11 N12 1.1(4) . y
N20 C11 N12 C13 -177.9(3) . y
N10 C11 N12 C13 1.8(4) . y
C11 N12 C13 N14 -3.8(5) . y
C11 N12 C13 N30 179.5(3) . y
N30 C13 N14 C9 179.1(3) . y
N12 C13 N14 C9 2.6(4) . y
N10 C9 N14 C13 0.9(4) . y
N8 C9 N14 C13 178.0(3) . y
N12 C11 N20 C21 4.0(5) . y
N10 C11 N20 C21 -175.8(3) . y
C11 N20 C21 C22 103.8(5) . y
N20 C21 C22 C23 -35.4(7) . y
C21 C22 C23 S24 -81.1(6) . y
C22 C23 S24 C25 -82.4(7) . y
N14 C13 N30 C31 2.3(5) . y
N12 C13 N30 C31 179.2(3) . y
C13 N30 C31 C32 -157.8(4) . y
N30 C31 C32 C33 172.3(4) . y
C31 C32 C33 S34 70.0(4) . y
C32 C33 S34 C35 11.2(3) . y
|
1501626.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/16/1501626.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_1501626
loop_
_publ_author_name
'Philippe Brunet'
'Eric Demers'
'Thierry Maris'
'Gary D. Enright'
'James D. Wuest'
_publ_section_title
;
Designing Permeable Molecular Crystals That React with External Agents To
Give Crystalline Products
;
_journal_name_full 'Angewandte Chemie International Edition'
_journal_page_first 5303
_journal_page_last 5306
_journal_paper_doi 10.1002/anie.200352252
_journal_volume 42
_journal_year 2003
_chemical_formula_sum 'C46 H30 N12 S'
_chemical_formula_weight 782.88
_chemical_name_systematic
;
?
;
_space_group_IT_number 88
_symmetry_cell_setting tetragonal
_symmetry_space_group_name_Hall '-I 4ad'
_symmetry_space_group_name_H-M 'I 41/a :2'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 8
_cell_length_a 23.233(16)
_cell_length_b 23.233(16)
_cell_length_c 16.274(17)
_cell_measurement_temperature 173(2)
_cell_volume 8784(13)
_computing_cell_refinement 'Smart (Bruker, 1999)'
_computing_data_collection 'Smart (Bruker, 1999)'
_computing_data_reduction 'Saint (Bruker, 1999)'
_computing_molecular_graphics 'XP (Sheldrick, 1997)'
_computing_publication_material 'Platon (Spek, 1999)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type 'Bruker Smart 1K'
_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 0.1523
_diffrn_reflns_av_sigmaI/netI 0.0875
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_l_max 10
_diffrn_reflns_limit_l_min -10
_diffrn_reflns_number 6088
_diffrn_reflns_theta_full 13.77
_diffrn_reflns_theta_max 13.77
_diffrn_reflns_theta_min 1.53
_exptl_absorpt_coefficient_mu 0.120
_exptl_absorpt_correction_T_max 0.9823
_exptl_absorpt_correction_T_min 0.9650
_exptl_crystal_colour Colourless
_exptl_crystal_density_diffrn 1.184
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 3248
_exptl_crystal_size_max 0.30
_exptl_crystal_size_mid 0.30
_exptl_crystal_size_min 0.15
_refine_diff_density_max 0.342
_refine_diff_density_min -0.372
_refine_diff_density_rms 0.097
_refine_ls_extinction_coef 0.0
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.766
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 182
_refine_ls_number_reflns 688
_refine_ls_number_restraints 192
_refine_ls_restrained_S_all 1.744
_refine_ls_R_factor_all 0.2278
_refine_ls_R_factor_gt 0.1888
_refine_ls_shift/su_max 0.121
_refine_ls_shift/su_mean 0.025
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.4321
_refine_ls_wR_factor_ref 0.4611
_reflns_number_gt 462
_reflns_number_total 688
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file deposit.cif
_cod_data_source_block jiw278
_cod_original_cell_volume 8785(13)
_cod_original_sg_symbol_H-M I41/a
_cod_database_code 1501626
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5000 0.7500 1.1250 0.054(4) Uani 1 4 d SDU . 1
C2 C 0.4626(4) 0.7845(3) 1.0678(4) 0.051(3) Uani 1 1 d GDU A 1
C3 C 0.3998(4) 0.7829(5) 1.0741(5) 0.060(3) Uani 1 1 d GDU A 1
H3 H 0.3815 0.7609 1.1158 0.071 Uiso 1 1 calc R A 1
C4 C 0.3676(4) 0.8143(3) 1.0179(5) 0.066(3) Uani 1 1 d DU A 1
H4 H 0.3269 0.8113 1.0212 0.079 Uiso 1 1 calc R A 1
C5 C 0.3903(2) 0.8498(5) 0.9572(7) 0.051(3) Uani 1 1 d DU A 1
C6 C 0.4500(2) 0.8474(4) 0.9543(7) 0.066(3) Uani 1 1 d DU A 1
H6 H 0.4679 0.8705 0.9134 0.079 Uiso 1 1 calc R A 1
C7 C 0.4869(4) 0.8154(4) 1.0036(5) 0.060(3) Uani 1 1 d DU A 1
H7 H 0.5272 0.8148 0.9937 0.071 Uiso 1 1 calc R A 1
N8 N 0.3491(7) 0.8767(7) 0.9027(10) 0.057(3) Uani 1 1 d U A 1
H8 H 0.3123 0.8701 0.9115 0.068 Uiso 1 1 calc R A 1
C9 C 0.3641(5) 0.9123(4) 0.8371(5) 0.054(4) Uani 1 1 d GDU A 1
N10 N 0.3166(4) 0.9336(5) 0.8043(7) 0.055(2) Uani 1 1 d GDU A 1
C11 C 0.3261(6) 0.9652(5) 0.7381(7) 0.062(4) Uani 1 1 d GDU A 1
N12 N 0.3782(7) 0.9754(5) 0.7043(6) 0.055(2) Uani 1 1 d GDU A 1
C13 C 0.4229(5) 0.9513(6) 0.7418(8) 0.057(4) Uani 1 1 d GDU A 1
N14 N 0.4184(5) 0.9151(5) 0.8079(7) 0.057(3) Uani 1 1 d GDU A 1
N20 N 0.2824(4) 0.9893(9) 0.6975(11) 0.114(3) Uani 1 1 d DU A 1
H20 H 0.2902 1.0006 0.6471 0.137 Uiso 1 1 calc . B 1
N30 N 0.4720(9) 0.9566(7) 0.7113(6) 0.114(3) Uani 1 1 d DU A 1
H30 H 0.5036 0.9456 0.7366 0.137 Uiso 1 1 calc . C 1
C21 C 0.2239(5) 0.9994(11) 0.7246(14) 0.226(15) Uani 1 1 d DU A 1
H21A H 0.2269 1.0083 0.7839 0.271 Uiso 1 1 calc R A 1
H21B H 0.2045 0.9616 0.7210 0.271 Uiso 1 1 calc R A 1
C22 C 0.1794(6) 1.0440(13) 0.6895(19) 0.226(15) Uani 1 1 d DU A 1
H22A H 0.1926 1.0818 0.7102 0.271 Uiso 1 1 calc R A 1
H22B H 0.1865 1.0445 0.6295 0.271 Uiso 1 1 calc R A 1
C23 C 0.1125(5) 1.0454(4) 0.6985(7) 0.40(4) Uani 1 1 d DU A 1
H23A H 0.0972 1.0841 0.6854 0.520 Uiso 1 1 calc R A 1
H23B H 0.1007 1.0349 0.7550 0.520 Uiso 1 1 calc R A 1
S24 S 0.0875(2) 0.9929(4) 0.6254(5) 0.31(2) Uani 0.470(15) 1 d PDU A 1
C251 C 0.0434(5) 0.9614(7) 0.5465(8) 0.168(3) Uani 0.23 1 d PDU A 1
H25A H 0.0694 0.9441 0.5052 0.201 Uiso 0.23 1 calc PR A 1
H25B H 0.0214 0.9294 0.5717 0.201 Uiso 0.23 1 calc PR A 1
C252 C 0.0192(4) 1.0180(10) 0.5872(9) 0.168(3) Uani 0.23 1 d PDU A 1
H25C H -0.0108 1.0051 0.6261 0.201 Uiso 0.23 1 calc PR A 1
H25D H 0.0198 1.0606 0.5890 0.201 Uiso 0.23 1 calc PR A 1
C26 C 0.0000 1.0000 0.5000 0.22(3) Uani 0.94(3) 2 d SPDU . 1
C31 C 0.4720(4) 0.9826(8) 0.6303(5) 0.26(3) Uani 0.470(15) 1 d PDU A 1
H31A H 0.5124 0.9811 0.6110 0.342 Uiso 0.470(15) 1 calc PR A 1
H31B H 0.4629 1.0237 0.6388 0.342 Uiso 0.470(15) 1 calc PR A 1
C32 C 0.4347(6) 0.9630(5) 0.5563(5) 0.26(3) Uani 0.470(15) 1 d PDU A 1
H32 H 0.4062 0.9337 0.5560 0.342 Uiso 0.47 1 calc P A 1
C33 C 0.4506(15) 0.9950(10) 0.4949(12) 0.21(4) Uani 0.470(15) 1 d PDU A 1
H33A H 0.4798 1.0232 0.5023 0.270 Uiso 0.47 1 calc P A 1
H33B H 0.4330 0.9903 0.4426 0.270 Uiso 0.47 1 calc P A 1
C40 C 0.097(4) 0.942(4) 0.609(6) 0.250 Uiso 0.530(15) 1 d P A 2
C41 C 0.059(4) 0.991(4) 0.489(6) 0.250 Uiso 0.530(15) 1 d P A 2
C42 C 0.054(4) 1.016(4) 0.558(6) 0.250 Uiso 0.530(15) 1 d P A 2
C43 C 0.519(4) 0.942(4) 0.585(5) 0.250 Uiso 0.530(15) 1 d P A 2
C44 C 0.516(4) 0.989(4) 0.631(6) 0.250 Uiso 0.530(15) 1 d P A 2
C45 C 0.497(4) 0.940(4) 0.476(5) 0.250 Uiso 0.530(15) 1 d P A 2
C46 C 0.113(4) 0.954(4) 0.521(6) 0.250 Uiso 0.530(15) 1 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
C1 0.054(4) 0.054(4) 0.054(6) 0.000 0.000 0.000
C2 0.051(4) 0.052(4) 0.051(4) 0.000(3) 0.000(3) -0.002(3)
C3 0.059(4) 0.060(4) 0.059(4) -0.002(3) 0.000(3) 0.000(3)
C4 0.066(4) 0.066(4) 0.065(4) 0.001(3) -0.001(3) 0.000(3)
C5 0.051(4) 0.052(4) 0.051(4) 0.000(3) 0.000(3) -0.002(3)
C6 0.066(4) 0.066(4) 0.065(4) 0.001(3) -0.001(3) 0.000(3)
C7 0.059(4) 0.060(4) 0.059(4) -0.002(3) 0.000(3) 0.000(3)
N8 0.056(3) 0.057(4) 0.057(4) 0.001(3) 0.001(3) 0.000(3)
C9 0.054(5) 0.053(5) 0.055(6) 0.001(4) 0.000(4) 0.001(4)
N10 0.054(3) 0.056(3) 0.054(3) 0.000(2) -0.001(2) 0.000(2)
C11 0.062(5) 0.061(5) 0.062(6) 0.001(4) 0.000(4) -0.002(4)
N12 0.054(3) 0.056(3) 0.054(3) 0.000(2) -0.001(2) 0.000(2)
C13 0.057(5) 0.057(5) 0.057(6) 0.002(4) 0.002(4) 0.001(4)
N14 0.056(3) 0.057(4) 0.057(4) 0.001(3) 0.001(3) 0.000(3)
N20 0.114(4) 0.115(4) 0.114(4) 0.002(3) 0.000(3) 0.000(3)
N30 0.114(4) 0.115(4) 0.114(4) 0.002(3) 0.000(3) 0.000(3)
C21 0.22(3) 0.33(4) 0.13(2) 0.05(2) -0.02(2) 0.02(3)
C22 0.22(3) 0.33(4) 0.13(2) 0.05(2) -0.02(2) 0.02(3)
C23 0.33(6) 0.39(6) 0.49(7) 0.00(5) 0.02(5) 0.08(5)
S24 0.29(4) 0.29(4) 0.35(4) -0.07(3) -0.07(3) -0.03(3)
C251 0.168(4) 0.168(4) 0.168(4) 0.000(3) 0.000(3) 0.000(3)
C252 0.168(4) 0.168(4) 0.168(4) 0.000(3) 0.000(3) 0.000(3)
C26 0.11(4) 0.23(5) 0.31(6) 0.06(5) -0.03(4) 0.06(4)
C31 0.27(5) 0.27(5) 0.24(5) 0.12(4) -0.01(4) 0.10(4)
C32 0.27(5) 0.27(5) 0.24(5) 0.12(4) -0.01(4) 0.10(4)
C33 0.21(6) 0.17(6) 0.24(6) 0.04(6) 0.03(6) -0.01(5)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C2 112.5(3) 15_567 6_564 y
C2 C1 C2 112.5(3) 15_567 . y
C2 C1 C2 103.6(6) 6_564 . y
C2 C1 C2 103.6(6) 15_567 12_768 y
C2 C1 C2 112.5(3) 6_564 12_768 y
C2 C1 C2 112.5(3) . 12_768 y
C7 C2 C3 118.1(7) . . y
C7 C2 C1 120.4(7) . . y
C3 C2 C1 121.2(4) . . y
C4 C3 C2 118.6(8) . . y
C3 C4 C5 125.1(9) . . y
C4 C5 C6 112.3(9) . . y
C4 C5 N8 116.2(8) . . y
C6 C5 N8 131.0(10) . . y
C7 C6 C5 128.2(9) . . y
C2 C7 C6 117.4(9) . . y
C9 N8 C5 124.1(13) . . y
N10 C9 N14 128.2 . . y
N10 C9 N8 108.9(11) . . y
N14 C9 N8 122.2(10) . . y
C9 N10 C11 113.5 . . y
N10 C11 N20 120.6(12) . . y
N10 C11 N12 125.4 . . y
N20 C11 N12 114.0(12) . . y
C13 N12 C11 116.1 . . y
N30 C13 N12 119.4(12) . . y
N30 C13 N14 116.2(12) . . y
N12 C13 N14 124.0 . . y
C9 N14 C13 112.3 . . y
C11 N20 C21 129.2(18) . . y
C13 N30 C31 113.6(15) . . y
N20 C21 C22 127.9(18) . . y
C23 C22 C21 129.4(18) . . y
C22 C23 S24 104.2(14) . . y
C23 S24 C251 158.8(8) . . y
C23 S24 C252 107.1(9) . . y
C251 S24 C252 52.0(9) . . y
C26 C251 S24 118.9(9) . . y
C26 C252 S24 119.0(10) . . y
C252 C26 C252 180.000(4) . 9_576 y
C252 C26 C251 118.7(8) . 9_576 y
C252 C26 C251 61.3(8) 9_576 9_576 y
C252 C26 C251 61.3(8) . . y
C252 C26 C251 118.7(8) 9_576 . y
C251 C26 C251 180.000(5) 9_576 . y
N30 C31 C32 125.8(12) . . y
C33 C32 C31 105.7(16) . . y
C42 C41 C46 91(8) . . y
C44 C43 C45 123(8) . . y
C40 C46 C41 102(8) . . y
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.505(8) 15_567 y
C1 C2 1.505(8) 6_564 y
C1 C2 1.505(7) . y
C1 C2 1.505(8) 12_768 y
C2 C7 1.389(5) . y
C2 C3 1.4625 . y
C3 C4 1.389(5) . y
C4 C5 1.390(5) . y
C5 C6 1.390(5) . y
C5 N8 1.447(17) . y
C6 C7 1.389(5) . y
N8 C9 1.394(17) . y
C9 N10 1.3210 . y
C9 N14 1.3512 . y
N10 C11 1.3220 . y
C11 N20 1.335(18) . y
C11 N12 1.3497 . y
N12 C13 1.3285 . y
C13 N30 1.25(2) . y
C13 N14 1.3694 . y
N20 C21 1.448(10) . y
N30 C31 1.450(10) . y
C21 C22 1.571(19) . y
C22 C23 1.561(16) . y
C23 S24 1.800(6) . y
S24 C251 1.800(6) . y
S24 C252 1.800(6) . y
C251 C26 1.547(14) . y
C252 C26 1.545(16) . y
C26 C252 1.545(16) 9_576 y
C26 C251 1.547(14) 9_576 y
C31 C32 1.550(6) . y
C32 C33 1.300(6) . y
C40 C46 1.50(12) . y
C41 C42 1.27(12) . y
C41 C46 1.61(12) . y
C43 C44 1.32(11) . y
C43 C45 1.84(11) . y
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N8 H8 N12 0.88 2.14 3.00(3) 165.6 8_354
N20 H20 N10 0.88 2.24 3.05(4) 152.8 7_554
|
1501627.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/16/1501627.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_1501627
loop_
_publ_author_name
'Yang, Sihai'
'Callear, Samantha K.'
'Ramirez-Cuesta, Anibal J.'
'David, William I. F.'
'Sun, Junliang'
'Blake, Alexander J.'
'Champness, Neil R.'
'Schr\"oder, Martin'
_publ_section_title
;
Pore with gate: modulating hydrogen storage in metal-organic framework
materials via cation exchange
;
_journal_name_full 'Faraday Discussions'
_journal_page_first 19
_journal_paper_doi 10.1039/c1fd00006c
_journal_volume 151
_journal_year 2011
_chemical_formula_moiety
'In (C22 O8 H10) (C2 H8 N), 2(C3 H7 N O), 4(H2 O)'
_chemical_formula_sum 'C30 H40 In N3 O14'
_chemical_formula_weight 781.47
_chemical_name_systematic
;
?
;
_space_group_IT_number 131
_symmetry_cell_setting tetragonal
_symmetry_space_group_name_Hall '-P 4c 2'
_symmetry_space_group_name_H-M 'P 42/m m c'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method 'enCIFer editing of SHELXL97 CIF output'
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 2
_cell_length_a 9.9532(3)
_cell_length_b 9.9532(3)
_cell_length_c 26.7005(11)
_cell_measurement_reflns_used 700
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 33.22
_cell_measurement_theta_min 3.68
_cell_volume 2645.12(16)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
(compiled Jan 12 2007,17:49:11)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
(compiled Jan 12 2007,17:49:11)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
(compiled Jan 12 2007,17:49:11)
;
_computing_publication_material
'enCIFer (Allen et al., 2004); PLATON (Spek, 2009)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean 16.546
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type 'CrysAlis CCD area detector'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'Enhance (Mo) X-ray Source'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0899
_diffrn_reflns_av_sigmaI/netI 0.0351
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 29
_diffrn_reflns_limit_l_min -29
_diffrn_reflns_number 24345
_diffrn_reflns_theta_full 23.25
_diffrn_reflns_theta_max 23.25
_diffrn_reflns_theta_min 4.09
_exptl_absorpt_coefficient_mu 0.493
_exptl_absorpt_correction_T_max 0.959
_exptl_absorpt_correction_T_min 0.907
_exptl_absorpt_correction_type analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
(compiled Jan 12 2007,17:49:11)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour Colorless
_exptl_crystal_density_diffrn 0.981
_exptl_crystal_description Octahedron
_exptl_crystal_F_000 804
_exptl_crystal_size_max 0.14
_exptl_crystal_size_mid 0.14
_exptl_crystal_size_min 0.12
_platon_squeeze_details
;
Approximately 73% of the unit cell volume comprises a large region of
disordered solvent and counter-cations which could not be modelled as
discrete atomic sites. We employed PLATON SQUEEZE to calculate the
contribution to the diffraction from the solvent/cation region and
thereby produced a set of solvent-free diffraction intensities. SQUEEZE
estimated a total count of 570 electrons per unit cell, which were
assigned to be 2.0 DMF and 4.0 water molecules per indium. The final
formula was calculated from the TGA combined with elemental analysis data.
;
_refine_diff_density_max 0.35
_refine_diff_density_min -0.49
_refine_diff_density_rms 0.09
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.02
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 49
_refine_ls_number_reflns 1073
_refine_ls_number_restraints 26
_refine_ls_restrained_S_all 1.01
_refine_ls_R_factor_all 0.0805
_refine_ls_R_factor_gt 0.0621
_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^)+(0.115P)^2^+1.00P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.167
_refine_ls_wR_factor_ref 0.174
_reflns_number_gt 774
_reflns_number_total 1073
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file c1fd00006c.txt
_cod_data_source_block NOTT-210
_cod_original_sg_symbol_H-M 'P 42/mmc'
_cod_database_code 1501627
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x, z+1/2'
'-x, -y, z'
'y, -x, z+1/2'
'x, -y, -z'
'y, x, -z+1/2'
'-x, y, -z'
'-y, -x, -z+1/2'
'-x, -y, -z'
'y, -x, -z-1/2'
'x, y, -z'
'-y, x, -z-1/2'
'-x, y, z'
'-y, -x, z-1/2'
'x, -y, z'
'y, x, 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
In1 In 0.5000 0.5000 0.2500 0.0530(5) Uani 1 8 d SU
O1 O 0.3557(5) 0.5000 0.18755(18) 0.0710(14) Uani 1 2 d SU
O2 O 0.2569(6) 0.5000 0.2605(2) 0.099(2) Uani 1 2 d SU
C1 C 0.2529(9) 0.5000 0.2134(4) 0.087(3) Uani 1 2 d SU
C2 C 0.1205(7) 0.5000 0.1875(3) 0.080(2) Uani 1 2 d SU
C3 C 0.1225(8) 0.5000 0.1363(3) 0.093(3) Uani 1 2 d SU
H3 H 0.2048 0.5000 0.1198 0.112 Uiso 1 2 calc SR
C4 C 0.0000 0.5000 0.2142(4) 0.080(3) Uani 1 4 d SU
H4 H 0.0000 0.5000 0.2491 0.096 Uiso 1 4 calc SR
C5 C 0.0000 0.5000 0.1070(4) 0.098(4) Uani 1 4 d SU
C6 C 0.0000 0.5000 0.0527(5) 0.116(6) Uani 1 4 d SU
C7 C 0.1109(15) 0.460(2) 0.0272(4) 0.163(9) Uiso 0.50 1 d PU
H7A H 0.1898 0.4361 0.0459 0.196 Uiso 0.50 1 d PR
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
In1 0.0572(5) 0.0572(5) 0.0448(7) 0.000 0.000 0.000
O1 0.043(3) 0.092(4) 0.079(4) 0.000 0.001(3) 0.000
O2 0.061(4) 0.157(7) 0.079(5) 0.000 -0.009(3) 0.000
C1 0.059(5) 0.117(7) 0.084(6) 0.000 -0.015(5) 0.000
C2 0.055(5) 0.111(7) 0.073(6) 0.000 -0.012(4) 0.000
C3 0.053(5) 0.145(9) 0.080(6) 0.000 -0.004(4) 0.000
C4 0.044(6) 0.125(11) 0.071(8) 0.000 0.000 0.000
C5 0.066(8) 0.158(14) 0.068(8) 0.000 0.000 0.000
C6 0.051(8) 0.213(18) 0.083(9) 0.000 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
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'
In In -0.7276 1.3100 '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'
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
O1 In1 O1 125.03(16) 10_566 .
O1 In1 O1 81.5(3) 3_665 .
O1 In1 O2 84.98(9) 10_566 .
O1 In1 O2 137.4(2) 3_665 .
O1 In1 O2 55.88(17) . .
O2 In1 O2 166.7(3) . 3_665
O2 In1 O2 90.76(3) . 10_566
C1 O1 In1 96.7(5) . .
C1 O2 In1 85.2(5) . .
O1 C1 O2 122.2(8) . .
O1 C1 C2 118.3(9) . .
O2 C1 C2 119.5(8) . .
C3 C2 C4 121.6(8) . .
C3 C2 C1 116.8(8) . .
C4 C2 C1 121.6(8) . .
C2 C3 C5 121.8(8) . .
C2 C3 H3 119.1 . .
C5 C3 H3 119.1 . .
C2 C4 C2 118.5(10) 3_565 .
C2 C4 H4 120.7 3_565 .
C2 C4 H4 120.7 . .
C3 C5 C6 122.7(5) 3_565 .
C3 C5 C6 122.7(5) . .
C7 C6 C7 119.8(16) 13 15_565
C7 C6 C5 120.1(8) . .
C7 C6 C5 120.1(8) 13 .
C7 C6 C5 120.1(8) 3_565 .
C7 C6 C5 120.1(8) 15_565 .
C6 C7 C7 120.1(8) . 11
C7 C7 H7A 121.4 11 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
In1 O1 2.201(5) .
In1 O2 2.436(6) .
O1 C1 1.235(10) .
O2 C1 1.258(11) .
C1 C2 1.488(11) .
C2 C3 1.368(10) .
C2 C4 1.395(9) .
C3 C5 1.449(10) .
C3 H3 0.9300 .
C4 H4 0.9300 .
C5 C6 1.450(17) .
C6 C7 1.358(15) .
C7 C7 1.45(2) 11
C7 H7A 0.9601 .
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 -0.014 -0.009 -0.005 1914 570
|
1501628.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/16/1501628.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_1501628
loop_
_publ_author_name
'Yang, Sihai'
'Callear, Samantha K.'
'Ramirez-Cuesta, Anibal J.'
'David, William I. F.'
'Sun, Junliang'
'Blake, Alexander J.'
'Champness, Neil R.'
'Schr\"oder, Martin'
_publ_section_title
;
Pore with gate: modulating hydrogen storage in metal-organic framework
materials via cation exchange
;
_journal_name_full 'Faraday Discussions'
_journal_page_first 19
_journal_paper_doi 10.1039/c1fd00006c
_journal_volume 151
_journal_year 2011
_chemical_formula_moiety
'In (C24 O8 H12) (C2 H8 N), 2(C3 H7 N O), 2(H2 O)'
_chemical_formula_sum 'C32 H38 In N3 O12'
_chemical_formula_weight 771.47
_chemical_name_systematic
;
?
;
_space_group_IT_number 131
_symmetry_cell_setting tetragonal
_symmetry_space_group_name_Hall '-P 4c 2'
_symmetry_space_group_name_H-M 'P 42/m m c'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method 'enCIFer editing of SHELXL97 CIF output'
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 2
_cell_length_a 9.9617(4)
_cell_length_b 9.9617(4)
_cell_length_c 26.747(2)
_cell_measurement_reflns_used 790
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 33.22
_cell_measurement_theta_min 3.68
_cell_volume 2654.3(2)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
(compiled Jan 12 2007,17:49:11)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
(compiled Jan 12 2007,17:49:11)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
(compiled Jan 12 2007,17:49:11)
;
_computing_publication_material
'enCIFer (Allen et al., 2004); PLATON (Spek, 2009)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean 16.5467
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type 'CrysAlis CCD area detector'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'Enhance (Mo) X-ray Source'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.130
_diffrn_reflns_av_sigmaI/netI 0.169
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 8
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_l_max 29
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_number 8753
_diffrn_reflns_theta_full 23.24
_diffrn_reflns_theta_max 23.24
_diffrn_reflns_theta_min 4.16
_exptl_absorpt_coefficient_mu 0.488
_exptl_absorpt_correction_T_max 0.91
_exptl_absorpt_correction_T_min 0.90
_exptl_absorpt_correction_type analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
(compiled Jan 12 2007,17:49:11)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour Colorless
_exptl_crystal_density_diffrn 0.965
_exptl_crystal_description Octahedron
_exptl_crystal_F_000 792
_exptl_crystal_size_max 0.14
_exptl_crystal_size_mid 0.14
_exptl_crystal_size_min 0.12
_platon_squeeze_details
;
Approximately 65% of the unit cell volume comprises a large region of
disordered solvent and counter-cations which could not be modelled as
discrete atomic sites. We employed PLATON SQUEEZE to calculate the
contribution to the diffraction from the solvent/cation region and
thereby produced a set of solvent-free diffraction intensities. SQUEEZE
estimated a total count of 28 electrons per unit cell, which were
assigned to be 2.0 DMF and 2.0 water molecules per indium. The final
formula was calculated from the TGA combined with elemental analysis data.
;
_refine_diff_density_max 1.12
_refine_diff_density_min -0.34
_refine_diff_density_rms 0.08
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.02
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 51
_refine_ls_number_reflns 1084
_refine_ls_number_restraints 21
_refine_ls_restrained_S_all 1.03
_refine_ls_R_factor_all 0.178
_refine_ls_R_factor_gt 0.0818
_refine_ls_shift/su_max 0.009
_refine_ls_shift/su_mean 0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.060P)^2^+6.000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.173
_refine_ls_wR_factor_ref 0.189
_reflns_number_gt 503
_reflns_number_total 1084
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file c1fd00006c.txt
_cod_data_source_block NOTT-211
_cod_original_cell_volume 2654.3(3)
_cod_original_sg_symbol_H-M 'P 42/mmc'
_cod_database_code 1501628
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z+1/2'
'y, -x, z+1/2'
'-x, y, -z'
'x, -y, -z'
'y, x, -z+1/2'
'-y, -x, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z-1/2'
'-y, x, -z-1/2'
'x, -y, z'
'-x, y, z'
'-y, -x, z-1/2'
'y, x, 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
In1 In 0.5000 0.5000 0.2500 0.0684(8) Uani 1 8 d SU
O1 O 0.2608(11) 0.5000 0.2408(3) 0.121(4) Uani 1 2 d SU
O2 O 0.5000 0.3562(9) 0.1878(3) 0.088(3) Uani 1 2 d SU
C1 C 0.5000 0.2497(14) 0.2137(5) 0.083(4) Uani 1 2 d SU
C2 C 0.5000 0.1196(13) 0.1871(5) 0.092(5) Uani 1 2 d SU
C3 C 0.5000 0.0000 0.2122(7) 0.087(7) Uani 1 4 d SU
H3A H 0.5000 0.0000 0.2470 0.105 Uiso 1 4 calc SR
C4 C 0.5000 0.1194(13) 0.1337(5) 0.107(6) Uani 1 2 d SU
H4A H 0.5000 0.2003 0.1163 0.128 Uiso 1 2 calc SR
C5 C 0.5000 0.0000 0.1078(7) 0.126(10) Uani 1 4 d SDU
C6 C 0.5000 0.0000 0.0512(7) 0.131(9) Uiso 1 4 d SDU
C7 C 0.389(2) 0.058(2) 0.0298(6) 0.121(9) Uiso 0.50 1 d PDU
C8 C 0.258(3) 0.117(5) 0.0477(17) 0.148(18) Uiso 0.25 1 d PDU
H8A H 0.2083 0.1500 0.0196 0.177 Uiso 0.25 1 calc PR
H8B H 0.2763 0.1896 0.0703 0.177 Uiso 0.25 1 calc PR
H8C H 0.2073 0.0491 0.0645 0.177 Uiso 0.25 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
In1 0.0824(11) 0.0824(11) 0.0404(9) 0.000 0.000 0.000
O1 0.127(8) 0.205(11) 0.031(6) 0.000 0.012(5) 0.000
O2 0.141(9) 0.044(6) 0.078(6) -0.007(5) 0.000 0.000
C1 0.139(13) 0.035(7) 0.075(9) 0.007(7) 0.000 0.000
C2 0.153(14) 0.024(7) 0.098(9) 0.005(7) 0.000 0.000
C3 0.15(2) 0.027(10) 0.086(12) 0.000 0.000 0.000
C4 0.219(18) 0.033(9) 0.069(8) -0.006(7) 0.000 0.000
C5 0.23(3) 0.092(17) 0.057(12) 0.000 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
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'
In In -0.7276 1.3100 '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
O2 In1 O2 125.0(3) 11_566 .
O2 In1 O2 81.5(5) 2_665 .
O2 In1 O1 55.1(3) 11_566 .
O2 In1 O1 85.53(14) . .
O2 In1 O1 136.6(3) . 11_566
O1 In1 O1 90.61(4) . 11_566
O2 In1 O1 85.54(14) . 2_665
O1 In1 O1 168.2(4) . 2_665
C1 O1 In1 89.3(9) 11_566 .
C1 O2 In1 97.7(8) . .
O1 C1 O2 117.8(14) 12_656 .
O1 C1 C2 124.0(14) 12_656 .
O2 C1 C2 118.2(12) . .
C3 C2 C4 119.3(14) . .
C3 C2 C1 121.8(13) . .
C4 C2 C1 118.9(12) . .
C2 C3 C2 121.1(18) . 2_655
C5 C4 C2 120.3(13) . .
C4 C5 C4 119.5(17) 2_655 .
C4 C5 C6 120.2(9) 2_655 .
C4 C5 C6 120.2(9) . .
C7 C6 C5 114.6(11) 13 .
C7 C6 C5 114.6(11) 14_655 .
C7 C6 C5 114.6(11) 2_655 .
C7 C6 C5 114.6(11) . .
C8 C7 C7 119(2) . 6
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
In1 O2 2.195(8) .
In1 O1 2.395(11) .
O1 C1 1.223(14) 11_566
O2 C1 1.266(13) .
C1 C2 1.477(16) .
C2 C3 1.368(15) .
C2 C4 1.429(17) .
C3 C2 1.368(15) 2_655
C4 C5 1.377(14) .
C5 C4 1.376(14) 2_655
C5 C6 1.513(10) .
C6 C7 1.38(2) .
C7 C8 1.503(10) .
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 -0.027 -0.017 -0.008 1660 28
|
1501629.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/16/1501629.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_1501629
loop_
_publ_author_name
'Yang, Sihai'
'Callear, Samantha K.'
'Ramirez-Cuesta, Anibal J.'
'David, William I. F.'
'Sun, Junliang'
'Blake, Alexander J.'
'Champness, Neil R.'
'Schr\"oder, Martin'
_publ_section_title
;
Pore with gate: modulating hydrogen storage in metal-organic framework
materials via cation exchange
;
_journal_name_full 'Faraday Discussions'
_journal_page_first 19
_journal_paper_doi 10.1039/c1fd00006c
_journal_volume 151
_journal_year 2011
_chemical_formula_moiety
'In (C22 O8 H6 F4) (C2 H8 N), 2(C3 H7 N O), 4.0(H2 O)'
_chemical_formula_sum 'C30 H36 F4 In N3 O14'
_chemical_formula_weight 853.44
_chemical_name_systematic
;
?
;
_space_group_IT_number 142
_symmetry_cell_setting tetragonal
_symmetry_space_group_name_Hall '-I 4bd 2c'
_symmetry_space_group_name_H-M 'I 41/a c d :2'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method 'enCIFer editing of SHELXL97 CIF output'
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 16
_cell_length_a 19.807(5)
_cell_length_b 19.807(5)
_cell_length_c 53.454(9)
_cell_measurement_reflns_used 937
_cell_measurement_temperature 120(2)
_cell_measurement_theta_max 24.84
_cell_measurement_theta_min 2.50
_cell_volume 20971(8)
_computing_cell_refinement 'Bruker SAINT'
_computing_data_collection 'Bruker APEX2'
_computing_data_reduction 'Bruker SAINT'
_computing_publication_material
'enCIFer (Allen et al., 2004); PLATON (Spek, 2009)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature 120(2)
_diffrn_detector_area_resol_mean 66.06
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type 'Bruker SMART APEXII CCD diffractometer'
_diffrn_measurement_method 'fine-slice \w scans'
_diffrn_radiation_monochromator 'silicon 111'
_diffrn_radiation_source 'Daresbury SRS Station 9.8'
_diffrn_radiation_type synchrotron
_diffrn_radiation_wavelength 0.6943
_diffrn_reflns_av_R_equivalents 0.054
_diffrn_reflns_av_sigmaI/netI 0.022
_diffrn_reflns_limit_h_max 21
_diffrn_reflns_limit_h_min -22
_diffrn_reflns_limit_k_max 21
_diffrn_reflns_limit_k_min -22
_diffrn_reflns_limit_l_max 59
_diffrn_reflns_limit_l_min -59
_diffrn_reflns_number 61209
_diffrn_reflns_theta_full 22.69
_diffrn_reflns_theta_max 22.69
_diffrn_reflns_theta_min 2.28
_exptl_absorpt_coefficient_mu 0.513
_exptl_absorpt_correction_T_max 1.00
_exptl_absorpt_correction_T_min 0.86
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Bruker SADABS'
_exptl_crystal_colour COLOURLESS
_exptl_crystal_density_diffrn 1.081
_exptl_crystal_description BLOCK
_exptl_crystal_F_000 6944
_exptl_crystal_size_max 0.14
_exptl_crystal_size_mid 0.12
_exptl_crystal_size_min 0.12
_platon_squeeze_details
;
Approximately 70% of the unit cell volume comprises a large region of
disordered solvent and counter-cations which could not be modelled as
discrete atomic sites. We employed PLATON SQUEEZE to calculate the
contribution to the diffraction from the solvent/cation region and
thereby produced a set of solvent-free diffraction intensities. SQUEEZE
estimated a total count of 1559 electrons per unit cell, which were
assigned to be 2.0 DMF and 4.0 water molecules per indium. The final
formula was calculated from the TGA combined with elemental analysis data.
;
_refine_diff_density_max 0.30
_refine_diff_density_min -0.77
_refine_diff_density_rms 0.06
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.05
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 159
_refine_ls_number_reflns 3732
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.05
_refine_ls_R_factor_all 0.0685
_refine_ls_R_factor_gt 0.0548
_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^)+(0.093P)^2^+40.85P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.168
_refine_ls_wR_factor_ref 0.177
_reflns_number_gt 2959
_reflns_number_total 3732
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file c1fd00006c.txt
_cod_data_source_block NOTT-212
_cod_original_sg_symbol_H-M 'I 41/acd'
_cod_database_code 1501629
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+1/4, x+3/4, z+1/4'
'y+1/4, -x+1/4, z+3/4'
'-x+1/2, y, -z'
'x, -y, -z+1/2'
'y+1/4, x+3/4, -z+3/4'
'-y+1/4, -x+1/4, -z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+3/4, x+5/4, z+3/4'
'y+3/4, -x+3/4, z+5/4'
'-x+1, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1'
'y+3/4, x+5/4, -z+5/4'
'-y+3/4, -x+3/4, -z+3/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-1/4, -x-3/4, -z-1/4'
'-y-1/4, x-1/4, -z-3/4'
'x-1/2, -y, z'
'-x, y, z-1/2'
'-y-1/4, -x-3/4, z-3/4'
'y-1/4, x-1/4, z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y+1/4, -x-1/4, -z+1/4'
'-y+1/4, x+1/4, -z-1/4'
'x, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z'
'-y+1/4, -x-1/4, z-1/4'
'y+1/4, x+1/4, z+1/4'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
In1 In 0.756915(17) 0.006915(17) 0.1250 0.0579(3) Uani 1 2 d S
O1 O 0.3827(2) 0.0032(2) 0.13142(8) 0.1064(14) Uani 1 1 d .
O2 O 0.33033(16) -0.01273(18) 0.09579(7) 0.0843(10) Uani 1 1 d .
O3 O 0.64166(18) 0.00522(16) 0.12862(6) 0.0737(9) Uani 1 1 d .
O4 O 0.68837(15) 0.00914(15) 0.09170(5) 0.0674(8) Uani 1 1 d .
F1 F 0.57550(17) 0.0949(2) 0.02376(5) 0.1129(12) Uani 1 1 d .
F2 F 0.56952(16) 0.0949(2) -0.02570(5) 0.1124(12) Uani 1 1 d .
C1 C 0.3838(3) -0.0043(3) 0.10824(12) 0.0842(15) Uani 1 1 d .
C2 C 0.6366(3) 0.0061(2) 0.10514(9) 0.0707(13) Uani 1 1 d .
C3 C 0.5691(2) 0.0045(3) 0.09287(9) 0.0728(13) Uani 1 1 d .
C4 C 0.5095(2) 0.0032(2) 0.10657(10) 0.0788(15) Uani 1 1 d .
H4 H 0.5108 0.0055 0.1243 0.095 Uiso 1 1 calc R
C5 C 0.4478(3) -0.0016(3) 0.09425(9) 0.0830(15) Uani 1 1 d .
C6 C 0.4464(3) -0.0043(3) 0.06853(10) 0.0894(17) Uani 1 1 d .
H6 H 0.4041 -0.0079 0.0602 0.107 Uiso 1 1 calc R
C7 C 0.5054(2) -0.0017(3) 0.05436(11) 0.093(2) Uani 1 1 d .
C8 C 0.5672(2) 0.0021(3) 0.06683(9) 0.0812(15) Uani 1 1 d .
H8 H 0.6080 0.0030 0.0575 0.097 Uiso 1 1 calc R
C9 C 0.5023(2) -0.0013(3) 0.02679(10) 0.086(2) Uani 1 1 d .
C10 C 0.5377(3) 0.0472(4) 0.01253(10) 0.1002(19) Uani 1 1 d .
C11 C 0.5356(3) 0.0461(4) -0.01352(10) 0.0995(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
In1 0.0691(3) 0.0691(3) 0.0355(3) 0.00185(12) -0.00185(12) -0.00173(17)
O1 0.092(3) 0.152(4) 0.076(3) 0.010(2) 0.021(2) 0.002(2)
O2 0.052(2) 0.114(3) 0.087(2) 0.0029(19) 0.0093(18) -0.0020(17)
O3 0.067(2) 0.109(3) 0.0449(18) 0.0055(15) 0.0016(14) -0.0020(15)
O4 0.0580(18) 0.092(2) 0.0525(17) 0.0062(14) -0.0019(15) 0.0112(14)
F1 0.101(2) 0.171(3) 0.0669(19) 0.007(2) -0.0089(17) -0.023(2)
F2 0.094(2) 0.174(3) 0.0693(19) 0.014(2) -0.0018(16) -0.029(2)
C1 0.070(4) 0.107(4) 0.075(4) 0.005(3) 0.019(3) 0.005(3)
C2 0.081(3) 0.081(3) 0.050(3) 0.002(2) -0.003(2) 0.003(2)
C3 0.059(3) 0.104(4) 0.056(3) 0.010(2) -0.004(2) 0.009(2)
C4 0.069(3) 0.111(4) 0.057(3) 0.000(3) 0.006(2) 0.002(2)
C5 0.058(3) 0.128(5) 0.063(3) 0.014(3) 0.002(2) 0.002(2)
C6 0.057(3) 0.142(5) 0.070(3) 0.019(3) -0.004(2) -0.006(3)
C7 0.061(3) 0.162(6) 0.056(3) 0.000(3) -0.002(2) 0.004(3)
C8 0.057(3) 0.132(5) 0.055(3) 0.005(3) -0.002(2) 0.012(3)
C9 0.034(2) 0.170(6) 0.055(3) 0.007(3) -0.0033(19) 0.002(3)
C10 0.068(3) 0.170(6) 0.063(3) 0.009(4) -0.012(3) -0.014(4)
C11 0.070(4) 0.166(6) 0.063(3) 0.016(4) -0.006(3) -0.002(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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
O2 In1 O2 117.42(19) 20_656 21_655
O2 In1 O4 80.26(13) 20_656 15_534
O2 In1 O4 126.88(12) 20_656 .
O4 In1 O4 130.97(16) 15_534 .
O2 In1 O3 137.79(13) 20_656 15_534
O2 In1 O3 90.11(12) 20_656 .
O4 In1 O3 86.76(11) 15_534 .
O4 In1 O3 57.54(11) . .
O3 In1 O3 88.74(16) 15_534 .
O2 In1 O1 84.34(13) 20_656 21_655
O4 In1 O1 79.89(13) 15_534 21_655
O3 In1 O1 166.22(14) . 21_655
O2 In1 O1 55.35(13) 20_656 20_656
O4 In1 O1 135.11(12) 15_534 20_656
O3 In1 O1 86.96(12) . 20_656
O1 In1 O1 100.09(19) 21_655 20_656
C1 O1 In1 82.7(3) . 27_565
C1 O2 In1 100.3(3) . 27_565
C2 O3 In1 89.7(3) . .
C2 O4 In1 92.3(3) . .
O1 C1 O2 121.7(5) . .
O1 C1 C5 121.0(6) . .
O2 C1 C5 117.3(5) . .
O4 C2 O3 120.4(5) . .
O4 C2 C3 118.9(4) . .
O3 C2 C3 120.7(5) . .
C4 C3 C8 120.1(4) . .
C4 C3 C2 122.1(4) . .
C8 C3 C2 117.8(4) . .
C5 C4 C3 119.9(5) . .
C6 C5 C4 119.6(5) . .
C6 C5 C1 119.2(5) . .
C4 C5 C1 121.2(5) . .
C5 C6 C7 121.6(5) . .
C6 C7 C8 118.6(5) . .
C6 C7 C9 120.6(4) . .
C8 C7 C9 120.8(4) . .
C3 C8 C7 120.2(5) . .
C11 C9 C10 115.8(5) 17_655 .
C11 C9 C7 122.6(5) 17_655 .
C10 C9 C7 121.5(5) . .
F1 C10 C11 118.2(5) . .
F1 C10 C9 120.8(5) . .
C11 C10 C9 120.9(6) . .
F2 C11 C9 119.5(5) . 17_655
F2 C11 C10 117.2(6) . .
C9 C11 C10 123.2(6) 17_655 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
In1 O2 2.137(3) 20_656
In1 O4 2.239(3) .
In1 O3 2.291(4) .
In1 O1 2.523(5) 20_656
O1 C1 1.248(7) .
O2 C1 1.262(7) .
O3 C2 1.259(5) .
O4 C2 1.254(6) .
F1 C10 1.347(7) .
F2 C11 1.346(7) .
C1 C5 1.474(7) .
C2 C3 1.488(7) .
C3 C4 1.391(7) .
C3 C8 1.393(7) .
C4 C5 1.390(7) .
C5 C6 1.376(7) .
C6 C7 1.394(7) .
C7 C8 1.396(7) .
C7 C9 1.475(8) .
C9 C11 1.361(8) 17_655
C9 C10 1.412(8) .
C10 C11 1.393(7) .
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 -0.023 0.217 -0.002 14633 1559
|
1501630.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/16/1501630.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_1501630
loop_
_publ_author_name
'Yang, Sihai'
'Callear, Samantha K.'
'Ramirez-Cuesta, Anibal J.'
'David, William I. F.'
'Sun, Junliang'
'Blake, Alexander J.'
'Champness, Neil R.'
'Schr\"oder, Martin'
_publ_section_title
;
Pore with gate: modulating hydrogen storage in metal-organic framework
materials via cation exchange
;
_journal_name_full 'Faraday Discussions'
_journal_page_first 19
_journal_paper_doi 10.1039/c1fd00006c
_journal_volume 151
_journal_year 2011
_chemical_formula_moiety
'In (C26 O8 H10) (C2 H8 N), 2(C3 H7 N O), 2(H2 O)'
_chemical_formula_sum 'C34 H36 In N3 O12'
_chemical_formula_weight 793.48
_chemical_name_systematic
;
?
;
_space_group_IT_number 131
_symmetry_cell_setting tetragonal
_symmetry_space_group_name_Hall '-P 4c 2'
_symmetry_space_group_name_H-M 'P 42/m m c'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method 'enCIFer editing of SHELXL97 CIF output'
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 2
_cell_length_a 9.9617(4)
_cell_length_b 9.9617(4)
_cell_length_c 26.747(2)
_cell_measurement_reflns_used 760
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 33.22
_cell_measurement_theta_min 3.68
_cell_volume 2654.3(2)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
(compiled Jan 12 2007,17:49:11)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
(compiled Jan 12 2007,17:49:11)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
(compiled Jan 12 2007,17:49:11)
;
_computing_publication_material
'enCIFer (Allen et al., 2004); PLATON (Spek, 2003)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean 16.5467
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type 'CrysAlis CCD area detector'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'Enhance (Mo) X-ray Source'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.093
_diffrn_reflns_av_sigmaI/netI 0.056
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 29
_diffrn_reflns_limit_l_min -29
_diffrn_reflns_number 24009
_diffrn_reflns_theta_full 23.24
_diffrn_reflns_theta_max 23.24
_diffrn_reflns_theta_min 4.16
_exptl_absorpt_coefficient_mu 0.489
_exptl_absorpt_correction_T_max 0.92
_exptl_absorpt_correction_T_min 0.90
_exptl_absorpt_correction_type analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
(compiled Jan 12 2007,17:49:11)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour Colorless
_exptl_crystal_density_diffrn 0.993
_exptl_crystal_description Octahedron
_exptl_crystal_F_000 812
_exptl_crystal_size_max 0.14
_exptl_crystal_size_mid 0.14
_exptl_crystal_size_min 0.12
_platon_squeeze_details
;
Approximately 65% of the unit cell volume comprises a large region of
disordered solvent and counter-cations which could not be modelled as
discrete atomic sites. We employed PLATON SQUEEZE to calculate the
contribution to the diffraction from the solvent/cation region and
thereby produced a set of solvent-free diffraction intensities. SQUEEZE
estimated a total count of 30 electrons per unit cell, which were
assigned to be 2.0 DMF and 2.0 water molecules per indium. The final
formula was calculated from the TGA combined with elemental analysis data.
;
_refine_diff_density_max 0.62
_refine_diff_density_min -0.26
_refine_diff_density_rms 0.05
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.01
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 55
_refine_ls_number_reflns 1085
_refine_ls_number_restraints 30
_refine_ls_restrained_S_all 1.00
_refine_ls_R_factor_all 0.0908
_refine_ls_R_factor_gt 0.0458
_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^)+(0.043P)^2^+2.000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0980
_refine_ls_wR_factor_ref 0.105
_reflns_number_gt 696
_reflns_number_total 1085
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file c1fd00006c.txt
_cod_data_source_block NOTT-213
_cod_original_cell_volume 2654.3(3)
_cod_original_sg_symbol_H-M 'P 42/mmc'
_cod_database_code 1501630
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z+1/2'
'y, -x, z+1/2'
'-x, y, -z'
'x, -y, -z'
'y, x, -z+1/2'
'-y, -x, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z-1/2'
'-y, x, -z-1/2'
'x, -y, z'
'-x, y, z'
'-y, -x, z-1/2'
'y, x, 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
In1 In 0.5000 0.5000 0.2500 0.0562(3) Uani 1 8 d SU . .
O1 O 0.2575(5) 0.5000 0.24041(15) 0.1041(18) Uani 1 2 d SU . .
O2 O 0.5000 0.3581(4) 0.18774(17) 0.0848(14) Uani 1 2 d SU . .
C1 C 0.5000 0.2525(7) 0.2136(3) 0.074(2) Uani 1 2 d SU . .
C2 C 0.5000 0.1188(6) 0.1864(3) 0.0751(19) Uani 1 2 d SU . .
C3 C 0.5000 0.0000 0.2131(3) 0.069(3) Uani 1 4 d SU . .
H3A H 0.5000 0.0000 0.2478 0.083 Uiso 1 4 calc SR . .
C4 C 0.5000 0.1202(7) 0.1350(2) 0.090(2) Uani 1 2 d SU . .
H4A H 0.5000 0.2012 0.1177 0.108 Uiso 1 2 calc SR . .
C5 C 0.5000 0.0000 0.1093(3) 0.103(4) Uani 1 4 d SU . .
C6 C 0.5000 0.0000 0.0514(5) 0.109(4) Uiso 1 4 d SDU . .
C7 C 0.3821(11) 0.0536(10) 0.02725(17) 0.118(4) Uiso 0.50 1 d PDU . .
C8 C 0.2555(18) 0.094(2) 0.0501(10) 0.139(9) Uiso 0.25 1 d PDU . -1
H8A H 0.2485 0.0746 0.0852 0.167 Uiso 0.25 1 d PR . -1
C9 C 0.135(3) 0.148(2) 0.0272(2) 0.226(17) Uiso 0.25 1 d PD A -2
H9A H 0.0594 0.1830 0.0455 0.271 Uiso 0.25 1 d PR 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
In1 0.0666(4) 0.0666(4) 0.0355(4) 0.000 0.000 0.000
O1 0.081(3) 0.182(5) 0.049(3) 0.000 0.015(2) 0.000
O2 0.124(4) 0.050(3) 0.080(3) -0.008(3) 0.000 0.000
C1 0.084(5) 0.059(5) 0.079(5) -0.005(4) 0.000 0.000
C2 0.100(5) 0.049(4) 0.076(5) -0.006(4) 0.000 0.000
C3 0.101(8) 0.045(6) 0.062(6) 0.000 0.000 0.000
C4 0.166(8) 0.048(4) 0.056(4) -0.008(4) 0.000 0.000
C5 0.179(13) 0.076(8) 0.052(6) 0.000 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
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'
In In -0.7276 1.3100 '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
O2 In1 O2 125.53(16) . 11_566
O2 In1 O2 80.7(3) . 2_665
O2 In1 O1 136.39(16) . 11_566
O2 In1 O1 85.38(7) . .
O2 In1 O1 55.73(16) 11_566 .
O1 In1 O1 90.64(2) 11_566 .
O1 In1 O1 167.88(19) 2_665 .
C1 O1 In1 86.2(5) 11_566 .
C1 O2 In1 96.9(4) . .
O1 C1 O2 121.1(7) 12_656 .
O1 C1 C2 120.9(7) 12_656 .
O2 C1 C2 118.0(6) . .
C4 C2 C3 121.6(7) . .
C4 C2 C1 118.1(6) . .
C3 C2 C1 120.3(6) . .
C2 C3 C2 118.0(8) 2_655 .
C2 C4 C5 119.3(7) . .
C4 C5 C4 120.4(9) 2_655 .
C4 C5 C6 119.8(4) 2_655 .
C4 C5 C6 119.8(4) . .
C8 C7 C7 120.0(10) . 6
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
In1 O2 2.184(4) .
In1 O1 2.430(5) .
O1 C1 1.230(8) 11_566
O2 C1 1.259(7) .
C1 C2 1.518(8) .
C2 C4 1.377(9) .
C2 C3 1.381(8) .
C4 C5 1.380(7) .
C5 C6 1.549(15) .
C6 C7 1.443(8) .
C7 C8 1.457(10) .
C7 C7 1.458(9) 10
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 -0.019 0.436 -0.004 1529 30
|
1501631.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/16/1501631.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_1501631
loop_
_publ_author_name
'Thierry Maris'
'NGuyen Ba Chanh'
'Jean-Claude Bissey'
'Nathalie Filloleau'
'Serge Flandrois'
'Ridha Zouari'
'Abdelaziz Daoud'
_publ_section_title
;
Phase Transitions in a Two-Dimensional Molecular Complex
NH~3~-(CH~2~)~4~-NH~3~ CuC1~4~
;
_journal_name_full 'Phase Transition'
_journal_page_first 81
_journal_page_last 98
_journal_paper_doi 10.1080/01411599808222119
_journal_volume 66
_journal_year 1998
_chemical_formula_sum 'C4 H14 Cl4 Cu N2'
_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
_cell_angle_beta 103.11(5)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 9.264(3)
_cell_length_b 7.593(4)
_cell_length_c 7.577(4)
_cell_volume 519.1(4)
_diffrn_ambient_temperature 295
_diffrn_radiation_source 'Sealed Tube'
_diffrn_radiation_type 'Cu K\a'
_diffrn_radiation_wavelength 1.5418
_diffrn_reflns_reduction_process 'Merging of equivalent reflections'
_diffrn_reflns_theta_max 74.33
_diffrn_reflns_theta_min 2
_exptl_crystal_colour green
_refine_ls_R_factor_gt 0.0856
_refine_ls_wR_factor_gt 0.1042
_reflns_number_gt 831
_reflns_threshold_expression '> 3sigma(I)'
_cod_data_source_file deposit.cif
_cod_data_source_block 2C4CuRT
_cod_original_sg_symbol_H-M P21/c
_cod_original_formula_sum 'C4 H14 N2 Cu Cl4'
_cod_database_code 1501631
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_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_type_symbol
Cu1 0 0 0 0.024(1) Uani Cu
Cl2 0.0335(3) 0.2043(3) 0.2309(3) 0.030(1) Uani Cl
Cl3 -0.2503(3) 0.0435(3) -0.0532(4) 0.033(1) Uani Cl
N1 0.2262(10) -0.037(1) 0.568(1) 0.032(4) Uani N
C2 0.3626(12) 0.0632(14) 0.6486(16) 0.035(5) Uani C
C3 0.4636 0.0828 0.5191 0.030(5) Uani C
H2A 0.41738 -0.00014 0.75937 0.05 Uiso H
H2B 0.33379 0.1831 0.68308 0.05 Uiso H
H3A 0.54283 0.16955 0.57203 0.05 Uiso H
H3B 0.40359 0.12934 0.40178 0.05 Uiso H
H1A 0.1692 -0.0457 0.64928 0.05 Uiso H
H1B 0.25093 -0.14552 0.53723 0.05 Uiso H
H1C 0.17569 0.01941 0.46857 0.05 Uiso 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
Cu1 0.0194(9) 0.0251(10) 0.0286(11) -0.0056(9) 0.0070(8) 0.0030(8)
Cl2 0.0297(12) 0.0294(12) 0.0309(12) -0.0069(11) 0.0098(10) -0.003(10)
Cl3 0.0202(10) 0.0317(13) 0.0485(15) -0.0044(12) 0.0079(11) 0.0036(10)
N1 0.0259(46) 0.0230(43) 0.0461(54) -0.0007(40) 0.0084(42) 0.0001(37)
C2 0.0252(52) 0.0381(60) 0.0453(64) -0.0131(54) 0.0127(49) -0.0045(48)
C3 0.0269(53) 0.0246(50) 0.0406(60) 0.005(48) 0.0138(48) 0.0007(45)
loop_
_atom_type_symbol
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cu 2 -1.965 0.589 International_Table_Volume_IV_Table_2.3.1
Cl 8 0.364 0.702 International_Table_Volume_IV_Table_2.3.1
N 4 0.031 0.018 International_Table_Volume_IV_Table_2.3.1
C 8 0.018 0.009 International_Table_Volume_IV_Table_2.3.1
H 32 0.000 0.000 International_Table_Volume_IV_Table_2.3.1
|
1501632.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/16/1501632.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_1501632
loop_
_publ_author_name
'Sparta, K'
'Redhammer, G J'
'Roussel, P'
'Heger, G'
'Roth, G'
'Lemmens, P'
'Ionescu, A'
'Grove, M'
'Guentherodt, G'
'Huehning, F'
'Lueken, H'
'Kageyama, H.'
'Onizuka, K'
'Ueda, Y'
_publ_section_title
;
Structural phase transition in the 2D spin dimer compound SrCu2(BO3)2
;
_journal_name_full 'The European Physical Journal B'
_journal_page_first 507-516
_journal_volume 19
_journal_year 2001
_chemical_formula_moiety '2(B Cu O3), Sr'
_chemical_formula_sum 'B2 Cu2 O6 Sr'
_chemical_formula_weight 332.32
_chemical_name_common 'strontium copper borate'
_chemical_name_systematic
;
?
;
_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 none
_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 8.99060(14)
_cell_length_b 8.99060(14)
_cell_length_c 6.64800(11)
_cell_measurement_temperature 100(1)
_cell_volume 537.364(15)
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 100(1)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type 'STOE IPDS 1'
_diffrn_measurement_method 'rotation method'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71069
_diffrn_reflns_av_R_equivalents 0.0372
_diffrn_reflns_av_sigmaI/netI 0.0157
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 8
_diffrn_reflns_limit_l_min -8
_diffrn_reflns_number 2990
_diffrn_reflns_theta_full 28.04
_diffrn_reflns_theta_max 28.04
_diffrn_reflns_theta_min 3.20
_diffrn_standards_decay_% 0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 17.366
_exptl_absorpt_correction_T_max 0.2555
_exptl_absorpt_correction_T_min 0.0845
_exptl_absorpt_correction_type empirical
_exptl_absorpt_process_details 'X-SHAPE v. 1.03 (Stoe)'
_exptl_crystal_colour blue
_exptl_crystal_density_diffrn 4.108
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 616
_refine_diff_density_max 0.759
_refine_diff_density_min -0.738
_refine_diff_density_rms 0.151
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack 0.517(18)
_refine_ls_extinction_coef 0.0077(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 1.989
_refine_ls_hydrogen_treatment none
_refine_ls_matrix_type full
_refine_ls_number_parameters 26
_refine_ls_number_reflns 361
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.989
_refine_ls_R_factor_all 0.0177
_refine_ls_R_factor_gt 0.0175
_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^)+(0.0100P)^2^+0.4000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0402
_refine_ls_wR_factor_ref 0.0402
_reflns_number_gt 359
_reflns_number_total 361
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file scb100.cif
_cod_data_source_block scb100
_cod_database_code 1501632
_cod_database_fobs_code 1501632
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'y, -x, -z'
'-x, -y, z'
'-y, x, -z'
'-x, y, -z'
'-y, -x, z'
'x, -y, -z'
'y, x, z'
'x+1/2, y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'x+1/2, -y+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
Sr Sr 0.0000 0.5000 0.0000 0.00298(16) Uani 1 4 d S
Cu Cu 0.11454(4) 0.11454(4) 0.28838(9) 0.00349(18) Uani 1 2 d S
B B 0.2946(3) 0.2946(3) 0.2390(8) 0.0040(9) Uiso 1 2 d S
O1 O 0.4005(2) 0.4005(2) 0.1995(5) 0.0070(8) Uani 1 2 d S
O2 O 0.3276(2) 0.1458(2) 0.2573(5) 0.0053(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
Sr 0.0029(3) 0.0027(3) 0.0033(3) 0.000 0.000 0.000
Cu 0.00160(19) 0.00160(19) 0.0073(3) 0.00024(14) 0.00024(14) 0.000
O1 0.0035(8) 0.0035(8) 0.014(2) 0.0018(10) 0.0018(10) 0.000
O2 0.0049(10) 0.0021(10) 0.0088(11) 0.0013(10) 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
Sr Sr -1.6570 3.2640 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.2630 1.2660 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0000 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0080 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O2 Sr O2 119.28(10) 13 9_454
O2 Sr O2 106.58(10) 13 11_554
O2 Sr O2 103.04(12) 9_454 11_554
O2 Sr O2 103.04(12) 13 15_455
O2 Sr O2 106.58(10) 9_454 15_455
O2 Sr O2 119.28(10) 11_554 15_455
O2 Sr O2 172.42(9) 13 4
O2 Sr O2 66.36(3) 9_454 4
O2 Sr O2 66.36(3) 11_554 4
O2 Sr O2 79.09(6) 15_455 4
O2 Sr O2 66.36(3) 13 6_565
O2 Sr O2 79.09(6) 9_454 6_565
O2 Sr O2 172.42(9) 11_554 6_565
O2 Sr O2 66.36(3) 15_455 6_565
O2 Sr O2 120.83(10) 4 6_565
O2 Sr O2 66.36(3) 13 8
O2 Sr O2 172.42(9) 9_454 8
O2 Sr O2 79.09(6) 11_554 8
O2 Sr O2 66.36(3) 15_455 8
O2 Sr O2 108.55(11) 4 8
O2 Sr O2 99.75(12) 6_565 8
O2 Sr O2 79.09(6) 13 2_565
O2 Sr O2 66.36(3) 9_454 2_565
O2 Sr O2 66.36(3) 11_554 2_565
O2 Sr O2 172.42(9) 15_455 2_565
O2 Sr O2 99.75(12) 4 2_565
O2 Sr O2 108.55(11) 6_565 2_565
O2 Sr O2 120.83(10) 8 2_565
O1 Cu O1 81.88(14) 15_455 12_545
O1 Cu O2 102.53(9) 15_455 8
O1 Cu O2 174.32(13) 12_545 8
O1 Cu O2 174.32(13) 15_455 .
O1 Cu O2 102.53(9) 12_545 .
O2 Cu O2 72.85(13) 8 .
O1 B O2 122.85(18) . 8
O1 B O2 122.85(18) . .
O2 B O2 114.3(4) 8 .
B O1 Cu 129.43(10) . 12
B O1 Cu 129.43(10) . 10
Cu O1 Cu 97.92(14) 12 10
B O2 Cu 86.43(18) . .
B O2 Sr 132.5(3) . 9_545
Cu O2 Sr 116.70(12) . 9_545
B O2 Sr 123.3(3) . 2
Cu O2 Sr 124.87(12) . 2
Sr O2 Sr 78.60(6) 9_545 2
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sr O2 2.593(3) 13
Sr O2 2.593(3) 9_454
Sr O2 2.593(3) 11_554
Sr O2 2.593(3) 15_455
Sr O2 2.654(3) 4
Sr O2 2.654(3) 6_565
Sr O2 2.654(3) 8
Sr O2 2.654(3) 2_565
Cu O1 1.931(2) 15_455
Cu O1 1.931(2) 12_545
Cu O2 1.947(2) 8
Cu O2 1.947(2) .
B O1 1.371(5) .
B O2 1.376(3) 8
B O2 1.376(3) .
O1 Cu 1.931(2) 12
O1 Cu 1.931(2) 10
O2 Sr 2.593(3) 9_545
O2 Sr 2.654(3) 2
|
1501633.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/16/1501633.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_1501633
loop_
_publ_author_name
'Sparta, K'
'Redhammer, G J'
'Roussel, P'
'Heger, G'
'Roth, G'
'Lemmens, P'
'Ionescu, A'
'Grove, M'
'Guentherodt, G'
'Huehning, F'
'Lueken, H'
'Kageyama, H.'
'Onizuka, K'
'Ueda, Y'
_publ_section_title
;
Structural phase transition in the 2D spin dimer compound SrCu2(BO3)2
;
_journal_name_full 'The European Physical Journal B'
_journal_page_first 507-516
_journal_volume 19
_journal_year 2001
_chemical_formula_moiety '2(B Cu O3), Sr'
_chemical_formula_sum 'B2 Cu2 O6 Sr'
_chemical_formula_weight 332.32
_chemical_name_common 'strontium copper borate'
_chemical_name_systematic
;
?
;
_space_group_IT_number 140
_symmetry_cell_setting tetragonal
_symmetry_space_group_name_Hall '-I 4 2c'
_symmetry_space_group_name_H-M 'I 4/m c m'
_atom_sites_solution_hydrogens none
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 9.005(2)
_cell_length_b 9.005(2)
_cell_length_c 6.647(2)
_cell_measurement_temperature 423(2)
_cell_volume 539.0(2)
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 423(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type 'STOE IPDS 1'
_diffrn_measurement_method 'rotation method'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71069
_diffrn_reflns_av_R_equivalents 0.0333
_diffrn_reflns_av_sigmaI/netI 0.0119
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_l_max 7
_diffrn_reflns_limit_l_min -7
_diffrn_reflns_number 1801
_diffrn_reflns_theta_full 24.13
_diffrn_reflns_theta_max 24.13
_diffrn_reflns_theta_min 3.20
_diffrn_standards_decay_% 0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 17.313
_exptl_absorpt_correction_T_max 0.2619
_exptl_absorpt_correction_T_min 0.0921
_exptl_absorpt_correction_type empirical
_exptl_absorpt_process_details 'X-SHAPE v. 1.03 (Stoe)'
_exptl_crystal_colour blue
_exptl_crystal_density_diffrn 4.095
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 616
_refine_diff_density_max 0.407
_refine_diff_density_min -0.382
_refine_diff_density_rms 0.106
_refine_ls_extinction_coef 0.0092(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method SHELXL
_refine_ls_goodness_of_fit_ref 1.984
_refine_ls_hydrogen_treatment none
_refine_ls_matrix_type full
_refine_ls_number_parameters 20
_refine_ls_number_reflns 135
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.984
_refine_ls_R_factor_all 0.0155
_refine_ls_R_factor_gt 0.0154
_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^)+(0.0100P)^2^+0.9000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0399
_refine_ls_wR_factor_ref 0.0399
_reflns_number_gt 134
_reflns_number_total 135
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file sc423.cif
_cod_data_source_block sc423
_cod_original_cell_volume 539.0(3)
_cod_database_code 1501633
_cod_database_fobs_code 1501633
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'-x, y, z+1/2'
'y, x, z+1/2'
'x, -y, z+1/2'
'-y, -x, z+1/2'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, z+1'
'y+1/2, x+1/2, z+1'
'x+1/2, -y+1/2, z+1'
'-y+1/2, -x+1/2, z+1'
'-x, -y, -z'
'y, -x, -z'
'x, y, -z'
'-y, x, -z'
'x, -y, -z-1/2'
'-y, -x, -z-1/2'
'-x, y, -z-1/2'
'y, x, -z-1/2'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-y+1/2, -x+1/2, -z'
'-x+1/2, y+1/2, -z'
'y+1/2, x+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
Sr Sr 0.0000 0.0000 0.2500 0.0104(3) Uani 1 8 d S
Cu Cu 0.38606(6) -0.11394(6) 0.0000 0.0184(4) Uani 1 4 d S
B B 0.2951(6) 0.2049(6) 0.0000 0.0105(15) Uiso 1 4 d S
O1 O 0.4017(4) 0.0983(4) 0.0000 0.0409(18) Uani 1 4 d S
O2 O 0.1728(3) -0.1455(3) 0.0000 0.0133(7) Uani 1 2 d S
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Sr 0.0101(4) 0.0101(4) 0.0109(5) 0.000 0.000 0.000
Cu 0.0053(4) 0.0053(4) 0.0446(6) 0.000 0.000 -0.0011(3)
O1 0.0058(15) 0.0058(15) 0.111(6) 0.000 0.000 -0.0012(18)
O2 0.0060(16) 0.0080(16) 0.0259(17) 0.000 0.000 -0.0021(12)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Sr Sr -1.6570 3.2640 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.2630 1.2660 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0000 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0080 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O2 Sr O2 172.41(13) 21_556 18
O2 Sr O2 79.01(9) 21_556 2
O2 Sr O2 101.50(9) 18 2
O2 Sr O2 66.40(5) 21_556 6
O2 Sr O2 120.16(12) 18 6
O2 Sr O2 107.35(12) 2 6
O2 Sr O2 107.35(12) 21_556 .
O2 Sr O2 66.40(5) 18 .
O2 Sr O2 66.40(5) 2 .
O2 Sr O2 172.41(13) 6 .
O2 Sr O2 120.16(12) 21_556 17
O2 Sr O2 66.40(5) 18 17
O2 Sr O2 66.40(5) 2 17
O2 Sr O2 79.01(9) 6 17
O2 Sr O2 101.50(9) . 17
O2 Sr O2 66.40(5) 21_556 22_556
O2 Sr O2 107.35(12) 18 22_556
O2 Sr O2 120.16(12) 2 22_556
O2 Sr O2 101.50(9) 6 22_556
O2 Sr O2 79.01(9) . 22_556
O2 Sr O2 172.41(13) 17 22_556
O2 Sr O2 101.50(9) 21_556 5
O2 Sr O2 79.01(9) 18 5
O2 Sr O2 172.41(13) 2 5
O2 Sr O2 66.40(5) 6 5
O2 Sr O2 120.16(12) . 5
O2 Sr O2 107.35(12) 17 5
O2 Sr O2 66.40(5) 22_556 5
O1 Cu O1 81.6(2) 17_655 .
O1 Cu O2 175.80(15) 17_655 .
O1 Cu O2 102.63(14) . .
O1 Cu O2 102.63(14) 17_655 14_544
O1 Cu O2 175.80(15) . 14_544
O2 Cu O2 73.17(19) . 14_544
O1 B O2 122.9(3) . 13_554
O1 B O2 122.9(3) . 2
O2 B O2 114.3(6) 13_554 2
B O1 Cu 130.78(11) . 17_655
B O1 Cu 130.78(11) . .
Cu O1 Cu 98.4(2) 17_655 .
B O2 Cu 86.3(3) 18 .
B O2 Sr 127.75(19) 18 17
Cu O2 Sr 120.86(10) . 17
B O2 Sr 127.75(19) 18 .
Cu O2 Sr 120.86(10) . .
Sr O2 Sr 78.50(9) 17 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sr O2 2.626(3) 21_556
Sr O2 2.626(3) 18
Sr O2 2.626(3) 2
Sr O2 2.626(3) 6
Sr O2 2.626(3) .
Sr O2 2.626(3) 17
Sr O2 2.626(3) 22_556
Sr O2 2.626(3) 5
Cu O1 1.916(3) 17_655
Cu O1 1.916(3) .
Cu O2 1.942(3) .
Cu O2 1.942(3) 14_544
B O1 1.358(9) .
B O2 1.378(5) 13_554
B O2 1.378(5) 2
O1 Cu 1.916(3) 17_655
O2 B 1.378(5) 18
O2 Sr 2.626(3) 17
|
1501634.cif | #------------------------------------------------------------------------------
#$Date: 2017-10-13 02:32:00 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201954 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/50/16/1501634.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_1501634
loop_
_publ_author_name
'M. Amine Fourati'
'Thierry Maris'
'William G. Skene'
'C. G\'eraldine Bazuin'
'Robert E. Prud'homme'
_publ_section_title
;
Photophysical, Electrochemical and Crystallographic Investigations of the
Fluorophore 2,5-Bis(5-tert-butyl-benzoxazol-2-yl)thiophene
;
_journal_name_full 'The Journal of Physical Chemistry B'
_journal_page_first 12362
_journal_page_last 12369
_journal_paper_doi 10.1021/jp207136k
_journal_volume 115
_journal_year 2011
_chemical_compound_source 'Synthesized by the authors. See text'
_chemical_formula_moiety 'C26 H26 N2 O2 S'
_chemical_formula_sum 'C26 H26 N2 O2 S'
_chemical_formula_weight 430.55
_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
_cell_angle_beta 107.512(2)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 17.9167(7)
_cell_length_b 6.2563(2)
_cell_length_c 21.1871(8)
_cell_measurement_reflns_used 9918
_cell_measurement_temperature 150
_cell_measurement_theta_max 66.60
_cell_measurement_theta_min 3.86
_cell_volume 2264.84(14)
_computing_cell_refinement 'SAINT V7.60A(Bruker AXS, 2008)'
_computing_data_collection 'APEX2 (Bruker AXS, 2009)'
_computing_data_reduction 'SAINT V7.60A(Bruker AXS, 2008)'
_computing_molecular_graphics 'SHELXTL v6.12 (Bruker AXS, 2001)'
_computing_publication_material 'UdMX (Maris, 2004)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution 'SIR97 (Altomare et al., 1997)'
_diffrn_ambient_temperature 150
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type 'Bruker Microstar'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator 'Helios optics'
_diffrn_radiation_source 'Rotating Anode'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.052
_diffrn_reflns_av_sigmaI/netI 0.0354
_diffrn_reflns_limit_h_max 21
_diffrn_reflns_limit_h_min -21
_diffrn_reflns_limit_k_max 7
_diffrn_reflns_limit_k_min -6
_diffrn_reflns_limit_l_max 25
_diffrn_reflns_limit_l_min -25
_diffrn_reflns_number 27199
_diffrn_reflns_theta_full 67.13
_diffrn_reflns_theta_max 67.13
_diffrn_reflns_theta_min 3.86
_exptl_absorpt_coefficient_mu 1.462
_exptl_absorpt_correction_T_max 0.9295
_exptl_absorpt_correction_T_min 0.7317
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Sadabs (Sheldrick, 2008)'
_exptl_crystal_colour 'light green'
_exptl_crystal_density_diffrn 1.263
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 912
_exptl_crystal_size_max 0.15
_exptl_crystal_size_mid 0.10
_exptl_crystal_size_min 0.05
_refine_diff_density_max 0.403
_refine_diff_density_min -0.270
_refine_diff_density_rms 0.049
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.065
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 286
_refine_ls_number_reflns 4009
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.065
_refine_ls_R_factor_all 0.0680
_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^)+(0.0636P)^2^+1.5822P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1277
_refine_ls_wR_factor_ref 0.1390
_reflns_number_gt 3173
_reflns_number_total 4009
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file deposit.cif
_cod_data_source_block amin02
_cod_original_cell_volume 2264.87(15)
_cod_original_sg_symbol_H-M P21/n
_cod_database_code 1501634
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
S1 S 0.86939(4) 0.05844(9) 0.39097(3) 0.03673(19) Uani 1 1 d .
C1 C 0.86115(15) -0.3224(4) 0.34455(12) 0.0386(6) Uani 1 1 d .
H1 H 0.8411 -0.4541 0.3241 0.046 Uiso 1 1 calc R
C2 C 0.81527(15) -0.1557(4) 0.35095(11) 0.0356(6) Uani 1 1 d .
C3 C 0.73113(15) -0.1368(4) 0.32891(11) 0.0367(6) Uani 1 1 d .
C4 C 0.61168(15) -0.0420(4) 0.30619(12) 0.0362(5) Uani 1 1 d .
C5 C 0.61350(14) -0.2409(4) 0.27793(11) 0.0358(5) Uani 1 1 d .
C6 C 0.54669(16) -0.3489(4) 0.24330(12) 0.0421(6) Uani 1 1 d .
H6 H 0.5487 -0.4859 0.2245 0.051 Uiso 1 1 calc R
C7 C 0.47689(15) -0.2467(4) 0.23752(12) 0.0413(6) Uani 1 1 d .
H7 H 0.4297 -0.3150 0.2130 0.050 Uiso 1 1 calc R
C8 C 0.47191(15) -0.0453(4) 0.26626(11) 0.0377(6) Uani 1 1 d .
C9 C 0.54055(15) 0.0570(4) 0.30060(12) 0.0384(6) Uani 1 1 d .
H9 H 0.5391 0.1931 0.3201 0.046 Uiso 1 1 calc R
C10 C 0.39076(15) 0.0475(4) 0.25956(13) 0.0420(6) Uani 1 1 d .
C11 C 0.3461(2) -0.1041(6) 0.2907(2) 0.0840(12) Uani 1 1 d .
H11A H 0.3373 -0.2395 0.2662 0.126 Uiso 1 1 calc R
H11B H 0.2956 -0.0404 0.2890 0.126 Uiso 1 1 calc R
H11C H 0.3764 -0.1307 0.3368 0.126 Uiso 1 1 calc R
C12 C 0.3467(2) 0.0882(8) 0.18778(16) 0.0930(14) Uani 1 1 d .
H12A H 0.3766 0.1871 0.1689 0.140 Uiso 1 1 calc R
H12B H 0.2955 0.1510 0.1845 0.140 Uiso 1 1 calc R
H12C H 0.3392 -0.0471 0.1633 0.140 Uiso 1 1 calc R
C13 C 0.39607(19) 0.2595(5) 0.2971(2) 0.0737(10) Uani 1 1 d .
H13A H 0.4268 0.2387 0.3435 0.111 Uiso 1 1 calc R
H13B H 0.3433 0.3080 0.2948 0.111 Uiso 1 1 calc R
H13C H 0.4215 0.3672 0.2770 0.111 Uiso 1 1 calc R
C14 C 0.94107(15) -0.2789(4) 0.37142(11) 0.0372(6) Uani 1 1 d .
H14 H 0.9812 -0.3777 0.3710 0.045 Uiso 1 1 calc R
C15 C 0.95526(15) -0.0775(4) 0.39845(11) 0.0362(6) Uani 1 1 d .
C16 C 1.02933(14) 0.0284(4) 0.42435(11) 0.0340(5) Uani 1 1 d .
C17 C 1.14761(15) 0.1330(4) 0.45239(11) 0.0352(5) Uani 1 1 d .
C18 C 1.10410(14) 0.2954(4) 0.46804(11) 0.0352(5) Uani 1 1 d .
C19 C 1.13628(16) 0.4858(4) 0.49593(13) 0.0415(6) Uani 1 1 d .
H19 H 1.1054 0.5962 0.5062 0.050 Uiso 1 1 calc R
C20 C 1.21597(16) 0.5068(4) 0.50808(13) 0.0421(6) Uani 1 1 d .
H20 H 1.2403 0.6356 0.5277 0.050 Uiso 1 1 calc R
C21 C 1.26323(15) 0.3462(4) 0.49283(12) 0.0376(6) Uani 1 1 d .
C22 C 1.22801(15) 0.1566(4) 0.46483(12) 0.0384(6) Uani 1 1 d .
H22 H 1.2583 0.0451 0.4544 0.046 Uiso 1 1 calc R
C23 C 1.35030(16) 0.3903(4) 0.50367(13) 0.0428(6) Uani 1 1 d .
C24 C 1.35748(18) 0.5372(5) 0.44776(14) 0.0552(7) Uani 1 1 d .
H24A H 1.3340 0.4671 0.4050 0.083 Uiso 1 1 calc R
H24B H 1.4129 0.5663 0.4534 0.083 Uiso 1 1 calc R
H24C H 1.3301 0.6719 0.4491 0.083 Uiso 1 1 calc R
C25 C 1.39630(18) 0.1844(5) 0.50269(19) 0.0661(9) Uani 1 1 d .
H25A H 1.3912 0.0882 0.5377 0.099 Uiso 1 1 calc R
H25B H 1.4516 0.2192 0.5102 0.099 Uiso 1 1 calc R
H25C H 1.3755 0.1143 0.4596 0.099 Uiso 1 1 calc R
C26 C 1.38762(19) 0.5033(6) 0.56945(15) 0.0641(9) Uani 1 1 d .
H26A H 1.3610 0.6397 0.5700 0.096 Uiso 1 1 calc R
H26B H 1.4431 0.5296 0.5748 0.096 Uiso 1 1 calc R
H26C H 1.3828 0.4131 0.6058 0.096 Uiso 1 1 calc R
O1 O 1.02688(10) 0.2307(2) 0.45009(8) 0.0371(4) Uani 1 1 d .
N2 N 0.68894(12) 0.0208(3) 0.33876(10) 0.0389(5) Uani 1 1 d .
N1 N 1.09758(12) -0.0370(3) 0.42436(10) 0.0387(5) Uani 1 1 d .
O2 O 0.69047(10) -0.3040(3) 0.29218(8) 0.0392(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
S1 0.0402(4) 0.0324(3) 0.0369(3) -0.0026(2) 0.0105(3) 0.0009(3)
C1 0.0484(15) 0.0301(11) 0.0361(13) -0.0007(10) 0.0111(11) -0.0015(11)
C2 0.0431(14) 0.0335(12) 0.0307(12) 0.0018(10) 0.0121(11) 0.0008(11)
C3 0.0424(14) 0.0358(12) 0.0309(12) -0.0012(10) 0.0094(11) -0.0049(11)
C4 0.0399(14) 0.0354(12) 0.0326(12) -0.0014(10) 0.0101(10) -0.0068(11)
C5 0.0401(14) 0.0385(12) 0.0296(12) -0.0033(10) 0.0116(10) -0.0021(11)
C6 0.0524(16) 0.0407(13) 0.0349(13) -0.0109(11) 0.0157(12) -0.0086(12)
C7 0.0426(14) 0.0465(14) 0.0333(13) -0.0054(11) 0.0090(11) -0.0107(12)
C8 0.0421(14) 0.0402(13) 0.0316(12) 0.0014(10) 0.0125(11) -0.0058(11)
C9 0.0424(14) 0.0341(12) 0.0390(13) -0.0029(10) 0.0125(11) -0.0020(11)
C10 0.0407(14) 0.0456(14) 0.0408(14) 0.0003(11) 0.0139(11) -0.0043(12)
C11 0.072(2) 0.064(2) 0.136(4) 0.021(2) 0.061(2) 0.0024(18)
C12 0.076(3) 0.144(4) 0.052(2) 0.003(2) 0.0089(18) 0.049(3)
C13 0.0502(19) 0.0580(19) 0.113(3) -0.0186(19) 0.0247(19) -0.0017(15)
C14 0.0438(14) 0.0311(11) 0.0368(13) 0.0033(10) 0.0123(11) 0.0045(11)
C15 0.0440(14) 0.0330(12) 0.0304(12) 0.0057(10) 0.0094(10) 0.0018(11)
C16 0.0424(14) 0.0289(11) 0.0310(12) 0.0027(9) 0.0116(10) 0.0022(10)
C17 0.0442(14) 0.0278(11) 0.0339(12) 0.0024(9) 0.0122(11) 0.0005(10)
C18 0.0401(14) 0.0320(12) 0.0331(12) 0.0035(10) 0.0106(10) 0.0023(10)
C19 0.0495(16) 0.0327(12) 0.0439(14) -0.0026(10) 0.0164(12) 0.0026(11)
C20 0.0539(16) 0.0314(12) 0.0417(14) -0.0036(10) 0.0155(12) -0.0045(11)
C21 0.0439(14) 0.0354(12) 0.0334(12) 0.0030(10) 0.0115(11) -0.0026(11)
C22 0.0445(15) 0.0317(12) 0.0401(13) 0.0012(10) 0.0144(11) 0.0035(11)
C23 0.0454(15) 0.0397(13) 0.0421(14) 0.0004(11) 0.0112(12) -0.0059(11)
C24 0.0531(18) 0.0652(18) 0.0499(16) 0.0072(14) 0.0192(14) -0.0101(15)
C25 0.0423(17) 0.0514(17) 0.101(3) -0.0002(17) 0.0162(17) -0.0015(14)
C26 0.0567(19) 0.083(2) 0.0478(17) -0.0075(16) 0.0091(15) -0.0152(17)
O1 0.0418(10) 0.0303(8) 0.0390(9) -0.0015(7) 0.0119(7) 0.0014(7)
N2 0.0394(12) 0.0351(10) 0.0405(11) -0.0047(9) 0.0094(9) -0.0012(9)
N1 0.0423(12) 0.0310(10) 0.0419(12) -0.0004(9) 0.0115(10) 0.0008(9)
O2 0.0438(10) 0.0361(9) 0.0373(9) -0.0065(7) 0.0117(8) -0.0028(8)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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_publ_flag
C2 S1 C15 90.94(12) y
C2 C1 C14 112.7(2) y
C2 C1 H1 123.7 ?
C14 C1 H1 123.7 ?
C1 C2 C3 129.4(2) y
C1 C2 S1 112.24(19) y
C3 C2 S1 118.36(18) y
N2 C3 O2 115.7(2) y
N2 C3 C2 127.8(2) y
O2 C3 C2 116.4(2) y
C5 C4 C9 120.2(2) y
C5 C4 N2 108.4(2) y
C9 C4 N2 131.3(2) y
O2 C5 C6 128.9(2) y
O2 C5 C4 108.3(2) y
C6 C5 C4 122.7(2) y
C7 C6 C5 116.1(2) y
C7 C6 H6 121.9 ?
C5 C6 H6 121.9 ?
C6 C7 C8 123.3(2) y
C6 C7 H7 118.4 ?
C8 C7 H7 118.4 ?
C9 C8 C7 118.5(2) y
C9 C8 C10 122.8(2) y
C7 C8 C10 118.6(2) y
C8 C9 C4 119.1(2) y
C8 C9 H9 120.5 ?
C4 C9 H9 120.5 ?
C12 C10 C11 111.1(3) y
C12 C10 C8 110.6(2) y
C11 C10 C8 109.5(2) y
C12 C10 C13 108.0(3) y
C11 C10 C13 105.9(3) y
C8 C10 C13 111.7(2) y
C10 C11 H11A 109.5 ?
C10 C11 H11B 109.5 ?
H11A C11 H11B 109.5 ?
C10 C11 H11C 109.5 ?
H11A C11 H11C 109.5 ?
H11B C11 H11C 109.5 ?
C10 C12 H12A 109.5 ?
C10 C12 H12B 109.5 ?
H12A C12 H12B 109.5 ?
C10 C12 H12C 109.5 ?
H12A C12 H12C 109.5 ?
H12B C12 H12C 109.5 ?
C10 C13 H13A 109.5 ?
C10 C13 H13B 109.5 ?
H13A C13 H13B 109.5 ?
C10 C13 H13C 109.5 ?
H13A C13 H13C 109.5 ?
H13B C13 H13C 109.5 ?
C15 C14 C1 112.7(2) y
C15 C14 H14 123.6 ?
C1 C14 H14 123.6 ?
C14 C15 C16 128.0(2) y
C14 C15 S1 111.46(19) y
C16 C15 S1 120.29(18) y
N1 C16 O1 115.6(2) y
N1 C16 C15 128.4(2) y
O1 C16 C15 115.9(2) y
C18 C17 C22 120.2(2) y
C18 C17 N1 109.0(2) y
C22 C17 N1 130.8(2) y
C19 C18 C17 123.1(2) y
C19 C18 O1 128.8(2) y
C17 C18 O1 108.0(2) y
C18 C19 C20 116.0(2) y
C18 C19 H19 122 ?
C20 C19 H19 122 ?
C19 C20 C21 123.2(2) y
C19 C20 H20 118.4 ?
C21 C20 H20 118.4 ?
C22 C21 C20 118.6(2) y
C22 C21 C23 121.9(2) y
C20 C21 C23 119.4(2) y
C21 C22 C17 118.8(2) y
C21 C22 H22 120.6 ?
C17 C22 H22 120.6 ?
C26 C23 C21 111.5(2) y
C26 C23 C25 108.2(3) y
C21 C23 C25 112.0(2) y
C26 C23 C24 108.2(2) y
C21 C23 C24 108.1(2) y
C25 C23 C24 108.8(3) y
C23 C24 H24A 109.5 ?
C23 C24 H24B 109.5 ?
H24A C24 H24B 109.5 ?
C23 C24 H24C 109.5 ?
H24A C24 H24C 109.5 ?
H24B C24 H24C 109.5 ?
C23 C25 H25A 109.5 ?
C23 C25 H25B 109.5 ?
H25A C25 H25B 109.5 ?
C23 C25 H25C 109.5 ?
H25A C25 H25C 109.5 ?
H25B C25 H25C 109.5 ?
C23 C26 H26A 109.5 ?
C23 C26 H26B 109.5 ?
H26A C26 H26B 109.5 ?
C23 C26 H26C 109.5 ?
H26A C26 H26C 109.5 ?
H26B C26 H26C 109.5 ?
C18 O1 C16 103.21(18) y
C3 N2 C4 104.2(2) y
C16 N1 C17 104.2(2) y
C3 O2 C5 103.37(18) y
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
S1 C2 1.720(2) y
S1 C15 1.723(3) y
C1 C2 1.360(3) y
C1 C14 1.399(4) y
C1 H1 0.95 ?
C2 C3 1.443(4) y
C3 N2 1.297(3) y
C3 O2 1.375(3) y
C4 C5 1.386(3) y
C4 C9 1.390(4) y
C4 N2 1.404(3) y
C5 O2 1.378(3) y
C5 C6 1.378(3) y
C6 C7 1.377(4) y
C6 H6 0.95 ?
C7 C8 1.414(4) y
C7 H7 0.95 ?
C8 C9 1.383(3) y
C8 C10 1.532(4) y
C9 H9 0.95 ?
C10 C12 1.510(4) y
C10 C11 1.514(4) y
C10 C13 1.535(4) y
C11 H11a 0.98 ?
C11 H11b 0.98 ?
C11 H11c 0.98 ?
C12 H12a 0.98 ?
C12 H12b 0.98 ?
C12 H12c 0.98 ?
C13 H13a 0.98 ?
C13 H13b 0.98 ?
C13 H13c 0.98 ?
C14 C15 1.376(3) y
C14 H14 0.95 ?
C15 C16 1.436(3) y
C16 N1 1.289(3) y
C16 O1 1.385(3) y
C17 C18 1.380(3) y
C17 C22 1.392(3) y
C17 N1 1.402(3) y
C18 C19 1.377(3) y
C18 O1 1.381(3) y
C19 C20 1.379(4) y
C19 H19 0.95 ?
C20 C21 1.413(4) y
C20 H20 0.95 ?
C21 C22 1.390(3) y
C21 C23 1.532(4) y
C22 H22 0.95 ?
C23 C26 1.526(4) y
C23 C25 1.533(4) y
C23 C24 1.535(4) y
C24 H24a 0.98 ?
C24 H24b 0.98 ?
C24 H24c 0.98 ?
C25 H25a 0.98 ?
C25 H25b 0.98 ?
C25 H25c 0.98 ?
C26 H26a 0.98 ?
C26 H26b 0.98 ?
C26 H26c 0.98 ?
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
C14 C1 C2 C3 178.9(2) y
C14 C1 C2 S1 -0.6(3) y
C15 S1 C2 C1 0.61(19) y
C15 S1 C2 C3 -178.90(19) y
C1 C2 C3 N2 176.2(3) y
S1 C2 C3 N2 -4.4(3) y
C1 C2 C3 O2 -4.9(4) y
S1 C2 C3 O2 174.53(16) y
C9 C4 C5 O2 -178.5(2) y
N2 C4 C5 O2 0.0(3) y
C9 C4 C5 C6 0.3(4) y
N2 C4 C5 C6 178.8(2) y
O2 C5 C6 C7 179.1(2) y
C4 C5 C6 C7 0.6(4) y
C5 C6 C7 C8 -1.6(4) y
C6 C7 C8 C9 1.6(4) y
C6 C7 C8 C10 -176.8(2) y
C7 C8 C9 C4 -0.6(4) y
C10 C8 C9 C4 177.8(2) y
C5 C4 C9 C8 -0.3(4) y
N2 C4 C9 C8 -178.4(2) y
C9 C8 C10 C12 118.4(3) y
C7 C8 C10 C12 -63.2(3) y
C9 C8 C10 C11 -118.9(3) y
C7 C8 C10 C11 59.5(3) y
C9 C8 C10 C13 -1.9(4) y
C7 C8 C10 C13 176.5(2) y
C2 C1 C14 C15 0.2(3) y
C1 C14 C15 C16 -173.5(2) y
C1 C14 C15 S1 0.3(3) y
C2 S1 C15 C14 -0.50(19) y
C2 S1 C15 C16 173.78(19) y
C14 C15 C16 N1 4.4(4) y
S1 C15 C16 N1 -168.8(2) y
C14 C15 C16 O1 -178.6(2) y
S1 C15 C16 O1 8.1(3) y
C22 C17 C18 C19 0.2(4) y
N1 C17 C18 C19 -179.4(2) y
C22 C17 C18 O1 179.5(2) y
N1 C17 C18 O1 -0.2(3) y
C17 C18 C19 C20 -0.3(4) y
O1 C18 C19 C20 -179.4(2) y
C18 C19 C20 C21 0.6(4) y
C19 C20 C21 C22 -0.7(4) y
C19 C20 C21 C23 175.7(2) y
C20 C21 C22 C17 0.6(3) y
C23 C21 C22 C17 -175.8(2) y
C18 C17 C22 C21 -0.3(3) y
N1 C17 C22 C21 179.2(2) y
C22 C21 C23 C26 -140.5(3) y
C20 C21 C23 C26 43.2(3) y
C22 C21 C23 C25 -19.1(3) y
C20 C21 C23 C25 164.6(3) y
C22 C21 C23 C24 100.7(3) y
C20 C21 C23 C24 -75.6(3) y
C19 C18 O1 C16 179.3(2) y
C17 C18 O1 C16 0.1(2) y
N1 C16 O1 C18 -0.1(3) y
C15 C16 O1 C18 -177.41(19) y
O2 C3 N2 C4 0.2(3) y
C2 C3 N2 C4 179.2(2) y
C5 C4 N2 C3 -0.1(3) y
C9 C4 N2 C3 178.1(3) y
O1 C16 N1 C17 0.0(3) y
C15 C16 N1 C17 176.9(2) y
C18 C17 N1 C16 0.1(3) y
C22 C17 N1 C16 -179.5(2) y
N2 C3 O2 C5 -0.2(3) y
C2 C3 O2 C5 -179.3(2) y
C6 C5 O2 C3 -178.5(2) y
C4 C5 O2 C3 0.1(2) y
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 258050
|
1501635.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/16/1501635.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_1501635
loop_
_publ_author_name
'Ulrich Darbost'
'Janie Cabana'
'Eric Demers'
'Thierry Maris'
'James D. Wuest'
_publ_section_title
;
Molecular Tectonics. Use of Br...aryl Supramolecular Interactions for the
construction of Organized Networks from 9,9'-spirobifluorene in the
Crystalline State.
;
_journal_name_full CheM
_journal_page_first 52
_journal_page_last 12369
_journal_paper_doi 10.5618/chem.2011.v1.n1.7
_journal_volume 1
_journal_year 2011
_chemical_compound_source 'Synthesized by the authors. See text'
_chemical_formula_moiety 'C25 H12 Br4'
_chemical_formula_sum 'C25 H12 Br4'
_chemical_formula_weight 631.99
_chemical_name_systematic
;
?
