data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Lee, Shim Sung' _publ_contact_author_email sslee@gnu.ac.kr _publ_section_title ; Preparation and characterisation of divalent hard and soft metal (M = Ca, Co, Cu, Zn, Cd, Hg, and Pb) complexes of 1,10-dithia-18-crown-6: structural versatility ; loop_ _publ_author_name I.-H.Park K.-M.Park S.S.Lee # Attachment '- IHDT-F.cif' data_compound1 _database_code_depnum_ccdc_archive 'CCDC 769787' #TrackingRef '- IHDT-F.cif' _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H24 Ca Cl2 O12 S2' _chemical_formula_sum 'C12 H24 Ca Cl2 O12 S2' _chemical_formula_weight 535.41 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' 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' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' 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' _cell_length_a 10.9749(7) _cell_length_b 12.3579(8) _cell_length_c 15.5092(10) _cell_angle_alpha 90.00 _cell_angle_beta 91.1070(10) _cell_angle_gamma 90.00 _cell_volume 2103.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 166(2) _cell_measurement_reflns_used 5050 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 30.04 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.691 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1112 _exptl_absorpt_coefficient_mu 0.809 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8234 _exptl_absorpt_correction_T_max 0.8681 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 166(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 10285 _diffrn_reflns_av_R_equivalents 0.0339 _diffrn_reflns_av_sigmaI/netI 0.0294 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 28.00 _reflns_number_total 2533 _reflns_number_gt 2277 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker APEX2' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0522P)^2^+7.7178P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2533 _refine_ls_number_parameters 132 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0497 _refine_ls_R_factor_gt 0.0453 _refine_ls_wR_factor_ref 0.1178 _refine_ls_wR_factor_gt 0.1140 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.471 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 Ca1 Ca 0.0000 0.10241(7) 0.2500 0.0186(2) Uani 1 2 d S . . S1 S -0.25995(8) 0.16847(8) 0.27810(6) 0.0290(2) Uani 1 1 d . . . O1 O -0.0927(2) -0.0133(2) 0.35640(17) 0.0281(6) Uani 1 1 d . . . O2 O 0.1521(2) -0.0006(2) 0.34200(15) 0.0256(5) Uani 1 1 d . . . C1 C -0.2830(3) 0.0784(4) 0.3687(2) 0.0330(8) Uani 1 1 d . . . H1A H -0.2522 0.1144 0.4219 0.040 Uiso 1 1 calc R . . H1B H -0.3716 0.0668 0.3751 0.040 Uiso 1 1 calc R . . C2 C -0.2219(3) -0.0301(3) 0.3613(2) 0.0311(8) Uani 1 1 d . . . H2A H -0.2405 -0.0752 0.4121 0.037 Uiso 1 1 calc R . . H2B H -0.2522 -0.0680 0.3089 0.037 Uiso 1 1 calc R . . C3 C -0.0213(4) -0.1080(3) 0.3743(3) 0.0326(8) Uani 1 1 d . . . H3A H -0.0132 -0.1521 0.3214 0.039 Uiso 1 1 calc R . . H3B H -0.0606 -0.1527 0.4188 0.039 Uiso 1 1 calc R . . C4 C 0.1013(4) -0.0706(4) 0.4058(2) 0.0322(8) Uani 1 1 d . . . H4A H 0.0933 -0.0312 0.4610 0.039 Uiso 1 1 calc R . . H4B H 0.1554 -0.1336 0.4157 0.039 Uiso 1 1 calc R . . C5 C 0.2556(3) 0.0569(4) 0.3778(2) 0.0310(8) Uani 1 1 d . . . H5A H 0.3011 0.0092 