;
_space_group_IT_number 41
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall 'A 2 -2ab'
_symmetry_space_group_name_H-M 'A b a 2'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 10.0693(7)
_cell_length_b 13.9976(7)
_cell_length_c 16.2481(8)
_cell_measurement_reflns_used 25
_cell_measurement_temperature 295
_cell_measurement_theta_max 26.16
_cell_measurement_theta_min 15.5
_cell_volume 2290.1(2)
_computing_cell_refinement 'CAD4 Program (Nonius 1989)'
_computing_data_collection 'CAD4 Program (Nonius 1989)'
_computing_data_reduction 'Local Program'
_computing_molecular_graphics 'SHELXTL (Bruker, 1997)'
_computing_publication_material 'UdMX (Maris, 2004)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature 295
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type Enraf-Nonius-CAD4
_diffrn_measurement_method \w/2\q
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'X-ray sealed tube'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.054
_diffrn_reflns_av_sigmaI/netI 0.0931
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 8546
_diffrn_reflns_theta_full 69.95
_diffrn_reflns_theta_max 69.95
_diffrn_reflns_theta_min 5.44
_diffrn_standards_interval_time 60
_diffrn_standards_number 5
_exptl_absorpt_coefficient_mu 8.638
_exptl_absorpt_correction_T_max 0.2112
_exptl_absorpt_correction_T_min 0.1499
_exptl_absorpt_correction_type analytical
_exptl_absorpt_process_details 'from crystal shape'
_exptl_crystal_colour Colorless
_exptl_crystal_density_diffrn 1.833
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 1208
_exptl_crystal_size_max 0.25
_exptl_crystal_size_mid 0.20
_exptl_crystal_size_min 0.18
_refine_diff_density_max 0.327
_refine_diff_density_min -0.476
_refine_diff_density_rms 0.101
_refine_ls_abs_structure_details 'Flack H D (1983), 1037 Friedel Pairs'
_refine_ls_abs_structure_Flack 0.07(4)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.041
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 132
_refine_ls_number_reflns 2158
_refine_ls_number_restraints 1
_refine_ls_restrained_S_all 1.033
_refine_ls_R_factor_all 0.0433
_refine_ls_R_factor_gt 0.0424
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0483P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1009
_refine_ls_wR_factor_ref 0.1011
_reflns_number_gt 1817
_reflns_number_total 2158
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file deposit.cif
_cod_data_source_block jiw787
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana
;
_cod_original_sg_symbol_Hall 'A 2 -2ac'
_cod_original_sg_symbol_H-M Aba2
_cod_database_code 1501635
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,1/2+y,1/2+z
-x,1/2-y,1/2+z
1/2-x,1/2+y,z
1/2+x,1/2-y,z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Br1 Br 1.10977(2) 0.88087(3) 0.13657(2) 0.04299(19) Uani 1 1 d .
Br2 Br 0.54260(2) 0.70045(2) 0.48968(3) 0.0399(2) Uani 1 1 d .
C1 C 1.0000 0.5000 0.3110(2) 0.0393(2) Uani 1 2 d SU
C2 C 1.0389(2) 0.5891(3) 0.2629(2) 0.0479(13) Uani 1 1 d U
C3 C 1.1351(3) 0.5987(2) 0.2044(3) 0.0360(9) Uani 1 1 d U
H3 H 1.1864 0.5465 0.1888 0.043 Uiso 1 1 calc .
C4 C 1.1552(3) 0.6856(3) 0.1693(2) 0.0456(12) Uani 1 1 d U
H4 H 1.2234 0.6930 0.1312 0.055 Uiso 1 1 calc .
C5 C 1.0767(3) 0.7631(2) 0.1890(3) 0.0400(11) Uani 1 1 d U
C6 C 0.9787(2) 0.7504(2) 0.2458(2) 0.0389(9) Uani 1 1 d U
H6 H 0.9283 0.8027 0.2623 0.047 Uiso 1 1 calc .
C7 C 0.9526(3) 0.6625(2) 0.2794(3) 0.0329(8) Uani 1 1 d U
C8 C 0.8589(2) 0.6337(2) 0.3457(2) 0.0308(9) Uani 1 1 d U
C9 C 0.7498(3) 0.6810(2) 0.3813(3) 0.0377(9) Uani 1 1 d U
H9 H 0.7241 0.7419 0.3649 0.045 Uiso 1 1 calc .
C10 C 0.6816(2) 0.6300(2) 0.4437(2) 0.0393(11) Uani 1 1 d U
C11 C 0.7022(3) 0.5354(3) 0.4579(2) 0.0462(12) Uani 1 1 d U
H11 H 0.6455 0.5024 0.4930 0.055 Uiso 1 1 calc .
C12 C 0.8075(2) 0.4873(2) 0.4204(2) 0.0401(10) Uani 1 1 d U
H12 H 0.8269 0.4244 0.4344 0.048 Uiso 1 1 calc .
C13 C 0.8836(2) 0.5359(2) 0.3612(2) 0.0377(10) Uani 1 1 d U
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Br1 0.0431(3) 0.0425(3) 0.0434(3) -0.0009(4) -0.0007(4) -0.0005(3)
Br2 0.0393(4) 0.0403(4) 0.0400(4) 0.0004(5) -0.0001(4) -0.0007(4)
C1 0.044(3) 0.0462(18) 0.028(3) 0.000 0.000 0.0118(18)
C2 0.044(3) 0.044(2) 0.056(3) -0.003(2) 0.016(2) 0.0045(19)
C3 0.031(2) 0.0403(19) 0.037(2) -0.0085(18) -0.0008(14) 0.0014(16)
C4 0.045(3) 0.055(3) 0.036(3) 0.011(2) -0.0003(19) 0.012(2)
C5 0.053(3) 0.042(2) 0.025(2) 0.0039(19) 0.0009(17) 0.0024(19)
C6 0.042(3) 0.0405(16) 0.034(2) -0.0030(17) -0.0009(16) -0.0054(18)
C7 0.025(2) 0.0376(16) 0.036(2) -0.0061(16) -0.0016(14) -0.0038(15)
C8 0.033(2) 0.0376(18) 0.0212(19) -0.0053(16) -0.0045(14) 0.0014(15)
C9 0.035(2) 0.0332(18) 0.045(2) -0.0067(19) 0.0078(16) -0.0045(18)
C10 0.039(3) 0.039(2) 0.040(3) -0.005(2) 0.0065(19) -0.004(2)
C11 0.054(3) 0.043(2) 0.042(3) 0.002(2) 0.014(2) 0.002(2)
C12 0.036(3) 0.040(2) 0.043(3) 0.0017(18) 0.0012(18) -0.0004(18)
C13 0.037(2) 0.0419(19) 0.034(2) 0.0022(17) 0.0005(16) 0.0067(18)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C13 101.76(16) . . y
C2 C1 C2 118.3(3) . 2_765 y
C2 C1 C13 110.44(13) . 2_765 y
C2 C1 C13 110.44(13) 2_765 . y
C13 C1 C13 114.8(3) . 2_765 y
C2 C1 C13 101.76(16) 2_765 2_765 y
C1 C2 C3 128.4(3) . . y
C1 C2 C7 110.5(2) . . y
C3 C2 C7 120.8(4) . . y
C2 C3 C4 119.1(3) . . y
C3 C4 C5 121.4(3) . . y
Br1 C5 C4 118.8(3) . . y
Br1 C5 C6 123.2(2) . . y
C4 C5 C6 118.0(3) . . y
C5 C6 C7 121.7(3) . . y
C2 C7 C6 118.2(3) . . y
C2 C7 C8 109.9(3) . . y
C6 C7 C8 130.8(3) . . y
C7 C8 C9 131.7(3) . . y
C7 C8 C13 106.3(2) . . y
C9 C8 C13 121.3(3) . . y
C8 C9 C10 115.8(3) . . y
Br2 C10 C9 112.5(2) . . y
Br2 C10 C11 124.1(2) . . y
C9 C10 C11 122.5(3) . . y
C10 C11 C12 120.8(3) . . y
C11 C12 C13 118.7(3) . . y
C1 C13 C8 111.2(2) . . y
C1 C13 C12 129.1(2) . . y
C8 C13 C12 119.7(2) . . y
C2 C3 H3 120.00 . . n
C4 C3 H3 120.00 . . n
C3 C4 H4 119.00 . . n
C5 C4 H4 119.00 . . n
C5 C6 H6 119.00 . . n
C7 C6 H6 119.00 . . n
C8 C9 H9 122.00 . . n
C10 C9 H9 122.00 . . n
C10 C11 H11 120.00 . . n
C12 C11 H11 120.00 . . n
C11 C12 H12 121.00 . . n
C13 C12 H12 121.00 . . n
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
Br1 C5 1.885(3) . y
Br2 C10 1.868(2) . y
C1 C2 1.523(4) . y
C1 C13 1.514(3) . y
C1 C2 1.523(4) 2_765 y
C1 C13 1.514(3) 2_765 y
C2 C3 1.364(5) . y
C2 C7 1.372(5) . y
C3 C4 1.359(5) . y
C4 C5 1.380(5) . y
C5 C6 1.363(5) . y
C6 C7 1.372(4) . y
C7 C8 1.488(5) . y
C8 C9 1.407(4) . y
C8 C13 1.414(4) . y
C9 C10 1.418(5) . y
C10 C11 1.360(5) . y
C11 C12 1.396(4) . y
C12 C13 1.405(4) . y
C3 H3 0.9300 . n
C4 H4 0.9300 . n
C6 H6 0.9300 . n
C9 H9 0.9300 . n
C11 H11 0.9300 . n
C12 H12 0.9300 . n
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
Br1 Br2 3.7984(6) 3_654 n
Br1 C11 3.659(3) 6_764 n
Br2 C5 3.564(5) 3_655 n
Br2 Br1 3.7984(6) 3_655 n
Br2 C4 3.539(3) 3_655 n
Br1 H3 3.2100 7_755 n
C4 Br2 3.539(3) 3_654 n
C4 C6 3.600(4) 8_565 n
C5 Br2 3.564(5) 3_654 n
C6 C4 3.600(4) 8_465 n
C11 Br1 3.659(3) 6_765 n
H3 Br1 3.2100 7_745 n
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C3 H3 Br1 0.93 3.21 4.136(6) 173.7 7_745
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_publ_flag
C13 C1 C2 C3 -176.9(3) . y
C13 C1 C2 C7 -3.3(3) . y
C2 C1 C2 C3 -55.8(4) 2_765 y
C2 C1 C2 C7 117.8(3) 2_765 y
C13 C1 C2 C3 60.8(4) 2_765 y
C13 C1 C2 C7 -125.6(3) 2_765 y
C2 C1 C13 C8 -0.9(3) . y
C2 C1 C13 C12 -177.5(3) . y
C2 C1 C13 C8 -127.3(3) 2_765 y
C2 C1 C13 C12 56.1(4) 2_765 y
C13 C1 C13 C8 118.4(2) 2_765 y
C13 C1 C13 C12 -58.2(3) 2_765 y
C1 C2 C3 C4 -179.2(3) . y
C7 C2 C3 C4 7.8(5) . y
C1 C2 C7 C6 175.3(3) . y
C1 C2 C7 C8 6.2(4) . y
C3 C2 C7 C6 -10.6(5) . y
C3 C2 C7 C8 -179.6(3) . y
C2 C3 C4 C5 -2.8(6) . y
C3 C4 C5 Br1 -179.3(3) . y
C3 C4 C5 C6 0.8(6) . y
Br1 C5 C6 C7 176.3(3) . y
C4 C5 C6 C7 -3.7(5) . y
C5 C6 C7 C2 8.5(5) . y
C5 C6 C7 C8 174.9(4) . y
C2 C7 C8 C9 -176.6(3) . y
C2 C7 C8 C13 -6.6(4) . y
C6 C7 C8 C9 16.1(6) . y
C6 C7 C8 C13 -173.9(4) . y
C7 C8 C9 C10 179.3(3) . y
C13 C8 C9 C10 10.6(5) . y
C7 C8 C13 C1 4.4(3) . y
C7 C8 C13 C12 -178.7(3) . y
C9 C8 C13 C1 175.7(3) . y
C9 C8 C13 C12 -7.4(4) . y
C8 C9 C10 Br2 177.9(2) . y
C8 C9 C10 C11 -12.3(5) . y
Br2 C10 C11 C12 179.2(2) . y
C9 C10 C11 C12 10.5(5) . y
C10 C11 C12 C13 -6.5(4) . y
C11 C12 C13 C1 -178.8(3) . y
C11 C12 C13 C8 4.9(4) . y
|
1501636.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/16/1501636.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_1501636
loop_
_publ_author_name
'Ulrich Darbost'
'Janie Cabana'
'Eric Demers'
'Thierry Maris'
'James D. Wuest'
_publ_section_title
;
Molecular Tectonics. Use of Br...aryl Supramolecular Interactions for the
construction of Organized Networks from 9,9'-spirobifluorene in the
Crystalline State.
;
_journal_name_full CheM
_journal_page_first 52
_journal_page_last 12369
_journal_paper_doi 10.5618/chem.2011.v1.n1.7
_journal_volume 1
_journal_year 2011
_chemical_compound_source 'Synthesized by the authors. See text'
_chemical_formula_moiety 'C25 H16, 4 (C Br4)'
_chemical_formula_sum 'C29 H16 Br16'
_chemical_formula_weight 1642.98
_chemical_name_systematic
;
?
;
_space_group_IT_number 86
_symmetry_cell_setting tetragonal
_symmetry_space_group_name_Hall '-P 4bc'
_symmetry_space_group_name_H-M 'P 42/n :2'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 2
_cell_length_a 13.5519(2)
_cell_length_b 13.5519(2)
_cell_length_c 10.7761(4)
_cell_measurement_reflns_used 15094
_cell_measurement_temperature 150(2)
_cell_measurement_theta_max 68.44
_cell_measurement_theta_min 4.62
_cell_volume 1979.07(8)
_computing_cell_refinement 'SMART (Bruker, 2003)'
_computing_data_collection 'SMART (Bruker, 2003)'
_computing_data_reduction 'SAINT (Bruker, 2004)'
_computing_molecular_graphics 'SHELXTL (Bruker, 1997)'
_computing_publication_material 'UdMX (local program)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 150(2)
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type 'Bruker Smart 6000'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator 'Montel 200 optics'
_diffrn_radiation_source 'Rotating Anode'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.067
_diffrn_reflns_av_sigmaI/netI 0.0300
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_limit_l_min -12
_diffrn_reflns_number 19219
_diffrn_reflns_theta_full 68.56
_diffrn_reflns_theta_max 68.56
_diffrn_reflns_theta_min 4.61
_diffrn_standards_decay_% -0.26
_diffrn_standards_interval_time 1440
_diffrn_standards_number 207
_exptl_absorpt_coefficient_mu 19.344
_exptl_absorpt_correction_T_max 0.175
_exptl_absorpt_correction_T_min 0.085
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Sadabs (Sheldrick,1996)'
_exptl_crystal_colour Colorless
_exptl_crystal_density_diffrn 2.757
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 1500
_exptl_crystal_size_max 0.15
_exptl_crystal_size_mid 0.10
_exptl_crystal_size_min 0.09
_refine_diff_density_max 0.493
_refine_diff_density_min -0.598
_refine_diff_density_rms 0.130
_refine_ls_extinction_coef 0.00079(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 1.071
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 103
_refine_ls_number_reflns 1823
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.071
_refine_ls_R_factor_all 0.0262
_refine_ls_R_factor_gt 0.0262
_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^)+(0.0300P)^2^+4.5244P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0672
_refine_ls_wR_factor_ref 0.0672
_reflns_number_gt 1816
_reflns_number_total 1823
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file deposit.cif
_cod_data_source_block jw1006
_cod_original_sg_symbol_H-M P42/n
_cod_database_code 1501636
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-y,1/2+x,1/2+z
1/2-x,1/2-y,z
1/2+y,-x,1/2+z
-x,-y,-z
y,1/2-x,1/2-z
1/2+x,1/2+y,-z
1/2-y,x,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
C1 C 0.2500 0.2500 0.2500 0.0167(12) Uani 1 4 d S
C2 C 0.1769(2) 0.2025(2) 0.1604(3) 0.0173(6) Uani 1 1 d .
C3 C 0.2045(2) 0.2208(2) 0.0379(3) 0.0177(6) Uani 1 1 d .
C4 C 0.1465(3) 0.1850(2) -0.0596(3) 0.0230(7) Uani 1 1 d .
H4 H 0.1644 0.1973 -0.1434 0.028 Uiso 1 1 calc R
C5 C 0.0621(2) 0.1311(2) -0.0313(3) 0.0248(7) Uani 1 1 d .
H5 H 0.0216 0.1068 -0.0965 0.030 Uiso 1 1 calc R
C6 C 0.0361(3) 0.1124(2) 0.0915(3) 0.0246(8) Uani 1 1 d .
H6 H -0.0215 0.0751 0.1090 0.030 Uiso 1 1 calc R
C7 C 0.0936(2) 0.1477(2) 0.1887(3) 0.0208(6) Uani 1 1 d .
H7 H 0.0762 0.1345 0.2725 0.025 Uiso 1 1 calc R
C8 C 0.6794(3) 0.0733(3) 0.0977(3) 0.0222(7) Uani 1 1 d .
Br1 Br 0.75454(3) 0.07841(3) -0.05473(4) 0.03300(15) Uani 1 1 d .
Br2 Br 0.58593(3) 0.18138(3) 0.09996(4) 0.03118(15) Uani 1 1 d .
Br3 Br 0.60959(3) -0.05079(3) 0.10664(4) 0.03067(15) Uani 1 1 d .
Br4 Br 0.76721(3) 0.08643(3) 0.23801(4) 0.02857(14) 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 0.0162(17) 0.0162(17) 0.018(3) 0.000 0.000 0.000
C2 0.0173(15) 0.0162(14) 0.0185(15) -0.0018(12) -0.0015(12) 0.0027(11)
C3 0.0228(15) 0.0146(13) 0.0159(14) 0.0000(12) -0.0001(12) 0.0041(12)
C4 0.0307(18) 0.0214(15) 0.0168(16) -0.0004(13) -0.0063(14) 0.0021(13)
C5 0.0271(17) 0.0202(15) 0.0271(18) -0.0012(14) -0.0118(14) 0.0008(12)
C6 0.0196(16) 0.0193(16) 0.035(2) 0.0005(13) -0.0007(13) 0.0014(12)
C7 0.0184(15) 0.0192(15) 0.0246(17) 0.0012(13) 0.0005(13) 0.0015(12)
C8 0.0237(17) 0.0237(17) 0.0192(17) 0.0001(12) -0.0003(12) 0.0005(13)
Br1 0.0384(2) 0.0421(2) 0.0185(2) 0.00130(15) 0.00431(15) 0.00231(15)
Br2 0.0285(2) 0.0232(2) 0.0419(3) -0.00549(15) -0.00485(15) 0.00515(14)
Br3 0.0327(2) 0.0215(2) 0.0378(3) 0.00092(14) -0.00721(15) -0.00520(14)
Br4 0.0276(2) 0.0387(2) 0.0194(2) 0.00233(14) -0.00561(14) -0.00639(14)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C2 101.48(16) . 3_555 no
C2 C1 C2 113.61(15) . 6_555 no
C2 C1 C2 113.61(15) . 8_555 no
C2 C1 C2 113.61(15) 3_555 6_555 no
C2 C1 C2 113.61(15) 3_555 8_555 no
C2 C1 C2 101.48(16) 6_555 8_555 no
C1 C2 C3 110.5(2) . . no
C1 C2 C7 128.0(3) . . no
C3 C2 C7 121.5(3) . . no
C2 C3 C4 119.9(3) . . no
C2 C3 C3 108.8(3) . 3_555 no
C3 C3 C4 131.3(3) 3_555 . no
C3 C4 C5 118.7(3) . . no
C4 C5 C6 120.8(3) . . no
C5 C6 C7 120.8(3) . . no
C2 C7 C6 118.4(3) . . no
C3 C4 H4 121.00 . . no
C5 C4 H4 121.00 . . no
C4 C5 H5 120.00 . . no
C6 C5 H5 120.00 . . no
C5 C6 H6 120.00 . . no
C7 C6 H6 120.00 . . no
C2 C7 H7 121.00 . . no
C6 C7 H7 121.00 . . no
Br1 C8 Br2 109.15(18) . . yes
Br1 C8 Br3 109.35(18) . . yes
Br1 C8 Br4 109.7(2) . . yes
Br2 C8 Br3 109.7(2) . . yes
Br2 C8 Br4 108.86(18) . . yes
Br3 C8 Br4 110.04(18) . . yes
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
Br1 C8 1.934(4) . yes
Br2 C8 1.937(4) . yes
Br3 C8 1.932(4) . yes
Br4 C8 1.932(4) . yes
C1 C2 1.526(3) 8_555 no
C1 C2 1.526(3) . no
C1 C2 1.526(3) 3_555 no
C1 C2 1.526(3) 6_555 no
C2 C7 1.385(4) . no
C2 C3 1.394(5) . no
C3 C4 1.399(5) . no
C3 C3 1.465(4) 3_555 no
C4 C5 1.391(5) . no
C5 C6 1.393(5) . no
C6 C7 1.390(5) . no
C4 H4 0.9500 . no
C5 H5 0.9500 . no
C6 H6 0.9500 . no
C7 H7 0.9500 . no
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
Br1 Br2 3.8224(6) 2_644 no
Br1 Br4 3.8152(6) 4_564 no
Br2 Br1 3.8224(6) 4_565 no
Br2 C7 3.493(3) 3_555 no
Br2 C5 3.533(3) 3_555 no
Br2 C6 3.249(3) 3_555 no
Br2 Br3 3.8871(6) 5_655 no
Br3 Br2 3.8871(6) 5_655 no
Br3 C4 3.651(3) 7_545 no
Br3 C3 3.696(3) 7_545 no
Br4 C5 3.692(3) 4_555 no
Br4 Br1 3.8152(6) 2_645 no
Br1 H7 3.2400 4_554 no
Br3 H5 3.2200 4_555 no
Br4 H6 3.1900 1_655 no
Br4 H5 3.1700 4_555 no
C3 Br3 3.696(3) 7_455 no
C4 Br3 3.651(3) 7_455 no
C5 Br2 3.533(3) 3_555 no
C5 Br4 3.692(3) 2_544 no
C6 Br2 3.249(3) 3_555 no
C7 Br2 3.493(3) 3_555 no
C5 H6 2.9700 5_555 no
C6 H5 3.0700 5_555 no
H5 Br3 3.2200 2_544 no
H5 C6 3.0700 5_555 no
H5 H6 2.4700 5_555 no
H5 Br4 3.1700 2_544 no
H6 Br4 3.1900 1_455 no
H6 H5 2.4700 5_555 no
H6 C5 2.9700 5_555 no
H7 Br1 3.2400 2_545 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C5 H5 Br4 0.95 3.17 3.692(3) 116.4 2_544
C6 H6 Br4 0.95 3.19 3.987(3) 143.2 1_455
C5 H5 Br3 0.95 3.22 3.915(4) 131.3 2_544
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_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 C1 C2 C3 -0.2(2) 3_555 . . no
C2 C1 C2 C7 179.6(3) 3_555 . . no
C2 C1 C2 C3 122.1(2) 6_555 . . no
C2 C1 C2 C7 -58.1(3) 6_555 . . no
C2 C1 C2 C3 -122.5(2) 8_555 . . no
C2 C1 C2 C7 57.3(3) 8_555 . . no
C1 C2 C3 C4 -179.0(2) . . . no
C1 C2 C3 C3 0.5(3) . . 3_555 no
C7 C2 C3 C4 1.2(4) . . . no
C7 C2 C3 C3 -179.3(2) . . 3_555 no
C1 C2 C7 C6 179.0(2) . . . no
C3 C2 C7 C6 -1.3(4) . . . no
C2 C3 C4 C5 -0.3(4) . . . no
C3 C3 C4 C5 -179.6(3) 3_555 . . no
C2 C3 C3 C2 -0.6(3) . 3_555 3_555 no
C2 C3 C3 C4 178.8(3) . 3_555 3_555 no
C4 C3 C3 C2 178.8(3) . 3_555 3_555 no
C4 C3 C3 C4 -1.8(5) . 3_555 3_555 no
C3 C4 C5 C6 -0.5(4) . . . no
C4 C5 C6 C7 0.4(5) . . . no
C5 C6 C7 C2 0.5(4) . . . no
|
1501637.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/16/1501637.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_1501637
loop_
_publ_author_name
'Ulrich Darbost'
'Janie Cabana'
'Eric Demers'
'Thierry Maris'
'James D. Wuest'
_publ_section_title
;
Molecular Tectonics. Use of Br...aryl Supramolecular Interactions for the
construction of Organized Networks from 9,9'-spirobifluorene in the
Crystalline State.
;
_journal_name_full CheM
_journal_page_first 52
_journal_page_last 12369
_journal_paper_doi 10.5618/chem.2011.v1.n1.7
_journal_volume 1
_journal_year 2011
_chemical_compound_source 'Synthesized by the authors. See text'
_chemical_formula_moiety 'C25 H16, 2(C H Br3)'
_chemical_formula_sum 'C27 H18 Br6'
_chemical_formula_weight 821.87
_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 94.857(2)
_cell_angle_gamma 90.00
_cell_formula_units_Z 8
_cell_length_a 19.2957(10)
_cell_length_b 13.8813(8)
_cell_length_c 20.0269(10)
_cell_measurement_reflns_used 27389
_cell_measurement_temperature 150(2)
_cell_measurement_theta_max 68.37
_cell_measurement_theta_min 3.88
_cell_volume 5344.9(5)
_computing_cell_refinement 'SMART (Bruker, 2003)'
_computing_data_collection 'SMART (Bruker, 2003)'
_computing_data_reduction 'SAINT (Bruker, 2004)'
_computing_molecular_graphics 'SHELXTL (Bruker, 1997)'
_computing_publication_material 'UdMX (local program)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 150(2)
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type 'Bruker Smart 6000'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator 'Montel 200 optics'
_diffrn_radiation_source 'Rotating Anode'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.056
_diffrn_reflns_av_sigmaI/netI 0.0372
_diffrn_reflns_limit_h_max 23
_diffrn_reflns_limit_h_min -23
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_l_max 24
_diffrn_reflns_limit_l_min -23
_diffrn_reflns_number 49712
_diffrn_reflns_theta_full 68.68
_diffrn_reflns_theta_max 68.68
_diffrn_reflns_theta_min 3.05
_diffrn_standards_decay_% -1.31
_diffrn_standards_number 482
_exptl_absorpt_coefficient_mu 10.962
_exptl_absorpt_correction_T_max 0.6400
_exptl_absorpt_correction_T_min 0.4100
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Sadabs (Sheldrick,1996)'
_exptl_crystal_colour Colorless
_exptl_crystal_density_diffrn 2.043
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 3120
_exptl_crystal_size_max 0.10
_exptl_crystal_size_mid 0.07
_exptl_crystal_size_min 0.04
_refine_diff_density_max 1.649
_refine_diff_density_min -1.414
_refine_diff_density_rms 0.125
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.030
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 595
_refine_ls_number_reflns 9747
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.030
_refine_ls_R_factor_all 0.0477
_refine_ls_R_factor_gt 0.0427
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0528P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1076
_refine_ls_wR_factor_ref 0.1119
_reflns_number_gt 8619
_reflns_number_total 9747
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file deposit.cif
_cod_data_source_block jw1005
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana
;
_cod_original_sg_symbol_H-M P21/n
_cod_database_code 1501637
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_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
C1 C 0.75422(19) 0.3795(3) 0.31302(18) 0.0233(8) Uani 1 1 d .
C2 C 0.81089(19) 0.4561(3) 0.30923(18) 0.0242(8) Uani 1 1 d .
C3 C 0.8035(2) 0.5543(3) 0.29958(19) 0.0268(8) Uani 1 1 d .
H3 H 0.7587 0.5835 0.2964 0.032 Uiso 1 1 calc R
C4 C 0.8631(2) 0.6096(3) 0.2946(2) 0.0320(9) Uani 1 1 d .
H4 H 0.8589 0.6771 0.2872 0.038 Uiso 1 1 calc R
C5 C 0.9290(2) 0.5675(3) 0.3001(2) 0.0350(9) Uani 1 1 d .
H5 H 0.9690 0.6064 0.2968 0.042 Uiso 1 1 calc R
C6 C 0.9364(2) 0.4692(3) 0.3106(2) 0.0298(9) Uani 1 1 d .
H6 H 0.9813 0.4405 0.3142 0.036 Uiso 1 1 calc R
C7 C 0.87728(19) 0.4135(3) 0.31552(19) 0.0250(8) Uani 1 1 d .
C8 C 0.86922(19) 0.3096(3) 0.32588(19) 0.0250(8) Uani 1 1 d .
C9 C 0.9184(2) 0.2366(3) 0.3348(2) 0.0323(9) Uani 1 1 d .
H9 H 0.9667 0.2506 0.3354 0.039 Uiso 1 1 calc R
C10 C 0.8957(2) 0.1425(3) 0.3427(2) 0.0347(10) Uani 1 1 d .
H10 H 0.9288 0.0919 0.3490 0.042 Uiso 1 1 calc R
C11 C 0.8250(2) 0.1217(3) 0.3415(2) 0.0339(9) Uani 1 1 d .
H11 H 0.8103 0.0570 0.3468 0.041 Uiso 1 1 calc R
C12 C 0.7754(2) 0.1945(3) 0.3327(2) 0.0280(8) Uani 1 1 d .
H12 H 0.7272 0.1803 0.3322 0.034 Uiso 1 1 calc R
C13 C 0.79806(19) 0.2881(3) 0.32481(18) 0.0234(8) Uani 1 1 d .
C14 C 0.70475(18) 0.3749(3) 0.24949(19) 0.0223(7) Uani 1 1 d .
C15 C 0.7207(2) 0.3564(3) 0.18420(19) 0.0258(8) Uani 1 1 d .
H15 H 0.7670 0.3418 0.1748 0.031 Uiso 1 1 calc R
C16 C 0.6672(2) 0.3598(3) 0.1329(2) 0.0297(8) Uani 1 1 d .
H16 H 0.6773 0.3486 0.0880 0.036 Uiso 1 1 calc R
C17 C 0.5990(2) 0.3794(3) 0.1469(2) 0.0316(9) Uani 1 1 d .
H17 H 0.5633 0.3825 0.1112 0.038 Uiso 1 1 calc R
C18 C 0.5826(2) 0.3943(3) 0.2119(2) 0.0292(8) Uani 1 1 d .
H18 H 0.5360 0.4062 0.2214 0.035 Uiso 1 1 calc R
C19 C 0.63631(19) 0.3915(3) 0.2637(2) 0.0248(8) Uani 1 1 d .
C20 C 0.6349(2) 0.4031(3) 0.3364(2) 0.0248(8) Uani 1 1 d .
C21 C 0.5795(2) 0.4141(3) 0.3758(2) 0.0322(9) Uani 1 1 d .
H21 H 0.5331 0.4183 0.3560 0.039 Uiso 1 1 calc R
C22 C 0.5936(2) 0.4188(3) 0.4451(2) 0.0392(10) Uani 1 1 d .
H22 H 0.5563 0.4255 0.4729 0.047 Uiso 1 1 calc R
C23 C 0.6612(3) 0.4140(3) 0.4741(2) 0.0370(10) Uani 1 1 d .
H23 H 0.6697 0.4178 0.5215 0.044 Uiso 1 1 calc R
C24 C 0.7173(2) 0.4035(3) 0.4349(2) 0.0327(9) Uani 1 1 d .
H24 H 0.7636 0.4008 0.4549 0.039 Uiso 1 1 calc R
C25 C 0.70341(19) 0.3971(3) 0.3661(2) 0.0251(8) Uani 1 1 d .
C26 C 0.75234(18) 0.2567(3) 0.67975(18) 0.0234(8) Uani 1 1 d .
C27 C 0.80146(19) 0.2370(3) 0.62513(19) 0.0234(8) Uani 1 1 d .
C28 C 0.7854(2) 0.2233(3) 0.5572(2) 0.0302(9) Uani 1 1 d .
H28 H 0.7384 0.2203 0.5391 0.036 Uiso 1 1 calc R
C29 C 0.8393(2) 0.2142(3) 0.5162(2) 0.0340(9) Uani 1 1 d .
H29 H 0.8290 0.2046 0.4695 0.041 Uiso 1 1 calc R
C30 C 0.9085(2) 0.2188(3) 0.5425(2) 0.0339(9) Uani 1 1 d .
H30 H 0.9446 0.2130 0.5134 0.041 Uiso 1 1 calc R
C31 C 0.9251(2) 0.2316(3) 0.6105(2) 0.0309(9) Uani 1 1 d .
H31 H 0.9722 0.2347 0.6285 0.037 Uiso 1 1 calc R
C32 C 0.87090(19) 0.2399(3) 0.6521(2) 0.0246(8) Uani 1 1 d .
C33 C 0.87227(19) 0.2549(3) 0.7250(2) 0.0253(8) Uani 1 1 d .
C34 C 0.9274(2) 0.2589(3) 0.7747(2) 0.0302(9) Uani 1 1 d .
H34 H 0.9741 0.2526 0.7636 0.036 Uiso 1 1 calc R
C35 C 0.9124(2) 0.2722(3) 0.8405(2) 0.0323(9) Uani 1 1 d .
H35 H 0.9494 0.2749 0.8750 0.039 Uiso 1 1 calc R
C36 C 0.8442(2) 0.2818(3) 0.8570(2) 0.0308(9) Uani 1 1 d .
H36 H 0.8353 0.2909 0.9025 0.037 Uiso 1 1 calc R
C37 C 0.7891(2) 0.2783(3) 0.8080(2) 0.0267(8) Uani 1 1 d .
H37 H 0.7425 0.2853 0.8193 0.032 Uiso 1 1 calc R
C38 C 0.80355(19) 0.2640(3) 0.74147(19) 0.0239(8) Uani 1 1 d .
C39 C 0.69364(19) 0.1841(3) 0.68526(18) 0.0241(8) Uani 1 1 d .
C40 C 0.6990(2) 0.0866(3) 0.69956(19) 0.0280(8) Uani 1 1 d .
H40 H 0.7433 0.0564 0.7061 0.034 Uiso 1 1 calc R
C41 C 0.6383(2) 0.0341(3) 0.7040(2) 0.0297(8) Uani 1 1 d .
H41 H 0.6410 -0.0328 0.7137 0.036 Uiso 1 1 calc R
C42 C 0.5730(2) 0.0788(3) 0.6945(2) 0.0321(9) Uani 1 1 d .
H42 H 0.5320 0.0418 0.6976 0.039 Uiso 1 1 calc R
C43 C 0.5678(2) 0.1765(3) 0.6805(2) 0.0313(9) Uani 1 1 d .
H43 H 0.5236 0.2069 0.6746 0.038 Uiso 1 1 calc R
C44 C 0.62859(19) 0.2292(3) 0.67547(19) 0.0253(8) Uani 1 1 d .
C45 C 0.63942(19) 0.3323(3) 0.66226(19) 0.0254(8) Uani 1 1 d .
C46 C 0.5926(2) 0.4079(3) 0.6491(2) 0.0298(9) Uani 1 1 d .
H46 H 0.5439 0.3969 0.6469 0.036 Uiso 1 1 calc R
C47 C 0.6187(2) 0.4997(3) 0.6394(2) 0.0322(9) Uani 1 1 d .
H47 H 0.5873 0.5517 0.6303 0.039 Uiso 1 1 calc R
C48 C 0.6902(2) 0.5167(3) 0.6428(2) 0.0323(9) Uani 1 1 d .
H48 H 0.7069 0.5801 0.6362 0.039 Uiso 1 1 calc R
C49 C 0.7370(2) 0.4417(3) 0.65584(19) 0.0271(8) Uani 1 1 d .
H49 H 0.7857 0.4531 0.6581 0.033 Uiso 1 1 calc R
C50 C 0.71133(19) 0.3499(3) 0.66549(18) 0.0236(8) Uani 1 1 d .
C60 C 0.8746(2) 0.1609(3) 0.0750(2) 0.0365(10) Uani 1 1 d .
H60 H 0.8801 0.0902 0.0675 0.044 Uiso 1 1 calc R
Br60 Br 0.78352(3) 0.19647(5) 0.03720(3) 0.05170(15) Uani 1 1 d .
Br61 Br 0.94649(3) 0.22552(5) 0.03100(3) 0.05475(16) Uani 1 1 d .
Br62 Br 0.88536(2) 0.18273(4) 0.17033(2) 0.03723(12) Uani 1 1 d .
C70 C 0.5841(2) 0.0435(3) 0.4387(2) 0.050(1) Uani 1 1 d .
H70 H 0.5352 0.0258 0.4229 0.076 Uiso 1 1 calc R
Br70 Br 0.60014(3) 0.01062(6) 0.53208(3) 0.06055(18) Uani 1 1 d .
Br71 Br 0.59513(3) 0.17990(4) 0.42815(4) 0.0674(2) Uani 1 1 d .
Br72 Br 0.64601(4) -0.02494(5) 0.38565(3) 0.06708(19) Uani 1 1 d .
C80 C 0.6316(2) 0.4817(3) 0.9042(2) 0.045(2) Uani 1 1 d .
H80 H 0.6336 0.5535 0.9070 0.068 Uiso 1 1 calc R
Br80 Br 0.55635(3) 0.44049(5) 0.95336(3) 0.05688(17) Uani 1 1 d .
Br81 Br 0.61501(3) 0.44848(4) 0.81114(2) 0.04396(13) Uani 1 1 d .
Br82 Br 0.71838(3) 0.43373(5) 0.94315(3) 0.05236(16) Uani 1 1 d .
C90 C 0.5726(2) 0.0983(3) 0.9480(2) 0.046(2) Uani 1 1 d .
H90 H 0.5217 0.1084 0.9363 0.069 Uiso 1 1 calc R
Br90 Br 0.62166(3) 0.15852(4) 0.87910(3) 0.05273(15) Uani 1 1 d .
Br91 Br 0.58933(3) -0.03757(4) 0.94974(4) 0.06122(18) Uani 1 1 d .
Br92 Br 0.59615(3) 0.15625(6) 1.03332(3) 0.06153(18) 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 0.0224(18) 0.027(2) 0.0193(18) 0.0006(15) -0.0032(14) 0.0021(15)
C2 0.0221(18) 0.032(2) 0.0186(18) -0.0025(15) -0.0003(14) -0.0007(15)
C3 0.0274(19) 0.029(2) 0.0231(19) 0.0005(15) -0.0030(15) 0.0012(15)
C4 0.038(2) 0.026(2) 0.031(2) 0.0008(17) -0.0037(17) -0.0032(17)
C5 0.032(2) 0.039(2) 0.033(2) 0.0014(18) -0.0012(18) -0.0115(18)
C6 0.0222(18) 0.037(2) 0.029(2) 0.0003(17) -0.0039(16) -0.0006(16)
C7 0.0233(18) 0.031(2) 0.0193(18) -0.0006(15) -0.0033(14) 0.0007(15)
C8 0.0242(18) 0.028(2) 0.0211(19) -0.0027(15) -0.0056(15) 0.0030(15)
C9 0.028(2) 0.037(2) 0.030(2) -0.0062(18) -0.0065(16) 0.0058(17)
C10 0.038(2) 0.031(2) 0.033(2) -0.0031(18) -0.0100(18) 0.0111(17)
C11 0.045(2) 0.026(2) 0.029(2) 0.0005(17) -0.0072(18) 0.0016(17)
C12 0.031(2) 0.028(2) 0.024(2) -0.0004(16) -0.0047(16) -0.0023(16)
C13 0.0245(18) 0.0270(19) 0.0180(18) -0.0005(15) -0.0022(14) 0.0037(15)
C14 0.0214(17) 0.0220(18) 0.0226(19) 0.0021(14) -0.0034(14) -0.0001(14)
C15 0.0280(19) 0.0252(19) 0.0238(19) -0.0003(15) 0.0002(15) -0.0005(15)
C16 0.036(2) 0.030(2) 0.022(2) -0.0020(16) -0.0026(16) -0.0071(16)
C17 0.031(2) 0.029(2) 0.032(2) 0.0032(17) -0.0103(17) -0.0060(16)
C18 0.0213(18) 0.028(2) 0.037(2) 0.0054(17) -0.0036(16) -0.0020(15)
C19 0.0230(18) 0.0234(19) 0.027(2) 0.0021(15) -0.0010(15) -0.0005(14)
C20 0.0261(18) 0.0212(18) 0.027(2) 0.0030(15) 0.0011(15) -0.0002(14)
C21 0.027(2) 0.031(2) 0.039(2) 0.0004(18) 0.0074(17) 0.0008(16)
C22 0.046(3) 0.035(2) 0.040(3) -0.0001(19) 0.022(2) 0.0026(19)
C23 0.053(3) 0.034(2) 0.025(2) 0.0016(18) 0.0079(19) 0.0019(19)
C24 0.038(2) 0.033(2) 0.026(2) 0.0011(17) -0.0010(17) 0.0023(17)
C25 0.0262(18) 0.0231(19) 0.026(2) 0.0005(15) 0.0026(15) -0.0008(14)
C26 0.0211(17) 0.029(2) 0.0195(18) -0.0017(15) -0.0021(14) 0.0017(14)
C27 0.0238(18) 0.0227(18) 0.0236(19) 0.0018(15) 0.0023(15) 0.0015(14)
C28 0.032(2) 0.030(2) 0.027(2) 0.0023(16) -0.0037(17) 0.0053(16)
C29 0.044(2) 0.035(2) 0.023(2) 0.0021(17) 0.0015(18) 0.0068(18)
C30 0.038(2) 0.034(2) 0.031(2) 0.0034(18) 0.0130(18) 0.0074(17)
C31 0.0269(19) 0.030(2) 0.036(2) 0.0033(17) 0.0046(17) 0.0038(16)
C32 0.0230(18) 0.0238(19) 0.027(2) -0.0005(15) 0.0001(15) 0.0020(14)
C33 0.0228(18) 0.0240(19) 0.028(2) 0.0019(15) -0.0015(15) -0.0005(14)
C34 0.0239(18) 0.029(2) 0.037(2) 0.0027(17) -0.0043(16) 0.0018(15)
C35 0.030(2) 0.034(2) 0.031(2) 0.0012(17) -0.0109(17) -0.0016(16)
C36 0.039(2) 0.030(2) 0.023(2) -0.0014(16) -0.0022(17) -0.0012(17)
C37 0.0289(19) 0.027(2) 0.024(2) 0.0019(15) 0.0004(16) -0.0002(15)
C38 0.0216(17) 0.0251(19) 0.0243(19) 0.0011(15) -0.0019(15) 0.0020(14)
C39 0.0232(18) 0.031(2) 0.0174(18) -0.0039(15) -0.0005(14) 0.0007(15)
C40 0.0279(19) 0.034(2) 0.0212(19) -0.0012(16) -0.0010(15) 0.0022(16)
C41 0.037(2) 0.028(2) 0.024(2) -0.0025(16) 0.0011(17) -0.0043(16)
C42 0.030(2) 0.042(2) 0.025(2) -0.0022(17) 0.0017(16) -0.0092(17)
C43 0.0234(19) 0.041(2) 0.029(2) -0.0026(18) -0.0001(16) 0.0001(16)
C44 0.0229(18) 0.032(2) 0.0200(19) -0.0022(15) -0.0006(14) 0.0004(15)
C45 0.0223(18) 0.033(2) 0.0197(19) -0.0052(15) -0.0020(14) 0.0013(15)
C46 0.0228(18) 0.037(2) 0.029(2) -0.0038(17) -0.0005(16) 0.0061(16)
C47 0.034(2) 0.033(2) 0.028(2) -0.0011(17) -0.0009(17) 0.0097(17)
C48 0.037(2) 0.029(2) 0.030(2) -0.0015(17) -0.0013(17) 0.0024(17)
C49 0.0246(19) 0.032(2) 0.024(2) -0.0023(16) -0.0013(15) -0.0007(15)
C50 0.0234(18) 0.031(2) 0.0163(17) -0.0019(15) -0.0019(14) 0.0045(15)
C60 0.037(2) 0.043(3) 0.028(2) -0.0029(19) -0.0034(18) 0.0047(19)
Br60 0.0306(2) 0.0779(4) 0.0447(3) -0.0047(3) -0.0081(2) 0.0068(2)
Br61 0.0353(3) 0.0972(5) 0.0321(3) 0.0112(3) 0.0048(2) 0.0042(3)
Br62 0.0308(2) 0.0521(3) 0.0287(2) 0.00179(19) 0.00225(17) -0.00264(18)
C70 0.048(2) 0.055(3) 0.049(2) 0.002(2) 0.0019(18) 0.0012(19)
Br70 0.0380(3) 0.1083(5) 0.0351(3) 0.0059(3) 0.0014(2) 0.0027(3)
Br71 0.0398(3) 0.0407(3) 0.1222(6) 0.0052(3) 0.0089(3) 0.0047(2)
Br72 0.0924(5) 0.0567(4) 0.0568(4) -0.0067(3) 0.0341(3) 0.0108(3)
C80 0.044(2) 0.048(2) 0.044(2) -0.0026(17) -0.0010(17) 0.0025(17)
Br80 0.0330(3) 0.1013(5) 0.0375(3) 0.0019(3) 0.0103(2) -0.0034(3)
Br81 0.0396(3) 0.0660(3) 0.0258(2) -0.0033(2) 0.00015(19) -0.0001(2)
Br82 0.0297(2) 0.0883(4) 0.0380(3) -0.0021(3) -0.0034(2) 0.0125(2)
C90 0.040(2) 0.052(2) 0.046(2) -0.0021(19) 0.0010(18) -0.0026(18)
Br90 0.0516(3) 0.0638(4) 0.0437(3) 0.0071(2) 0.0092(2) -0.0060(3)
Br91 0.0492(3) 0.0398(3) 0.0962(5) 0.0029(3) 0.0155(3) 0.0015(2)
Br92 0.0410(3) 0.1020(5) 0.0416(3) -0.0268(3) 0.0032(2) -0.0138(3)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 '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_publ_flag
C2 C1 C13 101.3(3) no
C2 C1 C14 112.7(3) no
C2 C1 C25 115.3(3) no
C13 C1 C14 113.1(3) no
C13 C1 C25 113.8(3) no
C14 C1 C25 101.2(3) no
C1 C2 C3 128.7(3) no
C1 C2 C7 110.6(3) no
C3 C2 C7 120.6(4) no
C2 C3 C4 118.5(4) no
C3 C4 C5 121.1(4) no
C4 C5 C6 120.4(4) no
C5 C6 C7 119.0(4) no
C2 C7 C6 120.5(4) no
C2 C7 C8 108.6(3) no
C6 C7 C8 130.9(4) no
C7 C8 C9 131.0(3) no
C7 C8 C13 108.8(3) no
C9 C8 C13 120.2(4) no
C8 C9 C10 118.8(4) no
C9 C10 C11 120.7(4) no
C10 C11 C12 120.9(4) no
C11 C12 C13 118.4(4) no
C1 C13 C8 110.7(3) no
C1 C13 C12 128.3(3) no
C8 C13 C12 121.1(4) no
C1 C14 C15 128.2(3) no
C1 C14 C19 111.1(3) no
C15 C14 C19 120.7(3) no
C14 C15 C16 118.5(4) no
C15 C16 C17 120.7(4) no
C16 C17 C18 120.9(4) no
C17 C18 C19 118.6(4) no
C14 C19 C18 120.5(4) no
C14 C19 C20 108.6(3) no
C18 C19 C20 131.0(3) no
C19 C20 C21 130.9(4) no
C19 C20 C25 108.5(3) no
C21 C20 C25 120.5(4) no
C20 C21 C22 118.4(4) no
C21 C22 C23 120.9(4) no
C22 C23 C24 121.1(4) no
C23 C24 C25 118.2(4) no
C1 C25 C20 110.6(3) no
C1 C25 C24 128.5(3) no
C20 C25 C24 120.9(4) no
C2 C3 H3 121.00 no
C4 C3 H3 121.00 no
C3 C4 H4 120.00 no
C5 C4 H4 119.00 no
C4 C5 H5 120.00 no
C6 C5 H5 120.00 no
C5 C6 H6 120.00 no
C7 C6 H6 121.00 no
C8 C9 H9 121.00 no
C10 C9 H9 121.00 no
C9 C10 H10 120.00 no
C11 C10 H10 120.00 no
C10 C11 H11 120.00 no
C12 C11 H11 119.00 no
C11 C12 H12 121.00 no
C13 C12 H12 121.00 no
C14 C15 H15 121.00 no
C16 C15 H15 121.00 no
C15 C16 H16 120.00 no
C17 C16 H16 120.00 no
C16 C17 H17 120.00 no
C18 C17 H17 120.00 no
C17 C18 H18 121.00 no
C19 C18 H18 121.00 no
C20 C21 H21 121.00 no
C22 C21 H21 121.00 no
C21 C22 H22 120.00 no
C23 C22 H22 119.00 no
C22 C23 H23 120.00 no
C24 C23 H23 119.00 no
C23 C24 H24 121.00 no
C25 C24 H24 121.00 no
C27 C26 C38 101.2(3) no
C27 C26 C39 116.2(3) no
C27 C26 C50 111.0(3) no
C38 C26 C39 114.9(3) no
C38 C26 C50 112.7(3) no
C39 C26 C50 101.3(3) no
C26 C27 C28 128.8(3) no
C26 C27 C32 110.4(3) no
C28 C27 C32 120.7(4) no
C27 C28 C29 118.6(4) no
C28 C29 C30 121.0(4) no
C29 C30 C31 120.8(4) no
C30 C31 C32 118.4(4) no
C27 C32 C31 120.5(4) no
C27 C32 C33 108.8(3) no
C31 C32 C33 130.7(3) no
C32 C33 C34 131.4(3) no
C32 C33 C38 108.0(3) no
C34 C33 C38 120.6(4) no
C33 C34 C35 118.4(4) no
C34 C35 C36 121.1(4) no
C35 C36 C37 120.9(4) no
C36 C37 C38 118.5(4) no
C26 C38 C33 111.5(3) no
C26 C38 C37 128.1(3) no
C33 C38 C37 120.5(4) no
C26 C39 C40 128.1(3) no
C26 C39 C44 110.9(3) no
C40 C39 C44 121.0(4) no
C39 C40 C41 118.5(4) no
C40 C41 C42 120.8(4) no
C41 C42 C43 120.6(4) no
C42 C43 C44 118.8(4) no
C39 C44 C43 120.3(4) no
C39 C44 C45 108.7(3) no
C43 C44 C45 131.0(4) no
C44 C45 C46 131.7(3) no
C44 C45 C50 108.4(3) no
C46 C45 C50 119.9(4) no
C45 C46 C47 118.7(4) no
C46 C47 C48 121.1(4) no
C47 C48 C49 120.5(4) no
C48 C49 C50 118.8(4) no
C26 C50 C45 110.8(3) no
C26 C50 C49 128.1(3) no
C45 C50 C49 121.1(4) no
C27 C28 H28 121.00 no
C29 C28 H28 121.00 no
C28 C29 H29 119.00 no
C30 C29 H29 120.00 no
C29 C30 H30 120.00 no
C31 C30 H30 120.00 no
C30 C31 H31 121.00 no
C32 C31 H31 121.00 no
C33 C34 H34 121.00 no
C35 C34 H34 121.00 no
C34 C35 H35 119.00 no
C36 C35 H35 119.00 no
C35 C36 H36 120.00 no
C37 C36 H36 120.00 no
C36 C37 H37 121.00 no
C38 C37 H37 121.00 no
C39 C40 H40 121.00 no
C41 C40 H40 121.00 no
C40 C41 H41 120.00 no
C42 C41 H41 120.00 no
C41 C42 H42 120.00 no
C43 C42 H42 120.00 no
C42 C43 H43 121.00 no
C44 C43 H43 121.00 no
C45 C46 H46 121.00 no
C47 C46 H46 121.00 no
C46 C47 H47 119.00 no
C48 C47 H47 120.00 no
C47 C48 H48 120.00 no
C49 C48 H48 120.00 no
C48 C49 H49 121.00 no
C50 C49 H49 121.00 no
Br60 C60 Br61 111.8(2) yes
Br60 C60 Br62 111.6(2) yes
Br61 C60 Br62 111.0(2) yes
Br60 C60 H60 107.00 no
Br61 C60 H60 107.00 no
Br62 C60 H60 107.00 no
Br70 C70 Br71 109.3(2) yes
Br70 C70 Br72 111.4(2) yes
Br71 C70 Br72 110.4(2) yes
Br70 C70 H70 109.00 no
Br71 C70 H70 109.00 no
Br72 C70 H70 109.00 no
Br80 C80 Br81 110.9(2) yes
Br80 C80 Br82 111.4(2) yes
Br81 C80 Br82 112.4(2) yes
Br80 C80 H80 107.00 no
Br81 C80 H80 107.00 no
Br82 C80 H80 107.00 no
Br90 C90 Br91 110.4(2) yes
Br90 C90 Br92 111.3(2) yes
Br91 C90 Br92 111.9(2) yes
Br90 C90 H90 108.00 no
Br91 C90 H90 108.00 no
Br92 C90 H90 108.00 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Br60 C60 1.918(4) yes
Br61 C60 1.927(4) yes
Br62 C60 1.927(4) yes
Br70 C70 1.924(4) yes
Br71 C70 1.919(4) yes
Br72 C70 1.917(4) yes
Br80 C80 1.910(4) yes
Br81 C80 1.920(4) yes
Br82 C80 1.907(4) yes
Br90 C90 1.929(4) yes
Br91 C90 1.913(4) yes
Br92 C90 1.908(4) yes
C1 C2 1.532(6) no
C1 C25 1.526(5) no
C1 C13 1.532(6) no
C1 C14 1.526(5) no
C2 C3 1.383(6) no
C2 C7 1.407(5) no
C3 C4 1.393(6) no
C4 C5 1.395(6) no
C5 C6 1.386(6) no
C6 C7 1.389(6) no
C7 C8 1.467(6) no
C8 C9 1.390(6) no
C8 C13 1.404(5) no
C9 C10 1.391(6) no
C10 C11 1.393(5) no
C11 C12 1.393(6) no
C12 C13 1.384(6) no
C14 C15 1.392(5) no
C14 C19 1.394(5) no
C15 C16 1.394(5) no
C16 C17 1.395(6) no
C17 C18 1.381(6) no
C18 C19 1.404(6) no
C19 C20 1.467(6) no
C20 C25 1.405(5) no
C20 C21 1.390(6) no
C21 C22 1.393(6) no
C22 C23 1.384(7) no
C23 C24 1.398(7) no
C24 C25 1.384(6) no
C3 H3 0.9500 no
C4 H4 0.9500 no
C5 H5 0.9500 no
C6 H6 0.9500 no
C9 H9 0.9500 no
C10 H10 0.9500 no
C11 H11 0.9500 no
C12 H12 0.9500 no
C15 H15 0.9500 no
C16 H16 0.9500 no
C17 H17 0.9500 no
C18 H18 0.9500 no
C21 H21 0.9500 no
C22 H22 0.9500 no
C23 H23 0.9500 no
C24 H24 0.9500 no
C26 C39 1.527(5) no
C26 C50 1.531(6) no
C26 C27 1.531(5) no
C26 C38 1.519(5) no
C27 C32 1.402(5) no
C27 C28 1.383(6) no
C28 C29 1.384(6) no
C29 C30 1.395(6) no
C30 C31 1.384(6) no
C31 C32 1.396(5) no
C32 C33 1.473(6) no
C33 C34 1.395(5) no
C33 C38 1.399(5) no
C34 C35 1.385(6) no
C35 C36 1.390(5) no
C36 C37 1.385(6) no
C37 C38 1.398(6) no
C39 C40 1.385(6) no
C39 C44 1.402(5) no
C40 C41 1.389(6) no
C41 C42 1.403(6) no
C42 C43 1.387(6) no
C43 C44 1.393(6) no
C44 C45 1.474(6) no
C45 C46 1.395(6) no
C45 C50 1.405(5) no
C46 C47 1.390(6) no
C47 C48 1.396(5) no
C48 C49 1.388(6) no
C49 C50 1.387(6) no
C28 H28 0.9500 no
C29 H29 0.9500 no
C30 H30 0.9500 no
C31 H31 0.9500 no
C34 H34 0.9500 no
C35 H35 0.9500 no
C36 H36 0.9500 no
C37 H37 0.9500 no
C40 H40 0.9500 no
C41 H41 0.9500 no
C42 H42 0.9500 no
C43 H43 0.9500 no
C46 H46 0.9500 no
C47 H47 0.9500 no
C48 H48 0.9500 no
C49 H49 0.9500 no
C60 H60 1.0000 no
C70 H70 1.0000 no
C80 H80 1.0000 no
C90 H90 1.0000 no
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
Br60 Br92 3.6526(9) 1_554 no
Br61 Br71 3.8978(9) 4_554 no
Br62 C9 3.385(4) . no
Br62 C10 3.486(4) . no
Br62 C8 3.615(4) . no
Br70 Br82 3.6543(9) 2_646 no
Br70 C70 3.728(4) 3_656 no
Br70 C42 3.470(4) . no
Br70 C41 3.475(4) . no
Br71 Br61 3.8978(9) 4_455 no
Br71 C22 3.334(4) . no
Br71 C23 3.582(4) . no
Br71 C20 3.715(4) . no
Br71 C21 3.421(4) . no
Br72 C15 3.449(4) 2_645 no
Br80 Br80 3.4112(9) 3_667 no
Br81 C47 3.519(4) . no
Br81 C46 3.286(4) . no
Br81 C45 3.457(4) . no
Br82 C36 3.745(4) . no
Br91 C31 3.427(4) 2_646 no
Br91 C30 3.386(4) 2_646 no
Br92 Br60 3.6526(9) 1_556 no
Br60 H16 3.1700 . no
Br60 H36 3.2300 1_554 no
Br61 H35 3.2000 1_554 no
Br62 H3 3.2200 2_645 no
Br62 H43 3.0700 4_554 no
Br62 H15 3.1800 . no
Br70 H70 2.8800 3_656 no
Br71 H35 2.9900 4_454 no
Br72 H15 2.8400 2_645 no
Br80 H10 3.1200 4_455 no
Br81 H40 3.1600 2_656 no
Br82 H36 3.1600 . no
Br90 H6 3.2100 4_455 no
Br90 H37 3.2300 . no
C3 C12 3.527(6) 2_655 no
C4 Br92 3.529(4) 2_656 no
C5 Br92 3.627(4) 2_656 no
C8 Br62 3.615(4) . no
C9 Br62 3.385(4) . no
C10 Br62 3.486(4) . no
C12 C3 3.527(6) 2_645 no
C15 Br72 3.449(4) 2_655 no
C16 Br92 3.658(4) 1_554 no
C20 Br71 3.715(4) . no
C21 Br71 3.421(4) . no
C22 Br71 3.334(4) . no
C22 C60 3.446(6) 2_655 no
C23 Br71 3.582(4) . no
C30 Br91 3.386(4) 2_656 no
C30 C80 3.565(6) 2_646 no
C31 Br91 3.427(4) 2_656 no
C36 Br82 3.745(4) . no
C41 Br70 3.475(4) . no
C42 Br70 3.470(4) . no
C45 Br81 3.457(4) . no
C46 Br81 3.286(4) . no
C47 Br81 3.519(4) . no
C60 C22 3.446(6) 2_645 no
C70 Br70 3.728(4) 3_656 no
C80 C30 3.565(6) 2_656 no
C6 H42 3.0400 4_554 no
C6 H90 3.0800 4_554 no
C10 H29 3.0700 . no
C11 H29 2.8000 . no
C12 H29 2.8500 . no
C12 H3 3.0300 2_645 no
C14 H4 3.0700 2_645 no
C15 H11 2.9000 2_655 no
C15 H4 3.0100 2_645 no
C16 H11 2.8000 2_655 no
C16 H4 3.0600 2_645 no
C17 H11 3.0200 2_655 no
C17 H31 2.9100 4_454 no
C17 H10 3.0000 2_655 no
C18 H10 3.0000 2_655 no
C21 H60 2.7800 2_655 no
C22 H60 2.4500 2_655 no
C23 H60 2.6800 2_655 no
C27 H49 3.0900 . no
C27 H80 2.9300 2_646 no
C28 H80 2.8800 2_646 no
C29 H80 2.7300 2_646 no
C30 H80 2.6600 2_646 no
C31 H80 2.7300 2_646 no
C32 H80 2.8400 2_646 no
C35 H41 3.0600 2_656 no
C36 H48 2.9800 2_646 no
C36 H41 2.9600 2_656 no
C37 H48 2.9700 2_646 no
C37 H41 3.0000 2_656 no
C46 H23 3.0700 . no
C47 H23 2.8700 . no
C48 H23 2.7900 . no
C49 H23 2.9100 . no
C50 H23 3.0800 . no
H3 Br62 3.2200 2_655 no
H3 C12 3.0300 2_655 no
H4 C15 3.0100 2_655 no
H4 C16 3.0600 2_655 no
H4 C14 3.0700 2_655 no
H5 H34 2.5900 3_766 no
H6 H90 2.5900 4_554 no
H6 Br90 3.2100 4_554 no
H10 Br80 3.1200 4_554 no
H10 C17 3.0000 2_645 no
H10 C18 3.0000 2_645 no
H11 C16 2.8000 2_645 no
H11 C17 3.0200 2_645 no
H11 C15 2.9000 2_645 no
H15 Br72 2.8400 2_655 no
H15 Br62 3.1800 . no
H16 Br60 3.1700 . no
H16 Br92 3.2400 1_554 no
H17 H31 2.4400 4_454 no
H21 H47 2.4000 3_666 no
H23 C48 2.7900 . no
H23 C49 2.9100 . no
H23 C46 3.0700 . no
H23 C47 2.8700 . no
H23 C50 3.0800 . no
H29 C10 3.0700 . no
H29 C12 2.8500 . no
H29 C11 2.8000 . no
H31 C17 2.9100 4_555 no
H31 H17 2.4400 4_555 no
H34 H5 2.5900 3_766 no
H35 Br71 2.9900 4_555 no
H35 Br61 3.2000 1_556 no
H36 Br82 3.1600 . no
H36 Br60 3.2300 1_556 no
H37 Br90 3.2300 . no
H40 Br81 3.1600 2_646 no
H41 C35 3.0600 2_646 no
H41 C37 3.0000 2_646 no
H41 C36 2.9600 2_646 no
H42 C6 3.0400 4_455 no
H43 Br62 3.0700 4_455 no
H47 H21 2.4000 3_666 no
H48 C36 2.9800 2_656 no
H48 C37 2.9700 2_656 no
H49 C27 3.0900 . no
H60 C22 2.4500 2_645 no
H60 C21 2.7800 2_645 no
H60 C23 2.6800 2_645 no
H70 Br70 2.8800 3_656 no
H80 C31 2.7300 2_656 no
H80 C32 2.8400 2_656 no
H80 C27 2.9300 2_656 no
H80 C28 2.8800 2_656 no
H80 C29 2.7300 2_656 no
H80 C30 2.6600 2_656 no
H90 C6 3.0800 4_455 no
H90 H6 2.5900 4_455 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C15 H15 Br72 0.95 2.84 3.448(4) 123.0 2_655
C70 H70 Br70 1.00 2.88 3.728(5) 143.2 3_656
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_publ_flag
C13 C1 C2 C3 -179.6(4) no
C13 C1 C2 C7 1.9(4) no
C14 C1 C2 C3 59.3(5) no
C14 C1 C2 C7 -119.2(4) no
C25 C1 C2 C3 -56.2(5) no
C25 C1 C2 C7 125.3(4) no
C2 C1 C13 C8 -1.3(4) no
C2 C1 C13 C12 179.8(4) no
C14 C1 C13 C8 119.6(4) no
C14 C1 C13 C12 -59.3(5) no
C25 C1 C13 C8 -125.6(4) no
C25 C1 C13 C12 55.4(5) no
C2 C1 C14 C15 59.0(6) no
C2 C1 C14 C19 -121.5(4) no
C13 C1 C14 C15 -55.1(6) no
C13 C1 C14 C19 124.4(4) no
C25 C1 C14 C15 -177.3(4) no
C25 C1 C14 C19 2.2(4) no
C2 C1 C25 C20 121.1(4) no
C2 C1 C25 C24 -61.3(6) no
C13 C1 C25 C20 -122.5(4) no
C13 C1 C25 C24 55.1(6) no
C14 C1 C25 C20 -0.8(4) no
C14 C1 C25 C24 176.7(4) no
C1 C2 C3 C4 -176.9(4) no
C7 C2 C3 C4 1.6(6) no
C1 C2 C7 C6 177.2(3) no
C1 C2 C7 C8 -1.9(4) no
C3 C2 C7 C6 -1.5(6) no
C3 C2 C7 C8 179.5(3) no
C2 C3 C4 C5 -0.9(6) no
C3 C4 C5 C6 0.1(6) no
C4 C5 C6 C7 0.0(6) no
C5 C6 C7 C2 0.7(6) no
C5 C6 C7 C8 179.5(4) no
C2 C7 C8 C9 -180.0(4) no
C2 C7 C8 C13 1.0(4) no
C6 C7 C8 C9 1.1(7) no
C6 C7 C8 C13 -178.0(4) no
C7 C8 C9 C10 -179.1(4) no
C13 C8 C9 C10 -0.1(6) no
C7 C8 C13 C1 0.3(4) no
C7 C8 C13 C12 179.3(3) no
C9 C8 C13 C1 -178.9(3) no
C9 C8 C13 C12 0.2(6) no
C8 C9 C10 C11 0.2(6) no
C9 C10 C11 C12 -0.3(6) no
C10 C11 C12 C13 0.3(6) no
C11 C12 C13 C1 178.6(4) no
C11 C12 C13 C8 -0.3(6) no
C1 C14 C15 C16 -177.3(4) no
C19 C14 C15 C16 3.3(6) no
C1 C14 C19 C18 177.5(4) no
C1 C14 C19 C20 -2.8(5) no
C15 C14 C19 C18 -3.0(6) no
C15 C14 C19 C20 176.7(4) no
C14 C15 C16 C17 -1.3(6) no
C15 C16 C17 C18 -1.1(6) no
C16 C17 C18 C19 1.4(6) no
C17 C18 C19 C14 0.6(6) no
C17 C18 C19 C20 -179.1(4) no
C14 C19 C20 C21 -174.9(4) no
C14 C19 C20 C25 2.2(5) no
C18 C19 C20 C21 4.7(8) no
C18 C19 C20 C25 -178.1(4) no
C19 C20 C21 C22 176.8(4) no
C25 C20 C21 C22 -0.1(6) no
C19 C20 C25 C1 -0.8(5) no
C19 C20 C25 C24 -178.5(4) no
C21 C20 C25 C1 176.8(4) no
C21 C20 C25 C24 -1.0(6) no
C20 C21 C22 C23 0.9(6) no
C21 C22 C23 C24 -0.5(6) no
C22 C23 C24 C25 -0.6(6) no
C23 C24 C25 C1 -176.0(4) no
C23 C24 C25 C20 1.4(6) no
C38 C26 C27 C28 180.0(4) no
C38 C26 C27 C32 -3.8(4) no
C39 C26 C27 C28 54.9(6) no
C39 C26 C27 C32 -128.9(4) no
C50 C26 C27 C28 -60.2(5) no
C50 C26 C27 C32 116.1(4) no
C27 C26 C38 C33 2.6(4) no
C27 C26 C38 C37 -177.6(4) no
C39 C26 C38 C33 128.6(4) no
C39 C26 C38 C37 -51.6(6) no
C50 C26 C38 C33 -116.0(4) no
C50 C26 C38 C37 63.7(5) no
C27 C26 C39 C40 61.3(5) no
C27 C26 C39 C44 -120.4(4) no
C38 C26 C39 C40 -56.5(5) no
C38 C26 C39 C44 121.9(4) no
C50 C26 C39 C40 -178.2(4) no
C50 C26 C39 C44 0.1(4) no
C27 C26 C50 C45 123.2(3) no
C27 C26 C50 C49 -56.3(5) no
C38 C26 C50 C45 -124.1(3) no
C38 C26 C50 C49 56.4(5) no
C39 C26 C50 C45 -0.9(4) no
C39 C26 C50 C49 179.7(4) no
C26 C27 C28 C29 174.8(4) no
C32 C27 C28 C29 -1.1(6) no
C26 C27 C32 C31 -174.9(4) no
C26 C27 C32 C33 3.6(5) no
C28 C27 C32 C31 1.8(6) no
C28 C27 C32 C33 -179.8(4) no
C27 C28 C29 C30 -0.1(6) no
C28 C29 C30 C31 0.7(6) no
C29 C30 C31 C32 -0.1(6) no
C30 C31 C32 C27 -1.1(6) no
C30 C31 C32 C33 -179.2(4) no
C27 C32 C33 C34 176.9(4) no
C27 C32 C33 C38 -1.8(5) no
C31 C32 C33 C34 -4.9(8) no
C31 C32 C33 C38 176.4(4) no
C32 C33 C34 C35 -178.6(4) no
C38 C33 C34 C35 -0.1(6) no
C32 C33 C38 C26 -0.7(5) no
C32 C33 C38 C37 179.6(4) no
C34 C33 C38 C26 -179.6(4) no
C34 C33 C38 C37 0.7(6) no
C33 C34 C35 C36 -0.3(6) no
C34 C35 C36 C37 0.0(6) no
C35 C36 C37 C38 0.6(6) no
C36 C37 C38 C26 179.4(4) no
C36 C37 C38 C33 -0.9(6) no
C26 C39 C40 C41 178.2(4) no
C44 C39 C40 C41 0.0(6) no
C26 C39 C44 C43 -178.0(3) no
C26 C39 C44 C45 0.7(4) no
C40 C39 C44 C43 0.5(6) no
C40 C39 C44 C45 179.1(3) no
C39 C40 C41 C42 -0.3(6) no
C40 C41 C42 C43 0.0(6) no
C41 C42 C43 C44 0.6(6) no
C42 C43 C44 C39 -0.8(6) no
C42 C43 C44 C45 -179.1(4) no
C39 C44 C45 C46 179.7(4) no
C39 C44 C45 C50 -1.2(4) no
C43 C44 C45 C46 -1.9(7) no
C43 C44 C45 C50 177.2(4) no
C44 C45 C46 C47 179.1(4) no
C50 C45 C46 C47 0.0(6) no
C44 C45 C50 C26 1.3(4) no
C44 C45 C50 C49 -179.2(3) no
C46 C45 C50 C26 -179.5(3) no
C46 C45 C50 C49 0.1(6) no
C45 C46 C47 C48 -0.1(6) no
C46 C47 C48 C49 0.2(6) no
C47 C48 C49 C50 -0.1(6) no
C48 C49 C50 C26 179.4(4) no
C48 C49 C50 C45 0.0(6) no
|
1501638.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/16/1501638.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_1501638
loop_
_publ_author_name
'Ulrich Darbost'
'Janie Cabana'
'Eric Demers'
'Thierry Maris'
'James D. Wuest'
_publ_section_title
;
Molecular Tectonics. Use of Br...aryl Supramolecular Interactions for the
construction of Organized Networks from 9,9'-spirobifluorene in the
Crystalline State.
;
_journal_name_full CheM
_journal_page_first 52
_journal_page_last 12369
_journal_paper_doi 10.5618/chem.2011.v1.n1.7
_journal_volume 1
_journal_year 2011
_chemical_compound_source 'Synthesized by the authors. See text'
_chemical_formula_moiety 'C25 H16, C H2 Br2 '
_chemical_formula_sum 'C26 H18 Br2'
_chemical_formula_weight 490.22
_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 90.380(2)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 10.3840(4)
_cell_length_b 17.9690(7)
_cell_length_c 11.1880(3)
_cell_measurement_reflns_used 16744
_cell_measurement_temperature 150(2)
_cell_measurement_theta_max 27.48
_cell_measurement_theta_min 2.55
_cell_volume 2087.52(13)
_computing_cell_refinement 'CAD4 Program (Nonius 1989)'
_computing_data_collection 'CAD4 Program (Nonius 1989)'
_computing_data_reduction 'Local Program'
_computing_molecular_graphics 'SHELXTL (Bruker, 1997)'
_computing_publication_material 'UdMX (local program)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type 'Nonius Kappa CCD'
_diffrn_measurement_method \w/2\q
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'X-ray sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.050
_diffrn_reflns_av_sigmaI/netI 0.0546
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 23
_diffrn_reflns_limit_k_min -23
_diffrn_reflns_limit_l_max 11
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_number 13403
_diffrn_reflns_theta_full 27.48
_diffrn_reflns_theta_max 27.48
_diffrn_reflns_theta_min 2.67
_diffrn_standards_decay_% 0.00
_diffrn_standards_interval_time 60
_diffrn_standards_number 13403
_exptl_absorpt_coefficient_mu 3.892
_exptl_absorpt_correction_T_max 0.378
_exptl_absorpt_correction_T_min 0.208
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details Sortav
_exptl_crystal_colour Colorless
_exptl_crystal_density_diffrn 1.560
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 976
_exptl_crystal_size_max 0.40
_exptl_crystal_size_mid 0.34
_exptl_crystal_size_min 0.25
_refine_diff_density_max 0.383
_refine_diff_density_min -0.558
_refine_diff_density_rms 0.076
_refine_ls_extinction_coef 0.0025(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method SHELXL
_refine_ls_goodness_of_fit_ref 1.041
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 282
_refine_ls_number_reflns 4785
_refine_ls_number_restraints 3
_refine_ls_restrained_S_all 1.047
_refine_ls_R_factor_all 0.0788
_refine_ls_R_factor_gt 0.0432
_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^)+(0.0481P)^2^+1.2348P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0942
_refine_ls_wR_factor_ref 0.1138
_reflns_number_gt 3190
_reflns_number_total 4785
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file deposit.cif
_cod_data_source_block jw1074
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.
'_geom_bond_publ_flag'
value 'Y' changed to 'y' according to the built-in table from CIF
Core dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29
(34 times).
'_geom_angle_publ_flag' value 'Y' changed to 'y'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (48
times).
'_geom_torsion_publ_flag' value 'Y' changed to 'y' according
to the built-in table from CIF Core dictionary named 'cif_core.dic'
version 2.4.1 from 2010-06-29 (76 times).
Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana
;
_cod_original_sg_symbol_H-M P21/n
_cod_database_code 1501638
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.1168(2) 0.23910(15) 0.5221(2) 0.0238(6) Uani 1 1 d . . .
C2 C 0.1718(3) 0.18020(16) 0.6072(2) 0.0269(6) Uani 1 1 d . . .
C3 C 0.2249(3) 0.18926(18) 0.7200(3) 0.0321(7) Uani 1 1 d . . .
H3 H 0.2289 0.2360 0.7555 0.039 Uiso 1 1 calc R . .
C4 C 0.2725(3) 0.1266(2) 0.7793(3) 0.0393(8) Uani 1 1 d . . .
H4 H 0.3082 0.1317 0.8553 0.047 Uiso 1 1 calc R . .
C5 C 0.2672(3) 0.0570(2) 0.7266(3) 0.0434(8) Uani 1 1 d . . .
H5 H 0.3003 0.0160 0.7672 0.052 Uiso 1 1 calc R . .
C6 C 0.2135(3) 0.04756(18) 0.6147(3) 0.0391(8) Uani 1 1 d . . .
H6 H 0.2099 0.0006 0.5798 0.047 Uiso 1 1 calc R . .
C7 C 0.1646(3) 0.10943(16) 0.5546(3) 0.0294(6) Uani 1 1 d . . .
C8 C 0.0982(3) 0.11625(16) 0.4390(3) 0.0283(6) Uani 1 1 d . . .
C9 C 0.0607(3) 0.06218(18) 0.3560(3) 0.0352(7) Uani 1 1 d . . .
H9 H 0.0808 0.0123 0.3679 0.042 Uiso 1 1 calc R . .
C10 C -0.0075(3) 0.08505(18) 0.2553(3) 0.0366(7) Uani 1 1 d . . .
H10 H -0.0342 0.0497 0.1997 0.044 Uiso 1 1 calc R . .
C11 C -0.0367(3) 0.15913(18) 0.2359(3) 0.0328(7) Uani 1 1 d . . .
H11 H -0.0822 0.1731 0.1676 0.039 Uiso 1 1 calc R . .
C12 C 0.0016(3) 0.21282(17) 0.3181(2) 0.0290(6) Uani 1 1 d . . .
H12 H -0.0177 0.2627 0.3053 0.035 Uiso 1 1 calc R . .
C13 C 0.0688(3) 0.19086(15) 0.4192(2) 0.0243(6) Uani 1 1 d . . .
C14 C 0.2183(3) 0.29627(16) 0.4845(2) 0.0252(6) Uani 1 1 d . . .
C15 C 0.3337(3) 0.28370(18) 0.4272(2) 0.0307(7) Uani 1 1 d . . .
H15 H 0.3583 0.2357 0.4059 0.037 Uiso 1 1 calc R . .
C16 C 0.4122(3) 0.34403(19) 0.4019(3) 0.0366(7) Uani 1 1 d . . .
H16 H 0.4903 0.3365 0.3636 0.044 Uiso 1 1 calc R . .
C17 C 0.3754(3) 0.41544(18) 0.4332(3) 0.0367(7) Uani 1 1 d . . .
H17 H 0.4294 0.4553 0.4160 0.044 Uiso 1 1 calc R . .
C18 C 0.2592(3) 0.42844(17) 0.4898(3) 0.0317(7) Uani 1 1 d . . .
H18 H 0.2348 0.4765 0.5106 0.038 Uiso 1 1 calc R . .
C19 C 0.1798(3) 0.36806(16) 0.5150(2) 0.0265(6) Uani 1 1 d . . .
C20 C 0.0514(3) 0.36415(16) 0.5706(2) 0.0260(6) Uani 1 1 d . . .
C21 C -0.0301(3) 0.41991(17) 0.6119(3) 0.0329(7) Uani 1 1 d . . .
H21 H -0.0053 0.4696 0.6097 0.039 Uiso 1 1 calc R . .
C22 C -0.1492(3) 0.39939(19) 0.6564(3) 0.0387(8) Uani 1 1 d . . .
H22 H -0.2049 0.4358 0.6847 0.046 Uiso 1 1 calc R . .
C23 C -0.1864(3) 0.3254(2) 0.6594(3) 0.0390(8) Uani 1 1 d . . .
H23 H -0.2673 0.3129 0.6885 0.047 Uiso 1 1 calc R . .
C24 C -0.1051(3) 0.26962(18) 0.6195(3) 0.0327(7) Uani 1 1 d . . .
H24 H -0.1301 0.2200 0.6226 0.039 Uiso 1 1 calc R . .
C25 C 0.0138(3) 0.28930(16) 0.5751(2) 0.0252(6) Uani 1 1 d . . .
C30 C 0.5359(7) 0.1041(8) 0.5499(7) 0.065(3) Uani 0.505(8) 1 d PD A 1
H30A H 0.4658 0.1370 0.5716 0.078 Uiso 0.505(8) 1 calc PR A 1
H30B H 0.4987 0.0567 0.5266 0.078 Uiso 0.505(8) 1 calc PR A 1
Br1 Br 0.6433(6) 0.0896(4) 0.6841(4) 0.0600(14) Uani 0.505(8) 1 d PD A 1
Br2 Br 0.6249(3) 0.14547(14) 0.4165(3) 0.0564(6) Uani 0.505(8) 1 d PD A 1
C31 C 0.5495(8) 0.1519(5) 0.5659(5) 0.056(2) Uani 0.495(8) 1 d PD A 2
H31A H 0.5706 0.2044 0.5704 0.067 Uiso 0.495(8) 1 calc PR A 2
H31B H 0.4597 0.1467 0.5876 0.067 Uiso 0.495(8) 1 calc PR A 2
Br1A Br 0.6496(6) 0.1014(4) 0.6812(3) 0.0443(6) Uani 0.495(8) 1 d PD A 2
Br2A Br 0.5674(6) 0.1208(3) 0.40332(13) 0.0776(14) Uani 0.495(8) 1 d PD 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
C1 0.0222(14) 0.0250(14) 0.0241(13) 0.0010(11) 0.0006(10) -0.0001(11)
C2 0.0198(14) 0.0327(16) 0.0281(14) 0.0051(12) -0.0002(11) -0.0006(12)
C3 0.0232(15) 0.0430(18) 0.0302(15) 0.0023(13) -0.0008(11) -0.0037(13)
C4 0.0285(17) 0.059(2) 0.0299(16) 0.0162(15) -0.0051(12) -0.0042(15)
C5 0.0334(18) 0.044(2) 0.052(2) 0.0205(16) -0.0079(15) -0.0015(15)
C6 0.0331(18) 0.0325(17) 0.052(2) 0.0099(15) -0.0075(14) 0.0017(14)
C7 0.0226(15) 0.0312(16) 0.0344(16) 0.0039(12) 0.0005(12) -0.0005(12)
C8 0.0201(15) 0.0308(16) 0.0338(16) -0.0018(12) -0.0003(11) 0.0009(12)
C9 0.0300(17) 0.0298(16) 0.0459(19) -0.0042(14) -0.0011(13) 0.0010(13)
C10 0.0294(16) 0.0432(19) 0.0373(17) -0.0130(14) -0.0020(13) -0.0025(14)
C11 0.0247(16) 0.0444(19) 0.0292(16) -0.0017(13) -0.0033(12) -0.0010(13)
C12 0.0225(15) 0.0341(16) 0.0305(15) 0.0010(12) -0.0015(11) 0.0012(12)
C13 0.0178(14) 0.0286(15) 0.0264(14) -0.0014(11) 0.0004(10) -0.0014(11)
C14 0.0234(14) 0.0330(15) 0.0191(13) 0.0023(11) -0.0037(10) -0.0011(12)
C15 0.0239(15) 0.0402(17) 0.0280(15) -0.0022(13) -0.0010(11) 0.0032(13)
C16 0.0232(16) 0.054(2) 0.0327(16) 0.0036(15) 0.0019(12) -0.0068(15)
C17 0.0351(18) 0.0434(19) 0.0317(16) 0.0089(14) -0.0008(13) -0.0155(15)
C18 0.0337(17) 0.0311(16) 0.0303(15) 0.0034(12) -0.0039(12) -0.0062(13)
C19 0.0250(15) 0.0317(16) 0.0226(14) 0.0014(11) -0.0042(11) -0.0005(12)
C20 0.0260(15) 0.0328(16) 0.0192(13) 0.0007(11) -0.0022(10) 0.0031(12)
C21 0.0390(18) 0.0310(16) 0.0286(15) -0.0017(12) 0.0003(12) 0.0031(14)
C22 0.0366(18) 0.047(2) 0.0324(17) 0.0004(14) 0.0071(13) 0.0131(15)
C23 0.0258(16) 0.053(2) 0.0387(18) 0.0024(15) 0.0073(13) 0.0051(15)
C24 0.0267(16) 0.0383(18) 0.0332(16) 0.0055(13) 0.0011(12) -0.0035(13)
C25 0.0232(15) 0.0298(15) 0.0225(13) 0.0016(11) -0.0004(10) 0.0008(12)
C30 0.052(5) 0.095(8) 0.049(5) 0.016(5) -0.006(4) -0.015(6)
Br1 0.0569(15) 0.062(3) 0.0609(15) 0.0224(11) -0.0089(9) 0.0064(14)
Br2 0.0688(10) 0.0579(8) 0.0425(8) 0.0152(5) 0.0096(6) 0.0097(8)
C31 0.057(5) 0.053(5) 0.058(4) -0.008(3) -0.006(3) 0.015(4)
Br1A 0.0512(10) 0.0419(12) 0.0397(11) 0.0046(8) -0.0166(8) -0.0023(7)
Br2A 0.119(3) 0.0776(17) 0.0362(5) -0.0124(6) -0.0136(8) 0.0597(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'
Br Br -0.2901 2.4595 '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_publ_flag
C13 C1 C25 113.9(2) y
C13 C1 C2 101.3(2) y
C25 C1 C2 115.3(2) y
C13 C1 C14 113.4(2) y
C25 C1 C14 101.3(2) y
C2 C1 C14 112.3(2) y
C3 C2 C7 120.6(3) y
C3 C2 C1 129.1(3) y
C7 C2 C1 110.3(2) y
C2 C3 C4 118.5(3) y
C2 C3 H3 120.8 ?
C4 C3 H3 120.8 ?
C5 C4 C3 120.9(3) y
C5 C4 H4 119.5 ?
C3 C4 H4 119.5 ?
C6 C5 C4 120.9(3) y
C6 C5 H5 119.6 ?
C4 C5 H5 119.6 ?
C5 C6 C7 118.9(3) y
C5 C6 H6 120.5 ?
C7 C6 H6 120.5 ?
C6 C7 C2 120.2(3) y
C6 C7 C8 131.3(3) y
C2 C7 C8 108.5(2) y
C13 C8 C9 120.3(3) y
C13 C8 C7 108.8(2) y
C9 C8 C7 130.9(3) y
C10 C9 C8 118.1(3) y
C10 C9 H9 120.9 ?
C8 C9 H9 120.9 ?
C11 C10 C9 121.5(3) y
C11 C10 H10 119.2 ?
C9 C10 H10 119.2 ?
C10 C11 C12 120.2(3) y
C10 C11 H11 119.9 ?
C12 C11 H11 119.9 ?
C13 C12 C11 118.9(3) y
C13 C12 H12 120.5 ?
C11 C12 H12 120.5 ?
C12 C13 C8 120.9(3) y
C12 C13 C1 128.1(3) y
C8 C13 C1 111.0(2) y
C15 C14 C19 121.1(3) y
C15 C14 C1 128.2(3) y
C19 C14 C1 110.7(2) y
C14 C15 C16 118.7(3) y
C14 C15 H15 120.7 ?
C16 C15 H15 120.7 ?
C17 C16 C15 120.6(3) y
C17 C16 H16 119.7 ?
C15 C16 H16 119.7 ?
C16 C17 C18 120.9(3) y
C16 C17 H17 119.5 ?
C18 C17 H17 119.5 ?
C17 C18 C19 118.6(3) y
C17 C18 H18 120.7 ?
C19 C18 H18 120.7 ?
C18 C19 C14 120.0(3) y
C18 C19 C20 131.3(3) y
C14 C19 C20 108.7(2) y
C21 C20 C25 120.6(3) y
C21 C20 C19 131.2(3) y
C25 C20 C19 108.3(2) y
C22 C21 C20 118.3(3) y
C22 C21 H21 120.9 ?
C20 C21 H21 120.9 ?
C23 C22 C21 120.9(3) y
C23 C22 H22 119.6 ?
C21 C22 H22 119.6 ?
C22 C23 C24 121.0(3) y
C22 C23 H23 119.5 ?
C24 C23 H23 119.5 ?
C25 C24 C23 118.6(3) y
C25 C24 H24 120.7 ?
C23 C24 H24 120.7 ?
C24 C25 C20 120.6(3) y
C24 C25 C1 128.4(3) y
C20 C25 C1 111.0(2) y
BR1 C30 BR2 112.9(4) y
BR1 C30 H30A 109 ?
BR2 C30 H30A 109 ?
BR1 C30 H30B 109 ?
BR2 C30 H30B 109 ?
H30A C30 H30B 107.8 ?
BR1A C31 BR2A 117.0(3) y
BR1A C31 H31A 108 ?
BR2A C31 H31A 108 ?
BR1A C31 H31B 108 ?
BR2A C31 H31B 108 ?
H31A C31 H31B 107.3 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
C1 C13 1.522(4) y
C1 C25 1.522(4) y
C1 C2 1.532(4) y
C1 C14 1.533(4) y
C2 C3 1.384(4) y
C2 C7 1.403(4) y
C3 C4 1.395(4) y
C3 H3 0.93 ?
C4 C5 1.384(5) y
C4 H4 0.93 ?
C5 C6 1.378(5) y
C5 H5 0.93 ?
C6 C7 1.393(4) y
C6 H6 0.93 ?
C7 C8 1.467(4) y
C8 C13 1.392(4) y
C8 C9 1.398(4) y
C9 C10 1.389(5) y
C9 H9 0.93 ?
C10 C11 1.382(4) y
C10 H10 0.93 ?
C11 C12 1.389(4) y
C11 H11 0.93 ?
C12 C13 1.384(4) y
C12 H12 0.93 ?
C14 C15 1.382(4) y
C14 C19 1.394(4) y
C15 C16 1.386(4) y
C15 H15 0.93 ?
C16 C17 1.385(5) y
C16 H16 0.93 ?
C17 C18 1.386(5) y
C17 H17 0.93 ?
C18 C19 1.392(4) y
C18 H18 0.93 ?
C19 C20 1.477(4) y
C20 C21 1.393(4) y
C20 C25 1.401(4) y
C21 C22 1.386(5) y
C21 H21 0.93 ?
C22 C23 1.385(5) y
C22 H22 0.93 ?
C23 C24 1.386(4) y
C23 H23 0.93 ?
C24 C25 1.380(4) y
C24 H24 0.93 ?
C30 Br1 1.882(6) y
C30 Br2 1.911(6) y
C30 H30a 0.97 ?
C30 H30b 0.97 ?
C31 Br1a 1.884(5) y
C31 Br2a 1.912(5) y
C31 H31a 0.97 ?
C31 H31b 0.97 ?
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
C13 C1 C2 C3 -176.9(3) y
C25 C1 C2 C3 -53.5(4) y
C14 C1 C2 C3 61.8(4) y
C13 C1 C2 C7 4.1(3) y
C25 C1 C2 C7 127.5(3) y
C14 C1 C2 C7 -117.1(3) y
C7 C2 C3 C4 0.8(4) y
C1 C2 C3 C4 -178.1(3) y
C2 C3 C4 C5 0.3(5) y
C3 C4 C5 C6 -0.8(5) y
C4 C5 C6 C7 0.2(5) y
C5 C6 C7 C2 0.8(5) y
C5 C6 C7 C8 -177.1(3) y
C3 C2 C7 C6 -1.3(4) y
C1 C2 C7 C6 177.7(3) y
C3 C2 C7 C8 177.0(3) y
C1 C2 C7 C8 -3.9(3) y
C6 C7 C8 C13 -180.0(3) y
C2 C7 C8 C13 1.9(3) y
C6 C7 C8 C9 2.2(6) y
C2 C7 C8 C9 -175.9(3) y
C13 C8 C9 C10 -0.9(4) y
C7 C8 C9 C10 176.8(3) y
C8 C9 C10 C11 0.8(5) y
C9 C10 C11 C12 -0.3(5) y
C10 C11 C12 C13 -0.1(4) y
C11 C12 C13 C8 0.1(4) y
C11 C12 C13 C1 -178.2(3) y
C9 C8 C13 C12 0.4(4) y
C7 C8 C13 C12 -177.7(3) y
C9 C8 C13 C1 179.0(3) y
C7 C8 C13 C1 0.8(3) y
C25 C1 C13 C12 51.1(4) y
C2 C1 C13 C12 175.4(3) y
C14 C1 C13 C12 -64.1(4) y
C25 C1 C13 C8 -127.3(3) y
C2 C1 C13 C8 -2.9(3) y
C14 C1 C13 C8 117.6(3) y
C13 C1 C14 C15 -55.5(4) y
C25 C1 C14 C15 -177.9(3) y
C2 C1 C14 C15 58.5(4) y
C13 C1 C14 C19 123.9(2) y
C25 C1 C14 C19 1.5(3) y
C2 C1 C14 C19 -122.1(2) y
C19 C14 C15 C16 1.0(4) y
C1 C14 C15 C16 -179.6(3) y
C14 C15 C16 C17 -0.2(4) y
C15 C16 C17 C18 -0.4(5) y
C16 C17 C18 C19 0.1(4) y
C17 C18 C19 C14 0.7(4) y
C17 C18 C19 C20 -178.3(3) y
C15 C14 C19 C18 -1.3(4) y
C1 C14 C19 C18 179.3(2) y
C15 C14 C19 C20 177.9(2) y
C1 C14 C19 C20 -1.5(3) y
C18 C19 C20 C21 1.8(5) y
C14 C19 C20 C21 -177.2(3) y
C18 C19 C20 C25 180.0(3) y
C14 C19 C20 C25 0.9(3) y
C25 C20 C21 C22 -0.5(4) y
C19 C20 C21 C22 177.4(3) y
C20 C21 C22 C23 -0.2(5) y
C21 C22 C23 C24 0.9(5) y
C22 C23 C24 C25 -0.8(5) y
C23 C24 C25 C20 0.1(4) y
C23 C24 C25 C1 -177.4(3) y
C21 C20 C25 C24 0.6(4) y
C19 C20 C25 C24 -177.8(2) y
C21 C20 C25 C1 178.4(2) y
C19 C20 C25 C1 0.1(3) y
C13 C1 C25 C24 54.7(4) y
C2 C1 C25 C24 -61.8(4) y
C14 C1 C25 C24 176.7(3) y
C13 C1 C25 C20 -122.9(3) y
C2 C1 C25 C20 120.6(3) y
C14 C1 C25 C20 -0.9(3) y
|
1501639.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/16/1501639.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_1501639
loop_
_publ_author_name
'Ulrich Darbost'
'Janie Cabana'
'Eric Demers'
'Thierry Maris'
'James D. Wuest'
_publ_section_title
;
Molecular Tectonics. Use of Br...aryl Supramolecular Interactions for the
construction of Organized Networks from 9,9'-spirobifluorene in the
Crystalline State.
;
_journal_name_full CheM
_journal_page_first 52
_journal_page_last 12369
_journal_paper_doi 10.5618/chem.2011.v1.n1.7
_journal_volume 1
_journal_year 2011
_chemical_compound_source 'Synthesized by the authors. See text'
_chemical_formula_moiety 'C25 H16, C2 H5 Br'
_chemical_formula_sum 'C27 H21 Br'
_chemical_formula_weight 425.35
_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 90.004(1)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 10.4523(2)
_cell_length_b 17.8465(3)
_cell_length_c 11.0390(2)
_cell_measurement_reflns_used 18828
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 69.03
_cell_measurement_theta_min 4.71
_cell_volume 2059.18(6)
_computing_cell_refinement 'SMART (Bruker, 2003)'
_computing_data_collection 'SMART (Bruker, 2003)'
_computing_data_reduction 'SAINT (Bruker, 2004)'
_computing_molecular_graphics 'SHELXTL (Bruker, 1997)'
_computing_publication_material 'UdMX (local program)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type 'Bruker Smart 6000'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator 'Montel 200 optics'
_diffrn_radiation_source 'Rotating Anode'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.049
_diffrn_reflns_av_sigmaI/netI 0.0260
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 21
_diffrn_reflns_limit_k_min -21
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_number 28205
_diffrn_reflns_theta_full 69.02
_diffrn_reflns_theta_max 69.02
_diffrn_reflns_theta_min 4.71
_diffrn_standards_decay_% 5.64
_diffrn_standards_number 173
_exptl_absorpt_coefficient_mu 2.766
_exptl_absorpt_correction_T_max 0.7800
_exptl_absorpt_correction_T_min 0.5500
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Sadabs (Sheldrick,1996)'
_exptl_crystal_colour Colorless
_exptl_crystal_density_diffrn 1.372
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 872
_exptl_crystal_size_max 0.20
_exptl_crystal_size_mid 0.17
_exptl_crystal_size_min 0.09
_refine_diff_density_max 0.793
_refine_diff_density_min -0.432
_refine_diff_density_rms 0.068
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.068
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 274
_refine_ls_number_reflns 3816
_refine_ls_number_restraints 1
_refine_ls_restrained_S_all 1.068
_refine_ls_R_factor_all 0.0339
_refine_ls_R_factor_gt 0.0332
_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^)+(0.0510P)^2^+1.2090P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0897
_refine_ls_wR_factor_ref 0.0905
_reflns_number_gt 3600
_reflns_number_total 3816
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file deposit.cif
_cod_data_source_block jw1104
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.
'_geom_bond_publ_flag'
value 'Y' changed to 'y' according to the built-in table from CIF
Core dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29
(34 times).
'_geom_angle_publ_flag' value 'Y' changed to 'y'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (48
times).
'_geom_torsion_publ_flag' value 'Y' changed to 'y' according
to the built-in table from CIF Core dictionary named 'cif_core.dic'
version 2.4.1 from 2010-06-29 (76 times).
Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana
;
_cod_original_sg_symbol_H-M P21/n
_cod_database_code 1501639
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.11958(15) 0.25944(9) -0.02006(14) 0.0196(3) Uani 1 1 d . . .
C2 C 0.06959(15) 0.30645(9) 0.08507(15) 0.0198(3) Uani 1 1 d . . .
C3 C 0.00479(16) 0.28191(10) 0.18711(15) 0.0224(4) Uani 1 1 d . . .
H3 H -0.0118 0.2301 0.1995 0.027 Uiso 1 1 calc R . .
C4 C -0.03543(17) 0.33535(11) 0.27129(16) 0.0259(4) Uani 1 1 d . . .
H4 H -0.0802 0.3198 0.3418 0.031 Uiso 1 1 calc R . .
C5 C -0.01077(18) 0.41079(10) 0.25309(18) 0.0282(4) Uani 1 1 d . . .
H5 H -0.0400 0.4463 0.3109 0.034 Uiso 1 1 calc R . .
C6 C 0.05615(17) 0.43559(10) 0.15155(17) 0.0263(4) Uani 1 1 d . . .
H6 H 0.0742 0.4873 0.1402 0.032 Uiso 1 1 calc R . .
C7 C 0.09578(16) 0.38241(10) 0.06708(16) 0.0220(3) Uani 1 1 d . . .
C8 C 0.16235(17) 0.39086(10) -0.04906(16) 0.0232(4) Uani 1 1 d . . .
C9 C 0.20961(18) 0.45450(10) -0.10697(18) 0.0288(4) Uani 1 1 d . . .
H9 H 0.2032 0.5024 -0.0698 0.035 Uiso 1 1 calc R . .
C10 C 0.26621(18) 0.44650(11) -0.22002(18) 0.0320(4) Uani 1 1 d . . .
H10 H 0.2988 0.4894 -0.2605 0.038 Uiso 1 1 calc R . .
C11 C 0.27578(17) 0.37675(12) -0.27469(17) 0.0292(4) Uani 1 1 d . . .
H11 H 0.3140 0.3725 -0.3524 0.035 Uiso 1 1 calc R . .
C12 C 0.22969(16) 0.31263(11) -0.21648(16) 0.0241(4) Uani 1 1 d . . .
H12 H 0.2366 0.2648 -0.2537 0.029 Uiso 1 1 calc R . .
C13 C 0.17359(16) 0.32035(10) -0.10321(15) 0.0207(3) Uani 1 1 d . . .
C14 C 0.01773(16) 0.20917(9) -0.07592(14) 0.0202(3) Uani 1 1 d . . .
C15 C -0.10076(16) 0.22971(10) -0.12196(15) 0.0238(4) Uani 1 1 d . . .
H15 H -0.1266 0.2807 -0.1237 0.029 Uiso 1 1 calc R . .
C16 C -0.18093(17) 0.17335(11) -0.16565(16) 0.0283(4) Uani 1 1 d . . .
H16 H -0.2627 0.1862 -0.1968 0.034 Uiso 1 1 calc R . .
C17 C -0.14313(19) 0.09870(10) -0.16433(18) 0.0289(4) Uani 1 1 d . . .
H17 H -0.1987 0.0614 -0.1958 0.035 Uiso 1 1 calc R . .
C18 C -0.02472(18) 0.07803(11) -0.11742(16) 0.0257(4) Uani 1 1 d . . .
H18 H 0.0009 0.0270 -0.1161 0.031 Uiso 1 1 calc R . .
C19 C 0.05546(16) 0.13381(10) -0.07241(15) 0.0216(3) Uani 1 1 d . . .
C20 C 0.18194(16) 0.12951(10) -0.01411(14) 0.0207(3) Uani 1 1 d . . .
C21 C 0.25960(18) 0.06831(10) 0.01300(16) 0.0254(4) Uani 1 1 d . . .
H21 H 0.2344 0.0190 -0.0089 0.030 Uiso 1 1 calc R . .
C22 C 0.37487(19) 0.08100(11) 0.07281(17) 0.0286(4) Uani 1 1 d . . .
H22 H 0.4289 0.0398 0.0918 0.034 Uiso 1 1 calc R . .
C23 C 0.41206(17) 0.15306(11) 0.10512(16) 0.0277(4) Uani 1 1 d . . .
H23 H 0.4910 0.1606 0.1461 0.033 Uiso 1 1 calc R . .
C24 C 0.33446(16) 0.21436(10) 0.07793(15) 0.0232(4) Uani 1 1 d . . .
H24 H 0.3597 0.2637 0.0999 0.028 Uiso 1 1 calc R . .
C25 C 0.21997(16) 0.20187(9) 0.01822(14) 0.0198(3) Uani 1 1 d . . .
Br1 Br 0.14869(2) 0.093587(12) 0.339014(19) 0.03867(11) Uani 1 1 d . . .
C30 C 0.0520(3) 0.1079(3) 0.4904(3) 0.0412(10) Uani 0.831(10) 1 d PD A 1
H30A H -0.0340 0.1281 0.4714 0.049 Uiso 0.831(10) 1 calc PR A 1
H30B H 0.0408 0.0590 0.5314 0.049 Uiso 0.831(10) 1 calc PR A 1
C31 C 0.1206(4) 0.1610(3) 0.5732(4) 0.0392(10) Uani 0.831(10) 1 d PD A 1
H31A H 0.2048 0.1404 0.5937 0.059 Uiso 0.831(10) 1 calc PR A 1
H31B H 0.0705 0.1678 0.6475 0.059 Uiso 0.831(10) 1 calc PR A 1
H31C H 0.1312 0.2094 0.5327 0.059 Uiso 0.831(10) 1 calc PR A 1
C30B C 0.0555(12) 0.1524(10) 0.4606(10) 0.030(4) Uani 0.169(10) 1 d PD A 2
H30C H 0.0733 0.2063 0.4487 0.037 Uiso 0.169(10) 1 calc PR A 2
H30D H -0.0376 0.1443 0.4509 0.037 Uiso 0.169(10) 1 calc PR A 2
C31B C 0.095(2) 0.1296(13) 0.5843(15) 0.038(5) Uani 0.169(10) 1 d PD A 2
H31D H 0.0859 0.0752 0.5930 0.057 Uiso 0.169(10) 1 calc PR A 2
H31E H 0.0415 0.1550 0.6443 0.057 Uiso 0.169(10) 1 calc PR A 2
H31F H 0.1851 0.1435 0.5973 0.057 Uiso 0.169(10) 1 calc PR 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
C1 0.0165(8) 0.0234(8) 0.0188(8) 0.0007(6) -0.0002(6) 0.0010(6)
C2 0.0148(8) 0.0237(8) 0.0209(8) -0.0010(7) -0.0020(6) 0.0004(6)
C3 0.0179(8) 0.0262(9) 0.0231(8) 0.0005(7) -0.0005(6) -0.0030(6)
C4 0.0195(9) 0.0361(10) 0.0220(8) -0.0033(7) 0.0028(6) -0.0035(7)
C5 0.0216(10) 0.0331(10) 0.0299(10) -0.0113(7) 0.0029(7) -0.0003(7)
C6 0.0220(9) 0.0229(9) 0.0340(10) -0.0044(7) 0.0010(7) -0.0016(7)
C7 0.0164(8) 0.0235(8) 0.0262(9) -0.0005(7) -0.0012(6) -0.0002(6)
C8 0.0170(8) 0.0249(8) 0.0275(9) 0.0028(7) -0.0006(7) 0.0012(6)
C9 0.0256(9) 0.0237(9) 0.0371(10) 0.0056(8) 0.0031(7) 0.0004(7)
C10 0.0252(10) 0.0330(10) 0.0378(11) 0.0157(8) 0.0051(8) 0.0013(7)
C11 0.0214(9) 0.0402(11) 0.0259(9) 0.0098(8) 0.0037(7) 0.0048(8)
C12 0.0199(9) 0.0302(9) 0.0223(8) 0.0029(7) -0.0006(6) 0.0038(7)
C13 0.0157(8) 0.0244(8) 0.0218(8) 0.0038(7) -0.0008(6) 0.0009(6)
C14 0.0200(8) 0.0239(8) 0.0168(7) 0.0012(6) 0.0010(6) -0.0013(6)
C15 0.0209(9) 0.0279(9) 0.0226(8) 0.0031(7) -0.0012(6) 0.0008(7)
C16 0.0212(9) 0.0385(10) 0.0253(9) 0.0045(8) -0.0049(7) -0.0029(7)
C17 0.0268(10) 0.0341(10) 0.0258(9) -0.0012(7) -0.0041(7) -0.0101(7)
C18 0.0289(10) 0.0252(9) 0.0231(9) 0.0004(7) -0.0001(7) -0.0030(7)
C19 0.0218(9) 0.0249(9) 0.0180(8) 0.0007(6) 0.0014(6) -0.0001(7)
C20 0.0205(8) 0.0252(9) 0.0163(7) 0.0011(6) 0.0025(6) 0.0007(6)
C21 0.0282(10) 0.0244(9) 0.0235(8) 0.0029(7) 0.0041(7) 0.0036(7)
C22 0.0266(10) 0.0343(10) 0.0249(9) 0.0071(7) 0.0020(7) 0.0114(7)
C23 0.0199(9) 0.0410(11) 0.0222(8) 0.0024(7) -0.0025(6) 0.0038(7)
C24 0.0199(9) 0.0296(9) 0.0201(8) -0.0006(7) 0.0006(6) -0.0006(7)
C25 0.0184(8) 0.0253(8) 0.0156(7) 0.0018(6) 0.0024(6) 0.0022(6)
Br1 0.04145(17) 0.03980(17) 0.03477(16) -0.00878(8) 0.00210(10) 0.00494(8)
C30 0.0364(15) 0.048(2) 0.0391(17) -0.0064(16) 0.0065(12) -0.0042(13)
C31 0.0371(19) 0.044(2) 0.0364(17) -0.0101(17) -0.0012(13) 0.0043(17)
C30B 0.037(7) 0.030(9) 0.024(6) 0.002(5) 0.011(5) 0.015(5)
C31B 0.040(11) 0.044(12) 0.029(8) -0.002(8) -0.001(6) 0.016(9)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 '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_publ_flag
C14 C1 C2 113.14(13) y
C14 C1 C25 101.30(13) y
C2 C1 C25 113.26(13) y
C14 C1 C13 115.69(13) y
C2 C1 C13 101.08(13) y
C25 C1 C13 112.95(13) y
C3 C2 C7 121.21(16) y
C3 C2 C1 127.78(15) y
C7 C2 C1 111.01(14) y
C2 C3 C4 118.19(16) y
C2 C3 H3 120.9 ?
C4 C3 H3 120.9 ?
C5 C4 C3 120.75(17) y
C5 C4 H4 119.6 ?
C3 C4 H4 119.6 ?
C4 C5 C6 121.24(17) y
C4 C5 H5 119.4 ?
C6 C5 H5 119.4 ?
C5 C6 C7 118.11(17) y
C5 C6 H6 120.9 ?
C7 C6 H6 120.9 ?
C6 C7 C2 120.49(17) y
C6 C7 C8 130.99(17) y
C2 C7 C8 108.49(15) y
C9 C8 C13 120.50(17) y
C9 C8 C7 130.76(18) y
C13 C8 C7 108.73(15) y
C10 C9 C8 118.65(18) y
C10 C9 H9 120.7 ?
C8 C9 H9 120.7 ?
C11 C10 C9 120.94(17) y
C11 C10 H10 119.5 ?
C9 C10 H10 119.5 ?
C10 C11 C12 120.65(18) y
C10 C11 H11 119.7 ?
C12 C11 H11 119.7 ?
C13 C12 C11 118.59(18) y
C13 C12 H12 120.7 ?
C11 C12 H12 120.7 ?
C12 C13 C8 120.66(16) y
C12 C13 C1 128.73(16) y
C8 C13 C1 110.60(14) y
C15 C14 C19 120.95(16) y
C15 C14 C1 128.07(16) y
C19 C14 C1 110.94(14) y
C14 C15 C16 118.18(17) y
C14 C15 H15 120.9 ?
C16 C15 H15 120.9 ?
C17 C16 C15 121.11(17) y
C17 C16 H16 119.4 ?
C15 C16 H16 119.4 ?
C16 C17 C18 120.73(17) y
C16 C17 H17 119.6 ?
C18 C17 H17 119.6 ?
C17 C18 C19 118.58(17) y
C17 C18 H18 120.7 ?
C19 C18 H18 120.7 ?
C18 C19 C14 120.43(16) y
C18 C19 C20 131.21(16) y
C14 C19 C20 108.34(15) y
C21 C20 C25 120.26(16) y
C21 C20 C19 131.13(17) y
C25 C20 C19 108.59(15) y
C22 C21 C20 118.58(17) y
C22 C21 H21 120.7 ?
C20 C21 H21 120.7 ?
C23 C22 C21 120.94(17) y
C23 C22 H22 119.5 ?
C21 C22 H22 119.5 ?
C22 C23 C24 120.53(16) y
C22 C23 H23 119.7 ?
C24 C23 H23 119.7 ?
C25 C24 C23 118.62(17) y
C25 C24 H24 120.7 ?
C23 C24 H24 120.7 ?
C24 C25 C20 121.08(16) y
C24 C25 C1 128.10(16) y
C20 C25 C1 110.82(14) y
C31 C30 BR1 110.7(3) y
C31 C30 H30A 109.5 ?
BR1 C30 H30A 109.5 ?
C31 C30 H30B 109.5 ?
BR1 C30 H30B 109.5 ?
H30A C30 H30B 108.1 ?
C31B C30B BR1 110.10(11) y
C31B C30B H30C 109.6 ?
BR1 C30B H30C 109.6 ?
C31B C30B H30D 109.6 ?
BR1 C30B H30D 109.6 ?
H30C C30B H30D 108.2 ?
C30B C31B H31D 109.5 ?
C30B C31B H31E 109.5 ?
H31D C31B H31E 109.5 ?
C30B C31B H31F 109.5 ?
H31D C31B H31F 109.5 ?
H31E C31B H31F 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
C1 C14 1.523(2) y
C1 C2 1.524(2) y
C1 C25 1.528(2) y
C1 C13 1.531(2) y
C2 C3 1.385(2) y
C2 C7 1.397(2) y
C3 C4 1.396(3) y
C3 H3 0.95 ?
C4 C5 1.385(3) y
C4 H4 0.95 ?
C5 C6 1.393(3) y
C5 H5 0.95 ?
C6 C7 1.394(3) y
C6 H6 0.95 ?
C7 C8 1.467(2) y
C8 C9 1.394(3) y
C8 C13 1.398(3) y
C9 C10 1.389(3) y
C9 H9 0.95 ?
C10 C11 1.387(3) y
C10 H10 0.95 ?
C11 C12 1.398(3) y
C11 H11 0.95 ?
C12 C13 1.388(2) y
C12 H12 0.95 ?
C14 C15 1.388(2) y
C14 C19 1.402(2) y
C15 C16 1.395(3) y
C15 H15 0.95 ?
C16 C17 1.390(3) y
C16 H16 0.95 ?
C17 C18 1.391(3) y
C17 H17 0.95 ?
C18 C19 1.393(3) y
C18 H18 0.95 ?
C19 C20 1.472(2) y
C20 C21 1.393(3) y
C20 C25 1.397(2) y
C21 C22 1.392(3) y
C21 H21 0.95 ?
C22 C23 1.390(3) y
C22 H22 0.95 ?
C23 C24 1.394(3) y
C23 H23 0.95 ?
C24 C25 1.384(2) y
C24 H24 0.95 ?
Br1 C30b 1.962(11) y
Br1 C30 1.970(3) y
C30 C31 1.499(5) y
C30 H30a 0.99 ?
C30 H30b 0.99 ?
C31 H31a 0.98 ?
C31 H31b 0.98 ?
C31 H31c 0.98 ?
C30b C31b 1.484(15) y
C30b H30c 0.99 ?
C30b H30d 0.99 ?
C31b H31d 0.98 ?
C31b H31e 0.98 ?
C31b H31f 0.98 ?
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
C14 C1 C2 C3 52.8(2) y
C25 C1 C2 C3 -61.8(2) y
C13 C1 C2 C3 177.13(16) y
C14 C1 C2 C7 -126.47(15) y
C25 C1 C2 C7 118.98(16) y
C13 C1 C2 C7 -2.14(17) y
C7 C2 C3 C4 0.8(2) y
C1 C2 C3 C4 -178.36(15) y
C2 C3 C4 C5 -0.2(3) y
C3 C4 C5 C6 -0.9(3) y
C4 C5 C6 C7 1.2(3) y
C5 C6 C7 C2 -0.5(3) y
C5 C6 C7 C8 177.36(17) y
C3 C2 C7 C6 -0.5(3) y
C1 C2 C7 C6 178.82(15) y
C3 C2 C7 C8 -178.82(14) y
C1 C2 C7 C8 0.51(19) y
C6 C7 C8 C9 2.6(3) y
C2 C7 C8 C9 -179.29(18) y
C6 C7 C8 C13 -176.50(18) y
C2 C7 C8 C13 1.57(19) y
C13 C8 C9 C10 0.9(3) y
C7 C8 C9 C10 -178.13(17) y
C8 C9 C10 C11 0.0(3) y
C9 C10 C11 C12 -0.7(3) y
C10 C11 C12 C13 0.3(3) y
C11 C12 C13 C8 0.6(3) y
C11 C12 C13 C1 -178.19(16) y
C9 C8 C13 C12 -1.3(3) y
C7 C8 C13 C12 177.99(15) y
C9 C8 C13 C1 177.74(16) y
C7 C8 C13 C1 -3.01(19) y
C14 C1 C13 C12 -55.4(2) y
C2 C1 C13 C12 -177.99(16) y
C25 C1 C13 C12 60.7(2) y
C14 C1 C13 C8 125.70(16) y
C2 C1 C13 C8 3.12(17) y
C25 C1 C13 C8 -118.22(16) y
C2 C1 C14 C15 55.0(2) y
C25 C1 C14 C15 176.60(16) y
C13 C1 C14 C15 -60.9(2) y
C2 C1 C14 C19 -122.61(15) y
C25 C1 C14 C19 -1.06(17) y
C13 C1 C14 C19 121.45(16) y
C19 C14 C15 C16 -0.6(2) y
C1 C14 C15 C16 -178.00(16) y
C14 C15 C16 C17 -0.6(3) y
C15 C16 C17 C18 1.0(3) y
C16 C17 C18 C19 -0.4(3) y
C17 C18 C19 C14 -0.8(3) y
C17 C18 C19 C20 177.51(17) y
C15 C14 C19 C18 1.2(3) y
C1 C14 C19 C18 179.09(15) y
C15 C14 C19 C20 -177.39(15) y
C1 C14 C19 C20 0.46(18) y
C18 C19 C20 C21 0.3(3) y
C14 C19 C20 C21 178.78(17) y
C18 C19 C20 C25 -178.01(18) y
C14 C19 C20 C25 0.42(19) y
C25 C20 C21 C22 0.1(2) y
C19 C20 C21 C22 -178.05(17) y
C20 C21 C22 C23 0.1(3) y
C21 C22 C23 C24 -0.1(3) y
C22 C23 C24 C25 0.0(3) y
C23 C24 C25 C20 0.2(2) y
C23 C24 C25 C1 179.52(16) y
C21 C20 C25 C24 -0.3(2) y
C19 C20 C25 C24 178.27(15) y
C21 C20 C25 C1 -179.70(14) y
C19 C20 C25 C1 -1.14(18) y
C14 C1 C25 C24 -178.02(16) y
C2 C1 C25 C24 -56.6(2) y
C13 C1 C25 C24 57.6(2) y
C14 C1 C25 C20 1.32(17) y
C2 C1 C25 C20 122.79(15) y
C13 C1 C25 C20 -123.05(15) y
|
1501640.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/16/1501640.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_1501640
loop_
_publ_author_name
'Ulrich Darbost'
'Janie Cabana'
'Eric Demers'
'Thierry Maris'
'James D. Wuest'
_publ_section_title
;
Molecular Tectonics. Use of Br...aryl Supramolecular Interactions for the
construction of Organized Networks from 9,9'-spirobifluorene in the
Crystalline State.
;
_journal_name_full CheM
_journal_page_first 52
_journal_page_last 12369
_journal_paper_doi 10.5618/chem.2011.v1.n1.7
_journal_volume 1
_journal_year 2011
_chemical_compound_source 'Synthesized by the authors. See text'
_chemical_formula_moiety 'C25 H16 Br4 N4, C H2 Cl2'
_chemical_formula_sum 'C26 H18 Br4 Cl2 N4'
_chemical_formula_weight 776.98
_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 112.641(18)
_cell_angle_gamma 90.00
_cell_formula_units_Z 8
_cell_length_a 17.865(3)
_cell_length_b 19.788(3)
_cell_length_c 16.886(5)
_cell_measurement_reflns_used 16193
_cell_measurement_temperature 295(2)
_cell_measurement_theta_max 68.91
_cell_measurement_theta_min 2.83
_cell_volume 5509(2)
_computing_cell_refinement 'SMART (Bruker, 1999)'
_computing_data_collection 'SMART (Bruker, 1999)'
_computing_data_reduction 'SAINT (Bruker, 1999)'
_computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)'
_computing_publication_material 'UdMX (local program)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 295(2)
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type 'Bruker AXS Smart 4K/Platform'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'Sealed Tube'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.091
_diffrn_reflns_av_sigmaI/netI 0.0326
_diffrn_reflns_limit_h_max 21
_diffrn_reflns_limit_h_min -21
_diffrn_reflns_limit_k_max 23
_diffrn_reflns_limit_k_min -23
_diffrn_reflns_limit_l_max 20
_diffrn_reflns_limit_l_min -20
_diffrn_reflns_number 29398
_diffrn_reflns_theta_full 68.99
_diffrn_reflns_theta_max 68.99
_diffrn_reflns_theta_min 3.49
_diffrn_standards_decay_% 1.05
_diffrn_standards_number 213
_exptl_absorpt_coefficient_mu 9.108
_exptl_absorpt_correction_T_max 0.9130
_exptl_absorpt_correction_T_min 0.3800
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Sadabs (Sheldrick,1996)'
_exptl_crystal_colour red
_exptl_crystal_density_diffrn 1.873
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 3008
_exptl_crystal_size_max 0.15
_exptl_crystal_size_mid 0.09
_exptl_crystal_size_min 0.01
_refine_diff_density_max 0.840
_refine_diff_density_min -0.774
_refine_diff_density_rms 0.130
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.082
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 326
_refine_ls_number_reflns 5086
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.082
_refine_ls_R_factor_all 0.0717
_refine_ls_R_factor_gt 0.0653
_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^)+(0.1224P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1925
_refine_ls_wR_factor_ref 0.2004
_reflns_number_gt 4234
_reflns_number_total 5086
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file deposit.cif
_cod_data_source_block jiw743
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.
'_geom_bond_publ_flag'
value 'Y' changed to 'y' according to the built-in table from CIF
Core dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29
(42 times).
'_geom_angle_publ_flag' value 'Y' changed to 'y'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (64
times).
'_geom_torsion_publ_flag' value 'Y' changed to 'y' according
to the built-in table from CIF Core dictionary named 'cif_core.dic'
version 2.4.1 from 2010-06-29 (96 times).
Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana
;
_cod_original_sg_symbol_H-M C2/c
_cod_database_code 1501640
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
Br1 Br 0.82930(4) 0.86113(4) -0.36411(4) 0.0810(3) Uani 1 1 d . A 1
Br2 Br 1.17399(4) 1.01849(3) 0.10729(5) 0.0776(3) Uani 1 1 d . A 1
Br3 Br 1.16732(6) 0.47210(4) 0.06458(6) 0.0962(3) Uani 1 1 d . A 1
Br4 Br 0.80658(5) 0.65321(4) 0.21619(5) 0.0909(3) Uani 1 1 d . A 1
C1 C 0.9964(3) 0.7474(2) 0.0005(3) 0.0479(10) Uani 1 1 d . A 1
C2 C 0.9502(3) 0.7680(2) -0.0938(3) 0.0466(10) Uani 1 1 d . A 1
C3 C 0.8986(3) 0.7281(3) -0.1593(3) 0.0532(11) Uani 1 1 d . A 1
H3 H 0.8881 0.6837 -0.1488 0.064 Uiso 1 1 calc . B 1
C4 C 0.8622(3) 0.7556(3) -0.2418(3) 0.0536(11) Uani 1 1 d . A 1
C5 C 0.8814(3) 0.8221(3) -0.2535(3) 0.0562(12) Uani 1 1 d . A 1
C6 C 0.9337(3) 0.8618(3) -0.1882(3) 0.0561(12) Uani 1 1 d . A 1
H6 H 0.9449 0.9060 -0.1987 0.067 Uiso 1 1 calc . C 1
C7 C 0.9691(3) 0.8339(2) -0.1069(3) 0.0492(10) Uani 1 1 d . A 1
C8 C 1.0277(3) 0.8611(2) -0.0263(3) 0.0511(11) Uani 1 1 d . A 1
C9 C 1.0653(3) 0.9236(2) -0.0048(4) 0.0549(11) Uani 1 1 d . A 1
H9 H 1.0532 0.9582 -0.0451 0.066 Uiso 1 1 calc . D 1
C10 C 1.1208(3) 0.9332(3) 0.0775(4) 0.0569(12) Uani 1 1 d . A 1
C11 C 1.1411(3) 0.8833(3) 0.1417(3) 0.0559(11) Uani 1 1 d . A 1
C12 C 1.1014(3) 0.8208(3) 0.1186(3) 0.0546(11) Uani 1 1 d . A 1
H12 H 1.1125 0.7864 0.1591 0.065 Uiso 1 1 calc . E 1
C13 C 1.0466(3) 0.8104(2) 0.0369(3) 0.0481(10) Uani 1 1 d . A 1
C14 C 1.0445(3) 0.6824(2) 0.0110(3) 0.0470(10) Uani 1 1 d . A 1
C15 C 1.1009(3) 0.6680(3) -0.0231(3) 0.0557(12) Uani 1 1 d . A 1
H15 H 1.1143 0.7001 -0.0557 0.067 Uiso 1 1 calc . F 1
C16 C 1.1386(3) 0.6040(3) -0.0082(3) 0.0589(13) Uani 1 1 d . A 1
C17 C 1.1163(3) 0.5583(3) 0.0419(4) 0.0608(13) Uani 1 1 d . A 1
C18 C 1.0586(4) 0.5725(3) 0.0753(4) 0.0627(13) Uani 1 1 d . A 1
H18 H 1.0442 0.5403 0.1069 0.075 Uiso 1 1 calc . G 1
C19 C 1.0227(3) 0.6359(2) 0.0608(3) 0.0510(11) Uani 1 1 d . A 1
C20 C 0.9592(3) 0.6666(2) 0.0848(3) 0.0516(11) Uani 1 1 d . A 1
C21 C 0.9188(4) 0.6431(3) 0.1349(4) 0.0621(13) Uani 1 1 d . A 1
H21 H 0.9303 0.6007 0.1607 0.075 Uiso 1 1 calc . H 1
C22 C 0.8605(3) 0.6849(3) 0.1455(4) 0.0610(13) Uani 1 1 d . A 1
C23 C 0.8407(3) 0.7484(3) 0.1078(3) 0.0578(13) Uani 1 1 d . A 1
C24 C 0.8833(3) 0.7713(3) 0.0588(3) 0.0559(11) Uani 1 1 d . A 1
H24 H 0.8725 0.8138 0.0334 0.067 Uiso 1 1 calc . I 1
C25 C 0.9418(3) 0.7305(2) 0.0481(3) 0.0472(10) Uani 1 1 d . A 1
N1 N 0.8105(3) 0.7165(3) -0.3094(3) 0.0704(13) Uani 1 1 d . A 1
H1A H 0.7895 0.7333 -0.3602 0.106 Uiso 1 1 calc . J 1
H1B H 0.7997 0.6756 -0.3003 0.106 Uiso 1 1 calc . K 1
N2 N 1.2005(3) 0.8926(3) 0.2239(3) 0.0701(13) Uani 1 1 d . A 1
H2A H 1.2127 0.8601 0.2604 0.105 Uiso 1 1 calc . L 1
H2B H 1.2247 0.9309 0.2379 0.105 Uiso 1 1 calc . M 1
N3 N 1.1966(3) 0.5891(3) -0.0409(4) 0.0814(15) Uani 1 1 d . A 1
H3A H 1.2205 0.5504 -0.0306 0.122 Uiso 1 1 calc . N 1
H3B H 1.2088 0.6184 -0.0715 0.122 Uiso 1 1 calc . O 1
N4 N 0.7818(3) 0.7893(3) 0.1193(3) 0.0725(13) Uani 1 1 d . A 1
H4A H 0.7565 0.7754 0.1504 0.109 Uiso 1 1 calc . P 1
H4B H 0.7709 0.8284 0.0952 0.109 Uiso 1 1 calc . Q 1
C30 C 1.0000 0.6016(7) -0.2500 0.122(5) Uani 1 2 d S . 1
H30A H 1.0215 0.6304 -0.1998 0.146 Uiso 0.50 1 calc PR . 1
H30B H 0.9785 0.6304 -0.3002 0.146 Uiso 0.50 1 calc PR . 1
Cl1 Cl 1.0771(2) 0.55255(19) -0.2567(3) 0.1666(14) Uani 1 1 d . R 1
C31 C 1.0000 0.8964(8) 0.2500 0.179(10) Uani 1 2 d S . 1
H31A H 0.9721 0.8677 0.2764 0.215 Uiso 0.50 1 calc PR . 1
H31B H 1.0279 0.8677 0.2236 0.215 Uiso 0.50 1 calc PR . 1
Cl2 Cl 1.0713(4) 0.9472(2) 0.3293(3) 0.218(2) Uani 1 1 d . S 1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Br1 0.0683(4) 0.1088(6) 0.0584(4) 0.0272(3) 0.0162(3) 0.0016(3)
Br2 0.0782(5) 0.0547(4) 0.1038(6) -0.0181(3) 0.0392(4) -0.0088(3)
Br3 0.0985(6) 0.0641(4) 0.1227(7) -0.0024(4) 0.0388(5) 0.0260(4)
Br4 0.1067(6) 0.0949(6) 0.1014(6) -0.0173(4) 0.0736(5) -0.0309(4)
C1 0.046(2) 0.050(2) 0.050(2) 0.003(2) 0.022(2) 0.002(2)
C2 0.044(2) 0.052(2) 0.047(2) 0.0035(19) 0.0203(19) 0.0052(19)
C3 0.049(3) 0.056(3) 0.056(3) 0.000(2) 0.022(2) 0.002(2)
C4 0.045(2) 0.071(3) 0.050(2) 0.002(2) 0.023(2) 0.003(2)
C5 0.045(2) 0.079(3) 0.046(2) 0.015(2) 0.019(2) 0.010(2)
C6 0.054(3) 0.059(3) 0.061(3) 0.012(2) 0.027(2) 0.004(2)
C7 0.045(2) 0.054(3) 0.052(2) 0.003(2) 0.022(2) 0.003(2)
C8 0.049(3) 0.050(3) 0.060(3) 0.002(2) 0.027(2) 0.005(2)
C9 0.057(3) 0.046(2) 0.067(3) 0.000(2) 0.030(2) 0.001(2)
C10 0.054(3) 0.047(2) 0.076(3) -0.014(2) 0.032(2) -0.004(2)
C11 0.053(3) 0.059(3) 0.059(3) -0.010(2) 0.025(2) 0.002(2)
C12 0.053(3) 0.059(3) 0.053(3) 0.000(2) 0.022(2) 0.002(2)
C13 0.043(2) 0.052(2) 0.051(2) -0.0010(19) 0.0207(19) 0.0008(19)
C14 0.041(2) 0.052(2) 0.047(2) -0.0021(19) 0.0145(18) 0.0018(19)
C15 0.054(3) 0.065(3) 0.051(3) -0.002(2) 0.023(2) 0.001(2)
C16 0.050(3) 0.065(3) 0.056(3) -0.013(2) 0.015(2) 0.007(2)
C17 0.057(3) 0.049(3) 0.064(3) -0.009(2) 0.010(2) 0.008(2)
C18 0.066(3) 0.052(3) 0.072(3) 0.003(2) 0.028(3) 0.003(2)
C19 0.051(3) 0.048(2) 0.054(3) -0.0003(19) 0.020(2) -0.001(2)
C20 0.054(3) 0.050(2) 0.054(3) -0.005(2) 0.023(2) -0.005(2)
C21 0.072(3) 0.055(3) 0.067(3) 0.000(2) 0.035(3) -0.011(3)
C22 0.063(3) 0.069(3) 0.061(3) -0.015(2) 0.034(3) -0.017(3)
C23 0.048(3) 0.074(3) 0.054(3) -0.017(2) 0.023(2) -0.006(2)
C24 0.053(3) 0.056(3) 0.057(3) -0.003(2) 0.020(2) 0.004(2)
C25 0.045(2) 0.051(2) 0.047(2) -0.0008(18) 0.0192(19) -0.0004(19)
N1 0.068(3) 0.087(3) 0.050(2) -0.003(2) 0.015(2) -0.008(3)
N2 0.070(3) 0.071(3) 0.062(3) -0.011(2) 0.017(2) -0.011(2)
N3 0.076(3) 0.093(4) 0.085(4) -0.012(3) 0.041(3) 0.018(3)
N4 0.067(3) 0.083(3) 0.079(3) -0.014(3) 0.040(3) 0.005(3)
C30 0.150(13) 0.114(10) 0.098(9) 0.000 0.044(9) 0.000
Cl1 0.162(3) 0.164(3) 0.195(3) -0.078(3) 0.092(3) -0.031(2)
C31 0.26(2) 0.107(11) 0.29(3) 0.000 0.24(2) 0.000
Cl2 0.285(6) 0.181(4) 0.214(5) -0.054(3) 0.126(4) 0.047(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 '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
C14 C1 C13 . . 115.4(4) y
C14 C1 C25 . . 101.6(4) y
C13 C1 C25 . . 111.4(4) y
C14 C1 C2 . . 113.5(4) y
C13 C1 C2 . . 101.5(4) y
C25 C1 C2 . . 114.0(4) y
C3 C2 C7 . . 122.6(4) y
C3 C2 C1 . . 127.1(4) y
C7 C2 C1 . . 110.3(4) y
C2 C3 C4 . . 119.1(5) y
C2 C3 H3 . . 120.5 ?
C4 C3 H3 . . 120.5 ?
C5 C4 N1 . . 122.0(5) y
C5 C4 C3 . . 117.5(5) y
N1 C4 C3 . . 120.4(5) y
C6 C5 C4 . . 123.5(5) y
C6 C5 BR1 . . 118.5(4) y
C4 C5 BR1 . . 118.0(4) y
C5 C6 C7 . . 118.3(5) y
C5 C6 H6 . . 120.9 ?
C7 C6 H6 . . 120.9 ?
C6 C7 C2 . . 119.0(5) y
C6 C7 C8 . . 131.8(5) y
C2 C7 C8 . . 109.2(4) y
C9 C8 C13 . . 119.1(5) y
C9 C8 C7 . . 132.1(5) y
C13 C8 C7 . . 108.7(4) y
C10 C9 C8 . . 118.3(5) y
C10 C9 H9 . . 120.8 ?
C8 C9 H9 . . 120.8 ?
C9 C10 C11 . . 123.6(5) y
C9 C10 BR2 . . 118.7(4) y
C11 C10 BR2 . . 117.6(4) y
N2 C11 C12 . . 120.0(5) y
N2 C11 C10 . . 123.0(5) y
C12 C11 C10 . . 116.9(5) y
C13 C12 C11 . . 120.1(5) y
C13 C12 H12 . . 120 ?
C11 C12 H12 . . 120 ?
C12 C13 C8 . . 121.9(5) y
C12 C13 C1 . . 127.8(5) y
C8 C13 C1 . . 110.3(4) y
C15 C14 C19 . . 122.4(5) y
C15 C14 C1 . . 127.0(5) y
C19 C14 C1 . . 110.5(4) y
C14 C15 C16 . . 119.3(5) y
C14 C15 H15 . . 120.3 ?
C16 C15 H15 . . 120.3 ?
N3 C16 C17 . . 122.5(5) y
N3 C16 C15 . . 120.0(6) y
C17 C16 C15 . . 117.5(5) y
C18 C17 C16 . . 123.2(5) y
C18 C17 BR3 . . 118.4(4) y
C16 C17 BR3 . . 118.4(4) y
C17 C18 C19 . . 118.7(5) y
C17 C18 H18 . . 120.7 ?
C19 C18 H18 . . 120.7 ?
C18 C19 C14 . . 118.9(5) y
C18 C19 C20 . . 132.6(5) y
C14 C19 C20 . . 108.4(4) y
C21 C20 C25 . . 119.9(5) y
C21 C20 C19 . . 131.7(5) y
C25 C20 C19 . . 108.4(4) y
C20 C21 C22 . . 117.9(5) y
C20 C21 H21 . . 121 ?
C22 C21 H21 . . 121 ?
C23 C22 C21 . . 123.2(5) y
C23 C22 BR4 . . 118.9(4) y
C21 C22 BR4 . . 117.9(4) y
C22 C23 N4 . . 122.1(5) y
C22 C23 C24 . . 117.6(5) y
N4 C23 C24 . . 120.2(5) y
C25 C24 C23 . . 119.8(5) y
C25 C24 H24 . . 120.1 ?
C23 C24 H24 . . 120.1 ?
C24 C25 C20 . . 121.6(5) y
C24 C25 C1 . . 127.6(4) y
C20 C25 C1 . . 110.9(4) y
C4 N1 H1A . . 120 ?
C4 N1 H1B . . 120 ?
H1A N1 H1B . . 120 ?
C11 N2 H2A . . 120 ?
C11 N2 H2B . . 120 ?
H2A N2 H2B . . 120 ?
C16 N3 H3A . . 120 ?
C16 N3 H3B . . 120 ?
H3A N3 H3B . . 120 ?
C23 N4 H4A . . 120 ?
C23 N4 H4B . . 120 ?
H4A N4 H4B . . 120 ?
CL1 C30 CL1 2_754 . 111.5(8) y
CL1 C30 H30A 2_754 . 109.3 ?
CL1 C30 H30A . . 109.3 ?
CL1 C30 H30B 2_754 . 109.3 ?
CL1 C30 H30B . . 109.3 ?
H30A C30 H30B . . 108 ?
CL2 C31 CL2 . 2_755 110.5(9) y
CL2 C31 H31A . . 109.5 ?
CL2 C31 H31A 2_755 . 109.5 ?
CL2 C31 H31B . . 109.5 ?
CL2 C31 H31B 2_755 . 109.5 ?
H31A C31 H31B . . 108.1 ?
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
Br1 C5 . 1.902(5) y
Br2 C10 . 1.907(5) y
Br3 C17 . 1.902(5) y
Br4 C22 . 1.905(5) y
C1 C14 . 1.518(6) y
C1 C13 . 1.521(7) y
C1 C25 . 1.522(6) y
C1 C2 . 1.541(6) y
C2 C3 . 1.382(7) y
C2 C7 . 1.387(7) y
C3 C4 . 1.401(7) y
C3 H3 . 0.93 ?
C4 C5 . 1.392(8) y
C4 N1 . 1.394(7) y
C5 C6 . 1.383(8) y
C6 C7 . 1.386(7) y
C6 H6 . 0.93 ?
C7 C8 . 1.463(7) y
C8 C9 . 1.389(7) y
C8 C13 . 1.406(7) y
C9 C10 . 1.375(8) y
C9 H9 . 0.93 ?
C10 C11 . 1.406(8) y
C11 N2 . 1.397(7) y
C11 C12 . 1.404(8) y
C12 C13 . 1.366(7) y
C12 H12 . 0.93 ?
C14 C15 . 1.369(7) y
C14 C19 . 1.400(7) y
C15 C16 . 1.411(8) y
C15 H15 . 0.93 ?
C16 N3 . 1.380(7) y
C16 C17 . 1.397(9) y
C17 C18 . 1.380(8) y
C18 C19 . 1.387(7) y
C18 H18 . 0.93 ?
C19 C20 . 1.474(7) y
C20 C21 . 1.386(8) y
C20 C25 . 1.390(7) y
C21 C22 . 1.396(8) y
C21 H21 . 0.93 ?
C22 C23 . 1.391(8) y
C23 N4 . 1.400(7) y
C23 C24 . 1.400(8) y
C24 C25 . 1.385(7) y
C24 H24 . 0.93 ?
N1 H1A . 0.86 ?
N1 H1B . 0.86 ?
N2 H2A . 0.86 ?
N2 H2B . 0.86 ?
N3 H3A . 0.86 ?
N3 H3B . 0.86 ?
N4 H4A . 0.86 ?
N4 H4B . 0.86 ?
C30 Cl1 2_754 1.723(9) y
C30 Cl1 . 1.723(9) y
C30 H30a . 0.97 ?
C30 H30b . 0.97 ?
C31 Cl2 . 1.764(10) y
C31 Cl2 2_755 1.764(10) y
C31 H31a . 0.97 ?
C31 H31b . 0.97 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1B N2 0.86 2.39 3.114(8) 142.7 8_465
N2 H2A N4 0.86 2.44 3.263(7) 161 2_755
N3 H3B N1 0.86 2.72 3.538(8) 159.6 2_754
N1 H1A BR1 0.86 2.64 3.065(6) 112.2 .
N2 H2B BR2 0.86 2.67 3.096(5) 111.6 .
N3 H3A BR3 0.86 2.66 3.085(7) 112 .
N4 H4A BR4 0.86 2.67 3.093(6) 111.9 .
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
C14 C1 C2 C3 51.3(6) y
C13 C1 C2 C3 175.7(5) y
C25 C1 C2 C3 -64.4(6) y
C14 C1 C2 C7 -126.9(4) y
C13 C1 C2 C7 -2.5(5) y
C25 C1 C2 C7 117.4(4) y
C7 C2 C3 C4 -1.5(7) y
C1 C2 C3 C4 -179.6(4) y
C2 C3 C4 C5 1.0(7) y
C2 C3 C4 N1 179.2(5) y
N1 C4 C5 C6 -178.5(5) y
C3 C4 C5 C6 -0.3(7) y
N1 C4 C5 BR1 4.1(7) y
C3 C4 C5 BR1 -177.7(4) y
C4 C5 C6 C7 0.1(8) y
BR1 C5 C6 C7 177.5(4) y
C5 C6 C7 C2 -0.6(7) y
C5 C6 C7 C8 177.9(5) y
C3 C2 C7 C6 1.3(7) y
C1 C2 C7 C6 179.6(4) y
C3 C2 C7 C8 -177.5(5) y
C1 C2 C7 C8 0.9(5) y
C6 C7 C8 C9 1.7(9) y
C2 C7 C8 C9 -179.7(5) y
C6 C7 C8 C13 -177.3(5) y
C2 C7 C8 C13 1.3(5) y
C13 C8 C9 C10 1.1(7) y
C7 C8 C9 C10 -177.8(5) y
C8 C9 C10 C11 -0.7(8) y
C8 C9 C10 BR2 179.1(4) y
C9 C10 C11 N2 176.8(5) y
BR2 C10 C11 N2 -3.0(7) y
C9 C10 C11 C12 -0.2(8) y
BR2 C10 C11 C12 -180.0(4) y
N2 C11 C12 C13 -176.4(5) y
C10 C11 C12 C13 0.6(7) y
C11 C12 C13 C8 -0.3(8) y
C11 C12 C13 C1 -178.5(5) y
C9 C8 C13 C12 -0.6(7) y
C7 C8 C13 C12 178.5(5) y
C9 C8 C13 C1 177.9(4) y
C7 C8 C13 C1 -3.0(5) y
C14 C1 C13 C12 -55.2(7) y
C25 C1 C13 C12 60.0(6) y
C2 C1 C13 C12 -178.3(5) y
C14 C1 C13 C8 126.4(4) y
C25 C1 C13 C8 -118.4(4) y
C2 C1 C13 C8 3.3(5) y
C13 C1 C14 C15 -62.5(6) y
C25 C1 C14 C15 176.8(5) y
C2 C1 C14 C15 53.9(6) y
C13 C1 C14 C19 118.4(4) y
C25 C1 C14 C19 -2.2(5) y
C2 C1 C14 C19 -125.1(4) y
C19 C14 C15 C16 0.4(7) y
C1 C14 C15 C16 -178.5(4) y
C14 C15 C16 N3 -178.9(5) y
C14 C15 C16 C17 -0.5(7) y
N3 C16 C17 C18 179.7(6) y
C15 C16 C17 C18 1.4(8) y
N3 C16 C17 BR3 -0.7(7) y
C15 C16 C17 BR3 -179.0(4) y
C16 C17 C18 C19 -2.0(8) y
BR3 C17 C18 C19 178.4(4) y
C17 C18 C19 C14 1.8(8) y
C17 C18 C19 C20 178.2(5) y
C15 C14 C19 C18 -1.0(7) y
C1 C14 C19 C18 178.1(4) y
C15 C14 C19 C20 -178.3(4) y
C1 C14 C19 C20 0.8(5) y
C18 C19 C20 C21 5.1(8) y
C14 C19 C20 C21 -178.0(5) y
C18 C19 C20 C25 -175.6(5) y
C14 C19 C20 C25 1.2(6) y
C25 C20 C21 C22 1.0(8) y
C19 C20 C21 C22 -179.9(5) y
C20 C21 C22 C23 0.5(9) y
C20 C21 C22 BR4 -178.8(4) y
C21 C22 C23 N4 179.8(5) y
BR4 C22 C23 N4 -0.9(7) y
C21 C22 C23 C24 -1.6(8) y
BR4 C22 C23 C24 177.7(4) y
C22 C23 C24 C25 1.1(7) y
N4 C23 C24 C25 179.8(5) y
C23 C24 C25 C20 0.3(8) y
C23 C24 C25 C1 -177.4(5) y
C21 C20 C25 C24 -1.4(8) y
C19 C20 C25 C24 179.3(4) y
C21 C20 C25 C1 176.6(5) y
C19 C20 C25 C1 -2.7(5) y
C14 C1 C25 C24 -179.1(5) y
C13 C1 C25 C24 57.5(6) y
C2 C1 C25 C24 -56.6(6) y
C14 C1 C25 C20 3.0(5) y
C13 C1 C25 C20 -120.4(4) y
C2 C1 C25 C20 125.5(4) y
|
1501641.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/16/1501641.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_1501641
loop_
_publ_author_name
'Mohamed Osman Awaleh'
'Idriss Guirreh Farah'
'Elias Said Dirieh'
'Thierry Maris'
'Samatar Mohamed Bouh'
_publ_section_title
;
Synthesis, crystal structures and thermal analysis of two new
coordination polymers.
;
_journal_name_full 'Comptes Rendus Chimie'
_journal_page_first 991
_journal_page_last 996
_journal_paper_doi 10.1016/j.crci.2011.06.002
_journal_volume 14
_journal_year 2011
_chemical_compound_source 'Synthesized by the authors. See text'
_chemical_formula_moiety 'C5 H12 Ag N O3 S2'
_chemical_formula_sum 'C5 H12 Ag N O3 S2'
_chemical_formula_weight 306.15
_chemical_name_systematic
;
?
;
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90
_cell_angle_beta 94.180(1)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 8.3329(1)
_cell_length_b 6.9106(1)
_cell_length_c 17.0680(3)
_cell_measurement_temperature 150
_cell_volume 980.25(3)
_computing_cell_refinement 'SAINT (Bruker AXS, 2010)'
_computing_data_collection 'APEX2 (Bruker AXS, 2010)'
_computing_data_reduction 'SAINT (Bruker AXS, 2010)'
_computing_molecular_graphics 'SHELXTL v6.12 (Bruker AXS, 2001)'
_computing_publication_material 'UdMX (Maris, 2004)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature 150
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type 'Bruker Microstar'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator 'Helios optics'
_diffrn_radiation_source 'Rotating Anode'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.155
_diffrn_reflns_av_sigmaI/netI 0.0681
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 8
_diffrn_reflns_limit_k_min -7
_diffrn_reflns_limit_l_max 20
_diffrn_reflns_limit_l_min -20
_diffrn_reflns_number 12155
_diffrn_reflns_theta_full 68.32
_diffrn_reflns_theta_max 68.32
_diffrn_reflns_theta_min 5.20
_exptl_absorpt_coefficient_mu 20.273
_exptl_absorpt_correction_T_max 0.3629
_exptl_absorpt_correction_T_min 0.1350
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Sadabs (Sheldrick, 2008)'
_exptl_crystal_colour Colorless
_exptl_crystal_density_diffrn 2.074
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 608
_exptl_crystal_size_max 0.14
_exptl_crystal_size_mid 0.09
_exptl_crystal_size_min 0.05
_refine_diff_density_max 1.019
_refine_diff_density_min -1.495
_refine_diff_density_rms 0.190
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.190
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 109
_refine_ls_number_reflns 1764
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.190
_refine_ls_R_factor_all 0.0468
_refine_ls_R_factor_gt 0.0401
_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^)+(0.0669P)^2^+1.9394P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0997
_refine_ls_wR_factor_ref 0.1314
_reflns_number_gt 1599
_reflns_number_total 1764
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file deposit.cif
_cod_data_source_block complex1
_cod_original_sg_symbol_H-M P21/c
_cod_database_code 1501641
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
Ag1 Ag 0.47676(4) 1.13851(6) 0.34042(2) 0.0269(2) Uani 1 1 d .
S1 S 0.65336(14) 0.9842(2) 0.44699(7) 0.0240(4) Uani 1 1 d .
S2 S 0.63325(14) 0.4220(2) 0.27312(7) 0.0238(3) Uani 1 1 d .
O1 O 0.3237(5) 1.4394(8) 0.3758(3) 0.0431(12) Uani 1 1 d .
O2 O 0.1696(5) 1.1865(8) 0.3724(2) 0.0391(11) Uani 1 1 d .
O3 O 0.0769(5) 1.4665(8) 0.4051(3) 0.0479(13) Uani 1 1 d .
N1 N 0.1888(6) 1.3656(8) 0.3849(3) 0.0308(14) Uani 1 1 d .
C11 C 0.7452(7) 1.1723(9) 0.5078(3) 0.0275(13) Uani 1 1 d .
H11A H 0.7987 1.1149 0.5553 0.041 Uiso 1 1 calc R
H11B H 0.6623 1.2632 0.5226 0.041 Uiso 1 1 calc R
H11C H 0.8246 1.2413 0.4787 0.041 Uiso 1 1 calc R
C12 C 0.8313(6) 0.8832(9) 0.4064(3) 0.0282(14) Uani 1 1 d .
H12A H 0.9021 0.9898 0.3913 0.034 Uiso 1 1 calc R
H12B H 0.8918 0.8045 0.4470 0.034 Uiso 1 1 calc R
C13 C 0.7861(6) 0.7568(9) 0.3343(3) 0.0274(13) Uani 1 1 d .
H13A H 0.7238 0.8349 0.2941 0.033 Uiso 1 1 calc R
H13B H 0.8854 0.7119 0.3115 0.033 Uiso 1 1 calc R
C14 C 0.6875(6) 0.5834(10) 0.3555(3) 0.0286(13) Uani 1 1 d .
H14A H 0.5876 0.6297 0.3775 0.034 Uiso 1 1 calc R
H14B H 0.7491 0.5089 0.3971 0.034 Uiso 1 1 calc R
C21 C 0.8256(7) 0.3286(10) 0.2484(3) 0.0297(13) Uani 1 1 d .
H21A H 0.8903 0.4341 0.2288 0.045 Uiso 1 1 calc R
H21B H 0.8089 0.2291 0.2077 0.045 Uiso 1 1 calc R
H21C H 0.8821 0.2719 0.2953 0.045 Uiso 1 1 calc R
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ag1 0.0192(3) 0.0312(5) 0.0290(3) -0.00080(14) -0.0062(2) 0.00071(13)
S1 0.0172(6) 0.0322(9) 0.0219(6) -0.0029(5) -0.0035(5) -0.0012(5)
S2 0.0164(6) 0.0296(9) 0.0246(6) -0.0007(6) -0.0029(5) -0.0009(5)
O1 0.023(2) 0.044(3) 0.062(3) -0.010(3) 0.006(2) -0.006(2)
O2 0.043(3) 0.037(3) 0.036(2) -0.004(2) -0.0020(19) -0.001(2)
O3 0.023(2) 0.057(4) 0.064(3) -0.017(3) 0.000(2) 0.007(2)
N1 0.021(2) 0.047(4) 0.024(2) -0.001(2) -0.005(2) 0.0012(19)
C11 0.033(3) 0.018(3) 0.030(3) -0.006(2) -0.008(2) -0.003(2)
C12 0.012(2) 0.042(4) 0.030(3) -0.006(2) -0.003(2) 0.001(2)
C13 0.015(2) 0.036(4) 0.030(3) 0.002(2) -0.001(2) 0.002(2)
C14 0.016(2) 0.047(4) 0.022(2) 0.001(3) 0.000(2) -0.002(2)
C21 0.020(3) 0.039(4) 0.029(3) 0.005(3) 0.000(2) 0.004(2)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag 0.1306 4.2820 '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
S1 AG1 O1 . . 117.22(11) y
S1 AG1 S2 . 2_655 117.45(5) y
O1 AG1 S2 . 2_655 120.02(10) y
S1 AG1 S2 . 1_565 110.37(4) y
O1 AG1 S2 . 1_565 76.69(11) y
S2 AG1 S2 2_655 1_565 105.24(2) y
C11 S1 C12 . . 99.9(3) y
C11 S1 AG1 . . 108.4(2) y
C12 S1 AG1 . . 109.88(19) y
C21 S2 C14 . . 103.0(3) y
C21 S2 AG1 . 2_645 107.9(2) y
C14 S2 AG1 . 2_645 106.3(2) y
C21 S2 AG1 . 1_545 108.0(2) y
C14 S2 AG1 . 1_545 102.6(2) y
AG1 S2 AG1 2_645 1_545 126.62(5) y
N1 O1 AG1 . . 99.6(4) y
O3 N1 O1 . . 120.5(6) y
O3 N1 O2 . . 120.7(5) y
O1 N1 O2 . . 118.8(5) y
S1 C11 H11A . . 109.5 ?
S1 C11 H11B . . 109.5 ?
H11A C11 H11B . . 109.5 ?
S1 C11 H11C . . 109.5 ?
H11A C11 H11C . . 109.5 ?
H11B C11 H11C . . 109.5 ?
C13 C12 S1 . . 111.4(4) y
C13 C12 H12A . . 109.4 ?
S1 C12 H12A . . 109.4 ?
C13 C12 H12B . . 109.4 ?
S1 C12 H12B . . 109.4 ?
H12A C12 H12B . . 108.0 ?
C14 C13 C12 . . 111.5(5) y
C14 C13 H13A . . 109.3 ?
C12 C13 H13A . . 109.3 ?
C14 C13 H13B . . 109.3 ?
C12 C13 H13B . . 109.3 ?
H13A C13 H13B . . 108.0 ?
C13 C14 S2 . . 114.1(4) y
C13 C14 H14A . . 108.7 ?
S2 C14 H14A . . 108.7 ?
C13 C14 H14B . . 108.7 ?
S2 C14 H14B . . 108.7 ?
H14A C14 H14B . . 107.6 ?
S2 C21 H21A . . 109.5 ?
S2 C21 H21B . . 109.5 ?
H21A C21 H21B . . 109.5 ?
S2 C21 H21C . . 109.5 ?
H21A C21 H21C . . 109.5 ?
H21B C21 H21C . . 109.5 ?
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
Ag1 S1 . 2.4942(12) y
Ag1 O1 . 2.535(5) y
Ag1 S2 2_655 2.5644(14) y
Ag1 S2 1_565 2.6600(15) y
S1 C11 . 1.799(5) y
S1 C12 . 1.820(6) y
S2 C21 . 1.806(6) y
S2 C14 . 1.826(6) y
S2 Ag1 2_645 2.5643(14) y
S2 Ag1 1_545 2.6600(15) y
O1 N1 . 1.254(7) y
O2 N1 . 1.264(6) y
O3 N1 . 1.234(7) y
C11 H11a . 0.9800 ?
C11 H11b . 0.9800 ?
C11 H11c . 0.9800 ?
C12 C13 . 1.533(8) y
C12 H12a . 0.9900 ?
C12 H12b . 0.9900 ?
C13 C14 . 1.512(9) y
C13 H13a . 0.9900 ?
C13 H13b . 0.9900 ?
C14 H14a . 0.9900 ?
C14 H14b . 0.9900 ?
C21 H21a . 0.9800 ?
C21 H21b . 0.9800 ?
C21 H21c . 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_site_symmetry_1
_geom_torsion
_geom_torsion_publ_flag
O1 AG1 S1 C11 . -37.0(3) y
S2 AG1 S1 C11 2_655 168.7(2) y
S2 AG1 S1 C11 1_565 48.1(2) y
O1 AG1 S1 C12 . -145.3(2) y
S2 AG1 S1 C12 2_655 60.4(2) y
S2 AG1 S1 C12 1_565 -60.2(2) y
S1 AG1 O1 N1 . -99.6(3) y
S2 AG1 O1 N1 2_655 54.0(4) y
S2 AG1 O1 N1 1_565 154.1(3) y
AG1 O1 N1 O3 . 178.1(4) y
AG1 O1 N1 O2 . -2.3(5) y
C11 S1 C12 C13 . -163.8(4) y
AG1 S1 C12 C13 . -50.0(5) y
S1 C12 C13 C14 . -63.1(6) y
C12 C13 C14 S2 . -178.5(4) y
C21 S2 C14 C13 . 65.3(5) y
AG1 S2 C14 C13 2_645 -47.9(4) y
AG1 S2 C14 C13 1_545 177.4(4) y
|
1501642.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/16/1501642.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_1501642
loop_
_publ_author_name
'Mohamed Osman Awaleh'
'Idriss Guirreh Farah'
'Elias Said Dirieh'
'Thierry Maris'
'Samatar Mohamed Bouh'
_publ_section_title
;
Synthesis, crystal structures and thermal analysis of two new
coordination polymers.
;
_journal_name_full 'Comptes Rendus Chimie'
_journal_page_first 991
_journal_page_last 996
_journal_paper_doi 10.1016/j.crci.2011.06.002
_journal_volume 14
_journal_year 2011
_chemical_compound_source 'Synthesized by the authors. See text'
_chemical_formula_moiety 'C16 H24 Ag2 F10 O4 S4'
_chemical_formula_sum 'C16 H24 Ag2 F10 O4 S4'
_chemical_formula_weight 814.33
_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
_cell_angle_beta 93.532(1)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 8.0030(2)
_cell_length_b 20.5242(4)
_cell_length_c 15.8557(3)
_cell_measurement_temperature 100
_cell_volume 2599.43(10)
_computing_cell_refinement 'SAINT (Bruker AXS, 2010)'
_computing_data_collection 'APEX2 (Bruker AXS, 2010)'
_computing_data_reduction 'SAINT (Bruker AXS, 2010)'
_computing_molecular_graphics 'SHELXTL v6.12 (Bruker AXS, 2001)'
_computing_publication_material 'UdMX (Maris, 2004)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature 100
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type 'Bruker Microstar'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator 'Helios optics'
_diffrn_radiation_source 'Rotating Anode'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.051
_diffrn_reflns_av_sigmaI/netI 0.0246
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 24
_diffrn_reflns_limit_k_min -24
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_number 34580
_diffrn_reflns_theta_full 68.80
_diffrn_reflns_theta_max 68.80
_diffrn_reflns_theta_min 3.53
_exptl_absorpt_coefficient_mu 15.993
_exptl_absorpt_correction_T_max 0.3831
_exptl_absorpt_correction_T_min 0.1788
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Sadabs (Sheldrick, 2008)'
_exptl_crystal_colour Colorless
_exptl_crystal_density_diffrn 2.081
_exptl_crystal_description block
_exptl_crystal_F_000 1600
_exptl_crystal_size_max 0.14
_exptl_crystal_size_mid 0.09
_exptl_crystal_size_min 0.06
_refine_diff_density_max 0.836
_refine_diff_density_min -0.436
_refine_diff_density_rms 0.099
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.979
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 329
_refine_ls_number_reflns 4779
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.979
_refine_ls_R_factor_all 0.0270
_refine_ls_R_factor_gt 0.0247
_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^)+(0.0455P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0627
_refine_ls_wR_factor_ref 0.0638
_reflns_number_gt 4351
_reflns_number_total 4779
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file deposit.cif
_cod_data_source_block complex2
_cod_original_sg_symbol_H-M P21/n
_cod_database_code 1501642
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
Ag1 Ag 0.92851(2) 0.171375(9) 0.742949(12) 0.01866(7) Uani 1 1 d .
Ag2 Ag 0.45755(2) 0.110904(9) 0.593916(12) 0.01845(7) Uani 1 1 d .
S1 S 1.21753(8) 0.19137(3) 0.68900(4) 0.01774(14) Uani 1 1 d .
S2 S 1.81126(8) 0.16346(3) 0.88583(4) 0.01884(14) Uani 1 1 d .
S3 S 0.78206(8) 0.09227(3) 0.63136(4) 0.01648(13) Uani 1 1 d .
S4 S 0.63035(8) -0.16547(3) 0.53871(4) 0.01658(14) Uani 1 1 d .
F1 F 0.4317(2) -0.08369(8) 0.77587(11) 0.0308(4) Uani 1 1 d .
F2 F 0.1655(2) -0.09165(8) 0.73906(11) 0.0326(4) Uani 1 1 d .
F3 F 0.1182(2) 0.02450(11) 0.82709(12) 0.0447(5) Uani 1 1 d .
F4 F 0.3739(2) 0.01752(9) 0.87720(11) 0.0326(4) Uani 1 1 d .
F5 F 0.2030(3) -0.05958(10) 0.89876(11) 0.0438(5) Uani 1 1 d .
F6 F 0.6897(2) 0.39469(8) 0.67368(11) 0.0306(4) Uani 1 1 d .
F7 F 0.5143(2) 0.33793(9) 0.59322(13) 0.0340(4) Uani 1 1 d .
F8 F 0.9176(2) 0.38534(9) 0.54844(13) 0.0372(5) Uani 1 1 d .
F9 F 0.7252(2) 0.34146(9) 0.46657(11) 0.0349(4) Uani 1 1 d .
F10 F 0.6849(3) 0.43610(9) 0.51852(12) 0.0395(5) Uani 1 1 d .
O1 O 0.4278(2) 0.04083(9) 0.70447(12) 0.0203(4) Uani 1 1 d .
O2 O 0.2252(3) -0.00585(10) 0.62161(12) 0.0266(4) Uani 1 1 d .
O3 O 0.8150(2) 0.28127(10) 0.71976(13) 0.0255(4) Uani 1 1 d .
O4 O 0.7584(3) 0.23978(10) 0.59059(15) 0.0360(5) Uani 1 1 d .
C1 C 0.3143(3) 0.00038(12) 0.68670(16) 0.0163(5) Uani 1 1 d .
C2 C 0.2896(3) -0.04868(13) 0.75959(18) 0.0199(6) Uani 1 1 d .
C3 C 0.2465(4) -0.01608(15) 0.84242(18) 0.0246(6) Uani 1 1 d .
C4 C 0.7603(3) 0.28270(13) 0.64459(18) 0.0206(6) Uani 1 1 d .
C5 C 0.6798(3) 0.34782(14) 0.61350(17) 0.0195(6) Uani 1 1 d .
C6 C 0.7527(4) 0.37796(14) 0.53541(19) 0.0233(6) Uani 1 1 d .
C11 C 1.1721(4) 0.26232(14) 0.6234(2) 0.0255(6) Uani 1 1 d .
H11A H 1.1317 0.2977 0.6582 0.038 Uiso 1 1 calc R
H11B H 1.0859 0.2513 0.5791 0.038 Uiso 1 1 calc R
H11C H 1.2741 0.2763 0.5973 0.038 Uiso 1 1 calc R
C12 C 1.3574(3) 0.22657(15) 0.77301(19) 0.0260(6) Uani 1 1 d .
H12A H 1.3993 0.2693 0.7545 0.031 Uiso 1 1 calc R
H12B H 1.2949 0.2336 0.8242 0.031 Uiso 1 1 calc R
C13 C 1.5034(3) 0.18136(13) 0.79356(18) 0.0184(5) Uani 1 1 d .
H13A H 1.5716 0.1777 0.7437 0.022 Uiso 1 1 calc R
H13B H 1.4607 0.1374 0.8064 0.022 Uiso 1 1 calc R
C14 C 1.6126(3) 0.20594(13) 0.86855(17) 0.0194(6) Uani 1 1 d .
H14A H 1.5496 0.2018 0.9201 0.023 Uiso 1 1 calc R
H14B H 1.6354 0.2528 0.8602 0.023 Uiso 1 1 calc R
C21 C 1.7420(4) 0.07985(14) 0.89578(19) 0.0262(6) Uani 1 1 d .
H21A H 1.6709 0.0763 0.9437 0.039 Uiso 1 1 calc R
H21B H 1.8396 0.0513 0.9051 0.039 Uiso 1 1 calc R
H21C H 1.6780 0.0667 0.8439 0.039 Uiso 1 1 calc R
C31 C 0.9122(3) 0.09983(13) 0.54240(18) 0.0199(6) Uani 1 1 d .
H31A H 1.0266 0.0860 0.5594 0.030 Uiso 1 1 calc R
H31B H 0.9132 0.1453 0.5237 0.030 Uiso 1 1 calc R
H31C H 0.8672 0.0722 0.4960 0.030 Uiso 1 1 calc R
C32 C 0.8048(3) 0.00574(12) 0.65505(17) 0.0181(5) Uani 1 1 d .
H32A H 0.9249 -0.0060 0.6567 0.022 Uiso 1 1 calc R
H32B H 0.7640 -0.0028 0.7117 0.022 Uiso 1 1 calc R
C33 C 0.7088(3) -0.03728(12) 0.59043(16) 0.0161(5) Uani 1 1 d .
H33A H 0.7407 -0.0260 0.5329 0.019 Uiso 1 1 calc R
H33B H 0.5871 -0.0296 0.5930 0.019 Uiso 1 1 calc R
C34 C 0.7477(3) -0.10885(12) 0.60844(18) 0.0183(6) Uani 1 1 d .
H34A H 0.7232 -0.1186 0.6676 0.022 Uiso 1 1 calc R
H34B H 0.8689 -0.1162 0.6031 0.022 Uiso 1 1 calc R
C41 C 0.4392(4) -0.17428(14) 0.59275(18) 0.0226(6) Uani 1 1 d .
H41A H 0.4656 -0.1906 0.6501 0.034 Uiso 1 1 calc R
H41B H 0.3647 -0.2051 0.5618 0.034 Uiso 1 1 calc R
H41C H 0.3835 -0.1319 0.5956 0.034 Uiso 1 1 calc R
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ag1 0.01679(11) 0.01790(11) 0.02073(12) 0.00226(7) -0.00323(8) -0.00028(7)
Ag2 0.02206(12) 0.01752(11) 0.01498(11) 0.00243(7) -0.00520(8) -0.00152(7)
S1 0.0139(3) 0.0194(3) 0.0191(3) -0.0029(2) -0.0061(2) 0.0008(2)
S2 0.0164(3) 0.0215(3) 0.0176(3) -0.0001(2) -0.0069(2) 0.0001(2)
S3 0.0156(3) 0.0147(3) 0.0186(3) -0.0016(2) -0.0037(2) -0.0018(2)
S4 0.0202(3) 0.0124(3) 0.0164(3) 0.0002(2) -0.0041(2) 0.0014(2)
F1 0.0352(10) 0.0251(9) 0.0313(10) 0.0079(7) -0.0049(8) 0.0109(7)
F2 0.0411(10) 0.0280(9) 0.0279(9) 0.0016(7) -0.0057(8) -0.0199(8)
F3 0.0359(11) 0.0671(14) 0.0314(10) -0.0067(10) 0.0050(8) 0.0208(10)
F4 0.0365(10) 0.0409(10) 0.0201(8) -0.0078(8) -0.0012(7) -0.0186(8)
F5 0.0575(13) 0.0535(12) 0.0205(9) 0.0049(9) 0.0020(8) -0.0297(10)
F6 0.0476(11) 0.0216(9) 0.0223(9) -0.0033(7) -0.0003(8) 0.0096(8)
F7 0.0151(8) 0.0376(10) 0.0486(12) 0.0092(8) -0.0044(8) 0.0016(7)
F8 0.0273(10) 0.0460(11) 0.0380(11) 0.0066(9) 0.0001(8) -0.0119(8)
F9 0.0477(11) 0.0356(10) 0.0207(9) -0.0058(8) -0.0034(8) -0.0012(8)
F10 0.0615(13) 0.0250(9) 0.0320(10) 0.0117(8) 0.0034(9) 0.0111(9)
O1 0.0224(10) 0.0182(9) 0.0199(10) 0.0025(8) -0.0023(7) -0.0042(8)
O2 0.0269(11) 0.0335(11) 0.0185(10) 0.0028(8) -0.0072(8) -0.0018(9)
O3 0.0272(11) 0.0236(10) 0.0250(11) 0.0058(8) -0.0027(9) 0.0036(8)
O4 0.0469(14) 0.0205(11) 0.0391(13) -0.0052(10) -0.0102(11) 0.0091(10)
C1 0.0160(13) 0.0158(12) 0.0171(13) -0.0003(10) 0.0002(10) 0.0047(10)
C2 0.0206(14) 0.0173(13) 0.0209(14) 0.0001(11) -0.0056(11) -0.0036(11)
C3 0.0237(15) 0.0310(16) 0.0190(14) 0.0023(12) 0.0003(11) -0.0074(12)
C4 0.0143(13) 0.0185(13) 0.0285(15) 0.0015(12) -0.0028(11) 0.0002(11)
C5 0.0154(13) 0.0214(13) 0.0212(14) -0.0010(11) -0.0039(10) 0.0021(11)
C6 0.0256(15) 0.0201(13) 0.0237(15) 0.0003(11) -0.0017(12) 0.0010(11)
C11 0.0245(15) 0.0216(14) 0.0302(16) 0.0031(12) -0.0005(12) -0.0008(12)
C12 0.0193(14) 0.0303(16) 0.0271(15) -0.0125(12) -0.0085(12) 0.0045(12)
C13 0.0149(13) 0.0177(13) 0.0221(14) -0.0037(11) -0.0046(11) 0.0011(10)
C14 0.0152(13) 0.0213(13) 0.0208(14) -0.0042(11) -0.0051(11) 0.0010(11)
C21 0.0288(16) 0.0231(15) 0.0264(15) 0.0069(12) -0.0003(12) 0.0005(12)
C31 0.0196(14) 0.0190(13) 0.0209(14) -0.0014(11) 0.0001(11) -0.0040(11)
C32 0.0194(13) 0.0147(12) 0.0194(13) 0.0009(10) -0.0056(10) -0.0013(10)
C33 0.0167(13) 0.0143(13) 0.0167(12) -0.0018(10) -0.0047(10) 0.0009(10)
C34 0.0181(14) 0.0175(13) 0.0184(13) 0.0005(10) -0.0059(11) 0.0002(10)
C41 0.0219(15) 0.0260(15) 0.0195(14) 0.0015(11) -0.0025(11) -0.0052(11)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag 0.1306 4.2820 '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
O3 AG1 S2 . 1_455 92.24(5) y
O3 AG1 S1 . . 97.89(5) y
S2 AG1 S1 1_455 . 135.31(2) y
O3 AG1 S3 . . 108.80(5) y
S2 AG1 S3 1_455 . 113.09(2) y
S1 AG1 S3 . . 104.49(2) y
O1 AG2 S4 . 3_656 155.06(5) y
O1 AG2 S3 . . 83.39(5) y
S4 AG2 S3 3_656 . 118.91(2) y
C11 S1 C12 . . 101.09(14) y
C11 S1 AG1 . . 99.66(10) y
C12 S1 AG1 . . 110.22(10) y
C21 S2 C14 . . 101.41(13) y
C21 S2 AG1 . 1_655 105.84(10) y
C14 S2 AG1 . 1_655 101.82(9) y
C31 S3 C32 . . 100.91(13) y
C31 S3 AG1 . . 102.58(9) y
C32 S3 AG1 . . 115.43(9) y
C31 S3 AG2 . . 114.51(9) y
C32 S3 AG2 . . 105.68(9) y
AG1 S3 AG2 . . 116.85(2) y
C41 S4 C34 . . 101.28(13) y
C41 S4 AG2 . 3_656 104.25(10) y
C34 S4 AG2 . 3_656 109.83(9) y
C1 O1 AG2 . . 110.65(16) y
C4 O3 AG1 . . 105.69(17) y
O2 C1 O1 . . 129.6(3) y
O2 C1 C2 . . 117.7(2) y
O1 C1 C2 . . 112.7(2) y
F2 C2 F1 . . 107.1(2) y
F2 C2 C3 . . 106.9(2) y
F1 C2 C3 . . 107.4(2) y
F2 C2 C1 . . 111.6(2) y
F1 C2 C1 . . 109.9(2) y
C3 C2 C1 . . 113.6(2) y
F4 C3 F5 . . 107.3(2) y
F4 C3 F3 . . 108.4(3) y
F5 C3 F3 . . 108.2(2) y
F4 C3 C2 . . 112.1(2) y
F5 C3 C2 . . 111.5(2) y
F3 C3 C2 . . 109.1(2) y
O4 C4 O3 . . 129.8(3) y
O4 C4 C5 . . 114.2(2) y
O3 C4 C5 . . 116.1(2) y
F6 C5 F7 . . 106.7(2) y
F6 C5 C6 . . 105.9(2) y
F7 C5 C6 . . 106.5(2) y
F6 C5 C4 . . 112.5(2) y
F7 C5 C4 . . 109.0(2) y
C6 C5 C4 . . 115.7(2) y
F9 C6 F10 . . 107.1(2) y
F9 C6 F8 . . 107.7(2) y
F10 C6 F8 . . 108.5(2) y
F9 C6 C5 . . 112.6(2) y
F10 C6 C5 . . 110.7(2) y
F8 C6 C5 . . 110.1(2) y
S1 C11 H11A . . 109.5 ?
S1 C11 H11B . . 109.5 ?
H11A C11 H11B . . 109.5 ?
S1 C11 H11C . . 109.5 ?
H11A C11 H11C . . 109.5 ?
H11B C11 H11C . . 109.5 ?
C13 C12 S1 . . 110.11(19) y
C13 C12 H12A . . 109.6 ?
S1 C12 H12A . . 109.6 ?
C13 C12 H12B . . 109.6 ?
S1 C12 H12B . . 109.6 ?
H12A C12 H12B . . 108.2 ?
C12 C13 C14 . . 111.4(2) y
C12 C13 H13A . . 109.3 ?
C14 C13 H13A . . 109.3 ?
C12 C13 H13B . . 109.3 ?
C14 C13 H13B . . 109.3 ?
H13A C13 H13B . . 108.0 ?
C13 C14 S2 . . 114.48(19) y
C13 C14 H14A . . 108.6 ?
S2 C14 H14A . . 108.6 ?
C13 C14 H14B . . 108.6 ?
S2 C14 H14B . . 108.6 ?
H14A C14 H14B . . 107.6 ?
S2 C21 H21A . . 109.5 ?
S2 C21 H21B . . 109.5 ?
H21A C21 H21B . . 109.5 ?
S2 C21 H21C . . 109.5 ?
H21A C21 H21C . . 109.5 ?
H21B C21 H21C . . 109.5 ?
S3 C31 H31A . . 109.5 ?
S3 C31 H31B . . 109.5 ?
H31A C31 H31B . . 109.5 ?
S3 C31 H31C . . 109.5 ?
H31A C31 H31C . . 109.5 ?
H31B C31 H31C . . 109.5 ?
C33 C32 S3 . . 112.74(18) y
C33 C32 H32A . . 109.0 ?
S3 C32 H32A . . 109.0 ?
C33 C32 H32B . . 109.0 ?
S3 C32 H32B . . 109.0 ?
H32A C32 H32B . . 107.8 ?
C32 C33 C34 . . 110.1(2) y
C32 C33 H33A . . 109.6 ?
C34 C33 H33A . . 109.6 ?
C32 C33 H33B . . 109.6 ?
C34 C33 H33B . . 109.6 ?
H33A C33 H33B . . 108.2 ?
C33 C34 S4 . . 114.11(18) y
C33 C34 H34A . . 108.7 ?
S4 C34 H34A . . 108.7 ?
C33 C34 H34B . . 108.7 ?
S4 C34 H34B . . 108.7 ?
H34A C34 H34B . . 107.6 ?
S4 C41 H41A . . 109.5 ?
S4 C41 H41B . . 109.5 ?
H41A C41 H41B . . 109.5 ?
S4 C41 H41C . . 109.5 ?
H41A C41 H41C . . 109.5 ?
H41B C41 H41C . . 109.5 ?
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
Ag1 O3 . 2.451(2) y
Ag1 S2 1_455 2.5102(7) y
Ag1 S1 . 2.5484(7) y
Ag1 S3 . 2.6239(6) y
Ag2 O1 . 2.2911(18) y
Ag2 S4 3_656 2.4471(6) y
Ag2 S3 . 2.6558(6) y
S1 C11 . 1.813(3) y
S1 C12 . 1.835(3) y
S2 C21 . 1.813(3) y
S2 C14 . 1.819(3) y
S2 Ag1 1_655 2.5101(7) y
S3 C31 . 1.811(3) y
S3 C32 . 1.822(3) y
S4 C41 . 1.808(3) y
S4 C34 . 1.824(3) y
S4 Ag2 3_656 2.4473(6) y
F1 C2 . 1.357(3) y
F2 C2 . 1.353(3) y
F3 C3 . 1.333(4) y
F4 C3 . 1.323(3) y
F5 C3 . 1.324(3) y
F6 C5 . 1.354(3) y
F7 C5 . 1.359(3) y
F8 C6 . 1.331(3) y
F9 C6 . 1.331(3) y
F10 C6 . 1.331(3) y
O1 C1 . 1.250(3) y
O2 C1 . 1.224(3) y
O3 C4 . 1.244(3) y
O4 C4 . 1.228(4) y
C1 C2 . 1.555(4) y
C2 C3 . 1.532(4) y
C4 C5 . 1.551(4) y
C5 C6 . 1.531(4) y
C11 H11a . 0.9800 ?
C11 H11b . 0.9800 ?
C11 H11c . 0.9800 ?
C12 C13 . 1.512(4) y
C12 H12a . 0.9900 ?
C12 H12b . 0.9900 ?
C13 C14 . 1.518(4) y
C13 H13a . 0.9900 ?
C13 H13b . 0.9900 ?
C14 H14a . 0.9900 ?
C14 H14b . 0.9900 ?
C21 H21a . 0.9800 ?
C21 H21b . 0.9800 ?
C21 H21c . 0.9800 ?
C31 H31a . 0.9800 ?
C31 H31b . 0.9800 ?
C31 H31c . 0.9800 ?
C32 C33 . 1.524(3) y
C32 H32a . 0.9900 ?
C32 H32b . 0.9900 ?
C33 C34 . 1.525(3) y
C33 H33a . 0.9900 ?
C33 H33b . 0.9900 ?
C34 H34a . 0.9900 ?
C34 H34b . 0.9900 ?
C41 H41a . 0.9800 ?
C41 H41b . 0.9800 ?
C41 H41c . 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_site_symmetry_1
_geom_torsion
_geom_torsion_publ_flag
O3 AG1 S1 C11 . -21.68(11) y
S2 AG1 S1 C11 1_455 -123.00(10) y
S3 AG1 S1 C11 . 90.15(10) y
O3 AG1 S1 C12 . 84.02(11) y
S2 AG1 S1 C12 1_455 -17.30(11) y
S3 AG1 S1 C12 . -164.15(11) y
O3 AG1 S3 C31 . 87.51(11) y
S2 AG1 S3 C31 1_455 -171.53(9) y
S1 AG1 S3 C31 . -16.24(10) y
O3 AG1 S3 C32 . -163.78(11) y
S2 AG1 S3 C32 1_455 -62.82(10) y
S1 AG1 S3 C32 . 92.47(10) y
O3 AG1 S3 AG2 . -38.61(6) y
S2 AG1 S3 AG2 1_455 62.35(3) y
S1 AG1 S3 AG2 . -142.36(3) y
O1 AG2 S3 C31 . 150.86(11) y
S4 AG2 S3 C31 3_656 -17.31(10) y
O1 AG2 S3 C32 . 40.73(10) y
S4 AG2 S3 C32 3_656 -127.43(9) y
O1 AG2 S3 AG1 . -89.20(5) y
S4 AG2 S3 AG1 3_656 102.63(3) y
S4 AG2 O1 C1 3_656 17.6(3) y
S3 AG2 O1 C1 . -137.25(17) y
S2 AG1 O3 C4 1_455 -139.05(17) y
S1 AG1 O3 C4 . 84.60(17) y
S3 AG1 O3 C4 . -23.71(18) y
AG2 O1 C1 O2 . 0.7(4) y
AG2 O1 C1 C2 . 179.68(16) y
O2 C1 C2 F2 . -1.2(3) y
O1 C1 C2 F2 . 179.6(2) y
O2 C1 C2 F1 . 117.5(3) y
O1 C1 C2 F1 . -61.6(3) y
O2 C1 C2 C3 . -122.2(3) y
O1 C1 C2 C3 . 58.7(3) y
F2 C2 C3 F4 . 167.7(2) y
F1 C2 C3 F4 . 53.1(3) y
C1 C2 C3 F4 . -68.7(3) y
F2 C2 C3 F5 . 47.4(3) y
F1 C2 C3 F5 . -67.3(3) y
C1 C2 C3 F5 . 170.9(2) y
F2 C2 C3 F3 . -72.1(3) y
F1 C2 C3 F3 . 173.2(2) y
C1 C2 C3 F3 . 51.4(3) y
AG1 O3 C4 O4 . 0.7(4) y
AG1 O3 C4 C5 . 179.73(18) y
O4 C4 C5 F6 . -177.7(2) y
O3 C4 C5 F6 . 3.1(3) y
O4 C4 C5 F7 . 64.1(3) y
O3 C4 C5 F7 . -115.1(3) y
O4 C4 C5 C6 . -55.8(3) y
O3 C4 C5 C6 . 125.0(3) y
F6 C5 C6 F9 . -169.2(2) y
F7 C5 C6 F9 . -55.9(3) y
C4 C5 C6 F9 . 65.4(3) y
F6 C5 C6 F10 . -49.3(3) y
F7 C5 C6 F10 . 64.0(3) y
C4 C5 C6 F10 . -174.7(2) y
F6 C5 C6 F8 . 70.7(3) y
F7 C5 C6 F8 . -176.1(2) y
C4 C5 C6 F8 . -54.7(3) y
C11 S1 C12 C13 . -137.1(2) y
AG1 S1 C12 C13 . 118.1(2) y
S1 C12 C13 C14 . -174.5(2) y
C12 C13 C14 S2 . -169.1(2) y
C21 S2 C14 C13 . -56.5(2) y
AG1 S2 C14 C13 1_655 52.6(2) y
C31 S3 C32 C33 . -73.5(2) y
AG1 S3 C32 C33 . 176.76(16) y
AG2 S3 C32 C33 . 46.0(2) y
S3 C32 C33 C34 . 173.97(18) y
C32 C33 C34 S4 . 176.62(19) y
C41 S4 C34 C33 . -85.9(2) y
AG2 S4 C34 C33 3_656 23.9(2) y
|
1501643.cif | #------------------------------------------------------------------------------
#$Date: 2016-11-16 18:57:30 +0200 (Wed, 16 Nov 2016) $
#$Revision: 188516 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/50/16/1501643.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_1501643
loop_
_publ_author_name
'Christian Courseille'
'NGuyen Ba Chanh'
'Thierry Maris'
'Abdelaziz Daoud'
'Younes Abid'
'Michel Laguerre'
_publ_section_title
;
Crystal structure and phase transition in the perovskite-type layer
molecular composite NH~3~-(CH~2~)~4~-NH~3~ PbC1~4~
;
_journal_name_full 'Physica Statu Solidi A'
_journal_page_first 203
_journal_page_last 214
_journal_paper_doi 10.1002/pssa.2211430202
_journal_volume 143
_journal_year 1994
_chemical_formula_sum 'C4 H14 Cl4 N2 Pb'
_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
_cell_angle_beta 94.84(3)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 7.944(2)
_cell_length_b 7.772(5)
_cell_length_c 19.761(8)
_cell_volume 1215.7(10)
_exptl_crystal_colour colorless
_cod_data_source_file deposit.cif
_cod_data_source_block 2C4CuRT
_cod_original_cell_volume 1215.71
_cod_original_sg_symbol_H-M P21/c
_cod_original_formula_sum 'C4 H14 N2 Pb Cl4'
_cod_database_code 1501643
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_adp_type
_atom_site_attached_hydrogens
Pb1 Pb -0.2613(1) 0.6599(1) 0.2519(1) Uani 0
Cl1 Cl -0.2566(8) 0.6856(9) 0.1090(3) Uani 0
Cl2 Cl -0.1916(8) 0.6864(9) 0.3993(3) Uani 0
Cl3 Cl -0.0482(8) 0.3563(8) 0.2485(3) Uani 0
Cl4 Cl -0.5824(8) 0.4847(8) 0.2485(3) Uani 0
N1 N 0.8662(23) 0.4135(25) -0.1252(9) Uani 3
C1 C 0.7455(40) 0.3014(39) -0.0920(14) Uani 2
C2 C 0.7734(31) 0.3025(45) -0.0163(12) Uani 2
C3 C 0.6485(30) 0.1920(37) 0.0161(12) Uani 2
C4 C 0.6564(32) 0.1961(34) 0.0899(13) Uani 2
N2 N 0.8056(27) 0.0890(30) 0.1224(11) Uani 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_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Pb1 0.0107(6) 0.0246(7) 0.0204(6) 0.0005(3) 0.0030(4) 0.0007(4)
Cl1 0.0257(9) 0.0406(35) 0.0314(28) 0.0051(24) -0.0039(23) -0.0003(25)
Cl2 0.0321(32) 0.0397(35) 0.0325(29) 0.0023(26) 0.0053(25) 0.0018(26)
Cl3 0.0385(44) 0.0320(22) 0.0314(29) 0.0093(25) 0.0054(27) 0.0021(25)
Cl4 0.0387(33) 0.0452(39) 0.0353(29) -0.0152(31) -0.0014(25) 0.0008(30)
N1 0.0268(80) 0.0354(96) 0.0216(90) -0.0246(88) 0.0057(77) 0.0057(82)
C1 0.0741(79) 0.0416(91) 0.0399(90) 0.0259(89) 0.0076(85) 0.0275(85)
C2 0.0281(85) 0.0866(84) 0.0154(75) -0.0051(45) -0.0024(98) 0.0172(70)
C3 0.0297(83) 0.0528(78) 0.0283(80) 0.0024(76) -0.0142(95) 0.0026(29)
C4 0.0374(76) 0.0350(95) 0.0299(85) -0.0020(19) 0.0054(53) 0.0163(60)
N2 0.0400(1) 0.0400(1) 0.0400(1) 0.0000(1) 0.0034(1) 0.0000(1)
|
1501644.cif | #------------------------------------------------------------------------------
#$Date: 2020-10-02 17:43:13 +0300 (Fri, 02 Oct 2020) $
#$Revision: 256941 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/50/16/1501644.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_1501644
loop_
_publ_author_name
'Adam Duong'
'Marc-Andr\'e Dubois'
'Thierry Maris'
'Val\'erie M\'etivaud'
'Ji-Hyun Yi'
'Antonio Nanci'
'Alain Rochefort'
'Wuest,James D'
_publ_section_title
;
Engineering Homologous Molecular Organization in 2D and 3D.
Cocrystallization of Pyridyl-Substituted Diaminotriazines with
Alkanecarboxylic Acids
;
_journal_name_full 'The Journal of Physical Chemistry C'
_journal_page_first 12908
_journal_page_last 12919
_journal_paper_doi 10.1021/jp201119g
_journal_volume 115
_journal_year 2011
_chemical_compound_source 'Synthesized by the authors. See text'
_chemical_formula_moiety 'C9 H18 O2, C8 H8 N6'
_chemical_formula_sum 'C17 H26 N6 O2'
_chemical_formula_weight 346.44
_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 92.130(11)
_cell_angle_beta 106.824(12)
_cell_angle_gamma 95.885(12)
_cell_formula_units_Z 4
_cell_length_a 10.3277(19)
_cell_length_b 13.405(2)
_cell_length_c 13.648(2)
_cell_measurement_reflns_used 1398
_cell_measurement_temperature 150
_cell_measurement_theta_max 64.69
_cell_measurement_theta_min 3.32
_cell_volume 1794.6(5)
_computing_cell_refinement 'SAINT V7.60A(Bruker AXS, 2008)'
_computing_data_collection 'APEX2 (Bruker AXS, 2009)'
_computing_data_reduction 'SAINT V7.60A(Bruker AXS, 2008)'
_computing_molecular_graphics 'SHELXTL v6.12 (Bruker AXS, 2001)'
_computing_publication_material 'UdMX (Maris, 2004)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature 150
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type 'Bruker Microstar'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator 'Helios optics'
_diffrn_radiation_source 'Rotating Anode'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.114
_diffrn_reflns_av_sigmaI/netI 0.1200
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_l_max 14
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_number 20766
_diffrn_reflns_theta_full 67.86
_diffrn_reflns_theta_max 67.86
_diffrn_reflns_theta_min 3.32
_exptl_absorpt_coefficient_mu 0.711
_exptl_absorpt_correction_T_max 0.9789
_exptl_absorpt_correction_T_min 0.9018
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Sadabs (Sheldrick, 2008)'
_exptl_crystal_colour Colorless
_exptl_crystal_density_diffrn 1.282
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description Block
_exptl_crystal_F_000 744
_exptl_crystal_size_max 0.09
_exptl_crystal_size_mid 0.03
_exptl_crystal_size_min 0.03
_refine_diff_density_max 0.370
_refine_diff_density_min -0.307
_refine_diff_density_rms 0.076
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.004
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 453
_refine_ls_number_reflns 6368
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.004
_refine_ls_R_factor_all 0.1584
_refine_ls_R_factor_gt 0.0870
_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^)+(0.1183P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2091
_refine_ls_wR_factor_ref 0.2563
_reflns_number_gt 3085
_reflns_number_total 6368
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file COD_jp201119g_si_003.cif
_cod_data_source_block adam14
_cod_depositor_comments
;
Updated values of the _geom_bond_atom_site_label_* data items to establish
relationships between loop packets from different data loops.
Antanas Vaitkus,
2020-10-02
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.
'_geom_bond_publ_flag'
value 'Y' changed to 'y' according to the built-in table from CIF
Core dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29
(50 times).
'_geom_angle_publ_flag' value 'Y' changed to 'y'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (60 times).
Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana
;
_cod_original_sg_symbol_H-M P-1
_cod_database_code 1501644
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
N3 N 0.7801(3) 0.2774(2) 0.4835(3) 0.0455(8) Uani 1 1 d .
N2 N 0.6901(3) 0.4101(2) 0.5548(3) 0.0464(8) Uani 1 1 d .
N4 N 0.6403(3) 0.2404(2) 0.5930(2) 0.0439(8) Uani 1 1 d .
C24 C 0.6293(4) 0.3395(3) 0.5985(3) 0.0426(9) Uani 1 1 d .
N1 N 0.4505(4) 0.5105(3) 0.7251(3) 0.0555(9) Uani 1 1 d .
N6 N 0.7317(4) 0.1160(2) 0.5230(3) 0.0507(9) Uani 1 1 d .
H6A H 0.6936 0.0714 0.5550 0.061 Uiso 1 1 calc R
H6B H 0.7806 0.0967 0.4842 0.061 Uiso 1 1 calc R
C22 C 0.5436(4) 0.3740(3) 0.6605(3) 0.0411(9) Uani 1 1 d .
C21 C 0.4764(4) 0.3075(3) 0.7098(3) 0.0504(10) Uani 1 1 d .
H21 H 0.4852 0.2377 0.7053 0.061 Uiso 1 1 calc R
C26 C 0.7153(4) 0.2133(3) 0.5334(3) 0.0430(9) Uani 1 1 d .
C20 C 0.3973(4) 0.3431(3) 0.7650(3) 0.0553(11) Uani 1 1 d .
H20 H 0.3507 0.2983 0.7993 0.066 Uiso 1 1 calc R
C23 C 0.5254(4) 0.4748(3) 0.6704(3) 0.0506(10) Uani 1 1 d .
H23 H 0.5693 0.5212 0.6358 0.061 Uiso 1 1 calc R
C25 C 0.7661(4) 0.3755(3) 0.4996(3) 0.0441(9) Uani 1 1 d .
N5 N 0.8363(4) 0.4427(2) 0.4596(3) 0.0540(9) Uani 1 1 d .
H5A H 0.8318 0.5073 0.4699 0.065 Uiso 1 1 calc R
H5B H 0.8873 0.4226 0.4228 0.065 Uiso 1 1 calc R
C19 C 0.3858(4) 0.4440(3) 0.7705(3) 0.0534(11) Uani 1 1 d .
H19 H 0.3295 0.4676 0.8082 0.064 Uiso 1 1 calc R
N9 N 0.5221(3) 0.1099(2) 0.2746(2) 0.0447(8) Uani 1 1 d .
N10 N 0.3902(3) 0.0737(2) 0.3889(2) 0.0448(8) Uani 1 1 d .
N8 N 0.4308(3) 0.2420(2) 0.3456(2) 0.0458(8) Uani 1 1 d .
N7 N 0.1770(3) 0.3377(2) 0.5070(3) 0.0504(9) Uani 1 1 d .
C30 C 0.2878(4) 0.2058(3) 0.4541(3) 0.0434(9) Uani 1 1 d .
C29 C 0.2296(4) 0.1388(3) 0.5095(3) 0.0522(11) Uani 1 1 d .
H29 H 0.2475 0.0706 0.5105 0.063 Uiso 1 1 calc R
C32 C 0.3751(4) 0.1716(3) 0.3927(3) 0.0431(9) Uani 1 1 d .
N12 N 0.4850(4) -0.0500(2) 0.3210(3) 0.0527(9) Uani 1 1 d .
H12A H 0.4494 -0.0945 0.3545 0.063 Uiso 1 1 calc R
H12B H 0.5339 -0.0689 0.2820 0.063 Uiso 1 1 calc R
C34 C 0.5043(4) 0.2075(3) 0.2879(3) 0.0434(9) Uani 1 1 d .
C33 C 0.4650(4) 0.0458(3) 0.3292(3) 0.0448(9) Uani 1 1 d .
N11 N 0.5634(3) 0.2744(2) 0.2394(3) 0.0511(9) Uani 1 1 d .
H11A H 0.5534 0.3385 0.2460 0.061 Uiso 1 1 calc R
H11B H 0.6123 0.2545 0.2009 0.061 Uiso 1 1 calc R
C31 C 0.2591(4) 0.3047(3) 0.4573(3) 0.0461(10) Uani 1 1 d .
H31 H 0.3008 0.3515 0.4218 0.055 Uiso 1 1 calc R
C27 C 0.1216(4) 0.2712(3) 0.5579(3) 0.0503(11) Uani 1 1 d .
H27 H 0.0617 0.2933 0.5932 0.060 Uiso 1 1 calc R
C28 C 0.1464(4) 0.1721(3) 0.5624(3) 0.0533(11) Uani 1 1 d .
H28 H 0.1065 0.1279 0.6014 0.064 Uiso 1 1 calc R
O2 O 0.8809(3) 0.2188(2) 0.3270(2) 0.0552(8) Uani 1 1 d .
H2 H 0.8398 0.2287 0.3707 0.083 Uiso 1 1 calc .
O1 O 0.8702(3) 0.0622(2) 0.3777(2) 0.0595(8) Uani 1 1 d .
C8 C 0.9781(4) 0.0988(3) 0.2481(3) 0.0475(10) Uani 1 1 d .
H8A H 1.0641 0.1446 0.2636 0.057 Uiso 1 1 calc R
H8B H 0.9211 0.1116 0.1789 0.057 Uiso 1 1 calc R
C9 C 0.9053(4) 0.1232(3) 0.3246(3) 0.0481(10) Uani 1 1 d .
C4 C 1.1927(4) -0.1634(3) 0.0888(3) 0.0520(11) Uani 1 1 d .
H4A H 1.1425 -0.1420 0.0210 0.062 Uiso 1 1 calc R
H4B H 1.2828 -0.1224 0.1113 0.062 Uiso 1 1 calc R
C5 C 1.1152(4) -0.1415(3) 0.1646(3) 0.0510(10) Uani 1 1 d .
H5C H 1.1678 -0.1591 0.2334 0.061 Uiso 1 1 calc R
H5D H 1.0269 -0.1850 0.1443 0.061 Uiso 1 1 calc R
C7 C 1.0109(4) -0.0091(3) 0.2470(3) 0.0499(10) Uani 1 1 d .
H7A H 0.9247 -0.0549 0.2294 0.060 Uiso 1 1 calc R
H7B H 1.0657 -0.0225 0.3167 0.060 Uiso 1 1 calc R
C6 C 1.0885(4) -0.0325(3) 0.1713(3) 0.0507(10) Uani 1 1 d .
H6D H 1.0362 -0.0151 0.1024 0.061 Uiso 1 1 calc R
H6E H 1.1769 0.0108 0.1914 0.061 Uiso 1 1 calc R
C3 C 1.2141(4) -0.2729(3) 0.0766(3) 0.0525(11) Uani 1 1 d .
H3A H 1.1243 -0.3136 0.0487 0.063 Uiso 1 1 calc R
H3B H 1.2583 -0.2960 0.1451 0.063 Uiso 1 1 calc R
C2 C 1.3013(5) -0.2910(4) 0.0062(4) 0.0642(13) Uani 1 1 d .
H2A H 1.2564 -0.2685 -0.0624 0.077 Uiso 1 1 calc R
H2B H 1.3906 -0.2495 0.0337 0.077 Uiso 1 1 calc R
C1 C 1.3247(5) -0.3996(4) -0.0055(4) 0.0752(15) Uani 1 1 d .