0.4184 0.037 Uiso 1 1 calc R . . H5B H 0.2272 0.1208 0.4103 0.037 Uiso 1 1 calc R . . C6 C 0.3384(3) 0.0930(3) 0.3074(3) 0.0321(8) Uani 1 1 d . . . H6A H 0.3775 0.0286 0.2820 0.038 Uiso 1 1 calc R . . H6B H 0.4036 0.1390 0.3329 0.038 Uiso 1 1 calc R . . Cl1 Cl -0.00134(8) 0.30575(7) 0.41996(5) 0.0240(2) Uani 1 1 d U . . O3 O 0.0282(4) 0.2166(4) 0.3675(3) 0.0693(11) Uani 1 1 d U . . O4 O -0.1189(3) 0.2872(4) 0.4542(3) 0.0591(10) Uani 1 1 d U . . O5 O -0.0015(4) 0.4000(4) 0.3695(4) 0.0874(16) Uani 1 1 d U . . O6 O 0.0898(4) 0.3126(4) 0.4852(2) 0.0666(12) 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 Ca1 0.0173(4) 0.0192(5) 0.0192(4) 0.000 0.0004(3) 0.000 S1 0.0228(4) 0.0278(5) 0.0362(5) -0.0048(4) -0.0020(3) 0.0008(3) O1 0.0232(12) 0.0307(14) 0.0304(13) 0.0090(11) -0.0003(10) -0.0029(10) O2 0.0244(12) 0.0320(14) 0.0204(11) 0.0025(10) -0.0007(9) 0.0031(10) C1 0.0245(17) 0.047(2) 0.0276(18) -0.0036(17) 0.0057(14) -0.0061(16) C2 0.0257(17) 0.040(2) 0.0277(17) 0.0058(16) 0.0020(14) -0.0091(16) C3 0.040(2) 0.0271(19) 0.0308(19) 0.0087(15) 0.0021(15) -0.0004(16) C4 0.0332(19) 0.038(2) 0.0250(17) 0.0110(16) 0.0018(14) 0.0070(16) C5 0.0245(17) 0.042(2) 0.0260(17) -0.0021(15) -0.0071(14) 0.0056(16) C6 0.0219(17) 0.040(2) 0.0337(19) 0.0032(16) -0.0063(14) 0.0009(15) Cl1 0.0287(4) 0.0205(4) 0.0230(4) -0.0020(3) 0.0038(3) -0.0015(3) O3 0.0646(15) 0.0699(15) 0.0733(15) -0.0434(12) -0.0025(12) 0.0055(12) O4 0.0462(19) 0.075(3) 0.057(2) -0.0094(19) 0.0239(16) -0.0188(18) O5 0.057(2) 0.068(3) 0.138(4) 0.062(3) 0.007(2) 0.006(2) O6 0.069(2) 0.093(3) 0.0372(17) 0.0057(18) -0.0180(17) -0.042(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Ca1 O3 2.320(4) 2 ? Ca1 O3 2.320(4) . ? Ca1 O1 2.422(3) 2 ? Ca1 O1 2.422(3) . ? Ca1 O2 2.520(2) 2 ? Ca1 O2 2.520(2) . ? Ca1 S1 3.0073(10) 2 ? Ca1 S1 3.0073(10) . ? S1 C1 1.814(4) . ? S1 C6 1.824(4) 2 ? O1 C3 1.433(5) . ? O1 C2 1.436(4) . ? O2 C4 1.435(4) . ? O2 C5 1.443(4) . ? C1 C2 1.505(6) . ? C3 C4 1.496(6) . ? C5 C6 1.502(6) . ? C6 S1 1.824(4) 2 ? Cl1 O5 1.403(4) . ? Cl1 O6 1.412(4) . ? Cl1 O3 1.412(4) . ? Cl1 O4 1.423(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Ca1 O3 105.1(3) 2 . ? O3 Ca1 O1 82.84(14) 2 2 ? O3 Ca1 O1 147.40(12) . 2 ? O3 Ca1 O1 147.40(12) 2 . ? O3 Ca1 O1 82.84(14) . . ? O1 Ca1 O1 107.66(14) 2 . ? O3 Ca1 O2 77.64(13) 2 2 ? O3 Ca1 O2 145.94(12) . 2 ? O1 Ca1 O2 66.34(8) 2 2 ? O1 Ca1 O2 78.76(9) . 2 ? O3 Ca1 O2 145.94(12) 2 . ? O3 Ca1 O2 77.64(13) . . ? O1 Ca1 O2 78.76(9) 2 . ? O1 Ca1 O2 66.34(8) . . ? O2 Ca1 O2 119.32(13) 2 . ? O3 Ca1 S1 80.41(11) 2 2 ? O3 Ca1 S1 80.58(11) . 2 ? O1 Ca1 S1 69.47(6) 2 2 ? O1 Ca1 S1 132.16(6) . 2 ? O2 Ca1 S1 132.46(6) 2 2 ? O2 Ca1 S1 66.38(6) . 2 ? O3 Ca1 S1 80.58(11) 2 . ? O3 Ca1 S1 80.41(11) . . ? O1 Ca1 S1 132.16(6) 2 . ? O1 Ca1 S1 69.47(6) . . ? O2 Ca1 S1 66.37(6) 2 . ? O2 Ca1 S1 132.46(6) . . ? S1 Ca1 S1 148.50(5) 2 . ? C1 S1 C6 100.31(19) . 2 ? C1 S1 Ca1 95.32(13) . . ? C6 S1 Ca1 101.05(13) 2 . ? C3 O1 C2 114.1(3) . . ? C3 O1 Ca1 112.2(2) . . ? C2 O1 Ca1 123.3(2) . . ? C4 O2 C5 110.2(3) . . ? C4 O2 Ca1 115.6(2) . . ? C5 O2 Ca1 118.5(2) . . ? C2 C1 S1 114.7(3) . . ? O1 C2 C1 108.5(3) . . ? O1 C3 C4 107.2(3) . . ? O2 C4 C3 108.7(3) . . ? O2 C5 C6 110.4(3) . . ? C5 C6 S1 113.4(3) . 