H1A H 1.2378 -0.4402 -0.0402 0.113 Uiso 1 1 calc R
H1B H 1.3634 -0.4239 0.0625 0.113 Uiso 1 1 calc R
H1C H 1.3881 -0.4051 -0.0462 0.113 Uiso 1 1 calc R
O4 O 0.6335(3) 0.0510(2) 0.1272(2) 0.0567(8) Uani 1 1 d .
H4 H 0.6023 0.0625 0.1763 0.085 Uiso 1 1 calc .
O3 O 0.6094(3) -0.1071(2) 0.1711(2) 0.0665(9) Uani 1 1 d .
C15 C 0.7834(4) -0.2085(3) -0.0619(3) 0.0494(10) Uani 1 1 d .
H15A H 0.8748 -0.1694 -0.0423 0.059 Uiso 1 1 calc R
H15B H 0.7305 -0.1863 -0.1286 0.059 Uiso 1 1 calc R
C16 C 0.7131(4) -0.1846(3) 0.0184(3) 0.0512(11) Uani 1 1 d .
H16A H 0.6219 -0.2240 -0.0007 0.061 Uiso 1 1 calc R
H16B H 0.7665 -0.2057 0.0854 0.061 Uiso 1 1 calc R
C17 C 0.6974(5) -0.0740(3) 0.0295(3) 0.0518(11) Uani 1 1 d .
H17A H 0.7873 -0.0343 0.0403 0.062 Uiso 1 1 calc R
H17B H 0.6354 -0.0550 -0.0353 0.062 Uiso 1 1 calc R
C12 C 0.9012(5) -0.4490(3) -0.1631(3) 0.0530(11) Uani 1 1 d .
H12C H 0.9533 -0.4680 -0.0947 0.064 Uiso 1 1 calc R
H12D H 0.8133 -0.4929 -0.1847 0.064 Uiso 1 1 calc R
C18 C 0.6428(4) -0.0467(3) 0.1167(3) 0.0499(10) Uani 1 1 d .
C14 C 0.7992(5) -0.3193(3) -0.0757(3) 0.0544(11) Uani 1 1 d .
H14A H 0.8499 -0.3423 -0.0088 0.065 Uiso 1 1 calc R
H14B H 0.7078 -0.3585 -0.0977 0.065 Uiso 1 1 calc R
C11 C 0.9797(5) -0.4685(3) -0.2384(4) 0.0591(12) Uani 1 1 d .
H11D H 0.9253 -0.4533 -0.3076 0.071 Uiso 1 1 calc R
H11E H 1.0655 -0.4222 -0.2190 0.071 Uiso 1 1 calc R
C13 C 0.8731(5) -0.3406(3) -0.1536(3) 0.0547(11) Uani 1 1 d .
H13A H 0.9610 -0.2966 -0.1347 0.066 Uiso 1 1 calc R
H13B H 0.8182 -0.3226 -0.2215 0.066 Uiso 1 1 calc R
C10 C 1.0132(5) -0.5750(4) -0.2429(4) 0.0677(14) Uani 1 1 d .
H10A H 0.9287 -0.6213 -0.2643 0.102 Uiso 1 1 calc R
H10B H 1.0684 -0.5904 -0.1749 0.102 Uiso 1 1 calc R
H10C H 1.0645 -0.5825 -0.2924 0.102 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
N3 0.058(2) 0.0326(18) 0.0535(19) 0.0085(15) 0.0263(16) 0.0093(14)
N2 0.060(2) 0.0321(18) 0.056(2) 0.0060(15) 0.0297(17) 0.0082(15)
N4 0.058(2) 0.0287(18) 0.055(2) 0.0055(15) 0.0291(17) 0.0101(14)
C24 0.050(2) 0.034(2) 0.045(2) 0.0038(18) 0.0154(19) 0.0073(17)
N1 0.073(2) 0.038(2) 0.070(2) 0.0064(17) 0.042(2) 0.0114(17)
N6 0.074(2) 0.0330(18) 0.061(2) 0.0084(16) 0.0420(19) 0.0124(16)
C22 0.049(2) 0.033(2) 0.043(2) 0.0027(17) 0.0163(18) 0.0054(16)
C21 0.069(3) 0.031(2) 0.061(3) 0.0065(19) 0.033(2) 0.0117(19)
C26 0.054(2) 0.033(2) 0.045(2) 0.0034(17) 0.0198(19) 0.0088(17)
C20 0.073(3) 0.039(2) 0.067(3) 0.003(2) 0.041(2) 0.005(2)
C23 0.066(3) 0.034(2) 0.063(3) 0.0048(19) 0.036(2) 0.0067(18)
C25 0.058(2) 0.031(2) 0.048(2) 0.0065(17) 0.0216(19) 0.0075(17)
N5 0.080(2) 0.0308(18) 0.068(2) 0.0091(16) 0.046(2) 0.0113(16)
C19 0.070(3) 0.042(2) 0.062(3) 0.005(2) 0.039(2) 0.009(2)
N9 0.059(2) 0.0315(17) 0.0517(19) 0.0064(15) 0.0265(16) 0.0105(14)
N10 0.060(2) 0.0297(18) 0.054(2) 0.0051(15) 0.0292(17) 0.0097(15)
N8 0.062(2) 0.0301(17) 0.0534(19) 0.0055(15) 0.0294(17) 0.0070(15)
N7 0.064(2) 0.038(2) 0.058(2) 0.0050(16) 0.0306(18) 0.0117(16)
C30 0.052(2) 0.033(2) 0.049(2) 0.0040(18) 0.0196(19) 0.0071(17)
C29 0.069(3) 0.034(2) 0.062(3) 0.0023(19) 0.033(2) 0.0066(19)
C32 0.055(2) 0.033(2) 0.047(2) 0.0055(18) 0.0218(19) 0.0075(17)
N12 0.080(2) 0.0280(18) 0.069(2) 0.0077(16) 0.050(2) 0.0144(16)
C34 0.056(2) 0.031(2) 0.051(2) 0.0035(18) 0.026(2) 0.0102(17)
C33 0.056(2) 0.034(2) 0.051(2) 0.0060(18) 0.024(2) 0.0094(18)
N11 0.074(2) 0.0328(18) 0.063(2) 0.0087(16) 0.0439(19) 0.0126(16)
C31 0.058(2) 0.034(2) 0.054(2) 0.0067(18) 0.027(2) 0.0079(18)
C27 0.063(3) 0.040(2) 0.058(3) 0.000(2) 0.034(2) 0.0069(19)
C28 0.071(3) 0.040(2) 0.059(3) 0.002(2) 0.036(2) 0.007(2)
O2 0.0772(19) 0.0384(16) 0.0650(18) 0.0092(13) 0.0416(16) 0.0126(14)
O1 0.090(2) 0.0369(17) 0.0698(19) 0.0114(15) 0.0490(18) 0.0140(14)
C8 0.060(2) 0.036(2) 0.052(2) 0.0045(18) 0.026(2) 0.0051(18)
C9 0.060(3) 0.035(2) 0.056(3) 0.007(2) 0.025(2) 0.0105(19)
C4 0.060(3) 0.046(3) 0.056(3) 0.004(2) 0.025(2) 0.011(2)
C5 0.061(3) 0.048(3) 0.052(2) 0.0096(19) 0.027(2) 0.011(2)
C7 0.061(3) 0.044(2) 0.054(2) 0.008(2) 0.027(2) 0.014(2)
C6 0.064(3) 0.043(2) 0.053(2) 0.0074(19) 0.026(2) 0.012(2)
C3 0.060(3) 0.048(3) 0.056(3) 0.004(2) 0.026(2) 0.013(2)
C2 0.076(3) 0.058(3) 0.072(3) 0.000(2) 0.039(3) 0.018(2)
C1 0.080(3) 0.071(4) 0.082(3) -0.017(3) 0.033(3) 0.020(3)
O4 0.082(2) 0.0354(16) 0.0681(19) 0.0072(14) 0.0448(16) 0.0114(14)
O3 0.106(2) 0.0391(17) 0.080(2) 0.0107(16) 0.067(2) 0.0109(16)
C15 0.060(3) 0.041(2) 0.052(2) 0.0024(19) 0.023(2) 0.0092(19)
C16 0.063(3) 0.039(2) 0.060(3) 0.0021(19) 0.033(2) 0.0060(19)
C17 0.065(3) 0.042(2) 0.057(3) 0.004(2) 0.030(2) 0.0091(19)
C12 0.067(3) 0.042(2) 0.058(3) 0.004(2) 0.030(2) 0.012(2)
C18 0.055(2) 0.043(2) 0.058(3) -0.001(2) 0.025(2) 0.0117(19)
C14 0.068(3) 0.045(3) 0.060(3) 0.006(2) 0.033(2) 0.011(2)
C11 0.074(3) 0.050(3) 0.061(3) 0.002(2) 0.029(2) 0.017(2)
C13 0.073(3) 0.048(3) 0.053(2) 0.006(2) 0.030(2) 0.015(2)
C10 0.081(3) 0.061(3) 0.072(3) -0.005(3) 0.038(3) 0.016(2)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 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_publ_flag
C25 N3 C26 114.5(3) y
C24 N2 C25 114.7(3) y
C26 N4 C24 114.3(3) y
N2 C24 N4 126.1(3) y
N2 C24 C22 116.8(3) y
N4 C24 C22 117.0(3) y
C23 N1 C19 117.2(4) y
C26 N6 H6A 120 ?
C26 N6 H6B 120 ?
H6A N6 H6B 120 ?
C21 C22 C23 116.9(3) y
C21 C22 C24 121.7(3) y
C23 C22 C24 121.3(4) y
C20 C21 C22 119.4(4) y
C20 C21 H21 120.3 ?
C22 C21 H21 120.3 ?
N4 C26 N6 118.6(4) y
N4 C26 N3 125.1(3) y
N6 C26 N3 116.3(3) y
C21 C20 C19 119.5(4) y
C21 C20 H20 120.3 ?
C19 C20 H20 120.3 ?
N1 C23 C22 124.2(4) y
N1 C23 H23 117.9 ?
C22 C23 H23 117.9 ?
N5 C25 N2 117.6(3) y
N5 C25 N3 117.3(3) y
N2 C25 N3 125.1(4) y
C25 N5 H5A 120 ?
C25 N5 H5B 120 ?
H5A N5 H5B 120 ?
N1 C19 C20 122.8(4) y
N1 C19 H19 118.6 ?
C20 C19 H19 118.6 ?
C34 N9 C33 115.1(3) y
C32 N10 C33 115.4(3) y
C32 N8 C34 114.7(3) y
C31 N7 C27 117.0(3) y
C31 C30 C29 117.3(3) y
C31 C30 C32 121.8(4) y
C29 C30 C32 120.9(4) y
C28 C29 C30 119.4(4) y
C28 C29 H29 120.3 ?
C30 C29 H29 120.3 ?
N8 C32 N10 125.8(3) y
N8 C32 C30 116.6(3) y
N10 C32 C30 117.6(3) y
C33 N12 H12A 120 ?
C33 N12 H12B 120 ?
H12A N12 H12B 120 ?
N11 C34 N8 117.5(3) y
N11 C34 N9 117.6(3) y
N8 C34 N9 124.9(4) y
N12 C33 N10 119.4(4) y
N12 C33 N9 116.6(3) y
N10 C33 N9 124.0(3) y
C34 N11 H11A 120 ?
C34 N11 H11B 120 ?
H11A N11 H11B 120 ?
N7 C31 C30 124.0(4) y
N7 C31 H31 118 ?
C30 C31 H31 118 ?
N7 C27 C28 123.8(3) y
N7 C27 H27 118.1 ?
C28 C27 H27 118.1 ?
C29 C28 C27 118.5(4) y
C29 C28 H28 120.7 ?
C27 C28 H28 120.7 ?
C9 O2 H2 109.5 ?
C9 C8 C7 113.7(3) y
C9 C8 H8A 108.8 ?
C7 C8 H8A 108.8 ?
C9 C8 H8B 108.8 ?
C7 C8 H8B 108.8 ?
H8A C8 H8B 107.7 ?
O1 C9 O2 123.3(4) y
O1 C9 C8 123.6(4) y
O2 C9 C8 113.0(4) y
C3 C4 C5 114.5(3) y
C3 C4 H4A 108.6 ?
C5 C4 H4A 108.6 ?
C3 C4 H4B 108.6 ?
C5 C4 H4B 108.6 ?
H4A C4 H4B 107.6 ?
C4 C5 C6 113.5(3) y
C4 C5 H5C 108.9 ?
C6 C5 H5C 108.9 ?
C4 C5 H5D 108.9 ?
C6 C5 H5D 108.9 ?
H5C C5 H5D 107.7 ?
C8 C7 C6 113.5(3) y
C8 C7 H7A 108.9 ?
C6 C7 H7A 108.9 ?
C8 C7 H7B 108.9 ?
C6 C7 H7B 108.9 ?
H7A C7 H7B 107.7 ?
C5 C6 C7 114.2(3) y
C5 C6 H6D 108.7 ?
C7 C6 H6D 108.7 ?
C5 C6 H6E 108.7 ?
C7 C6 H6E 108.7 ?
H6D C6 H6E 107.6 ?
C4 C3 C2 113.1(4) y
C4 C3 H3A 109 ?
C2 C3 H3A 109 ?
C4 C3 H3B 109 ?
C2 C3 H3B 109 ?
H3A C3 H3B 107.8 ?
C1 C2 C3 113.6(4) y
C1 C2 H2A 108.9 ?
C3 C2 H2A 108.9 ?
C1 C2 H2B 108.9 ?
C3 C2 H2B 108.9 ?
H2A C2 H2B 107.7 ?
C2 C1 H1A 109.5 ?
C2 C1 H1B 109.5 ?
H1A C1 H1B 109.5 ?
C2 C1 H1C 109.5 ?
H1A C1 H1C 109.5 ?
H1B C1 H1C 109.5 ?
C18 O4 H4 109.5 ?
C16 C15 C14 114.1(3) y
C16 C15 H15A 108.7 ?
C14 C15 H15A 108.7 ?
C16 C15 H15B 108.7 ?
C14 C15 H15B 108.7 ?
H15A C15 H15B 107.6 ?
C17 C16 C15 112.9(3) y
C17 C16 H16A 109 ?
C15 C16 H16A 109 ?
C17 C16 H16B 109 ?
C15 C16 H16B 109 ?
H16A C16 H16B 107.8 ?
C18 C17 C16 113.8(4) y
C18 C17 H17A 108.8 ?
C16 C17 H17A 108.8 ?
C18 C17 H17B 108.8 ?
C16 C17 H17B 108.8 ?
H17A C17 H17B 107.7 ?
C11 C12 C13 114.1(4) y
C11 C12 H12C 108.7 ?
C13 C12 H12C 108.7 ?
C11 C12 H12D 108.7 ?
C13 C12 H12D 108.7 ?
H12C C12 H12D 107.6 ?
O3 C18 O4 123.2(3) y
O3 C18 C17 123.8(4) y
O4 C18 C17 113.0(4) y
C13 C14 C15 113.1(3) y
C13 C14 H14A 109 ?
C15 C14 H14A 109 ?
C13 C14 H14B 109 ?
C15 C14 H14B 109 ?
H14A C14 H14B 107.8 ?
C10 C11 C12 113.5(4) y
C10 C11 H11D 108.9 ?
C12 C11 H11D 108.9 ?
C10 C11 H11E 108.9 ?
C12 C11 H11E 108.9 ?
H11D C11 H11E 107.7 ?
C14 C13 C12 114.6(4) y
C14 C13 H13A 108.6 ?
C12 C13 H13A 108.6 ?
C14 C13 H13B 108.6 ?
C12 C13 H13B 108.6 ?
H13A C13 H13B 107.6 ?
C11 C10 H10A 109.5 ?
C11 C10 H10B 109.5 ?
H10A C10 H10B 109.5 ?
C11 C10 H10C 109.5 ?
H10A C10 H10C 109.5 ?
H10B C10 H10C 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
N3 C25 1.354(5) y
N3 C26 1.356(5) y
N2 C24 1.334(5) y
N2 C25 1.337(5) y
N4 C26 1.340(5) y
N4 C24 1.346(5) y
C24 C22 1.485(5) y
N1 C23 1.330(5) y
N1 C19 1.336(5) y
N6 C26 1.341(5) y
N6 H6A 0.88 ?
N6 H6B 0.88 ?
C22 C21 1.385(5) y
C22 C23 1.389(5) y
C21 C20 1.369(5) y
C21 H21 0.95 ?
C20 C19 1.370(6) y
C20 H20 0.95 ?
C23 H23 0.95 ?
C25 N5 1.329(5) y
N5 H5A 0.88 ?
N5 H5B 0.88 ?
C19 H19 0.95 ?
N9 C34 1.352(5) y
N9 C33 1.356(5) y
N10 C32 1.338(5) y
N10 C33 1.343(5) y
N8 C32 1.335(5) y
N8 C34 1.342(5) y
N7 C31 1.327(5) y
N7 C27 1.333(5) y
C30 C31 1.389(5) y
C30 C29 1.394(6) y
C30 C32 1.489(5) y
C29 C28 1.369(6) y
C29 H29 0.95 ?
N12 C33 1.327(5) y
N12 H12A 0.88 ?
N12 H12B 0.88 ?
C34 N11 1.334(5) y
N11 H11A 0.88 ?
N11 H11B 0.88 ?
C31 H31 0.95 ?
C27 C28 1.379(6) y
C27 H27 0.95 ?
C28 H28 0.95 ?
O2 C9 1.333(5) y
O2 H2 0.84 ?
O1 C9 1.208(5) y
C8 C9 1.497(6) y
C8 C7 1.520(5) y
C8 H8A 0.99 ?
C8 H8B 0.99 ?
C4 C3 1.517(6) y
C4 C5 1.517(5) y
C4 H4A 0.99 ?
C4 H4B 0.99 ?
C5 C6 1.518(6) y
C5 H5C 0.99 ?
C5 H5D 0.99 ?
C7 C6 1.522(5) y
C7 H7A 0.99 ?
C7 H7B 0.99 ?
C6 H6D 0.99 ?
C6 H6E 0.99 ?
C3 C2 1.524(6) y
C3 H3A 0.99 ?
C3 H3B 0.99 ?
C2 C1 1.510(6) y
C2 H2A 0.99 ?
C2 H2B 0.99 ?
C1 H1A 0.98 ?
C1 H1B 0.98 ?
C1 H1C 0.98 ?
O4 C18 1.328(5) y
O4 H4 0.84 ?
O3 C18 1.208(5) y
C15 C16 1.521(5) y
C15 C14 1.521(5) y
C15 H15A 0.99 ?
C15 H15B 0.99 ?
C16 C17 1.515(5) y
C16 H16A 0.99 ?
C16 H16B 0.99 ?
C17 C18 1.506(5) y
C17 H17A 0.99 ?
C17 H17B 0.99 ?
C12 C11 1.512(6) y
C12 C13 1.519(6) y
C12 H12C 0.99 ?
C12 H12D 0.99 ?
C14 C13 1.512(5) y
C14 H14A 0.99 ?
C14 H14B 0.99 ?
C11 C10 1.506(6) y
C11 H11D 0.99 ?
C11 H11E 0.99 ?
C13 H13A 0.99 ?
C13 H13B 0.99 ?
C10 H10A 0.98 ?
C10 H10B 0.98 ?
C10 H10C 0.98 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N6 H6A N10 0.88 2.29 3.153(5) 165.1 2_656
N6 H6A N10 0.88 2.29 3.153(5) 165.1 2_656
N6 H6B O1 0.88 2 2.872(4) 170.8 .
N5 H5A N7 0.88 2.11 2.986(5) 179.1 2_666
N12 H12A N4 0.88 2.31 3.162(5) 164.5 2_656
N12 H12B O3 0.88 1.97 2.833(4) 167.9 .
N11 H11A N1 0.88 2.05 2.930(5) 173.6 2_666
O2 H2 N3 0.84 1.93 2.756(4) 166.2 .
O4 H4 N9 0.84 1.89 2.720(4) 169.4 .
|
1501645.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/16/1501645.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_1501645
loop_
_publ_author_name
'Lakadamyali, Fezile'
'Kato, Masaru'
'Reisner, Erwin'
_publ_section_title
;
Colloidal metal oxide particles loaded with synthetic catalysts for solar
H2 production
;
_journal_name_full 'Faraday Discussions'
_journal_page_first 191
_journal_paper_doi 10.1039/c1fd00077b
_journal_volume 155
_journal_year 2012
_chemical_formula_moiety 'C17 H28 Cl Co N5 O7 P'
_chemical_formula_sum 'C17 H28 Cl Co N5 O7 P'
_chemical_formula_weight 539.79
_chemical_name_common '[CoCl(dmgH)2(C5H4N-PO3Et2)]'
_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 94.937(7)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 8.2787(6)
_cell_length_b 12.8802(10)
_cell_length_c 21.4315(18)
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 26.37
_cell_measurement_theta_min 3.61
_cell_volume 2276.8(3)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET)
(compiled Dec 8 2009,17:31:18)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET)
(compiled Dec 8 2009,17:31:18)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET)
(compiled Dec 8 2009,17:31:18)
;
_computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean 8.3367
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type 'Oxford Diffraction XCalibur 2'
_diffrn_measurement_method 'phi and omega'
_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 0.0366
_diffrn_reflns_av_sigmaI/netI 0.0631
_diffrn_reflns_limit_h_max 6
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min -7
_diffrn_reflns_limit_l_max 21
_diffrn_reflns_limit_l_min -26
_diffrn_reflns_number 7793
_diffrn_reflns_theta_full 26.37
_diffrn_reflns_theta_max 26.37
_diffrn_reflns_theta_min 3.61
_exptl_absorpt_coefficient_mu 0.990
_exptl_absorpt_correction_T_max 0.9709
_exptl_absorpt_correction_T_min 0.8657
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'see below'
_exptl_crystal_colour brown
_exptl_crystal_density_diffrn 1.575
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 1120
_exptl_crystal_size_max 0.15
_exptl_crystal_size_mid 0.10
_exptl_crystal_size_min 0.03
_refine_diff_density_max 0.509
_refine_diff_density_min -0.466
_refine_diff_density_rms 0.074
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.896
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 301
_refine_ls_number_reflns 4616
_refine_ls_number_restraints 8
_refine_ls_restrained_S_all 0.912
_refine_ls_R_factor_all 0.0515
_refine_ls_R_factor_gt 0.0319
_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^)+(0.0330P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0662
_refine_ls_wR_factor_ref 0.0685
_reflns_number_gt 3178
_reflns_number_total 4616
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file c1fd00077b.txt
_cod_data_source_block
;
;
_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_values 1715 2011-07-08 13:25:40Z adriana
;
_cod_original_sg_symbol_H-M P2(1)/n
_cod_database_code 1501645
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
Co1 Co 0.76766(4) 0.95883(2) 0.157616(14) 0.00884(9) Uani 1 1 d .
Cl1 Cl 0.62779(7) 0.96603(4) 0.06467(3) 0.01426(13) Uani 1 1 d .
P1 P 1.22609(7) 0.93887(5) 0.41985(3) 0.01128(14) Uani 1 1 d .
N1 N 0.8876(2) 0.95242(14) 0.24035(8) 0.0078(4) Uani 1 1 d .
O3 O 0.65661(19) 0.75417(11) 0.17131(8) 0.0136(4) Uani 1 1 d .
O2 O 0.9113(2) 0.76995(12) 0.11975(8) 0.0162(4) Uani 1 1 d D
O1 O 0.8806(2) 1.16538(13) 0.13928(8) 0.0174(4) Uani 1 1 d D
N2 N 0.6130(2) 1.04386(14) 0.19062(9) 0.0103(4) Uani 1 1 d .
N3 N 0.6287(2) 0.85397(14) 0.18140(9) 0.0093(4) Uani 1 1 d .
O4 O 0.6246(2) 1.14678(12) 0.19011(8) 0.0155(4) Uani 1 1 d .
N5 N 0.9080(2) 1.06323(14) 0.13155(9) 0.0118(4) Uani 1 1 d .
N4 N 0.9232(2) 0.87465(14) 0.12226(9) 0.0116(4) Uani 1 1 d .
C2 C 1.0179(3) 1.03595(17) 0.33000(11) 0.0110(5) Uani 1 1 d .
H2A H 1.0396 1.0981 0.3531 0.013 Uiso 1 1 calc R
C11 C 1.0333(3) 1.03370(19) 0.10454(11) 0.0138(5) Uani 1 1 d .
C6 C 0.4943(3) 0.99754(18) 0.21378(11) 0.0106(5) Uani 1 1 d .
C3 C 1.0817(3) 0.94259(17) 0.35229(10) 0.0098(5) Uani 1 1 d .
C10 C 1.0412(3) 0.92045(19) 0.09853(11) 0.0141(5) Uani 1 1 d .
C7 C 0.5032(3) 0.88474(18) 0.20875(11) 0.0114(5) Uani 1 1 d .
C5 C 0.9417(3) 0.86047(17) 0.26356(11) 0.0109(5) Uani 1 1 d .
H5A H 0.9129 0.7987 0.2410 0.013 Uiso 1 1 calc R
C4 C 1.0377(3) 0.85362(17) 0.31913(11) 0.0113(5) Uani 1 1 d .
H4A H 1.0737 0.7877 0.3346 0.014 Uiso 1 1 calc R
C1 C 0.9232(3) 1.03824(17) 0.27432(11) 0.0109(5) Uani 1 1 d .
H1A H 0.8811 1.1030 0.2592 0.013 Uiso 1 1 calc R
C13 C 1.1541(3) 1.1045(2) 0.08010(12) 0.0224(6) Uani 1 1 d .
H13A H 1.1392 1.1057 0.0342 0.034 Uiso 1 1 calc R
H13B H 1.2637 1.0799 0.0935 0.034 Uiso 1 1 calc R
H13C H 1.1394 1.1746 0.0964 0.034 Uiso 1 1 calc R
C9 C 0.3818(3) 0.81240(19) 0.23113(12) 0.0200(6) Uani 1 1 d .
H9A H 0.3807 0.7481 0.2066 0.030 Uiso 1 1 calc R
H9B H 0.2743 0.8447 0.2261 0.030 Uiso 1 1 calc R
H9C H 0.4101 0.7965 0.2754 0.030 Uiso 1 1 calc R
C8 C 0.3619(3) 1.05284(19) 0.24225(12) 0.0201(6) Uani 1 1 d .
H8A H 0.3839 1.1276 0.2428 0.030 Uiso 1 1 calc R
H8B H 0.3553 1.0281 0.2852 0.030 Uiso 1 1 calc R
H8C H 0.2588 1.0394 0.2176 0.030 Uiso 1 1 calc R
C12 C 1.1693(3) 0.8675(2) 0.06625(12) 0.0221(6) Uani 1 1 d .
H12A H 1.1504 0.7924 0.0663 0.033 Uiso 1 1 calc R
H12B H 1.2755 0.8827 0.0881 0.033 Uiso 1 1 calc R
H12C H 1.1668 0.8924 0.0230 0.033 Uiso 1 1 calc R
O5 O 1.2224(2) 1.03150(12) 0.45834(8) 0.0187(4) Uani 1 1 d .
O6 O 1.38111(19) 0.91821(13) 0.38515(8) 0.0177(4) Uani 1 1 d .
O7 O 1.20456(18) 0.83362(12) 0.45405(8) 0.0138(4) Uani 1 1 d .
C16 C 1.0871(3) 0.8209(2) 0.50072(12) 0.0226(6) Uani 1 1 d .
H16A H 1.0529 0.8900 0.5151 0.027 Uiso 1 1 calc R
H16B H 1.1379 0.7828 0.5374 0.027 Uiso 1 1 calc R
C14 C 1.5393(3) 0.9118(2) 0.42014(12) 0.0196(6) Uani 1 1 d .
H14A H 1.5818 0.8401 0.4186 0.023 Uiso 1 1 calc R
H14B H 1.5302 0.9305 0.4645 0.023 Uiso 1 1 calc R
C17 C 0.9433(3) 0.7626(2) 0.47300(14) 0.0262(6) Uani 1 1 d .
H17A H 0.8650 0.7544 0.5045 0.039 Uiso 1 1 calc R
H17B H 0.9774 0.6940 0.4593 0.039 Uiso 1 1 calc R
H17C H 0.8927 0.8010 0.4370 0.039 Uiso 1 1 calc R
C18 C 1.6497(4) 0.9841(2) 0.39201(15) 0.0386(8) Uani 1 1 d U
H18A H 1.7569 0.9808 0.4152 0.058 Uiso 1 1 calc R
H18B H 1.6070 1.0549 0.3939 0.058 Uiso 1 1 calc R
H18C H 1.6588 0.9647 0.3482 0.058 Uiso 1 1 calc R
H1 H 0.788(3) 1.165(2) 0.1569(13) 0.035(9) Uiso 1 1 d D
H2 H 0.817(3) 0.760(3) 0.1342(16) 0.066(13) 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
Co1 0.00782(17) 0.00941(16) 0.00918(16) 0.00041(13) 0.00009(11) 0.00006(14)
Cl1 0.0134(3) 0.0182(3) 0.0104(3) 0.0013(2) -0.0026(2) -0.0005(3)
P1 0.0081(3) 0.0150(3) 0.0102(3) -0.0009(2) -0.0018(2) -0.0005(3)
N1 0.0040(9) 0.0088(9) 0.0111(10) 0.0006(8) 0.0026(7) 0.0001(8)
O3 0.0143(9) 0.0071(8) 0.0194(9) -0.0014(7) 0.0011(7) -0.0018(7)
O2 0.0163(10) 0.0087(8) 0.0239(10) -0.0034(7) 0.0039(8) 0.0014(8)
O1 0.0178(10) 0.0108(9) 0.0238(10) 0.0018(7) 0.0031(8) -0.0030(8)
N2 0.0123(10) 0.0079(10) 0.0099(9) 0.0002(8) -0.0030(8) 0.0035(9)
N3 0.0092(10) 0.0087(10) 0.0092(10) -0.0005(8) -0.0027(8) 0.0006(8)
O4 0.0190(10) 0.0061(8) 0.0213(10) 0.0005(7) 0.0013(7) 0.0029(7)
N5 0.0149(11) 0.0096(10) 0.0102(10) 0.0011(8) -0.0023(8) -0.0003(8)
N4 0.0118(11) 0.0102(10) 0.0123(11) 0.0000(8) -0.0019(8) 0.0000(9)
C2 0.0086(11) 0.0111(11) 0.0137(12) -0.0031(10) 0.0039(9) -0.0023(10)
C11 0.0108(12) 0.0197(13) 0.0111(12) 0.0009(10) 0.0020(9) -0.0024(11)
C6 0.0073(12) 0.0142(12) 0.0104(12) 0.0015(9) 0.0002(9) 0.0034(10)
C3 0.0034(11) 0.0147(12) 0.0113(11) 0.0002(9) 0.0012(8) 0.0000(10)
C10 0.0105(12) 0.0206(13) 0.0113(12) -0.0017(10) 0.0016(9) 0.0001(11)
C7 0.0087(12) 0.0154(12) 0.0098(12) 0.0011(10) -0.0009(9) -0.0009(10)
C5 0.0088(12) 0.0098(11) 0.0146(12) 0.0007(10) 0.0031(9) -0.0028(10)
C4 0.0092(12) 0.0095(11) 0.0151(13) 0.0021(9) 0.0014(9) 0.0008(10)
C1 0.0083(11) 0.0092(11) 0.0154(12) 0.0002(10) 0.0020(9) 0.0003(10)
C13 0.0197(15) 0.0283(15) 0.0196(14) 0.0048(11) 0.0046(11) -0.0105(12)
C9 0.0154(14) 0.0224(14) 0.0231(14) 0.0029(11) 0.0066(11) -0.0037(11)
C8 0.0159(13) 0.0229(14) 0.0227(14) 0.0026(11) 0.0072(10) 0.0086(12)
C12 0.0143(14) 0.0299(15) 0.0230(15) -0.0025(12) 0.0074(11) 0.0018(12)
O5 0.0209(10) 0.0157(9) 0.0182(9) -0.0034(7) -0.0061(7) 0.0000(8)
O6 0.0059(9) 0.0320(10) 0.0148(9) -0.0030(8) -0.0011(7) -0.0001(8)
O7 0.0115(9) 0.0162(9) 0.0138(9) 0.0021(7) 0.0015(7) 0.0009(7)
C16 0.0239(15) 0.0300(15) 0.0148(14) 0.0045(11) 0.0071(11) -0.0062(12)
C14 0.0068(13) 0.0290(14) 0.0217(14) -0.0037(11) -0.0055(10) -0.0001(11)
C17 0.0231(15) 0.0254(15) 0.0312(17) 0.0040(13) 0.0087(12) -0.0052(13)
C18 0.0257(13) 0.0540(15) 0.0353(14) 0.0078(12) -0.0011(11) -0.0122(12)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
N2 Co1 N3 82.11(8)
N2 Co1 N4 178.54(8)
N3 Co1 N4 98.68(8)
N2 Co1 N5 98.82(8)
N3 Co1 N5 178.55(8)
N4 Co1 N5 80.37(8)
N2 Co1 N1 89.57(7)
N3 Co1 N1 89.92(8)
N4 Co1 N1 91.66(8)
N5 Co1 N1 91.21(8)
N2 Co1 Cl1 89.64(6)
N3 Co1 Cl1 89.38(6)
N4 Co1 Cl1 89.14(6)
N5 Co1 Cl1 89.51(6)
N1 Co1 Cl1 179.00(6)
O5 P1 O7 116.02(9)
O5 P1 O6 117.98(10)
O7 P1 O6 101.99(9)
O5 P1 C3 113.00(10)
O7 P1 C3 107.88(10)
O6 P1 C3 97.93(10)
C1 N1 C5 118.26(19)
C1 N1 Co1 121.80(15)
C5 N1 Co1 119.90(15)
N4 O2 H2 101(2)
N5 O1 H1 102(2)
C6 N2 O4 121.65(19)
C6 N2 Co1 116.45(15)
O4 N2 Co1 121.90(15)
C7 N3 O3 121.77(19)
C7 N3 Co1 115.90(16)
O3 N3 Co1 122.32(14)
C11 N5 O1 119.6(2)
C11 N5 Co1 117.47(16)
O1 N5 Co1 122.92(15)
C10 N4 O2 119.8(2)
C10 N4 Co1 117.60(15)
O2 N4 Co1 122.54(15)
C1 C2 C3 119.5(2)
C1 C2 H2A 120.2
C3 C2 H2A 120.2
N5 C11 C10 112.2(2)
N5 C11 C13 124.9(2)
C10 C11 C13 122.9(2)
N2 C6 C7 112.9(2)
N2 C6 C8 123.6(2)
C7 C6 C8 123.6(2)
C4 C3 C2 117.9(2)
C4 C3 P1 121.35(17)
C2 C3 P1 120.64(17)
N4 C10 C11 112.4(2)
N4 C10 C12 125.0(2)
C11 C10 C12 122.6(2)
N3 C7 C6 112.6(2)
N3 C7 C9 123.1(2)
C6 C7 C9 124.2(2)
N1 C5 C4 121.7(2)
N1 C5 H5A 119.2
C4 C5 H5A 119.2
C5 C4 C3 119.9(2)
C5 C4 H4A 120.0
C3 C4 H4A 120.0
N1 C1 C2 122.5(2)
N1 C1 H1A 118.8
C2 C1 H1A 118.8
C11 C13 H13A 109.5
C11 C13 H13B 109.5
H13A C13 H13B 109.5
C11 C13 H13C 109.5
H13A C13 H13C 109.5
H13B C13 H13C 109.5
C7 C9 H9A 109.5
C7 C9 H9B 109.5
H9A C9 H9B 109.5
C7 C9 H9C 109.5
H9A C9 H9C 109.5
H9B C9 H9C 109.5
C6 C8 H8A 109.5
C6 C8 H8B 109.5
H8A C8 H8B 109.5
C6 C8 H8C 109.5
H8A C8 H8C 109.5
H8B C8 H8C 109.5
C10 C12 H12A 109.5
C10 C12 H12B 109.5
H12A C12 H12B 109.5
C10 C12 H12C 109.5
H12A C12 H12C 109.5
H12B C12 H12C 109.5
C14 O6 P1 120.33(16)
C16 O7 P1 121.88(16)
O7 C16 C17 109.8(2)
O7 C16 H16A 109.7
C17 C16 H16A 109.7
O7 C16 H16B 109.7
C17 C16 H16B 109.7
H16A C16 H16B 108.2
O6 C14 C18 108.5(2)
O6 C14 H14A 110.0
C18 C14 H14A 110.0
O6 C14 H14B 110.0
C18 C14 H14B 110.0
H14A C14 H14B 108.4
C16 C17 H17A 109.5
C16 C17 H17B 109.5
H17A C17 H17B 109.5
C16 C17 H17C 109.5
H17A C17 H17C 109.5
H17B C17 H17C 109.5
C14 C18 H18A 109.5
C14 C18 H18B 109.5
H18A C18 H18B 109.5
C14 C18 H18C 109.5
H18A C18 H18C 109.5
H18B C18 H18C 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Co1 N2 1.8697(19)
Co1 N3 1.8729(19)
Co1 N4 1.891(2)
Co1 N5 1.892(2)
Co1 N1 1.9578(18)
Co1 Cl1 2.2181(6)
P1 O5 1.4522(17)
P1 O7 1.5587(16)
P1 O6 1.5605(17)
P1 C3 1.797(2)
N1 C1 1.342(3)
N1 C5 1.346(3)
O3 N3 1.327(2)
O2 N4 1.353(2)
O2 H2 0.874(18)
O1 N5 1.348(2)
O1 H1 0.884(17)
N2 C6 1.285(3)
N2 O4 1.329(2)
N3 C7 1.298(3)
N5 C11 1.288(3)
N4 C10 1.283(3)
C2 C1 1.371(3)
C2 C3 1.382(3)
C2 H2A 0.9500
C11 C10 1.466(3)
C11 C13 1.482(3)
C6 C7 1.459(3)
C6 C8 1.482(3)
C3 C4 1.381(3)
C10 C12 1.481(3)
C7 C9 1.480(3)
C5 C4 1.376(3)
C5 H5A 0.9500
C4 H4A 0.9500
C1 H1A 0.9500
C13 H13A 0.9800
C13 H13B 0.9800
C13 H13C 0.9800
C9 H9A 0.9800
C9 H9B 0.9800
C9 H9C 0.9800
C8 H8A 0.9800
C8 H8B 0.9800
C8 H8C 0.9800
C12 H12A 0.9800
C12 H12B 0.9800
C12 H12C 0.9800
O6 C14 1.455(3)
O7 C16 1.463(3)
C16 C17 1.488(4)
C16 H16A 0.9900
C16 H16B 0.9900
C14 C18 1.469(4)
C14 H14A 0.9900
C14 H14B 0.9900
C17 H17A 0.9800
C17 H17B 0.9800
C17 H17C 0.9800
C18 H18A 0.9800
C18 H18B 0.9800
C18 H18C 0.9800
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O1 H1 O4 0.884(17) 1.598(18) 2.476(2) 172(3)
|
1501646.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/16/1501646.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_1501646
loop_
_publ_author_name
'Kotani, Hiroaki'
'Ohkubo, Kei'
'Fukuzumi, Shunichi'
_publ_section_title
;
Formation of a long-lived electron-transfer state of a
naphthalene--quinolinium ion dyad and the \p-dimer radical cation
;
_journal_name_full 'Faraday Discussions'
_journal_page_first 89
_journal_paper_doi 10.1039/c1fd00084e
_journal_volume 155
_journal_year 2012
_chemical_formula_sum 'C26 H20 Cl N O4'
_chemical_formula_weight 445.88
_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 9.2173(5)
_cell_length_b 9.9916(8)
_cell_length_c 22.5665(17)
_cell_measurement_reflns_used 4352
_cell_measurement_temperature 123(2)
_cell_measurement_theta_max 27.4835
_cell_measurement_theta_min 3.0088
_cell_volume 2078.3(3)
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 123(2)
_diffrn_detector_area_resol_mean 14.6306
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type 'Rigaku AFC7R'
_diffrn_measurement_method dtintegrate.ref
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71070
_diffrn_reflns_av_R_equivalents 0.0272
_diffrn_reflns_av_sigmaI/netI 0.0469
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_k_min -7
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_limit_l_min -29
_diffrn_reflns_number 7640
_diffrn_reflns_theta_full 27.47
_diffrn_reflns_theta_max 27.47
_diffrn_reflns_theta_min 3.01
_exptl_absorpt_coefficient_mu 0.219
_exptl_absorpt_correction_T_max 0.9371
_exptl_absorpt_correction_T_min 0.8983
_exptl_absorpt_correction_type numerical
_exptl_crystal_colour Yellow
_exptl_crystal_density_diffrn 1.425
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description Prism
_exptl_crystal_F_000 928
_exptl_crystal_size_max 0.50
_exptl_crystal_size_mid 0.50
_exptl_crystal_size_min 0.30
_refine_diff_density_max 0.574
_refine_diff_density_min -0.452
_refine_diff_density_rms 0.086
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack 0.80(12)
_refine_ls_extinction_coef 0.003(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method SHELXL
_refine_ls_goodness_of_fit_ref 1.109
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 370
_refine_ls_number_reflns 4422
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.109
_refine_ls_R_factor_all 0.0798
_refine_ls_R_factor_gt 0.0653
_refine_ls_shift/su_max 0.006
_refine_ls_shift/su_mean 0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1256P)^2^+0.6647P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1852
_refine_ls_wR_factor_ref 0.2084
_reflns_number_gt 3524
_reflns_number_total 4422
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file c1fd00084e.txt
_cod_data_source_block crystal
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Numerical' changed to
'numerical' 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_values 1715 2011-07-08 13:25:40Z adriana
;
_cod_original_sg_symbol_H-M P212121
_cod_database_code 1501646
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -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
N1 N 0.4922(3) 0.8877(3) 0.14853(14) 0.0322(7) Uani 1 1 d
C1 C 0.3821(4) 0.8033(4) 0.13468(18) 0.0335(8) Uani 1 1 d
C2 C 0.3530(4) 0.7759(4) 0.07501(18) 0.0357(9) Uani 1 1 d
H1 H 0.282(6) 0.719(5) 0.069(2) 0.052(15) Uiso 1 1 d
C3 C 0.4273(4) 0.8378(4) 0.03000(18) 0.0345(9) Uani 1 1 d
C4 C 0.5349(4) 0.9340(4) 0.04469(18) 0.0356(9) Uani 1 1 d
C5 C 0.6129(5) 1.0072(5) 0.00122(19) 0.0384(9) Uani 1 1 d
H2 H 0.590(5) 0.992(5) -0.041(2) 0.048(13) Uiso 1 1 d
C6 C 0.7189(5) 1.0966(5) 0.0172(2) 0.0413(10) Uani 1 1 d
H3 H 0.761(5) 1.137(4) -0.0094(18) 0.025(10) Uiso 1 1 d
C7 C 0.7517(5) 1.1169(4) 0.07698(19) 0.0426(9) Uani 1 1 d
H4 H 0.838(4) 1.197(4) 0.0861(16) 0.025(10) Uiso 1 1 d
C8 C 0.6771(5) 1.0498(5) 0.1205(2) 0.0396(10) Uani 1 1 d
H5 H 0.687(6) 1.059(5) 0.155(2) 0.046(14) Uiso 1 1 d
C9 C 0.5685(4) 0.9567(4) 0.10492(18) 0.0334(8) Uani 1 1 d
C10 C 0.5396(5) 0.9057(5) 0.21099(18) 0.0374(9) Uani 1 1 d
H6 H 0.512(4) 0.993(5) 0.2230(18) 0.029(10) Uiso 1 1 d
H7 H 0.487(5) 0.842(5) 0.238(2) 0.038(12) Uiso 1 1 d
H8 H 0.648(5) 0.895(4) 0.2154(17) 0.026(10) Uiso 1 1 d
C11 C 0.3917(4) 0.8104(4) -0.03369(17) 0.0338(8) Uani 1 1 d
C12 C 0.4612(5) 0.7080(4) -0.06267(18) 0.0368(9) Uani 1 1 d
H9 H 0.531(6) 0.646(6) -0.038(3) 0.066(17) Uiso 1 1 d
C13 C 0.4373(5) 0.6865(5) -0.12376(19) 0.0390(9) Uani 1 1 d
H10 H 0.479(6) 0.628(5) -0.141(2) 0.049(15) Uiso 1 1 d
C14 C 0.3449(5) 0.7687(5) -0.15411(19) 0.0392(9) Uani 1 1 d
H11 H 0.340(5) 0.748(5) -0.196(2) 0.041(12) Uiso 1 1 d
C15 C 0.2657(4) 0.8714(4) -0.12522(16) 0.0334(8) Uani 1 1 d
C16 C 0.1638(5) 0.9507(5) -0.1549(2) 0.0426(10) Uani 1 1 d
H12 H 0.149(5) 0.937(5) -0.201(2) 0.041(13) Uiso 1 1 d
C17 C 0.0887(5) 1.0523(5) -0.1266(2) 0.0445(10) Uani 1 1 d
H13 H 0.007(4) 1.126(4) -0.1425(18) 0.032(11) Uiso 1 1 d
C18 C 0.1146(5) 1.0733(5) -0.0660(2) 0.0419(10) Uani 1 1 d
H14 H 0.050(6) 1.146(5) -0.045(2) 0.056(15) Uiso 1 1 d
C19 C 0.2123(4) 0.9990(4) -0.03527(18) 0.0357(9) Uani 1 1 d
H15 H 0.225(5) 1.006(5) 0.003(2) 0.044(13) Uiso 1 1 d
C20 C 0.2913(4) 0.8940(4) -0.06341(17) 0.0324(8) Uani 1 1 d
C21 C 0.2879(4) 0.7417(4) 0.18054(17) 0.0354(9) Uani 1 1 d
C22 C 0.2514(5) 0.6068(4) 0.17582(17) 0.0356(8) Uani 1 1 d
H16 H 0.306(4) 0.556(4) 0.1440(19) 0.031(11) Uiso 1 1 d
C23 C 0.1540(5) 0.5514(5) 0.2153(2) 0.0411(10) Uani 1 1 d
H17 H 0.134(5) 0.469(5) 0.212(2) 0.038(13) Uiso 1 1 d
C24 C 0.0939(5) 0.6276(5) 0.26015(18) 0.0408(10) Uani 1 1 d
H18 H 0.009(5) 0.582(4) 0.2866(19) 0.031(11) Uiso 1 1 d
C25 C 0.1302(5) 0.7628(5) 0.26521(19) 0.0411(10) Uani 1 1 d
H19 H 0.092(5) 0.809(4) 0.299(2) 0.036(11) Uiso 1 1 d
C26 C 0.2277(4) 0.8195(5) 0.22524(16) 0.0383(9) Uani 1 1 d
H20 H 0.248(5) 0.918(4) 0.2294(18) 0.033(10) Uiso 1 1 d
Cl1 Cl 0.24514(11) 1.18372(10) 0.13535(4) 0.0368(3) Uani 1 1 d
O1 O 0.3561(3) 1.2027(4) 0.09212(14) 0.0510(8) Uani 1 1 d
O2 O 0.1801(5) 1.0567(4) 0.12617(18) 0.0645(11) Uani 1 1 d
O3 O 0.1377(4) 1.2851(4) 0.12941(17) 0.0646(11) Uani 1 1 d
O4 O 0.3052(5) 1.1858(4) 0.19343(14) 0.0702(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
N1 0.0306(15) 0.0396(18) 0.0265(15) -0.0002(13) 0.0016(12) 0.0031(14)
C1 0.0290(17) 0.038(2) 0.0337(19) 0.0033(18) -0.0014(15) 0.0018(15)
C2 0.0321(18) 0.045(2) 0.0299(19) 0.0038(17) -0.0060(15) 0.0006(17)
C3 0.0332(19) 0.037(2) 0.033(2) -0.0033(16) -0.0022(15) 0.0030(16)
C4 0.0331(19) 0.039(2) 0.034(2) 0.0035(17) -0.0036(16) 0.0028(17)
C5 0.035(2) 0.042(2) 0.038(2) 0.0023(18) -0.0012(16) -0.0011(17)
C6 0.042(2) 0.040(2) 0.042(2) 0.0046(18) 0.0031(18) -0.0050(18)
C7 0.038(2) 0.043(2) 0.046(2) 0.0036(18) -0.005(2) -0.003(2)
C8 0.042(2) 0.041(2) 0.036(2) -0.0028(18) -0.0083(18) 0.0028(18)
C9 0.0288(18) 0.037(2) 0.0340(19) -0.0005(16) -0.0008(15) 0.0009(15)
C10 0.034(2) 0.052(3) 0.0259(19) -0.0052(18) -0.0040(15) 0.0018(19)
C11 0.0346(18) 0.0359(19) 0.0311(19) 0.0018(17) -0.0009(15) -0.0001(17)
C12 0.038(2) 0.041(2) 0.0316(19) -0.0015(17) 0.0001(15) -0.0017(17)
C13 0.037(2) 0.044(2) 0.035(2) -0.0036(19) 0.0011(16) -0.0001(19)
C14 0.036(2) 0.046(2) 0.036(2) -0.0057(18) 0.0049(17) -0.0064(18)
C15 0.0341(19) 0.0356(19) 0.0306(18) 0.0071(15) 0.0010(15) -0.0056(16)
C16 0.045(2) 0.045(2) 0.038(2) 0.0104(18) -0.0046(18) -0.0084(19)
C17 0.045(2) 0.046(2) 0.042(2) 0.009(2) -0.0077(19) 0.0016(19)
C18 0.037(2) 0.046(2) 0.044(2) 0.009(2) -0.0026(18) -0.0002(19)
C19 0.039(2) 0.037(2) 0.0317(19) 0.0009(16) -0.0001(16) -0.0023(16)
C20 0.0300(18) 0.037(2) 0.0306(18) 0.0024(15) -0.0021(14) -0.0026(15)
C21 0.036(2) 0.043(2) 0.0274(18) 0.0031(17) -0.0043(15) -0.0012(17)
C22 0.0374(18) 0.037(2) 0.0324(18) 0.0021(15) -0.0022(18) 0.0002(17)
C23 0.038(2) 0.042(3) 0.043(2) 0.0078(19) -0.0042(18) 0.0002(19)
C24 0.034(2) 0.055(3) 0.033(2) 0.0082(19) -0.0005(16) 0.0019(19)
C25 0.038(2) 0.055(3) 0.030(2) 0.0056(19) -0.0021(16) 0.0043(19)
C26 0.036(2) 0.054(2) 0.0250(17) 0.0000(17) 0.0001(15) 0.001(2)
Cl1 0.0418(5) 0.0364(5) 0.0322(5) 0.0016(4) 0.0023(4) -0.0010(4)
O1 0.0384(15) 0.066(2) 0.0486(18) 0.0148(16) 0.0106(13) -0.0002(16)
O2 0.083(3) 0.046(2) 0.065(2) -0.0021(17) 0.001(2) -0.0254(19)
O3 0.071(2) 0.062(2) 0.060(2) 0.0043(18) 0.0107(19) 0.034(2)
O4 0.096(3) 0.081(3) 0.0334(17) -0.0002(18) -0.0197(18) -0.005(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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C1 N1 C9 121.5(3)
C1 N1 C10 120.9(3)
C9 N1 C10 117.5(3)
N1 C1 C2 119.1(4)
N1 C1 C21 122.3(3)
C2 C1 C21 118.5(4)
C3 C2 C1 121.8(4)
C3 C2 H1 123(3)
C1 C2 H1 115(3)
C2 C3 C4 118.7(4)
C2 C3 C11 121.2(4)
C4 C3 C11 120.0(4)
C9 C4 C5 118.1(4)
C9 C4 C3 119.1(4)
C5 C4 C3 122.8(4)
C6 C5 C4 121.0(4)
C6 C5 H2 120(3)
C4 C5 H2 119(3)
C5 C6 C7 120.1(4)
C5 C6 H3 118(3)
C7 C6 H3 122(3)
C8 C7 C6 120.8(4)
C8 C7 H4 124.0(19)
C6 C7 H4 115.1(19)
C7 C8 C9 119.9(4)
C7 C8 H5 126(4)
C9 C8 H5 114(4)
N1 C9 C8 120.6(4)
N1 C9 C4 119.3(4)
C8 C9 C4 120.1(4)
N1 C10 H6 108(2)
N1 C10 H7 111(3)
H6 C10 H7 107(3)
N1 C10 H8 112(2)
H6 C10 H8 109(4)
H7 C10 H8 110(4)
C12 C11 C20 121.3(4)
C12 C11 C3 119.4(4)
C20 C11 C3 119.3(3)
C11 C12 C13 120.3(4)
C11 C12 H9 118(3)
C13 C12 H9 122(3)
C14 C13 C12 119.7(4)
C14 C13 H10 119(4)
C12 C13 H10 121(4)
C13 C14 C15 121.7(4)
C13 C14 H11 113(3)
C15 C14 H11 126(3)
C16 C15 C14 122.3(4)
C16 C15 C20 119.2(4)
C14 C15 C20 118.5(4)
C17 C16 C15 121.9(4)
C17 C16 H12 119(3)
C15 C16 H12 119(3)
C16 C17 C18 118.3(4)
C16 C17 H13 132(2)
C18 C17 H13 109(2)
C19 C18 C17 121.9(4)
C19 C18 H14 121(3)
C17 C18 H14 117(3)
C18 C19 C20 120.9(4)
C18 C19 H15 123(3)
C20 C19 H15 116(3)
C11 C20 C19 123.8(4)
C11 C20 C15 118.5(3)
C19 C20 C15 117.7(3)
C26 C21 C22 120.0(4)
C26 C21 C1 120.5(4)
C22 C21 C1 119.3(4)
C23 C22 C21 119.7(4)
C23 C22 H16 126(2)
C21 C22 H16 115(2)
C22 C23 C24 120.8(4)
C22 C23 H17 118(3)
C24 C23 H17 121(3)
C23 C24 C25 119.8(4)
C23 C24 H18 117(2)
C25 C24 H18 122(2)
C26 C25 C24 119.7(4)
C26 C25 H19 124(3)
C24 C25 H19 116(3)
C21 C26 C25 120.0(4)
C21 C26 H20 123(2)
C25 C26 H20 117(2)
O2 Cl1 O3 109.2(3)
O2 Cl1 O4 108.2(3)
O3 Cl1 O4 110.3(3)
O2 Cl1 O1 108.8(2)
O3 Cl1 O1 109.9(2)
O4 Cl1 O1 110.4(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
N1 C1 1.356(5)
N1 C9 1.392(5)
N1 C10 1.487(5)
C1 C2 1.400(6)
C1 C21 1.485(5)
C2 C3 1.373(6)
C2 H1 0.88(5)
C3 C4 1.420(6)
C3 C11 1.500(5)
C4 C9 1.412(6)
C4 C5 1.419(6)
C5 C6 1.372(6)
C5 H2 0.99(5)
C6 C7 1.398(6)
C6 H3 0.82(4)
C7 C8 1.374(6)
C7 H4 1.15(4)
C8 C9 1.411(6)
C8 H5 0.78(5)
C10 H6 0.95(5)
C10 H7 1.01(5)
C10 H8 1.01(4)
C11 C12 1.373(6)
C11 C20 1.415(5)
C12 C13 1.413(6)
C12 H9 1.05(6)
C13 C14 1.367(7)
C13 H10 0.80(5)
C14 C15 1.418(6)
C14 H11 0.97(5)
C15 C16 1.400(6)
C15 C20 1.433(5)
C16 C17 1.385(7)
C16 H12 1.06(4)
C17 C18 1.405(6)
C17 H13 1.11(4)
C18 C19 1.357(6)
C18 H14 1.06(5)
C19 C20 1.426(6)
C19 H15 0.88(5)
C21 C26 1.389(6)
C21 C22 1.393(6)
C22 C23 1.381(6)
C22 H16 1.01(4)
C23 C24 1.382(6)
C23 H17 0.85(5)
C24 C25 1.397(7)
C24 H18 1.08(4)
C25 C26 1.393(6)
C25 H19 0.96(5)
C26 H20 1.01(4)
Cl1 O2 1.419(3)
Cl1 O3 1.423(3)
Cl1 O4 1.423(3)
Cl1 O1 1.426(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
C9 N1 C1 C2 5.7(5)
C10 N1 C1 C2 -171.8(4)
C9 N1 C1 C21 -172.3(4)
C10 N1 C1 C21 10.1(6)
N1 C1 C2 C3 -3.7(6)
C21 C1 C2 C3 174.4(4)
C1 C2 C3 C4 -1.1(6)
C1 C2 C3 C11 -178.1(4)
C2 C3 C4 C9 4.0(6)
C11 C3 C4 C9 -179.0(4)
C2 C3 C4 C5 -177.3(4)
C11 C3 C4 C5 -0.2(6)
C9 C4 C5 C6 0.6(6)
C3 C4 C5 C6 -178.2(4)
C4 C5 C6 C7 0.0(7)
C5 C6 C7 C8 -1.2(7)
C6 C7 C8 C9 1.6(7)
C1 N1 C9 C8 176.4(4)
C10 N1 C9 C8 -6.0(5)
C1 N1 C9 C4 -2.8(5)
C10 N1 C9 C4 174.8(4)
C7 C8 C9 N1 179.8(4)
C7 C8 C9 C4 -1.0(6)
C5 C4 C9 N1 179.1(4)
C3 C4 C9 N1 -2.1(6)
C5 C4 C9 C8 -0.1(6)
C3 C4 C9 C8 178.7(4)
C2 C3 C11 C12 -89.7(5)
C4 C3 C11 C12 93.4(5)
C2 C3 C11 C20 92.8(5)
C4 C3 C11 C20 -84.2(5)
C20 C11 C12 C13 2.1(6)
C3 C11 C12 C13 -175.4(4)
C11 C12 C13 C14 0.3(6)
C12 C13 C14 C15 -3.4(6)
C13 C14 C15 C16 -175.8(4)
C13 C14 C15 C20 4.1(6)
C14 C15 C16 C17 -178.9(4)
C20 C15 C16 C17 1.2(6)
C15 C16 C17 C18 -1.3(7)
C16 C17 C18 C19 1.3(7)
C17 C18 C19 C20 -1.2(7)
C12 C11 C20 C19 177.9(4)
C3 C11 C20 C19 -4.7(6)
C12 C11 C20 C15 -1.4(6)
C3 C11 C20 C15 176.1(4)
C18 C19 C20 C11 -178.2(4)
C18 C19 C20 C15 1.1(6)
C16 C15 C20 C11 178.3(4)
C14 C15 C20 C11 -1.6(5)
C16 C15 C20 C19 -1.0(5)
C14 C15 C20 C19 179.1(4)
N1 C1 C21 C26 47.8(5)
C2 C1 C21 C26 -130.2(4)
N1 C1 C21 C22 -137.0(4)
C2 C1 C21 C22 45.0(5)
C26 C21 C22 C23 0.7(6)
C1 C21 C22 C23 -174.5(4)
C21 C22 C23 C24 -1.0(6)
C22 C23 C24 C25 0.9(6)
C23 C24 C25 C26 -0.5(6)
C22 C21 C26 C25 -0.3(6)
C1 C21 C26 C25 174.9(4)
C24 C25 C26 C21 0.2(6)
|
1501647.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/16/1501647.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_1501647
loop_
_publ_author_name
'Sergey Konchenko'
'Rosa Llusar'
'Pavel Petrov'
'Aleksandr Virovets'
'Artem Bogomyakov'
'Carlos Gomez Garcia'
'Victor Polo'
_publ_section_title
;
Synthesis, molecular and electronic structure of an incomplete cuboidal
Re3S4 cluster with an unusual quadruplet ground state
;
_journal_name_full 'Che. Commun.'
_journal_page_first 2713
_journal_paper_doi 10.1039/c2cc17287a
_journal_volume 48
_journal_year 2012
_chemical_formula_sum 'C84 H81 Br4 N3 P6 Re3 S4'
_chemical_formula_weight 2324.82
_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 98.4630(10)
_cell_angle_gamma 90.00
_cell_formula_units_Z 8
_cell_length_a 44.6606(12)
_cell_length_b 13.7072(4)
_cell_length_c 29.2555(8)
_cell_measurement_reflns_used 9930
_cell_measurement_temperature 100.0(2)
_cell_measurement_theta_max 31.5933
_cell_measurement_theta_min 2.3514
_cell_volume 17714.4(9)
_computing_cell_refinement 'Apex2 V.1.27 (Bruker, 2005)'
_computing_data_collection 'Apex2 V.1.27 (Bruker, 2005)'
_computing_data_reduction 'Apex2 V.1.27 (Bruker, 2005)'
_computing_molecular_graphics 'SHELXTL V6.22 (Bruker, 2000-2005)'
_computing_publication_material 'local programs'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 100.0(2)
_diffrn_detector_area_resol_mean 25
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.885
_diffrn_measurement_device_type 'Bruker X8Apex CCD detector'
_diffrn_measurement_method 'combined omega- and phi-scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0234
_diffrn_reflns_av_sigmaI/netI 0.0361
_diffrn_reflns_limit_h_max 64
_diffrn_reflns_limit_h_min -63
_diffrn_reflns_limit_k_max 19
_diffrn_reflns_limit_k_min -19
_diffrn_reflns_limit_l_max 42
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 54964
_diffrn_reflns_theta_full 25.00
_diffrn_reflns_theta_max 31.62
_diffrn_reflns_theta_min 1.68
_diffrn_standards_decay_% 0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 6.140
_exptl_absorpt_correction_T_max 1
_exptl_absorpt_correction_T_min 0.647042
_exptl_absorpt_correction_type empirical
_exptl_absorpt_process_details 'based on intensities (SADABS, Bruker, 2005)'
_exptl_crystal_colour black
_exptl_crystal_density_diffrn 1.743
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 9000
_exptl_crystal_size_max 0.34
_exptl_crystal_size_mid 0.28
_exptl_crystal_size_min 0.27
_refine_diff_density_max 3.921
_refine_diff_density_min -2.058
_refine_diff_density_rms 0.194
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.049
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 975
_refine_ls_number_reflns 26356
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.049
_refine_ls_R_factor_all 0.0473
_refine_ls_R_factor_gt 0.0339
_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^)+(0.0424P)^2^+204.4582P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0915
_refine_ls_wR_factor_ref 0.0976
_reflns_number_gt 21811
_reflns_number_total 26356
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file c2cc17287a.txt
_cod_data_source_block 1Br*3MeCN
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.
Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas
;
_cod_original_sg_symbol_H-M C2/c
_cod_database_code 1501647
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
Re1 Re 0.117681(4) 0.952507(12) 0.157264(5) 0.01078(4) Uani 1 1 d .
Re2 Re 0.157673(4) 0.808024(12) 0.138910(6) 0.01142(4) Uani 1 1 d .
Re3 Re 0.124680(4) 0.909887(13) 0.066194(6) 0.01293(4) Uani 1 1 d .
S1 S 0.16148(2) 0.97526(8) 0.12333(4) 0.01302(19) Uani 1 1 d .
S2 S 0.12067(2) 0.79290(8) 0.18409(4) 0.01391(19) Uani 1 1 d .
S3 S 0.07979(2) 0.91785(9) 0.09783(4) 0.0170(2) Uani 1 1 d .
S4 S 0.12782(3) 0.74409(9) 0.07379(4) 0.0178(2) Uani 1 1 d .
Br1 Br 0.148681(9) 1.00457(3) 0.235181(14) 0.01462(8) Uani 1 1 d .
Br2 Br 0.204697(10) 0.78283(4) 0.098859(15) 0.01770(9) Uani 1 1 d .
Br3 Br 0.114997(11) 1.08614(4) 0.034837(16) 0.02188(10) Uani 1 1 d .
Br4 Br 0.09046(2) 0.26234(5) 0.32931(2) 0.05018(18) Uani 1 1 d .
P11 P 0.10838(3) 1.13439(8) 0.15763(4) 0.0141(2) Uani 1 1 d .
P12 P 0.07582(2) 0.95829(8) 0.20536(4) 0.0132(2) Uani 1 1 d .
P21 P 0.20079(3) 0.81923(9) 0.20509(4) 0.0146(2) Uani 1 1 d .
P22 P 0.16527(3) 0.63017(9) 0.15813(4) 0.0192(2) Uani 1 1 d .
P31 P 0.16190(3) 0.92473(9) 0.00817(4) 0.0161(2) Uani 1 1 d .
P32 P 0.09124(3) 0.85986(10) -0.00692(4) 0.0179(2) Uani 1 1 d .
C11 C 0.08901(11) 1.1569(3) 0.20806(16) 0.0180(9) Uani 1 1 d .
H11F H 0.1035 1.1487 0.2369 0.022 Uiso 1 1 calc R
H11G H 0.0812 1.2246 0.2071 0.022 Uiso 1 1 calc R
C12 C 0.06277(10) 1.0850(3) 0.20756(17) 0.0184(9) Uani 1 1 d .
H12F H 0.0473 1.0982 0.1804 0.022 Uiso 1 1 calc R
H12G H 0.0532 1.0945 0.2357 0.022 Uiso 1 1 calc R
C21 C 0.21967(11) 0.6995(4) 0.20615(17) 0.0202(9) Uani 1 1 d .
H21F H 0.2302 0.6930 0.1788 0.024 Uiso 1 1 calc R
H21G H 0.2350 0.6944 0.2341 0.024 Uiso 1 1 calc R
C22 C 0.19668(12) 0.6181(4) 0.20612(17) 0.0229(10) Uani 1 1 d .
H22F H 0.1885 0.6189 0.2358 0.027 Uiso 1 1 calc R
H22G H 0.2069 0.5546 0.2036 0.027 Uiso 1 1 calc R
C31 C 0.13712(11) 0.9392(4) -0.04730(16) 0.0215(10) Uani 1 1 d .
H31F H 0.1255 1.0008 -0.0478 0.026 Uiso 1 1 calc R
H31G H 0.1492 0.9402 -0.0731 0.026 Uiso 1 1 calc R
C32 C 0.11576(11) 0.8519(4) -0.05182(16) 0.0229(10) Uani 1 1 d .
H32F H 0.1276 0.7905 -0.0482 0.027 Uiso 1 1 calc R
H32G H 0.1033 0.8517 -0.0827 0.027 Uiso 1 1 calc R
C111 C 0.08229(11) 1.2028(4) 0.11479(16) 0.0185(9) Uani 1 1 d .
C112 C 0.05461(11) 1.1611(4) 0.09560(17) 0.0222(10) Uani 1 1 d .
H11C H 0.0508 1.0941 0.1009 0.027 Uiso 1 1 calc R
C113 C 0.03270(13) 1.2175(4) 0.06878(19) 0.0290(12) Uani 1 1 d .
H11A H 0.0139 1.1892 0.0562 0.035 Uiso 1 1 calc R
C114 C 0.03845(15) 1.3150(5) 0.0604(2) 0.0372(14) Uani 1 1 d .
H11D H 0.0235 1.3534 0.0422 0.045 Uiso 1 1 calc R
C115 C 0.06577(15) 1.3559(4) 0.0784(2) 0.0379(14) Uani 1 1 d .
H11E H 0.0697 1.4223 0.0722 0.046 Uiso 1 1 calc R
C116 C 0.08778(13) 1.3004(4) 0.1058(2) 0.0289(11) Uani 1 1 d .
H11B H 0.1065 1.3293 0.1183 0.035 Uiso 1 1 calc R
C121 C 0.14275(11) 1.2078(3) 0.16667(17) 0.0191(9) Uani 1 1 d .
C122 C 0.15373(12) 1.2466(4) 0.20948(19) 0.0256(10) Uani 1 1 d .
H12A H 0.1427 1.2379 0.2346 0.031 Uiso 1 1 calc R
C123 C 0.18086(13) 1.2985(4) 0.2162(2) 0.0335(13) Uani 1 1 d .
H12C H 0.1884 1.3243 0.2458 0.040 Uiso 1 1 calc R
C124 C 0.19672(13) 1.3122(4) 0.1796(2) 0.0349(13) Uani 1 1 d .
H12D H 0.2151 1.3484 0.1840 0.042 Uiso 1 1 calc R
C125 C 0.18623(14) 1.2739(4) 0.1370(2) 0.0353(13) Uani 1 1 d .
H12E H 0.1975 1.2829 0.1122 0.042 Uiso 1 1 calc R
C126 C 0.15929(13) 1.2221(4) 0.1300(2) 0.0284(11) Uani 1 1 d .
H12B H 0.1520 1.1963 0.1003 0.034 Uiso 1 1 calc R
C131 C 0.04159(10) 0.8876(4) 0.18724(16) 0.0173(9) Uani 1 1 d .
C132 C 0.04250(12) 0.7966(4) 0.16542(19) 0.0247(10) Uani 1 1 d .
H13B H 0.0611 0.7725 0.1579 0.030 Uiso 1 1 calc R
C133 C 0.01635(12) 0.7420(4) 0.1549(2) 0.0309(12) Uani 1 1 d .
H13D H 0.0171 0.6806 0.1401 0.037 Uiso 1 1 calc R
C134 C -0.01099(12) 0.7762(5) 0.1659(2) 0.0307(12) Uani 1 1 d .
H13E H -0.0289 0.7383 0.1587 0.037 Uiso 1 1 calc R
C135 C -0.01209(11) 0.8659(4) 0.18749(17) 0.0243(10) Uani 1 1 d .
H13C H -0.0307 0.8896 0.1950 0.029 Uiso 1 1 calc R
C136 C 0.01401(10) 0.9209(4) 0.19801(16) 0.0195(9) Uani 1 1 d .
H13A H 0.0131 0.9823 0.2128 0.023 Uiso 1 1 calc R
C141 C 0.08494(10) 0.9215(3) 0.26560(15) 0.0157(8) Uani 1 1 d .
C142 C 0.08977(11) 0.9909(4) 0.30065(17) 0.0228(10) Uani 1 1 d .
H14B H 0.0885 1.0585 0.2933 0.027 Uiso 1 1 calc R
C143 C 0.09648(12) 0.9610(5) 0.34650(18) 0.0295(12) Uani 1 1 d .
H14D H 0.0995 1.0085 0.3704 0.035 Uiso 1 1 calc R
C144 C 0.09885(13) 0.8640(5) 0.35764(18) 0.0325(13) Uani 1 1 d .
H14E H 0.1039 0.8444 0.3890 0.039 Uiso 1 1 calc R
C145 C 0.09387(12) 0.7943(4) 0.32286(19) 0.0287(11) Uani 1 1 d .
H14C H 0.0954 0.7270 0.3305 0.034 Uiso 1 1 calc R
C146 C 0.08675(11) 0.8228(4) 0.27710(17) 0.0222(10) Uani 1 1 d .
H14A H 0.0831 0.7749 0.2535 0.027 Uiso 1 1 calc R
C211 C 0.22978(10) 0.9084(4) 0.19682(16) 0.0190(9) Uani 1 1 d .
C212 C 0.22341(11) 1.0078(4) 0.19823(16) 0.0202(9) Uani 1 1 d .
H21A H 0.2045 1.0287 0.2057 0.024 Uiso 1 1 calc R
C213 C 0.24461(12) 1.0768(4) 0.18871(18) 0.0270(11) Uani 1 1 d .
H21B H 0.2401 1.1444 0.1895 0.032 Uiso 1 1 calc R
C214 C 0.27256(13) 1.0460(5) 0.17801(19) 0.0314(12) Uani 1 1 d .
H21C H 0.2871 1.0927 0.1714 0.038 Uiso 1 1 calc R
C215 C 0.27909(12) 0.9478(5) 0.1771(2) 0.0316(12) Uani 1 1 d .
H21E H 0.2982 0.9273 0.1700 0.038 Uiso 1 1 calc R
C216 C 0.25802(11) 0.8783(5) 0.18638(18) 0.0266(11) Uani 1 1 d .
H21D H 0.2628 0.8108 0.1857 0.032 Uiso 1 1 calc R
C221 C 0.19690(11) 0.8275(4) 0.26646(15) 0.0186(9) Uani 1 1 d .
C222 C 0.21875(13) 0.8765(5) 0.29693(19) 0.0325(13) Uani 1 1 d .
H22C H 0.2341 0.9132 0.2854 0.039 Uiso 1 1 calc R
C223 C 0.21813(16) 0.8717(6) 0.3441(2) 0.0465(18) Uani 1 1 d .
H22E H 0.2330 0.9055 0.3648 0.056 Uiso 1 1 calc R
C224 C 0.19621(15) 0.8184(5) 0.36105(19) 0.0382(15) Uani 1 1 d .
H22D H 0.1963 0.8138 0.3935 0.046 Uiso 1 1 calc R
C225 C 0.17404(13) 0.7714(4) 0.33119(18) 0.0292(12) Uani 1 1 d .
H22B H 0.1587 0.7356 0.3431 0.035 Uiso 1 1 calc R
C226 C 0.17415(12) 0.7763(4) 0.28440(17) 0.0229(10) Uani 1 1 d .
H22A H 0.1586 0.7447 0.2640 0.027 Uiso 1 1 calc R
C231 C 0.17554(13) 0.5523(4) 0.11195(19) 0.0262(11) Uani 1 1 d .
C232 C 0.20558(13) 0.5377(4) 0.10699(18) 0.0261(11) Uani 1 1 d .
H23A H 0.2212 0.5642 0.1291 0.031 Uiso 1 1 calc R
C233 C 0.21302(15) 0.4844(4) 0.0699(2) 0.0343(13) Uani 1 1 d .
H23B H 0.2337 0.4745 0.0669 0.041 Uiso 1 1 calc R
C234 C 0.19086(19) 0.4461(5) 0.0376(2) 0.0476(19) Uani 1 1 d .
H23E H 0.1962 0.4108 0.0121 0.057 Uiso 1 1 calc R
C235 C 0.16092(19) 0.4588(5) 0.0422(3) 0.051(2) Uani 1 1 d .
H23D H 0.1456 0.4311 0.0201 0.062 Uiso 1 1 calc R
C236 C 0.15307(15) 0.5123(5) 0.0791(2) 0.0397(15) Uani 1 1 d .
H23C H 0.1323 0.5215 0.0820 0.048 Uiso 1 1 calc R
C241 C 0.13336(15) 0.5663(4) 0.1773(2) 0.0357(14) Uani 1 1 d .
C242 C 0.13756(18) 0.5050(5) 0.2149(3) 0.0490(19) Uani 1 1 d .
H24B H 0.1573 0.4957 0.2313 0.059 Uiso 1 1 calc R
C243 C 0.1132(2) 0.4563(6) 0.2292(4) 0.071(3) Uani 1 1 d .
H24D H 0.1162 0.4149 0.2555 0.085 Uiso 1 1 calc R
C244 C 0.0846(2) 0.4695(6) 0.2042(4) 0.074(3) Uani 1 1 d .
H24E H 0.0679 0.4368 0.2140 0.089 Uiso 1 1 calc R
C245 C 0.07960(18) 0.5287(5) 0.1656(4) 0.057(2) Uani 1 1 d .
H24C H 0.0599 0.5350 0.1483 0.069 Uiso 1 1 calc R
C246 C 0.10401(15) 0.5788(4) 0.1526(3) 0.0436(17) Uani 1 1 d .
H24A H 0.1009 0.6219 0.1269 0.052 Uiso 1 1 calc R
C311 C 0.18635(11) 1.0315(4) 0.01633(16) 0.0200(9) Uani 1 1 d .
C312 C 0.18090(13) 1.1142(4) -0.01153(18) 0.0256(11) Uani 1 1 d .
H31A H 0.1641 1.1155 -0.0356 0.031 Uiso 1 1 calc R
C313 C 0.19988(16) 1.1944(4) -0.0041(2) 0.0350(14) Uani 1 1 d .
H31D H 0.1963 1.2501 -0.0234 0.042 Uiso 1 1 calc R
C314 C 0.22404(15) 1.1937(5) 0.0313(2) 0.0362(14) Uani 1 1 d .
H31C H 0.2366 1.2496 0.0369 0.043 Uiso 1 1 calc R
C315 C 0.22987(13) 1.1116(5) 0.0585(2) 0.0325(13) Uani 1 1 d .
H31E H 0.2469 1.1103 0.0822 0.039 Uiso 1 1 calc R
C316 C 0.21105(12) 1.0309(4) 0.05132(18) 0.0248(10) Uani 1 1 d .
H31B H 0.2150 0.9749 0.0704 0.030 Uiso 1 1 calc R
C321 C 0.18699(10) 0.8315(4) -0.01140(15) 0.0181(9) Uani 1 1 d .
C322 C 0.18100(12) 0.7324(4) -0.00951(17) 0.0242(10) Uani 1 1 d .
H32A H 0.1651 0.7101 0.0060 0.029 Uiso 1 1 calc R
C323 C 0.19811(14) 0.6657(4) -0.03015(19) 0.0313(12) Uani 1 1 d .
H32B H 0.1939 0.5980 -0.0285 0.038 Uiso 1 1 calc R
C324 C 0.22126(14) 0.6973(5) -0.0532(2) 0.0357(14) Uani 1 1 d .
H32D H 0.2328 0.6512 -0.0675 0.043 Uiso 1 1 calc R
C325 C 0.22766(13) 0.7963(5) -0.05536(19) 0.0318(13) Uani 1 1 d .
H32E H 0.2436 0.8180 -0.0710 0.038 Uiso 1 1 calc R
C326 C 0.21058(11) 0.8632(4) -0.03463(17) 0.0237(10) Uani 1 1 d .
H32C H 0.2149 0.9309 -0.0362 0.028 Uiso 1 1 calc R
C331 C 0.05945(11) 0.9336(4) -0.03432(16) 0.0197(9) Uani 1 1 d .
C332 C 0.04716(12) 0.9087(4) -0.07970(17) 0.0235(10) Uani 1 1 d .
H33B H 0.0561 0.8580 -0.0952 0.028 Uiso 1 1 calc R
C333 C 0.02190(12) 0.9578(4) -0.10224(19) 0.0281(11) Uani 1 1 d .
H33A H 0.0138 0.9404 -0.1330 0.034 Uiso 1 1 calc R
C334 C 0.00876(12) 1.0310(5) -0.08031(19) 0.0312(12) Uani 1 1 d .
H33D H -0.0082 1.0653 -0.0960 0.037 Uiso 1 1 calc R
C335 C 0.02045(14) 1.0549(5) -0.0348(2) 0.0381(15) Uani 1 1 d .
H33E H 0.0111 1.1048 -0.0192 0.046 Uiso 1 1 calc R
C336 C 0.04574(12) 1.0059(5) -0.01209(19) 0.0314(13) Uani 1 1 d .
H33C H 0.0536 1.0225 0.0189 0.038 Uiso 1 1 calc R
C341 C 0.07280(12) 0.7417(4) -0.00557(18) 0.0254(11) Uani 1 1 d .
C342 C 0.0789(2) 0.6659(5) -0.0329(4) 0.073(3) Uani 1 1 d .
H34D H 0.0929 0.6740 -0.0540 0.087 Uiso 1 1 calc R
C343 C 0.0645(3) 0.5772(7) -0.0300(5) 0.101(5) Uani 1 1 d .
H34E H 0.0697 0.5241 -0.0481 0.121 Uiso 1 1 calc R
C344 C 0.0436(2) 0.5641(5) -0.0023(3) 0.062(2) Uani 1 1 d .
H34B H 0.0334 0.5033 -0.0019 0.074 Uiso 1 1 calc R
C345 C 0.03706(19) 0.6389(7) 0.0255(2) 0.060(2) Uani 1 1 d .
H34A H 0.0227 0.6300 0.0461 0.072 Uiso 1 1 calc R
C346 C 0.05156(18) 0.7279(6) 0.0232(2) 0.054(2) Uani 1 1 d .
H34C H 0.0467 0.7804 0.0420 0.065 Uiso 1 1 calc R
N1S N 0.21987(17) 1.1139(6) 0.3268(3) 0.072(2) Uani 1 1 d .
C11S C 0.19606(17) 1.1331(6) 0.3330(2) 0.0486(18) Uani 1 1 d .
C12S C 0.16583(19) 1.1558(9) 0.3422(3) 0.069(3) Uani 1 1 d .
N2AS N 0.1820(3) 0.5897(8) 0.4160(4) 0.051(3) Uani 0.604(11) 1 d P
N2BS N 0.1468(7) 0.542(3) 0.3247(15) 0.145(15) Uani 0.396(11) 1 d P
C21S C 0.1639(3) 0.5372(9) 0.4031(4) 0.046(3) Uani 0.604(11) 1 d P
C22S C 0.1402(6) 0.4987(19) 0.3573(12) 0.066(7) Uani 0.396(11) 1 d P
C23S C 0.1377(3) 0.4587(10) 0.3900(6) 0.107(5) Uani 1 1 d .
N3AS N 0.1025(7) 0.6421(17) 0.4308(11) 0.230(18) Uani 0.735(17) 1 d P
N3BS N 0.1369(9) 0.6885(19) 0.4404(9) 0.067(11) Uani 0.265(17) 1 d P
C31S C 0.0827(4) 0.6941(11) 0.4448(7) 0.139(7) Uani 1 1 d .
C32S C 0.0613(3) 0.7522(10) 0.4521(4) 0.065(4) Uani 0.735(17) 1 d P
C33S C 0.1122(12) 0.7040(18) 0.4512(8) 0.058(13) Uani 0.265(17) 1 d P
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Re1 0.01039(7) 0.01278(7) 0.00931(7) -0.00013(6) 0.00185(5) 0.00124(6)
Re2 0.01092(7) 0.01396(8) 0.00910(7) -0.00082(6) 0.00051(5) 0.00216(6)
Re3 0.01217(7) 0.01768(8) 0.00868(7) -0.00034(6) 0.00068(5) 0.00356(6)
S1 0.0124(4) 0.0161(5) 0.0107(5) 0.0004(4) 0.0023(3) 0.0008(4)
S2 0.0158(5) 0.0128(5) 0.0137(5) 0.0016(4) 0.0042(4) 0.0010(4)
S3 0.0119(4) 0.0258(6) 0.0129(5) -0.0031(4) 0.0008(4) 0.0016(4)
S4 0.0189(5) 0.0185(5) 0.0143(5) -0.0042(4) -0.0029(4) 0.0042(4)
Br1 0.01466(18) 0.01700(19) 0.01192(19) -0.00111(15) 0.00097(14) 0.00083(15)
Br2 0.01529(19) 0.0255(2) 0.01255(19) -0.00028(16) 0.00277(15) 0.00689(17)
Br3 0.0272(2) 0.0234(2) 0.0159(2) 0.00306(17) 0.00617(17) 0.00871(19)
Br4 0.0826(5) 0.0371(3) 0.0331(3) 0.0021(3) 0.0160(3) 0.0085(4)
P11 0.0152(5) 0.0129(5) 0.0143(5) 0.0002(4) 0.0030(4) 0.0012(4)
P12 0.0118(5) 0.0159(5) 0.0122(5) -0.0009(4) 0.0026(4) 0.0001(4)
P21 0.0136(5) 0.0181(5) 0.0115(5) -0.0006(4) 0.0000(4) 0.0022(4)
P22 0.0205(6) 0.0149(5) 0.0221(6) -0.0022(5) 0.0032(5) 0.0020(5)
P31 0.0152(5) 0.0234(6) 0.0100(5) 0.0003(4) 0.0026(4) 0.0022(4)
P32 0.0157(5) 0.0248(6) 0.0120(5) 0.0001(4) -0.0019(4) 0.0034(5)
C11 0.020(2) 0.017(2) 0.019(2) -0.0029(17) 0.0077(17) 0.0016(17)
C12 0.017(2) 0.018(2) 0.022(2) -0.0017(17) 0.0056(17) 0.0020(17)
C21 0.023(2) 0.022(2) 0.015(2) 0.0018(17) -0.0018(17) 0.0090(19)
C22 0.036(3) 0.015(2) 0.017(2) 0.0025(17) 0.0027(19) 0.010(2)
C31 0.020(2) 0.032(3) 0.011(2) 0.0013(18) -0.0005(16) 0.004(2)
C32 0.021(2) 0.036(3) 0.011(2) -0.0044(19) -0.0013(17) 0.005(2)
C111 0.021(2) 0.019(2) 0.015(2) 0.0026(17) 0.0022(17) 0.0051(18)
C112 0.024(2) 0.023(2) 0.019(2) 0.0008(18) 0.0006(18) 0.0058(19)
C113 0.026(3) 0.036(3) 0.023(3) 0.001(2) -0.003(2) 0.013(2)
C114 0.040(3) 0.033(3) 0.036(3) 0.011(3) -0.005(3) 0.016(3)
C115 0.048(4) 0.018(3) 0.044(4) 0.010(2) -0.005(3) 0.006(2)
C116 0.033(3) 0.020(2) 0.031(3) 0.007(2) -0.002(2) 0.003(2)
C121 0.020(2) 0.016(2) 0.022(2) 0.0020(17) 0.0031(18) -0.0003(17)
C122 0.028(3) 0.023(2) 0.024(3) 0.000(2) 0.000(2) -0.002(2)
C123 0.031(3) 0.029(3) 0.037(3) -0.005(2) -0.003(2) -0.009(2)
C124 0.027(3) 0.021(3) 0.057(4) -0.003(3) 0.006(3) -0.007(2)
C125 0.034(3) 0.025(3) 0.050(4) -0.002(3) 0.019(3) -0.010(2)
C126 0.029(3) 0.028(3) 0.031(3) -0.001(2) 0.011(2) -0.005(2)
C131 0.0140(19) 0.024(2) 0.014(2) 0.0004(17) 0.0012(15) -0.0004(17)
C132 0.019(2) 0.026(3) 0.029(3) -0.002(2) 0.0040(19) 0.000(2)
C133 0.024(3) 0.028(3) 0.040(3) -0.007(2) 0.002(2) -0.006(2)
C134 0.018(2) 0.038(3) 0.036(3) -0.005(2) 0.002(2) -0.009(2)
C135 0.013(2) 0.039(3) 0.021(2) -0.002(2) 0.0028(17) -0.002(2)
C136 0.016(2) 0.027(2) 0.016(2) -0.0022(18) 0.0040(16) -0.0022(18)
C141 0.0138(19) 0.023(2) 0.0113(19) 0.0004(16) 0.0041(15) -0.0009(17)
C142 0.022(2) 0.030(3) 0.017(2) 0.0002(19) 0.0049(18) -0.006(2)
C143 0.027(3) 0.048(3) 0.013(2) -0.003(2) 0.0023(19) -0.007(2)
C144 0.031(3) 0.052(4) 0.014(2) 0.006(2) 0.004(2) 0.000(3)
C145 0.027(3) 0.033(3) 0.027(3) 0.011(2) 0.010(2) 0.002(2)
C146 0.023(2) 0.027(3) 0.018(2) 0.0009(19) 0.0071(18) 0.003(2)
C211 0.017(2) 0.027(2) 0.013(2) -0.0038(17) -0.0005(16) -0.0028(18)
C212 0.019(2) 0.025(2) 0.016(2) -0.0030(18) -0.0006(17) -0.0024(19)
C213 0.027(3) 0.029(3) 0.023(3) -0.004(2) 0.000(2) -0.007(2)
C214 0.026(3) 0.045(3) 0.023(3) -0.003(2) 0.003(2) -0.014(2)
C215 0.015(2) 0.048(3) 0.033(3) -0.005(3) 0.006(2) -0.003(2)
C216 0.017(2) 0.038(3) 0.025(3) -0.002(2) 0.0025(19) 0.000(2)
C221 0.019(2) 0.025(2) 0.012(2) -0.0012(17) 0.0005(16) 0.0085(18)
C222 0.027(3) 0.051(4) 0.018(3) -0.002(2) 0.000(2) -0.006(3)
C223 0.047(4) 0.074(5) 0.016(3) -0.009(3) -0.004(2) -0.012(4)
C224 0.044(3) 0.057(4) 0.013(3) 0.004(2) 0.005(2) 0.006(3)
C225 0.031(3) 0.039(3) 0.019(2) 0.009(2) 0.007(2) 0.010(2)
C226 0.024(2) 0.028(3) 0.016(2) 0.0034(19) 0.0017(18) 0.004(2)
C231 0.031(3) 0.018(2) 0.028(3) -0.006(2) -0.003(2) 0.009(2)
C232 0.035(3) 0.022(2) 0.020(2) -0.0010(19) 0.002(2) 0.012(2)
C233 0.049(4) 0.028(3) 0.027(3) 0.000(2) 0.009(3) 0.019(3)
C234 0.078(5) 0.035(3) 0.027(3) -0.012(3) -0.003(3) 0.029(3)
C235 0.069(5) 0.035(4) 0.042(4) -0.020(3) -0.021(3) 0.016(3)
C236 0.037(3) 0.032(3) 0.045(4) -0.017(3) -0.012(3) 0.011(3)
C241 0.040(3) 0.014(2) 0.059(4) -0.005(2) 0.023(3) -0.002(2)
C242 0.054(4) 0.025(3) 0.075(5) 0.011(3) 0.030(4) 0.002(3)
C243 0.086(7) 0.031(4) 0.109(8) 0.020(4) 0.053(6) 0.004(4)
C244 0.060(5) 0.034(4) 0.142(10) 0.000(5) 0.059(6) -0.007(4)
C245 0.042(4) 0.028(3) 0.109(7) -0.007(4) 0.030(4) -0.002(3)
C246 0.038(3) 0.020(3) 0.077(5) -0.011(3) 0.019(3) -0.008(2)
C311 0.023(2) 0.024(2) 0.014(2) -0.0020(17) 0.0073(17) -0.0018(19)
C312 0.038(3) 0.024(2) 0.017(2) -0.0002(19) 0.009(2) 0.002(2)
C313 0.059(4) 0.024(3) 0.024(3) -0.002(2) 0.014(3) -0.006(3)
C314 0.050(4) 0.038(3) 0.023(3) -0.006(2) 0.014(3) -0.021(3)
C315 0.028(3) 0.046(3) 0.025(3) -0.002(2) 0.007(2) -0.013(3)
C316 0.023(2) 0.033(3) 0.019(2) 0.001(2) 0.0045(18) -0.003(2)
C321 0.016(2) 0.027(2) 0.011(2) -0.0017(17) 0.0017(15) 0.0064(18)
C322 0.025(2) 0.030(3) 0.016(2) -0.0008(19) -0.0006(18) 0.004(2)
C323 0.043(3) 0.027(3) 0.023(3) -0.006(2) 0.001(2) 0.012(2)
C324 0.037(3) 0.047(4) 0.023(3) -0.010(2) 0.003(2) 0.019(3)
C325 0.026(3) 0.049(4) 0.022(3) -0.002(2) 0.009(2) 0.011(3)
C326 0.020(2) 0.035(3) 0.017(2) -0.001(2) 0.0060(18) 0.006(2)
C331 0.017(2) 0.025(2) 0.016(2) 0.0041(18) -0.0020(16) 0.0016(18)
C332 0.023(2) 0.026(2) 0.018(2) 0.0008(19) -0.0054(18) -0.001(2)
C333 0.026(3) 0.036(3) 0.020(2) 0.006(2) -0.0086(19) 0.001(2)
C334 0.022(2) 0.044(3) 0.025(3) 0.007(2) -0.006(2) 0.009(2)
C335 0.032(3) 0.053(4) 0.028(3) 0.000(3) 0.000(2) 0.023(3)
C336 0.025(3) 0.049(4) 0.018(2) -0.005(2) -0.0019(19) 0.014(2)
C341 0.025(2) 0.029(3) 0.018(2) 0.005(2) -0.0098(18) -0.001(2)
C342 0.072(6) 0.026(3) 0.131(9) -0.022(5) 0.051(6) -0.007(4)
C343 0.090(8) 0.033(4) 0.193(14) -0.026(6) 0.063(9) -0.010(5)
C344 0.066(5) 0.027(3) 0.088(7) 0.021(4) -0.007(5) -0.010(3)
C345 0.060(5) 0.085(6) 0.030(4) 0.011(4) -0.006(3) -0.045(5)
C346 0.062(5) 0.069(5) 0.033(4) -0.016(3) 0.011(3) -0.039(4)
N1S 0.054(4) 0.071(5) 0.097(6) -0.022(5) 0.028(4) -0.032(4)
C11S 0.049(4) 0.061(5) 0.038(4) 0.002(3) 0.011(3) -0.028(4)
C12S 0.046(4) 0.125(9) 0.038(4) -0.008(5) 0.012(3) 0.005(5)
N2AS 0.071(8) 0.039(6) 0.044(6) 0.013(5) 0.008(5) -0.004(5)
N2BS 0.067(18) 0.18(4) 0.19(4) -0.03(3) 0.02(2) -0.02(2)
C21S 0.063(8) 0.032(6) 0.042(7) 0.001(5) 0.005(6) 0.011(6)
C22S 0.048(12) 0.049(14) 0.10(2) -0.028(14) 0.014(14) -0.004(11)
C23S 0.113(11) 0.071(8) 0.123(12) -0.013(8) -0.027(9) 0.001(8)
N3AS 0.29(3) 0.113(17) 0.35(3) 0.15(2) 0.25(3) 0.14(2)
N3BS 0.12(3) 0.030(13) 0.040(15) 0.007(11) -0.031(16) -0.005(16)
C31S 0.099(11) 0.098(11) 0.23(2) 0.102(12) 0.048(12) -0.005(9)
C32S 0.072(8) 0.073(9) 0.056(7) -0.011(6) 0.026(6) -0.005(7)
C33S 0.14(4) 0.012(11) 0.014(11) 0.010(8) -0.012(16) 0.006(16)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.2310 '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
Re2 Re1 Re3 59.960(6)
S1 Re1 Re2 53.89(3)
S1 Re1 Re3 53.48(3)
S1 Re1 Br1 87.97(3)
S1 Re1 P11 91.06(4)
S1 Re1 P12 167.09(4)
S2 Re1 Re2 52.09(3)
S2 Re1 Re3 96.70(3)
S2 Re1 S1 105.01(4)
S2 Re1 Br1 88.02(3)
S2 Re1 P11 158.33(4)
S2 Re1 P12 81.38(4)
S3 Re1 Re2 97.46(3)
S3 Re1 Re3 53.54(3)
S3 Re1 S1 106.01(4)
S3 Re1 S2 93.47(4)
S3 Re1 Br1 164.98(3)
S3 Re1 P11 95.99(4)
S3 Re1 P12 84.48(4)
Br1 Re1 Re2 95.235(11)
Br1 Re1 Re3 141.131(12)
P11 Re1 Re2 144.74(3)
P11 Re1 Re3 104.61(3)
P11 Re1 Br1 77.95(3)
P12 Re1 Re2 133.47(3)
P12 Re1 Re3 137.90(3)
P12 Re1 Br1 80.96(3)
P12 Re1 P11 80.18(4)
Re1 Re2 Re3 60.340(6)
S1 Re2 Re1 53.65(3)
S1 Re2 Re3 53.59(3)
S1 Re2 Br2 87.44(3)
S1 Re2 P21 91.18(4)
S1 Re2 P22 168.22(4)
S2 Re2 Re1 53.70(3)
S2 Re2 Re3 98.17(3)
S2 Re2 S1 106.35(4)
S2 Re2 S4 93.65(4)
S2 Re2 Br2 164.65(3)
S2 Re2 P21 95.59(4)
S2 Re2 P22 82.37(4)
S4 Re2 Re1 96.87(3)
S4 Re2 Re3 52.26(3)
S4 Re2 S1 104.93(4)
S4 Re2 Br2 89.10(3)
S4 Re2 P21 158.35(4)
S4 Re2 P22 81.96(4)
Br2 Re2 Re1 140.907(13)
Br2 Re2 Re3 95.458(12)
P21 Re2 Re1 104.38(3)
P21 Re2 Re3 144.54(3)
P21 Re2 Br2 77.06(3)
P22 Re2 Re1 135.99(3)
P22 Re2 Re3 134.22(3)
P22 Re2 Br2 83.07(3)
P22 Re2 P21 79.92(4)
Re2 Re3 Re1 59.699(6)
S1 Re3 Re1 53.41(3)
S1 Re3 Re2 53.76(3)
S1 Re3 Br3 87.65(3)
S1 Re3 P31 89.25(4)
S1 Re3 P32 167.59(4)
S3 Re3 Re1 52.21(3)
S3 Re3 Re2 96.30(3)
S3 Re3 S1 104.65(4)
S3 Re3 Br3 89.34(3)
S3 Re3 P31 160.48(4)
S3 Re3 P32 84.99(4)
S4 Re3 Re1 97.43(3)
S4 Re3 Re2 53.70(3)
S4 Re3 S1 106.52(4)
S4 Re3 S3 92.98(4)
S4 Re3 Br3 164.50(3)
S4 Re3 P31 96.16(4)
S4 Re3 P32 80.33(4)
Br3 Re3 Re1 96.100(12)
Br3 Re3 Re2 141.214(14)
P31 Re3 Re1 142.54(3)
P31 Re3 Re2 103.02(3)
P31 Re3 Br3 77.40(3)
P32 Re3 Re1 137.12(3)
P32 Re3 Re2 134.03(3)
P32 Re3 Br3 84.61(3)
P32 Re3 P31 79.61(4)
Re1 S1 Re2 72.47(3)
Re1 S1 Re3 73.11(3)
Re3 S1 Re2 72.66(3)
Re2 S2 Re1 74.21(3)
Re1 S3 Re3 74.25(3)
Re3 S4 Re2 74.04(3)
C11 P11 Re1 105.38(16)
C111 P11 Re1 126.05(16)
C111 P11 C11 97.8(2)
C121 P11 Re1 114.20(16)
C121 P11 C11 106.0(2)
C121 P11 C111 104.7(2)
C12 P12 Re1 108.49(15)
C131 P12 Re1 118.96(15)
C131 P12 C12 104.9(2)
C141 P12 Re1 117.17(14)
C141 P12 C12 104.8(2)
C141 P12 C131 101.1(2)
C21 P21 Re2 104.71(16)
C211 P21 Re2 114.53(16)
C211 P21 C21 105.5(2)
C211 P21 C221 105.1(2)
C221 P21 Re2 125.66(16)
C221 P21 C21 98.5(2)
C22 P22 Re2 108.68(16)
C231 P22 Re2 116.11(18)
C231 P22 C22 105.4(2)
C241 P22 Re2 116.55(19)
C241 P22 C22 105.3(3)
C241 P22 C231 103.8(3)
C31 P31 Re3 103.28(16)
C31 P31 C321 96.6(2)
C311 P31 Re3 114.43(15)
C311 P31 C31 107.5(2)
C311 P31 C321 102.6(2)
C321 P31 Re3 129.47(16)
C32 P32 Re3 106.44(16)
C331 P32 Re3 123.18(17)
C331 P32 C32 103.1(2)
C341 P32 Re3 115.97(16)
C341 P32 C32 106.4(3)
C341 P32 C331 100.2(2)
C12 C11 P11 109.5(3)
C11 C12 P12 111.3(3)
C22 C21 P21 110.3(3)
C21 C22 P22 112.0(3)
C32 C31 P31 106.3(3)
C31 C32 P32 108.9(3)
C112 C111 P11 119.8(4)
C116 C111 P11 120.5(4)
C116 C111 C112 119.1(5)
C113 C112 C111 120.2(5)
C114 C113 C112 120.0(6)
C115 C114 C113 120.1(5)
C114 C115 C116 120.4(5)
C111 C116 C115 120.2(5)
C122 C121 P11 121.5(4)
C122 C121 C126 118.8(5)
C126 C121 P11 119.6(4)
C121 C122 C123 120.6(5)
C124 C123 C122 119.7(6)
C125 C124 C123 120.5(5)
C124 C125 C126 120.3(6)
C125 C126 C121 120.1(5)
C132 C131 P12 121.7(4)
C136 C131 P12 119.5(4)
C136 C131 C132 118.7(4)
C133 C132 C131 120.1(5)
C132 C133 C134 120.5(5)
C135 C134 C133 119.8(5)
C136 C135 C134 120.0(5)
C135 C136 C131 121.0(5)
C142 C141 P12 120.8(4)
C142 C141 C146 119.2(4)
C146 C141 P12 120.0(4)
C143 C142 C141 119.7(5)
C144 C143 C142 120.9(5)
C143 C144 C145 119.6(5)
C146 C145 C144 120.2(5)
C145 C146 C141 120.2(5)
C212 C211 P21 120.0(4)
C212 C211 C216 119.2(5)
C216 C211 P21 120.7(4)
C211 C212 C213 120.6(5)
C212 C213 C214 119.7(5)
C215 C214 C213 119.9(5)
C214 C215 C216 120.9(5)
C215 C216 C211 119.7(5)
C222 C221 P21 119.9(4)
C222 C221 C226 118.7(5)
C226 C221 P21 121.0(4)
C223 C222 C221 119.9(6)
C224 C223 C222 120.3(6)
C223 C224 C225 120.3(5)
C226 C225 C224 120.1(5)
C225 C226 C221 120.6(5)
C232 C231 P22 120.9(4)
C232 C231 C236 118.7(5)
C236 C231 P22 120.3(4)
C231 C232 C233 120.3(6)
C234 C233 C232 120.6(6)
C233 C234 C235 120.0(6)
C234 C235 C236 120.1(6)
C235 C236 C231 120.2(6)
C242 C241 P22 121.1(6)
C242 C241 C246 119.3(6)
C246 C241 P22 119.6(5)
C241 C242 C243 120.9(8)
C244 C243 C242 118.7(9)
C245 C244 C243 122.0(7)
C244 C245 C246 118.4(8)
C245 C246 C241 120.6(8)
C312 C311 P31 121.8(4)
C316 C311 P31 119.2(4)
C316 C311 C312 119.1(5)
C313 C312 C311 120.1(5)
C314 C313 C312 120.4(6)
C313 C314 C315 119.8(5)
C314 C315 C316 120.3(6)
C315 C316 C311 120.3(5)
C322 C321 P31 122.4(4)
C322 C321 C326 119.1(5)
C326 C321 P31 117.9(4)
C323 C322 C321 120.4(5)
C324 C323 C322 120.4(6)
C323 C324 C325 120.1(5)
C326 C325 C324 119.7(5)
C325 C326 C321 120.4(5)
C332 C331 P32 116.8(4)
C336 C331 P32 124.1(4)
C336 C331 C332 118.9(5)
C333 C332 C331 120.5(5)
C334 C333 C332 120.3(5)
C333 C334 C335 119.6(5)
C336 C335 C334 120.2(6)
C331 C336 C335 120.4(5)
C342 C341 P32 122.4(5)
C342 C341 C346 118.2(6)
C346 C341 P32 119.4(5)
C341 C342 C343 119.9(9)
C344 C343 C342 121.9(9)
C343 C344 C345 119.3(8)
C344 C345 C346 119.3(8)
C341 C346 C345 121.3(8)
N1S C11S C12S 178.2(10)
N2AS C21S C22S 145.7(17)
N2AS C21S C23S 174.0(14)
C23S C21S C22S 40.3(11)
N2BS C22S C21S 106(2)
C23S C22S N2BS 171(3)
C23S C22S C21S 66.3(19)
C22S C23S C21S 73.5(17)
C31S N3AS N3BS 114(3)
C33S N3AS N3BS 47(3)
C33S N3AS C31S 68(3)
C33S N3BS N3AS 41.5(19)
N3AS C31S C32S 170(2)
N3AS C31S C33S 50(2)
C32S C31S C33S 132(2)
N3AS C33S N3BS 91(3)
N3AS C33S C31S 62(3)
N3BS C33S C31S 152(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Re1 Re2 2.7718(2)
Re1 Re3 2.7897(2)
Re1 S1 2.3411(10)
Re1 S2 2.3215(11)
Re1 S3 2.2907(11)
Re1 Br1 2.5872(5)
Re1 P11 2.5277(12)
Re1 P12 2.5010(11)
Re2 Re3 2.7791(2)
Re2 S1 2.3483(11)
Re2 S2 2.2727(10)
Re2 S4 2.3297(11)
Re2 Br2 2.5743(5)
Re2 P21 2.5265(11)
Re2 P22 2.5136(13)
Re3 S1 2.3430(11)
Re3 S3 2.3312(11)
Re3 S4 2.2858(12)
Re3 Br3 2.5978(5)
Re3 P31 2.5527(11)
Re3 P32 2.5170(12)
P11 C11 1.843(5)
P11 C111 1.838(5)
P11 C121 1.822(5)
P12 C12 1.836(5)
P12 C131 1.822(5)
P12 C141 1.821(5)
P21 C21 1.844(5)
P21 C211 1.823(5)
P21 C221 1.833(5)
P22 C22 1.840(5)
P22 C231 1.832(5)
P22 C241 1.829(6)
P31 C31 1.836(5)
P31 C311 1.820(5)
P31 C321 1.846(5)
P32 C32 1.833(5)
P32 C331 1.829(5)
P32 C341 1.821(6)
C11 C12 1.529(6)
C21 C22 1.516(7)
C31 C32 1.524(7)
C111 C112 1.403(7)
C111 C116 1.392(7)
C112 C113 1.395(7)
C113 C114 1.389(9)
C114 C115 1.375(9)
C115 C116 1.398(8)
C121 C122 1.383(7)
C121 C126 1.403(7)
C122 C123 1.394(8)
C123 C124 1.379(9)
C124 C125 1.369(9)
C125 C126 1.386(8)
C131 C132 1.405(7)
C131 C136 1.393(6)
C132 C133 1.383(7)
C133 C134 1.389(8)
C134 C135 1.386(8)
C135 C136 1.384(7)
C141 C142 1.393(7)
C141 C146 1.393(7)
C142 C143 1.393(7)
C143 C144 1.369(9)
C144 C145 1.389(9)
C145 C146 1.386(7)
C211 C212 1.393(7)
C211 C216 1.403(7)
C212 C213 1.396(7)
C213 C214 1.396(8)
C214 C215 1.378(9)
C215 C216 1.394(8)
C221 C222 1.394(7)
C221 C226 1.399(7)
C222 C223 1.387(8)
C223 C224 1.371(10)
C224 C225 1.380(9)
C225 C226 1.371(7)
C231 C232 1.385(8)
C231 C236 1.396(8)
C232 C233 1.389(7)
C233 C234 1.368(10)
C234 C235 1.374(11)
C235 C236 1.393(9)
C241 C242 1.376(10)
C241 C246 1.410(10)
C242 C243 1.391(10)
C243 C244 1.389(15)
C244 C245 1.384(14)
C245 C246 1.387(9)
C311 C312 1.397(7)
C311 C316 1.390(7)
C312 C313 1.385(8)
C313 C314 1.381(9)
C314 C315 1.381(9)
C315 C316 1.386(8)
C321 C322 1.387(7)
C321 C326 1.404(7)
C322 C323 1.385(7)
C323 C324 1.383(9)
C324 C325 1.391(9)
C325 C326 1.388(7)
C331 C332 1.402(7)
C331 C336 1.378(7)
C332 C333 1.393(7)
C333 C334 1.368(8)
C334 C335 1.396(8)
C335 C336 1.396(8)
C341 C342 1.363(9)
C341 C346 1.371(9)
C342 C343 1.383(12)
C343 C344 1.334(14)
C344 C345 1.366(13)
C345 C346 1.388(10)
N1S C11S 1.136(10)
C11S C12S 1.449(11)
N2AS C21S 1.107(16)
N2BS C22S 1.19(5)
C21S C22S 1.67(3)
C21S C23S 1.59(2)
C22S C23S 1.12(3)
N3AS N3BS 1.65(5)
N3AS C31S 1.25(2)
N3AS C33S 1.09(4)
N3BS C33S 1.21(5)
C31S C32S 1.28(2)
C31S C33S 1.31(5)
|
1501648.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/16/1501648.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_1501648
loop_
_publ_author_name
'Sergey Konchenko'
'Rosa Llusar'
'Pavel Petrov'
'Aleksandr Virovets'
'Artem Bogomyakov'
'Carlos Gomez Garcia'
'Victor Polo'
_publ_section_title
;
Synthesis, molecular and electronic structure of an incomplete cuboidal
Re3S4 cluster with an unusual quadruplet ground state
;
_journal_name_full 'Che. Commun.'
_journal_page_first 2713
_journal_paper_doi 10.1039/c2cc17287a
_journal_volume 48
_journal_year 2012
_chemical_formula_sum 'C82.5 H81 Br2.6 Cl10.4 P6 Re3 S4'
_chemical_formula_weight 2521.58
_chemical_name_systematic
;
?
;
_space_group_IT_number 2
_symmetry_cell_setting triclinic
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 80.5320(10)
_cell_angle_beta 72.6390(10)
_cell_angle_gamma 83.4320(10)
_cell_formula_units_Z 2
_cell_length_a 13.6395(3)
_cell_length_b 15.3991(3)
_cell_length_c 22.8431(5)
_cell_measurement_reflns_used 9927
_cell_measurement_temperature 100.0(2)
_cell_measurement_theta_max 30.6227
_cell_measurement_theta_min 2.4379
_cell_volume 4506.04(17)
_computing_cell_refinement 'Apex2 V.1.27 (Bruker, 2005)'
_computing_data_collection 'Apex2 V.1.27 (Bruker, 2005)'
_computing_data_reduction 'Apex2 V.1.27 (Bruker, 2005)'
_computing_molecular_graphics 'SHELXTL V6.22 (Bruker, 2000-2005)'
_computing_publication_material 'local programs'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 100.0(2)
_diffrn_detector_area_resol_mean 25
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.771
_diffrn_measurement_device_type 'Bruker X8Apex CCD detector'
_diffrn_measurement_method 'combined omega- and phi-scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0273
_diffrn_reflns_av_sigmaI/netI 0.0519
_diffrn_reflns_limit_h_max 19
_diffrn_reflns_limit_h_min -19
_diffrn_reflns_limit_k_max 21
_diffrn_reflns_limit_k_min -18
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_limit_l_min -33
_diffrn_reflns_number 47320
_diffrn_reflns_theta_full 25.00
_diffrn_reflns_theta_max 31.57
_diffrn_reflns_theta_min 1.89
_diffrn_standards_decay_% 0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 5.723
_exptl_absorpt_correction_T_max 1
_exptl_absorpt_correction_T_min 0.779722
_exptl_absorpt_correction_type empirical
_exptl_absorpt_process_details 'based on intensities (SADABS, Bruker, 2005)'
_exptl_crystal_colour brown
_exptl_crystal_density_diffrn 1.858
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 2446
_exptl_crystal_size_max 0.20
_exptl_crystal_size_mid 0.20
_exptl_crystal_size_min 0.20
_refine_diff_density_max 2.747
_refine_diff_density_min -3.012
_refine_diff_density_rms 0.219
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.059
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 1032
_refine_ls_number_reflns 23261
_refine_ls_number_restraints 11
_refine_ls_restrained_S_all 1.060
_refine_ls_R_factor_all 0.0761
_refine_ls_R_factor_gt 0.0497
_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^)+(0.0401P)^2^+61.1813P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1151
_refine_ls_wR_factor_ref 0.1290
_reflns_number_gt 17767
_reflns_number_total 23261
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file c2cc17287a.txt
_cod_data_source_block 2Br*4.5CH2Cl2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.
Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas
;
_cod_original_sg_symbol_H-M P-1
_cod_original_formula_sum 'C82.50 H81 Br2.60 Cl10.40 P6 Re3 S4'
_cod_database_code 1501648
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re 0.34141(2) 0.276422(19) 0.187418(12) 0.01637(7) Uani 1 1 d . . .
Re2 Re 0.14501(2) 0.313309(18) 0.262628(12) 0.01511(6) Uani 1 1 d . . .
Re3 Re 0.21759(2) 0.139515(18) 0.249640(12) 0.01521(6) Uani 1 1 d . . .
S1 S 0.18604(13) 0.24857(12) 0.17196(8) 0.0178(3) Uani 1 1 d . . .
S2 S 0.29893(14) 0.36436(12) 0.26409(8) 0.0206(4) Uani 1 1 d . . .
S3 S 0.38287(13) 0.15181(12) 0.25061(8) 0.0196(3) Uani 1 1 d . . .
S4 S 0.14825(13) 0.20015(11) 0.34234(8) 0.0160(3) Uani 1 1 d . . .
Br1 Br 0.43208(8) 0.20127(7) 0.09289(5) 0.0242(4) Uani 0.484(4) 1 d P . .
Cl1T Cl 0.43208(8) 0.20127(7) 0.09289(5) 0.0242(4) Uani 0.52 1 d P . .
Br2 Br 0.11182(8) 0.45815(7) 0.19634(5) 0.0233(3) Uani 0.566(4) 1 d P . .
Cl2T Cl 0.11182(8) 0.45815(7) 0.19634(5) 0.0233(3) Uani 0.43 1 d P . .
Br3 Br 0.04403(8) 0.08199(7) 0.26023(5) 0.0237(3) Uani 0.549(4) 1 d P . .
Cl3T Cl 0.04403(8) 0.08199(7) 0.26023(5) 0.0237(3) Uani 0.45 1 d P . .
Br4 Br 0.7598(5) 0.6180(3) 0.3304(4) 0.155(3) Uani 0.571(12) 1 d P A 1
Br4 Br 0.7843(4) 0.6267(4) 0.2919(8) 0.196(6) Uani 0.429(12) 1 d P A 2
P11 P 0.52136(15) 0.30770(14) 0.18000(9) 0.0242(4) Uani 1 1 d . . .
P12 P 0.36860(15) 0.40223(14) 0.10003(9) 0.0225(4) Uani 1 1 d . . .
P21 P 0.07392(15) 0.40732(12) 0.34695(9) 0.0196(4) Uani 1 1 d . . .
P22 P -0.04462(14) 0.31388(12) 0.27377(8) 0.0181(4) Uani 1 1 d . . .
P31 P 0.24037(14) 0.00211(13) 0.32181(9) 0.0199(4) Uani 1 1 d . . .
P32 P 0.26330(15) 0.02704(13) 0.17480(9) 0.0229(4) Uani 1 1 d . . .
C1 C 0.5611(6) 0.4009(6) 0.1178(4) 0.0321(19) Uani 1 1 d . . .
H1A H 0.5429 0.4570 0.1356 0.038 Uiso 1 1 calc R . .
H1B H 0.6367 0.3953 0.0997 0.038 Uiso 1 1 calc R . .
C2 C 0.5096(6) 0.4033(6) 0.0673(4) 0.0272(17) Uani 1 1 d . . .
H2A H 0.5359 0.3516 0.0451 0.033 Uiso 1 1 calc R . .
H2B H 0.5266 0.4573 0.0371 0.033 Uiso 1 1 calc R . .
C3 C -0.0665(6) 0.4172(5) 0.3658(3) 0.0231(15) Uani 1 1 d . . .
H3A H -0.0949 0.3694 0.3993 0.028 Uiso 1 1 calc R . .
H3B H -0.0927 0.4742 0.3813 0.028 Uiso 1 1 calc R . .
C4 C -0.1038(6) 0.4119(5) 0.3100(4) 0.0267(17) Uani 1 1 d . . .
H4A H -0.0862 0.4654 0.2794 0.032 Uiso 1 1 calc R . .
H4B H -0.1796 0.4098 0.3233 0.032 Uiso 1 1 calc R . .
C5 C 0.2935(6) -0.0851(5) 0.2729(4) 0.0293(18) Uani 1 1 d . . .
H5A H 0.3673 -0.0777 0.2514 0.035 Uiso 1 1 calc R . .
H5B H 0.2872 -0.1437 0.2986 0.035 Uiso 1 1 calc R . .
C6 C 0.2335(7) -0.0784(5) 0.2257(4) 0.0304(19) Uani 1 1 d . . .
H6A H 0.1587 -0.0792 0.2468 0.036 Uiso 1 1 calc R . .
H6B H 0.2548 -0.1285 0.2014 0.036 Uiso 1 1 calc R . .
C111 C 0.6205(6) 0.2185(6) 0.1605(4) 0.0319(19) Uani 1 1 d . . .
C112 C 0.6717(7) 0.2088(7) 0.0981(5) 0.045(2) Uani 1 1 d . . .
H11A H 0.6564 0.2501 0.0657 0.054 Uiso 1 1 calc R . .
C113 C 0.7188(8) 0.0890(8) 0.1924(6) 0.057(3) Uani 1 1 d . . .
H11B H 0.7352 0.0479 0.2245 0.069 Uiso 1 1 calc R . .
C114 C 0.7683(8) 0.0802(8) 0.1317(6) 0.058(3) Uani 1 1 d . . .
H11C H 0.8196 0.0335 0.1220 0.070 Uiso 1 1 calc R . .
C115 C 0.7438(8) 0.1393(9) 0.0845(6) 0.062(3) Uani 1 1 d . . .
H11D H 0.7771 0.1318 0.0426 0.074 Uiso 1 1 calc R . .
C116 C 0.6444(7) 0.1579(7) 0.2071(5) 0.040(2) Uani 1 1 d . . .
H11E H 0.6099 0.1635 0.2492 0.048 Uiso 1 1 calc R . .
C121 C 0.5438(6) 0.3418(6) 0.2475(4) 0.0308(18) Uani 1 1 d . . .
C122 C 0.6044(7) 0.4108(7) 0.2409(5) 0.042(2) Uani 1 1 d . . .
H12A H 0.6354 0.4402 0.2007 0.051 Uiso 1 1 calc R . .
C123 C 0.6207(9) 0.4380(8) 0.2927(6) 0.055(3) Uani 1 1 d . . .
H12B H 0.6604 0.4869 0.2878 0.066 Uiso 1 1 calc R . .
C124 C 0.5785(9) 0.3931(9) 0.3507(6) 0.061(3) Uani 1 1 d . . .
H12C H 0.5911 0.4101 0.3858 0.073 Uiso 1 1 calc R . .
C125 C 0.5179(9) 0.3231(9) 0.3583(5) 0.054(3) Uani 1 1 d . . .
H12D H 0.4889 0.2927 0.3984 0.065 Uiso 1 1 calc R . .
C126 C 0.4999(7) 0.2979(7) 0.3068(4) 0.036(2) Uani 1 1 d . . .
H12E H 0.4576 0.2507 0.3120 0.043 Uiso 1 1 calc R . .
C131 C 0.3357(6) 0.5193(5) 0.1091(4) 0.0298(18) Uani 1 1 d . . .
C132 C 0.3572(7) 0.5524(6) 0.1574(4) 0.037(2) Uani 1 1 d . . .
H13A H 0.3815 0.5134 0.1877 0.044 Uiso 1 1 calc R . .
C133 C 0.3429(9) 0.6419(7) 0.1607(5) 0.053(3) Uani 1 1 d . . .
H13B H 0.3604 0.6649 0.1921 0.063 Uiso 1 1 calc R . .
C134 C 0.3032(10) 0.6979(7) 0.1185(5) 0.059(3) Uani 1 1 d . . .
H13C H 0.2923 0.7592 0.1215 0.071 Uiso 1 1 calc R . .
C135 C 0.2791(9) 0.6663(7) 0.0721(5) 0.051(3) Uani 1 1 d . . .
H13D H 0.2517 0.7055 0.0432 0.062 Uiso 1 1 calc R . .
C136 C 0.2951(7) 0.5773(6) 0.0676(4) 0.035(2) Uani 1 1 d . . .
H13E H 0.2781 0.5554 0.0356 0.042 Uiso 1 1 calc R . .
C141 C 0.3232(6) 0.3882(5) 0.0347(4) 0.0267(17) Uani 1 1 d . . .
C142 C 0.3902(7) 0.3705(6) -0.0217(4) 0.0324(19) Uani 1 1 d . . .
H14A H 0.4624 0.3687 -0.0279 0.039 Uiso 1 1 calc R . .
C143 C 0.3530(8) 0.3555(6) -0.0688(4) 0.038(2) Uani 1 1 d . . .
H14B H 0.3997 0.3434 -0.1072 0.046 Uiso 1 1 calc R . .
C144 C 0.2481(8) 0.3582(6) -0.0605(4) 0.040(2) Uani 1 1 d . . .
H14C H 0.2228 0.3475 -0.0930 0.048 Uiso 1 1 calc R . .
C145 C 0.1797(7) 0.3765(6) -0.0045(4) 0.036(2) Uani 1 1 d . . .
H14D H 0.1076 0.3790 0.0013 0.043 Uiso 1 1 calc R . .
C146 C 0.2173(6) 0.3910(6) 0.0430(4) 0.0284(17) Uani 1 1 d . . .
H14E H 0.1706 0.4029 0.0814 0.034 Uiso 1 1 calc R . .
C211 C 0.1112(7) 0.5211(5) 0.3303(4) 0.0276(17) Uani 1 1 d . . .
C212 C 0.1997(8) 0.5410(6) 0.3423(4) 0.039(2) Uani 1 1 d . . .
H21A H 0.2430 0.4953 0.3569 0.046 Uiso 1 1 calc R . .
C213 C 0.2242(9) 0.6292(7) 0.3327(5) 0.051(3) Uani 1 1 d . . .
H21B H 0.2833 0.6437 0.3420 0.062 Uiso 1 1 calc R . .
C214 C 0.1627(11) 0.6944(7) 0.3100(5) 0.056(3) Uani 1 1 d . . .
H21C H 0.1802 0.7539 0.3029 0.067 Uiso 1 1 calc R . .
C215 C 0.0770(10) 0.6751(6) 0.2974(4) 0.048(3) Uani 1 1 d . . .
H21D H 0.0353 0.7214 0.2818 0.058 Uiso 1 1 calc R . .
C216 C 0.0493(8) 0.5881(5) 0.3070(4) 0.034(2) Uani 1 1 d . . .
H21E H -0.0104 0.5749 0.2979 0.041 Uiso 1 1 calc R . .
C221 C 0.1013(6) 0.3718(5) 0.4216(3) 0.0235(16) Uani 1 1 d . . .
C222 C 0.0271(7) 0.3923(5) 0.4758(4) 0.0286(17) Uani 1 1 d . . .
H22A H -0.0385 0.4187 0.4738 0.034 Uiso 1 1 calc R . .
C223 C 0.0488(8) 0.3743(6) 0.5319(4) 0.036(2) Uani 1 1 d . . .
H22B H -0.0023 0.3878 0.5684 0.043 Uiso 1 1 calc R . .
C224 C 0.1443(8) 0.3367(6) 0.5355(4) 0.038(2) Uani 1 1 d . . .
H22C H 0.1594 0.3256 0.5742 0.046 Uiso 1 1 calc R . .
C225 C 0.2181(7) 0.3153(7) 0.4822(4) 0.036(2) Uani 1 1 d . . .
H22D H 0.2837 0.2891 0.4843 0.043 Uiso 1 1 calc R . .
C226 C 0.1961(6) 0.3322(6) 0.4257(4) 0.0292(18) Uani 1 1 d . . .
H22E H 0.2464 0.3166 0.3895 0.035 Uiso 1 1 calc R . .
C231 C -0.0784(6) 0.3295(5) 0.2007(3) 0.0231(15) Uani 1 1 d . . .
C232 C -0.0564(6) 0.2599(6) 0.1650(4) 0.0278(17) Uani 1 1 d . . .
H23A H -0.0270 0.2047 0.1797 0.033 Uiso 1 1 calc R . .
C233 C -0.0777(7) 0.2718(7) 0.1084(4) 0.040(2) Uani 1 1 d . . .
H23B H -0.0627 0.2246 0.0843 0.048 Uiso 1 1 calc R . .
C234 C -0.1203(7) 0.3516(7) 0.0868(4) 0.041(2) Uani 1 1 d . . .
H23C H -0.1340 0.3597 0.0478 0.049 Uiso 1 1 calc R . .
C235 C -0.1428(8) 0.4189(7) 0.1219(5) 0.042(2) Uani 1 1 d . . .
H23D H -0.1732 0.4736 0.1073 0.050 Uiso 1 1 calc R . .
C236 C -0.1219(7) 0.4085(6) 0.1788(4) 0.0329(19) Uani 1 1 d . . .
H23E H -0.1376 0.4561 0.2026 0.039 Uiso 1 1 calc R . .
C241 C -0.1298(5) 0.2317(5) 0.3256(3) 0.0215(15) Uani 1 1 d . . .
C242 C -0.1184(6) 0.2010(5) 0.3839(3) 0.0223(15) Uani 1 1 d . . .
H24A H -0.0617 0.2170 0.3949 0.027 Uiso 1 1 calc R . .
C243 C -0.1891(6) 0.1471(5) 0.4265(4) 0.0252(16) Uani 1 1 d . . .
H24B H -0.1820 0.1282 0.4668 0.030 Uiso 1 1 calc R . .
C244 C -0.2690(7) 0.1210(6) 0.4106(4) 0.040(2) Uani 1 1 d . . .
H24C H -0.3161 0.0827 0.4395 0.048 Uiso 1 1 calc R . .
C245 C -0.2815(7) 0.1505(7) 0.3523(4) 0.044(3) Uani 1 1 d . . .
H24D H -0.3376 0.1330 0.3415 0.052 Uiso 1 1 calc R . .
C246 C -0.2114(7) 0.2058(6) 0.3098(4) 0.034(2) Uani 1 1 d . . .
H24E H -0.2197 0.2257 0.2699 0.041 Uiso 1 1 calc R . .
C311 C 0.3299(6) 0.0101(5) 0.3655(4) 0.0288(18) Uani 1 1 d . . .
C312 C 0.4327(6) -0.0166(7) 0.3464(5) 0.041(2) Uani 1 1 d . . .
H31A H 0.4591 -0.0465 0.3112 0.049 Uiso 1 1 calc R . .
C313 C 0.4989(8) 0.0008(8) 0.3797(7) 0.064(4) Uani 1 1 d . . .
H31B H 0.5699 -0.0180 0.3669 0.077 Uiso 1 1 calc R . .
C314 C 0.4615(9) 0.0445(9) 0.4304(6) 0.063(4) Uani 1 1 d . . .
H31C H 0.5070 0.0575 0.4517 0.076 Uiso 1 1 calc R . .
C315 C 0.3590(9) 0.0694(8) 0.4503(5) 0.054(3) Uani 1 1 d . . .
H31D H 0.3331 0.0986 0.4860 0.065 Uiso 1 1 calc R . .
C316 C 0.2923(7) 0.0520(6) 0.4183(4) 0.036(2) Uani 1 1 d . . .
H31E H 0.2209 0.0688 0.4326 0.044 Uiso 1 1 calc R . .
C321 C 0.1342(5) -0.0505(5) 0.3820(3) 0.0215(15) Uani 1 1 d . . .
C322 C 0.0361(6) -0.0111(5) 0.4013(4) 0.0278(17) Uani 1 1 d . . .
H32A H 0.0207 0.0474 0.3839 0.033 Uiso 1 1 calc R . .
C323 C -0.0406(7) -0.0577(6) 0.4464(4) 0.035(2) Uani 1 1 d . . .
H32B H -0.1088 -0.0315 0.4585 0.042 Uiso 1 1 calc R . .
C324 C -0.0175(7) -0.1416(6) 0.4736(4) 0.0328(19) Uani 1 1 d . . .
H32C H -0.0695 -0.1728 0.5046 0.039 Uiso 1 1 calc R . .
C325 C 0.0812(7) -0.1799(5) 0.4554(4) 0.0293(18) Uani 1 1 d . . .
H32D H 0.0970 -0.2375 0.4741 0.035 Uiso 1 1 calc R . .
C326 C 0.1578(6) -0.1348(5) 0.4102(4) 0.0268(16) Uani 1 1 d . . .
H32E H 0.2260 -0.1612 0.3984 0.032 Uiso 1 1 calc R . .
C331 C 0.1853(7) 0.0411(6) 0.1215(4) 0.0298(18) Uani 1 1 d . . .
C332 C 0.1079(8) -0.0150(7) 0.1271(4) 0.045(3) Uani 1 1 d . . .
H33A H 0.0939 -0.0622 0.1603 0.054 Uiso 1 1 calc R . .
C333 C 0.0518(8) -0.0019(8) 0.0846(5) 0.053(3) Uani 1 1 d . . .
H33B H 0.0005 -0.0410 0.0884 0.064 Uiso 1 1 calc R . .
C334 C 0.0693(8) 0.0673(8) 0.0368(5) 0.047(3) Uani 1 1 d . . .
H33C H 0.0288 0.0766 0.0087 0.056 Uiso 1 1 calc R . .
C335 C 0.1464(7) 0.1233(7) 0.0298(4) 0.040(2) Uani 1 1 d . . .
H33D H 0.1598 0.1702 -0.0036 0.048 Uiso 1 1 calc R . .
C336 C 0.2033(6) 0.1103(6) 0.0718(4) 0.0285(17) Uani 1 1 d . . .
H33E H 0.2556 0.1488 0.0670 0.034 Uiso 1 1 calc R . .
C341 C 0.3904(7) -0.0109(5) 0.1274(4) 0.0298(18) Uani 1 1 d . . .
C342 C 0.3928(8) -0.0618(6) 0.0810(4) 0.039(2) Uani 1 1 d . . .
H34A H 0.3316 -0.0672 0.0706 0.047 Uiso 1 1 calc R . .
C343 C 0.4854(10) -0.1039(7) 0.0504(5) 0.054(3) Uani 1 1 d . . .
H34B H 0.4876 -0.1379 0.0188 0.065 Uiso 1 1 calc R . .
C344 C 0.5735(9) -0.0962(7) 0.0660(5) 0.059(3) Uani 1 1 d . . .
H34C H 0.6362 -0.1257 0.0453 0.071 Uiso 1 1 calc R . .
C345 C 0.5725(8) -0.0467(7) 0.1111(5) 0.050(3) Uani 1 1 d . . .
H34D H 0.6342 -0.0415 0.1210 0.060 Uiso 1 1 calc R . .
C346 C 0.4804(7) -0.0041(6) 0.1421(5) 0.038(2) Uani 1 1 d . . .
H34E H 0.4794 0.0299 0.1734 0.045 Uiso 1 1 calc R . .
Cl1 Cl 1.0097(4) 0.6218(3) 0.0880(2) 0.0836(18) Uani 0.844(10) 1 d P A .
Cl2 Cl 1.0422(6) 0.7812(4) 0.1275(4) 0.142(3) Uani 0.835(11) 1 d P A .
Cl1A Cl 0.8926(11) 0.6567(8) 0.1947(5) 0.087(5) Uani 0.320(10) 1 d P . .
C1SA C 1.0146(13) 0.6692(9) 0.1505(7) 0.024(3) Uani 0.50 1 d P A .
C1SB C 0.9939(10) 0.7411(9) 0.0730(6) 0.014(2) Uani 0.50 1 d PU . .
Cl3 Cl 0.4519(6) 0.7399(5) 0.3666(5) 0.183(3) Uani 1 1 d . . .
Cl4 Cl 0.5048(6) 0.7791(4) 0.4752(3) 0.143(2) Uani 1 1 d . . .
C2S C 0.542(3) 0.699(3) 0.4283(15) 0.235(18) Uani 1 1 d . . .
Cl5 Cl 0.8971(4) 0.9002(4) 0.2646(3) 0.173(3) Uani 1 1 d . . .
Cl6 Cl 0.7445(4) 0.8733(4) 0.3855(2) 0.1121(17) Uani 1 1 d . . .
C3S C 0.8558(13) 0.8393(15) 0.3335(9) 0.116(7) Uani 1 1 d . . .
Cl7 Cl 0.2876(5) 0.6355(4) 0.5086(4) 0.162(3) Uani 1 1 d . . .
Cl8 Cl 0.3923(5) 0.4852(5) 0.4501(5) 0.204(4) Uani 1 1 d . . .
C4S C 0.314(3) 0.501(3) 0.515(2) 0.43(4) Uani 1 1 d . . .
Cl9 Cl 0.4742(7) 0.2519(6) 0.7812(4) 0.099(4) Uani 0.489(9) 1 d PD . .
Cl10 Cl 0.2340(8) 0.1954(7) 0.8420(5) 0.035(4) Uani 0.192(8) 1 d PD . .
Cl11 Cl 0.3534(8) 0.1419(6) 0.7503(4) 0.060(3) Uani 0.320(9) 1 d PD . .
C5S C 0.3517(14) 0.2267(17) 0.7854(12) 0.103(11) Uiso 0.50 1 d PD . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Re1 0.01554(12) 0.01959(14) 0.01359(13) -0.00304(10) -0.00136(9) -0.00613(10)
Re2 0.01703(12) 0.01618(13) 0.01210(13) -0.00342(9) -0.00168(9) -0.00563(10)
Re3 0.01472(12) 0.01727(13) 0.01373(13) -0.00422(10) -0.00173(9) -0.00478(9)
S1 0.0171(7) 0.0231(9) 0.0133(8) -0.0046(6) -0.0018(6) -0.0057(6)
S2 0.0208(8) 0.0241(9) 0.0173(9) -0.0061(7) -0.0010(6) -0.0096(7)
S3 0.0161(7) 0.0220(9) 0.0204(9) -0.0015(7) -0.0043(6) -0.0051(6)
S4 0.0171(7) 0.0164(8) 0.0140(8) -0.0034(6) -0.0012(6) -0.0058(6)
Br1 0.0228(6) 0.0289(6) 0.0194(6) -0.0067(4) -0.0002(4) -0.0064(4)
Cl1T 0.0228(6) 0.0289(6) 0.0194(6) -0.0067(4) -0.0002(4) -0.0064(4)
Br2 0.0242(5) 0.0222(5) 0.0199(6) -0.0023(4) 0.0004(4) -0.0066(4)
Cl2T 0.0242(5) 0.0222(5) 0.0199(6) -0.0023(4) 0.0004(4) -0.0066(4)
Br3 0.0228(5) 0.0280(6) 0.0220(6) -0.0076(4) -0.0056(4) -0.0048(4)
Cl3T 0.0228(5) 0.0280(6) 0.0220(6) -0.0076(4) -0.0056(4) -0.0048(4)
Br4 0.176(5) 0.066(3) 0.333(8) -0.119(4) -0.221(6) 0.073(3)
Br4 0.047(2) 0.028(2) 0.487(16) 0.010(5) -0.060(5) -0.0035(17)
P11 0.0186(9) 0.0319(11) 0.0227(10) -0.0017(8) -0.0046(7) -0.0104(8)
P12 0.0208(9) 0.0275(10) 0.0169(9) 0.0002(7) -0.0015(7) -0.0078(7)
P21 0.0254(9) 0.0176(9) 0.0157(9) -0.0054(7) -0.0019(7) -0.0070(7)
P22 0.0178(8) 0.0201(9) 0.0163(9) -0.0025(7) -0.0035(7) -0.0044(7)
P31 0.0167(8) 0.0197(9) 0.0228(10) -0.0027(7) -0.0033(7) -0.0058(7)
P32 0.0236(9) 0.0235(10) 0.0201(10) -0.0088(8) 0.0019(7) -0.0093(7)
C1 0.028(4) 0.038(5) 0.030(4) 0.004(4) -0.007(3) -0.017(4)
C2 0.019(3) 0.035(4) 0.021(4) 0.008(3) 0.000(3) -0.009(3)
C3 0.027(4) 0.018(4) 0.021(4) -0.001(3) -0.002(3) -0.005(3)
C4 0.021(3) 0.023(4) 0.035(5) -0.003(3) -0.008(3) 0.001(3)
C5 0.031(4) 0.020(4) 0.030(4) -0.008(3) 0.003(3) 0.003(3)
C6 0.038(4) 0.019(4) 0.028(4) -0.010(3) 0.008(3) -0.012(3)
C111 0.017(3) 0.042(5) 0.038(5) -0.006(4) -0.009(3) -0.009(3)
C112 0.020(4) 0.059(7) 0.051(6) -0.011(5) 0.001(4) -0.005(4)
C113 0.036(5) 0.053(7) 0.080(9) 0.001(6) -0.019(6) 0.003(5)
C114 0.030(5) 0.047(7) 0.091(10) -0.015(6) -0.008(6) 0.000(5)
C115 0.030(5) 0.068(8) 0.077(9) -0.022(7) 0.008(5) -0.006(5)
C116 0.025(4) 0.045(6) 0.052(6) -0.005(4) -0.016(4) -0.003(4)
C121 0.027(4) 0.036(5) 0.034(5) -0.004(4) -0.015(3) -0.008(3)
C122 0.034(5) 0.046(6) 0.051(6) -0.010(5) -0.015(4) -0.008(4)
C123 0.047(6) 0.063(7) 0.071(8) -0.026(6) -0.030(6) -0.012(5)
C124 0.048(6) 0.092(10) 0.058(7) -0.031(7) -0.025(6) -0.013(6)
C125 0.058(7) 0.081(8) 0.035(6) -0.008(5) -0.025(5) -0.020(6)
C126 0.034(4) 0.048(6) 0.034(5) -0.007(4) -0.018(4) -0.008(4)
C131 0.028(4) 0.027(4) 0.027(4) -0.004(3) 0.007(3) -0.010(3)
C132 0.044(5) 0.039(5) 0.030(5) -0.008(4) -0.005(4) -0.021(4)
C133 0.072(7) 0.043(6) 0.037(6) -0.012(5) 0.009(5) -0.031(5)
C134 0.086(9) 0.025(5) 0.043(6) -0.006(4) 0.022(6) -0.014(5)
C135 0.070(7) 0.030(5) 0.033(6) -0.002(4) 0.016(5) -0.002(5)
C136 0.036(5) 0.028(4) 0.029(5) -0.001(3) 0.010(3) -0.006(4)
C141 0.028(4) 0.030(4) 0.021(4) 0.003(3) -0.006(3) -0.008(3)
C142 0.034(4) 0.038(5) 0.023(4) -0.007(4) -0.004(3) -0.001(4)
C143 0.051(6) 0.043(5) 0.021(4) -0.008(4) -0.009(4) 0.000(4)
C144 0.054(6) 0.041(5) 0.031(5) 0.001(4) -0.025(4) -0.006(4)
C145 0.036(5) 0.042(5) 0.029(5) 0.012(4) -0.016(4) -0.010(4)
C146 0.026(4) 0.035(5) 0.022(4) 0.003(3) -0.006(3) -0.004(3)
C211 0.042(5) 0.021(4) 0.018(4) -0.007(3) 0.001(3) -0.012(3)
C212 0.048(5) 0.029(5) 0.037(5) -0.010(4) 0.001(4) -0.019(4)
C213 0.069(7) 0.047(6) 0.039(6) -0.012(5) -0.003(5) -0.032(6)
C214 0.100(10) 0.031(5) 0.033(6) -0.006(4) -0.002(6) -0.028(6)
C215 0.089(8) 0.024(5) 0.029(5) -0.008(4) -0.010(5) -0.005(5)
C216 0.061(6) 0.019(4) 0.020(4) -0.005(3) -0.002(4) -0.009(4)
C221 0.037(4) 0.021(4) 0.012(3) -0.001(3) -0.005(3) -0.011(3)
C222 0.043(5) 0.018(4) 0.022(4) -0.008(3) -0.002(3) -0.004(3)
C223 0.064(6) 0.022(4) 0.017(4) -0.004(3) 0.001(4) -0.009(4)
C224 0.065(6) 0.038(5) 0.018(4) -0.008(4) -0.014(4) -0.018(5)
C225 0.038(5) 0.052(6) 0.027(4) -0.008(4) -0.016(4) -0.014(4)
C226 0.034(4) 0.036(5) 0.020(4) -0.008(3) -0.004(3) -0.014(4)
C231 0.020(3) 0.030(4) 0.018(4) 0.003(3) -0.005(3) -0.006(3)
C232 0.023(4) 0.041(5) 0.021(4) -0.004(3) -0.009(3) -0.001(3)
C233 0.035(5) 0.063(7) 0.026(5) -0.011(4) -0.013(4) -0.008(4)
C234 0.031(4) 0.070(7) 0.022(4) 0.006(4) -0.012(3) -0.013(4)
C235 0.042(5) 0.043(6) 0.041(6) 0.010(4) -0.021(4) -0.008(4)
C236 0.036(4) 0.034(5) 0.030(5) 0.003(4) -0.013(4) -0.008(4)
C241 0.020(3) 0.022(4) 0.020(4) -0.002(3) -0.001(3) -0.006(3)
C242 0.021(3) 0.026(4) 0.022(4) -0.005(3) -0.008(3) -0.004(3)
C243 0.021(3) 0.031(4) 0.021(4) 0.000(3) -0.003(3) -0.008(3)
C244 0.030(4) 0.045(5) 0.039(5) 0.020(4) -0.010(4) -0.020(4)
C245 0.039(5) 0.055(6) 0.042(5) 0.016(4) -0.021(4) -0.030(5)
C246 0.039(5) 0.038(5) 0.031(5) 0.012(4) -0.021(4) -0.018(4)
C311 0.021(4) 0.029(4) 0.038(5) 0.011(3) -0.015(3) -0.014(3)
C312 0.022(4) 0.044(5) 0.055(6) 0.006(4) -0.011(4) -0.006(4)
C313 0.033(5) 0.063(8) 0.093(10) 0.036(7) -0.036(6) -0.013(5)
C314 0.058(7) 0.076(9) 0.067(8) 0.033(7) -0.043(6) -0.046(7)
C315 0.061(7) 0.070(8) 0.041(6) 0.018(5) -0.030(5) -0.040(6)
C316 0.036(5) 0.043(5) 0.036(5) 0.011(4) -0.023(4) -0.018(4)
C321 0.021(3) 0.026(4) 0.017(4) -0.006(3) 0.000(3) -0.009(3)
C322 0.026(4) 0.024(4) 0.027(4) 0.005(3) -0.001(3) -0.007(3)
C323 0.027(4) 0.040(5) 0.032(5) 0.001(4) 0.001(3) -0.012(4)
C324 0.032(4) 0.040(5) 0.026(4) -0.003(4) -0.002(3) -0.020(4)
C325 0.043(5) 0.023(4) 0.023(4) 0.003(3) -0.009(3) -0.014(3)
C326 0.027(4) 0.030(4) 0.024(4) -0.004(3) -0.007(3) -0.006(3)
C331 0.035(4) 0.035(5) 0.022(4) -0.016(3) -0.003(3) -0.011(4)
C332 0.048(6) 0.062(7) 0.030(5) -0.018(4) -0.004(4) -0.032(5)
C333 0.050(6) 0.076(8) 0.043(6) -0.025(6) -0.009(5) -0.032(6)
C334 0.048(6) 0.067(7) 0.033(5) -0.020(5) -0.015(4) -0.014(5)
C335 0.037(5) 0.057(6) 0.030(5) -0.017(4) -0.009(4) -0.010(4)
C336 0.027(4) 0.040(5) 0.020(4) -0.016(3) -0.002(3) -0.006(3)
C341 0.037(4) 0.019(4) 0.024(4) -0.006(3) 0.009(3) -0.008(3)
C342 0.052(6) 0.033(5) 0.025(5) -0.011(4) 0.006(4) -0.006(4)
C343 0.079(8) 0.032(5) 0.034(6) -0.012(4) 0.014(5) -0.002(5)
C344 0.052(7) 0.043(6) 0.053(7) -0.002(5) 0.023(5) 0.009(5)
C345 0.032(5) 0.044(6) 0.059(7) -0.014(5) 0.013(4) 0.001(4)
C346 0.029(4) 0.029(5) 0.044(5) -0.008(4) 0.009(4) -0.007(3)
Cl1 0.090(3) 0.111(4) 0.067(3) -0.010(2) -0.046(2) -0.018(3)
Cl2 0.150(6) 0.049(3) 0.214(8) -0.018(4) -0.037(5) 0.009(3)
Cl1A 0.124(11) 0.076(8) 0.063(7) -0.010(6) -0.035(7) 0.012(7)
C1SA 0.044(9) 0.005(6) 0.021(8) 0.004(5) -0.009(7) -0.004(6)
C1SB 0.018(4) 0.016(4) 0.010(4) 0.006(3) -0.009(3) -0.004(3)
Cl3 0.174(7) 0.113(5) 0.278(10) 0.000(6) -0.110(7) 0.005(5)
Cl4 0.208(7) 0.111(4) 0.111(4) 0.011(3) -0.061(4) -0.010(4)
C2S 0.20(3) 0.31(5) 0.17(3) -0.12(3) -0.04(2) 0.12(3)
Cl5 0.091(3) 0.149(5) 0.212(7) 0.108(5) -0.009(4) -0.020(3)
Cl6 0.091(3) 0.136(4) 0.112(4) -0.044(3) -0.041(3) 0.052(3)
C3S 0.075(11) 0.151(19) 0.089(13) -0.010(12) 0.014(9) 0.012(11)
Cl7 0.102(4) 0.114(5) 0.229(8) -0.036(5) 0.016(4) -0.001(3)
Cl8 0.092(4) 0.162(6) 0.336(12) -0.121(7) 0.023(5) -0.023(4)
C4S 0.38(5) 0.41(5) 0.41(5) -0.38(5) 0.30(4) -0.34(5)
Cl9 0.123(7) 0.094(6) 0.125(7) -0.073(6) -0.086(6) 0.037(5)
Cl10 0.041(6) 0.039(6) 0.040(7) -0.026(5) -0.031(5) 0.025(5)
Cl11 0.080(7) 0.056(6) 0.049(5) -0.019(4) -0.030(5) 0.025(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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.2310 '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
Re2 Re1 Re3 60.066(9)
S1 Re1 Re2 53.55(4)
S1 Re1 Re3 53.49(4)
S1 Re1 Br1 86.99(5)
S1 Re1 P11 168.09(6)
S1 Re1 P12 91.44(6)
S2 Re1 Re2 53.98(4)
S2 Re1 Re3 98.40(4)
S2 Re1 S1 106.45(6)
S2 Re1 S3 93.97(7)
S2 Re1 Br1 164.57(5)
S2 Re1 P11 83.04(7)
S2 Re1 P12 95.05(7)
S3 Re1 Re2 96.87(4)
S3 Re1 Re3 52.43(4)
S3 Re1 S1 104.97(6)
S3 Re1 Br1 89.69(5)
S3 Re1 P11 81.04(6)
S3 Re1 P12 158.18(6)
Br1 Re1 Re2 140.39(3)
Br1 Re1 Re3 95.72(3)
P11 Re1 Re2 136.86(5)
P11 Re1 Re3 133.47(5)
P11 Re1 Br1 82.73(5)
P11 Re1 P12 80.38(7)
P12 Re1 Re2 104.50(5)
P12 Re1 Re3 144.73(5)
P12 Re1 Br1 76.69(5)
Re1 Re2 Re3 60.084(10)
S1 Re2 Re1 53.88(4)
S1 Re2 Re3 53.58(4)
S1 Re2 Br2 86.46(5)
S1 Re2 P21 166.16(6)
S1 Re2 P22 90.90(6)
S2 Re2 Re1 52.38(4)
S2 Re2 Re3 97.24(5)
S2 Re2 S1 105.22(6)
S2 Re2 Br2 88.94(5)
S2 Re2 P21 81.31(6)
S2 Re2 P22 158.49(6)
S4 Re2 Re1 97.19(4)
S4 Re2 Re3 53.98(4)
S4 Re2 S1 106.73(6)
S4 Re2 S2 92.80(6)
S4 Re2 Br2 165.68(5)
S4 Re2 P21 84.81(6)
S4 Re2 P22 96.14(6)
Br2 Re2 Re1 95.12(2)
Br2 Re2 Re3 139.84(3)
P21 Re2 Re1 133.67(4)
P21 Re2 Re3 138.74(5)
P21 Re2 Br2 81.41(5)
P21 Re2 P22 80.07(6)
P22 Re2 Re1 144.64(4)
P22 Re2 Re3 103.85(4)
P22 Re2 Br2 77.73(5)
Re2 Re3 Re1 59.850(10)
S1 Re3 Re1 53.77(4)
S1 Re3 Re2 53.52(4)
S1 Re3 S4 105.54(6)
S1 Re3 Br3 87.71(5)
S1 Re3 P31 168.64(6)
S1 Re3 P32 90.15(7)
S3 Re3 Re1 53.62(5)
S3 Re3 Re2 97.57(5)
S3 Re3 S1 106.42(6)
S3 Re3 S4 92.14(6)
S3 Re3 Br3 164.26(5)
S3 Re3 P31 80.47(6)
S3 Re3 P32 95.93(7)
S4 Re3 Re1 96.19(4)
S4 Re3 Re2 52.82(4)
S4 Re3 Br3 90.65(5)
S4 Re3 P31 82.87(6)
S4 Re3 P32 159.57(6)
Br3 Re3 Re1 141.33(3)
Br3 Re3 Re2 96.46(3)
P31 Re3 Re1 134.06(4)
P31 Re3 Re2 135.65(5)
P31 Re3 Br3 84.51(5)
P31 Re3 P32 80.02(7)
P32 Re3 Re1 103.72(4)
P32 Re3 Re2 143.52(5)
P32 Re3 Br3 76.72(5)
Re2 S1 Re1 72.57(5)
Re2 S1 Re3 72.90(5)
Re3 S1 Re1 72.74(5)
Re1 S2 Re2 73.64(5)
Re3 S3 Re1 73.95(5)
Re2 S4 Re3 73.20(5)
C1 P11 Re1 108.5(3)
C111 P11 Re1 116.3(3)
C111 P11 C1 105.4(4)
C111 P11 C121 103.3(4)
C121 P11 Re1 117.7(3)
C121 P11 C1 104.2(4)
C2 P12 Re1 104.9(3)
C131 P12 Re1 125.0(3)
C131 P12 C2 100.1(4)
C141 P12 Re1 115.6(3)
C141 P12 C2 104.1(4)
C141 P12 C131 104.2(4)
C3 P21 Re2 109.2(3)
C3 P21 C211 104.7(4)
C3 P21 C221 104.8(4)
C211 P21 Re2 116.9(3)
C211 P21 C221 100.9(4)
C221 P21 Re2 118.8(3)
C4 P22 Re2 105.4(3)
C4 P22 C231 104.6(4)
C4 P22 C241 99.0(4)
C231 P22 Re2 115.1(2)
C231 P22 C241 105.5(3)
C241 P22 Re2 124.4(3)
C5 P31 Re3 106.1(3)
C311 P31 Re3 113.9(3)
C311 P31 C5 107.6(4)
C311 P31 C321 101.5(4)
C321 P31 Re3 124.0(3)
C321 P31 C5 102.3(4)
C6 P32 Re3 103.4(3)
C331 P32 Re3 114.1(3)
C331 P32 C6 107.4(4)
C331 P32 C341 102.9(4)
C341 P32 Re3 129.3(3)
C341 P32 C6 96.8(4)
C2 C1 P11 111.6(5)
C1 C2 P12 110.9(5)
C4 C3 P21 112.1(5)
C3 C4 P22 110.9(5)
C6 C5 P31 108.1(5)
C5 C6 P32 106.3(5)
C112 C111 P11 120.7(7)
C116 C111 P11 120.0(7)
C116 C111 C112 119.2(9)
C115 C112 C111 119.7(11)
C114 C113 C116 120.2(11)
C113 C114 C115 120.3(11)
C112 C115 C114 120.4(12)
C111 C116 C113 120.3(10)
C122 C121 P11 120.7(7)
C122 C121 C126 119.1(8)
C126 C121 P11 120.2(6)
C121 C122 C123 121.0(10)
C124 C123 C122 119.3(10)
C123 C124 C125 120.7(10)
C124 C125 C126 119.7(11)
C125 C126 C121 120.3(9)
C132 C131 P12 119.3(7)
C136 C131 P12 121.9(7)
C136 C131 C132 118.7(8)
C133 C132 C131 119.7(10)
C134 C133 C132 120.0(10)
C135 C134 C133 121.0(10)
C134 C135 C136 119.5(11)
C135 C136 C131 121.1(10)
C142 C141 P12 122.3(6)
C142 C141 C146 118.9(8)
C146 C141 P12 118.7(6)
C143 C142 C141 120.6(8)
C142 C143 C144 120.4(9)
C143 C144 C145 119.8(8)
C146 C145 C144 119.7(8)
C145 C146 C141 120.5(8)
C212 C211 P21 119.9(7)
C212 C211 C216 120.2(8)
C216 C211 P21 119.8(7)
C211 C212 C213 119.4(10)
C214 C213 C212 119.8(11)
C215 C214 C213 121.0(9)
C214 C215 C216 120.9(11)
C211 C216 C215 118.7(10)
C222 C221 P21 118.7(6)
C226 C221 P21 122.2(6)
C226 C221 C222 118.9(7)
C223 C222 C221 120.3(9)
C222 C223 C224 120.6(8)
C223 C224 C225 119.5(8)
C226 C225 C224 120.0(9)
C225 C226 C221 120.7(8)
C232 C231 P22 119.2(6)
C236 C231 P22 121.8(7)
C236 C231 C232 119.0(7)
C233 C232 C231 119.9(8)
C234 C233 C232 120.5(9)
C235 C234 C233 119.5(8)
C234 C235 C236 120.9(9)
C231 C236 C235 120.1(9)
C242 C241 P22 119.6(6)
C246 C241 P22 121.2(6)
C246 C241 C242 118.9(7)
C243 C242 C241 120.6(7)
C244 C243 C242 120.3(7)
C243 C244 C245 120.0(7)
C244 C245 C246 119.8(8)
C241 C246 C245 120.4(8)
C312 C311 P31 123.3(8)
C312 C311 C316 119.3(8)
C316 C311 P31 117.1(6)
C311 C312 C313 119.5(11)
C314 C313 C312 120.6(11)
C315 C314 C313 120.2(10)
C314 C315 C316 120.0(12)
C311 C316 C315 120.4(10)
C322 C321 P31 124.0(6)
C322 C321 C326 119.8(7)
C326 C321 P31 116.2(6)
C321 C322 C323 119.7(8)
C324 C323 C322 120.3(8)
C325 C324 C323 119.8(7)
C324 C325 C326 120.5(8)
C325 C326 C321 119.8(8)
C332 C331 P32 122.8(7)
C332 C331 C336 118.0(8)
C336 C331 P32 119.2(6)
C333 C332 C331 120.3(10)
C334 C333 C332 120.9(9)
C333 C334 C335 119.9(10)
C336 C335 C334 119.6(10)
C335 C336 C331 121.3(8)
C342 C341 P32 117.3(7)
C346 C341 P32 122.6(7)
C346 C341 C342 119.2(8)
C343 C342 C341 119.7(10)
C344 C343 C342 119.8(10)
C345 C344 C343 121.2(10)
C344 C345 C346 119.6(11)
C341 C346 C345 120.4(10)
C1SA Cl1 C1SB 69.0(6)
C1SA Cl2 C1SB 68.7(7)
C1SA Cl1A Br4 147.0(9)
Cl1 C1SA Cl2 110.5(8)
Cl1 C1SA C1SB 57.5(6)
Cl2 C1SA C1SB 56.2(6)
Cl1A C1SA Cl1 98.6(9)
Cl1A C1SA Cl2 112.7(10)
Cl1A C1SA C1SB 102.0(10)
Cl1 C1SB C1SA 53.5(5)
Cl2 C1SB Cl1 105.7(6)
Cl2 C1SB C1SA 55.1(6)
Cl4 C2S Cl3 100.7(15)
Cl5 C3S Cl6 119.4(12)
Cl8 C4S Cl7 105(2)
C5S Cl10 Cl11 42.1(6)
C5S Cl11 Cl10 47.3(7)
Cl9 C5S Cl10 140.1(18)
Cl11 C5S Cl9 112.2(13)
Cl11 C5S Cl10 90.5(10)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Re1 Re2 2.7707(4)
Re1 Re3 2.7773(4)
Re1 S1 2.3461(17)
Re1 S2 2.2873(18)
Re1 S3 2.3265(18)
Re1 Br1 2.5362(11)
Re1 P11 2.5060(19)
Re1 P12 2.5151(19)
Re2 Re3 2.7768(4)
Re2 S1 2.3360(17)
Re2 S2 2.3355(17)
Re2 S4 2.3110(17)
Re2 Br2 2.5572(10)
Re2 P21 2.4955(19)
Re2 P22 2.5213(18)
Re3 S1 2.3376(18)
Re3 S3 2.2906(17)
Re3 S4 2.3459(17)
Re3 Br3 2.5524(10)
Re3 P31 2.5098(19)
Re3 P32 2.530(2)
Br4 Cl1A 2.277(19)
P11 C1 1.849(8)
P11 C111 1.825(9)
P11 C121 1.826(9)
P12 C2 1.844(7)
P12 C131 1.837(9)
P12 C141 1.830(8)
P21 C3 1.827(8)
P21 C211 1.828(8)
P21 C221 1.838(8)
P22 C4 1.830(8)
P22 C231 1.833(8)
P22 C241 1.837(7)
P31 C5 1.835(8)
P31 C311 1.818(8)
P31 C321 1.833(7)
P32 C6 1.845(8)
P32 C331 1.815(9)
P32 C341 1.837(8)
C1 C2 1.513(11)
C3 C4 1.524(11)
C5 C6 1.519(13)
C111 C112 1.410(13)
C111 C116 1.386(13)
C112 C115 1.378(15)
C113 C114 1.370(17)
C113 C116 1.391(14)
C114 C115 1.387(18)
C121 C122 1.381(12)
C121 C126 1.400(12)
C122 C123 1.402(14)
C123 C124 1.378(17)
C124 C125 1.390(16)
C125 C126 1.392(13)
C131 C132 1.406(12)
C131 C136 1.387(13)
C132 C133 1.382(14)
C133 C134 1.378(17)
C134 C135 1.371(17)
C135 C136 1.378(13)
C141 C142 1.387(11)
C141 C146 1.396(11)
C142 C143 1.380(12)
C143 C144 1.383(14)
C144 C145 1.390(14)
C145 C146 1.387(12)
C211 C212 1.392(13)
C211 C216 1.395(13)
C212 C213 1.402(13)
C213 C214 1.371(17)
C214 C215 1.358(17)
C215 C216 1.399(12)
C221 C222 1.401(11)
C221 C226 1.387(12)
C222 C223 1.378(12)
C223 C224 1.384(14)
C224 C225 1.390(13)
C225 C226 1.386(11)
C231 C232 1.403(12)
C231 C236 1.376(11)
C232 C233 1.388(11)
C233 C234 1.378(14)
C234 C235 1.366(15)
C235 C236 1.393(13)
C241 C242 1.388(10)
C241 C246 1.384(11)
C242 C243 1.386(10)
C243 C244 1.364(12)
C244 C245 1.388(13)
C245 C246 1.393(11)
C311 C312 1.373(12)
C311 C316 1.396(14)
C312 C313 1.413(15)
C313 C314 1.369(19)
C314 C315 1.365(17)
C315 C316 1.397(12)
C321 C322 1.380(11)
C321 C326 1.398(11)
C322 C323 1.399(10)
C323 C324 1.384(13)
C324 C325 1.377(12)
C325 C326 1.388(11)
C331 C332 1.403(11)
C331 C336 1.407(12)
C332 C333 1.383(15)
C333 C334 1.380(16)
C334 C335 1.393(13)
C335 C336 1.380(12)
C341 C342 1.410(12)
C341 C346 1.384(13)
C342 C343 1.392(14)
C343 C344 1.374(18)
C344 C345 1.374(17)
C345 C346 1.394(12)
Cl1 C1SA 1.728(16)
Cl1 C1SB 1.814(14)
Cl2 C1SA 1.768(14)
Cl2 C1SB 1.790(15)
Cl1A C1SA 1.68(2)
C1SA C1SB 2.007(18)
Cl3 C2S 2.11(3)
Cl4 C2S 1.70(3)
Cl5 C3S 1.667(19)
Cl6 C3S 1.714(16)
Cl7 C4S 2.05(4)
Cl8 C4S 1.58(2)
Cl9 C5S 1.729(17)
Cl10 Cl11 2.438(14)
Cl10 C5S 1.793(17)
Cl11 C5S 1.636(18)
|
1501649.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/16/1501649.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_1501649
loop_
_publ_author_name
'Chow, Cheuk-Fai'
'Kong, Hoi-Kuan'
'Leung, Shu-Wai'
'Chiu, Brenda K. W.'
'Koo, Chi-Kin'
'Lei, Elva N. Y.'
'Lam, Michael H. W.'
'Wong, Wing-Tak'
'Wong, Wai-Yeung'
_publ_section_title
;
Heterobimetallic Ru(II)-Eu(III) complex as chemodosimeter for selective
biogenic amine odorants detection in fish sample.
;
_journal_issue 1
_journal_name_full 'Analytical chemistry'
_journal_page_first 289
_journal_page_last 296
_journal_paper_doi 10.1021/ac102393f
_journal_volume 83
_journal_year 2011
_chemical_formula_moiety 'C44 H56 Eu N12 O4 Ru2, K, 8(H2O) '
_chemical_formula_sum 'C44 H72 Eu K N12 O12 Ru2'
_chemical_formula_weight 1354.32
_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 94.45(1)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 10.516(2)
_cell_length_b 13.136(3)
_cell_length_c 42.764(9)
_cell_measurement_reflns_used 37259
_cell_measurement_temperature 303(1)
_cell_measurement_theta_max 27.5
_cell_measurement_theta_min 1.0
_cell_volume 5890(2)
_computing_cell_refinement 'SAINT (Bruker, 1999)'
_computing_data_collection 'SMART (Bruker, 1998)'
_computing_data_reduction
'SAINT & CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2003)'
_computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material 'CrystalStructure Ver. 3.5.1'
_computing_structure_refinement 'CRYSTALS (Watkin et al., 1996)'
_computing_structure_solution 'SHELX97 (Sheldrick, 1997)'
_diffrn_measured_fraction_theta_full 0.9756
_diffrn_measured_fraction_theta_max 0.9756
_diffrn_measurement_device_type CCD
_diffrn_measurement_method \w
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.7107
_diffrn_reflns_av_R_equivalents 0.048
_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 55
_diffrn_reflns_limit_l_min -55
_diffrn_reflns_number 27704
_diffrn_reflns_theta_full 27.54
_diffrn_reflns_theta_max 27.54
_exptl_absorpt_coefficient_mu 1.690
_exptl_absorpt_correction_T_max 0.935
_exptl_absorpt_correction_T_min 0.798
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'SADABS (Sheldrick, 1997)'
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.527
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 2744.00
_exptl_crystal_size_max 0.26
_exptl_crystal_size_mid 0.12
_exptl_crystal_size_min 0.04
_refine_diff_density_max 2.47
_refine_diff_density_min -3.08
_refine_ls_extinction_coef 281.2(20)
_refine_ls_extinction_method
'Larson (1970) Crystallographic Computing eq. 22'
_refine_ls_goodness_of_fit_ref 1.030
_refine_ls_hydrogen_treatment refall
_refine_ls_number_parameters 685
_refine_ls_number_reflns 5964
_refine_ls_R_factor_gt 0.0680
_refine_ls_shift/su_max 0.0020
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
'w = 1/[0.0002Fo^2^ + 1.0000\s(Fo^2^) + 0.0350]'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_ref 0.0960
_reflns_number_gt 4933
_reflns_number_total 13852
_reflns_threshold_expression F^2^>2.0\s(F^2^)
_cod_data_source_file ac102393f_si_002.cif
_cod_data_source_block '_wt1033w'
_cod_original_cell_volume 5889.5(21)
_cod_original_sg_symbol_H-M 'P 21/n'
_cod_original_formula_sum 'C44 H72 Eu K N12 O12 Ru2 '
_cod_database_code 1501649
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
Eu(1) Eu 0.89017(12) 0.30861(7) 0.25710(3) 0.0248(3) Uani 1.00 1 d
Ru(1) Ru 0.8270(2) 0.6260(1) 0.34137(4) 0.0272(5) Uani 1.00 1 d
Ru(2) Ru 0.9373(2) 0.6297(1) 0.17289(4) 0.0257(5) Uani 1.00 1 d
K(1) K 1.0225(6) 0.6543(5) 0.2645(1) 0.059(2) Uani 1.00 1 d
O(1) O 0.957(2) 0.2436(13) 0.3108(4) 0.054(6) Uani 1.00 1 d
O(2) O 0.869(2) 0.1234(11) 0.2568(5) 0.067(6) Uani 1.00 1 d
O(3) O 1.013(2) 0.2406(13) 0.2145(4) 0.056(6) Uani 1.00 1 d
O(4) O 1.113(1) 0.3387(10) 0.2692(4) 0.038(5) Uani 1.00 1 d
O(5) O 1.229(2) 0.519(2) 0.2713(5) 0.084(8) Uani 1.00 1 d
O(6) O 1.235(2) 0.783(2) 0.2935(5) 0.072(7) Uani 1.00 1 d
O(7) O 0.915(2) 0.977(2) 0.3064(6) 0.089(8) Uani 1.00 1 d
O(8) O 0.167(2) 0.987(2) 0.2914(7) 0.127(11) Uani 1.00 1 d
O(9) O 0.279(2) 0.503(1) 0.3383(5) 0.073(7) Uani 1.00 1 d
O(10) O 0.179(2) 0.303(1) 0.3460(4) 0.059(6) Uani 1.00 1 d
O(11) O 0.081(2) 0.174(2) 0.3967(5) 0.084(8) Uani 1.00 1 d
O(12) O 0.522(3) 0.471(2) 0.2773(6) 0.111(10) Uani 1.00 1 d
N(1) N 1.123(2) 0.675(2) 0.3430(6) 0.061(8) Uani 1.00 1 d
N(2) N 0.532(2) 0.584(2) 0.3387(6) 0.061(8) Uani 1.00 1 d
N(3) N 0.877(2) 0.458(2) 0.2911(5) 0.047(7) Uani 1.00 1 d
N(4) N 0.722(2) 0.283(1) 0.2132(5) 0.043(6) Uani 1.00 1 d
N(5) N 0.690(2) 0.280(1) 0.2826(4) 0.044(7) Uani 1.00 1 d
N(6) N 0.908(2) 0.460(2) 0.2236(5) 0.042(7) Uani 1.00 1 d
N(7) N 1.205(2) 0.692(2) 0.2070(5) 0.059(7) Uani 1.00 1 d
N(8) N 0.658(2) 0.601(2) 0.1383(5) 0.051(7) Uani 1.00 1 d
N(9) N 0.798(2) 0.724(1) 0.3788(4) 0.033(6) Uani 1.00 1 d
N(10) N 0.852(2) 0.532(1) 0.3808(4) 0.032(5) Uani 1.00 1 d
N(11) N 1.032(2) 0.5361(12) 0.1418(4) 0.028(5) Uani 1.00 1 d
N(12) N 0.980(2) 0.729(1) 0.1366(4) 0.035(6) Uani 1.00 1 d
C(1) C 1.018(2) 0.658(1) 0.3432(5) 0.028(6) Uani 1.00 1 d
C(2) C 0.640(2) 0.597(2) 0.3391(5) 0.031(6) Uani 1.00 1 d
C(3) C 0.856(2) 0.521(2) 0.3095(5) 0.034(7) Uani 1.00 1 d
C(4) C 0.797(2) 0.722(2) 0.3075(5) 0.027(6) Uani 1.00 1 d
C(5) C 0.858(2) 0.725(2) 0.2001(5) 0.031(6) Uani 1.00 1 d
C(6) C 0.915(2) 0.523(2) 0.2046(5) 0.026(6) Uani 1.00 1 d
C(7) C 1.109(2) 0.666(1) 0.1951(5) 0.028(6) Uani 1.00 1 d
C(8) C 0.760(3) 0.607(2) 0.1495(6) 0.039(7) Uani 1.00 1 d
C(9) C 0.769(2) 0.825(2) 0.3766(6) 0.042(7) Uani 1.00 1 d
C(10) C 0.744(2) 0.883(2) 0.4027(5) 0.035(7) Uani 1.00 1 d
C(11) C 0.744(2) 0.840(2) 0.4310(5) 0.033(7) Uani 1.00 1 d
C(12) C 0.774(2) 0.739(2) 0.4338(5) 0.038(7) Uani 1.00 1 d
C(13) C 0.799(2) 0.681(2) 0.4072(5) 0.031(6) Uani 1.00 1 d
C(14) C 0.830(2) 0.570(2) 0.4087(5) 0.031(6) Uani 1.00 1 d
C(15) C 0.834(2) 0.514(2) 0.4363(5) 0.035(7) Uani 1.00 1 d
C(16) C 0.858(2) 0.410(2) 0.4359(6) 0.041(7) Uani 1.00 1 d
C(17) C 0.883(2) 0.370(2) 0.4072(6) 0.044(8) Uani 1.00 1 d
C(18) C 0.884(2) 0.432(2) 0.3811(6) 0.043(7) Uani 1.00 1 d
C(19) C 0.724(3) 0.909(2) 0.4598(7) 0.050(9) Uani 1.00 1 d
C(20) C 0.630(3) 0.992(2) 0.4524(7) 0.087(12) Uani 1.00 1 d
C(21) C 0.848(3) 0.960(3) 0.4707(8) 0.11(2) Uani 1.00 1 d
C(22) C 0.684(4) 0.847(3) 0.4860(9) 0.12(1) Uiso 1.00 1 d
C(23) C 0.859(3) 0.342(2) 0.4649(7) 0.057(9) Uani 1.00 1 d
C(24) C 0.818(4) 0.395(3) 0.4925(8) 0.12(2) Uani 1.00 1 d
C(25) C 0.990(3) 0.296(3) 0.4720(8) 0.102(12) Uiso 1.00 1 d
C(26) C 0.765(4) 0.259(3) 0.4577(8) 0.11(2) Uani 1.00 1 d
C(27) C 1.062(2) 0.436(2) 0.1461(6) 0.047(8) Uani 1.00 1 d
C(28) C 1.133(2) 0.383(2) 0.1268(6) 0.047(8) Uani 1.00 1 d
C(29) C 1.191(2) 0.430(2) 0.1027(5) 0.035(7) Uani 1.00 1 d
C(30) C 1.161(2) 0.533(2) 0.0978(5) 0.025(5) Uiso 1.00 1 d
C(31) C 1.085(2) 0.582(2) 0.1182(5) 0.029(6) Uani 1.00 1 d
C(32) C 1.054(2) 0.693(2) 0.1145(5) 0.026(5) Uani 1.00 1 d
C(33) C 1.096(2) 0.755(2) 0.0913(5) 0.029(6) Uani 1.00 1 d
C(34) C 1.062(2) 0.858(2) 0.0888(5) 0.038(7) Uani 1.00 1 d
C(35) C 0.983(2) 0.892(2) 0.1111(5) 0.041(8) Uani 1.00 1 d
C(36) C 0.945(2) 0.827(2) 0.1344(5) 0.039(7) Uani 1.00 1 d
C(37) C 1.278(3) 0.374(2) 0.0818(6) 0.054(9) Uani 1.00 1 d
C(38) C 1.412(3) 0.379(2) 0.0988(8) 0.091(13) Uani 1.00 1 d
C(39) C 1.242(3) 0.264(2) 0.0779(7) 0.073(11) Uani 1.00 1 d
C(40) C 1.281(3) 0.423(2) 0.0496(6) 0.080(12) Uani 1.00 1 d
C(41) C 1.118(3) 0.924(2) 0.0647(6) 0.047(8) Uani 1.00 1 d
C(42) C 1.119(4) 0.874(2) 0.0333(6) 0.097(13) Uani 1.00 1 d
C(43) C 1.042(3) 1.024(2) 0.0595(7) 0.076(11) Uani 1.00 1 d
C(44) C 1.255(3) 0.954(2) 0.0766(7) 0.071(11) Uani 1.00 1 d
H(1) H 0.766(2) 0.857(2) 0.3566(6) 0.050(8) Uiso 1.00 1 c
H(2) H 0.727(2) 0.954(2) 0.4002(5) 0.042(7) Uiso 1.00 1 c
H(3) H 0.778(2) 0.707(2) 0.4538(5) 0.045(7) Uiso 1.00 1 c
H(4) H 0.821(2) 0.547(2) 0.4555(5) 0.042(7) Uiso 1.00 1 c
H(5) H 0.901(2) 0.299(2) 0.4053(6) 0.053(8) Uiso 1.00 1 c
H(6) H 0.909(2) 0.403(2) 0.3622(6) 0.052(8) Uiso 1.00 1 c
H(7) H 0.602(3) 1.019(2) 0.4714(7) 0.10(1) Uiso 1.00 1 c
H(8) H 0.669(3) 1.045(2) 0.4414(7) 0.10(1) Uiso 1.00 1 c
H(9) H 0.559(3) 0.966(2) 0.4399(7) 0.10(1) Uiso 1.00 1 c
H(10) H 0.912(3) 0.910(3) 0.4758(8) 0.13(2) Uiso 1.00 1 c
H(11) H 0.875(3) 1.002(3) 0.4544(8) 0.13(2) Uiso 1.00 1 c
H(12) H 0.837(3) 1.000(3) 0.4887(8) 0.13(2) Uiso 1.00 1 c
H(13) H 0.705(4) 0.881(3) 0.5052(9) 0.14(2) Uiso 1.00 1 c
H(14) H 0.594(4) 0.836(3) 0.4833(9) 0.14(2) Uiso 1.00 1 c
H(15) H 0.726(4) 0.783(3) 0.4862(9) 0.14(2) Uiso 1.00 1 c
H(16) H 0.853(4) 0.462(3) 0.4932(8) 0.14(2) Uiso 1.00 1 c
H(17) H 0.728(4) 0.399(3) 0.4912(8) 0.14(2) Uiso 1.00 1 c
H(18) H 0.847(4) 0.359(3) 0.5110(8) 0.14(2) Uiso 1.00 1 c
H(19) H 0.988(3) 0.251(3) 0.4895(8) 0.12(1) Uiso 1.00 1 c
H(20) H 1.012(3) 0.258(3) 0.4542(8) 0.12(1) Uiso 1.00 1 c
H(21) H 1.051(3) 0.348(3) 0.4766(8) 0.12(1) Uiso 1.00 1 c
H(22) H 0.695(4) 0.285(3) 0.4446(8) 0.13(2) Uiso 1.00 1 c
H(23) H 0.805(4) 0.205(3) 0.4473(8) 0.13(2) Uiso 1.00 1 c
H(24) H 0.735(4) 0.234(3) 0.4767(8) 0.13(2) Uiso 1.00 1 c
H(25) H 1.030(2) 0.401(2) 0.1634(6) 0.057(8) Uiso 1.00 1 c
H(26) H 1.145(2) 0.312(2) 0.1299(6) 0.056(8) Uiso 1.00 1 c
H(27) H 1.192(2) 0.568(2) 0.0807(5) 0.030(6) Uiso 1.00 1 c
H(28) H 1.150(2) 0.727(2) 0.0766(5) 0.034(6) Uiso 1.00 1 c
H(29) H 0.954(2) 0.961(2) 0.1105(5) 0.050(8) Uiso 1.00 1 c
H(30) H 0.892(2) 0.853(2) 0.1495(5) 0.047(8) Uiso 1.00 1 c
H(31) H 1.412(3) 0.347(2) 0.1187(8) 0.11(1) Uiso 1.00 1 c
H(32) H 1.471(3) 0.345(2) 0.0866(8) 0.11(1) Uiso 1.00 1 c
H(33) H 1.437(3) 0.448(2) 0.1016(8) 0.11(1) Uiso 1.00 1 c
H(34) H 1.157(3) 0.259(2) 0.0688(7) 0.087(12) Uiso 1.00 1 c
H(35) H 1.298(3) 0.232(2) 0.0646(7) 0.087(12) Uiso 1.00 1 c
H(36) H 1.248(3) 0.231(2) 0.0978(7) 0.087(12) Uiso 1.00 1 c
H(37) H 1.308(3) 0.492(2) 0.0520(6) 0.096(13) Uiso 1.00 1 c
H(38) H 1.339(3) 0.387(2) 0.0377(6) 0.096(13) Uiso 1.00 1 c
H(39) H 1.198(3) 0.421(2) 0.0390(6) 0.096(13) Uiso 1.00 1 c
H(40) H 1.035(4) 0.856(2) 0.0259(6) 0.12(2) Uiso 1.00 1 c
H(41) H 1.155(4) 0.919(2) 0.0189(6) 0.12(2) Uiso 1.00 1 c
H(42) H 1.170(4) 0.813(2) 0.0352(6) 0.12(2) Uiso 1.00 1 c
H(43) H 1.023(3) 1.051(2) 0.0792(7) 0.092(12) Uiso 1.00 1 c
H(44) H 1.091(3) 1.072(2) 0.0489(7) 0.092(12) Uiso 1.00 1 c
H(45) H 0.965(3) 1.011(2) 0.0471(7) 0.092(12) Uiso 1.00 1 c
H(46) H 1.305(3) 0.894(2) 0.0799(7) 0.085(11) Uiso 1.00 1 c
H(47) H 1.291(3) 0.996(2) 0.0616(7) 0.085(11) Uiso 1.00 1 c
H(48) H 1.253(3) 0.990(2) 0.0959(7) 0.085(11) Uiso 1.00 1 c
H(49) H 0.124(2) 0.187(2) 0.3852(5) 0.100(8) Uiso 1.00 1 c
H(50) H 0.034(2) 0.136(2) 0.3992(5) 0.100(8) 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
Eu(1) 0.0270(6) 0.0184(5) 0.0292(6) -0.0014(6) 0.0040(5) -0.0001(6)
Ru(1) 0.0306(11) 0.0248(10) 0.0266(11) -0.0003(8) 0.0040(9) 0.0004(8)
Ru(2) 0.0282(11) 0.0227(10) 0.0270(11) 0.0003(8) 0.0074(9) 0.0019(8)
K(1) 0.071(4) 0.058(4) 0.047(4) -0.003(3) 0.008(3) -0.001(3)
O(1) 0.041(11) 0.057(12) 0.062(12) -0.007(9) -0.011(9) 0.017(10)
O(2) 0.10(2) 0.030(9) 0.072(12) 0.034(11) 0.010(11) 0.015(11)
O(3) 0.060(12) 0.049(11) 0.062(12) 0.004(10) 0.019(10) -0.017(10)
O(4) 0.038(9) 0.026(8) 0.049(10) -0.004(7) -0.002(8) -0.002(7)
O(5) 0.06(1) 0.06(1) 0.12(2) -0.023(11) 0.006(13) 0.008(13)
O(6) 0.07(1) 0.063(13) 0.09(1) 0.003(11) 0.024(11) 0.003(11)
O(7) 0.08(2) 0.06(2) 0.13(2) -0.014(12) 0.02(1) -0.01(1)
O(8) 0.07(2) 0.07(2) 0.24(3) 0.01(1) 0.03(2) 0.01(2)
O(9) 0.042(11) 0.042(11) 0.13(2) -0.010(9) 0.004(12) 0.006(12)
O(10) 0.050(11) 0.063(12) 0.062(12) -0.009(10) -0.004(9) -0.003(11)
O(11) 0.09(2) 0.07(2) 0.09(2) 0.009(13) -0.000(13) -0.002(13)
O(12) 0.12(2) 0.10(2) 0.12(2) -0.01(2) -0.01(2) 0.01(2)
N(1) 0.038(13) 0.06(2) 0.08(2) -0.005(12) 0.001(13) 0.00(1)
N(2) 0.028(13) 0.06(2) 0.10(2) -0.013(11) 0.010(13) 0.02(1)
N(3) 0.06(2) 0.06(2) 0.031(12) -0.010(12) 0.018(11) -0.006(11)
N(4) 0.06(1) 0.033(12) 0.041(12) 0.007(10) 0.010(11) 0.010(10)
N(5) 0.06(1) 0.038(12) 0.037(12) -0.010(10) 0.006(11) -0.001(10)
N(6) 0.025(11) 0.045(13) 0.06(1) -0.024(10) -0.003(10) 0.014(11)
N(7) 0.041(13) 0.06(2) 0.08(2) -0.008(13) -0.009(12) 0.01(1)
N(8) 0.04(1) 0.041(13) 0.06(2) -0.012(11) -0.028(12) -0.002(11)
N(9) 0.037(12) 0.029(11) 0.034(11) -0.001(9) 0.013(10) 0.004(9)
N(10) 0.033(11) 0.038(11) 0.025(10) 0.012(9) 0.005(9) 0.001(9)
N(11) 0.032(11) 0.013(9) 0.038(11) -0.004(8) -0.005(9) 0.002(8)
N(12) 0.037(12) 0.034(12) 0.037(12) 0.014(9) 0.010(10) -0.003(9)
C(1) 0.05(2) 0.013(10) 0.022(11) -0.005(10) 0.002(11) -0.008(8)
C(2) 0.04(1) 0.026(12) 0.030(12) -0.005(10) -0.003(11) 0.007(10)
C(3) 0.03(1) 0.05(2) 0.020(13) -0.008(13) -0.001(11) 0.012(12)
C(4) 0.025(12) 0.028(12) 0.028(12) -0.013(9) 0.005(10) -0.012(9)
C(5) 0.04(1) 0.033(13) 0.020(11) -0.017(11) 0.009(10) 0.009(9)
C(6) 0.015(11) 0.029(13) 0.03(1) -0.003(10) 0.000(10) -0.003(11)
C(7) 0.026(12) 0.016(11) 0.04(1) -0.003(9) 0.008(11) -0.003(9)
C(8) 0.05(2) 0.015(11) 0.06(2) 0.002(11) 0.02(1) -0.014(11)
C(9) 0.06(2) 0.020(12) 0.04(2) 0.027(12) 0.015(13) 0.024(11)
C(10) 0.05(2) 0.016(11) 0.04(1) 0.007(11) 0.005(12) 0.006(10)
C(11) 0.05(2) 0.032(13) 0.015(11) 0.000(11) -0.000(11) -0.002(9)
C(12) 0.06(2) 0.024(12) 0.027(12) 0.005(12) 0.012(12) 0.011(10)
C(13) 0.026(11) 0.032(13) 0.038(13) 0.002(10) 0.017(10) -0.013(11)
C(14) 0.026(12) 0.029(12) 0.037(13) 0.001(10) 0.001(10) -0.004(10)
C(15) 0.05(2) 0.04(1) 0.011(10) 0.017(12) 0.002(10) 0.012(10)
C(16) 0.05(2) 0.023(12) 0.05(2) -0.004(11) 0.015(13) -0.006(11)
C(17) 0.05(2) 0.031(13) 0.05(2) -0.006(13) -0.004(13) 0.013(12)
C(18) 0.05(2) 0.04(2) 0.04(1) 0.022(13) 0.006(12) -0.000(12)
C(19) 0.06(2) 0.03(1) 0.06(2) 0.003(13) 0.01(2) -0.007(13)
C(20) 0.10(3) 0.07(2) 0.09(3) 0.04(2) -0.01(2) -0.04(2)
C(21) 0.08(3) 0.17(4) 0.09(3) -0.00(3) 0.01(2) -0.07(3)
C(23) 0.06(2) 0.024(13) 0.08(2) 0.014(13) 0.01(2) 0.020(13)
C(24) 0.20(5) 0.10(3) 0.07(2) 0.03(3) 0.06(3) 0.03(2)
C(26) 0.13(4) 0.07(2) 0.11(3) -0.02(3) 0.00(3) 0.03(2)
C(27) 0.06(2) 0.022(12) 0.06(2) 0.005(12) 0.01(1) 0.020(12)
C(28) 0.04(2) 0.04(2) 0.05(2) 0.010(13) 0.008(13) -0.004(13)
C(29) 0.04(1) 0.035(13) 0.029(12) 0.004(11) 0.011(11) 0.013(10)
C(31) 0.028(12) 0.031(12) 0.027(12) -0.007(10) -0.002(10) 0.009(10)
C(32) 0.039(12) 0.015(10) 0.026(11) -0.001(10) 0.008(10) -0.015(9)
C(33) 0.034(13) 0.031(12) 0.024(12) 0.005(10) 0.021(10) 0.006(10)
C(34) 0.05(2) 0.03(1) 0.04(1) -0.021(12) 0.007(12) 0.004(11)
C(35) 0.05(2) 0.04(1) 0.04(2) 0.006(12) 0.033(13) -0.001(11)
C(36) 0.034(13) 0.06(2) 0.028(13) 0.015(12) 0.017(11) 0.011(12)
C(37) 0.07(2) 0.04(2) 0.05(2) 0.03(2) 0.03(2) -0.01(1)
C(38) 0.07(2) 0.08(2) 0.13(3) 0.04(2) 0.04(2) 0.04(2)
C(39) 0.12(3) 0.03(2) 0.07(2) 0.01(2) 0.03(2) -0.01(2)
C(40) 0.14(3) 0.06(2) 0.04(2) 0.03(2) 0.04(2) -0.01(2)
C(41) 0.06(2) 0.04(1) 0.05(2) 0.006(13) 0.03(1) 0.022(12)
C(42) 0.19(4) 0.05(2) 0.05(2) -0.05(2) 0.06(2) -0.00(2)
C(43) 0.09(3) 0.06(2) 0.08(2) 0.00(2) 0.02(2) 0.04(2)
C(44) 0.07(2) 0.05(2) 0.10(3) -0.01(2) 0.02(2) 0.02(2)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.000 0.000
;
International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.4)
;
N N 0.006 0.003
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.011 0.006
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Eu Eu -0.158 3.668
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Ru Ru -1.259 0.836
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
K K 0.200 0.250
;
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
O(1) Eu(1) O(2) 71.5(6) yes
O(1) Eu(1) O(3) 115.3(6) yes
O(1) Eu(1) O(4) 70.0(5) yes
O(1) Eu(1) N(3) 75.8(6) yes
O(1) Eu(1) N(4) 140.9(6) yes
O(1) Eu(1) N(5) 74.3(6) yes
O(1) Eu(1) N(6) 141.3(6) yes
O(2) Eu(1) O(3) 71.9(6) yes
O(2) Eu(1) O(4) 104.6(6) yes
O(2) Eu(1) N(3) 142.3(7) yes
O(2) Eu(1) N(4) 78.7(6) yes
O(2) Eu(1) N(5) 76.9(7) yes
O(2) Eu(1) N(6) 144.1(7) yes
O(3) Eu(1) O(4) 70.2(5) yes
O(3) Eu(1) N(3) 141.4(7) yes
O(3) Eu(1) N(4) 77.1(6) yes
O(3) Eu(1) N(5) 141.2(6) yes
O(3) Eu(1) N(6) 78.1(6) yes
O(4) Eu(1) N(3) 80.8(6) yes
O(4) Eu(1) N(4) 143.9(6) yes
O(4) Eu(1) N(5) 141.4(6) yes
O(4) Eu(1) N(6) 82.7(5) yes
N(3) Eu(1) N(4) 118.9(7) yes
N(3) Eu(1) N(5) 76.6(7) yes
N(3) Eu(1) N(6) 73.2(7) yes
N(4) Eu(1) N(5) 74.7(6) yes
N(4) Eu(1) N(6) 75.8(6) yes
N(5) Eu(1) N(6) 119.1(6) yes
N(9) Ru(1) N(10) 76.3(7) yes
N(9) Ru(1) C(1) 92.6(8) yes
N(9) Ru(1) C(2) 87.2(8) yes
N(9) Ru(1) C(3) 173.4(9) yes
N(9) Ru(1) C(4) 98.4(8) yes
N(10) Ru(1) C(1) 91.7(7) yes
N(10) Ru(1) C(2) 89.3(8) yes
N(10) Ru(1) C(3) 97.1(9) yes
N(10) Ru(1) C(4) 174.6(8) yes
C(1) Ru(1) C(2) 178.9(8) yes
C(1) Ru(1) C(3) 88.0(9) yes
C(1) Ru(1) C(4) 89.8(8) yes
C(2) Ru(1) C(3) 92.3(9) yes
C(2) Ru(1) C(4) 89.2(9) yes
C(3) Ru(1) C(4) 88.1(9) yes
N(11) Ru(2) N(12) 76.0(7) yes
N(11) Ru(2) C(5) 175.1(8) yes
N(11) Ru(2) C(6) 95.9(8) yes
N(11) Ru(2) C(7) 89.2(8) yes
N(11) Ru(2) C(8) 93.7(8) yes
N(12) Ru(2) C(5) 99.7(8) yes
N(12) Ru(2) C(6) 171.6(8) yes
N(12) Ru(2) C(7) 88.0(8) yes
N(12) Ru(2) C(8) 88.2(8) yes
C(5) Ru(2) C(6) 88.3(9) yes
C(5) Ru(2) C(7) 88.5(9) yes
C(5) Ru(2) C(8) 88.3(9) yes
C(6) Ru(2) C(7) 89.7(8) yes
C(6) Ru(2) C(8) 94.5(9) yes
C(7) Ru(2) C(8) 174.6(8) yes
O(5) K(1) O(6) 76.5(6) yes
O(5) K(1) N(3) 81.1(6) yes
O(5) K(1) N(6) 79.0(6) yes
O(5) K(1) N(7) 71.2(6) yes
O(5) K(1) C(3) 92.5(6) yes
O(5) K(1) C(4) 135.3(6) yes
O(5) K(1) C(5) 128.6(6) yes
O(5) K(1) C(6) 87.9(6) yes
O(5) K(1) C(7) 81.5(6) yes
O(6) K(1) N(3) 131.2(6) yes
O(6) K(1) N(6) 153.3(6) yes
O(6) K(1) N(7) 76.5(6) yes
O(6) K(1) C(3) 118.8(6) yes
O(6) K(1) C(4) 99.4(6) yes
O(6) K(1) C(5) 121.1(6) yes
O(6) K(1) C(6) 146.9(6) yes
O(6) K(1) C(7) 95.8(6) yes
N(3) K(1) N(6) 53.4(5) yes
N(3) K(1) N(7) 134.7(6) yes
N(3) K(1) C(3) 20.7(6) yes
N(3) K(1) C(4) 68.4(6) yes
N(3) K(1) C(5) 106.8(6) yes
N(3) K(1) C(6) 73.0(6) yes
N(3) K(1) C(7) 123.0(5) yes
N(6) K(1) N(7) 85.8(6) yes
N(6) K(1) C(3) 72.5(6) yes
N(6) K(1) C(4) 105.4(5) yes
N(6) K(1) C(5) 68.1(5) yes
N(6) K(1) C(6) 20.7(5) yes
N(6) K(1) C(7) 70.1(5) yes
N(7) K(1) C(3) 155.3(6) yes
N(7) K(1) C(4) 152.2(6) yes
N(7) K(1) C(5) 68.1(6) yes
N(7) K(1) C(6) 70.9(6) yes
N(7) K(1) C(7) 20.3(5) yes
C(3) K(1) C(4) 49.9(6) yes
C(3) K(1) C(5) 112.5(6) yes
C(3) K(1) C(6) 90.5(6) yes
C(3) K(1) C(7) 142.6(6) yes
C(4) K(1) C(5) 92.2(6) yes
C(4) K(1) C(6) 112.0(6) yes
C(4) K(1) C(7) 142.5(6) yes
C(5) K(1) C(6) 49.9(5) yes
C(5) K(1) C(7) 51.0(6) yes
C(6) K(1) C(7) 52.5(5) yes
H(49) O(11) H(50) 139(3) no
C(3) N(3) Eu(1) 169(2) yes
C(3) N(3) K(1) 78(1) yes
Eu(1) N(3) K(1) 112.0(7) yes
C(6) N(6) Eu(1) 171(1) yes
C(6) N(6) K(1) 77(1) yes
Eu(1) N(6) K(1) 111.2(7) yes
C(7) N(7) K(1) 75(1) yes
C(9) N(9) C(13) 117(1) yes
C(9) N(9) Ru(1) 126(1) yes
C(13) N(9) Ru(1) 116(1) yes
C(14) N(10) C(18) 114(1) yes
C(14) N(10) Ru(1) 118(1) yes
C(18) N(10) Ru(1) 126(1) yes
C(27) N(11) C(31) 115(1) yes
C(27) N(11) Ru(2) 126(1) yes
C(31) N(11) Ru(2) 117(1) yes
C(32) N(12) C(36) 116(1) yes
C(32) N(12) Ru(2) 117(1) yes
C(36) N(12) Ru(2) 125(1) yes
Ru(1) C(1) N(1) 177(2) yes
Ru(1) C(2) N(2) 177(1) yes
Ru(1) C(3) K(1) 98.7(9) yes
Ru(1) C(3) N(3) 178(1) yes
N(3) C(3) K(1) 80(1) yes
Ru(1) C(4) K(1) 99.4(8) yes
Ru(2) C(5) K(1) 95.6(8) yes
Ru(2) C(6) K(1) 96.3(8) yes
Ru(2) C(6) N(6) 176(1) yes
N(6) C(6) K(1) 82(1) yes
Ru(2) C(7) K(1) 96.6(8) yes
Ru(2) C(7) N(7) 176(2) yes
N(7) C(7) K(1) 84(1) yes
Ru(2) C(8) N(8) 173(2) yes
C(10) C(9) H(1) 118(2) no
C(10) C(9) N(9) 122(2) yes
H(1) C(9) N(9) 118(2) no
C(11) C(10) H(2) 119(2) no
C(11) C(10) C(9) 120(2) yes
H(2) C(10) C(9) 119(2) no
C(12) C(11) C(19) 122(1) yes
C(12) C(11) C(10) 118(2) yes
C(19) C(11) C(10) 119(2) yes
C(13) C(12) H(3) 119(2) no
C(13) C(12) C(11) 120(2) yes
H(3) C(12) C(11) 119(2) no
C(14) C(13) N(9) 115(1) yes
C(14) C(13) C(12) 122(1) yes
N(9) C(13) C(12) 121(2) yes
C(15) C(14) N(10) 124(2) yes
C(15) C(14) C(13) 123(2) yes
N(10) C(14) C(13) 112(1) yes
C(16) C(15) H(4) 119(2) no
C(16) C(15) C(14) 120(2) yes
H(4) C(15) C(14) 119(2) no
C(17) C(16) C(23) 119(2) yes
C(17) C(16) C(15) 115(2) yes
C(23) C(16) C(15) 124(2) yes
C(18) C(17) H(5) 120(2) no
C(18) C(17) C(16) 119(2) yes
H(5) C(17) C(16) 120(2) no
H(6) C(18) N(10) 117(2) no
H(6) C(18) C(17) 117(2) no
N(10) C(18) C(17) 124(2) yes
C(20) C(19) C(21) 106(2) yes
C(20) C(19) C(22) 109(2) yes
C(20) C(19) C(11) 112(2) yes
C(21) C(19) C(22) 107(2) yes
C(21) C(19) C(11) 109(2) yes
C(22) C(19) C(11) 110(2) yes
H(7) C(20) H(8) 109(4) no
H(7) C(20) H(9) 109(4) no
H(7) C(20) C(19) 109(3) no
H(8) C(20) H(9) 109(4) no
H(8) C(20) C(19) 109(3) no
H(9) C(20) C(19) 109(3) no
H(10) C(21) H(11) 109(4) no
H(10) C(21) H(12) 109(4) no
H(10) C(21) C(19) 109(4) no
H(11) C(21) H(12) 109(5) no
H(11) C(21) C(19) 108(3) no
H(12) C(21) C(19) 109(3) no
H(13) C(22) H(14) 109(5) no
H(13) C(22) H(15) 109(4) no
H(13) C(22) C(19) 109(4) no
H(14) C(22) H(15) 109(5) no
H(14) C(22) C(19) 109(4) no
H(15) C(22) C(19) 109(4) no
C(24) C(23) C(25) 110(2) yes
C(24) C(23) C(26) 106(2) yes
C(24) C(23) C(16) 112(2) yes
C(25) C(23) C(26) 109(2) yes
C(25) C(23) C(16) 110(2) yes
C(26) C(23) C(16) 107(2) yes
H(16) C(24) H(17) 109(5) no
H(16) C(24) H(18) 109(4) no
H(16) C(24) C(23) 109(3) no
H(17) C(24) H(18) 109(5) no
H(17) C(24) C(23) 109(3) no
H(18) C(24) C(23) 109(4) no
H(19) C(25) H(20) 109(4) no
H(19) C(25) H(21) 109(4) no
H(19) C(25) C(23) 109(3) no
H(20) C(25) H(21) 109(4) no
H(20) C(25) C(23) 108(3) no
H(21) C(25) C(23) 110(3) no
H(22) C(26) H(23) 109(4) no
H(22) C(26) H(24) 109(4) no
H(22) C(26) C(23) 109(3) no
H(23) C(26) H(24) 109(4) no
H(23) C(26) C(23) 109(4) no
H(24) C(26) C(23) 109(3) no
C(28) C(27) H(25) 118(2) no
C(28) C(27) N(11) 122(2) yes
H(25) C(27) N(11) 118(2) no
C(29) C(28) H(26) 119(2) no
C(29) C(28) C(27) 121(2) yes
H(26) C(28) C(27) 119(2) no
C(30) C(29) C(37) 121(2) yes
C(30) C(29) C(28) 115(2) yes
C(37) C(29) C(28) 122(2) yes
C(31) C(30) H(27) 120(2) no
C(31) C(30) C(29) 119(1) yes
H(27) C(30) C(29) 120(2) no
C(32) C(31) N(11) 114(1) yes
C(32) C(31) C(30) 121(1) yes
N(11) C(31) C(30) 124(1) yes
C(33) C(32) N(12) 122(1) yes
C(33) C(32) C(31) 124(1) yes
N(12) C(32) C(31) 113(1) yes
C(34) C(33) H(28) 119(2) no
C(34) C(33) C(32) 121(2) yes
H(28) C(33) C(32) 119(2) no
C(35) C(34) C(41) 124(2) yes
C(35) C(34) C(33) 115(2) yes
C(41) C(34) C(33) 120(2) yes
C(36) C(35) H(29) 119(2) no
C(36) C(35) C(34) 120(2) yes
H(29) C(35) C(34) 119(2) no
H(30) C(36) N(12) 118(2) no
H(30) C(36) C(35) 118(2) no
N(12) C(36) C(35) 123(2) yes
C(38) C(37) C(39) 107(2) yes
C(38) C(37) C(40) 108(2) yes
C(38) C(37) C(29) 105(2) yes
C(39) C(37) C(40) 109(2) yes
C(39) C(37) C(29) 112(2) yes
C(40) C(37) C(29) 112(2) yes
H(31) C(38) H(32) 109(4) no
H(31) C(38) H(33) 109(4) no
H(31) C(38) C(37) 109(3) no
H(32) C(38) H(33) 109(4) no
H(32) C(38) C(37) 109(3) no
H(33) C(38) C(37) 109(3) no
H(34) C(39) H(35) 109(3) no
H(34) C(39) H(36) 109(4) no
H(34) C(39) C(37) 109(2) no
H(35) C(39) H(36) 109(3) no
H(35) C(39) C(37) 109(3) no
H(36) C(39) C(37) 109(2) no
H(37) C(40) H(38) 109(4) no
H(37) C(40) H(39) 109(4) no
H(37) C(40) C(37) 109(2) no
H(38) C(40) H(39) 109(3) no
H(38) C(40) C(37) 109(3) no
H(39) C(40) C(37) 109(3) no
C(42) C(41) C(43) 106(2) yes
C(42) C(41) C(44) 109(2) yes
C(42) C(41) C(34) 112(2) yes
C(43) C(41) C(44) 107(2) yes
C(43) C(41) C(34) 111(2) yes
C(44) C(41) C(34) 108(2) yes
H(40) C(42) H(41) 109(3) no
H(40) C(42) H(42) 109(4) no
H(40) C(42) C(41) 109(3) no
H(41) C(42) H(42) 109(4) no
H(41) C(42) C(41) 109(3) no
H(42) C(42) C(41) 109(3) no
H(43) C(43) H(44) 109(3) no
H(43) C(43) H(45) 109(4) no
H(43) C(43) C(41) 109(3) no
H(44) C(43) H(45) 109(3) no
H(44) C(43) C(41) 109(3) no
H(45) C(43) C(41) 109(3) no
H(46) C(44) H(47) 109(3) no
H(46) C(44) H(48) 109(3) no
H(46) C(44) C(41) 109(2) no
H(47) C(44) H(48) 109(3) no
H(47) C(44) C(41) 109(3) no
H(48) C(44) C(41) 109(3) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Eu(1) O(1) 2.50(2) yes
Eu(1) O(2) 2.44(2) yes
Eu(1) O(3) 2.48(2) yes
Eu(1) O(4) 2.40(1) yes
Eu(1) N(3) 2.46(2) yes
Eu(1) N(4) 2.50(2) yes
Eu(1) N(5) 2.47(2) yes
Eu(1) N(6) 2.46(2) yes
Ru(1) N(9) 2.09(2) yes
Ru(1) N(10) 2.09(2) yes
Ru(1) C(1) 2.05(2) yes
Ru(1) C(2) 2.00(2) yes
Ru(1) C(3) 1.98(2) yes
Ru(1) C(4) 1.93(2) yes
Ru(2) N(11) 2.12(2) yes
Ru(2) N(12) 2.10(2) yes
Ru(2) C(5) 1.94(2) yes
Ru(2) C(6) 1.98(2) yes
Ru(2) C(7) 2.03(2) yes
Ru(2) C(8) 2.07(2) yes
K(1) O(5) 2.81(2) yes
K(1) O(6) 2.99(2) yes
K(1) N(3) 3.25(2) yes
K(1) N(6) 3.27(2) yes
K(1) N(7) 3.27(2) yes
K(1) C(3) 3.22(3) yes
K(1) C(4) 3.24(2) yes
K(1) C(5) 3.27(2) yes
K(1) C(6) 3.22(2) yes
K(1) C(7) 3.17(2) yes
O(11) H(49) 0.72(3) no
O(11) H(50) 0.71(3) no
N(1) C(1) 1.14(3) yes
N(2) C(2) 1.15(3) yes
N(3) C(3) 1.16(3) yes
N(6) C(6) 1.17(3) yes
N(7) C(7) 1.14(3) yes
N(8) C(8) 1.14(3) yes
N(9) C(9) 1.36(3) yes
N(9) C(13) 1.33(3) yes
N(10) C(14) 1.33(3) yes
N(10) C(18) 1.35(3) yes
N(11) C(27) 1.37(3) yes
N(11) C(31) 1.33(3) yes
N(12) C(32) 1.35(3) yes
N(12) C(36) 1.34(3) yes
C(9) C(10) 1.39(3) yes
C(9) H(1) 0.95(3) no
C(10) C(11) 1.33(3) yes
C(10) H(2) 0.95(3) no
C(11) C(12) 1.37(3) yes
C(11) C(19) 1.55(3) yes
C(12) C(13) 1.41(3) yes
C(12) H(3) 0.95(3) no
C(13) C(14) 1.50(3) yes
C(14) C(15) 1.39(3) yes
C(15) C(16) 1.38(3) yes
C(15) H(4) 0.95(3) no
C(16) C(17) 1.39(3) yes
C(16) C(23) 1.54(4) yes
C(17) C(18) 1.38(3) yes
C(17) H(5) 0.95(3) no
C(18) H(6) 0.95(3) no
C(19) C(20) 1.50(4) yes
C(19) C(21) 1.51(4) yes
C(19) C(22) 1.47(5) yes
C(20) H(7) 0.95(4) no
C(20) H(8) 0.95(4) no
C(20) H(9) 0.95(4) no
C(21) H(10) 0.95(5) no
C(21) H(11) 0.95(5) no
C(21) H(12) 0.95(5) no
C(22) H(13) 0.95(5) no
C(22) H(14) 0.95(5) no
C(22) H(15) 0.95(6) no
C(23) C(24) 1.47(5) yes
C(23) C(25) 1.51(4) yes
C(23) C(26) 1.49(4) yes
C(24) H(16) 0.95(5) no
C(24) H(17) 0.95(6) no
C(24) H(18) 0.95(5) no
C(25) H(19) 0.95(5) no
C(25) H(20) 0.95(5) no
C(25) H(21) 0.95(5) no
C(26) H(22) 0.95(5) no
C(26) H(23) 0.95(5) no
C(26) H(24) 0.95(5) no
C(27) C(28) 1.35(4) yes
C(27) H(25) 0.95(4) no
C(28) C(29) 1.38(3) yes
C(28) H(26) 0.95(4) no
C(29) C(30) 1.40(3) yes
C(29) C(37) 1.52(4) yes
C(30) C(31) 1.38(3) yes
C(30) H(27) 0.95(3) no
C(31) C(32) 1.50(3) yes
C(32) C(33) 1.39(3) yes
C(33) C(34) 1.40(3) yes
C(33) H(28) 0.95(3) no
C(34) C(35) 1.40(3) yes
C(34) C(41) 1.51(4) yes
C(35) C(36) 1.40(3) yes
C(35) H(29) 0.95(3) no
C(36) H(30) 0.95(3) no
C(37) C(38) 1.54(4) yes
C(37) C(39) 1.50(4) yes
C(37) C(40) 1.52(4) yes
C(38) H(31) 0.95(5) no
C(38) H(32) 0.95(5) no
C(38) H(33) 0.95(4) no
C(39) H(34) 0.95(4) no
C(39) H(35) 0.95(4) no
C(39) H(36) 0.95(4) no
C(40) H(37) 0.95(4) no
C(40) H(38) 0.95(4) no
C(40) H(39) 0.95(5) no
C(41) C(42) 1.50(4) yes
C(41) C(43) 1.55(4) yes
C(41) C(44) 1.54(4) yes
C(42) H(40) 0.95(5) no
C(42) H(41) 0.95(4) no
C(42) H(42) 0.95(5) no
C(43) H(43) 0.95(4) no
C(43) H(44) 0.95(4) no
C(43) H(45) 0.95(4) no
C(44) H(46) 0.95(4) no
C(44) H(47) 0.95(4) no
C(44) H(48) 0.95(4) no
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_publ_flag
_geom_contact_site_symmetry_2
Ru(1) N(1) 3.18(2) yes 1_555
Ru(1) N(2) 3.15(2) yes 1_555
Ru(1) N(3) 3.15(2) yes 1_555
Ru(1) N(4) 3.13(2) yes 2_655
Ru(1) N(9) 2.09(2) yes 1_555
Ru(1) N(10) 2.09(2) yes 1_555
Ru(1) C(1) 2.05(2) yes 1_555
Ru(1) C(9) 3.10(2) yes 1_555
Ru(1) C(13) 2.94(2) yes 1_555
Ru(1) C(14) 2.97(2) yes 1_555
Ru(1) C(18) 3.09(2) yes 1_555
Ru(1) H(1) 3.18(2) no 1_555
Ru(1) H(6) 3.16(2) no 1_555
Ru(2) N(5) 3.12(2) yes 2_655
Ru(2) N(6) 3.15(2) yes 1_555
Ru(2) N(7) 3.17(2) yes 1_555
Ru(2) N(8) 3.21(2) yes 1_555
Ru(2) N(11) 2.12(2) yes 1_555
Ru(2) N(12) 2.10(2) yes 1_555
Ru(2) C(7) 2.03(2) yes 1_555
Ru(2) C(8) 2.07(2) yes 1_555
Ru(2) C(27) 3.12(2) yes 1_555
Ru(2) C(31) 2.98(2) yes 1_555
Ru(2) C(32) 2.98(2) yes 1_555
Ru(2) C(36) 3.07(2) yes 1_555
Ru(2) H(25) 3.19(2) no 1_555
Ru(2) H(30) 3.12(2) no 1_555
K(1) O(5) 2.81(2) yes 1_555
K(1) O(6) 2.99(2) yes 1_555
K(1) N(1) 3.45(2) yes 1_555
K(1) N(3) 3.25(2) yes 1_555
K(1) N(4) 3.28(2) yes 2_655
K(1) N(5) 3.33(2) yes 2_655
K(1) N(6) 3.27(2) yes 1_555
K(1) N(7) 3.27(2) yes 1_555
K(1) C(1) 3.37(2) yes 1_555
K(1) C(3) 3.22(3) yes 1_555
K(1) C(4) 3.24(2) yes 1_555
K(1) C(5) 3.27(2) yes 1_555
K(1) C(6) 3.22(2) yes 1_555
K(1) C(7) 3.17(2) yes 1_555
K(1) K(1) 8.741(9) yes 2_655
Eu(1) Eu(1) 7.206(1) yes 2_655
Eu(1) Ru(1) 5.584(2) yes .
Eu(1) Ru(2) 5.593(2) yes .
Eu(1) K(1) 4.753(6) yes .
Ru(1) Ru(2) 7.386(2) yes .
Ru(1) K(1) 4.029(7) yes .
Ru(2) K(1) 3.962(6) yes .
|
1501650.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/16/1501650.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_1501650
loop_
_publ_author_name
'Vaiyapuri, Rajendran'
'Greenland, Barnaby W.'
'Elliott, Joanne M.'
'Hayes, Wayne'
'Bennett, Roger A.'
'Cardin, Christine J.'
'Colquhoun, Howard M.'
'Etman, Haitham'
'Murray, Claire A.'
_publ_section_title
;
Pyrene-modified quartz crystal microbalance for the detection of
polynitroaromatic compounds.
;
_journal_issue 16
_journal_name_full 'Analytical chemistry'
_journal_page_first 6208
_journal_page_last 6214
_journal_paper_doi 10.1021/ac200755c
_journal_volume 83
_journal_year 2011
_chemical_formula_moiety 'C16 H10, C7 H3 N3 O4 '
_chemical_formula_sum 'C23 H13 N3 O4'
_chemical_formula_weight 395.37
_chemical_name_systematic '3,5-dinitrobenzonitrile and pyrene'
_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
_audit_creation_date 11-02-17
_audit_creation_method CRYSTALS_ver_14.06
_cell_angle_alpha 90
_cell_angle_beta 109.674(2)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 10.8636(2)
_cell_length_b 14.0746(2)
_cell_length_c 12.4274(3)
_cell_measurement_reflns_used 7398
_cell_measurement_temperature 150
_cell_measurement_theta_max 62.7
_cell_measurement_theta_min 4.69
_cell_volume 1789.23(6)
_computing_cell_refinement 'CrysAlis RED, (Oxford Diffraction, 2002)'
_computing_data_collection 'Gemini, (Oxford Diffraction, 2006)'
_computing_data_reduction 'CrysAlis RED'
_computing_molecular_graphics 'CAMERON (Watkin et al., 1996)'
_computing_publication_material CRYSTALS
_computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature 150
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device Area
_diffrn_measurement_device_type 'Oxford Diffraction Gemini'
_diffrn_measurement_method \w/2\q
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type 'Cu K\a'
_diffrn_radiation_wavelength 1.54180
_diffrn_reflns_av_R_equivalents 0.0209
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 14
_diffrn_reflns_limit_l_min -14
_diffrn_reflns_number 7398
_diffrn_reflns_theta_full 62.749
_diffrn_reflns_theta_max 62.749
_diffrn_reflns_theta_min 4.687
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 0.852
_exptl_absorpt_correction_T_max 0.959
_exptl_absorpt_correction_T_min 0.948
_exptl_absorpt_correction_type psi-scan
_exptl_absorpt_process_details '(North et al., 1968)'
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.468
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 816
_exptl_crystal_size_max 0.16
_exptl_crystal_size_mid 0.05
_exptl_crystal_size_min 0.05
_refine_diff_density_max 0.16
_refine_diff_density_min -0.25
_refine_ls_extinction_method None
_refine_ls_goodness_of_fit_ref 1.0322
_refine_ls_hydrogen_treatment none
_refine_ls_matrix_type full
_refine_ls_number_parameters 271
_refine_ls_number_reflns 2848
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0392
_refine_ls_R_factor_gt 0.0361
_refine_ls_shift/su_max 0.0005892
_refine_ls_shift/su_mean 0.0000534
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.10P)^2^ + 0.00P]
,where P=p(6)*max(Fo^2^,0) + (1-p(6))Fc^2^
;
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_all 0.1217
_refine_ls_wR_factor_gt 0.1157
_refine_ls_wR_factor_ref 0.1217
_reflns_limit_h_max 11
_reflns_limit_h_min -12
_reflns_limit_k_max 16
_reflns_limit_k_min 0
_reflns_limit_l_max 14
_reflns_limit_l_min 0
_reflns_number_gt 2574
_reflns_number_total 2863
_reflns_threshold_expression I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor 2.26
_oxford_diffrn_Wilson_scale 0.10
_oxford_refine_ls_r_factor_ref 0.0392
_oxford_refine_ls_scale 3.51(7)
_oxford_reflns_number_all 2848
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file ac200755c_si_001.cif
_cod_data_source_block global
_cod_original_cell_volume 1789.23(7)
_cod_original_sg_symbol_Hall '-P 2yn '
_cod_original_sg_symbol_H-M 'P 21/n '
_cod_database_code 1501650
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_type_symbol
_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
O1 O 1.01803(10) 0.83267(8) 0.37171(9) 0.0462 1.0000 Uani
N2 N 0.95825(10) 0.76352(8) 0.38764(9) 0.0354 1.0000 Uani
O3 O 0.98203(10) 0.68096(7) 0.37007(8) 0.0467 1.0000 Uani
C4 C 0.84882(12) 0.78062(9) 0.43033(9) 0.0299 1.0000 Uani
C5 C 0.78692(12) 0.70362(9) 0.45792(9) 0.0304 1.0000 Uani
C6 C 0.68513(11) 0.72257(9) 0.49765(9) 0.0290 1.0000 Uani
N7 N 0.61990(10) 0.64165(8) 0.53113(8) 0.0346 1.0000 Uani
O8 O 0.64910(10) 0.56142(6) 0.50967(8) 0.0437 1.0000 Uani
O9 O 0.54153(10) 0.65916(8) 0.57950(9) 0.0470 1.0000 Uani
C10 C 0.64296(12) 0.81368(9) 0.50856(9) 0.0304 1.0000 Uani
C11 C 0.70778(11) 0.88894(9) 0.47838(9) 0.0298 1.0000 Uani
C12 C 0.81269(12) 0.87336(9) 0.44035(9) 0.0304 1.0000 Uani
C13 C 0.66450(12) 0.98551(9) 0.48463(10) 0.0339 1.0000 Uani
N14 N 0.63099(12) 1.06243(8) 0.48683(10) 0.0444 1.0000 Uani
C15 C 0.47155(11) 0.63646(9) 0.24379(9) 0.0305 1.0000 Uani
C16 C 0.47030(11) 0.73715(9) 0.23214(9) 0.0268 1.0000 Uani
C17 C 0.56212(11) 0.78251(9) 0.19003(9) 0.0268 1.0000 Uani
C18 C 0.56112(11) 0.88327(9) 0.17786(10) 0.0319 1.0000 Uani
C19 C 0.46598(13) 0.93641(9) 0.20949(11) 0.0375 1.0000 Uani
C20 C 0.38028(13) 0.89369(10) 0.25079(10) 0.0381 1.0000 Uani
C21 C 0.37865(12) 0.79215(10) 0.26368(9) 0.0330 1.0000 Uani
C22 C 0.29028(12) 0.74595(11) 0.30610(10) 0.0407 1.0000 Uani
C23 C 0.29293(13) 0.64812(12) 0.31726(11) 0.0442 1.0000 Uani
C24 C 0.38233(13) 0.59384(10) 0.28707(10) 0.0383 1.0000 Uani
C25 C 0.65365(14) 0.92523(10) 0.13770(11) 0.0389 1.0000 Uani
C26 C 0.74542(13) 0.87133(10) 0.11036(11) 0.0405 1.0000 Uani
C27 C 0.74679(12) 0.77344(10) 0.12158(10) 0.0355 1.0000 Uani
C28 C 0.65645(11) 0.72773(9) 0.16092(9) 0.0285 1.0000 Uani
C29 C 0.65487(12) 0.62590(9) 0.17523(10) 0.0334 1.0000 Uani
C30 C 0.56787(13) 0.58312(9) 0.21407(10) 0.0346 1.0000 Uani
H51 H 0.8137 0.6398 0.4504 0.0300 1.0000 Uani
H101 H 0.5723 0.8240 0.5359 0.0303 1.0000 Uani
H121 H 0.8579 0.9253 0.4214 0.0321 1.0000 Uani
H191 H 0.4623 1.0040 0.2002 0.0395 1.0000 Uani
H201 H 0.3190 0.9324 0.2707 0.0423 1.0000 Uani
H221 H 0.2276 0.7815 0.3288 0.0421 1.0000 Uani
H231 H 0.2313 0.6175 0.3466 0.0466 1.0000 Uani
H241 H 0.3819 0.5258 0.2974 0.0406 1.0000 Uani
H251 H 0.6550 0.9922 0.1282 0.0410 1.0000 Uani
H261 H 0.8076 0.9011 0.0830 0.0405 1.0000 Uani
H271 H 0.8128 0.7373 0.1038 0.0366 1.0000 Uani
H291 H 0.7192 0.5873 0.1584 0.0350 1.0000 Uani
H301 H 0.5694 0.5159 0.2197 0.0348 1.0000 Uani
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 0.0404(5) 0.0516(6) 0.0538(6) 0.0071(5) 0.0252(5) 0.0047(5)
N2 0.0321(6) 0.0421(7) 0.0317(5) 0.0025(5) 0.0105(4) 0.0088(5)
O3 0.0448(6) 0.0462(6) 0.0531(6) -0.0031(4) 0.0217(5) 0.0149(5)
C4 0.0270(6) 0.0373(7) 0.0228(5) 0.0005(5) 0.0050(5) 0.0059(5)
C5 0.0306(6) 0.0312(6) 0.0241(6) -0.0003(5) 0.0023(5) 0.0051(5)
C6 0.0286(6) 0.0295(7) 0.0246(6) 0.0005(5) 0.0032(5) -0.0004(5)
N7 0.0302(5) 0.0362(7) 0.0319(5) 0.0010(4) 0.0032(4) -0.0024(5)
O8 0.0477(6) 0.0295(5) 0.0492(6) 0.0014(4) 0.0100(5) -0.0013(4)
O9 0.0438(6) 0.0477(6) 0.0557(6) -0.0011(4) 0.0249(5) -0.0082(5)
C10 0.0268(6) 0.0375(7) 0.0254(6) -0.0030(5) 0.0068(5) 0.0005(5)
C11 0.0297(6) 0.0316(7) 0.0263(6) -0.0024(5) 0.0070(5) 0.0013(5)
C12 0.0302(6) 0.0347(7) 0.0254(5) 0.0014(5) 0.0083(5) 0.0016(5)
C13 0.0349(6) 0.0348(8) 0.0364(6) -0.0026(5) 0.0180(5) -0.0017(6)
N14 0.0516(7) 0.0344(7) 0.0579(7) -0.0035(5) 0.0324(6) 0.0022(6)
C15 0.0300(7) 0.0341(7) 0.0228(6) 0.0004(5) 0.0029(5) -0.0044(5)
C16 0.0224(6) 0.0355(7) 0.0192(5) -0.0012(5) 0.0025(5) 0.0002(5)
C17 0.0255(6) 0.0292(7) 0.0215(5) -0.0022(4) 0.0020(5) -0.0009(5)
C18 0.0323(7) 0.0295(7) 0.0270(6) -0.0003(5) 0.0009(5) -0.0002(5)
C19 0.0406(7) 0.0284(7) 0.0364(6) -0.0016(5) 0.0036(6) 0.0076(6)
C20 0.0327(6) 0.0450(8) 0.0321(6) -0.0066(6) 0.0049(5) 0.0131(6)
C21 0.0272(6) 0.0449(8) 0.0228(6) -0.0032(5) 0.0032(5) 0.0055(6)
C22 0.0275(6) 0.0666(10) 0.0285(6) -0.0036(6) 0.0098(5) 0.0027(6)
C23 0.0332(7) 0.0675(10) 0.0326(7) 0.0033(6) 0.0120(6) -0.0111(7)
C24 0.0384(7) 0.0440(8) 0.0301(6) 0.0036(6) 0.0086(5) -0.0109(6)
C25 0.0436(7) 0.0301(7) 0.0381(7) 0.0023(5) 0.0074(6) -0.0086(6)
C26 0.0373(7) 0.0461(8) 0.0383(7) 0.0019(6) 0.0132(6) -0.0120(6)
C27 0.0299(6) 0.0439(8) 0.0330(6) -0.0037(6) 0.0109(5) -0.0030(6)
C28 0.0262(6) 0.0336(7) 0.0241(5) -0.0024(5) 0.0062(5) -0.0004(5)
C29 0.0342(7) 0.0321(7) 0.0335(6) -0.0035(5) 0.0107(5) 0.0050(6)
C30 0.0399(7) 0.0270(6) 0.0341(6) -0.0018(5) 0.0087(5) 0.0012(5)
H51 0.0300 0.0300 0.0300 0.0000 0.0101 0.0000
H101 0.0303 0.0303 0.0303 0.0000 0.0102 0.0000
H121 0.0321 0.0321 0.0321 0.0000 0.0108 0.0000
H191 0.0395 0.0395 0.0395 0.0000 0.0133 0.0000
H201 0.0423 0.0423 0.0423 0.0000 0.0142 0.0000
H221 0.0421 0.0421 0.0421 0.0000 0.0142 0.0000
H231 0.0466 0.0466 0.0466 0.0000 0.0157 0.0000
H241 0.0406 0.0406 0.0406 0.0000 0.0137 0.0000
H251 0.0410 0.0410 0.0410 0.0000 0.0138 0.0000
H261 0.0405 0.0405 0.0405 0.0000 0.0136 0.0000
H271 0.0366 0.0366 0.0366 0.0000 0.0123 0.0000
H291 0.0350 0.0350 0.0350 0.0000 0.0118 0.0000
H301 0.0348 0.0348 0.0348 0.0000 0.0117 0.0000
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 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0492 0.0322 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 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
O1 N2 O3 124.78(11) yes
O1 N2 C4 117.68(11) yes
O3 N2 C4 117.53(11) yes
N2 C4 C5 118.74(12) yes
N2 C4 C12 118.33(12) yes
C5 C4 C12 122.93(12) yes
C4 C5 C6 116.99(12) yes
C4 C5 H51 121.6 no
C6 C5 H51 121.4 no
C5 C6 N7 118.11(11) yes
C5 C6 C10 123.07(12) yes
N7 C6 C10 118.82(11) yes
C6 N7 O8 117.77(11) yes
C6 N7 O9 117.67(11) yes
O8 N7 O9 124.55(11) yes
C6 C10 C11 117.69(11) yes
C6 C10 H101 120.7 no
C11 C10 H101 121.6 no
C10 C11 C12 121.24(12) yes
C10 C11 C13 119.79(11) yes
C12 C11 C13 118.95(11) yes
C11 C12 C4 118.05(12) yes
C11 C12 H121 120.8 no
C4 C12 H121 121.1 no
C11 C13 N14 178.09(13) yes
C16 C15 C24 118.93(12) yes
C16 C15 C30 118.53(11) yes
C24 C15 C30 122.50(12) yes
C15 C16 C17 119.98(11) yes
C15 C16 C21 119.94(11) yes
C17 C16 C21 120.08(12) yes
C16 C17 C18 120.24(11) yes
C16 C17 C28 120.26(12) yes
C18 C17 C28 119.49(11) yes
C17 C18 C19 118.05(11) yes
C17 C18 C25 118.58(11) yes
C19 C18 C25 123.37(12) yes
C18 C19 C20 121.75(11) yes
C18 C19 H191 119.4 no
C20 C19 H191 118.9 no
C19 C20 C21 121.46(11) yes
C19 C20 H201 118.4 no
C21 C20 H201 120.1 no
C20 C21 C16 118.41(12) yes
C20 C21 C22 122.58(12) yes
C16 C21 C22 119.01(13) yes
C21 C22 C23 120.39(12) yes
C21 C22 H221 120.8 no
C23 C22 H221 118.8 no
C22 C23 C24 121.03(12) yes
C22 C23 H231 119.3 no
C24 C23 H231 119.7 no
C15 C24 C23 120.70(13) yes
C15 C24 H241 120.9 no
C23 C24 H241 118.4 no
C18 C25 C26 121.43(12) yes
C18 C25 H251 120.5 no
C26 C25 H251 118.1 no
C25 C26 C27 120.36(12) yes
C25 C26 H261 120.3 no
C27 C26 H261 119.4 no
C26 C27 C28 120.67(12) yes
C26 C27 H271 119.0 no
C28 C27 H271 120.3 no
C17 C28 C27 119.47(12) yes
C17 C28 C29 117.82(11) yes
C27 C28 C29 122.71(11) yes
C28 C29 C30 121.94(11) yes
C28 C29 H291 119.6 no
C30 C29 H291 118.5 no
C15 C30 C29 121.47(12) yes
C15 C30 H301 120.0 no
C29 C30 H301 118.5 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
O1 N2 1.2227(15) yes
N2 O3 1.2258(14) yes
N2 C4 1.4755(16) yes
C4 C5 1.378(2) yes
C4 C12 1.3807(18) yes
C5 C6 1.3803(18) yes
C5 H51 0.958 no
C6 N7 1.4734(16) yes
C6 C10 1.3837(17) yes
N7 O8 1.2263(14) yes
N7 O9 1.2212(15) yes
C10 C11 1.3916(18) yes
C10 H101 0.950 no
C11 C12 1.3904(18) yes
C11 C13 1.4487(18) yes
C12 H121 0.954 no
C13 N14 1.1455(17) yes
C15 C16 1.4242(18) yes
C15 C24 1.3927(18) yes
C15 C30 1.4335(18) yes
C16 C17 1.4240(17) yes
C16 C21 1.4168(17) yes
C17 C18 1.4259(18) yes
C17 C28 1.4230(17) yes
C18 C19 1.4337(18) yes
C18 C25 1.3950(19) yes
C19 C20 1.347(2) yes
C19 H191 0.958 no
C20 C21 1.4389(19) yes
C20 H201 0.955 no
C21 C22 1.401(2) yes
C22 C23 1.383(2) yes
C22 H221 0.961 no
C23 C24 1.383(2) yes
C23 H231 0.965 no
C24 H241 0.966 no
C25 C26 1.383(2) yes
C25 H251 0.951 no
C26 C27 1.384(2) yes
C26 H261 0.950 no
C27 C28 1.3926(18) yes
C27 H271 0.964 no
C28 C29 1.4450(18) yes
C29 C30 1.3401(19) yes
C29 H291 0.962 no
C30 H301 0.949 no
|
1501651.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/16/1501651.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_1501651
loop_
_publ_author_name
'Wu, Chunhui'
'Ye, Hongde'
'Bai, Wenjuan'
'Li, Qingning'
'Guo, Dadong'
'Lv, Gang'
'Yan, Hong'
'Wang, Xuemei'
_publ_section_title
;
New potential anticancer agent of carborane derivatives: selective
cellular interaction and activity of ferrocene-substituted
dithio-o-carborane conjugates.
;
_journal_issue 1
_journal_name_full 'Bioconjugate chemistry'
_journal_page_first 16
_journal_page_last 25
_journal_paper_doi 10.1021/bc100158b
_journal_volume 22
_journal_year 2011
_chemical_formula_moiety 'C15 H20 B10 Fe O S2'
_chemical_formula_sum 'C15 H20 B10 Fe O S2'
_chemical_formula_weight 444.38
_chemical_name_systematic
;
?
;
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 101.44(2)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 13.874(3)
_cell_length_b 20.663(2)
_cell_length_c 7.3166(15)
_cell_measurement_temperature 291(2)
_cell_volume 2055.8(7)
_computing_cell_refinement 'Bruker XSCANS'
_computing_data_collection 'Bruker XSCANS'
_computing_data_reduction 'Bruker SHELXTL'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 291(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type 'Bruker P4'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0757
_diffrn_reflns_av_sigmaI/netI 0.0753
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_h_min -17
_diffrn_reflns_limit_k_max 25
_diffrn_reflns_limit_k_min -25
_diffrn_reflns_limit_l_max 9
_diffrn_reflns_limit_l_min -9
_diffrn_reflns_number 18953
_diffrn_reflns_theta_full 26.00
_diffrn_reflns_theta_max 26.00
_diffrn_reflns_theta_min 3.01
_exptl_absorpt_coefficient_mu 0.941
_exptl_absorpt_correction_T_max 0.8056
_exptl_absorpt_correction_T_min 0.7655
_exptl_absorpt_correction_type multi-scan
_exptl_crystal_colour brown
_exptl_crystal_density_diffrn 1.436
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 904
_exptl_crystal_size_max 0.30
_exptl_crystal_size_mid 0.28
_exptl_crystal_size_min 0.24
_refine_diff_density_max 0.520
_refine_diff_density_min -0.389
_refine_diff_density_rms 0.078
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.082
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 263
_refine_ls_number_reflns 4018
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.082
_refine_ls_R_factor_all 0.0848
_refine_ls_R_factor_gt 0.0539
_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^)+(0.0551P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1139
_refine_ls_wR_factor_ref 0.1255
_reflns_number_gt 2670
_reflns_number_total 4018
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file bc100158b_si_002.cif
_cod_data_source_block FcSBCO
_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_values 1715 2011-07-08 13:25:40Z adriana
;
_cod_original_cell_volume 2055.8(6)
_cod_original_sg_symbol_H-M P2(1)/c
_cod_database_code 1501651
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
B3 B -0.1504(4) 0.3160(2) 0.2430(7) 0.0440(11) Uani 1 1 d .
H3 H -0.1289 0.2719 0.2385 0.053 Uiso 1 1 d R
B4 B -0.1824(4) 0.3617(3) 0.4247(6) 0.0446(12) Uani 1 1 d .
H4 H -0.1810 0.3330 0.5319 0.054 Uiso 1 1 d R
B5 B -0.1386(4) 0.4421(3) 0.4132(7) 0.0442(12) Uani 1 1 d .
H5 H -0.1051 0.4698 0.5412 0.053 Uiso 1 1 d R
B6 B -0.0772(4) 0.4479(2) 0.2216(7) 0.0413(11) Uani 1 1 d .
H6 H -0.0150 0.4758 0.2301 0.050 Uiso 1 1 d R
B7 B -0.2700(4) 0.3451(3) 0.2154(7) 0.0487(12) Uani 1 1 d .
H7 H -0.3320 0.3117 0.2094 0.058 Uiso 1 1 d R
B8 B -0.2637(4) 0.4232(3) 0.3231(7) 0.0494(12) Uani 1 1 d .
H8 H -0.3216 0.4407 0.3873 0.059 Uiso 1 1 d R
B9 B -0.1989(4) 0.4757(2) 0.1984(8) 0.0538(14) Uani 1 1 d .
H9 H -0.2143 0.5211 0.2061 0.065 Uiso 1 1 d R
B10 B -0.1636(4) 0.4317(3) 0.0166(7) 0.0465(12) Uani 1 1 d .
H10 H -0.1507 0.4473 -0.1152 0.056 Uiso 1 1 d R
B11 B -0.2067(3) 0.3510(3) 0.0251(7) 0.0444(11) Uani 1 1 d .
H11 H -0.2147 0.3199 -0.0911 0.11(2) Uiso 1 1 d R
B12 B -0.2795(4) 0.4170(3) 0.0774(7) 0.0497(12) Uani 1 1 d .
H12 H -0.3435 0.4264 -0.0158 0.060 Uiso 1 1 d R
C1 C -0.0760(3) 0.3773(2) 0.3522(5) 0.0370(8) Uani 1 1 d .
C2 C -0.0891(3) 0.3718(2) 0.1256(5) 0.0363(8) Uani 1 1 d .
C3 C 0.1231(3) 0.3613(2) 0.3664(6) 0.0455(11) Uani 1 1 d .
H3A H 0.1868 0.3685 0.4316 0.055 Uiso 1 1 calc R
C4 C 0.1142(3) 0.3575(2) 0.1816(6) 0.0383(9) Uani 1 1 d .
C5 C 0.2003(3) 0.35947(19) 0.0883(5) 0.0371(9) Uani 1 1 d .
C6 C 0.2885(3) 0.39590(19) 0.1699(5) 0.0340(8) Uani 1 1 d .
C7 C 0.3817(3) 0.3897(2) 0.1163(5) 0.0380(9) Uani 1 1 d .
H7A H 0.3982 0.3574 0.0294 0.046 Uiso 1 1 calc R
C8 C 0.4459(3) 0.4364(2) 0.2096(5) 0.0406(9) Uani 1 1 d .
H8A H 0.5147 0.4423 0.1994 0.049 Uiso 1 1 calc R
C9 C 0.3948(3) 0.4735(2) 0.3224(6) 0.0428(10) Uani 1 1 d .
H9A H 0.4220 0.5095 0.4037 0.051 Uiso 1 1 calc R
C10 C 0.2981(3) 0.4485(2) 0.3009(5) 0.0394(9) Uani 1 1 d .
H10A H 0.2464 0.4647 0.3628 0.047 Uiso 1 1 calc R
C11 C 0.3702(3) 0.2902(2) 0.5082(6) 0.0464(10) Uani 1 1 d .
H11A H 0.3164 0.2605 0.4581 0.056 Uiso 1 1 calc R
C12 C 0.4644(3) 0.2906(2) 0.4620(6) 0.0482(11) Uani 1 1 d .
H12A H 0.4873 0.2613 0.3742 0.058 Uiso 1 1 calc R
C13 C 0.5198(3) 0.3400(2) 0.5651(6) 0.0424(10) Uani 1 1 d .
H13A H 0.5880 0.3515 0.5622 0.051 Uiso 1 1 calc R
C14 C 0.4590(3) 0.3702(2) 0.6732(5) 0.0445(10) Uani 1 1 d .
H14A H 0.4778 0.4066 0.7587 0.053 Uiso 1 1 calc R
C15 C 0.3674(3) 0.3395(2) 0.6382(6) 0.0426(10) Uani 1 1 d .
H15A H 0.3112 0.3503 0.6952 0.051 Uiso 1 1 calc R
Fe1 Fe 0.39616(4) 0.37733(3) 0.39768(7) 0.03003(16) Uani 1 1 d .
O1 O 0.1935(2) 0.33097(17) -0.0606(4) 0.0546(8) Uani 1 1 d .
S1 S 0.03561(8) 0.35499(7) 0.50534(15) 0.0551(3) Uani 1 1 d .
S2 S 0.00584(7) 0.34109(5) 0.01648(14) 0.0427(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
B3 0.042(3) 0.036(2) 0.051(3) 0.003(2) 0.005(2) -0.007(2)
B4 0.040(3) 0.065(3) 0.030(2) 0.008(2) 0.009(2) -0.006(2)
B5 0.040(3) 0.058(3) 0.037(3) -0.011(2) 0.012(2) -0.005(2)
B6 0.044(3) 0.031(2) 0.048(3) -0.005(2) 0.010(2) -0.0074(19)
B7 0.037(3) 0.059(3) 0.051(3) -0.003(3) 0.011(2) -0.007(2)
B8 0.036(3) 0.068(4) 0.047(3) -0.006(3) 0.013(2) 0.003(2)
B9 0.064(4) 0.033(3) 0.065(3) 0.004(2) 0.014(3) 0.011(2)
B10 0.044(3) 0.060(3) 0.035(2) 0.010(2) 0.007(2) 0.005(2)
B11 0.032(2) 0.056(3) 0.045(3) -0.003(2) 0.007(2) -0.004(2)
B12 0.032(2) 0.071(4) 0.045(3) 0.004(3) 0.005(2) 0.012(2)
C1 0.037(2) 0.046(2) 0.0282(18) 0.0047(17) 0.0055(16) -0.0055(18)
C2 0.0301(19) 0.048(2) 0.0296(19) -0.0048(17) 0.0039(16) 0.0005(18)
C3 0.029(2) 0.066(3) 0.039(2) 0.008(2) 0.0020(18) -0.0037(18)
C4 0.029(2) 0.047(2) 0.039(2) -0.0014(18) 0.0063(17) 0.0037(16)
C5 0.0312(19) 0.044(2) 0.035(2) -0.0007(17) 0.0046(16) 0.0075(16)
C6 0.0299(19) 0.044(2) 0.0285(18) 0.0046(16) 0.0074(15) 0.0026(16)
C7 0.033(2) 0.055(3) 0.0266(18) 0.0039(17) 0.0073(16) 0.0028(17)
C8 0.035(2) 0.050(2) 0.037(2) 0.0140(18) 0.0079(18) 0.0012(18)
C9 0.042(2) 0.036(2) 0.050(2) 0.0070(18) 0.0074(19) -0.0036(17)
C10 0.042(2) 0.042(2) 0.034(2) 0.0032(16) 0.0090(18) 0.0107(17)
C11 0.053(3) 0.033(2) 0.048(2) 0.0106(19) -0.001(2) -0.0098(19)
C12 0.055(3) 0.044(2) 0.047(2) 0.009(2) 0.013(2) 0.014(2)
C13 0.031(2) 0.054(2) 0.038(2) 0.0125(19) -0.0034(17) 0.0004(18)
C14 0.050(2) 0.052(3) 0.028(2) 0.0051(18) -0.0010(18) -0.005(2)
C15 0.040(2) 0.052(3) 0.038(2) 0.0128(19) 0.0136(18) 0.0020(18)
Fe1 0.0307(3) 0.0341(3) 0.0250(3) 0.0014(2) 0.0049(2) 0.0003(2)
O1 0.0385(16) 0.077(2) 0.0481(18) -0.0225(16) 0.0084(14) 0.0055(15)
S1 0.0367(6) 0.0955(10) 0.0321(6) 0.0158(6) 0.0044(5) 0.0040(6)
S2 0.0323(5) 0.0524(6) 0.0423(6) -0.0270(5) 0.0048(4) 0.0035(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C1 B3 B7 105.6(4)
C1 B3 C2 56.0(2)
B7 B3 C2 105.0(3)
C1 B3 B4 58.2(3)
B7 B3 B4 61.5(3)
C2 B3 B4 103.7(3)
C1 B3 B11 103.4(3)
B7 B3 B11 61.1(3)
C2 B3 B11 57.7(2)
B4 B3 B11 109.1(4)
C1 B3 H3 123.4
B7 B3 H3 128.2
C2 B3 H3 115.0
B4 B3 H3 131.5
B11 B3 H3 115.9
C1 B4 B3 60.0(3)
C1 B4 B8 104.8(3)
B3 B4 B8 107.8(3)
C1 B4 B5 58.7(3)
B3 B4 B5 109.1(3)
B8 B4 B5 60.1(3)
C1 B4 B7 104.8(3)
B3 B4 B7 58.7(3)
B8 B4 B7 60.6(3)
B5 B4 B7 108.6(4)
C1 B4 H4 119.0
B3 B4 H4 108.2
B8 B4 H4 133.0
B5 B4 H4 130.6
B7 B4 H4 118.1
C1 B5 B9 104.6(3)
C1 B5 B8 104.0(3)
B9 B5 B8 60.0(3)
C1 B5 B4 58.2(3)
B9 B5 B4 107.6(4)
B8 B5 B4 59.5(3)
C1 B5 B6 59.9(2)
B9 B5 B6 59.4(3)
B8 B5 B6 107.9(3)
B4 B5 B6 108.7(3)
C1 B5 H5 118.2
B9 B5 H5 126.2
B8 B5 H5 129.7
B4 B5 H5 121.9
B6 B5 H5 116.2
C2 B6 C1 56.5(2)
C2 B6 B10 58.8(3)
C1 B6 B10 103.9(3)
C2 B6 B9 104.3(3)
C1 B6 B9 103.3(3)
B10 B6 B9 60.0(3)
C2 B6 B5 103.8(3)
C1 B6 B5 57.8(3)
B10 B6 B5 107.9(4)
B9 B6 B5 59.9(3)
C2 B6 H6 123.4
C1 B6 H6 121.3
B10 B6 H6 125.4
B9 B6 H6 126.8
B5 B6 H6 121.0
B3 B7 B12 108.4(4)
B3 B7 B4 59.8(3)
B12 B7 B4 106.6(4)
B3 B7 B8 107.4(4)
B12 B7 B8 59.4(3)
B4 B7 B8 59.0(3)
B3 B7 B11 60.7(3)
B12 B7 B11 59.8(3)
B4 B7 B11 107.3(3)
B8 B7 B11 107.0(4)
B3 B7 H7 120.7
B12 B7 H7 122.1
B4 B7 H7 123.3
B8 B7 H7 123.6
B11 B7 H7 120.9
B4 B8 B9 108.1(3)
B4 B8 B12 108.4(4)
B9 B8 B12 59.7(3)
B4 B8 B5 60.3(3)
B9 B8 B5 59.9(3)
B12 B8 B5 107.9(3)
B4 B8 B7 60.4(3)
B9 B8 B7 108.1(4)
B12 B8 B7 60.2(3)
B5 B8 B7 108.7(4)
B4 B8 H8 122.1
B9 B8 H8 121.4
B12 B8 H8 121.1
B5 B8 H8 121.8
B7 B8 H8 121.5
B10 B9 B6 59.9(3)
B10 B9 B12 60.6(3)
B6 B9 B12 108.9(4)
B10 B9 B5 108.4(4)
B6 B9 B5 60.7(3)
B12 B9 B5 108.5(4)
B10 B9 B8 108.6(4)
B6 B9 B8 109.0(4)
B12 B9 B8 60.2(3)
B5 B9 B8 60.1(3)
B10 B9 H9 130.1
B6 B9 H9 122.0
B12 B9 H9 124.9
B5 B9 H9 113.5
B8 B9 H9 115.0
C2 B10 B6 59.4(3)
C2 B10 B9 104.8(3)
B6 B10 B9 60.1(3)
C2 B10 B12 104.6(3)
B6 B10 B12 108.5(4)
B9 B10 B12 59.9(3)
C2 B10 B11 58.6(3)
B6 B10 B11 109.0(3)
B9 B10 B11 108.2(4)
B12 B10 B11 60.2(3)
C2 B10 H10 116.6
B6 B10 H10 120.5
B9 B10 H10 130.6
B12 B10 H10 126.9
B11 B10 H10 115.7
C2 B11 B10 58.6(3)
C2 B11 B12 104.4(3)
B10 B11 B12 59.9(3)
C2 B11 B3 60.3(3)
B10 B11 B3 108.7(3)
B12 B11 B3 106.5(4)
C2 B11 B7 104.8(3)
B10 B11 B7 108.1(4)
B12 B11 B7 60.0(3)
B3 B11 B7 58.2(3)
C2 B11 H11 116.2
B10 B11 H11 121.7
B12 B11 H11 131.7
B3 B11 H11 115.6
B7 B11 H11 126.6
B9 B12 B8 60.1(3)
B9 B12 B10 59.5(3)
B8 B12 B10 107.8(4)
B9 B12 B11 107.7(4)
B8 B12 B11 108.2(4)
B10 B12 B11 59.9(3)
B9 B12 B7 108.6(4)
B8 B12 B7 60.4(3)
B10 B12 B7 108.4(3)
B11 B12 B7 60.3(3)
B9 B12 H12 125.6
B8 B12 H12 125.3
B10 B12 H12 120.6
B11 B12 H12 117.1
B7 B12 H12 119.4
C2 C1 B4 112.0(3)
C2 C1 B5 111.1(3)
B4 C1 B5 63.1(3)
C2 C1 B3 62.9(3)
B4 C1 B3 61.8(3)
B5 C1 B3 114.2(3)
C2 C1 B6 61.0(2)
B4 C1 B6 114.7(3)
B5 C1 B6 62.3(3)
B3 C1 B6 114.9(3)
C2 C1 S1 121.8(3)
B4 C1 S1 117.1(3)
B5 C1 S1 117.6(3)
B3 C1 S1 117.7(3)
B6 C1 S1 118.3(3)
C1 C2 B10 111.0(3)
C1 C2 B11 111.0(3)
B10 C2 B11 62.8(3)
C1 C2 B6 62.6(3)
B10 C2 B6 61.8(3)
B11 C2 B6 114.5(3)
C1 C2 B3 61.1(2)
B10 C2 B3 113.5(3)
B11 C2 B3 62.0(3)
B6 C2 B3 114.8(3)
C1 C2 S2 122.3(3)
B10 C2 S2 118.7(3)
B11 C2 S2 116.4(3)
B6 C2 S2 119.2(3)
B3 C2 S2 117.2(3)
C4 C3 S1 130.9(3)
C4 C3 H3A 114.6
S1 C3 H3A 114.6
C3 C4 C5 122.8(4)
C3 C4 S2 126.8(3)
C5 C4 S2 110.1(3)
O1 C5 C6 121.5(4)
O1 C5 C4 117.8(4)
C6 C5 C4 120.7(3)
C7 C6 C10 106.4(3)
C7 C6 C5 124.9(3)
C10 C6 C5 128.5(3)
C7 C6 Fe1 69.6(2)
C10 C6 Fe1 69.0(2)
C5 C6 Fe1 130.9(3)
C8 C7 C6 109.1(4)
C8 C7 Fe1 70.6(2)
C6 C7 Fe1 69.4(2)
C8 C7 H7A 125.4
C6 C7 H7A 125.4
Fe1 C7 H7A 125.4
C7 C8 C9 108.4(4)
C7 C8 Fe1 69.6(2)
C9 C8 Fe1 70.0(2)
C7 C8 H8A 125.8
C9 C8 H8A 125.8
Fe1 C8 H8A 125.8
C8 C9 C10 108.0(4)
C8 C9 Fe1 69.8(2)
C10 C9 Fe1 68.6(2)
C8 C9 H9A 126.0
C10 C9 H9A 126.0
Fe1 C9 H9A 126.0
C9 C10 C6 108.1(4)
C9 C10 Fe1 70.9(2)
C6 C10 Fe1 69.7(2)
C9 C10 H10A 125.9
C6 C10 H10A 125.9
Fe1 C10 H10A 125.9
C15 C11 C12 108.1(4)
C15 C11 Fe1 69.9(2)
C12 C11 Fe1 69.8(2)
C15 C11 H11A 126.0
C12 C11 H11A 126.0
Fe1 C11 H11A 126.0
C13 C12 C11 108.0(4)
C13 C12 Fe1 70.4(2)
C11 C12 Fe1 69.6(2)
C13 C12 H12A 126.0
C11 C12 H12A 126.0
Fe1 C12 H12A 126.0
C12 C13 C14 107.3(4)
C12 C13 Fe1 69.4(2)
C14 C13 Fe1 69.3(2)
C12 C13 H13A 126.3
C14 C13 H13A 126.3
Fe1 C13 H13A 126.3
C15 C14 C13 108.7(4)
C15 C14 Fe1 69.9(2)
C13 C14 Fe1 70.3(2)
C15 C14 H14A 125.7
C13 C14 H14A 125.7
Fe1 C14 H14A 125.7
C14 C15 C11 107.9(4)
C14 C15 Fe1 69.9(2)
C11 C15 Fe1 69.9(2)
C14 C15 H15A 126.0
C11 C15 H15A 126.0
Fe1 C15 H15A 126.0
C10 Fe1 C11 128.28(18)
C10 Fe1 C15 110.26(17)
C11 Fe1 C15 40.21(17)
C10 Fe1 C14 121.51(17)
C11 Fe1 C14 67.49(18)
C15 Fe1 C14 40.14(17)
C10 Fe1 C12 164.74(19)
C11 Fe1 C12 40.61(18)
C15 Fe1 C12 67.94(17)
C14 Fe1 C12 67.64(18)
C10 Fe1 C6 41.32(15)
C11 Fe1 C6 109.40(16)
C15 Fe1 C6 122.71(16)
C14 Fe1 C6 157.17(16)
C12 Fe1 C6 125.80(17)
C10 Fe1 C7 68.53(16)
C11 Fe1 C7 121.36(18)
C15 Fe1 C7 157.09(17)
C14 Fe1 C7 160.56(16)
C12 Fe1 C7 106.87(17)
C6 Fe1 C7 40.96(14)
C10 Fe1 C13 154.57(17)
C11 Fe1 C13 67.83(17)
C15 Fe1 C13 67.89(17)
C14 Fe1 C13 40.40(17)
C12 Fe1 C13 40.16(17)
C6 Fe1 C13 161.48(16)
C7 Fe1 C13 123.48(16)
C10 Fe1 C8 68.17(16)
C11 Fe1 C8 154.09(18)
C15 Fe1 C8 162.72(17)
C14 Fe1 C8 124.80(17)
C12 Fe1 C8 118.28(17)
C6 Fe1 C8 68.32(15)
C7 Fe1 C8 39.79(16)
C13 Fe1 C8 105.72(16)
C10 Fe1 C9 40.49(16)
C11 Fe1 C9 165.08(18)
C15 Fe1 C9 127.46(18)
C14 Fe1 C9 108.30(18)
C12 Fe1 C9 152.72(17)
C6 Fe1 C9 68.54(16)
C7 Fe1 C9 67.48(17)
C13 Fe1 C9 119.00(17)
C8 Fe1 C9 40.20(16)
C3 S1 C1 103.51(19)
C4 S2 C2 103.28(18)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
B3 C1 1.727(6)
B3 B7 1.739(7)
B3 C2 1.755(6)
B3 B4 1.758(7)
B3 B11 1.784(7)
B3 H3 0.9603
B4 C1 1.695(6)
B4 B8 1.763(7)
B4 B5 1.777(7)
B4 B7 1.789(7)
B4 H4 0.9800
B5 C1 1.703(7)
B5 B9 1.769(8)
B5 B8 1.773(7)
B5 B6 1.783(7)
B5 H5 1.1166
B6 C2 1.716(6)
B6 C1 1.741(6)
B6 B10 1.756(7)
B6 B9 1.760(7)
B6 H6 1.0292
B7 B12 1.786(8)
B7 B8 1.792(8)
B7 B11 1.792(7)
B7 H7 1.0977
B8 B9 1.772(8)
B8 B12 1.773(7)
B8 H8 1.0705
B9 B10 1.758(8)
B9 B12 1.764(8)
B9 H9 0.9678
B10 C2 1.706(6)
B10 B12 1.778(7)
B10 B11 1.778(7)
B10 H10 1.0653
B11 C2 1.706(6)
B11 B12 1.783(7)
B11 H11 1.0530
B12 H12 1.0245
C1 C2 1.636(5)
C1 S1 1.783(4)
C2 S2 1.787(4)
C3 C4 1.335(6)
C3 S1 1.736(4)
C3 H3A 0.9300
C4 C5 1.489(5)
C4 S2 1.765(4)
C5 O1 1.225(5)
C5 C6 1.460(6)
C6 C7 1.430(5)
C6 C10 1.437(5)
C6 Fe1 2.042(4)
C7 C8 1.396(6)
C7 Fe1 2.044(4)
C7 H7A 0.9800
C8 C9 1.416(6)
C8 Fe1 2.058(4)
C8 H8A 0.9800
C9 C10 1.417(6)
C9 Fe1 2.062(4)
C9 H9A 0.9800
C10 Fe1 2.032(4)
C10 H10A 0.9800
C11 C15 1.399(6)
C11 C12 1.413(6)
C11 Fe1 2.035(4)
C11 H11A 0.9800
C12 C13 1.404(6)
C12 Fe1 2.038(4)
C12 H12A 0.9800
C13 C14 1.412(6)
C13 Fe1 2.051(4)
C13 H13A 0.9800
C14 C15 1.398(6)
C14 Fe1 2.037(4)
C14 H14A 0.9800
C15 Fe1 2.036(4)
C15 H15A 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
B7 B3 B4 C1 -134.1(4)
C2 B3 B4 C1 -34.2(3)
B11 B3 B4 C1 -94.3(3)
C1 B3 B4 B8 97.1(4)
B7 B3 B4 B8 -37.0(3)
C2 B3 B4 B8 62.9(4)
B11 B3 B4 B8 2.8(4)
C1 B3 B4 B5 33.4(3)
B7 B3 B4 B5 -100.7(4)
C2 B3 B4 B5 -0.8(4)
B11 B3 B4 B5 -60.9(4)
C1 B3 B4 B7 134.1(4)
C2 B3 B4 B7 99.9(4)
B11 B3 B4 B7 39.8(3)
B3 B4 B5 C1 -33.9(3)
B8 B4 B5 C1 -133.9(3)
B7 B4 B5 C1 -96.3(3)
C1 B4 B5 B9 96.5(4)
B3 B4 B5 B9 62.6(4)
B8 B4 B5 B9 -37.4(3)
B7 B4 B5 B9 0.2(5)
C1 B4 B5 B8 133.9(3)
B3 B4 B5 B8 100.0(4)
B7 B4 B5 B8 37.6(3)
C1 B4 B5 B6 33.7(3)
B3 B4 B5 B6 -0.2(5)
B8 B4 B5 B6 -100.2(4)
B7 B4 B5 B6 -62.6(4)
C1 B5 B6 C2 34.2(3)
B9 B5 B6 C2 -98.7(4)
B8 B5 B6 C2 -61.9(4)
B4 B5 B6 C2 1.2(4)
B9 B5 B6 C1 -132.9(4)
B8 B5 B6 C1 -96.1(4)
B4 B5 B6 C1 -33.0(3)
C1 B5 B6 B10 95.5(3)
B9 B5 B6 B10 -37.4(4)
B8 B5 B6 B10 -0.6(5)
B4 B5 B6 B10 62.4(4)
C1 B5 B6 B9 132.9(4)
B8 B5 B6 B9 36.8(4)
B4 B5 B6 B9 99.8(4)
C1 B3 B7 B12 59.6(4)
C2 B3 B7 B12 1.3(5)
B4 B3 B7 B12 98.9(4)
B11 B3 B7 B12 -37.4(3)
C1 B3 B7 B4 -39.3(3)
C2 B3 B7 B4 -97.6(3)
B11 B3 B7 B4 -136.3(4)
C1 B3 B7 B8 -3.1(4)
C2 B3 B7 B8 -61.4(4)
B4 B3 B7 B8 36.2(3)
B11 B3 B7 B8 -100.1(4)
C1 B3 B7 B11 97.0(4)
C2 B3 B7 B11 38.7(3)
B4 B3 B7 B11 136.3(4)
C1 B4 B7 B3 40.0(3)
B8 B4 B7 B3 138.9(4)
B5 B4 B7 B3 101.5(4)
C1 B4 B7 B12 -61.9(4)
B3 B4 B7 B12 -101.9(4)
B8 B4 B7 B12 37.0(3)
B5 B4 B7 B12 -0.5(4)
C1 B4 B7 B8 -98.9(4)
B3 B4 B7 B8 -138.9(4)
B5 B4 B7 B8 -37.4(3)
C1 B4 B7 B11 0.9(5)
B3 B4 B7 B11 -39.1(3)
B8 B4 B7 B11 99.8(4)
B5 B4 B7 B11 62.3(4)
C1 B4 B8 B9 -2.1(5)
B3 B4 B8 B9 -64.8(4)
B5 B4 B8 B9 37.4(3)
B7 B4 B8 B9 -100.9(4)
C1 B4 B8 B12 61.1(4)
B3 B4 B8 B12 -1.6(5)
B5 B4 B8 B12 100.6(4)
B7 B4 B8 B12 -37.7(3)
C1 B4 B8 B5 -39.5(3)
B3 B4 B8 B5 -102.2(3)
B7 B4 B8 B5 -138.4(3)
C1 B4 B8 B7 98.8(3)
B3 B4 B8 B7 36.1(3)
B5 B4 B8 B7 138.4(3)
C1 B5 B8 B4 39.1(3)
B9 B5 B8 B4 138.1(4)
B6 B5 B8 B4 101.6(4)
C1 B5 B8 B9 -98.9(3)
B4 B5 B8 B9 -138.1(4)
B6 B5 B8 B9 -36.5(3)
C1 B5 B8 B12 -62.2(4)
B9 B5 B8 B12 36.7(4)
B4 B5 B8 B12 -101.3(4)
B6 B5 B8 B12 0.2(5)
C1 B5 B8 B7 1.5(4)
B9 B5 B8 B7 100.5(4)
B4 B5 B8 B7 -37.6(3)
B6 B5 B8 B7 64.0(5)
B3 B7 B8 B4 -36.5(3)
B12 B7 B8 B4 -138.0(3)
B11 B7 B8 B4 -100.3(4)
B3 B7 B8 B9 64.5(5)
B12 B7 B8 B9 -37.0(3)
B4 B7 B8 B9 101.0(4)
B11 B7 B8 B9 0.6(5)
B3 B7 B8 B12 101.4(4)
B4 B7 B8 B12 138.0(3)
B11 B7 B8 B12 37.6(3)
B3 B7 B8 B5 1.0(5)
B12 B7 B8 B5 -100.4(4)
B4 B7 B8 B5 37.6(3)
B11 B7 B8 B5 -62.8(5)
C2 B6 B9 B10 -40.2(3)
C1 B6 B9 B10 -98.5(3)
B5 B6 B9 B10 -138.1(4)
C2 B6 B9 B12 -3.2(5)
C1 B6 B9 B12 -61.5(4)
B10 B6 B9 B12 37.0(4)
B5 B6 B9 B12 -101.1(4)
C2 B6 B9 B5 97.9(4)
C1 B6 B9 B5 39.6(3)
B10 B6 B9 B5 138.1(4)
C2 B6 B9 B8 60.8(4)
C1 B6 B9 B8 2.5(5)
B10 B6 B9 B8 101.0(4)
B5 B6 B9 B8 -37.1(3)
C1 B5 B9 B10 -3.4(5)
B8 B5 B9 B10 -101.4(4)
B4 B5 B9 B10 -64.2(5)
B6 B5 B9 B10 37.5(3)
C1 B5 B9 B6 -40.9(3)
B8 B5 B9 B6 -138.9(4)
B4 B5 B9 B6 -101.7(4)
C1 B5 B9 B12 60.9(4)
B8 B5 B9 B12 -37.1(3)
B4 B5 B9 B12 0.1(5)
B6 B5 B9 B12 101.8(4)
C1 B5 B9 B8 97.9(4)
B4 B5 B9 B8 37.2(3)
B6 B5 B9 B8 138.9(4)
B4 B8 B9 B10 63.3(5)
B12 B8 B9 B10 -37.8(4)
B5 B8 B9 B10 101.0(4)
B7 B8 B9 B10 -0.6(5)
B4 B8 B9 B6 -0.3(5)
B12 B8 B9 B6 -101.4(4)
B5 B8 B9 B6 37.3(3)
B7 B8 B9 B6 -64.2(5)
B4 B8 B9 B12 101.1(4)
B5 B8 B9 B12 138.8(4)
B7 B8 B9 B12 37.2(3)
B4 B8 B9 B5 -37.7(3)
B12 B8 B9 B5 -138.8(4)
B7 B8 B9 B5 -101.6(4)
C1 B6 B10 C2 -35.4(3)
B9 B6 B10 C2 -133.0(4)
B5 B6 B10 C2 -95.6(3)
C2 B6 B10 B9 133.0(4)
C1 B6 B10 B9 97.5(4)
B5 B6 B10 B9 37.4(3)
C2 B6 B10 B12 96.4(4)
C1 B6 B10 B12 61.0(4)
B9 B6 B10 B12 -36.6(4)
B5 B6 B10 B12 0.8(5)
C2 B6 B10 B11 32.4(3)
C1 B6 B10 B11 -3.0(4)
B9 B6 B10 B11 -100.5(4)
B5 B6 B10 B11 -63.2(4)
B6 B9 B10 C2 40.6(3)
B12 B9 B10 C2 -98.5(4)
B5 B9 B10 C2 2.8(5)
B8 B9 B10 C2 -61.0(4)
B12 B9 B10 B6 -139.2(4)
B5 B9 B10 B6 -37.9(4)
B8 B9 B10 B6 -101.6(4)
B6 B9 B10 B12 139.2(4)
B5 B9 B10 B12 101.3(4)
B8 B9 B10 B12 37.6(4)
B6 B9 B10 B11 101.9(4)
B12 B9 B10 B11 -37.3(3)
B5 B9 B10 B11 64.1(5)
B8 B9 B10 B11 0.3(5)
B6 B10 B11 C2 -32.7(3)
B9 B10 B11 C2 -96.5(4)
B12 B10 B11 C2 -133.7(4)
C2 B10 B11 B12 133.7(4)
B6 B10 B11 B12 100.9(4)
B9 B10 B11 B12 37.1(3)
C2 B10 B11 B3 35.0(3)
B6 B10 B11 B3 2.2(5)
B9 B10 B11 B3 -61.6(4)
B12 B10 B11 B3 -98.7(4)
C2 B10 B11 B7 96.6(4)
B6 B10 B11 B7 63.9(4)
B9 B10 B11 B7 0.1(5)
B12 B10 B11 B7 -37.0(3)
C1 B3 B11 C2 33.8(3)
B7 B3 B11 C2 134.4(4)
B4 B3 B11 C2 94.4(3)
C1 B3 B11 B10 -0.5(4)
B7 B3 B11 B10 100.1(4)
C2 B3 B11 B10 -34.3(3)
B4 B3 B11 B10 60.1(4)
C1 B3 B11 B12 -63.6(4)
B7 B3 B11 B12 37.0(3)
C2 B3 B11 B12 -97.4(4)
B4 B3 B11 B12 -3.0(4)
C1 B3 B11 B7 -100.6(4)
C2 B3 B11 B7 -134.4(4)
B4 B3 B11 B7 -40.0(3)
B3 B7 B11 C2 -39.9(3)
B12 B7 B11 C2 98.2(4)
B4 B7 B11 C2 -1.2(5)
B8 B7 B11 C2 60.8(4)
B3 B7 B11 B10 -101.2(4)
B12 B7 B11 B10 37.0(3)
B4 B7 B11 B10 -62.5(5)
B8 B7 B11 B10 -0.5(5)
B3 B7 B11 B12 -138.2(4)
B4 B7 B11 B12 -99.5(4)
B8 B7 B11 B12 -37.4(3)
B12 B7 B11 B3 138.2(4)
B4 B7 B11 B3 38.7(3)
B8 B7 B11 B3 100.7(4)
B10 B9 B12 B8 138.2(4)
B6 B9 B12 B8 101.5(4)
B5 B9 B12 B8 37.1(3)
B6 B9 B12 B10 -36.7(3)
B5 B9 B12 B10 -101.2(4)
B8 B9 B12 B10 -138.2(4)
B10 B9 B12 B11 37.0(3)
B6 B9 B12 B11 0.3(5)
B5 B9 B12 B11 -64.2(5)
B8 B9 B12 B11 -101.2(4)
B10 B9 B12 B7 100.8(4)
B6 B9 B12 B7 64.1(5)
B5 B9 B12 B7 -0.4(5)
B8 B9 B12 B7 -37.4(3)
B4 B8 B12 B9 -100.7(4)
B5 B8 B12 B9 -36.8(4)
B7 B8 B12 B9 -138.5(4)
B4 B8 B12 B10 -63.6(5)
B9 B8 B12 B10 37.1(4)
B5 B8 B12 B10 0.2(5)
B7 B8 B12 B10 -101.5(4)
B4 B8 B12 B11 -0.3(5)
B9 B8 B12 B11 100.4(4)
B5 B8 B12 B11 63.6(5)
B7 B8 B12 B11 -38.1(3)
B4 B8 B12 B7 37.9(3)
B9 B8 B12 B7 138.5(4)
B5 B8 B12 B7 101.7(4)
C2 B10 B12 B9 98.8(4)
B6 B10 B12 B9 36.7(3)
B11 B10 B12 B9 138.5(4)
C2 B10 B12 B8 61.5(5)
B6 B10 B12 B8 -0.6(5)
B9 B10 B12 B8 -37.3(4)
B11 B10 B12 B8 101.1(4)
C2 B10 B12 B11 -39.7(3)
B6 B10 B12 B11 -101.8(4)
B9 B10 B12 B11 -138.5(4)
C2 B10 B12 B7 -2.4(5)
B6 B10 B12 B7 -64.6(5)
B9 B10 B12 B7 -101.3(4)
B11 B10 B12 B7 37.2(4)
C2 B11 B12 B9 2.7(5)
B10 B11 B12 B9 -36.9(3)
B3 B11 B12 B9 65.5(4)
B7 B11 B12 B9 101.8(4)
C2 B11 B12 B8 -60.8(4)
B10 B11 B12 B8 -100.4(4)
B3 B11 B12 B8 2.0(5)
B7 B11 B12 B8 38.2(3)
C2 B11 B12 B10 39.6(3)
B3 B11 B12 B10 102.4(4)
B7 B11 B12 B10 138.6(4)
C2 B11 B12 B7 -99.0(4)
B10 B11 B12 B7 -138.6(4)
B3 B11 B12 B7 -36.2(3)
B3 B7 B12 B9 -62.4(5)
B4 B7 B12 B9 0.5(5)
B8 B7 B12 B9 37.3(3)
B11 B7 B12 B9 -100.2(4)
B3 B7 B12 B8 -99.7(4)
B4 B7 B12 B8 -36.8(3)
B11 B7 B12 B8 -137.5(4)
B3 B7 B12 B10 0.7(5)
B4 B7 B12 B10 63.7(5)
B8 B7 B12 B10 100.4(4)
B11 B7 B12 B10 -37.1(3)
B3 B7 B12 B11 37.8(3)
B4 B7 B12 B11 100.7(4)
B8 B7 B12 B11 137.5(4)
B3 B4 C1 C2 39.2(3)
B8 B4 C1 C2 -63.1(4)
B5 B4 C1 C2 -103.3(4)
B7 B4 C1 C2 -0.2(5)
B3 B4 C1 B5 142.5(3)
B8 B4 C1 B5 40.2(3)
B7 B4 C1 B5 103.1(4)
B8 B4 C1 B3 -102.3(4)
B5 B4 C1 B3 -142.5(3)
B7 B4 C1 B3 -39.4(3)
B3 B4 C1 B6 106.2(4)
B8 B4 C1 B6 4.0(4)
B5 B4 C1 B6 -36.3(3)
B7 B4 C1 B6 66.8(4)
B3 B4 C1 S1 -108.6(3)
B8 B4 C1 S1 149.1(3)
B5 B4 C1 S1 108.9(3)
B7 B4 C1 S1 -148.0(3)
B9 B5 C1 C2 2.8(4)
B8 B5 C1 C2 65.0(4)
B4 B5 C1 C2 104.8(3)
B6 B5 C1 C2 -37.8(3)
B9 B5 C1 B4 -101.9(4)
B8 B5 C1 B4 -39.8(3)
B6 B5 C1 B4 -142.6(3)
B9 B5 C1 B3 -65.9(4)
B8 B5 C1 B3 -3.7(4)
B4 B5 C1 B3 36.0(3)
B6 B5 C1 B3 -106.6(4)
B9 B5 C1 B6 40.7(3)
B8 B5 C1 B6 102.8(4)
B4 B5 C1 B6 142.6(3)
B9 B5 C1 S1 149.9(3)
B8 B5 C1 S1 -147.9(3)
B4 B5 C1 S1 -108.2(3)
B6 B5 C1 S1 109.2(3)
B7 B3 C1 C2 -97.9(4)
B4 B3 C1 C2 -138.8(3)
B11 B3 C1 C2 -34.5(3)
B7 B3 C1 B4 41.0(3)
C2 B3 C1 B4 138.8(3)
B11 B3 C1 B4 104.3(4)
B7 B3 C1 B5 4.5(5)
C2 B3 C1 B5 102.3(4)
B4 B3 C1 B5 -36.5(3)
B11 B3 C1 B5 67.8(4)
B7 B3 C1 B6 -64.9(4)
C2 B3 C1 B6 33.0(3)
B4 B3 C1 B6 -105.9(4)
B11 B3 C1 B6 -1.6(5)
B7 B3 C1 S1 148.6(3)
C2 B3 C1 S1 -113.5(3)
B4 B3 C1 S1 107.6(3)
B11 B3 C1 S1 -148.1(3)
B10 B6 C1 C2 36.5(3)
B9 B6 C1 C2 98.4(3)
B5 B6 C1 C2 139.1(3)
C2 B6 C1 B4 -102.6(3)
B10 B6 C1 B4 -66.0(4)
B9 B6 C1 B4 -4.1(4)
B5 B6 C1 B4 36.6(3)
C2 B6 C1 B5 -139.1(3)
B10 B6 C1 B5 -102.6(4)
B9 B6 C1 B5 -40.7(3)
C2 B6 C1 B3 -33.6(3)
B10 B6 C1 B3 2.9(4)
B9 B6 C1 B3 64.8(4)
B5 B6 C1 B3 105.5(4)
C2 B6 C1 S1 112.7(3)
B10 B6 C1 S1 149.2(3)
B9 B6 C1 S1 -148.9(3)
B5 B6 C1 S1 -108.2(3)
B4 C1 C2 B10 67.3(4)
B5 C1 C2 B10 -1.2(4)
B3 C1 C2 B10 106.0(4)
B6 C1 C2 B10 -39.6(3)
S1 C1 C2 B10 -146.7(3)
B4 C1 C2 B11 -0.6(5)
B5 C1 C2 B11 -69.1(4)
B3 C1 C2 B11 38.1(3)
B6 C1 C2 B11 -107.5(4)
S1 C1 C2 B11 145.5(3)
B4 C1 C2 B6 106.9(4)
B5 C1 C2 B6 38.4(3)
B3 C1 C2 B6 145.6(3)
S1 C1 C2 B6 -107.1(3)
B4 C1 C2 B3 -38.8(3)
B5 C1 C2 B3 -107.2(4)
B6 C1 C2 B3 -145.6(3)
S1 C1 C2 B3 107.3(4)
B4 C1 C2 S2 -144.3(3)
B5 C1 C2 S2 147.2(3)
B3 C1 C2 S2 -105.6(4)
B6 C1 C2 S2 108.8(3)
S1 C1 C2 S2 1.8(5)
B6 B10 C2 C1 39.9(3)
B9 B10 C2 C1 -1.1(4)
B12 B10 C2 C1 -63.2(4)
B11 B10 C2 C1 -103.6(3)
B6 B10 C2 B11 143.5(3)
B9 B10 C2 B11 102.6(4)
B12 B10 C2 B11 40.4(3)
B9 B10 C2 B6 -41.0(3)
B12 B10 C2 B6 -103.1(4)
B11 B10 C2 B6 -143.5(3)
B6 B10 C2 B3 106.5(4)
B9 B10 C2 B3 65.5(4)
B12 B10 C2 B3 3.4(5)
B11 B10 C2 B3 -37.0(3)
B6 B10 C2 S2 -109.7(3)
B9 B10 C2 S2 -150.7(3)
B12 B10 C2 S2 147.2(3)
B11 B10 C2 S2 106.7(3)
B10 B11 C2 C1 103.6(4)
B12 B11 C2 C1 63.3(4)
B3 B11 C2 C1 -37.8(3)
B7 B11 C2 C1 1.1(5)
B12 B11 C2 B10 -40.2(3)
B3 B11 C2 B10 -141.3(4)
B7 B11 C2 B10 -102.4(4)
B10 B11 C2 B6 35.1(3)
B12 B11 C2 B6 -5.1(5)
B3 B11 C2 B6 -106.2(4)
B7 B11 C2 B6 -67.3(4)
B10 B11 C2 B3 141.3(4)
B12 B11 C2 B3 101.1(4)
B7 B11 C2 B3 38.9(3)
B10 B11 C2 S2 -110.4(3)
B12 B11 C2 S2 -150.6(3)
B3 B11 C2 S2 108.3(3)
B7 B11 C2 S2 147.2(3)
B10 B6 C2 C1 -137.5(3)
B9 B6 C2 C1 -96.7(3)
B5 B6 C2 C1 -34.8(3)
C1 B6 C2 B10 137.5(3)
B9 B6 C2 B10 40.8(3)
B5 B6 C2 B10 102.8(4)
C1 B6 C2 B11 102.0(4)
B10 B6 C2 B11 -35.5(3)
B9 B6 C2 B11 5.3(5)
B5 B6 C2 B11 67.3(4)
C1 B6 C2 B3 33.0(3)
B10 B6 C2 B3 -104.5(4)
B9 B6 C2 B3 -63.7(4)
B5 B6 C2 B3 -1.8(4)
C1 B6 C2 S2 -113.5(3)
B10 B6 C2 S2 109.0(3)
B9 B6 C2 S2 149.8(3)
B5 B6 C2 S2 -148.3(3)
B7 B3 C2 C1 98.9(4)
B4 B3 C2 C1 35.1(3)
B11 B3 C2 C1 139.3(4)
C1 B3 C2 B10 -101.9(4)
B7 B3 C2 B10 -3.0(5)
B4 B3 C2 B10 -66.8(4)
B11 B3 C2 B10 37.3(4)
C1 B3 C2 B11 -139.3(4)
B7 B3 C2 B11 -40.4(3)
B4 B3 C2 B11 -104.1(4)
C1 B3 C2 B6 -33.5(3)
B7 B3 C2 B6 65.4(4)
B4 B3 C2 B6 1.6(4)
B11 B3 C2 B6 105.8(4)
C1 B3 C2 S2 113.7(3)
B7 B3 C2 S2 -147.4(3)
B4 B3 C2 S2 148.9(3)
B11 B3 C2 S2 -107.0(3)
S1 C3 C4 C5 -175.4(4)
S1 C3 C4 S2 -2.6(7)
C3 C4 C5 O1 151.1(4)
S2 C4 C5 O1 -22.7(5)
C3 C4 C5 C6 -30.6(6)
S2 C4 C5 C6 155.5(3)
O1 C5 C6 C7 -16.4(6)
C4 C5 C6 C7 165.4(4)
O1 C5 C6 C10 156.4(4)
C4 C5 C6 C10 -21.8(6)
O1 C5 C6 Fe1 -108.9(4)
C4 C5 C6 Fe1 73.0(5)
C10 C6 C7 C8 -0.2(4)
C5 C6 C7 C8 173.9(4)
Fe1 C6 C7 C8 -59.7(3)
C10 C6 C7 Fe1 59.5(3)
C5 C6 C7 Fe1 -126.4(4)
C6 C7 C8 C9 -0.6(4)
Fe1 C7 C8 C9 -59.5(3)
C6 C7 C8 Fe1 58.9(3)
C7 C8 C9 C10 1.1(4)
Fe1 C8 C9 C10 -58.1(3)
C7 C8 C9 Fe1 59.2(3)
C8 C9 C10 C6 -1.2(4)
Fe1 C9 C10 C6 -60.0(3)
C8 C9 C10 Fe1 58.8(3)
C7 C6 C10 C9 0.9(4)
C5 C6 C10 C9 -173.0(4)
Fe1 C6 C10 C9 60.8(3)
C7 C6 C10 Fe1 -59.9(3)
C5 C6 C10 Fe1 126.3(4)
C15 C11 C12 C13 0.5(5)
Fe1 C11 C12 C13 60.2(3)
C15 C11 C12 Fe1 -59.7(3)
C11 C12 C13 C14 -0.5(5)
Fe1 C12 C13 C14 59.1(3)
C11 C12 C13 Fe1 -59.7(3)
C12 C13 C14 C15 0.4(5)
Fe1 C13 C14 C15 59.6(3)
C12 C13 C14 Fe1 -59.2(3)
C13 C14 C15 C11 -0.1(5)
Fe1 C14 C15 C11 59.8(3)
C13 C14 C15 Fe1 -59.9(3)
C12 C11 C15 C14 -0.2(5)
Fe1 C11 C15 C14 -59.8(3)
C12 C11 C15 Fe1 59.6(3)
C9 C10 Fe1 C11 166.3(3)
C6 C10 Fe1 C11 -75.1(3)
C9 C10 Fe1 C15 124.5(3)
C6 C10 Fe1 C15 -116.9(2)
C9 C10 Fe1 C14 81.3(3)
C6 C10 Fe1 C14 -160.1(2)
C9 C10 Fe1 C12 -155.2(6)
C6 C10 Fe1 C12 -36.6(7)
C9 C10 Fe1 C6 -118.6(3)
C9 C10 Fe1 C7 -80.0(3)
C6 C10 Fe1 C7 38.6(2)
C9 C10 Fe1 C13 43.6(5)
C6 C10 Fe1 C13 162.2(3)
C9 C10 Fe1 C8 -37.1(2)
C6 C10 Fe1 C8 81.5(2)
C6 C10 Fe1 C9 118.6(3)
C15 C11 Fe1 C10 -75.5(3)
C12 C11 Fe1 C10 165.4(3)
C12 C11 Fe1 C15 -119.1(4)
C15 C11 Fe1 C14 37.7(3)
C12 C11 Fe1 C14 -81.4(3)
C15 C11 Fe1 C12 119.1(4)
C15 C11 Fe1 C6 -118.1(3)
C12 C11 Fe1 C6 122.8(3)
C15 C11 Fe1 C7 -161.8(2)
C12 C11 Fe1 C7 79.1(3)
C15 C11 Fe1 C13 81.5(3)
C12 C11 Fe1 C13 -37.6(3)
C15 C11 Fe1 C8 161.8(3)
C12 C11 Fe1 C8 42.7(5)
C15 C11 Fe1 C9 -38.7(8)
C12 C11 Fe1 C9 -157.8(6)
C14 C15 Fe1 C10 -115.2(3)
C11 C15 Fe1 C10 125.9(3)
C14 C15 Fe1 C11 118.9(4)
C11 C15 Fe1 C14 -118.9(4)
C14 C15 Fe1 C12 81.0(3)
C11 C15 Fe1 C12 -37.9(3)
C14 C15 Fe1 C6 -159.6(2)
C11 C15 Fe1 C6 81.5(3)
C14 C15 Fe1 C7 162.1(4)
C11 C15 Fe1 C7 43.3(5)
C14 C15 Fe1 C13 37.5(3)
C11 C15 Fe1 C13 -81.4(3)
C14 C15 Fe1 C8 -33.7(7)
C11 C15 Fe1 C8 -152.6(5)
C14 C15 Fe1 C9 -72.8(3)
C11 C15 Fe1 C9 168.3(2)
C15 C14 Fe1 C10 84.4(3)
C13 C14 Fe1 C10 -156.1(2)
C15 C14 Fe1 C11 -37.7(3)
C13 C14 Fe1 C11 81.8(3)
C13 C14 Fe1 C15 119.5(4)
C15 C14 Fe1 C12 -81.8(3)
C13 C14 Fe1 C12 37.7(2)
C15 C14 Fe1 C6 49.0(5)
C13 C14 Fe1 C6 168.5(4)
C15 C14 Fe1 C7 -159.0(5)
C13 C14 Fe1 C7 -39.5(6)
C15 C14 Fe1 C13 -119.5(4)
C15 C14 Fe1 C8 168.4(2)
C13 C14 Fe1 C8 -72.1(3)
C15 C14 Fe1 C9 127.0(3)
C13 C14 Fe1 C9 -113.5(3)
C13 C12 Fe1 C10 -167.6(6)
C11 C12 Fe1 C10 -48.8(7)
C13 C12 Fe1 C11 -118.9(4)
C13 C12 Fe1 C15 -81.4(3)
C11 C12 Fe1 C15 37.5(3)
C13 C12 Fe1 C14 -37.9(2)
C11 C12 Fe1 C14 81.0(3)
C13 C12 Fe1 C6 163.4(2)
C11 C12 Fe1 C6 -77.8(3)
C13 C12 Fe1 C7 122.3(3)
C11 C12 Fe1 C7 -118.8(3)
C11 C12 Fe1 C13 118.9(4)
C13 C12 Fe1 C8 80.8(3)
C11 C12 Fe1 C8 -160.3(3)
C13 C12 Fe1 C9 48.9(5)
C11 C12 Fe1 C9 167.8(4)
C7 C6 Fe1 C10 117.7(3)
C5 C6 Fe1 C10 -123.3(4)
C7 C6 Fe1 C11 -115.9(3)
C10 C6 Fe1 C11 126.5(3)
C5 C6 Fe1 C11 3.2(4)
C7 C6 Fe1 C15 -158.5(2)
C10 C6 Fe1 C15 83.9(3)
C5 C6 Fe1 C15 -39.4(4)
C7 C6 Fe1 C14 166.2(4)
C10 C6 Fe1 C14 48.5(5)
C5 C6 Fe1 C14 -74.7(6)
C7 C6 Fe1 C12 -73.4(3)
C10 C6 Fe1 C12 168.9(2)
C5 C6 Fe1 C12 45.6(4)
C10 C6 Fe1 C7 -117.7(3)
C5 C6 Fe1 C7 119.0(5)
C7 C6 Fe1 C13 -37.9(6)
C10 C6 Fe1 C13 -155.6(5)
C5 C6 Fe1 C13 81.1(6)
C7 C6 Fe1 C8 36.5(2)
C10 C6 Fe1 C8 -81.1(3)
C5 C6 Fe1 C8 155.6(4)
C7 C6 Fe1 C9 79.9(3)
C10 C6 Fe1 C9 -37.8(2)
C5 C6 Fe1 C9 -161.1(4)
C8 C7 Fe1 C10 81.2(3)
C6 C7 Fe1 C10 -38.9(2)
C8 C7 Fe1 C11 -156.1(2)
C6 C7 Fe1 C11 83.8(3)
C8 C7 Fe1 C15 172.7(4)
C6 C7 Fe1 C15 52.5(5)
C8 C7 Fe1 C14 -43.7(6)
C6 C7 Fe1 C14 -163.9(5)
C8 C7 Fe1 C12 -114.2(3)
C6 C7 Fe1 C12 125.7(3)
C8 C7 Fe1 C6 120.2(4)
C8 C7 Fe1 C13 -73.4(3)
C6 C7 Fe1 C13 166.5(2)
C6 C7 Fe1 C8 -120.2(4)
C8 C7 Fe1 C9 37.4(2)
C6 C7 Fe1 C9 -82.7(3)
C12 C13 Fe1 C10 172.5(3)
C14 C13 Fe1 C10 53.6(5)
C12 C13 Fe1 C11 38.0(3)
C14 C13 Fe1 C11 -80.8(3)
C12 C13 Fe1 C15 81.5(3)
C14 C13 Fe1 C15 -37.3(3)
C12 C13 Fe1 C14 118.8(4)
C14 C13 Fe1 C12 -118.8(4)
C12 C13 Fe1 C6 -47.0(6)
C14 C13 Fe1 C6 -165.8(4)
C12 C13 Fe1 C7 -75.9(3)
C14 C13 Fe1 C7 165.3(2)
C12 C13 Fe1 C8 -115.4(3)
C14 C13 Fe1 C8 125.7(3)
C12 C13 Fe1 C9 -156.8(3)
C14 C13 Fe1 C9 84.4(3)
C7 C8 Fe1 C10 -82.2(3)
C9 C8 Fe1 C10 37.3(2)
C7 C8 Fe1 C11 52.4(5)
C9 C8 Fe1 C11 172.0(4)
C7 C8 Fe1 C15 -170.4(5)
C9 C8 Fe1 C15 -50.9(6)
C7 C8 Fe1 C14 163.7(2)
C9 C8 Fe1 C14 -76.7(3)
C7 C8 Fe1 C12 82.5(3)
C9 C8 Fe1 C12 -158.0(2)
C7 C8 Fe1 C6 -37.6(2)
C9 C8 Fe1 C6 82.0(3)
C9 C8 Fe1 C7 119.6(3)
C7 C8 Fe1 C13 123.9(3)
C9 C8 Fe1 C13 -116.6(3)
C7 C8 Fe1 C9 -119.6(3)
C8 C9 Fe1 C10 -119.9(4)
C8 C9 Fe1 C11 -166.3(6)
C10 C9 Fe1 C11 -46.4(8)
C8 C9 Fe1 C15 163.1(2)
C10 C9 Fe1 C15 -77.0(3)
C8 C9 Fe1 C14 122.7(3)
C10 C9 Fe1 C14 -117.4(3)
C8 C9 Fe1 C12 46.1(5)
C10 C9 Fe1 C12 166.0(3)
C8 C9 Fe1 C6 -81.4(3)
C10 C9 Fe1 C6 38.5(2)
C8 C9 Fe1 C7 -37.1(2)
C10 C9 Fe1 C7 82.8(3)
C8 C9 Fe1 C13 79.9(3)
C10 C9 Fe1 C13 -160.2(2)
C10 C9 Fe1 C8 119.9(4)
C4 C3 S1 C1 -24.8(5)
C2 C1 S1 C3 22.8(4)
B4 C1 S1 C3 167.3(3)
B5 C1 S1 C3 -120.6(3)
B3 C1 S1 C3 96.5(3)
B6 C1 S1 C3 -48.8(3)
C3 C4 S2 C2 28.8(4)
C5 C4 S2 C2 -157.7(3)
C1 C2 S2 C4 -26.2(4)
B10 C2 S2 C4 119.9(3)
B11 C2 S2 C4 -168.1(3)
B6 C2 S2 C4 48.0(3)
B3 C2 S2 C4 -97.7(3)
|
1501652.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/16/1501652.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_1501652
loop_
_publ_author_name
'D'Souza, Christopher A'
'McBride, William J.'
'Sharkey, Robert M.'
'Todaro, Louis J.'
'Goldenberg, David M.'
_publ_section_title
;
High-yielding aqueous 18F-labeling of peptides via Al18F chelation.
;
_journal_issue 9
_journal_name_full 'Bioconjugate chemistry'
_journal_page_first 1793
_journal_page_last 1803
_journal_paper_doi 10.1021/bc200175c
_journal_volume 22
_journal_year 2011
_chemical_formula_sum 'C19 H27 Al F N3 O7'
_chemical_formula_weight 455.42
_chemical_name_systematic
;
?
;
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 107.52(3)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 20.463(4)
_cell_length_b 8.4950(17)
_cell_length_c 12.692(3)
_cell_measurement_reflns_used 4812
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 27.48
_cell_measurement_theta_min 2.93
_cell_volume 2103.9(8)
_computing_cell_refinement 'Bruker XSCANS'
_computing_data_collection 'Bruker XSCANS'
_computing_data_reduction 'Bruker SHELXTL'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type 'Bruker-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 0.0896
_diffrn_reflns_av_sigmaI/netI 0.0883
_diffrn_reflns_limit_h_max 26
_diffrn_reflns_limit_h_min -25
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -8
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_number 13148
_diffrn_reflns_theta_full 27.48
_diffrn_reflns_theta_max 27.48
_diffrn_reflns_theta_min 2.93
_exptl_absorpt_coefficient_mu 0.153
_exptl_absorpt_correction_T_max 0.9909
_exptl_absorpt_correction_T_min 0.9249
_exptl_absorpt_correction_type integration
_exptl_crystal_density_diffrn 1.438
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 960
_exptl_crystal_size_max 0.52
_exptl_crystal_size_mid 0.08
_exptl_crystal_size_min 0.06
_refine_diff_density_max 0.318
_refine_diff_density_min -0.388
_refine_diff_density_rms 0.076
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.023
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 281
_refine_ls_number_reflns 4812
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.023
_refine_ls_R_factor_all 0.1023
_refine_ls_R_factor_gt 0.0601
_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^)+(0.0438P)^2^+1.8452P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1181
_refine_ls_wR_factor_ref 0.1374
_reflns_number_gt 3241
_reflns_number_total 4812
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file bc200175c_si_002.cif
_cod_data_source_block x1703l
_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_values 1715 2011-07-08 13:25:40Z adriana
;
_cod_original_cell_volume 2103.9(7)
_cod_original_sg_symbol_H-M P2(1)/c
_cod_database_code 1501652
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
Al Al 0.19425(4) 0.26195(9) 0.54669(5) 0.01709(19) Uani 1 1 d .
F F 0.24155(7) 0.38580(17) 0.49165(11) 0.0220(3) Uani 1 1 d .
O11 O 0.17316(9) -0.1673(2) 0.43389(13) 0.0226(4) Uani 1 1 d .
O12 O 0.21021(8) 0.0776(2) 0.48014(12) 0.0185(4) Uani 1 1 d .
O13 O 0.03815(9) 0.5075(2) 0.37513(14) 0.0291(5) Uani 1 1 d .
O14 O 0.11183(9) 0.3114(2) 0.43837(13) 0.0198(4) Uani 1 1 d .
O22 O 0.66522(9) 0.2541(3) 0.90206(14) 0.0359(5) Uani 1 1 d .
O23 O 0.71008(9) 0.2332(2) 1.08582(13) 0.0253(4) Uani 1 1 d .
H23A H 0.7453 0.2693 1.0735 0.038 Uiso 1 1 calc R
N1 N 0.14259(10) 0.1106(3) 0.62232(15) 0.0179(5) Uani 1 1 d .
N4 N 0.16218(10) 0.4276(3) 0.63611(15) 0.0187(5) Uani 1 1 d .
N7 N 0.27554(10) 0.2322(3) 0.69029(15) 0.0193(5) Uani 1 1 d .
C2 C 0.08682(12) 0.2020(3) 0.64655(19) 0.0183(5) Uani 1 1 d .
H2A H 0.0682 0.1428 0.6983 0.022 Uiso 1 1 calc R
H2B H 0.0491 0.2208 0.5776 0.022 Uiso 1 1 calc R
C3 C 0.11675(13) 0.3587(3) 0.69804(19) 0.0193(6) Uani 1 1 d .
H3A H 0.0791 0.4331 0.6959 0.023 Uiso 1 1 calc R
H3B H 0.1436 0.3422 0.7763 0.023 Uiso 1 1 calc R
C5 C 0.22647(13) 0.4933(3) 0.7134(2) 0.0228(6) Uani 1 1 d .
H5A H 0.2155 0.5634 0.7680 0.027 Uiso 1 1 calc R
H5B H 0.2515 0.5552 0.6718 0.027 Uiso 1 1 calc R
C6 C 0.27015(13) 0.3564(3) 0.77171(19) 0.0237(6) Uani 1 1 d .
H6A H 0.3165 0.3949 0.8124 0.028 Uiso 1 1 calc R
H6B H 0.2496 0.3101 0.8260 0.028 Uiso 1 1 calc R
C8 C 0.26631(13) 0.0704(3) 0.73006(19) 0.0224(6) Uani 1 1 d .
H8A H 0.2966 0.0564 0.8066 0.027 Uiso 1 1 calc R
H8B H 0.2793 -0.0089 0.6827 0.027 Uiso 1 1 calc R
C9 C 0.19170(12) 0.0455(3) 0.72661(18) 0.0195(6) Uani 1 1 d .
H9A H 0.1830 -0.0686 0.7315 0.023 Uiso 1 1 calc R
H9B H 0.1836 0.0976 0.7913 0.023 Uiso 1 1 calc R
C10 C 0.11696(12) -0.0140(3) 0.53824(19) 0.0191(6) Uani 1 1 d .
H10A H 0.0732 0.0193 0.4845 0.023 Uiso 1 1 calc R
H10B H 0.1088 -0.1123 0.5742 0.023 Uiso 1 1 calc R
C11 C 0.17043(12) -0.0415(3) 0.47943(19) 0.0193(6) Uani 1 1 d .
C12 C 0.12334(14) 0.5403(3) 0.55099(19) 0.0228(6) Uani 1 1 d .
H12A H 0.1550 0.6184 0.5351 0.027 Uiso 1 1 calc R
H12B H 0.0894 0.5973 0.5781 0.027 Uiso 1 1 calc R
C13 C 0.08694(13) 0.4496(3) 0.4464(2) 0.0221(6) Uani 1 1 d .
C14 C 0.34181(12) 0.2469(3) 0.66270(19) 0.0227(6) Uani 1 1 d .
H14A H 0.3444 0.3546 0.6344 0.027 Uiso 1 1 calc R
H14B H 0.3405 0.1726 0.6020 0.027 Uiso 1 1 calc R
C15 C 0.40699(13) 0.2161(3) 0.7565(2) 0.0235(6) Uani 1 1 d .
C16 C 0.43623(13) 0.0677(4) 0.7734(2) 0.0242(6) Uani 1 1 d .
H16A H 0.4139 -0.0177 0.7287 0.029 Uiso 1 1 calc R
C17 C 0.49833(13) 0.0424(4) 0.8558(2) 0.0275(7) Uani 1 1 d .
H17A H 0.5174 -0.0604 0.8666 0.033 Uiso 1 1 calc R
C18 C 0.53240(13) 0.1647(4) 0.9216(2) 0.0270(7) Uani 1 1 d .
C19 C 0.50326(14) 0.3140(4) 0.9039(2) 0.0305(7) Uani 1 1 d .
H19A H 0.5258 0.3995 0.9483 0.037 Uiso 1 1 calc R
C20 C 0.44170(13) 0.3397(4) 0.8221(2) 0.0286(7) Uani 1 1 d .
H20A H 0.4229 0.4429 0.8107 0.034 Uiso 1 1 calc R
C21 C 0.59931(14) 0.1372(4) 1.0112(2) 0.0329(7) Uani 1 1 d .
H21A H 0.6079 0.0225 1.0187 0.039 Uiso 1 1 calc R
H21B H 0.5946 0.1758 1.0822 0.039 Uiso 1 1 calc R
C22 C 0.66086(13) 0.2161(3) 0.9913(2) 0.0253(6) Uani 1 1 d .
O24 O 0.03842(12) 0.6966(3) 0.18612(17) 0.0532(7) Uani 1 1 d .
H24A H 0.0405 0.6583 0.2490 0.064 Uiso 1 1 d R
H24B H 0.0129 0.7770 0.1802 0.064 Uiso 1 1 d R
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Al 0.0175(4) 0.0203(4) 0.0128(3) 0.0000(3) 0.0036(3) 0.0001(3)
F 0.0227(8) 0.0247(9) 0.0186(7) 0.0021(6) 0.0061(6) -0.0028(7)
O11 0.0233(10) 0.0211(11) 0.0231(9) -0.0040(8) 0.0065(7) 0.0017(8)
O12 0.0200(9) 0.0204(10) 0.0153(8) 0.0000(7) 0.0055(7) 0.0002(8)
O13 0.0247(10) 0.0352(12) 0.0253(9) 0.0091(9) 0.0042(8) 0.0089(9)
O14 0.0197(9) 0.0210(10) 0.0175(8) 0.0014(7) 0.0037(7) 0.0005(8)
O22 0.0232(10) 0.0587(15) 0.0233(9) 0.0101(10) 0.0031(8) -0.0063(10)
O23 0.0182(9) 0.0366(12) 0.0201(8) -0.0006(9) 0.0045(7) -0.0062(9)
N1 0.0166(11) 0.0207(12) 0.0147(9) 0.0003(9) 0.0023(8) 0.0002(9)
N4 0.0190(11) 0.0198(12) 0.0174(10) -0.0004(9) 0.0057(8) -0.0017(9)
N7 0.0184(11) 0.0242(13) 0.0158(9) 0.0007(9) 0.0058(8) 0.0003(10)
C2 0.0156(12) 0.0226(14) 0.0168(11) 0.0017(10) 0.0053(9) 0.0026(11)
C3 0.0194(13) 0.0224(15) 0.0166(11) 0.0010(11) 0.0062(9) 0.0006(11)
C5 0.0237(14) 0.0258(16) 0.0198(12) -0.0053(11) 0.0081(10) -0.0073(12)
C6 0.0206(13) 0.0344(17) 0.0140(11) -0.0039(12) 0.0024(9) -0.0015(12)
C8 0.0205(13) 0.0288(16) 0.0159(11) 0.0037(11) 0.0023(10) 0.0031(12)
C9 0.0189(13) 0.0230(15) 0.0153(11) 0.0041(11) 0.0029(9) 0.0018(11)
C10 0.0186(13) 0.0200(14) 0.0181(11) -0.0009(11) 0.0046(10) -0.0011(11)
C11 0.0169(13) 0.0229(15) 0.0154(11) 0.0040(11) 0.0008(9) 0.0028(12)
C12 0.0267(14) 0.0195(14) 0.0236(13) 0.0029(11) 0.0098(11) 0.0018(12)
C13 0.0185(13) 0.0279(16) 0.0214(12) 0.0058(12) 0.0085(10) -0.0033(12)
C14 0.0166(12) 0.0337(17) 0.0176(11) -0.0001(12) 0.0047(9) -0.0016(12)
C15 0.0169(13) 0.0352(17) 0.0199(12) -0.0014(12) 0.0079(10) -0.0014(12)
C16 0.0171(13) 0.0344(17) 0.0215(12) -0.0015(12) 0.0066(10) -0.0025(13)
C17 0.0188(14) 0.0375(18) 0.0260(13) 0.0059(13) 0.0067(11) 0.0007(13)
C18 0.0191(14) 0.0418(19) 0.0192(12) 0.0049(13) 0.0047(10) -0.0055(13)
C19 0.0221(15) 0.0403(19) 0.0275(14) -0.0067(13) 0.0053(11) -0.0093(14)
C20 0.0198(14) 0.0355(18) 0.0298(14) -0.0012(13) 0.0063(11) -0.0021(13)
C21 0.0214(14) 0.050(2) 0.0238(13) 0.0066(14) 0.0018(11) -0.0068(14)
C22 0.0220(14) 0.0315(17) 0.0208(12) 0.0043(12) 0.0041(10) 0.0010(12)
O24 0.0680(17) 0.0626(17) 0.0401(12) 0.0266(12) 0.0331(12) 0.0374(14)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0645 0.0514 '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
F Al O12 97.71(8)
F Al O14 93.28(8)
O12 Al O14 95.64(8)
F Al N4 96.85(9)
O12 Al N4 165.44(9)
O14 Al N4 83.35(8)
F Al N1 176.25(8)
O12 Al N1 82.62(8)
O14 Al N1 90.40(8)
N4 Al N1 82.86(9)
F Al N7 91.77(8)
O12 Al N7 95.30(8)
O14 Al N7 167.22(9)
N4 Al N7 84.40(8)
N1 Al N7 84.48(8)
C11 O12 Al 117.76(16)
C13 O14 Al 115.69(16)
C10 N1 C2 113.25(18)
C10 N1 C9 111.6(2)
C2 N1 C9 111.15(18)
C10 N1 Al 103.20(14)
C2 N1 Al 107.55(15)
C9 N1 Al 109.65(15)
C12 N4 C5 114.2(2)
C12 N4 C3 110.59(19)
C5 N4 C3 111.31(18)
C12 N4 Al 103.42(14)
C5 N4 Al 104.86(15)
C3 N4 Al 112.09(16)
C8 N7 C6 111.72(18)
C8 N7 C14 111.7(2)
C6 N7 C14 111.1(2)
C8 N7 Al 104.97(15)
C6 N7 Al 108.18(15)
C14 N7 Al 108.97(14)
N1 C2 C3 108.06(19)
N4 C3 C2 110.26(19)
N4 C5 C6 107.9(2)
N7 C6 C5 110.90(19)
N7 C8 C9 110.1(2)
N1 C9 C8 111.76(19)
N1 C10 C11 108.3(2)
O11 C11 O12 124.5(2)
O11 C11 C10 120.6(2)
O12 C11 C10 114.9(2)
N4 C12 C13 108.8(2)
O13 C13 O14 123.7(2)
O13 C13 C12 121.0(3)
O14 C13 C12 115.3(2)
N7 C14 C15 116.3(2)
C16 C15 C20 118.3(2)
C16 C15 C14 121.0(2)
C20 C15 C14 120.5(3)
C15 C16 C17 120.6(3)
C18 C17 C16 121.0(3)
C17 C18 C19 118.3(2)
C17 C18 C21 121.1(3)
C19 C18 C21 120.7(3)
C20 C19 C18 120.9(3)
C19 C20 C15 120.8(3)
C18 C21 C22 114.6(2)
O22 C22 O23 124.8(3)
O22 C22 C21 125.2(2)
O23 C22 C21 110.0(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Al F 1.7143(16)
Al O12 1.8542(19)
Al O14 1.8748(19)
Al N4 2.036(2)
Al N1 2.074(2)
Al N7 2.080(2)
O11 C11 1.224(3)
O12 C11 1.297(3)
O13 C13 1.230(3)
O14 C13 1.296(3)
O22 C22 1.206(3)
O23 C22 1.322(3)
N1 C10 1.482(3)
N1 C2 1.487(3)
N1 C9 1.506(3)
N4 C12 1.483(3)
N4 C5 1.492(3)
N4 C3 1.505(3)
N7 C8 1.496(3)
N7 C6 1.504(3)
N7 C14 1.504(3)
C2 C3 1.527(4)
C5 C6 1.517(4)
C8 C9 1.529(3)
C10 C11 1.517(3)
C12 C13 1.522(4)
C14 C15 1.519(3)
C15 C16 1.384(4)
C15 C20 1.394(4)
C16 C17 1.398(4)
C17 C18 1.383(4)
C18 C19 1.391(4)
C18 C21 1.511(4)
C19 C20 1.387(4)
C21 C22 1.514(4)
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O23 H23A O11 0.84 1.78 2.616(3) 171.6 2_656
O24 H24A O13 0.85 2.06 2.888(3) 163.6 .
O24 H24B O13 0.85 2.23 3.050(3) 162.0 2
|
1501653.cif | #------------------------------------------------------------------------------
#$Date: 2017-10-13 02:32:00 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201954 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/50/16/1501653.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_1501653
loop_
_publ_author_name
'Jacquemin, Denis'
'Br\'emond, Eric'
'Planchat, Aur\'elien'
'Ciofini, Ilaria'
'Adamo, Carlo'
_publ_section_title
;
TD-DFT Vibronic Couplings in Anthraquinones: From Basis Set and
Functional Benchmarks to Applications for Industrial Dyes
;
_journal_issue 6
_journal_name_full 'Journal of Chemical Theory and Computation'
_journal_page_first 1882
_journal_paper_doi 10.1021/ct200259k
_journal_volume 7
_journal_year 2011
_chemical_formula_moiety 'C14 H10 N2 O2'
_chemical_formula_sum 'C14 H10 N2 O2'
_chemical_formula_weight 238.2
_chemical_name_systematic 1,4-diaminoanthraquinone
_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 97.983(9)
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 13.0342(10)
_cell_length_b 12.2529(12)
_cell_length_c 13.7875(11)
_cell_measurement_temperature 293
_cell_volume 2180.6(3)
_diffrn_ambient_temperature 293
_diffrn_measured_fraction_theta_full 0.98
_diffrn_measured_fraction_theta_max 0.98
_diffrn_measurement_device 'four-cycle diffractometer'
_diffrn_measurement_device_type 'Nonius CCD'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'X-ray tube'
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71069
_diffrn_reflns_av_R_equivalents 0.0958
_diffrn_reflns_av_sigmaI/netI 0.0396
_diffrn_reflns_limit_h_max 16
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_number 38754
_diffrn_reflns_theta_full 27.5
_diffrn_reflns_theta_max 27.5
_diffrn_reflns_theta_min 6.61
_exptl_absorpt_coefficient_mu 0.1
_exptl_absorpt_correction_T_max 0.9865
_exptl_absorpt_correction_T_min 0.9772
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details
'Jana2006 (Petricek, Dusek & Palatinus, 2000)'
_exptl_crystal_colour purple
_exptl_crystal_density_diffrn 1.4509
_exptl_crystal_description block
_exptl_crystal_F_000 992
_exptl_crystal_size_max 0.31
_exptl_crystal_size_mid 0.16
_exptl_crystal_size_min 0.15
_refine_diff_density_max 0.49
_refine_diff_density_min -0.34
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_gt 2.02
_refine_ls_goodness_of_fit_ref 1.93
_refine_ls_hydrogen_treatment mixed
_refine_ls_number_constraints 24
_refine_ls_number_parameters 179
_refine_ls_number_reflns 2469
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.1372
_refine_ls_R_factor_gt 0.0741
_refine_ls_shift/su_max 0.0033
_refine_ls_shift/su_mean 0.0004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details w=1/(\s^2^(I)+0.001936I^2^)
_refine_ls_weighting_scheme sigma
_refine_ls_wR_factor_gt 0.1350
_refine_ls_wR_factor_ref 0.1665
_reflns_number_gt 1549
_reflns_number_total 2469
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file ct200259k_si_002.cif
_cod_data_source_block I
_cod_database_code 1501653
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_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_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
O1 O -0.00025(10) 0.78220(16) -0.05846(12) Uani 0.0572(7) 8 1 d
O2 O 0.36021(9) 0.94035(14) 0.12968(11) Uani 0.0486(6) 8 1 d
N1 N 0.00432(18) 0.6199(3) 0.0624(2) Uani 0.0676(10) 8 1 d
N2 N 0.37483(16) 0.7802(2) 0.25420(19) Uani 0.0569(9) 8 1 d
C1 C 0.09311(16) 0.6645(2) 0.10686(18) Uani 0.0455(8) 8 1 d
C2 C 0.14677(19) 0.6126(2) 0.19115(19) Uani 0.0560(9) 8 1 d
C3 C 0.23689(18) 0.6505(2) 0.23712(18) Uani 0.0516(9) 8 1 d
C4 C 0.28373(15) 0.7466(2) 0.20523(16) Uani 0.0398(7) 8 1 d
C5 C 0.24680(16) 1.0692(2) -0.01147(18) Uani 0.0504(9) 8 1 d
C6 C 0.1923(2) 1.1286(3) -0.0858(2) Uani 0.0635(11) 8 1 d
C7 C 0.1039(2) 1.0865(3) -0.1372(2) Uani 0.0686(11) 8 1 d
C8 C 0.06762(18) 0.9855(2) -0.11405(18) Uani 0.0555(10) 8 1 d
C9 C 0.08060(14) 0.8180(2) -0.00994(16) Uani 0.0390(8) 8 1 d
C10 C 0.27446(14) 0.90350(19) 0.09237(15) Uani 0.0350(7) 8 1 d
C8a C 0.12150(14) 0.9246(2) -0.03754(15) Uani 0.0385(7) 8 1 d
C9a C 0.13474(14) 0.76132(19) 0.07394(15) Uani 0.0352(7) 8 1 d
C10a C 0.21291(14) 0.96563(18) 0.01297(15) Uani 0.0360(7) 8 1 d
C4a C 0.23150(13) 0.80296(19) 0.12445(15) Uani 0.0332(7) 8 1 d
H1 H -0.015(2) 0.558(3) 0.084(2) Uiso 0.083(11) 8 1 d
H2 H 0.409(2) 0.843(3) 0.219(2) Uiso 0.083(10) 8 1 d
H3 H -0.026(2) 0.659(3) 0.002(3) Uiso 0.094(11) 8 1 d
H4 H 0.399(2) 0.751(3) 0.301(2) Uiso 0.070(10) 8 1 d
H1c2 H 0.117435 0.548165 0.215907 Uiso 0.0672 8 1 d
H1c3 H 0.270877 0.611894 0.293135 Uiso 0.062 8 1 d
H1c5 H 0.308922 1.09912 0.024271 Uiso 0.0605 8 1 d
H1c6 H 0.216312 1.199547 -0.101795 Uiso 0.0761 8 1 d
H1c7 H 0.066661 1.127744 -0.189954 Uiso 0.0823 8 1 d
H1c8 H 0.005284 0.956947 -0.150461 Uiso 0.0666 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
O1 O 0.0472(8) 0.0697(14) 0.0494(11) -0.0175(9) -0.0120(7) -0.0043(10)
O2 O 0.0407(7) 0.0482(12) 0.0533(11) -0.0136(8) -0.0062(7) -0.0033(9)
N1 N 0.0641(14) 0.0609(18) 0.0767(19) -0.0324(13) 0.0058(13) 0.0066(15)
N2 N 0.0503(11) 0.0760(19) 0.0395(13) 0.0049(12) -0.0113(10) 0.0070(13)
C1 C 0.0482(11) 0.0433(15) 0.0469(14) -0.0134(11) 0.0127(10) -0.0048(12)
C2 C 0.0733(15) 0.0450(17) 0.0533(16) -0.0095(13) 0.0218(13) 0.0121(14)
C3 C 0.0647(14) 0.0521(17) 0.0385(15) 0.0077(13) 0.0086(11) 0.0115(12)
C4 C 0.0436(11) 0.0445(15) 0.0314(12) 0.0044(11) 0.0055(9) -0.0016(11)
C5 C 0.0523(12) 0.0443(17) 0.0550(16) -0.0077(12) 0.0090(11) 0.0038(13)
C6 C 0.0769(16) 0.0470(19) 0.068(2) 0.0007(14) 0.0155(15) 0.0176(15)
C7 C 0.0820(17) 0.065(2) 0.0561(18) 0.0105(16) -0.0012(14) 0.0217(16)
C8 C 0.0575(13) 0.060(2) 0.0450(16) 0.0012(14) -0.0058(11) 0.0046(14)
C9 C 0.0345(9) 0.0475(16) 0.0339(12) -0.0061(10) 0.0010(9) -0.0073(11)
C10 C 0.0343(9) 0.0363(14) 0.0339(12) -0.0044(9) 0.0034(9) -0.0055(10)
C8a C 0.0408(10) 0.0440(15) 0.0299(11) 0.0006(10) 0.0029(9) 0.0002(11)
C9a C 0.0359(9) 0.0380(14) 0.0319(12) -0.0056(9) 0.0056(9) -0.0039(10)
C10a C 0.0391(10) 0.0353(14) 0.0346(12) -0.0024(10) 0.0086(9) 0.0002(10)
C4a C 0.0352(9) 0.0358(13) 0.0283(11) -0.0022(9) 0.0038(8) -0.0022(10)
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0.003 0.002 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
H 0.000 0.000 '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'
N 0.006 0.003 '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
_geom_angle_publ_flag
C1 N1 H1 118.2(17) yes
C1 N1 H3 113.7(16) yes
H1 N1 H3 128(2) yes
C4 N2 H2 113.4(14) yes
C4 N2 H4 121.3(19) yes
H2 N2 H4 125(2) yes
N1 C1 C2 118.9(2) yes
N1 C1 C9a 122.8(2) yes
C2 C1 C9a 118.35(18) yes
C1 C2 C3 122.0(2) yes
C1 C2 H1c2 118.9771 yes
C3 C2 H1c2 118.9777 yes
C2 C3 C4 121.8(2) yes
C2 C3 H1c3 119.102 yes
C4 C3 H1c3 119.1001 yes
N2 C4 C3 118.9(2) yes
N2 C4 C4a 123.0(2) yes
C3 C4 C4a 118.14(17) yes
C6 C5 C10a 120.89(19) yes
C6 C5 H1c5 119.5537 yes
C10a C5 H1c5 119.5536 yes
C5 C6 C7 119.9(3) yes
C5 C6 H1c6 120.0645 yes
C7 C6 H1c6 120.0635 yes
C6 C7 C8 120.7(2) yes
C6 C7 H1c7 119.656 yes
C8 C7 H1c7 119.6575 yes
C7 C8 C8a 120.1(2) yes
C7 C8 H1c8 119.9398 yes
C8a C8 H1c8 119.9409 yes
O1 C9 C8a 118.71(17) yes
O1 C9 C9a 122.78(19) yes
C8a C9 C9a 118.48(15) yes
O2 C10 C10a 118.83(18) yes
O2 C10 C4a 122.93(17) yes
C10a C10 C4a 118.23(14) yes
C8 C8a C9 120.28(17) yes
C8 C8a C10a 119.3(2) yes
C9 C8a C10a 120.38(17) yes
C1 C9a C9 119.79(16) yes
C1 C9a C4a 119.48(17) yes
C9 C9a C4a 120.73(18) yes
C5 C10a C10 119.31(16) yes
C5 C10a C8a 119.05(17) yes
C10 C10a C8a 121.64(18) yes
C4 C4a C10 119.79(15) yes
C4 C4a C9a 120.12(18) yes
C10 C4a C9a 120.09(16) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
O1 C9 1.248(2) yes
O2 C10 1.249(2) yes
N1 C1 1.348(3) yes
N1 H1 0.86(3) yes
N1 H3 1.00(3) yes
N2 C4 1.347(3) yes
N2 H2 1.05(3) yes
N2 H4 0.79(3) yes
C1 C2 1.421(3) yes
C1 C9a 1.404(3) yes
C2 C3 1.339(3) yes
C2 H1c2 0.96 yes
C3 C4 1.422(3) yes
C3 H1c3 0.96 yes
C4 C4a 1.403(3) yes
C5 C6 1.371(3) yes
C5 C10a 1.399(3) yes
C5 H1c5 0.96 yes
C6 C7 1.368(3) yes
C6 H1c6 0.96 yes
C7 C8 1.377(4) yes
C7 H1c7 0.96 yes
C8 C8a 1.399(3) yes
C8 H1c8 0.96 yes
C9 C8a 1.479(3) yes
C9 C9a 1.446(3) yes
C10 C10a 1.476(3) yes
C10 C4a 1.447(3) yes
C8a C10a 1.389(2) yes
C9a C4a 1.447(2) yes
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_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
N1 H1 O2 5_445 0.86(3) 2.33(3) 3.116(3) 153(2) yes
N2 H2 O2 . 1.05(3) 1.76(3) 2.598(3) 134(2) yes
N2 H2 C10 . 1.05(3) 2.41(3) 2.858(3) 104.5(16) yes
N1 H3 O1 . 1.00(3) 1.78(3) 2.590(3) 136(2) yes
N1 H3 C9 . 1.00(3) 2.41(3) 2.856(4) 106.2(18) yes
N2 H4 O1 8_565 0.79(3) 2.20(3) 2.956(3) 161(3) yes
C2 H1c2 O2 6_545 0.96 2.49 3.260(3) 137.33 yes
loop_
_refln_index_h
_refln_index_k
_refln_index_l
_refln_F_squared_calc
_refln_F_squared_meas
_refln_F_squared_sigma
_refln_observed_status
6 0 0 1916.92 2178.77 15.50 o
8 0 0 11846.91 12525.32 86.38 o
10 0 0 289.44 282.35 4.61 o
12 0 0 1.43 10.65 3.43 o
14 0 0 1028.57 1037.05 16.26 o
5 1 0 228.19 197.78 2.19 o
7 1 0 4868.19 5177.48 28.34 o
9 1 0 2.84 10.02 2.22 o
11 1 0 159.70 154.64 3.74 o
13 1 0 114.76 115.15 4.06 o
15 1 0 18.51 8.33 3.99 o
4 2 0 572.31 605.68 5.42 o
6 2 0 98.95 90.26 2.52 o
8 2 0 806.69 895.64 7.28 o
10 2 0 459.50 477.71 5.65 o
12 2 0 53.29 39.28 4.36 o
14 2 0 36.41 17.29 5.67 o
16 2 0 1.73 13.68 6.04 o
3 3 0 7.48 12.02 2.41 o
5 3 0 437.54 410.22 5.33 o
7 3 0 181.72 178.03 3.38 o
9 3 0 103.64 109.91 3.83 o
11 3 0 11.52 25.58 4.59 o
13 3 0 25.46 23.65 6.68 o
15 3 0 0.74 2.39 4.41 <
0 4 0 830.13 664.15 13.45 o
2 4 0 485.81 451.37 6.94 o
4 4 0 223.71 234.77 4.69 o
6 4 0 41.05 36.68 4.24 o
8 4 0 1.69 -4.28 4.94 <
10 4 0 20.25 33.90 5.85 o
12 4 0 205.69 209.09 8.05 o
14 4 0 201.51 213.54 11.21 o
16 4 0 4.57 19.45 7.31 o
1 5 0 4315.40 4428.17 38.59 o
3 5 0 1276.76 1285.43 15.61 o
5 5 0 5023.07 5202.75 35.54 o
7 5 0 35.63 46.95 5.49 o
9 5 0 293.96 295.65 8.04 o
11 5 0 79.60 81.01 6.39 o
13 5 0 1049.77 1163.00 18.09 o
15 5 0 8.87 10.76 4.81 o
0 6 0 6407.40 6904.99 82.07 o
2 6 0 1358.39 1304.26 16.90 o
4 6 0 607.36 634.65 10.60 o
6 6 0 1160.90 1240.98 12.85 o
8 6 0 2911.33 2965.96 24.30 o
10 6 0 59.66 35.33 8.04 o
12 6 0 518.51 509.67 13.75 o
14 6 0 23.68 4.41 14.98 <
1 7 0 851.12 904.78 15.17 o
3 7 0 1089.95 1080.59 16.15 o
5 7 0 139.96 158.77 6.97 o
7 7 0 70.23 90.06 7.56 o
9 7 0 1142.16 1079.91 14.02 o
11 7 0 94.86 103.14 10.41 o
13 7 0 70.70 89.00 13.71 o
15 7 0 28.46 35.04 6.21 o
0 8 0 15.36 51.49 14.14 o
2 8 0 32.18 5.72 10.52 <
4 8 0 251.62 227.38 10.08 o
6 8 0 1163.35 1224.61 15.20 o
8 8 0 181.90 158.75 7.30 o
10 8 0 89.22 156.64 15.17 o
12 8 0 65.47 36.66 19.54 <
14 8 0 47.89 62.70 21.74 o
1 9 0 167.92 193.74 12.33 o
3 9 0 0.01 10.40 8.00 <
5 9 0 20.28 31.85 9.56 o
7 9 0 15.64 3.37 7.17 <
9 9 0 3.17 -0.19 6.19 <
11 9 0 10.70 38.17 21.92 <
13 9 0 1.62 -129.45 25.24 <
0 10 0 18.28 24.61 12.37 <
2 10 0 222.27 261.12 14.66 o
4 10 0 98.66 71.21 11.26 o
6 10 0 20.17 35.33 9.51 o
8 10 0 6.71 -3.70 11.40 <
10 10 0 9.97 24.21 24.01 <
12 10 0 49.92 -32.38 28.98 <
1 11 0 70.08 57.67 12.18 o
3 11 0 0.08 22.77 14.73 <
5 11 0 543.02 568.68 18.74 o
7 11 0 26.49 7.61 15.03 <
9 11 0 11.06 8.84 18.05 <
11 11 0 1.37 3.49 6.06 <
0 12 0 25.52 38.31 16.94 o
2 12 0 0.95 12.66 17.59 <
4 12 0 225.14 206.05 17.89 o
6 12 0 550.61 587.90 18.39 o
8 12 0 0.09 62.24 13.77 o
10 12 0 10.70 9.90 7.84 <
1 13 0 58.51 94.76 20.01 o
3 13 0 12.21 -2.94 21.62 <
5 13 0 19.06 -26.40 16.34 <
7 13 0 386.83 399.35 16.31 o
9 13 0 8.94 27.76 9.11 o
0 14 0 20.18 -22.02 31.01 <
2 14 0 17.39 19.50 22.49 <
4 14 0 1.16 52.43 22.04 o
6 14 0 0.34 -61.69 20.99 <
1 15 0 0.52 1.31 21.58 <
3 15 0 1.77 -7.62 16.47 <
5 15 0 0.09 -66.46 31.58 <
-15 1 1 412.84 389.76 8.13 o
-13 1 1 242.79 253.69 5.13 o
-11 1 1 42.26 39.10 3.13 o
-9 1 1 394.65 418.98 4.07 o
-7 1 1 656.47 790.53 5.10 o
-5 1 1 0.00 7.20 1.17 o
5 1 1 5.71 8.59 1.56 o
7 1 1 2326.60 2565.56 14.89 o
9 1 1 12.73 10.22 2.38 o
11 1 1 19.74 15.47 3.12 o
13 1 1 22.64 21.61 3.24 o
15 1 1 15.88 28.59 5.35 o
-16 2 1 1.87 -1.73 5.88 <
-14 2 1 49.90 28.70 5.82 o
-12 2 1 128.88 121.60 4.40 o
-10 2 1 33.79 34.53 2.92 o
-8 2 1 8.82 11.81 2.28 o
-6 2 1 67.93 73.87 2.85 o
-4 2 1 4519.75 4150.48 21.66 o
4 2 1 15.70 18.66 1.55 o
6 2 1 99.05 107.34 2.61 o
8 2 1 64.63 73.94 3.39 o
10 2 1 57.24 55.17 3.56 o
12 2 1 243.59 223.25 5.61 o
14 2 1 25.06 5.72 5.68 <
16 2 1 0.31 16.23 7.93 o
-15 3 1 14.90 5.92 4.47 <
-13 3 1 60.22 78.88 6.50 o
-11 3 1 1.25 -2.09 3.77 <
-9 3 1 67.34 76.91 3.55 o
-7 3 1 34.82 37.71 3.19 o
-5 3 1 1514.89 1499.72 10.63 o
-3 3 1 1136.91 1068.00 9.87 o
3 3 1 300.07 370.73 4.99 o
5 3 1 245.61 226.61 5.31 o
7 3 1 55.13 34.13 3.96 o
9 3 1 610.75 659.46 8.65 o
11 3 1 641.84 587.47 8.82 o
13 3 1 259.65 241.84 9.22 o
15 3 1 26.88 41.36 5.82 o
-16 4 1 5.91 10.33 7.08 <
-14 4 1 223.05 189.87 8.36 o
-12 4 1 86.78 93.85 5.75 o
-10 4 1 57.97 58.51 5.06 o
-8 4 1 72.07 60.87 4.21 o
-6 4 1 97.34 89.09 3.23 o
-4 4 1 16.87 8.88 4.74 <
-2 4 1 576.16 582.55 8.17 o
0 4 1 534.15 557.33 7.57 o
2 4 1 751.28 676.51 9.02 o
4 4 1 5.36 4.74 3.63 <
6 4 1 4.80 -21.26 5.23 <
8 4 1 4.66 0.29 4.60 <
10 4 1 4.34 11.59 5.84 <
12 4 1 550.73 611.60 12.79 o
14 4 1 61.40 45.96 9.78 o
16 4 1 23.42 38.20 7.55 o
-15 5 1 29.12 85.31 16.04 o
-13 5 1 210.15 236.54 11.58 o
-11 5 1 60.22 51.58 5.86 o
-9 5 1 1241.42 1238.10 13.04 o
-7 5 1 438.11 460.37 5.59 o
-5 5 1 596.99 583.01 8.05 o
-3 5 1 1442.09 1376.36 13.12 o
-1 5 1 12606.65 12787.64 96.95 o
1 5 1 153.70 140.57 5.56 o
3 5 1 1577.86 1632.36 18.31 o
5 5 1 3063.49 3175.30 26.32 o
7 5 1 310.68 358.01 7.94 o
9 5 1 5.11 1.32 6.04 <
11 5 1 750.21 784.80 11.80 o
13 5 1 833.60 836.31 16.44 o
15 5 1 3.58 2.71 4.80 <
-14 6 1 0.03 -48.91 13.35 <
-12 6 1 0.26 -2.65 10.44 <
-10 6 1 685.19 719.79 11.37 o
-8 6 1 3399.93 3279.70 22.33 o
-6 6 1 606.78 574.84 8.16 o
-4 6 1 110.35 91.28 6.00 o
-2 6 1 5239.61 5604.61 48.83 o
0 6 1 2643.05 2711.70 24.65 o
2 6 1 128.49 144.78 6.90 o
4 6 1 1621.63 1688.22 19.54 o
6 6 1 842.20 904.33 11.32 o
8 6 1 0.12 -1.66 5.90 <
10 6 1 23.00 17.17 8.84 <
12 6 1 72.37 92.35 11.24 o
14 6 1 20.64 39.14 13.41 o
-15 7 1 112.46 138.95 47.57 o
-13 7 1 3.92 -3.51 11.01 <
-11 7 1 3.60 -5.59 7.95 <
-9 7 1 2542.00 2437.61 18.36 o
-7 7 1 724.41 700.58 9.41 o
-5 7 1 3.01 1.65 5.89 <
-3 7 1 140.10 137.38 5.92 o
-1 7 1 1790.60 1720.18 18.70 o
1 7 1 18.75 15.40 8.20 <
3 7 1 268.68 259.97 9.92 o
5 7 1 722.01 772.26 14.33 o
7 7 1 1558.22 1517.01 14.23 o
9 7 1 81.83 43.85 8.42 o
11 7 1 143.38 131.97 15.25 o
13 7 1 11.37 34.16 13.67 o
-14 8 1 3.29 30.43 19.82 <
-12 8 1 58.68 62.81 15.69 o
-10 8 1 26.70 34.56 10.30 o
-8 8 1 5.49 -7.25 5.17 <
-6 8 1 1.51 -13.52 7.44 <
-4 8 1 79.15 70.28 6.90 o
-2 8 1 196.99 232.94 9.07 o
0 8 1 1381.53 1524.01 20.94 o
2 8 1 179.46 161.94 9.58 o
4 8 1 13.73 20.25 9.36 o
6 8 1 3509.86 3299.32 29.43 o
8 8 1 383.60 360.85 6.12 o
10 8 1 20.91 40.45 13.68 o
12 8 1 4.21 -28.02 20.27 <
14 8 1 52.36 63.49 22.41 o
-13 9 1 0.16 49.68 24.30 o
-11 9 1 1.18 7.70 20.77 <
-9 9 1 0.22 6.11 7.77 <
-7 9 1 154.78 168.13 9.81 o
-5 9 1 1.43 -2.47 8.97 <
-3 9 1 0.12 -18.68 9.67 <
-1 9 1 3.99 21.98 10.19 o
1 9 1 8.29 3.11 11.15 <
3 9 1 47.97 12.70 10.71 <
5 9 1 0.25 -16.70 9.33 <
7 9 1 299.68 270.98 8.81 o
9 9 1 20.89 16.11 9.72 <
11 9 1 0.05 -49.80 25.07 <
13 9 1 34.51 79.43 30.90 o
-12 10 1 3.69 -0.82 6.63 <
-10 10 1 19.29 63.84 19.70 o
-8 10 1 0.48 3.92 9.87 <
-6 10 1 34.78 21.87 9.71 o
-4 10 1 74.53 81.01 10.60 o
-2 10 1 80.99 68.99 10.17 o
0 10 1 67.16 37.65 12.10 o
2 10 1 0.35 19.47 10.63 <
4 10 1 65.34 85.02 9.86 o
6 10 1 0.77 -17.90 10.03 <
8 10 1 69.07 70.73 12.12 o
10 10 1 84.28 128.89 26.43 o
12 10 1 55.88 72.12 24.72 o
-11 11 1 1.32 3.99 6.67 <
-9 11 1 7.82 3.93 16.69 <
-7 11 1 14.36 4.85 11.58 <
-5 11 1 158.70 134.39 14.71 o
-3 11 1 117.92 73.84 11.12 o
-1 11 1 4.65 -27.81 13.02 <
1 11 1 22.25 21.55 14.99 <
3 11 1 1212.89 1194.01 22.91 o
5 11 1 1166.55 1125.51 22.24 o
7 11 1 23.29 23.69 12.45 <
9 11 1 0.62 28.62 26.09 <
11 11 1 147.10 162.57 8.62 o
-10 12 1 177.07 194.92 11.43 o
-8 12 1 92.33 64.77 13.48 o
-6 12 1 213.98 240.94 16.59 o
-4 12 1 388.93 332.16 17.38 o
-2 12 1 174.07 151.13 16.19 o
0 12 1 8.05 -3.57 15.17 <
2 12 1 55.06 0.93 13.18 <
4 12 1 473.04 536.24 20.75 o
6 12 1 37.59 34.96 14.55 o
8 12 1 41.52 -2.68 17.87 <
10 12 1 14.19 42.52 8.39 o
-9 13 1 0.11 35.56 9.21 o
-7 13 1 187.98 137.21 19.67 o
-5 13 1 567.91 691.33 21.05 o
-3 13 1 0.03 9.08 22.53 <
-1 13 1 105.41 32.23 18.50 <
1 13 1 382.72 410.67 23.11 o
3 13 1 11.40 -39.49 23.52 <
5 13 1 0.00 -13.42 16.43 <
7 13 1 212.65 251.62 15.92 o
9 13 1 64.63 64.20 9.05 o
-8 14 1 68.86 108.51 11.70 o
-6 14 1 88.91 60.99 21.18 o
-4 14 1 1.13 -7.68 22.46 <
-2 14 1 0.21 97.76 25.79 o
0 14 1 46.46 25.33 23.78 <
2 14 1 101.52 28.39 27.15 <
4 14 1 48.41 74.38 20.78 o
6 14 1 0.03 -57.82 19.94 <
-5 15 1 1.36 50.04 28.90 <
-3 15 1 0.65 -40.49 28.51 <
-1 15 1 0.01 -4.74 5.50 <
1 15 1 48.15 99.46 29.21 o
3 15 1 6.20 19.11 24.18 <
5 15 1 1.55 -31.50 26.68 <
-16 0 2 9.46 18.54 6.19 o
-14 0 2 332.86 375.54 9.19 o
-12 0 2 394.66 414.78 6.93 o
-10 0 2 718.37 729.61 8.38 o
-8 0 2 282.58 299.74 4.97 o
-6 0 2 31.11 34.92 2.60 o
-4 0 2 8764.13 7958.42 49.16 o
4 0 2 4941.83 4892.50 32.89 o
6 0 2 901.24 900.05 7.62 o
8 0 2 5.07 8.63 2.24 o
10 0 2 615.22 646.28 9.42 o
12 0 2 101.07 78.22 4.81 o
14 0 2 1.99 16.43 4.51 o
16 0 2 60.25 89.39 15.74 o
-15 1 2 123.71 126.27 4.22 o
-13 1 2 131.76 140.45 4.48 o
-11 1 2 202.52 208.27 3.23 o
-9 1 2 1668.18 1762.93 9.87 o
-7 1 2 108.54 108.84 2.23 o
-5 1 2 1151.25 1088.06 6.33 o
5 1 2 22.76 17.73 1.54 o
7 1 2 148.61 178.75 3.15 o
9 1 2 301.54 314.15 4.30 o
11 1 2 95.64 84.46 3.63 o
13 1 2 91.81 94.49 4.22 o
15 1 2 3.79 6.45 4.99 <
-16 2 2 7.52 26.32 6.56 o
-14 2 2 16.69 49.05 6.78 o
-12 2 2 29.13 33.37 3.71 o
-10 2 2 247.29 247.76 4.19 o
-8 2 2 120.91 149.81 2.91 o
-6 2 2 19.00 14.46 2.28 o
-4 2 2 95.46 83.02 2.32 o
4 2 2 1201.44 1311.09 9.58 o
6 2 2 5268.05 5530.33 37.82 o
8 2 2 47.05 31.93 3.20 o
10 2 2 43.71 40.91 3.60 o
12 2 2 1632.85 1617.57 17.23 o
14 2 2 7.20 15.24 7.51 o
16 2 2 0.69 -25.51 8.76 <
-15 3 2 2.40 -7.74 10.74 <
-13 3 2 2.58 -0.28 5.82 <
-11 3 2 7.41 0.62 3.65 <
-9 3 2 40.02 38.90 4.17 o
-7 3 2 29.64 34.25 2.95 o
-5 3 2 418.96 454.55 5.03 o
-3 3 2 1913.55 1834.21 13.53 o
3 3 2 79.13 85.73 3.15 o
5 3 2 4330.31 4736.97 29.32 o
7 3 2 109.35 139.81 5.42 o
9 3 2 41.66 41.90 4.80 o
11 3 2 80.88 104.49 6.07 o
13 3 2 87.37 58.48 9.51 o
15 3 2 17.30 33.27 6.31 o
-16 4 2 7.15 15.90 7.28 o
-14 4 2 3.66 -25.95 8.22 <
-12 4 2 18.24 27.35 5.08 o
-10 4 2 0.06 6.33 4.19 <
-8 4 2 29.15 23.36 3.90 o
-6 4 2 10.19 10.39 3.44 o
-4 4 2 1030.37 975.07 10.11 o
-2 4 2 19.14 24.98 4.89 o
0 4 2 137.55 113.69 4.35 o
2 4 2 234.44 271.87 5.94 o
4 4 2 1397.78 1391.14 13.23 o
6 4 2 115.38 131.16 6.30 o
8 4 2 111.17 91.56 6.15 o
10 4 2 603.91 631.56 9.90 o
12 4 2 29.71 30.45 10.39 o
14 4 2 49.00 61.64 11.71 o
-15 5 2 2.94 -45.39 15.01 <
-13 5 2 204.83 220.90 10.19 o
-11 5 2 272.50 313.69 7.72 o
-9 5 2 1118.62 1101.04 12.21 o
-7 5 2 14.16 12.19 4.95 o
-5 5 2 10.20 15.88 4.46 o
-3 5 2 527.94 543.93 9.39 o
-1 5 2 6365.77 6568.10 47.89 o
1 5 2 1207.11 1151.01 12.79 o
3 5 2 1318.39 1397.93 13.02 o
5 5 2 1137.81 1217.65 14.45 o
7 5 2 0.46 5.45 6.42 <
9 5 2 44.97 50.84 7.55 o
11 5 2 0.00 -12.78 7.76 <
13 5 2 10.38 19.45 11.65 <
15 5 2 80.43 126.74 7.59 o
-14 6 2 261.43 232.63 12.91 o
-12 6 2 1.85 -0.63 7.90 <
-10 6 2 1035.31 1065.12 12.15 o
-8 6 2 4112.60 4133.61 28.23 o
-6 6 2 13.63 10.47 4.73 o
-4 6 2 1275.51 1291.29 14.05 o
-2 6 2 2354.89 2556.69 23.82 o
0 6 2 97.81 125.23 6.33 o
2 6 2 241.45 247.09 5.75 o
4 6 2 134.89 117.62 5.48 o
6 6 2 3.66 -0.58 5.74 <
8 6 2 6.58 32.10 7.70 o
10 6 2 49.95 23.37 9.25 o
12 6 2 0.43 -0.16 11.12 <
14 6 2 0.20 -33.60 14.74 <
-15 7 2 99.77 75.56 24.05 o
-13 7 2 81.29 126.44 13.86 o
-11 7 2 5.08 21.92 9.72 o
-9 7 2 473.58 455.58 7.57 o
-7 7 2 811.57 901.94 11.33 o
-5 7 2 175.12 170.94 7.28 o
-3 7 2 62.54 55.39 6.22 o
-1 7 2 7112.47 7280.03 52.39 o
1 7 2 10.60 18.31 7.09 o
3 7 2 90.64 93.79 6.70 o
5 7 2 141.54 150.67 9.65 o
7 7 2 1242.51 1230.55 14.43 o
9 7 2 86.31 94.62 10.56 o
11 7 2 95.17 116.00 16.11 o
13 7 2 20.69 -3.30 14.10 <
-14 8 2 55.41 -4.09 21.44 <
-12 8 2 18.29 -10.20 15.33 <
-10 8 2 141.84 167.77 7.83 o
-8 8 2 402.71 414.30 8.88 o
-6 8 2 246.31 230.12 8.12 o
-4 8 2 0.31 5.31 9.43 <
-2 8 2 1789.94 1965.85 22.12 o
0 8 2 1147.92 1230.49 17.35 o
2 8 2 27.98 29.08 6.68 o
4 8 2 0.00 -14.78 9.35 <
6 8 2 4874.75 4684.08 36.81 o
8 8 2 631.34 667.02 11.11 o
10 8 2 9.51 -21.16 14.65 <
12 8 2 1.30 22.40 19.25 <
14 8 2 43.49 50.05 20.39 o
-13 9 2 0.05 101.96 34.06 o
-11 9 2 10.44 36.60 17.61 o
-9 9 2 148.76 165.16 9.51 o
-7 9 2 13.54 16.73 9.11 <
-5 9 2 89.50 95.83 8.29 o
-3 9 2 172.93 176.92 9.16 o
-1 9 2 5.41 23.74 8.99 o
1 9 2 190.99 215.51 9.53 o
3 9 2 12.09 -15.24 9.57 <
5 9 2 444.78 465.78 13.44 o
7 9 2 1213.89 1130.92 16.01 o
9 9 2 33.54 13.87 11.14 <
11 9 2 2.31 32.38 22.49 <
13 9 2 62.42 129.57 29.76 o
-12 10 2 0.43 10.08 6.27 <
-10 10 2 78.17 56.35 12.27 o
-8 10 2 149.31 165.89 11.47 o
-6 10 2 9.39 21.66 8.95 o
-4 10 2 24.06 22.24 10.03 o
-2 10 2 3.47 11.92 11.66 <
0 10 2 63.81 44.79 9.46 o
2 10 2 1.12 -9.43 10.44 <
4 10 2 769.82 778.00 16.38 o
6 10 2 150.93 138.76 12.89 o
8 10 2 150.71 147.14 15.86 o
10 10 2 0.29 19.69 22.42 <
12 10 2 36.27 47.44 26.66 <
-11 11 2 78.77 139.48 8.59 o
-9 11 2 93.02 99.32 17.08 o
-7 11 2 0.52 35.43 12.25 o
-5 11 2 0.45 18.07 13.21 <
-3 11 2 298.47 226.34 13.26 o
-1 11 2 3.69 -9.78 11.24 <
1 11 2 19.54 10.96 13.11 <
3 11 2 1318.81 1390.18 22.65 o
5 11 2 536.58 519.63 18.31 o
7 11 2 10.11 14.24 14.53 <
9 11 2 33.67 96.02 38.84 o
11 11 2 19.02 25.08 7.14 o
-10 12 2 362.37 451.89 14.13 o
-8 12 2 148.54 121.76 14.53 o
-6 12 2 138.88 98.07 16.74 o
-4 12 2 417.02 332.85 17.39 o
-2 12 2 13.34 46.62 18.19 o
0 12 2 0.49 -12.67 16.33 <
2 12 2 16.98 18.09 14.75 <
4 12 2 392.34 407.77 19.56 o
6 12 2 0.97 -11.50 21.42 <
8 12 2 10.85 13.84 5.00 o
10 12 2 0.03 0.00 7.33 <
-9 13 2 55.49 77.53 10.72 o
-7 13 2 323.56 300.02 19.77 o
-5 13 2 160.39 171.24 15.67 o
-3 13 2 61.44 99.24 23.77 o
-1 13 2 4.17 0.78 20.74 <
1 13 2 81.20 41.36 20.19 o
3 13 2 0.28 -37.15 22.28 <
5 13 2 70.91 60.78 19.74 o
7 13 2 15.01 -9.86 16.28 <
9 13 2 0.41 -11.70 7.53 <
-8 14 2 0.21 -14.06 8.64 <
-6 14 2 120.61 125.11 28.73 o
-4 14 2 3.95 -17.36 19.62 <
-2 14 2 106.64 176.03 27.71 o
0 14 2 1.49 -48.89 27.68 <
2 14 2 66.68 51.44 29.12 <
4 14 2 13.08 34.76 25.73 <
6 14 2 8.77 96.93 32.23 o
-5 15 2 0.06 86.75 48.89 <
-3 15 2 23.68 26.29 29.97 <
-1 15 2 0.80 -22.20 5.95 <
1 15 2 0.48 -13.23 5.60 <
3 15 2 16.48 49.01 33.56 <
5 15 2 11.90 -4.72 27.75 <
-15 1 3 10.26 -3.82 5.31 <
-13 1 3 110.62 126.28 4.18 o
-11 1 3 107.98 106.50 3.42 o
-9 1 3 1275.53 1388.94 8.90 o
-7 1 3 222.54 223.03 3.23 o
-5 1 3 238.48 229.20 3.18 o
3 1 3 17.44 18.58 1.82 o
5 1 3 1708.32 1794.42 10.99 o
7 1 3 80.80 74.91 2.00 o
9 1 3 59.17 58.27 3.01 o
11 1 3 35.63 29.94 3.21 o
13 1 3 52.73 63.57 3.82 o
15 1 3 0.02 -31.01 6.61 <
-16 2 3 137.07 151.19 7.92 o
-14 2 3 7.66 11.81 5.90 o
-12 2 3 52.26 50.10 4.40 o
-10 2 3 965.61 1056.97 7.67 o
-8 2 3 12.91 25.72 2.62 o
-6 2 3 65.16 63.16 2.63 o
-4 2 3 302.91 293.86 3.71 o
2 2 3 2014.29 2000.88 13.19 o
4 2 3 623.28 693.14 6.63 o
6 2 3 3656.67 3969.60 21.86 o
8 2 3 225.51 242.12 5.05 o
10 2 3 439.05 462.71 6.87 o
12 2 3 130.78 136.53 7.25 o
14 2 3 0.72 -2.45 7.24 <
16 2 3 0.15 61.69 15.92 o
-15 3 3 2.07 10.31 8.79 <
-13 3 3 0.91 5.56 5.09 <
-11 3 3 689.61 712.35 8.10 o
-9 3 3 152.32 163.05 4.05 o
-7 3 3 23.74 15.71 3.49 o
-5 3 3 1055.76 1035.20 8.16 o
-3 3 3 21411.08 20690.62 109.85 o
-1 3 3 39.46 53.04 3.56 o
1 3 3 722.95 708.63 8.00 o
3 3 3 13220.59 13096.75 73.15 o
5 3 3 5444.74 5850.82 38.40 o
7 3 3 3.11 0.36 3.86 <
9 3 3 1023.92 1055.42 11.58 o
11 3 3 5183.18 5285.29 37.58 o
13 3 3 19.63 7.02 9.68 <
15 3 3 0.84 0.69 5.76 <
-16 4 3 0.32 -1.55 6.91 <
-14 4 3 162.74 174.06 8.63 o
-12 4 3 197.82 190.83 5.19 o
-10 4 3 400.57 411.15 6.37 o
-8 4 3 110.25 101.73 4.27 o
-6 4 3 843.10 811.30 7.79 o
-4 4 3 431.45 473.75 6.53 o
-2 4 3 335.41 377.40 6.09 o
0 4 3 3668.38 3334.35 24.12 o
2 4 3 6154.38 6355.00 45.45 o
4 4 3 6163.71 6373.87 42.23 o
6 4 3 47.91 38.12 3.10 o
8 4 3 302.09 307.17 8.20 o
10 4 3 1730.78 1730.60 16.72 o
12 4 3 9.66 1.89 9.34 <
14 4 3 4.85 -24.36 13.79 <
-15 5 3 0.21 39.91 14.49 o
-13 5 3 0.70 -1.38 8.98 <
-11 5 3 1586.73 1643.56 15.52 o
-9 5 3 52.87 33.68 6.01 o
-7 5 3 150.31 145.89 5.99 o
-5 5 3 13.14 30.85 4.58 o
-3 5 3 1641.72 1677.84 15.67 o
-1 5 3 892.75 823.03 11.20 o
1 5 3 2084.64 2049.69 19.35 o
3 5 3 265.82 313.24 6.69 o
5 5 3 176.21 203.45 5.22 o
7 5 3 222.69 230.43 8.52 o
9 5 3 34.26 15.56 6.25 o
11 5 3 17.97 19.96 9.47 o
13 5 3 1.59 -14.91 11.22 <
15 5 3 8.31 28.47 7.61 o
-14 6 3 21.28 7.74 15.75 <
-12 6 3 3.36 -11.98 7.98 <
-10 6 3 40.07 22.42 6.33 o
-8 6 3 106.27 109.05 6.57 o
-6 6 3 10.15 4.73 6.29 <
-4 6 3 9.85 4.05 5.52 <
-2 6 3 127.07 170.14 7.56 o
0 6 3 962.75 886.63 12.29 o
2 6 3 56.11 73.83 6.09 o
4 6 3 2.66 4.60 3.85 <
6 6 3 37.25 29.90 5.40 o
8 6 3 3.26 26.49 9.37 o
10 6 3 103.59 127.61 9.88 o
12 6 3 2.50 -28.12 14.08 <
14 6 3 6.31 56.46 15.63 o
-15 7 3 345.12 272.68 17.34 o
-13 7 3 155.81 154.03 13.39 o
-11 7 3 7.41 -20.23 8.16 <
-9 7 3 360.83 361.34 8.53 o
-7 7 3 645.05 678.08 10.96 o
-5 7 3 25.02 27.67 7.90 o
-3 7 3 559.22 560.53 11.61 o
-1 7 3 1500.74 1683.74 19.32 o
1 7 3 131.58 118.60 6.75 o
3 7 3 110.86 119.39 5.99 o
5 7 3 22.88 15.61 7.34 o
7 7 3 205.45 226.66 8.96 o
9 7 3 86.73 90.13 9.41 o
11 7 3 7.99 16.23 13.08 <
13 7 3 15.02 21.84 18.26 <
-14 8 3 44.54 85.66 23.55 o
-12 8 3 9.35 15.69 14.98 <
-10 8 3 2.39 3.82 6.99 <
-8 8 3 486.58 456.38 9.80 o
-6 8 3 21.22 22.98 7.31 o
-4 8 3 364.41 344.50 9.33 o
-2 8 3 261.68 292.26 10.07 o
0 8 3 0.35 -11.51 7.88 <
2 8 3 22.33 23.15 9.15 o
4 8 3 17.27 7.19 6.91 <
6 8 3 1935.83 1963.71 20.77 o
8 8 3 12.80 5.12 9.49 <
10 8 3 38.06 28.59 16.91 <
12 8 3 9.92 16.54 19.03 <
-13 9 3 1.06 -32.88 37.39 <
-11 9 3 0.93 -29.97 14.50 <
-9 9 3 7.87 -2.97 8.23 <
-7 9 3 56.35 72.89 9.76 o
-5 9 3 22.28 53.75 9.34 o
-3 9 3 307.74 293.18 11.44 o
-1 9 3 111.28 96.82 9.76 o
1 9 3 328.17 271.96 10.20 o
3 9 3 1946.20 2007.92 21.21 o
5 9 3 295.00 340.23 13.22 o
7 9 3 167.02 156.52 12.77 o
9 9 3 421.74 451.66 14.57 o
11 9 3 12.46 10.10 24.82 <
13 9 3 11.84 15.81 20.43 <
-12 10 3 17.13 12.80 6.97 <
-10 10 3 24.07 27.43 12.80 o
-8 10 3 250.13 230.00 10.57 o
-6 10 3 338.78 319.68 11.14 o
-4 10 3 0.88 -2.52 9.41 <
-2 10 3 4.05 -1.14 9.51 <
0 10 3 8.36 24.13 10.12 o
2 10 3 1026.75 1075.36 17.68 o
4 10 3 1418.13 1452.07 21.27 o
6 10 3 51.98 25.71 13.41 <
8 10 3 72.03 75.71 15.34 o
10 10 3 25.79 53.83 29.45 <
12 10 3 57.45 66.35 7.71 o
-11 11 3 29.87 27.83 9.05 o
-9 11 3 38.68 96.10 17.67 o
-7 11 3 48.94 37.36 14.64 o
-5 11 3 2.47 -7.76 10.75 <
-3 11 3 142.36 77.80 11.49 o
-1 11 3 157.02 160.38 11.84 o
1 11 3 26.93 -5.17 12.43 <
3 11 3 217.24 186.46 17.24 o
5 11 3 121.02 90.01 15.80 o
7 11 3 6.04 39.59 16.15 o
9 11 3 5.37 14.59 23.58 <
11 11 3 0.09 5.08 6.31 <
-10 12 3 149.10 201.69 12.01 o
-8 12 3 53.55 32.46 12.03 o
-6 12 3 29.82 10.81 16.22 <
-4 12 3 52.38 5.53 16.02 <
-2 12 3 2.13 19.45 18.15 <
0 12 3 1.44 -9.86 14.86 <
2 12 3 11.98 -31.32 17.05 <
4 12 3 7.36 6.53 18.97 <
6 12 3 30.69 79.60 19.39 o
8 12 3 4.50 11.57 5.02 o
10 12 3 0.05 9.20 7.21 <
-9 13 3 19.30 56.57 9.65 o
-7 13 3 126.78 166.58 19.40 o
-5 13 3 47.69 73.26 16.29 o
-3 13 3 6.77 15.31 22.89 <
-1 13 3 1.82 -2.93 22.54 <
1 13 3 102.94 126.64 21.20 o
3 13 3 0.17 9.46 25.21 <
5 13 3 29.84 22.52 15.49 <
7 13 3 25.50 13.04 6.46 o
-6 14 3 0.00 -41.42 26.34 <
-4 14 3 36.45 36.18 23.93 <
-2 14 3 0.02 77.54 28.13 o
0 14 3 21.33 50.55 21.62 o
2 14 3 0.64 -10.36 17.65 <
4 14 3 39.77 67.47 23.05 o
6 14 3 3.92 -12.29 5.44 <
-5 15 3 1.67 34.51 31.94 <
-3 15 3 1.43 -8.29 6.87 <
-1 15 3 65.70 43.59 8.42 o
1 15 3 0.50 -7.53 6.55 <
3 15 3 6.81 14.31 21.28 <
-16 0 4 141.83 136.01 9.38 o
-14 0 4 9.03 2.56 6.58 <
-12 0 4 0.13 -17.29 5.17 <
-10 0 4 91.18 108.30 5.14 o
-8 0 4 114.24 114.83 4.78 o
-6 0 4 264.43 237.16 4.85 o
-4 0 4 4735.44 4357.29 33.85 o
2 0 4 161.24 192.77 4.28 o
4 0 4 522.84 510.58 7.12 o
6 0 4 133.66 123.41 4.91 o
8 0 4 115.92 122.30 4.21 o
10 0 4 15.07 22.13 3.95 o
12 0 4 25.90 11.38 4.74 o
14 0 4 14.04 34.30 12.09 o
-15 1 4 87.66 110.63 7.11 o
-13 1 4 0.06 9.22 4.32 o
-11 1 4 282.48 271.12 4.65 o
-9 1 4 492.44 533.00 5.72 o
-7 1 4 192.81 184.37 3.56 o
-5 1 4 19.74 25.96 2.63 o
-3 1 4 5189.92 5187.56 29.07 o
1 1 4 24.68 23.86 2.45 o
3 1 4 334.57 365.30 4.10 o
5 1 4 24.17 23.94 2.47 o
7 1 4 203.25 186.22 3.19 o
9 1 4 97.23 92.35 3.27 o
11 1 4 127.28 130.21 3.78 o
13 1 4 49.85 49.26 6.22 o
15 1 4 5.73 10.17 13.65 <
-16 2 4 13.98 -3.14 5.33 <
-14 2 4 19.23 23.36 5.50 o
-12 2 4 85.49 95.25 4.49 o
-10 2 4 108.57 121.00 4.10 o
-8 2 4 74.09 74.52 3.42 o
-6 2 4 1.10 2.03 3.29 <
-4 2 4 6315.14 6234.79 33.15 o
-2 2 4 13548.18 13281.50 72.09 o
0 2 4 3762.67 3430.86 22.66 o
2 2 4 381.26 377.88 4.66 o
4 2 4 2196.18 2270.24 14.51 o
6 2 4 151.79 177.03 3.35 o
8 2 4 40.56 43.99 3.03 o
10 2 4 306.69 308.34 6.26 o
12 2 4 82.78 57.81 7.12 o
14 2 4 145.53 133.25 6.89 o
-15 3 4 0.35 -4.03 9.51 <
-13 3 4 0.90 5.17 5.76 <
-11 3 4 622.26 637.21 7.38 o
-9 3 4 0.26 0.45 3.45 <
-7 3 4 512.69 502.85 6.18 o
-5 3 4 3852.85 3693.52 21.56 o
-3 3 4 4040.37 4197.32 24.86 o
-1 3 4 570.65 613.02 7.39 o
1 3 4 282.05 279.52 5.14 o
3 3 4 3299.60 3312.71 21.12 o
5 3 4 1820.03 2130.80 17.09 o
7 3 4 269.11 264.32 4.64 o
9 3 4 1577.21 1613.26 16.77 o
11 3 4 904.71 925.04 14.21 o
13 3 4 52.15 30.07 8.17 o
15 3 4 8.02 1.65 9.05 <
-16 4 4 11.44 -8.97 5.72 <
-14 4 4 4.15 30.70 7.55 o
-12 4 4 822.32 855.91 9.98 o
-10 4 4 2081.84 2112.80 14.43 o
-8 4 4 42.77 42.07 3.78 o
-6 4 4 212.85 228.64 5.07 o
-4 4 4 6745.06 6724.71 45.93 o
-2 4 4 1255.19 1373.09 12.55 o
0 4 4 496.41 524.75 8.29 o
2 4 4 4369.17 4778.15 30.87 o
4 4 4 1816.97 2123.87 17.64 o
6 4 4 0.00 -6.74 3.47 <
8 4 4 209.87 225.09 6.26 o
10 4 4 22.65 13.81 6.66 o
12 4 4 1.33 13.54 9.52 <
14 4 4 7.75 11.27 3.98 o
-15 5 4 8.77 -12.94 13.10 <
-13 5 4 9.55 -11.20 8.71 <
-11 5 4 1837.06 1816.20 14.55 o
-9 5 4 32.50 8.92 6.55 <
-7 5 4 19.49 6.72 5.50 <
-5 5 4 94.24 104.55 5.42 o
-3 5 4 177.02 198.99 6.19 o
-1 5 4 127.60 108.16 5.27 o
1 5 4 0.69 3.90 5.79 <
3 5 4 245.03 259.24 6.48 o
5 5 4 9.42 17.96 5.50 o
7 5 4 111.16 105.12 4.49 o
9 5 4 403.18 347.26 10.28 o
11 5 4 260.21 241.49 10.46 o
13 5 4 7.21 -3.78 11.51 <
-14 6 4 90.52 61.60 16.26 o
-12 6 4 0.48 -19.00 7.46 <
-10 6 4 9.12 8.09 7.54 <
-8 6 4 5.17 -8.57 6.56 <
-6 6 4 0.01 22.93 7.57 o
-4 6 4 35.48 36.27 5.50 o
-2 6 4 17.22 10.65 5.88 <
0 6 4 2.79 -6.56 5.60 <
2 6 4 1.53 1.70 6.20 <
4 6 4 129.43 139.52 6.82 o
6 6 4 152.71 163.14 6.10 o
8 6 4 19.84 22.62 10.00 o
10 6 4 4.54 -12.14 11.03 <
12 6 4 22.73 1.66 12.49 <
14 6 4 7.25 -4.17 5.29 <
-15 7 4 46.56 47.39 34.40 <
-13 7 4 9.72 18.27 12.56 <
-11 7 4 48.81 40.83 8.64 o
-9 7 4 282.20 288.85 9.66 o
-7 7 4 44.27 44.89 7.75 o
-5 7 4 113.26 120.58 7.52 o
-3 7 4 42.81 23.80 6.76 o
-1 7 4 254.86 225.11 9.31 o
1 7 4 7.08 -8.50 7.31 <
3 7 4 35.46 42.24 8.11 o
5 7 4 60.20 50.60 6.02 o
7 7 4 4.78 -24.66 7.23 <
9 7 4 5.93 3.94 14.32 <
11 7 4 46.71 71.71 13.51 o
13 7 4 38.65 49.19 22.15 o
-14 8 4 0.00 26.62 26.64 <
-12 8 4 66.66 87.66 13.43 o
-10 8 4 37.60 15.71 8.60 <
-8 8 4 25.72 27.85 8.05 o
-6 8 4 16.51 41.35 8.22 o
-4 8 4 0.82 -10.23 8.55 <
-2 8 4 93.36 80.25 9.00 o
0 8 4 0.78 -26.72 7.89 <
2 8 4 114.46 96.36 7.82 o
4 8 4 7.27 12.02 8.64 <
6 8 4 331.62 341.55 10.08 o
8 8 4 242.97 235.42 11.02 o
10 8 4 143.14 101.49 20.93 o
12 8 4 1.72 4.17 19.74 <
-13 9 4 37.30 32.01 7.14 o
-11 9 4 13.86 70.92 13.91 o
-9 9 4 39.98 33.41 10.99 o
-7 9 4 275.94 283.73 7.86 o
-5 9 4 96.20 80.27 9.52 o
-3 9 4 955.22 1005.10 17.19 o
-1 9 4 200.47 188.06 8.56 o
1 9 4 2659.65 2647.46 26.18 o
3 9 4 217.91 178.66 11.02 o
5 9 4 1073.76 1138.60 16.20 o
7 9 4 38.78 21.20 11.52 <
9 9 4 32.26 -8.86 14.47 <
11 9 4 14.69 -19.91 22.72 <
-12 10 4 173.46 247.61 11.81 o
-10 10 4 11.85 -24.31 11.56 <
-8 10 4 39.65 25.27 11.40 o
-6 10 4 512.65 420.20 14.72 o
-4 10 4 451.63 401.12 11.03 o
-2 10 4 116.59 101.03 10.33 o
0 10 4 342.81 381.86 13.41 o
2 10 4 1847.27 1982.18 25.39 o
4 10 4 2047.59 2033.52 23.44 o
6 10 4 271.16 233.57 12.21 o
8 10 4 105.41 75.45 14.28 o
10 10 4 32.33 64.54 30.26 o
-11 11 4 0.34 16.09 7.83 o
-9 11 4 10.87 -16.12 10.23 <
-7 11 4 4.51 1.99 10.77 <
-5 11 4 27.79 32.40 10.45 o
-3 11 4 156.56 134.26 12.79 o
-1 11 4 5.13 -19.47 11.58 <
1 11 4 20.94 17.24 12.29 <
3 11 4 110.12 135.23 17.52 o
5 11 4 60.33 35.51 17.71 o
7 11 4 58.78 44.96 17.49 o
9 11 4 20.97 33.20 25.39 <
11 11 4 7.90 -2.63 6.42 <
-10 12 4 56.41 57.03 8.71 o
-8 12 4 4.19 4.09 10.79 <
-6 12 4 0.28 4.51 16.76 <
-4 12 4 14.66 -11.28 12.46 <
-2 12 4 0.02 2.14 16.75 <
0 12 4 2.61 -5.04 19.30 <
2 12 4 270.69 269.13 20.37 o
4 12 4 240.30 222.43 20.91 o
6 12 4 16.29 10.71 16.81 <
8 12 4 1.16 21.86 7.50 o
-9 13 4 7.50 27.78 10.12 o
-7 13 4 26.06 36.80 20.32 <
-5 13 4 7.23 -55.91 20.33 <
-3 13 4 11.33 -35.62 26.53 <
-1 13 4 11.37 30.94 25.18 <
1 13 4 0.98 33.53 24.22 <
3 13 4 3.98 25.75 24.16 <
5 13 4 4.64 22.04 15.81 <
7 13 4 9.47 9.47 5.59 <
-6 14 4 24.07 76.04 30.08 o
-4 14 4 14.11 89.51 28.47 o
-2 14 4 54.25 28.65 31.06 <
0 14 4 0.43 34.12 28.65 <
2 14 4 0.63 29.23 25.63 <
4 14 4 0.04 -23.70 22.99 <
6 14 4 1.99 16.92 8.25 o
-3 15 4 52.50 68.30 7.71 o
-1 15 4 144.41 174.37 8.43 o
1 15 4 87.42 96.90 6.97 o
3 15 4 6.59 19.23 6.89 o
-15 1 5 0.77 7.48 6.23 <
-13 1 5 4.16 -3.26 5.40 <
-11 1 5 97.28 99.60 4.56 o
-9 1 5 4.41 6.79 3.49 <
-7 1 5 578.39 604.34 6.30 o
-5 1 5 517.46 511.06 5.52 o
-3 1 5 0.00 -0.22 3.39 <
-1 1 5 2693.90 2490.86 16.19 o
1 1 5 2102.38 2127.68 13.39 o
3 1 5 178.66 187.47 3.68 o
5 1 5 117.86 129.86 3.38 o
7 1 5 160.47 159.60 3.71 o
9 1 5 2205.01 2160.36 13.34 o
11 1 5 8.10 -1.79 4.22 <
13 1 5 16.53 28.47 8.26 o
15 1 5 14.90 40.93 14.83 o
-16 2 5 68.79 74.06 5.76 o
-14 2 5 26.70 11.30 6.34 <
-12 2 5 223.74 221.80 5.76 o
-10 2 5 21.27 18.47 4.47 o
-8 2 5 33.78 22.48 3.98 o
-6 2 5 284.35 262.31 4.64 o
-4 2 5 403.49 433.48 5.38 o
-2 2 5 7465.93 7441.51 43.03 o
0 2 5 7901.57 7884.63 44.92 o
2 2 5 550.68 565.42 6.86 o
4 2 5 171.23 146.41 3.87 o
6 2 5 1.26 0.86 2.70 <
8 2 5 3057.36 3059.20 18.53 o
10 2 5 16.44 14.10 5.04 o
12 2 5 1.86 4.88 7.48 <
14 2 5 4.39 9.31 5.21 <
-15 3 5 49.69 31.30 10.70 o
-13 3 5 257.04 284.17 7.54 o
-11 3 5 7.29 9.98 4.55 o
-9 3 5 173.10 198.64 4.45 o
-7 3 5 24.12 13.44 3.99 o
-5 3 5 12094.48 12250.14 65.46 o
-3 3 5 112.28 107.94 4.74 o
-1 3 5 3195.42 2995.38 21.57 o
1 3 5 1122.44 1142.19 11.10 o
3 3 5 4299.52 4691.88 28.80 o
5 3 5 144.71 149.73 5.53 o
7 3 5 684.58 683.87 7.53 o
9 3 5 170.90 168.17 6.64 o
11 3 5 92.06 112.09 9.07 o
13 3 5 134.06 120.08 9.38 o
15 3 5 0.61 -34.92 14.84 <
-16 4 5 1.13 3.25 7.20 <
-14 4 5 44.04 20.74 8.08 o
-12 4 5 923.59 971.26 10.66 o
-10 4 5 1073.58 1120.24 9.83 o
-8 4 5 105.96 104.04 5.47 o
-6 4 5 341.72 344.43 6.22 o
-4 4 5 23193.72 23783.61 127.89 o
-2 4 5 306.74 321.77 7.14 o
0 4 5 177.25 149.14 5.19 o
2 4 5 127.24 142.53 5.22 o
4 4 5 2835.36 2999.28 20.52 o
6 4 5 44.94 38.10 4.96 o
8 4 5 95.94 72.28 5.23 o
10 4 5 1034.12 928.38 13.28 o
12 4 5 85.74 79.25 10.56 o
14 4 5 0.22 -6.22 6.42 <
-15 5 5 10.68 -12.84 13.97 <
-13 5 5 14.82 10.15 7.95 <
-11 5 5 947.38 905.92 9.70 o
-9 5 5 27.96 21.88 5.31 o
-7 5 5 3.19 -6.79 5.80 <
-5 5 5 1314.71 1289.99 12.75 o
-3 5 5 97.00 95.23 5.54 o
-1 5 5 48.15 47.79 6.36 o
1 5 5 894.57 833.69 10.43 o
3 5 5 1201.61 1220.06 13.29 o
5 5 5 27.30 21.87 5.35 o
7 5 5 2.77 -5.04 4.24 <
9 5 5 1533.44 1440.25 16.53 o
11 5 5 59.28 55.00 11.71 o
13 5 5 2.75 0.17 14.11 <
-14 6 5 2.90 5.59 14.41 <
-12 6 5 1.96 -3.25 6.82 <
-10 6 5 2.46 -6.38 6.92 <
-8 6 5 14.87 -6.84 7.40 <
-6 6 5 13.52 2.03 6.79 <
-4 6 5 14.47 21.21 5.59 o
-2 6 5 196.83 173.62 7.12 o
0 6 5 20.80 22.87 6.05 o
2 6 5 205.17 201.16 7.46 o
4 6 5 23.32 9.00 6.27 <
6 6 5 505.03 487.13 9.12 o
8 6 5 14.66 29.59 6.32 o
10 6 5 0.03 26.64 13.80 <
12 6 5 86.01 74.62 13.37 o
14 6 5 12.46 11.11 5.56 <
-13 7 5 2.38 0.76 18.17 <
-11 7 5 96.27 92.69 9.42 o
-9 7 5 0.02 11.77 7.87 <
-7 7 5 0.53 -2.80 8.62 <
-5 7 5 247.75 258.99 8.28 o
-3 7 5 58.38 39.26 6.57 o
-1 7 5 124.00 94.54 7.74 o
1 7 5 64.31 87.28 8.20 o
3 7 5 415.67 435.39 9.56 o
5 7 5 44.48 54.14 7.35 o
7 7 5 2.85 0.30 5.57 <
9 7 5 0.95 -50.35 15.73 <
11 7 5 1.40 -26.53 16.19 <
13 7 5 14.12 -6.93 18.75 <
-14 8 5 0.05 -19.79 6.67 <
-12 8 5 0.53 -34.83 16.78 <
-10 8 5 404.77 428.23 12.00 o
-8 8 5 0.89 0.71 9.06 <
-6 8 5 92.80 66.28 9.12 o
-4 8 5 342.05 338.78 11.10 o
-2 8 5 141.63 176.89 11.58 o
0 8 5 166.74 140.25 9.86 o
2 8 5 941.62 950.75 16.07 o
4 8 5 46.75 41.34 7.21 o
6 8 5 4.74 -10.71 9.10 <
8 8 5 0.21 -8.23 12.45 <
10 8 5 140.34 130.21 24.37 o
12 8 5 22.21 -29.76 31.26 <
-13 9 5 97.16 107.25 6.57 o
-11 9 5 108.62 103.71 12.77 o
-9 9 5 144.31 154.61 9.97 o
-7 9 5 1.18 27.29 9.96 o
-5 9 5 268.77 204.33 11.83 o
-3 9 5 1439.66 1479.80 19.11 o
-1 9 5 45.74 31.06 10.78 o
1 9 5 3148.18 3157.57 32.36 o
3 9 5 3581.06 3759.41 32.49 o
5 9 5 427.06 443.21 12.43 o
7 9 5 30.44 11.12 13.91 <
9 9 5 313.92 293.81 15.00 o
11 9 5 1.83 -47.41 26.46 <
-12 10 5 269.10 414.14 11.74 o
-10 10 5 67.73 98.39 19.19 o
-8 10 5 15.56 6.04 12.70 <
-6 10 5 823.66 680.97 14.46 o
-4 10 5 125.10 151.17 12.06 o
-2 10 5 77.39 38.00 11.01 o
0 10 5 417.01 451.09 13.49 o
2 10 5 918.40 919.93 15.55 o
4 10 5 2822.22 2992.66 36.32 o
6 10 5 33.75 -20.36 17.47 <
8 10 5 1.41 -15.69 21.39 <
10 10 5 0.47 88.41 26.38 o
-11 11 5 112.11 111.31 8.16 o
-9 11 5 12.27 13.37 10.51 <
-7 11 5 8.92 -16.47 12.29 <
-5 11 5 150.12 118.32 13.33 o
-3 11 5 0.87 -6.96 11.01 <
-1 11 5 57.97 20.34 12.39 <
1 11 5 84.41 68.32 15.83 o
3 11 5 245.84 223.56 13.83 o
5 11 5 263.74 260.53 19.89 o
7 11 5 72.74 100.46 22.42 o
9 11 5 3.30 10.87 7.15 <
-10 12 5 4.24 11.91 9.76 <
-8 12 5 70.48 95.83 16.42 o
-6 12 5 19.96 37.53 11.14 o
-4 12 5 2.72 2.25 21.92 <
-2 12 5 3.47 -39.40 21.58 <
0 12 5 15.96 -33.76 16.84 <
2 12 5 0.02 -11.77 16.04 <
4 12 5 3.77 -47.96 23.11 <
6 12 5 76.95 67.99 9.32 o
8 12 5 29.52 58.82 8.52 o
-9 13 5 1.54 5.98 8.17 <
-7 13 5 7.33 -37.16 20.93 <
-5 13 5 0.94 22.75 18.30 <
-3 13 5 64.37 164.90 25.50 o
-1 13 5 2.99 41.76 26.51 <
1 13 5 0.03 -20.03 23.68 <
3 13 5 8.06 -7.39 28.33 <
5 13 5 1.84 -58.34 26.30 <
7 13 5 0.07 1.77 8.35 <
-6 14 5 0.02 17.66 32.01 <
-4 14 5 0.47 -50.04 34.08 <
-2 14 5 0.00 -0.30 24.89 <
0 14 5 50.85 79.57 8.16 o
2 14 5 1.23 1.54 26.35 <
4 14 5 4.96 -77.82 26.41 <
-3 15 5 0.77 -16.00 6.96 <
-1 15 5 0.47 40.11 7.39 o
1 15 5 147.51 165.43 9.03 o
-16 0 6 6.65 -14.84 7.54 <
-14 0 6 68.83 80.32 9.04 o
-12 0 6 32.13 50.44 7.25 o
-10 0 6 101.90 89.35 6.69 o
-8 0 6 45.14 53.34 6.16 o
-6 0 6 2648.96 2623.63 22.41 o
-4 0 6 537.13 516.92 10.87 o
-2 0 6 810.96 834.22 13.06 o
0 0 6 5734.27 5766.35 44.53 o
2 0 6 3629.86 3655.45 33.38 o
4 0 6 124.92 117.45 5.25 o
6 0 6 8.99 -1.31 4.96 <
8 0 6 3415.25 3374.59 28.64 o
10 0 6 36.26 34.72 3.79 o
12 0 6 168.43 178.99 6.30 o
14 0 6 2.14 16.56 11.02 <
-15 1 6 17.06 19.67 10.78 <
-13 1 6 181.56 168.12 6.07 o
-11 1 6 2.70 10.94 4.72 o
-9 1 6 45.51 42.26 4.80 o
-7 1 6 125.09 136.34 4.92 o
-5 1 6 2012.51 2022.82 14.26 o
-3 1 6 307.02 261.91 5.83 o
-1 1 6 277.62 294.58 5.18 o
1 1 6 4071.26 4122.32 23.80 o
3 1 6 108.79 115.38 3.99 o
5 1 6 602.64 577.96 6.26 o
7 1 6 1063.00 1030.82 8.94 o
9 1 6 3587.68 3692.98 22.37 o
11 1 6 38.94 21.66 5.71 o
13 1 6 1.14 8.05 4.25 <
-16 2 6 49.70 36.69 6.36 o
-14 2 6 201.32 208.68 7.31 o
-12 2 6 601.64 622.96 8.46 o
-10 2 6 30.51 46.24 5.42 o
-8 2 6 246.20 240.50 5.57 o
-6 2 6 2335.53 2443.06 15.86 o
-4 2 6 344.79 372.61 5.94 o
-2 2 6 659.80 619.01 8.12 o
0 2 6 7424.76 7760.38 43.08 o
2 2 6 4381.57 4727.09 27.92 o
4 2 6 32.00 34.78 4.05 o
6 2 6 107.77 106.36 4.17 o
8 2 6 3318.42 3367.29 20.64 o
10 2 6 3.82 -1.96 5.49 <
12 2 6 22.11 56.88 10.02 o
14 2 6 27.73 -21.69 13.61 <
-15 3 6 47.29 67.21 8.78 o
-13 3 6 272.54 287.10 7.29 o
-11 3 6 170.04 188.66 6.00 o
-9 3 6 6.92 9.14 5.15 <
-7 3 6 148.20 155.09 5.39 o
-5 3 6 5736.08 5875.20 34.91 o
-3 3 6 1402.65 1483.99 13.29 o
-1 3 6 0.41 -10.54 5.07 <
1 3 6 2254.46 2589.16 18.77 o
3 3 6 236.82 223.63 5.21 o
5 3 6 34.41 43.21 4.90 o
7 3 6 191.14 191.22 4.23 o
9 3 6 14.01 5.19 4.42 <
11 3 6 31.86 38.35 10.29 o
13 3 6 6.72 16.53 14.31 <
-16 4 6 27.30 54.06 7.61 o
-14 4 6 68.78 47.30 9.37 o
-12 4 6 55.71 49.27 7.16 o
-10 4 6 15.00 3.87 6.66 <
-8 4 6 133.42 153.33 6.57 o
-6 4 6 698.75 713.78 9.13 o
-4 4 6 8227.15 8356.96 52.45 o
-2 4 6 944.02 907.45 11.12 o
0 4 6 11.78 -3.37 5.38 <
2 4 6 1914.93 2051.48 17.35 o
4 4 6 542.99 590.38 7.93 o
6 4 6 9.78 30.28 5.27 o
8 4 6 386.72 393.07 6.92 o
10 4 6 600.17 555.18 12.80 o
12 4 6 2.70 -20.78 11.04 <
14 4 6 10.79 9.35 5.54 <
-15 5 6 16.33 13.91 17.58 <
-13 5 6 127.22 127.23 7.06 o
-11 5 6 58.32 54.80 6.82 o
-9 5 6 26.16 17.86 6.55 o
-7 5 6 0.79 -17.70 5.87 <
-5 5 6 1317.57 1337.77 14.05 o
-3 5 6 80.71 72.94 6.26 o
-1 5 6 94.17 82.54 6.18 o
1 5 6 148.89 149.40 6.33 o
3 5 6 2976.90 3356.13 23.72 o
5 5 6 239.76 223.46 7.13 o
7 5 6 126.71 102.51 5.87 o
9 5 6 324.18 307.77 9.60 o
11 5 6 2.43 -3.95 9.87 <
13 5 6 0.47 -50.53 15.94 <
-14 6 6 10.54 -36.26 15.43 <
-12 6 6 92.07 86.74 9.70 o
-10 6 6 46.21 34.21 7.93 o
-8 6 6 17.63 16.45 7.30 o
-6 6 6 1101.78 1141.58 13.31 o
-4 6 6 189.72 194.74 7.23 o
-2 6 6 66.43 67.67 6.48 o
0 6 6 3.94 5.23 5.96 <
2 6 6 905.00 874.31 11.52 o
4 6 6 0.54 -11.73 6.47 <
6 6 6 30.43 29.06 7.19 o
8 6 6 5.83 -4.62 5.55 <
10 6 6 1.17 2.14 15.13 <
12 6 6 37.42 -14.77 14.88 <
-13 7 6 4.21 0.63 17.10 <
-11 7 6 18.48 21.15 11.37 <
-9 7 6 161.66 166.14 9.04 o
-7 7 6 1.35 -9.23 7.92 <
-5 7 6 107.06 91.33 7.71 o
-3 7 6 825.25 807.08 13.14 o
-1 7 6 869.75 824.01 15.05 o
1 7 6 818.26 797.30 14.35 o
3 7 6 77.83 90.41 7.75 o
5 7 6 164.67 163.77 7.84 o
7 7 6 549.60 482.63 10.15 o
9 7 6 54.06 54.13 15.92 o
11 7 6 19.28 30.95 16.42 <
13 7 6 90.86 79.29 22.59 o
-14 8 6 0.71 7.04 4.63 <
-12 8 6 44.87 44.83 24.26 <
-10 8 6 4.92 14.90 11.59 <
-8 8 6 155.59 150.35 11.00 o
-6 8 6 6.37 16.15 8.78 <
-4 8 6 31.92 44.90 10.14 o
-2 8 6 247.87 251.07 10.18 o
0 8 6 1772.32 1699.49 22.06 o
2 8 6 7.65 -6.33 10.36 <
4 8 6 92.17 76.73 9.00 o
6 8 6 23.30 24.86 8.35 o
8 8 6 6.71 23.80 10.88 o
10 8 6 9.18 -4.63 28.61 <
12 8 6 0.20 -0.48 21.36 <
-13 9 6 49.76 59.15 6.13 o
-11 9 6 59.99 38.28 17.81 o
-9 9 6 43.65 85.52 12.84 o
-7 9 6 5.36 -15.41 12.41 <
-5 9 6 2.78 25.89 8.41 o
-3 9 6 143.33 120.15 10.10 o
-1 9 6 64.05 56.57 10.08 o
1 9 6 419.21 350.73 14.06 o
3 9 6 22.42 20.69 10.36 <
5 9 6 109.09 133.82 9.20 o
7 9 6 58.35 24.16 13.04 <
9 9 6 11.07 44.99 31.76 <
11 9 6 4.42 4.96 18.86 <
-12 10 6 122.43 108.91 7.63 o
-10 10 6 28.56 34.56 10.40 o
-8 10 6 1.43 -1.13 14.97 <
-6 10 6 49.36 47.23 15.42 o
-4 10 6 100.51 52.00 13.09 o
-2 10 6 67.28 55.06 12.50 o
0 10 6 0.23 29.47 14.21 o
2 10 6 4.13 -2.87 12.03 <
4 10 6 516.31 490.51 14.03 o
6 10 6 21.32 -3.60 11.02 <
8 10 6 19.89 -33.16 24.77 <
10 10 6 0.93 -4.95 7.46 <
-11 11 6 7.73 17.69 7.32 o
-9 11 6 0.00 -16.47 14.20 <
-7 11 6 15.15 20.20 15.70 <
-5 11 6 37.53 -0.72 15.25 <
-3 11 6 3.69 -48.64 13.72 <
-1 11 6 54.23 60.01 16.53 o
1 11 6 65.09 26.12 18.83 <
3 11 6 84.43 50.61 14.37 o
5 11 6 0.05 -18.58 13.69 <
7 11 6 27.57 51.17 21.45 o
9 11 6 3.60 28.96 7.92 o
-10 12 6 2.21 -2.33 7.47 <
-8 12 6 5.40 -5.46 19.30 <
-6 12 6 47.43 13.52 18.65 <
-4 12 6 50.13 43.90 24.70 <
-2 12 6 13.66 12.39 20.57 <
0 12 6 0.61 14.31 22.54 <
2 12 6 316.16 356.61 25.35 o
4 12 6 6.85 -26.09 14.17 <
6 12 6 28.25 0.23 17.14 <
8 12 6 0.80 -8.55 7.91 <
-7 13 6 0.05 31.71 24.37 <
-5 13 6 9.93 -4.84 24.22 <
-3 13 6 0.41 -6.28 16.68 <
-1 13 6 2.59 -3.63 22.64 <
1 13 6 17.59 41.98 23.49 <
3 13 6 43.96 92.70 24.06 o
5 13 6 10.24 -7.75 22.15 <
7 13 6 1.16 3.42 8.10 <
-6 14 6 0.30 -59.47 21.67 <
-4 14 6 9.86 14.94 18.73 <
-2 14 6 7.38 25.01 5.53 o
0 14 6 17.11 14.04 4.98 o
2 14 6 1.46 40.30 30.06 <
4 14 6 11.81 19.56 30.26 <
-1 15 6 106.19 229.29 17.35 o
-15 1 7 29.40 12.55 9.08 <
-13 1 7 164.96 143.48 6.63 o
-11 1 7 28.44 11.30 5.77 <
-9 1 7 14.34 23.23 6.06 o
-7 1 7 320.62 309.23 5.90 o
-5 1 7 238.02 216.46 5.56 o
-3 1 7 675.24 642.77 8.81 o
-1 1 7 8.18 8.62 3.78 o
1 1 7 1202.45 1221.79 10.50 o
3 1 7 3.36 -2.31 3.99 <
5 1 7 71.13 84.48 4.07 o
7 1 7 691.74 694.03 8.08 o
9 1 7 592.23 582.92 7.16 o
11 1 7 296.81 307.71 5.33 o
13 1 7 10.83 17.74 6.45 o
-16 2 7 11.39 9.54 5.86 <
-14 2 7 300.36 331.36 8.84 o
-12 2 7 262.25 288.49 7.59 o
-10 2 7 0.00 1.54 5.42 <
-8 2 7 0.47 -0.83 4.85 <
-6 2 7 5079.49 5026.68 28.44 o
-4 2 7 1527.09 1587.46 12.79 o
-2 2 7 24.55 5.65 5.22 <
0 2 7 3717.73 3888.12 24.56 o
2 2 7 91.37 117.67 5.02 o
4 2 7 63.18 62.31 4.63 o
6 2 7 254.10 288.20 6.41 o
8 2 7 1036.07 1034.35 9.89 o
10 2 7 8.18 6.69 6.01 <
12 2 7 15.66 -8.10 9.98 <
14 2 7 3.28 -20.63 10.40 <
-15 3 7 51.98 27.76 13.91 <
-13 3 7 1688.14 1685.28 15.99 o
-11 3 7 398.20 349.65 7.25 o
-9 3 7 50.17 50.83 5.77 o
-7 3 7 957.69 964.34 10.27 o
-5 3 7 5228.77 5506.13 32.05 o
-3 3 7 7.19 4.02 5.55 <
-1 3 7 93.62 91.87 6.40 o
1 3 7 335.72 361.54 7.30 o
3 3 7 124.25 118.79 5.62 o
5 3 7 67.46 69.48 4.99 o
7 3 7 69.75 70.82 5.48 o
9 3 7 37.76 32.02 5.68 o
11 3 7 6.09 -0.89 12.27 <
13 3 7 5.67 23.50 5.31 o
-14 4 7 66.16 -15.16 13.38 <
-12 4 7 0.13 -9.09 7.95 <
-10 4 7 25.86 29.40 7.48 o
-8 4 7 116.69 93.73 6.71 o
-6 4 7 290.73 291.96 7.36 o
-4 4 7 2300.08 2298.23 19.87 o
-2 4 7 875.11 883.21 11.93 o
0 4 7 31.77 24.66 6.13 o
2 4 7 556.79 569.63 7.97 o
4 4 7 274.80 280.59 7.42 o
6 4 7 107.27 93.46 6.13 o
8 4 7 3.34 -9.94 5.52 <
10 4 7 34.57 21.59 8.86 o
12 4 7 63.81 107.56 17.58 o
-15 5 7 21.49 -12.57 20.56 <
-13 5 7 54.00 60.65 9.48 o
-11 5 7 2.19 -4.40 8.03 <
-9 5 7 5.83 6.02 6.68 <
-7 5 7 642.82 661.91 11.37 o
-5 5 7 1.46 0.62 6.71 <
-3 5 7 544.05 550.48 10.61 o
-1 5 7 693.08 760.15 11.47 o
1 5 7 0.77 -8.89 7.15 <
3 5 7 354.34 387.55 8.38 o
5 5 7 459.04 410.81 8.27 o
7 5 7 88.83 79.77 5.84 o
9 5 7 9.27 21.84 7.02 o
11 5 7 45.06 -13.10 15.96 <
13 5 7 0.16 -0.03 4.86 <
-14 6 7 1.18 36.89 22.31 <
-12 6 7 3.00 -17.06 9.76 <
-10 6 7 41.17 54.55 9.21 o
-8 6 7 0.14 -7.40 7.91 <
-6 6 7 137.99 116.98 8.46 o
-4 6 7 34.53 4.11 7.88 <
-2 6 7 113.08 94.23 8.29 o
0 6 7 54.85 34.91 6.99 o
2 6 7 447.86 469.47 9.75 o
4 6 7 445.92 451.46 9.25 o
6 6 7 209.53 189.68 8.76 o
8 6 7 1200.74 1127.21 12.82 o
10 6 7 8.60 7.27 10.93 <
12 6 7 7.12 10.33 18.55 <
-13 7 7 0.31 -16.14 19.11 <
-11 7 7 19.65 2.98 14.13 <
-9 7 7 120.97 137.88 10.33 o
-7 7 7 56.74 90.19 10.46 o
-5 7 7 0.16 6.11 6.87 <
-3 7 7 9.74 -3.62 8.81 <
-1 7 7 2861.56 2708.27 23.88 o
1 7 7 1588.77 1575.61 17.64 o
3 7 7 5.09 5.29 8.23 <
5 7 7 76.32 44.09 6.87 o
7 7 7 13.15 3.13 8.77 <
9 7 7 0.79 -2.48 8.68 <
11 7 7 18.46 -44.33 29.00 <
-12 8 7 4.80 52.95 30.55 <
-10 8 7 9.46 -0.52 12.49 <
-8 8 7 659.40 642.69 15.76 o
-6 8 7 88.36 55.36 9.68 o
-4 8 7 1.19 -8.74 9.41 <
-2 8 7 725.43 706.70 13.96 o
0 8 7 3464.96 3466.42 31.02 o
2 8 7 39.22 27.08 9.46 o
4 8 7 5.67 -14.25 9.53 <
6 8 7 226.73 188.93 10.47 o
8 8 7 57.59 -34.68 15.00 <
10 8 7 48.92 -40.94 23.50 <
12 8 7 7.47 16.46 23.60 <
-13 9 7 12.30 29.78 6.53 o
-11 9 7 7.41 20.31 23.11 <
-9 9 7 71.51 85.39 13.72 o
-7 9 7 36.62 0.17 17.48 <
-5 9 7 143.81 136.52 11.63 o
-3 9 7 63.13 52.86 11.63 o
-1 9 7 137.05 134.01 11.58 o
1 9 7 39.58 55.97 10.13 o
3 9 7 3.36 -11.30 11.38 <
5 9 7 13.06 39.60 11.96 o
7 9 7 11.21 -37.93 15.73 <
9 9 7 45.21 -57.09 35.84 <
11 9 7 7.74 -10.28 6.79 <
-12 10 7 67.70 68.24 10.02 o
-10 10 7 15.24 52.06 24.51 o
-8 10 7 9.51 -18.76 14.65 <
-6 10 7 94.67 96.57 12.77 o
-4 10 7 33.13 68.82 11.67 o
-2 10 7 48.97 21.39 16.88 <
0 10 7 17.53 -30.18 16.94 <
2 10 7 24.44 20.41 18.92 <
4 10 7 159.70 164.61 13.80 o
6 10 7 21.75 -34.84 19.91 <
8 10 7 34.04 20.77 31.26 <
10 10 7 0.08 -43.78 12.20 <
-11 11 7 4.67 -25.54 9.09 <
-9 11 7 40.17 10.17 16.25 <
-7 11 7 40.62 87.63 17.73 o
-5 11 7 416.15 447.76 22.89 o
-3 11 7 46.40 76.31 26.47 o
-1 11 7 25.68 81.64 22.42 o
1 11 7 985.71 939.86 23.13 o
3 11 7 350.89 313.97 15.73 o
5 11 7 29.59 46.75 13.47 o
7 11 7 113.04 156.84 6.49 o
9 11 7 13.89 15.43 7.47 o
-8 12 7 1.70 94.60 30.21 o
-6 12 7 36.81 2.05 18.45 <
-4 12 7 94.30 127.51 28.06 o
-2 12 7 13.68 104.66 27.69 o
0 12 7 41.21 46.26 48.24 <
2 12 7 744.88 864.43 32.37 o
4 12 7 108.97 130.57 14.63 o
6 12 7 51.15 85.05 27.59 o
-7 13 7 3.15 -49.08 34.34 <
-5 13 7 26.36 1.87 21.88 <
-3 13 7 1.86 -8.45 24.65 <
-1 13 7 69.36 23.66 18.36 <
1 13 7 169.63 229.45 24.64 o
3 13 7 11.54 -25.30 14.08 <
5 13 7 209.86 257.73 20.81 o
-4 14 7 2.56 3.27 5.49 <
-2 14 7 21.77 24.70 5.79 o
0 14 7 65.89 81.76 6.67 o
2 14 7 51.66 23.53 6.17 o
-16 0 8 31.88 38.24 9.17 o
-14 0 8 16.17 -25.80 14.07 <
-12 0 8 1.60 -14.18 12.13 <
-10 0 8 137.16 146.46 10.30 o
-8 0 8 288.05 273.38 9.53 o
-6 0 8 313.92 345.37 11.92 o
-4 0 8 3468.43 3687.87 36.68 o
-2 0 8 8007.07 7879.31 66.80 o
0 0 8 2878.73 3019.67 31.49 o
2 0 8 235.44 203.74 7.78 o
4 0 8 2.56 12.81 6.48 <
6 0 8 14461.27 14912.79 108.06 o
8 0 8 24.46 7.52 7.40 <
10 0 8 264.98 287.90 10.05 o
12 0 8 23.29 25.03 5.55 o
-15 1 8 13.11 3.74 13.73 <
-13 1 8 39.26 40.88 7.82 o
-11 1 8 2.79 15.13 5.78 o
-9 1 8 99.51 104.47 6.04 o
-7 1 8 6.18 -10.17 5.90 <
-5 1 8 83.89 110.20 6.25 o
-3 1 8 173.95 190.14 7.01 o
-1 1 8 245.79 290.90 6.70 o
1 1 8 185.69 204.59 5.81 o
3 1 8 260.50 249.24 6.56 o
5 1 8 101.95 122.23 5.54 o
7 1 8 1744.80 1786.21 14.07 o
9 1 8 89.16 67.04 5.08 o
11 1 8 67.96 79.51 5.04 o
-14 2 8 228.60 234.60 10.30 o
-12 2 8 146.93 149.23 8.42 o
-10 2 8 7.53 4.42 6.23 <
-8 2 8 1.98 24.06 6.52 o
-6 2 8 745.10 826.59 9.37 o
-4 2 8 582.69 614.57 9.20 o
-2 2 8 240.85 247.36 6.44 o
0 2 8 1655.47 1706.52 13.66 o
2 2 8 0.78 -1.20 5.49 <
4 2 8 36.22 30.25 5.65 o
6 2 8 331.51 295.73 6.64 o
8 2 8 50.75 51.21 5.51 o
10 2 8 48.71 64.89 7.44 o
12 2 8 18.29 27.54 16.62 <
-15 3 8 42.25 14.75 14.13 <
-13 3 8 264.77 251.25 10.08 o
-11 3 8 0.92 16.22 7.53 o
-9 3 8 13.18 29.63 6.90 o
-7 3 8 33.02 3.37 5.94 <
-5 3 8 96.87 99.36 5.99 o
-3 3 8 64.54 53.38 6.36 o
-1 3 8 4.04 25.74 6.37 o
1 3 8 406.70 423.49 7.95 o
3 3 8 0.86 -7.16 4.90 <
5 3 8 0.00 -7.47 5.69 <
7 3 8 101.06 71.74 6.12 o
9 3 8 114.57 119.73 7.96 o
11 3 8 28.25 41.11 14.24 o
13 3 8 0.01 10.49 9.71 <
-14 4 8 28.25 72.03 15.06 o
-12 4 8 2.13 20.21 7.30 o
-10 4 8 5.61 21.67 7.91 o
-8 4 8 423.31 422.06 9.45 o
-6 4 8 326.43 342.85 8.04 o
-4 4 8 4.14 4.23 7.70 <
-2 4 8 136.08 145.45 7.08 o
0 4 8 58.67 46.27 7.36 o
2 4 8 19.76 20.52 5.49 o
4 4 8 310.84 307.33 8.39 o
6 4 8 0.01 -4.17 7.21 <
8 4 8 1.93 3.94 7.07 <
10 4 8 15.06 17.18 7.58 o
12 4 8 8.66 -15.46 18.66 <
-15 5 8 4.67 -66.55 20.19 <
-13 5 8 0.28 -11.91 10.69 <
-11 5 8 4.60 7.04 8.80 <
-9 5 8 6.79 -13.44 8.07 <
-7 5 8 3282.52 3178.38 25.33 o
-5 5 8 78.70 48.09 8.92 o
-3 5 8 95.79 103.53 8.78 o
-1 5 8 0.06 -34.04 8.45 <
1 5 8 1857.60 1944.70 19.08 o
3 5 8 87.65 72.66 7.16 o
5 5 8 281.93 262.06 8.93 o
7 5 8 479.76 473.47 9.26 o
9 5 8 202.20 211.15 9.25 o
11 5 8 124.49 155.33 13.52 o
13 5 8 37.29 36.59 5.79 o
-14 6 8 7.17 -0.39 27.85 <
-12 6 8 33.38 -30.25 13.43 <
-10 6 8 29.10 40.61 11.57 o
-8 6 8 236.86 199.53 9.33 o
-6 6 8 1148.54 1178.23 16.06 o
-4 6 8 184.16 203.97 8.91 o
-2 6 8 143.10 158.21 8.20 o
0 6 8 1283.76 1380.18 16.51 o
2 6 8 65.27 108.98 9.08 o
4 6 8 33.43 73.20 7.90 o
6 6 8 140.49 146.84 9.76 o
8 6 8 353.34 313.70 10.20 o
10 6 8 3.75 -31.69 19.05 <
12 6 8 0.50 -34.58 23.16 <
-13 7 8 0.07 -49.54 21.62 <
-11 7 8 0.17 -48.98 14.93 <
-9 7 8 10.35 21.35 13.47 <
-7 7 8 332.76 340.17 12.01 o
-5 7 8 2.98 0.41 9.63 <
-3 7 8 25.20 11.09 9.05 <
-1 7 8 3019.55 3025.56 27.03 o
1 7 8 0.40 -15.55 8.68 <
3 7 8 1.72 15.06 8.59 <
5 7 8 90.36 50.92 9.00 o
7 7 8 1815.90 1627.45 21.08 o
9 7 8 4.53 -3.31 13.91 <
11 7 8 9.84 -73.88 26.44 <
-12 8 8 2.68 -44.02 25.70 <
-10 8 8 11.90 4.96 14.82 <
-8 8 8 851.98 808.98 19.58 o
-6 8 8 47.64 19.00 10.45 <
-4 8 8 0.00 -10.86 10.87 <
-2 8 8 1157.84 1147.47 17.10 o
0 8 8 2503.76 2472.57 26.25 o
2 8 8 18.99 -20.24 9.10 <
4 8 8 2.31 -4.07 9.28 <
6 8 8 1.68 11.47 13.75 <
8 8 8 5.56 -11.40 14.06 <
10 8 8 13.76 -24.10 17.41 <
-11 9 8 11.32 13.79 5.91 o
-9 9 8 18.72 -45.40 17.44 <
-7 9 8 80.18 40.89 16.19 o
-5 9 8 22.23 -15.14 15.40 <
-3 9 8 20.79 38.91 12.08 o
-1 9 8 19.00 2.38 12.18 <
1 9 8 22.81 60.20 11.60 o
3 9 8 140.55 179.19 12.31 o
5 9 8 17.63 16.03 12.61 <
7 9 8 2.06 3.71 16.52 <
9 9 8 14.48 86.92 33.95 o
-10 10 8 33.51 76.76 20.45 o
-8 10 8 19.52 93.54 21.05 o
-6 10 8 157.49 203.45 17.06 o
-4 10 8 1.66 -4.13 19.55 <
-2 10 8 9.84 30.27 21.16 <
0 10 8 1.31 42.72 15.22 o
2 10 8 49.41 85.70 16.37 o
4 10 8 13.94 84.75 16.02 o
6 10 8 68.25 64.92 17.70 o
8 10 8 16.84 45.66 7.25 o
-9 11 8 4.04 14.64 14.66 <
-7 11 8 24.66 70.15 19.99 o
-5 11 8 73.94 39.08 32.88 <
-3 11 8 0.00 -73.62 23.18 <
-1 11 8 1.90 40.02 22.54 <
1 11 8 994.49 1069.99 24.79 o
3 11 8 267.47 298.87 16.53 o
5 11 8 0.54 6.32 12.64 <
7 11 8 4.46 -31.76 5.94 <
-8 12 8 15.56 -19.12 19.51 <
-6 12 8 29.44 -64.01 31.39 <
-4 12 8 4.12 -17.02 26.71 <
-2 12 8 13.06 0.51 28.95 <
0 12 8 1.52 14.72 26.96 <
2 12 8 541.63 575.14 25.12 o
4 12 8 13.13 1.02 15.92 <
6 12 8 26.86 39.19 4.96 o
-7 13 8 1.60 -37.72 28.94 <
-5 13 8 5.17 32.12 27.78 <
-3 13 8 64.51 80.01 6.90 o
-1 13 8 349.10 408.90 10.90 o
1 13 8 43.18 5.66 41.70 <
3 13 8 78.69 15.81 26.72 <
5 13 8 36.08 35.98 7.06 o
-2 14 8 68.05 100.11 7.36 o
0 14 8 11.42 28.12 6.28 o
-15 1 9 490.84 490.01 15.89 o
-13 1 9 30.46 39.55 11.07 o
-11 1 9 1.24 2.31 7.94 <
-9 1 9 924.07 909.50 11.91 o
-7 1 9 723.34 709.51 10.23 o
-5 1 9 33.39 48.25 7.23 o
-3 1 9 877.50 907.79 12.01 o
-1 1 9 3474.72 3744.62 25.49 o
1 1 9 28.66 35.20 6.34 o
3 1 9 132.31 131.73 6.83 o
5 1 9 3413.94 3411.50 22.50 o
7 1 9 1761.07 1754.23 14.40 o
9 1 9 6.12 -3.84 6.08 <
11 1 9 22.70 21.45 12.92 <
13 1 9 105.80 94.57 15.80 o
-14 2 9 4.81 15.45 9.76 <
-12 2 9 20.98 33.07 9.19 o
-10 2 9 0.37 4.85 6.51 <
-8 2 9 78.62 72.80 7.08 o
-6 2 9 1.00 10.73 7.38 <
-4 2 9 504.39 495.80 8.56 o
-2 2 9 625.40 671.79 10.04 o
0 2 9 141.94 145.21 6.11 o
2 2 9 0.04 -10.38 6.02 <
4 2 9 90.86 92.84 6.51 o
6 2 9 420.73 435.26 8.32 o
8 2 9 243.57 276.17 8.28 o
10 2 9 96.19 62.35 8.56 o
12 2 9 0.21 -21.91 7.04 <
-15 3 9 24.12 20.62 15.57 <
-13 3 9 73.35 58.38 12.12 o
-11 3 9 12.34 3.59 7.61 <
-9 3 9 28.15 4.97 7.37 <
-7 3 9 258.40 266.22 7.96 o
-5 3 9 0.22 24.52 6.14 o
-3 3 9 31.55 46.86 7.37 o
-1 3 9 19.78 22.19 6.94 o
1 3 9 54.34 65.08 7.10 o
3 3 9 86.60 74.51 5.76 o
5 3 9 561.93 544.26 9.36 o
7 3 9 20.81 25.38 5.69 o
9 3 9 70.33 66.76 7.47 o
11 3 9 1.06 32.12 15.32 o
-14 4 9 22.07 37.43 17.97 o
-12 4 9 3.61 -29.67 12.04 <
-10 4 9 0.15 2.89 9.36 <
-8 4 9 26.38 22.20 8.08 o
-6 4 9 23.45 -0.92 8.16 <
-4 4 9 90.14 77.54 8.22 o
-2 4 9 31.92 55.37 8.28 o
0 4 9 137.00 135.44 8.23 o
2 4 9 213.27 213.17 8.77 o
4 4 9 16.43 24.37 8.55 o
6 4 9 43.79 46.27 7.66 o
8 4 9 14.94 31.37 7.16 o
10 4 9 126.63 149.42 13.52 o
12 4 9 106.68 148.74 9.30 o
-13 5 9 194.54 145.70 15.82 o
-11 5 9 42.12 11.05 10.53 <
-9 5 9 96.72 63.39 8.96 o
-7 5 9 2175.55 2219.98 20.82 o
-5 5 9 844.13 862.94 14.37 o
-3 5 9 338.23 357.81 11.05 o
-1 5 9 2.70 22.30 10.55 o
1 5 9 160.55 184.21 8.57 o
3 5 9 5.45 10.79 7.65 <
5 5 9 220.00 162.81 8.72 o
7 5 9 242.80 244.13 10.76 o
9 5 9 8.90 27.39 14.73 <
11 5 9 209.85 335.39 27.53 o
-14 6 9 24.61 -10.63 26.61 <
-12 6 9 0.94 4.82 15.14 <
-10 6 9 5.72 -6.43 12.36 <
-8 6 9 481.56 503.97 13.22 o
-6 6 9 799.45 749.11 14.30 o
-4 6 9 387.33 395.10 12.48 o
-2 6 9 1428.12 1389.93 17.56 o
0 6 9 832.35 920.39 14.27 o
2 6 9 300.09 308.32 10.32 o
4 6 9 122.72 110.40 7.22 o
6 6 9 125.29 121.73 8.16 o
8 6 9 127.57 102.64 10.72 o
10 6 9 3.90 -54.54 27.48 <
-13 7 9 18.47 5.14 16.57 <
-11 7 9 20.37 -47.51 19.55 <
-9 7 9 0.78 4.10 13.21 <
-7 7 9 445.56 438.44 15.57 o
-5 7 9 2.25 26.19 11.01 o
-3 7 9 825.99 803.72 15.12 o
-1 7 9 417.98 427.90 12.84 o
1 7 9 458.27 492.97 13.18 o
3 7 9 158.20 181.39 8.96 o
5 7 9 68.80 68.40 9.59 o
7 7 9 85.27 109.66 14.06 o
9 7 9 4.86 -19.29 17.21 <
11 7 9 26.38 9.42 17.87 <
-12 8 9 8.07 -5.31 4.91 <
-10 8 9 7.57 39.99 20.97 <
-8 8 9 1.68 -43.22 14.55 <
-6 8 9 11.30 13.98 15.86 <
-4 8 9 52.95 53.04 11.66 o
-2 8 9 39.13 37.56 11.48 o
0 8 9 61.48 69.32 10.80 o
2 8 9 2.69 36.73 12.47 o
4 8 9 0.03 -1.10 11.58 <
6 8 9 84.75 103.31 15.84 o
8 8 9 58.31 34.71 14.72 o
10 8 9 2.75 -42.55 23.62 <
-11 9 9 12.42 1.29 5.85 <
-9 9 9 1.53 11.10 19.81 <
-7 9 9 14.87 -19.45 21.29 <
-5 9 9 26.05 17.70 21.50 <
-3 9 9 32.49 90.73 18.33 o
-1 9 9 166.61 150.11 17.64 o
1 9 9 35.95 47.69 12.17 o
3 9 9 21.17 14.36 13.13 <
5 9 9 0.51 8.42 14.59 <
7 9 9 8.85 4.99 18.82 <
9 9 9 0.05 -1.86 6.73 <
-10 10 9 3.10 -28.29 20.92 <
-8 10 9 85.38 58.52 14.78 o
-6 10 9 0.12 33.90 24.59 <
-4 10 9 0.23 -13.23 21.88 <
-2 10 9 15.87 57.45 21.50 o
0 10 9 24.00 -19.47 18.50 <
2 10 9 33.62 99.47 19.02 o
4 10 9 0.73 -68.58 16.66 <
6 10 9 0.02 12.00 20.13 <
8 10 9 0.00 21.32 7.49 o
-9 11 9 0.01 12.43 23.54 <
-7 11 9 18.54 -10.50 22.13 <
-5 11 9 114.82 128.19 26.08 o
-3 11 9 16.90 -24.48 26.72 <
-1 11 9 0.48 23.30 21.69 <
1 11 9 42.06 84.29 22.19 o
3 11 9 84.90 59.37 19.39 o
5 11 9 6.86 -9.06 20.09 <
-8 12 9 2.91 13.41 27.89 <
-6 12 9 19.00 -12.99 19.25 <
-4 12 9 29.63 40.68 25.76 <
-2 12 9 179.67 241.99 27.03 o
0 12 9 4.25 13.97 24.74 <
2 12 9 67.15 22.37 26.90 <
4 12 9 6.90 100.79 33.32 o
-5 13 9 0.05 -1.38 9.35 <
-3 13 9 50.33 83.85 6.87 o
-1 13 9 1.35 5.43 6.19 <
1 13 9 28.45 40.79 6.79 o
3 13 9 43.25 -59.16 48.57 <
-14 0 10 358.42 348.60 25.23 o
-12 0 10 18.47 44.66 15.82 o
-10 0 10 19.95 -5.94 14.14 <
-8 0 10 3306.04 3537.31 35.92 o
-6 0 10 89.41 91.34 13.18 o
-4 0 10 93.65 109.77 12.77 o
-2 0 10 6415.38 6737.53 61.29 o
0 0 10 333.69 402.13 14.27 o
2 0 10 6.09 4.87 8.46 <
4 0 10 1187.81 1282.49 18.27 o
6 0 10 4438.78 4475.67 40.01 o
8 0 10 278.77 302.88 11.79 o
10 0 10 50.18 75.60 17.80 o
12 0 10 1.11 36.46 13.82 o
-15 1 10 110.49 105.57 5.81 o
-13 1 10 28.46 9.62 11.28 <
-11 1 10 37.87 37.40 10.42 o
-9 1 10 16.14 14.55 7.85 <
-7 1 10 42.84 72.08 9.65 o
-5 1 10 26.77 24.80 7.82 o
-3 1 10 63.78 78.63 7.68 o
-1 1 10 2.39 3.54 6.28 <
1 1 10 0.00 19.51 7.09 o
3 1 10 294.20 272.15 8.00 o
5 1 10 768.45 760.79 10.65 o
7 1 10 528.58 546.90 10.33 o
9 1 10 138.80 161.32 9.19 o
11 1 10 6.65 19.61 19.72 <
-14 2 10 11.51 -37.34 15.00 <
-12 2 10 2.00 -10.31 11.09 <
-10 2 10 26.89 36.78 8.33 o
-8 2 10 59.35 82.39 9.30 o
-6 2 10 207.59 209.47 8.49 o
-4 2 10 90.60 83.28 8.58 o
-2 2 10 73.30 91.89 8.37 o
0 2 10 194.77 187.16 7.65 o
2 2 10 189.54 176.70 7.18 o
4 2 10 519.89 530.05 9.21 o
6 2 10 15.05 22.76 7.26 o
8 2 10 210.35 221.45 7.27 o
10 2 10 0.34 -11.87 11.47 <
12 2 10 4.38 11.72 13.63 <
-13 3 10 0.00 -62.03 14.17 <
-11 3 10 8.08 0.10 10.59 <
-9 3 10 0.64 4.48 8.98 <
-7 3 10 50.93 42.44 8.67 o
-5 3 10 13.50 15.08 9.19 <
-3 3 10 73.48 68.08 7.74 o
-1 3 10 132.74 115.88 8.02 o
1 3 10 0.14 -2.75 6.83 <
3 3 10 15.75 2.39 7.73 <
5 3 10 152.02 160.41 8.02 o
7 3 10 19.52 17.17 6.81 o
9 3 10 0.10 -14.40 8.75 <
11 3 10 4.36 12.96 22.76 <
-14 4 10 13.92 -43.87 26.87 <
-12 4 10 0.03 22.84 12.74 <
-10 4 10 13.91 31.21 10.14 o
-8 4 10 19.67 11.91 9.25 <
-6 4 10 202.76 204.53 8.78 o
-4 4 10 349.96 321.19 10.13 o
-2 4 10 150.63 156.98 9.24 o
0 4 10 49.67 37.11 8.90 o
2 4 10 7.48 41.16 8.20 o
4 4 10 54.24 46.37 8.25 o
6 4 10 31.62 30.57 8.28 o
8 4 10 88.95 61.52 9.59 o
10 4 10 0.56 -0.69 12.13 <
-13 5 10 15.48 1.63 17.36 <
-11 5 10 91.16 76.47 13.83 o
-9 5 10 62.60 66.90 10.47 o
-7 5 10 614.53 674.43 13.95 o
-5 5 10 7.12 13.79 11.87 <
-3 5 10 2621.51 2587.03 24.99 o
-1 5 10 323.86 356.10 11.22 o
1 5 10 0.65 5.64 8.80 <
3 5 10 0.00 -21.02 9.27 <
5 5 10 812.06 721.63 13.29 o
7 5 10 8.00 8.27 10.17 <
9 5 10 0.00 34.23 17.76 <
11 5 10 183.52 237.56 30.53 o
-12 6 10 0.37 -15.47 22.01 <
-10 6 10 742.16 723.04 18.33 o
-8 6 10 3.08 23.48 12.53 <
-6 6 10 226.24 181.82 11.46 o
-4 6 10 2149.86 2209.48 23.66 o
-2 6 10 3680.34 3635.13 31.04 o
0 6 10 130.76 129.50 11.24 o
2 6 10 100.32 91.96 9.76 o
4 6 10 294.24 211.36 9.92 o
6 6 10 197.17 177.87 9.76 o
8 6 10 0.11 -3.59 16.81 <
10 6 10 57.63 81.79 32.18 o
-13 7 10 0.05 13.29 7.46 <
-11 7 10 63.72 43.67 16.24 o
-9 7 10 18.30 -3.91 15.88 <
-7 7 10 5.07 41.48 15.64 o
-5 7 10 7.03 4.39 13.23 <
-3 7 10 127.12 97.14 11.67 o
-1 7 10 95.24 94.08 11.35 o
1 7 10 69.96 62.58 10.47 o
3 7 10 40.02 28.85 9.90 o
5 7 10 321.54 294.91 14.83 o
7 7 10 0.70 22.12 13.94 <
9 7 10 42.67 55.62 30.46 <
-12 8 10 23.09 27.60 6.13 o
-10 8 10 34.09 72.92 22.77 o
-8 8 10 2.59 29.10 23.13 <
-6 8 10 11.61 42.09 18.10 o
-4 8 10 60.52 88.03 15.85 o
-2 8 10 50.43 28.26 14.09 o
0 8 10 103.36 78.56 14.79 o
2 8 10 135.14 168.75 14.30 o
4 8 10 80.13 81.99 12.84 o
6 8 10 98.96 167.56 18.41 o
8 8 10 10.01 15.61 18.29 <
-11 9 10 16.87 -4.87 7.08 <
-9 9 10 2.22 -54.78 23.68 <
-7 9 10 8.84 -46.95 25.65 <
-5 9 10 1.88 -45.95 23.55 <
-3 9 10 5.35 -19.25 17.04 <
-1 9 10 3.34 -22.50 21.32 <
1 9 10 20.18 22.54 20.29 <
3 9 10 9.15 33.60 13.03 o
5 9 10 380.57 368.58 18.07 o
7 9 10 0.00 -5.13 14.23 <
-10 10 10 1.20 58.47 28.52 o
-8 10 10 0.03 25.80 22.88 <
-6 10 10 22.91 13.61 28.92 <
-4 10 10 47.94 52.43 25.43 o
-2 10 10 7.88 -1.16 20.74 <
0 10 10 1.98 -44.20 22.87 <
2 10 10 19.04 -39.36 24.83 <
4 10 10 50.26 52.72 20.37 o
6 10 10 0.04 26.19 26.19 <
-9 11 10 2.09 -21.72 30.01 <
-7 11 10 5.59 -26.84 23.89 <
-5 11 10 27.80 37.39 31.28 <
-3 11 10 28.77 18.31 27.13 <
-1 11 10 21.83 99.09 25.48 o
1 11 10 12.86 95.52 33.89 o
3 11 10 204.99 253.30 25.25 o
5 11 10 2.41 -23.50 32.66 <
-6 12 10 36.43 77.42 8.68 o
-4 12 10 111.49 122.34 7.45 o
-2 12 10 34.41 25.42 5.74 o
0 12 10 11.28 28.66 6.10 o
2 12 10 168.37 325.02 30.08 o
4 12 10 9.30 52.04 37.26 <
-3 13 10 17.49 36.58 10.43 o
-1 13 10 447.48 419.14 11.57 o
1 13 10 87.62 78.60 6.60 o
-13 1 11 6.23 16.05 16.56 <
-11 1 11 40.50 20.00 13.26 <
-9 1 11 74.83 59.23 10.42 o
-7 1 11 50.03 53.07 9.63 o
-5 1 11 15.41 2.26 11.01 <
-3 1 11 237.70 192.11 9.08 o
-1 1 11 38.76 41.10 8.92 o
1 1 11 0.02 1.56 9.02 <
3 1 11 874.83 871.41 12.66 o
5 1 11 29.24 25.39 10.04 o
7 1 11 64.14 84.83 8.84 o
9 1 11 2.59 0.74 11.71 <
11 1 11 27.13 15.09 6.79 o
-14 2 11 1.67 -36.66 17.91 <
-12 2 11 0.08 -4.46 15.82 <
-10 2 11 13.15 12.67 12.84 <
-8 2 11 68.88 66.52 9.65 o
-6 2 11 50.70 40.68 9.13 o
-4 2 11 616.14 602.37 12.18 o
-2 2 11 21.16 -9.80 9.70 <
0 2 11 3.89 -19.99 9.31 <
2 2 11 144.10 158.53 8.96 o
4 2 11 2082.34 2238.63 19.27 o
6 2 11 0.74 -3.85 8.92 <
8 2 11 161.26 177.79 9.96 o
10 2 11 79.69 211.73 20.46 o
-13 3 11 2.59 -18.16 18.64 <
-11 3 11 53.16 61.76 12.53 o
-9 3 11 22.72 -0.28 12.89 <
-7 3 11 234.30 237.00 9.26 o
-5 3 11 78.75 77.47 10.46 o
-3 3 11 2.52 2.87 10.51 <
-1 3 11 81.67 83.43 8.91 o
1 3 11 331.72 335.54 9.62 o
3 3 11 779.02 831.42 12.02 o
5 3 11 308.02 293.92 9.21 o
7 3 11 169.90 169.58 8.65 o
9 3 11 210.39 277.42 14.29 o
11 3 11 5.62 -28.47 6.64 <
-12 4 11 1.67 20.75 17.60 <
-10 4 11 1.09 25.02 15.25 <
-8 4 11 18.63 27.13 14.62 <
-6 4 11 27.98 29.50 10.45 o
-4 4 11 92.99 73.44 10.32 o
-2 4 11 36.67 26.78 8.19 o
0 4 11 105.60 89.30 7.24 o
2 4 11 0.53 -21.62 8.30 <
4 4 11 498.28 514.96 12.58 o
6 4 11 73.11 62.86 10.10 o
8 4 11 0.01 -8.23 11.42 <
10 4 11 10.38 80.62 29.22 o
-13 5 11 15.17 -44.70 21.19 <
-11 5 11 13.60 -8.15 18.42 <
-9 5 11 28.94 49.49 13.23 o
-7 5 11 80.55 92.91 16.38 o
-5 5 11 90.67 110.07 12.46 o
-3 5 11 1124.73 1052.22 17.17 o
-1 5 11 68.49 66.95 10.10 o
1 5 11 18.06 -14.21 10.38 <
3 5 11 2.91 -5.05 8.99 <
5 5 11 414.49 363.47 12.75 o
7 5 11 1.72 19.47 15.08 <
9 5 11 4.84 -11.90 21.39 <
-12 6 11 1.33 -19.81 23.56 <
-10 6 11 0.42 35.40 22.66 <
-8 6 11 4.34 25.31 17.64 <
-6 6 11 3.62 23.51 17.27 <
-4 6 11 498.09 483.16 16.30 o
-2 6 11 742.95 712.21 16.04 o
0 6 11 12.85 34.59 10.50 o
2 6 11 1.73 20.14 10.39 <
4 6 11 88.55 64.47 12.84 o
6 6 11 52.09 52.95 13.63 o
8 6 11 5.86 -21.00 20.91 <
10 6 11 2.92 14.63 34.54 <
-11 7 11 129.08 158.60 20.70 o
-9 7 11 1052.70 754.37 29.52 o
-7 7 11 166.07 158.38 19.39 o
-5 7 11 61.97 112.68 22.24 o
-3 7 11 172.13 161.43 18.32 o
-1 7 11 117.13 142.35 15.77 o
1 7 11 43.09 93.10 14.15 o
3 7 11 0.03 -1.15 12.70 <
5 7 11 308.35 335.96 15.54 o
7 7 11 0.03 33.98 17.81 <
9 7 11 2.00 21.17 8.18 o
-10 8 11 213.87 340.96 25.64 o
-8 8 11 164.55 36.09 23.20 <
-6 8 11 25.56 -45.47 24.25 <
-4 8 11 62.98 21.30 22.90 <
-2 8 11 439.58 480.66 22.78 o
0 8 11 5.31 -61.15 18.49 <
2 8 11 64.62 89.90 15.29 o
4 8 11 389.85 458.06 18.29 o
6 8 11 93.80 85.09 23.38 o
8 8 11 0.43 6.09 7.23 <
-9 9 11 125.32 86.99 27.67 o
-7 9 11 36.27 19.80 25.79 <
-5 9 11 28.29 -26.62 26.24 <
-3 9 11 15.68 -6.75 22.60 <
-1 9 11 14.97 13.20 19.49 <
1 9 11 19.73 22.67 23.22 <
3 9 11 2.87 -73.52 20.13 <
5 9 11 186.81 229.67 29.00 o
7 9 11 1.20 5.81 5.17 <
-8 10 11 0.06 10.48 25.84 <
-6 10 11 1.54 126.17 29.92 o
-4 10 11 36.30 79.88 27.66 o
-2 10 11 146.26 181.46 23.46 o
0 10 11 0.03 -63.34 25.63 <
2 10 11 30.44 59.74 26.41 o
4 10 11 4.08 5.31 29.04 <
6 10 11 5.98 -24.31 6.93 <
-7 11 11 18.38 1.13 7.86 <
-5 11 11 70.47 94.84 7.25 o
-3 11 11 165.53 194.66 8.15 o
-1 11 11 8.09 15.47 5.88 o
1 11 11 160.48 105.47 25.95 o
3 11 11 133.36 133.12 31.25 o
-4 12 11 86.84 114.16 8.23 o
-2 12 11 7.38 37.94 7.24 o
0 12 11 21.65 19.64 6.89 o
2 12 11 49.86 132.29 10.90 o
-14 0 12 0.86 -80.74 32.79 <
-12 0 12 90.69 5.65 24.93 <
-10 0 12 29.84 44.13 21.55 o
-8 0 12 5.95 -16.40 17.74 <
-6 0 12 106.89 53.48 19.32 o
-4 0 12 10.97 34.19 13.79 o
-2 0 12 97.44 133.01 14.05 o
0 0 12 17.65 8.10 12.42 <
2 0 12 22.73 24.83 13.20 <
4 0 12 50.06 55.11 12.62 o
6 0 12 8.66 -6.16 11.49 <
8 0 12 27.72 26.23 12.77 o
10 0 12 6.83 -13.28 6.51 <
-13 1 12 14.22 -33.66 19.43 <
-11 1 12 214.49 213.69 18.08 o
-9 1 12 132.44 99.22 12.78 o
-7 1 12 27.81 9.79 11.15 <
-5 1 12 206.63 212.65 11.33 o
-3 1 12 682.84 711.83 14.09 o
-1 1 12 15.11 22.86 8.46 o
1 1 12 17.40 51.77 10.07 o
3 1 12 178.29 159.48 8.93 o
5 1 12 0.29 11.10 9.49 <
7 1 12 38.88 43.60 11.36 o
9 1 12 37.64 -10.09 20.23 <
-12 2 12 10.86 -8.84 17.71 <
-10 2 12 205.17 196.60 15.87 o
-8 2 12 56.32 26.19 15.50 <
-6 2 12 78.91 95.93 10.19 o
-4 2 12 1053.14 1106.07 16.58 o
-2 2 12 137.57 125.68 8.81 o
0 2 12 96.36 89.86 8.88 o
2 2 12 938.48 967.66 14.09 o
4 2 12 2662.82 2766.91 23.49 o
6 2 12 1.52 -21.28 10.28 <
8 2 12 21.83 43.00 15.58 o
10 2 12 0.16 115.04 38.18 o
-13 3 12 15.15 -65.75 23.53 <
-11 3 12 57.77 93.89 17.89 o
-9 3 12 7.87 1.95 17.08 <
-7 3 12 0.01 -0.58 16.56 <
-5 3 12 52.74 62.65 10.95 o
-3 3 12 53.60 50.59 10.45 o
-1 3 12 1.69 16.13 10.16 <
1 3 12 27.63 -3.35 8.69 <
3 3 12 298.24 314.41 10.80 o
5 3 12 210.69 214.46 10.29 o
7 3 12 13.09 21.08 15.46 <
9 3 12 357.15 399.51 23.68 o
-12 4 12 11.88 20.89 19.78 <
-10 4 12 1.42 12.95 20.21 <
-8 4 12 3.00 66.97 16.53 o
-6 4 12 644.58 635.78 17.73 o
-4 4 12 1348.22 1386.93 19.95 o
-2 4 12 0.11 -11.68 9.87 <
0 4 12 45.47 59.54 8.97 o
2 4 12 538.08 458.91 12.19 o
4 4 12 369.74 344.45 12.21 o
6 4 12 51.40 36.15 14.83 o
8 4 12 199.35 284.77 21.25 o
10 4 12 15.99 32.69 29.63 <
-11 5 12 9.38 -16.79 22.09 <
-9 5 12 98.29 95.80 20.14 o
-7 5 12 3.45 92.61 18.49 o
-5 5 12 477.99 529.93 24.39 o
-3 5 12 105.42 110.64 14.25 o
-1 5 12 0.26 16.03 12.29 <
1 5 12 0.95 7.40 11.15 <
3 5 12 68.92 67.73 12.62 o
5 5 12 17.85 86.02 16.57 o
7 5 12 26.30 18.60 18.50 <
9 5 12 27.17 10.96 33.43 <
-12 6 12 2.19 -72.81 31.14 <
-10 6 12 270.86 349.82 27.83 o
-8 6 12 52.94 80.84 26.41 o
-6 6 12 4.49 -106.74 20.94 <
-4 6 12 138.06 152.18 16.59 o
-2 6 12 8.93 1.06 15.59 <
0 6 12 54.75 73.32 15.09 o
2 6 12 3.62 -14.95 13.38 <
4 6 12 16.03 -21.92 12.61 <
6 6 12 0.46 -13.62 17.07 <
8 6 12 5.11 1.48 34.00 <
-11 7 12 23.26 47.39 28.11 <
-9 7 12 316.26 242.76 27.92 o
-7 7 12 24.18 -8.10 26.87 <
-5 7 12 14.84 34.99 26.84 <
-3 7 12 428.83 442.54 21.69 o
-1 7 12 111.66 105.08 18.03 o
1 7 12 0.75 68.59 16.77 o
3 7 12 24.24 12.56 17.12 <
5 7 12 8.16 -53.85 21.28 <
7 7 12 0.96 -47.51 17.08 <
-10 8 12 25.01 23.90 34.89 <
-8 8 12 170.97 146.31 29.35 o
-6 8 12 14.93 -8.75 27.01 <
-4 8 12 54.87 -24.70 25.50 <
-2 8 12 65.28 -12.38 22.03 <
0 8 12 32.13 55.24 19.45 o
2 8 12 0.09 32.48 19.77 <
4 8 12 134.85 104.66 24.48 o
6 8 12 83.12 50.88 21.50 o
-9 9 12 43.52 -56.00 29.97 <
-7 9 12 1.23 8.49 18.88 <
-5 9 12 70.92 51.43 24.84 o
-3 9 12 19.95 -162.55 47.71 <
-1 9 12 48.67 6.85 21.93 <
1 9 12 59.71 65.99 18.91 o
3 9 12 0.00 5.66 20.52 <
5 9 12 2.97 6.61 31.45 <
-8 10 12 3.40 -3.95 7.03 <
-6 10 12 21.79 22.15 6.94 o
-4 10 12 33.41 39.60 6.56 o
-2 10 12 0.15 -11.28 5.83 <
0 10 12 5.24 5.16 24.62 <
2 10 12 16.22 51.18 27.09 <
4 10 12 0.33 62.76 34.45 <
-5 11 12 56.14 57.50 6.96 o
-3 11 12 80.22 97.16 8.17 o
-1 11 12 32.76 38.15 6.90 o
1 11 12 0.91 -12.27 5.96 <
-13 1 13 0.01 -78.43 21.90 <
-11 1 13 59.94 67.48 20.08 o
-9 1 13 0.52 -26.69 15.86 <
-7 1 13 10.95 -1.32 14.75 <
-5 1 13 177.93 222.14 18.58 o
-3 1 13 1.59 13.16 11.21 <
-1 1 13 52.05 61.28 10.97 o
1 1 13 84.12 79.60 11.12 o
3 1 13 102.65 113.92 10.51 o
5 1 13 280.45 276.98 13.18 o
7 1 13 20.99 23.74 15.94 <
9 1 13 0.19 17.23 23.90 <
-12 2 13 17.52 51.60 22.88 o
-10 2 13 145.85 119.47 18.87 o
-8 2 13 25.76 67.42 16.63 o
-6 2 13 375.60 459.40 21.94 o
-4 2 13 182.66 178.39 15.99 o
-2 2 13 99.62 98.71 16.28 o
0 2 13 0.40 27.42 12.24 o
2 2 13 0.81 -13.63 10.96 <
4 2 13 613.66 626.34 14.43 o
6 2 13 6.45 33.03 13.58 o
8 2 13 46.70 43.74 23.77 <
-11 3 13 33.63 6.20 21.26 <
-9 3 13 3.68 -63.58 20.02 <
-7 3 13 0.76 75.94 18.90 o
-5 3 13 934.39 971.14 25.70 o
-3 3 13 61.58 40.95 20.52 <
-1 3 13 32.02 54.96 13.50 o
1 3 13 106.57 109.23 11.66 o
3 3 13 1327.56 1310.41 20.21 o
5 3 13 5.10 -14.67 14.33 <
7 3 13 88.91 129.97 19.78 o
9 3 13 174.04 342.37 32.79 o
-12 4 13 95.72 73.54 23.57 o
-10 4 13 9.46 140.20 24.60 o
-8 4 13 48.23 72.54 21.90 o
-6 4 13 1171.65 1177.66 31.92 o
-4 4 13 1201.90 1356.60 30.16 o
-2 4 13 23.92 77.32 17.68 o
0 4 13 78.24 60.47 12.38 o
2 4 13 958.76 881.76 18.05 o
4 4 13 12.55 31.05 14.42 o
6 4 13 80.19 105.16 19.92 o
8 4 13 22.41 62.85 36.04 <
-11 5 13 45.56 0.88 39.71 <
-9 5 13 50.54 37.45 27.86 <
-7 5 13 96.81 111.93 26.80 o
-5 5 13 580.54 599.13 25.01 o
-3 5 13 11.55 10.29 15.01 <
-1 5 13 85.05 105.05 15.72 o
1 5 13 2.12 -32.69 15.46 <
3 5 13 2.39 -4.01 16.72 <
5 5 13 31.11 28.24 18.30 <
7 5 13 11.17 -29.50 32.16 <
-10 6 13 13.71 119.56 33.34 o
-8 6 13 20.45 -16.73 27.52 <
-6 6 13 14.14 -10.90 26.95 <
-4 6 13 30.59 22.94 18.82 <
-2 6 13 1.44 40.06 17.24 o
0 6 13 0.13 -21.51 14.54 <
2 6 13 31.96 8.60 16.37 <
4 6 13 1.87 -12.60 20.30 <
6 6 13 6.56 0.07 21.58 <
-9 7 13 96.16 122.41 27.97 o
-7 7 13 1.50 -36.57 32.40 <
-5 7 13 0.21 -48.58 23.50 <
-3 7 13 3.61 -32.69 22.73 <
-1 7 13 15.83 -57.64 19.64 <
1 7 13 14.17 8.75 21.62 <
3 7 13 61.58 61.28 19.25 o
5 7 13 0.16 3.97 21.61 <
7 7 13 38.14 16.97 6.79 o
-8 8 13 14.44 28.28 25.78 <
-6 8 13 0.00 -17.32 23.50 <
-4 8 13 40.82 46.16 24.79 <
-2 8 13 5.14 65.44 27.40 o
0 8 13 87.97 87.36 20.01 o
2 8 13 6.05 120.30 23.97 o
4 8 13 39.70 -14.04 27.38 <
6 8 13 1.78 -21.97 6.31 <
-7 9 13 52.07 40.97 7.66 o
-5 9 13 82.98 64.30 8.66 o
-3 9 13 18.48 18.69 5.90 o
-1 9 13 22.25 22.06 4.63 o
1 9 13 142.38 312.55 28.48 o
3 9 13 134.41 156.50 29.88 o
-6 10 13 54.15 109.59 7.72 o
-4 10 13 17.77 0.24 6.85 <
-2 10 13 10.75 6.96 5.66 <
0 10 13 306.33 384.19 10.84 o
2 10 13 57.93 71.94 6.26 o
-12 0 14 2.12 -12.22 8.25 <
-10 0 14 37.74 -97.11 27.50 <
-8 0 14 0.79 17.42 27.06 <
-6 0 14 8.53 -58.46 28.77 <
-4 0 14 139.40 120.22 26.98 o
-2 0 14 3.86 78.09 28.86 o
0 0 14 15.44 113.76 24.19 o
2 0 14 78.92 88.50 20.17 o
4 0 14 158.19 251.09 22.79 o
6 0 14 203.34 249.77 20.10 o
8 0 14 20.58 -41.33 43.02 <
-11 1 14 58.54 79.68 16.34 o
-9 1 14 1.69 48.44 20.51 o
-7 1 14 14.45 -19.61 20.72 <
-5 1 14 9.99 -43.30 18.68 <
-3 1 14 4.02 3.11 18.19 <
-1 1 14 2.13 20.75 17.76 <
1 1 14 1.86 -42.68 17.60 <
3 1 14 12.88 16.08 15.98 <
5 1 14 0.30 16.26 17.27 <
7 1 14 59.85 63.07 27.53 o
-12 2 14 1.96 33.65 5.68 o
-10 2 14 0.03 -30.58 19.03 <
-8 2 14 17.42 58.20 24.63 o
-6 2 14 0.04 -24.82 21.50 <
-4 2 14 29.85 10.17 19.22 <
-2 2 14 4.65 -35.87 20.48 <
0 2 14 80.46 122.37 16.29 o
2 2 14 114.75 132.08 17.64 o
4 2 14 14.12 69.24 17.17 o
6 2 14 7.86 13.48 21.88 <
8 2 14 25.53 -29.46 28.43 <
-11 3 14 2.86 36.04 20.31 <
-9 3 14 57.31 65.90 26.28 o
-7 3 14 0.41 43.84 24.94 <
-5 3 14 761.09 771.03 25.79 o
-3 3 14 3.21 -74.00 21.89 <
-1 3 14 0.03 11.01 21.23 <
1 3 14 877.73 965.88 23.82 o
3 3 14 81.09 123.40 22.48 o
5 3 14 10.45 40.05 28.65 <
7 3 14 45.09 161.16 30.38 o
-10 4 14 19.15 11.41 27.67 <
-8 4 14 7.77 73.58 27.23 o
-6 4 14 58.92 72.56 27.48 o
-4 4 14 138.94 60.32 23.45 o
-2 4 14 7.13 44.14 23.36 <
0 4 14 95.65 86.49 19.01 o
2 4 14 450.38 531.47 22.19 o
4 4 14 67.61 67.53 21.78 o
6 4 14 32.15 42.70 26.94 <
-9 5 14 2.81 38.30 27.41 <
-7 5 14 138.78 260.96 32.18 o
-5 5 14 61.55 -66.38 33.01 <
-3 5 14 7.04 -49.34 25.39 <
-1 5 14 2.73 5.55 18.95 <
1 5 14 392.24 448.36 19.85 o
3 5 14 12.40 31.54 16.07 <
5 5 14 0.03 12.61 27.21 <
7 5 14 0.01 24.98 5.56 o
-10 6 14 2.53 -17.93 8.10 <
-8 6 14 2.47 -26.48 26.48 <
-6 6 14 149.06 127.27 25.39 o
-4 6 14 36.29 12.39 27.58 <
-2 6 14 8.54 -3.00 21.56 <
0 6 14 107.14 122.20 17.95 o
2 6 14 72.81 34.98 15.41 o
4 6 14 0.49 -6.42 20.83 <
6 6 14 0.19 -29.84 24.34 <
-9 7 14 27.99 29.07 7.35 o
-7 7 14 14.55 10.52 7.06 <
-5 7 14 5.99 3.26 5.94 <
-3 7 14 0.00 2.37 5.05 <
-1 7 14 4.36 -32.01 25.93 <
1 7 14 66.95 36.33 18.83 <
3 7 14 48.83 104.11 20.04 o
5 7 14 6.50 -43.55 26.83 <
-8 8 14 17.42 33.18 6.79 o
-6 8 14 149.10 156.84 8.93 o
-4 8 14 2.71 24.25 7.46 o
-2 8 14 17.31 33.91 5.63 o
0 8 14 8.55 6.69 4.99 <
2 8 14 8.78 57.51 19.53 o
4 8 14 16.99 52.91 39.32 <
-5 9 14 2.78 1.95 6.01 <
-3 9 14 18.27 18.99 8.70 o
-1 9 14 92.18 94.08 7.27 o
1 9 14 44.86 61.03 7.07 o
-11 1 15 0.01 16.37 6.78 o
-9 1 15 27.79 16.36 4.89 o
-7 1 15 136.54 96.18 22.00 o
-5 1 15 12.96 131.69 22.30 o
-3 1 15 0.77 -43.80 15.69 <
-1 1 15 17.39 97.01 31.23 o
1 1 15 134.82 85.75 23.88 o
3 1 15 0.51 -53.34 19.33 <
5 1 15 38.19 78.29 34.81 o
7 1 15 305.14 215.54 37.76 o
-10 2 15 2.85 -19.03 4.91 <
-8 2 15 296.25 271.74 22.87 o
-6 2 15 200.69 138.86 23.34 o
-4 2 15 25.67 53.38 25.83 o
-2 2 15 3.95 -22.82 27.85 <
0 2 15 164.30 184.51 25.26 o
2 2 15 110.72 98.57 24.13 o
4 2 15 7.94 42.52 25.72 <
6 2 15 196.81 195.57 29.86 o
-9 3 15 36.64 11.25 6.10 <
-7 3 15 789.45 806.12 26.40 o
-5 3 15 98.33 120.21 25.76 o
-3 3 15 30.59 -10.20 31.27 <
-1 3 15 232.48 182.96 26.32 o
1 3 15 466.98 459.02 23.56 o
3 3 15 0.03 39.14 26.15 <
5 3 15 16.89 -39.17 30.98 <
-10 4 15 3.59 27.02 7.13 o
-8 4 15 3.24 -27.23 6.34 <
-6 4 15 368.66 343.43 27.73 o
-4 4 15 65.72 72.46 25.02 o
-2 4 15 28.12 117.37 27.53 o
0 4 15 338.01 300.38 29.18 o
2 4 15 604.56 570.91 22.05 o
4 4 15 7.97 -45.12 30.15 <
6 4 15 21.00 -18.14 30.96 <
-9 5 15 19.33 22.21 7.19 o
-7 5 15 12.21 65.43 7.57 o
-5 5 15 97.03 114.37 7.47 o
-3 5 15 0.21 -8.29 5.86 <
-1 5 15 6.21 29.00 23.60 <
1 5 15 633.35 624.80 28.35 o
3 5 15 93.13 112.82 31.25 o
5 5 15 41.89 43.52 31.36 <
-8 6 15 0.56 24.63 7.38 o
-6 6 15 2.17 17.48 7.45 o
-4 6 15 12.42 -7.90 6.23 <
-2 6 15 5.89 -8.93 5.70 <
0 6 15 14.92 32.94 5.96 o
2 6 15 17.60 45.24 19.30 o
4 6 15 36.52 -75.92 55.02 <
-7 7 15 0.76 -14.54 7.36 <
-5 7 15 14.63 15.92 7.03 o
-3 7 15 0.01 -21.85 6.30 <
-1 7 15 5.55 -23.43 6.79 <
1 7 15 2.04 -17.78 6.51 <
3 7 15 5.20 -11.16 8.79 <
-4 8 15 5.85 -11.81 8.05 <
-2 8 15 79.14 130.61 8.30 o
0 8 15 5.39 11.72 6.67 <
-8 0 16 388.07 417.95 14.81 o
-6 0 16 21.00 -0.14 7.99 <
-4 0 16 4.58 12.95 7.78 <
-2 0 16 0.11 -16.97 6.71 <
0 0 16 392.38 495.47 46.05 o
2 0 16 55.23 61.23 12.51 o
4 0 16 0.17 39.84 11.73 o
-9 1 16 4.78 -4.81 6.87 <
-7 1 16 248.33 267.12 9.07 o
-5 1 16 37.84 30.89 8.61 o
-3 1 16 26.16 20.03 7.77 o
-1 1 16 20.51 -8.79 26.16 <
1 1 16 102.82 160.37 30.27 o
3 1 16 14.76 38.56 8.29 o
5 1 16 17.59 18.24 7.75 o
-8 2 16 497.95 502.81 11.74 o
-6 2 16 232.49 245.14 8.47 o
-4 2 16 2.59 -3.58 6.29 <
-2 2 16 50.79 40.45 7.21 o
0 2 16 163.38 125.80 7.70 o
2 2 16 36.53 38.97 9.56 o
4 2 16 3.48 -10.13 8.16 <
-7 3 16 99.67 108.02 7.22 o
-5 3 16 1.91 -10.65 5.93 <
-3 3 16 6.53 5.20 6.76 <
-1 3 16 0.27 -9.94 5.95 <
1 3 16 22.29 0.82 7.03 <
3 3 16 13.95 -4.58 8.35 <
-8 4 16 2.12 5.93 8.30 <
-6 4 16 10.17 -2.28 7.38 <
-4 4 16 11.01 9.53 6.91 <
-2 4 16 20.32 15.07 7.62 <
0 4 16 99.57 76.82 6.79 o
4 4 16 10.87 13.35 7.81 <
-7 5 16 10.50 14.47 8.92 <
-5 5 16 0.02 -4.44 6.41 <
-3 5 16 0.11 27.16 6.79 o
-1 5 16 178.31 186.75 8.06 o
1 5 16 23.33 7.46 8.27 <
3 5 16 0.02 -41.75 8.96 <
-6 6 16 1.29 0.51 8.15 <
-4 6 16 4.14 -19.68 7.81 <
-2 6 16 121.66 148.56 8.79 o
0 6 16 25.42 11.80 6.63 <
2 6 16 2.80 17.74 7.09 o
-3 7 16 61.19 66.06 8.12 o
-1 7 16 3.95 -31.71 8.04 <
-7 1 17 41.64 27.96 7.69 o
-5 1 17 5.38 4.62 5.59 <
-3 1 17 41.41 68.26 7.37 o
-1 1 17 0.82 -6.93 8.85 <
1 1 17 0.26 15.65 8.55 <
-6 2 17 101.94 111.13 7.55 o
-4 2 17 0.26 12.75 7.99 <
-2 2 17 20.45 22.86 7.49 o
0 2 17 70.35 68.95 9.25 o
2 2 17 3.66 8.76 8.92 <
-5 3 17 0.99 46.32 7.81 o
-3 3 17 9.39 -16.79 6.62 <
-1 3 17 11.96 4.60 7.14 <
1 3 17 26.32 -6.70 13.75 <
-4 4 17 0.57 5.35 8.06 <
-2 4 17 14.27 6.11 6.79 <
0 4 17 35.91 17.06 6.56 o
loop_
_cod_related_entry_id
_cod_related_entry_code
_cod_related_entry_database
1 29150 ChemSpider
|
1501654.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/16/1501654.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_1501654
loop_
_publ_author_name
'Wang, Shuao'
'Diwu, Juan'
'Simonetti, Antonio'
'Booth, Corwin H.'
'Albrecht-Schmitt, Thomas E'
_publ_section_title
;
Interstitial incorporation of plutonium into a low-dimensional potassium
borate.
;
_journal_issue 21
_journal_name_full 'Environmental science & technology'
_journal_page_first 9457
_journal_page_last 9463
_journal_paper_doi 10.1021/es2028247
_journal_volume 45
_journal_year 2011
_chemical_formula_moiety K[B5O7(OH)2]H2O:Pu
_chemical_formula_sum 'B5 H4 K0.99 O10'
_chemical_formula_weight 256.60
_chemical_melting_point ?
_chemical_name_common 'Plutonium doped potassium borate'
_chemical_name_systematic
;
?
;
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 97.4120(10)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 9.4619(12)
_cell_length_b 7.4691(10)
_cell_length_c 11.3740(15)
_cell_measurement_reflns_used 1826
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 27.49
_cell_measurement_theta_min 2.17
_cell_volume 797.11(18)
_computing_cell_refinement 'smart saint'
_computing_data_collection smart
_computing_data_reduction SAINT
_computing_molecular_graphics 'SHELXP-97 (Sheldrick, 1997)'
_computing_publication_material 'SHELXCIF-97 (Sheldrick, 2000)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type 'BRUKER apex II'
_diffrn_measurement_method '0.5 wide w/ exposures'
_diffrn_radiation_monochromator 'Quazar optics'
_diffrn_radiation_source 'Imus microfocused'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0373
_diffrn_reflns_av_sigmaI/netI 0.0295
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_k_min -9
_diffrn_reflns_limit_l_max 14
_diffrn_reflns_limit_l_min -14
_diffrn_reflns_number 8999
_diffrn_reflns_theta_full 27.49
_diffrn_reflns_theta_max 27.49
_diffrn_reflns_theta_min 2.17
_exptl_absorpt_coefficient_mu 0.700
_exptl_absorpt_correction_T_max 0.994
_exptl_absorpt_correction_T_min 0.942
_exptl_absorpt_correction_type numerical
_exptl_absorpt_process_details SHELTXPREP
_exptl_crystal_colour Yellow
_exptl_crystal_density_diffrn 2.138
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description Tablet
_exptl_crystal_F_000 511
_exptl_crystal_size_max 0.085
_exptl_crystal_size_mid 0.076
_exptl_crystal_size_min 0.009
_refine_diff_density_max 0.853
_refine_diff_density_min -0.377
_refine_diff_density_rms 0.107
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.141
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 161
_refine_ls_number_reflns 1826
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.141
_refine_ls_R_factor_all 0.0495
_refine_ls_R_factor_gt 0.0423
_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^)+(0.0425P)^2^+2.2689P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1083
_refine_ls_wR_factor_ref 0.1127
_reflns_number_gt 1585
_reflns_number_total 1826
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file es2028247_si_001.cif
_cod_data_source_block KBOPu
_cod_depositor_comments
;
The following automatic conversions were performed:
'_chemical_melting_point' value 'N/A' was changed to '?' - the value
is undefined or not given.
'_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_values 1715 2011-07-08 13:25:40Z adriana
The following automatic conversions were performed:
'_exptl_crystal_density_meas' value 'N/A' was changed to '?' - the
value is perceived as not measured.
Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas
;
_cod_original_sg_symbol_H-M P2(1)/c
_cod_database_code 1501654
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
K1 K 0.67180(6) 0.06972(8) 0.73235(5) 0.01106(18) Uani 0.98 1 d P
B1 B 0.5677(3) -0.1916(4) 1.0672(3) 0.0084(6) Uani 1 1 d .
B2 B 0.8267(3) -0.3877(4) 0.9477(3) 0.0085(6) Uani 1 1 d .
B3 B 0.6319(3) 0.4078(4) 0.9263(3) 0.0084(6) Uani 1 1 d .
B4 B 0.7470(3) 0.0224(4) 1.0388(3) 0.0080(6) Uani 1 1 d .
B5 B 0.2976(3) 0.0492(4) 0.7554(3) 0.0082(6) Uani 1 1 d .
O1 O 0.9343(2) -0.3039(3) 1.01785(18) 0.0107(4) Uani 1 1 d .
O2 O 0.8112(2) -0.3629(3) 0.82893(17) 0.0092(4) Uani 1 1 d .
O3 O 0.5416(2) 0.1987(3) 0.48404(17) 0.0091(4) Uani 1 1 d .
O4 O 0.8165(2) 0.1073(3) 0.95756(18) 0.0097(4) Uani 1 1 d .
O5 O 0.6382(2) -0.0924(3) 0.99035(17) 0.0090(4) Uani 1 1 d .
O6 O 0.7757(2) 0.4509(3) 0.65764(17) 0.0087(4) Uani 1 1 d .
O7 O 0.6194(2) 0.4223(3) 0.80755(17) 0.0089(4) Uani 1 1 d .
O8 O 0.7337(2) -0.0012(3) 0.49998(17) 0.0087(4) Uani 1 1 d .
O9 O 0.3957(2) 0.1836(3) 0.81421(17) 0.0090(4) Uani 1 1 d .
O1W O 0.9416(2) -0.0899(3) 0.73637(18) 0.0120(4) Uani 1 1 d .
H1 H 0.914(4) -0.178(6) 0.774(3) 0.021(10) Uiso 1 1 d .
H2 H 0.939(5) -0.347(6) 1.099(4) 0.038(12) Uiso 1 1 d .
H3 H 1.023(5) -0.059(6) 0.769(4) 0.030(11) Uiso 1 1 d .
H4 H 0.891(5) 0.161(7) 0.983(4) 0.046(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
K1 0.0110(3) 0.0126(3) 0.0096(3) -0.0029(2) 0.0012(2) 0.0002(2)
B1 0.0082(13) 0.0062(13) 0.0109(14) -0.0015(11) 0.0020(11) 0.0015(11)
B2 0.0072(13) 0.0073(14) 0.0110(14) -0.0010(11) 0.0013(11) 0.0018(11)
B3 0.0068(13) 0.0070(14) 0.0113(14) -0.0009(11) 0.0010(11) 0.0037(11)
B4 0.0078(13) 0.0094(14) 0.0069(14) -0.0019(11) 0.0016(11) 0.0024(11)
B5 0.0096(14) 0.0082(14) 0.0068(14) 0.0006(11) 0.0020(11) 0.0011(11)
O1 0.0098(9) 0.0121(10) 0.0101(10) 0.0002(8) 0.0005(7) -0.0035(8)
O2 0.0087(9) 0.0104(9) 0.0084(9) -0.0009(7) 0.0011(7) -0.0016(7)
O3 0.0080(9) 0.0088(10) 0.0104(9) -0.0002(7) 0.0012(7) 0.0013(7)
O4 0.0078(9) 0.0128(10) 0.0087(9) 0.0017(8) 0.0012(7) -0.0019(8)
O5 0.0091(9) 0.0090(9) 0.0089(9) 0.0010(7) 0.0011(7) -0.0013(7)
O6 0.0093(9) 0.0101(10) 0.0068(9) -0.0002(7) 0.0010(7) 0.0014(7)
O7 0.0116(9) 0.0081(9) 0.0067(9) 0.0001(7) -0.0001(7) -0.0012(8)
O8 0.0087(9) 0.0091(9) 0.0082(9) -0.0008(7) 0.0006(7) 0.0019(7)
O9 0.0095(9) 0.0096(9) 0.0082(9) -0.0002(7) 0.0018(7) -0.0013(7)
O1W 0.0114(10) 0.0150(11) 0.0094(10) 0.0013(8) 0.0009(8) -0.0042(8)
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'
K K 0.2009 0.2494 '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
O4 K1 O1W 71.79(6) . .
O4 K1 O8 138.48(6) . .
O1W K1 O8 68.85(6) . .
O4 K1 O7 73.15(6) . .
O1W K1 O7 125.67(6) . .
O8 K1 O7 121.43(6) . .
O4 K1 O7 121.54(6) . 2_646
O1W K1 O7 132.27(6) . 2_646
O8 K1 O7 95.06(6) . 2_646
O7 K1 O7 101.38(4) . 2_646
O4 K1 O9 109.40(6) . 2_646
O1W K1 O9 76.49(6) . 2_646
O8 K1 O9 73.68(6) . 2_646
O7 K1 O9 155.46(6) . 2_646
O7 K1 O9 55.78(5) 2_646 2_646
O4 K1 O9 91.75(6) . .
O1W K1 O9 159.69(6) . .
O8 K1 O9 129.40(6) . .
O7 K1 O9 56.68(5) . .
O7 K1 O9 47.24(5) 2_646 .
O9 K1 O9 98.83(4) 2_646 .
O4 K1 O3 155.46(6) . .
O1W K1 O3 113.66(6) . .
O8 K1 O3 46.36(5) . .
O7 K1 O3 85.49(5) . .
O7 K1 O3 73.80(5) 2_646 .
O9 K1 O3 95.06(5) 2_646 .
O9 K1 O3 86.27(5) . .
O4 K1 O6 91.35(6) . .
O1W K1 O6 94.18(6) . .
O8 K1 O6 78.96(6) . .
O7 K1 O6 46.92(5) . .
O7 K1 O6 127.70(5) 2_646 .
O9 K1 O6 152.64(5) 2_646 .
O9 K1 O6 98.12(5) . .
O3 K1 O6 64.81(5) . .
O4 K1 O5 44.70(5) . .
O1W K1 O5 91.25(6) . .
O8 K1 O5 146.65(6) . .
O7 K1 O5 91.88(5) . .
O7 K1 O5 78.47(5) 2_646 .
O9 K1 O5 75.82(5) 2_646 .
O9 K1 O5 68.49(5) . .
O3 K1 O5 151.00(5) . .
O6 K1 O5 130.71(5) . .
O4 K1 B3 53.58(7) . .
O1W K1 B3 118.69(7) . .
O8 K1 B3 142.87(7) . .
O7 K1 B3 22.58(6) . .
O7 K1 B3 101.37(7) 2_646 .
O9 K1 B3 142.35(7) 2_646 .
O9 K1 B3 54.30(6) . .
O3 K1 B3 107.26(7) . .
O6 K1 B3 64.60(7) . .
O5 K1 B3 69.96(7) . .
O4 K1 B3 144.14(7) . 2_646
O1W K1 B3 124.00(7) . 2_646
O8 K1 B3 72.62(7) . 2_646
O7 K1 B3 108.73(7) . 2_646
O7 K1 B3 22.96(6) 2_646 2_646
O9 K1 B3 54.38(6) 2_646 2_646
O9 K1 B3 63.76(7) . 2_646
O3 K1 B3 54.34(6) . 2_646
O6 K1 B3 116.53(6) . 2_646
O5 K1 B3 99.96(6) . 2_646
B3 K1 B3 116.69(6) . 2_646
O9 B1 O5 121.7(3) 3_657 .
O9 B1 O3 121.9(3) 3_657 2_646
O5 B1 O3 116.4(2) . 2_646
O9 B1 K1 58.41(14) 3_657 4_556
O5 B1 K1 130.79(18) . 4_556
O3 B1 K1 83.75(16) 2_646 4_556
O9 B1 K1 56.47(13) 3_657 3_657
O5 B1 K1 132.24(18) . 3_657
O3 B1 K1 85.31(15) 2_646 3_657
K1 B1 K1 91.24(7) 4_556 3_657
O2 B2 O1 119.9(3) . .
O2 B2 O8 120.9(3) . 4_556
O1 B2 O8 119.2(3) . 4_556
O7 B3 O8 122.2(3) . 4_566
O7 B3 O3 122.7(3) . 4_566
O8 B3 O3 115.1(2) 4_566 4_566
O7 B3 K1 53.98(14) . .
O8 B3 K1 129.80(18) 4_566 .
O3 B3 K1 90.46(16) 4_566 .
O7 B3 K1 58.77(14) . 2_656
O8 B3 K1 128.02(18) 4_566 2_656
O3 B3 K1 85.77(15) 4_566 2_656
K1 B3 K1 94.39(8) . 2_656
O7 B3 K1 172.5(2) . 4_566
O8 B3 K1 52.23(13) 4_566 4_566
O3 B3 K1 63.04(14) 4_566 4_566
K1 B3 K1 132.95(9) . 4_566
K1 B3 K1 119.39(9) 2_656 4_566
O4 B4 O6 123.8(3) . 4_566
O4 B4 O5 114.5(2) . .
O6 B4 O5 121.7(3) 4_566 .
O4 B4 K1 47.64(14) . .
O6 B4 K1 165.7(2) 4_566 .
O5 B4 K1 67.83(14) . .
O2 B5 O9 109.9(2) 2_656 .
O2 B5 O7 110.1(2) 2_656 2_646
O9 B5 O7 108.4(2) . 2_646
O2 B5 O6 108.1(2) 2_656 2_646
O9 B5 O6 111.0(2) . 2_646
O7 B5 O6 109.4(2) 2_646 2_646
O2 B5 K1 123.28(17) 2_656 .
O9 B5 K1 55.41(12) . .
O7 B5 K1 53.08(12) 2_646 .
O6 B5 K1 128.62(17) 2_646 .
B2 O2 B5 124.6(2) . 2_646
B1 O3 B3 127.5(2) 2_656 4_565
B1 O3 K1 139.19(17) 2_656 .
B3 O3 K1 93.26(16) 4_565 .
B4 O4 K1 111.02(17) . .
B1 O5 B4 118.1(2) . .
B1 O5 K1 152.70(17) . .
B4 O5 K1 88.53(15) . .
B4 O6 B5 122.9(2) 4_565 2_656
B4 O6 K1 111.74(16) 4_565 .
B5 O6 K1 94.50(15) 2_656 .
B3 O7 B5 123.8(2) . 2_656
B3 O7 K1 103.44(17) . .
B5 O7 K1 109.04(15) 2_656 .
B3 O7 K1 98.27(16) . 2_656
B5 O7 K1 103.36(15) 2_656 2_656
K1 O7 K1 119.83(7) . 2_656
B3 O8 B2 118.0(2) 4_565 4
B3 O8 K1 105.07(16) 4_565 .
B2 O8 K1 136.56(17) 4 .
B1 O9 B5 123.5(2) 3_657 .
B1 O9 K1 98.95(16) 3_657 2_656
B5 O9 K1 118.11(15) . 2_656
B1 O9 K1 101.56(16) 3_657 .
B5 O9 K1 100.89(15) . .
K1 O9 K1 113.12(6) 2_656 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
K1 O4 2.758(2) .
K1 O1W 2.813(2) .
K1 O8 2.830(2) .
K1 O7 2.832(2) .
K1 O7 2.947(2) 2_646
K1 O9 2.987(2) 2_646
K1 O9 3.007(2) .
K1 O3 3.086(2) .
K1 O6 3.164(2) .
K1 O5 3.228(2) .
K1 B3 3.406(3) .
K1 B3 3.411(3) 2_646
B1 O9 1.349(4) 3_657
B1 O5 1.382(4) .
B1 O3 1.388(4) 2_646
B1 K1 3.463(3) 4_556
B1 K1 3.534(3) 3_657
B2 O2 1.353(4) .
B2 O1 1.362(4) .
B2 O8 1.397(4) 4_556
B3 O7 1.345(4) .
B3 O8 1.382(4) 4_566
B3 O3 1.392(4) 4_566
B3 K1 3.411(3) 2_656
B3 K1 3.457(3) 4_566
B4 O4 1.358(4) .
B4 O6 1.358(4) 4_566
B4 O5 1.398(4) .
B5 O2 1.468(3) 2_656
B5 O9 1.468(4) .
B5 O7 1.474(3) 2_646
B5 O6 1.475(3) 2_646
O2 B5 1.468(3) 2_646
O3 B1 1.387(4) 2_656
O3 B3 1.392(4) 4_565
O6 B4 1.358(4) 4_565
O6 B5 1.475(3) 2_656
O7 B5 1.474(3) 2_656
O7 K1 2.947(2) 2_656
O8 B3 1.382(4) 4_565
O8 B2 1.397(4) 4
O9 B1 1.350(4) 3_657
O9 K1 2.987(2) 2_656
|
1501655.cif | #------------------------------------------------------------------------------
#$Date: 2017-10-13 02:32:00 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201954 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/50/16/1501655.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_1501655
loop_
_publ_author_name
'Harper, Naomi D.'
'Nizio, Katie D.'
'Hendsbee, Arthur D.'
'Masuda, Jason D.'
'Robertson, Katherine N.'
'Murphy, Luke J.'
'Johnson, Michel B.'
'Pye, Cory C.'
'Clyburne, Jason A. C.'
_publ_section_title
;
Survey of Carbon Dioxide Capture in Phosphonium-Based Ionic Liquids and
End-Capped Polyethylene Glycol Using DETA (DETA = Diethylenetriamine) as
a Model Absorbent§
;
_journal_issue 5
_journal_name_full
'Industrial & Engineering Chemistry Research'
_journal_page_first 2822
_journal_paper_doi 10.1021/ie101734h
_journal_volume 50
_journal_year 2011
_chemical_formula_moiety 'C5 H13 N3 O2'
_chemical_formula_sum 'C5 H13 N3 O2'
_chemical_formula_weight 147.18
_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 106.4030(10)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 8.8542(8)
_cell_length_b 8.1328(7)
_cell_length_c 10.5772(9)
_cell_measurement_reflns_used 1932
_cell_measurement_temperature 296(2)
_cell_measurement_theta_max 28.21
_cell_measurement_theta_min 2.40
_cell_volume 730.66(11)
_computing_cell_refinement 'Bruker SAINT'
_computing_data_collection 'Bruker APEX2'
_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 296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_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 0.0301
_diffrn_reflns_av_sigmaI/netI 0.0267
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_limit_l_min -12
_diffrn_reflns_number 6859
_diffrn_reflns_theta_full 26.00
_diffrn_reflns_theta_max 26.00
_diffrn_reflns_theta_min 2.40
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 0.104
_exptl_absorpt_correction_T_max 0.7457
_exptl_absorpt_correction_T_min 0.6665
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details SADABS
_exptl_crystal_colour 'clear yellow'
_exptl_crystal_density_diffrn 1.338
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description Platelette
_exptl_crystal_F_000 320
_exptl_crystal_size_max .400
_exptl_crystal_size_mid .168
_exptl_crystal_size_min .115
_refine_diff_density_max 0.277
_refine_diff_density_min -0.213
_refine_diff_density_rms 0.042
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.128
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 91
_refine_ls_number_reflns 1425
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.128
_refine_ls_R_factor_all 0.0673
_refine_ls_R_factor_gt 0.0471
_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^)+(0.0252P)^2^+0.5309P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0992
_refine_ls_wR_factor_ref 0.1089
_reflns_number_gt 1106
_reflns_number_total 1425
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file ie101734h_si_001.cif
_cod_data_source_block DETACO2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.
'_exptl_absorpt_correction_type' value 'Multi-Scan'
changed to 'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.
'_refine_ls_hydrogen_treatment' value 'CONSTR' changed
to 'constr' 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_values 1715 2011-07-08 13:25:40Z adriana
;
_cod_original_sg_symbol_H-M P2(1)/c
_cod_database_code 1501655
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
O1 O 0.1821(2) 0.13387(17) 0.54608(15) 0.0436(4) Uani 1 1 d .
O2 O 0.03232(18) 0.32220(18) 0.41394(15) 0.0423(4) Uani 1 1 d .
C1 C 0.1300(3) 0.2775(2) 0.5216(2) 0.0329(5) Uani 1 1 d .
N3 N 0.1229(2) 0.9397(2) 0.73823(18) 0.0381(5) Uani 1 1 d .
H3A H 0.1252 1.0210 0.6825 0.057 Uiso 1 1 calc R
H3B H 0.0646 0.9698 0.7905 0.057 Uiso 1 1 calc R
H3C H 0.0814 0.8504 0.6930 0.057 Uiso 1 1 calc R
N2 N 0.2401(2) 0.6096(2) 0.85273(17) 0.0361(4) Uani 1 1 d .
H2 H 0.2171 0.5435 0.9096 0.043 Uiso 1 1 d R
N1 N 0.1826(2) 0.3963(2) 0.61438(18) 0.0397(5) Uani 1 1 d .
H1 H 0.1460 0.4943 0.5976 0.048 Uiso 1 1 calc R
C2 C 0.2971(3) 0.3655(3) 0.7396(2) 0.0376(5) Uani 1 1 d .
H2A H 0.3833 0.3011 0.7258 0.045 Uiso 1 1 calc R
H2B H 0.2485 0.3027 0.7956 0.045 Uiso 1 1 calc R
C3 C 0.3600(3) 0.5251(3) 0.8067(2) 0.0400(5) Uani 1 1 d .
H3D H 0.4510 0.5029 0.8810 0.048 Uiso 1 1 calc R
H3E H 0.3934 0.5952 0.7455 0.048 Uiso 1 1 calc R
C4 C 0.2910(3) 0.7663(3) 0.9168(2) 0.0455(6) Uani 1 1 d .
H4A H 0.3981 0.7556 0.9729 0.055 Uiso 1 1 calc R
H4B H 0.2244 0.7945 0.9722 0.055 Uiso 1 1 calc R
C5 C 0.2845(3) 0.9033(3) 0.8190(2) 0.0450(6) Uani 1 1 d .
H5A H 0.3299 1.0018 0.8663 0.054 Uiso 1 1 calc R
H5B H 0.3479 0.8729 0.7613 0.054 Uiso 1 1 calc R
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.0683(11) 0.0253(8) 0.0376(9) 0.0001(7) 0.0158(8) 0.0073(7)
O2 0.0552(10) 0.0314(8) 0.0346(9) -0.0019(7) 0.0035(8) 0.0035(7)
C1 0.0424(12) 0.0263(11) 0.0331(13) 0.0037(9) 0.0157(10) 0.0040(9)
N3 0.0510(11) 0.0267(9) 0.0390(11) 0.0008(8) 0.0168(9) 0.0043(8)
N2 0.0499(11) 0.0266(9) 0.0324(11) 0.0032(8) 0.0127(9) 0.0008(8)
N1 0.0544(12) 0.0231(9) 0.0349(11) -0.0030(8) 0.0017(9) 0.0068(8)
C2 0.0428(12) 0.0299(11) 0.0373(13) 0.0003(10) 0.0070(10) 0.0064(9)
C3 0.0415(13) 0.0378(12) 0.0373(13) -0.0030(10) 0.0053(10) 0.0004(10)
C4 0.0606(15) 0.0328(12) 0.0376(14) -0.0015(10) 0.0051(11) 0.0041(11)
C5 0.0467(13) 0.0286(12) 0.0562(16) 0.0013(11) 0.0090(12) -0.0020(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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
O1 C1 O2 124.6(2)
O1 C1 N1 118.7(2)
O2 C1 N1 116.70(18)
C5 N3 H3A 109.5
C5 N3 H3B 109.5
H3A N3 H3B 109.5
C5 N3 H3C 109.5
H3A N3 H3C 109.5
H3B N3 H3C 109.5
C4 N2 C3 114.15(18)
C4 N2 H2 108.7
C3 N2 H2 105.9
C1 N1 C2 123.11(17)
C1 N1 H1 118.4
C2 N1 H1 118.4
N1 C2 C3 110.66(17)
N1 C2 H2A 109.5
C3 C2 H2A 109.5
N1 C2 H2B 109.5
C3 C2 H2B 109.5
H2A C2 H2B 108.1
N2 C3 C2 110.83(18)
N2 C3 H3D 109.5
C2 C3 H3D 109.5
N2 C3 H3E 109.5
C2 C3 H3E 109.5
H3D C3 H3E 108.1
N2 C4 C5 112.39(19)
N2 C4 H4A 109.1
C5 C4 H4A 109.1
N2 C4 H4B 109.1
C5 C4 H4B 109.1
H4A C4 H4B 107.9
N3 C5 C4 112.86(19)
N3 C5 H5A 109.0
C4 C5 H5A 109.0
N3 C5 H5B 109.0
C4 C5 H5B 109.0
H5A C5 H5B 107.8
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
O1 C1 1.255(2)
O2 C1 1.273(2)
C1 N1 1.362(3)
N3 C5 1.474(3)
N3 H3A 0.8900
N3 H3B 0.8900
N3 H3C 0.8900
N2 C4 1.454(3)
N2 C3 1.459(3)
N2 H2 0.8724
N1 C2 1.444(3)
N1 H1 0.8600
C2 C3 1.508(3)
C2 H2A 0.9700
C2 H2B 0.9700
C3 H3D 0.9700
C3 H3E 0.9700
C4 C5 1.510(3)
C4 H4A 0.9700
C4 H4B 0.9700
C5 H5A 0.9700
C5 H5B 0.9700
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 106298
|
1501656.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/16/1501656.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_1501656
loop_
_publ_author_name
'Li, Bing'
'Wei, Qing'
'Yang, Qi'
'Chen, Sanping'
'Gao, Shengli'
_publ_section_title
;
Synthesis, Structure, and Thermophysical Properties of an Energetic
Complex
Co(3-(2-pyridyl)-5-(3′-pyridyl)-1H-1,2,4-triazole)3·H2O
;
_journal_issue 7
_journal_name_full 'Journal of Chemical & Engineering Data'
_journal_page_first 3043
_journal_paper_doi 10.1021/je2000364
_journal_volume 56
_journal_year 2011
_chemical_formula_sum 'C36 H26 Co N15 O'
_chemical_formula_weight 743.65
_chemical_name_systematic
;
?
;
_space_group_IT_number 2
_symmetry_cell_setting triclinic
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 89.022(3)
_cell_angle_beta 71.794(2)
_cell_angle_gamma 66.990(2)
_cell_formula_units_Z 2
_cell_length_a 10.3230(18)
_cell_length_b 11.261(2)
_cell_length_c 16.139(3)
_cell_measurement_reflns_used 938
_cell_measurement_temperature 296(2)
_cell_measurement_theta_max 18.8547
_cell_measurement_theta_min 2.2725
_cell_volume 1628.5(5)
_computing_cell_refinement APEX2
_computing_data_collection 'APEX2 (Bruker, 2004)'
_computing_data_reduction APEX2
_computing_molecular_graphics APEX2
_computing_publication_material APEX2
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 296(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type 'Bruker APEX SMART II'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0401
_diffrn_reflns_av_sigmaI/netI 0.1054
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 12
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 8235
_diffrn_reflns_theta_full 25.10
_diffrn_reflns_theta_max 25.10
_diffrn_reflns_theta_min 1.98
_diffrn_standards_interval_time 0
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 0.585
_exptl_absorpt_correction_T_max 0.9019
_exptl_absorpt_correction_T_min 0.8820
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details SADABS
_exptl_crystal_colour red
_exptl_crystal_density_diffrn 1.517
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description Prism
_exptl_crystal_F_000 764
_exptl_crystal_size_max 0.22
_exptl_crystal_size_mid 0.19
_exptl_crystal_size_min 0.18
_refine_diff_density_max 0.306
_refine_diff_density_min -0.370
_refine_diff_density_rms 0.081
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.956
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 482
_refine_ls_number_reflns 5709
_refine_ls_number_restraints 1
_refine_ls_restrained_S_all 0.955
_refine_ls_R_factor_all 0.1315
_refine_ls_R_factor_gt 0.0633
_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^)+(0.0941P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1541
_refine_ls_wR_factor_ref 0.1971
_reflns_number_gt 2989
_reflns_number_total 5709
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file je2000364_si_001.cif
_cod_data_source_block xb3707_0m
_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_values 1715 2011-07-08 13:25:40Z adriana
;
_cod_original_sg_symbol_H-M P-1
_cod_database_code 1501656
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
O1 O 0.5173(8) 0.9657(8) 0.0893(6) 0.225(4) Uani 1 1 d .
H1A H 0.5096 1.0431 0.0960 0.337 Uiso 1 1 d R
H1B H 0.6100 0.9173 0.0651 0.337 Uiso 1 1 d R
Co2 Co 0.35393(8) 0.43668(7) 0.26192(5) 0.0481(3) Uani 1 1 d .
N12 N 0.2327(5) 0.3450(4) 0.2786(3) 0.0445(11) Uani 1 1 d .
N2 N 0.4278(5) 0.3688(4) 0.3546(3) 0.0457(11) Uani 1 1 d .
N7 N 0.2973(5) 0.4984(4) 0.1637(3) 0.0495(12) Uani 1 1 d .
N1 N 0.4786(5) 0.5342(4) 0.2562(3) 0.0536(12) Uani 1 1 d .
N6 N 0.5221(5) 0.3039(4) 0.1720(3) 0.0479(11) Uani 1 1 d .
N13 N 0.2478(5) 0.2274(4) 0.2451(3) 0.0463(11) Uani 1 1 d .
N11 N 0.1756(5) 0.5667(4) 0.3459(3) 0.0479(11) Uani 1 1 d .
N3 N 0.4113(5) 0.2804(4) 0.4114(3) 0.0494(11) Uani 1 1 d .
N14 N 0.0099(5) 0.3388(4) 0.3388(3) 0.0497(11) Uani 1 1 d .
C31 C 0.1110(6) 0.2295(5) 0.2838(3) 0.0458(13) Uani 1 1 d .
N8 N 0.1706(5) 0.5874(4) 0.1524(3) 0.0550(12) Uani 1 1 d .
C32 C 0.0752(6) 0.1195(5) 0.2698(3) 0.0484(14) Uani 1 1 d .
C6 C 0.1941(7) 0.5628(5) 0.0655(4) 0.0541(15) Uani 1 1 d .
C29 C 0.0580(6) 0.5338(5) 0.3738(3) 0.0486(14) Uani 1 1 d .
N9 N 0.3261(6) 0.4630(4) 0.0220(3) 0.0598(13) Uani 1 1 d .
C30 C 0.0923(6) 0.4067(5) 0.3325(3) 0.0465(13) Uani 1 1 d .
N4 N 0.5853(5) 0.3474(5) 0.4266(3) 0.0582(13) Uani 1 1 d .
C18 C 0.5305(6) 0.4066(5) 0.3649(4) 0.0510(14) Uani 1 1 d .
C19 C 0.5079(6) 0.2727(5) 0.4532(4) 0.0524(15) Uani 1 1 d .
C7 C 0.3837(6) 0.4263(5) 0.0856(4) 0.0546(15) Uani 1 1 d .
C17 C 0.5608(6) 0.4995(5) 0.3099(4) 0.0518(14) Uani 1 1 d .
C36 C 0.1790(7) 0.0070(6) 0.2146(4) 0.0627(16) Uani 1 1 d .
H36 H 0.2730 0.0040 0.1836 0.075 Uiso 1 1 calc R
C35 C 0.0121(11) -0.0883(8) 0.2486(5) 0.086(2) Uani 1 1 d .
H35 H -0.0097 -0.1595 0.2418 0.104 Uiso 1 1 calc R
C20 C 0.5303(7) 0.1848(6) 0.5206(4) 0.0564(15) Uani 1 1 d .
C8 C 0.5169(6) 0.3169(5) 0.0895(4) 0.0539(15) Uani 1 1 d .
C25 C 0.1610(7) 0.6811(5) 0.3807(4) 0.0606(16) Uani 1 1 d .
H25 H 0.2398 0.7065 0.3605 0.073 Uiso 1 1 calc R
N15 N 0.1514(8) -0.0977(5) 0.2034(4) 0.0849(18) Uani 1 1 d .
C16 C 0.6613(7) 0.5513(6) 0.3090(4) 0.0724(19) Uani 1 1 d .
H16 H 0.7202 0.5242 0.3448 0.087 Uiso 1 1 calc R
C4 C 0.0835(7) 0.6327(5) 0.0252(4) 0.0571(15) Uani 1 1 d .
C28 C -0.0736(6) 0.6101(6) 0.4388(4) 0.0571(15) Uani 1 1 d .
H28 H -0.1526 0.5845 0.4573 0.069 Uiso 1 1 calc R
C5 C -0.0522(7) 0.7312(6) 0.0706(4) 0.0688(18) Uani 1 1 d .
H5 H -0.0699 0.7558 0.1292 0.083 Uiso 1 1 calc R
C12 C 0.6349(7) 0.2055(6) 0.1841(4) 0.0690(18) Uani 1 1 d .
H12 H 0.6368 0.1938 0.2410 0.083 Uiso 1 1 calc R
C23 C 0.5799(11) 0.0273(7) 0.6469(5) 0.098(3) Uani 1 1 d U
H23 H 0.5975 -0.0261 0.6903 0.118 Uiso 1 1 calc R
N10 N -0.1609(6) 0.7945(5) 0.0370(4) 0.0839(17) Uani 1 1 d .
C27 C -0.0850(6) 0.7260(6) 0.4756(4) 0.0583(16) Uani 1 1 d .
H27 H -0.1713 0.7785 0.5203 0.070 Uiso 1 1 calc R
C10 C 0.7465(8) 0.1316(6) 0.0319(5) 0.088(2) Uani 1 1 d .
H10 H 0.8228 0.0734 -0.0150 0.105 Uiso 1 1 calc R
C33 C -0.0658(7) 0.1232(6) 0.3146(4) 0.0678(18) Uani 1 1 d .
H33 H -0.1383 0.1969 0.3522 0.081 Uiso 1 1 calc R
C9 C 0.6281(7) 0.2316(6) 0.0176(4) 0.0723(19) Uani 1 1 d .
H9 H 0.6230 0.2416 -0.0388 0.087 Uiso 1 1 calc R
C26 C 0.0314(7) 0.7616(6) 0.4457(4) 0.0617(16) Uani 1 1 d .
H26 H 0.0241 0.8400 0.4689 0.074 Uiso 1 1 calc R
C24 C 0.4321(8) 0.1348(6) 0.5648(4) 0.0713(19) Uani 1 1 d .
H24 H 0.3460 0.1559 0.5503 0.086 Uiso 1 1 calc R
C13 C 0.4895(7) 0.6256(6) 0.2033(4) 0.0684(18) Uani 1 1 d .
H13 H 0.4308 0.6510 0.1673 0.082 Uiso 1 1 calc R
C22 C 0.6835(9) 0.0719(8) 0.6056(5) 0.099(3) Uani 1 1 d U
H22 H 0.7702 0.0487 0.6198 0.119 Uiso 1 1 calc R
C14 C 0.5866(8) 0.6824(6) 0.2016(5) 0.078(2) Uani 1 1 d .
H14 H 0.5929 0.7461 0.1650 0.093 Uiso 1 1 calc R
C34 C -0.0982(8) 0.0185(7) 0.3036(5) 0.0752(19) Uani 1 1 d .
H34 H -0.1924 0.0204 0.3326 0.090 Uiso 1 1 calc R
C2 C -0.0024(9) 0.6627(8) -0.0968(5) 0.099(3) Uani 1 1 d .
H2 H 0.0134 0.6407 -0.1555 0.119 Uiso 1 1 calc R
C15 C 0.6737(8) 0.6446(7) 0.2539(5) 0.082(2) Uani 1 1 d .
H15 H 0.7408 0.6813 0.2525 0.099 Uiso 1 1 calc R
C21 C 0.6596(8) 0.1501(7) 0.5437(4) 0.083(2) Uani 1 1 d .
H21 H 0.7303 0.1823 0.5153 0.100 Uiso 1 1 calc R
C11 C 0.7509(8) 0.1188(6) 0.1142(5) 0.083(2) Uani 1 1 d .
H11 H 0.8310 0.0525 0.1243 0.099 Uiso 1 1 calc R
N5 N 0.4502(8) 0.0552(6) 0.6296(4) 0.102(2) Uani 1 1 d .
C1 C -0.1323(11) 0.7561(8) -0.0469(6) 0.090(2) Uani 1 1 d .
C3 C 0.1051(9) 0.6009(7) -0.0614(4) 0.095(3) Uani 1 1 d .
H3 H 0.1948 0.5360 -0.0959 0.114 Uiso 1 1 calc R
H1 H -0.225(6) 0.808(5) -0.065(4) 0.078(19) 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 0.153(7) 0.218(9) 0.265(10) 0.083(8) -0.044(7) -0.058(7)
Co2 0.0501(5) 0.0453(5) 0.0469(5) 0.0058(3) -0.0177(4) -0.0161(4)
N12 0.046(3) 0.045(3) 0.044(3) 0.007(2) -0.019(2) -0.018(2)
N2 0.047(3) 0.048(3) 0.044(3) 0.004(2) -0.015(2) -0.022(2)
N7 0.054(3) 0.042(3) 0.049(3) 0.007(2) -0.024(2) -0.011(2)
N1 0.055(3) 0.043(3) 0.054(3) 0.004(2) -0.008(2) -0.019(2)
N6 0.059(3) 0.041(3) 0.044(3) 0.011(2) -0.021(2) -0.018(2)
N13 0.048(3) 0.041(3) 0.046(3) 0.002(2) -0.018(2) -0.012(2)
N11 0.054(3) 0.044(3) 0.046(3) 0.005(2) -0.020(2) -0.017(2)
N3 0.052(3) 0.053(3) 0.047(3) 0.008(2) -0.023(2) -0.020(2)
N14 0.047(3) 0.050(3) 0.050(3) -0.001(2) -0.017(2) -0.016(2)
C31 0.050(4) 0.048(3) 0.044(3) 0.012(3) -0.025(3) -0.018(3)
N8 0.063(3) 0.043(3) 0.058(3) 0.008(2) -0.025(3) -0.017(2)
C32 0.051(4) 0.052(3) 0.048(3) 0.007(3) -0.025(3) -0.019(3)
C6 0.074(4) 0.049(3) 0.040(3) 0.008(3) -0.026(3) -0.020(3)
C29 0.046(3) 0.048(3) 0.047(3) 0.003(3) -0.018(3) -0.012(3)
N9 0.075(4) 0.054(3) 0.044(3) 0.007(2) -0.024(3) -0.016(3)
C30 0.047(3) 0.051(3) 0.042(3) 0.003(3) -0.020(3) -0.017(3)
N4 0.051(3) 0.065(3) 0.061(3) 0.002(3) -0.023(3) -0.023(3)
C18 0.044(3) 0.053(3) 0.051(4) 0.000(3) -0.012(3) -0.017(3)
C19 0.053(4) 0.051(3) 0.050(4) -0.003(3) -0.020(3) -0.015(3)
C7 0.060(4) 0.041(3) 0.050(4) 0.007(3) -0.008(3) -0.015(3)
C17 0.049(3) 0.054(3) 0.049(4) -0.004(3) -0.010(3) -0.022(3)
C36 0.058(4) 0.060(4) 0.062(4) -0.005(3) -0.019(3) -0.016(3)
C35 0.128(7) 0.087(6) 0.087(6) 0.026(5) -0.060(6) -0.067(6)
C20 0.059(4) 0.057(4) 0.048(4) 0.000(3) -0.024(3) -0.014(3)
C8 0.064(4) 0.042(3) 0.050(4) 0.010(3) -0.016(3) -0.018(3)
C25 0.061(4) 0.056(4) 0.063(4) -0.004(3) -0.014(3) -0.026(3)
N15 0.118(5) 0.062(4) 0.087(4) 0.002(3) -0.044(4) -0.040(4)
C16 0.067(4) 0.078(5) 0.074(5) -0.007(4) -0.010(4) -0.041(4)
C4 0.065(4) 0.048(3) 0.057(4) 0.011(3) -0.027(3) -0.017(3)
C28 0.050(4) 0.075(4) 0.051(4) 0.007(3) -0.021(3) -0.027(3)
C5 0.078(5) 0.070(4) 0.054(4) 0.007(3) -0.031(4) -0.018(4)
C12 0.070(4) 0.056(4) 0.066(4) 0.006(3) -0.027(4) -0.007(3)
C23 0.133(8) 0.068(5) 0.078(6) 0.011(4) -0.060(6) -0.006(5)
N10 0.077(4) 0.081(4) 0.087(5) 0.017(3) -0.037(4) -0.018(3)
C27 0.048(4) 0.062(4) 0.054(4) -0.007(3) -0.018(3) -0.010(3)
C10 0.084(5) 0.069(5) 0.066(5) -0.003(4) -0.012(4) 0.004(4)
C33 0.074(5) 0.059(4) 0.073(5) 0.001(3) -0.026(4) -0.028(3)
C9 0.082(5) 0.058(4) 0.051(4) 0.001(3) -0.010(4) -0.011(4)
C26 0.060(4) 0.055(4) 0.064(4) -0.005(3) -0.017(3) -0.019(3)
C24 0.082(5) 0.067(4) 0.071(5) 0.020(4) -0.043(4) -0.023(4)
C13 0.076(5) 0.052(4) 0.067(4) 0.012(3) -0.014(4) -0.024(4)
C22 0.081(6) 0.113(7) 0.082(6) 0.010(4) -0.059(5) 0.007(4)
C14 0.098(6) 0.065(4) 0.066(5) -0.003(4) -0.001(4) -0.049(4)
C34 0.079(5) 0.080(5) 0.088(5) 0.014(4) -0.031(4) -0.051(4)
C2 0.111(7) 0.105(6) 0.066(5) 0.002(5) -0.048(5) -0.013(5)
C15 0.085(5) 0.084(5) 0.076(5) -0.016(4) 0.007(4) -0.059(5)
C21 0.077(5) 0.102(6) 0.074(5) 0.012(4) -0.041(4) -0.027(4)
C11 0.082(5) 0.064(4) 0.071(5) -0.007(4) -0.032(4) 0.007(4)
N5 0.143(6) 0.078(4) 0.085(5) 0.010(3) -0.058(4) -0.030(4)
C1 0.108(7) 0.093(6) 0.088(6) 0.022(5) -0.061(6) -0.037(5)
C3 0.109(6) 0.091(5) 0.054(4) -0.007(4) -0.036(4) -0.002(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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
N12 Co2 N7 88.63(18)
N12 Co2 N2 93.98(18)
N7 Co2 N2 175.24(19)
N12 Co2 N11 82.37(19)
N7 Co2 N11 93.88(18)
N2 Co2 N11 90.41(17)
N12 Co2 N6 94.01(18)
N7 Co2 N6 82.41(18)
N2 Co2 N6 93.43(17)
N11 Co2 N6 174.91(18)
N12 Co2 N1 174.65(19)
N7 Co2 N1 96.08(19)
N2 Co2 N1 81.49(19)
N11 Co2 N1 94.77(18)
N6 Co2 N1 89.12(18)
C30 N12 N13 107.9(4)
C30 N12 Co2 116.2(4)
N13 N12 Co2 135.8(4)
C18 N2 N3 109.0(4)
C18 N2 Co2 115.2(4)
N3 N2 Co2 135.6(3)
C7 N7 N8 107.1(4)
C7 N7 Co2 116.5(4)
N8 N7 Co2 134.8(4)
C13 N1 C17 119.7(5)
C13 N1 Co2 126.0(4)
C17 N1 Co2 114.3(4)
C12 N6 C8 118.6(5)
C12 N6 Co2 127.2(4)
C8 N6 Co2 114.2(3)
C31 N13 N12 102.4(4)
C25 N11 C29 118.2(5)
C25 N11 Co2 126.8(4)
C29 N11 Co2 115.0(3)
C19 N3 N2 102.2(4)
C30 N14 C31 100.8(4)
N13 C31 N14 115.5(5)
N13 C31 C32 122.1(5)
N14 C31 C32 122.4(5)
C6 N8 N7 103.5(4)
C36 C32 C33 117.4(5)
C36 C32 C31 122.5(5)
C33 C32 C31 120.2(5)
N9 C6 N8 114.0(5)
N9 C6 C4 123.6(5)
N8 C6 C4 122.3(5)
N11 C29 C28 122.6(5)
N11 C29 C30 111.7(5)
C28 C29 C30 125.5(6)
C7 N9 C6 101.7(4)
N14 C30 N12 113.4(5)
N14 C30 C29 131.9(5)
N12 C30 C29 114.7(5)
C18 N4 C19 101.7(4)
N4 C18 N2 111.7(5)
N4 C18 C17 132.3(5)
N2 C18 C17 115.9(5)
N3 C19 N4 115.4(5)
N3 C19 C20 121.4(6)
N4 C19 C20 123.1(5)
N9 C7 N7 113.6(5)
N9 C7 C8 132.7(5)
N7 C7 C8 113.5(5)
N1 C17 C16 121.4(6)
N1 C17 C18 112.7(5)
C16 C17 C18 125.9(6)
N15 C36 C32 123.8(6)
N15 C35 C34 124.4(7)
C24 C20 C21 116.0(6)
C24 C20 C19 124.5(5)
C21 C20 C19 119.5(6)
N6 C8 C9 121.8(5)
N6 C8 C7 113.1(5)
C9 C8 C7 125.1(5)
N11 C25 C26 121.7(6)
C36 N15 C35 116.2(6)
C17 C16 C15 118.9(7)
C3 C4 C5 115.3(6)
C3 C4 C6 121.5(6)
C5 C4 C6 123.2(5)
C29 C28 C27 118.3(6)
N10 C5 C4 125.2(6)
N6 C12 C11 121.9(6)
C22 C23 N5 124.5(8)
C1 N10 C5 115.8(6)
C26 C27 C28 119.3(6)
C11 C10 C9 119.7(6)
C34 C33 C32 120.3(6)
C10 C9 C8 118.3(6)
C27 C26 C25 119.9(5)
C20 C24 N5 124.9(6)
N1 C13 C14 120.8(6)
C21 C22 C23 118.8(7)
C15 C14 C13 119.6(7)
C35 C34 C33 117.9(7)
C1 C2 C3 119.7(7)
C14 C15 C16 119.5(7)
C22 C21 C20 121.5(8)
C10 C11 C12 119.6(6)
C23 N5 C24 114.3(7)
N10 C1 C2 123.2(7)
C2 C3 C4 120.8(7)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Co2 N12 1.869(4)
Co2 N7 1.888(4)
Co2 N2 1.903(4)
Co2 N11 1.941(4)
Co2 N6 1.956(4)
Co2 N1 1.974(5)
N12 C30 1.336(6)
N12 N13 1.372(5)
N2 C18 1.340(6)
N2 N3 1.365(6)
N7 C7 1.345(6)
N7 N8 1.367(5)
N1 C13 1.343(7)
N1 C17 1.347(7)
N6 C12 1.322(6)
N6 C8 1.353(6)
N13 C31 1.344(6)
N11 C25 1.348(6)
N11 C29 1.348(7)
N3 C19 1.345(6)
N14 C30 1.330(6)
N14 C31 1.359(6)
C31 C32 1.464(7)
N8 C6 1.360(6)
C32 C36 1.387(7)
C32 C33 1.393(8)
C6 N9 1.358(6)
C6 C4 1.446(7)
C29 C28 1.383(7)
C29 C30 1.452(7)
N9 C7 1.324(7)
N4 C18 1.338(6)
N4 C19 1.352(7)
C18 C17 1.425(8)
C19 C20 1.469(8)
C7 C8 1.462(7)
C17 C16 1.371(8)
C36 N15 1.344(7)
C35 N15 1.356(9)
C35 C34 1.366(9)
C20 C24 1.355(8)
C20 C21 1.404(8)
C8 C9 1.389(7)
C25 C26 1.386(7)
C16 C15 1.383(9)
C4 C3 1.375(8)
C4 C5 1.379(7)
C28 C27 1.390(7)
C5 N10 1.343(7)
C12 C11 1.392(8)
C23 C22 1.342(11)
C23 N5 1.368(9)
N10 C1 1.333(8)
C27 C26 1.359(8)
C10 C11 1.347(8)
C10 C9 1.380(8)
C33 C34 1.374(8)
C24 N5 1.375(8)
C13 C14 1.377(8)
C22 C21 1.338(9)
C14 C15 1.365(9)
C2 C1 1.343(10)
C2 C3 1.350(9)
|