2 ? O5 Cl1 O6 110.1(3) . . ? O5 Cl1 O3 108.9(3) . . ? O6 Cl1 O3 107.0(3) . . ? O5 Cl1 O4 110.5(3) . . ? O6 Cl1 O4 112.2(2) . . ? O3 Cl1 O4 108.0(3) . . ? Cl1 O3 Ca1 154.0(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.471 _refine_diff_density_min -1.016 _refine_diff_density_rms 0.094 ############################################################ data_compound2a _database_code_depnum_ccdc_archive 'CCDC 769788' #TrackingRef '- IHDT-F.cif' _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H30 Co O7 S2, 2(Cl O4)' _chemical_formula_sum 'C12 H30 Cl2 Co O15 S2' _chemical_formula_weight 608.31 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' 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' 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' _cell_length_a 14.6164(9) _cell_length_b 18.5780(12) _cell_length_c 18.1561(11) _cell_angle_alpha 90.00 _cell_angle_beta 104.362(2) _cell_angle_gamma 90.00 _cell_volume 4776.1(5) _cell_formula_units_Z 8 _cell_measurement_temperature 171(2) _cell_measurement_reflns_used 9847 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 27.45 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.692 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2520 _exptl_absorpt_coefficient_mu 1.185 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7030 _exptl_absorpt_correction_T_max 0.7641 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 171(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 44138 _diffrn_reflns_av_R_equivalents 0.0315 _diffrn_reflns_av_sigmaI/netI 0.0289 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 27.48 _reflns_number_total 10899 _reflns_number_gt 9222 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker APEX2' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0386P)^2^+4.0012P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10899 _refine_ls_number_parameters 577 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0425 _refine_ls_R_factor_gt 0.0341 _refine_ls_wR_factor_ref 0.0878 _refine_ls_wR_factor_gt 0.0836 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.186783(18) 0.535841(15) 0.916975(15) 0.01839(7) Uani 1 1 d . . . S1 S -0.06733(4) 0.46891(4) 0.76183(3) 0.03073(13) Uani 1 1 d . . . S2 S 0.27787(4) 0.51331(3) 1.04866(3) 0.02589(12) Uani 1 1 d . . . O1W O 0.21065(10) 0.44390(8) 0.86151(8) 0.0248(3) Uani 1 1 d . . . H1WA H 0.2654 0.4272 0.8719 0.030 Uiso 1 1 d R . . H1WB H 0.1728 0.4071 0.8575 0.030 Uiso 1 1 d R . . O2W O 0.29973(10) 0.58090(9) 0.88734(9) 0.0320(4) Uani 1 1 d . . . H2WA H 0.2939 0.6158 0.8555 0.038 Uiso 1 1 d R . . H2WB H 0.3553 0.5877 0.9186 0.038 Uiso 1 1 d R . . O3W O 0.06419(10) 0.49010(8) 0.93404(8) 0.0227(3) Uani 1 1 d . . . H3WA H 0.0760 0.4501 0.9556 0.027 Uiso 1 1 d R . . H3WB H 0.0253 0.4854 0.8915 0.027 Uiso 1 1 d R . . O1 O 0.08998(10) 0.58330(8) 0.82352(8) 0.0261(3) Uani 1 1 d . . . O2 O 0.15301(10) 0.63365(8) 0.96270(9) 0.0302(4) Uani 1 1 d . . . O3 O 0.14228(11) 0.37125(9) 1.00902(9) 0.0334(4) Uani 1 1 d . . . O4 O 0.06621(11) 0.34727(8) 0.85581(9) 0.0302(3) Uani 1 1 d . . . C1 C -0.02639(17) 0.54119(15) 0.71094(13) 0.0364(6) Uani 1 1 d . . . H1A H -0.0327 0.5257 0.6577 0.044 Uiso 1 1 calc R . . H1B H -0.0680 0.5835 0.7098 0.044 Uiso 1 1 calc R . . C2 C 0.07488(16) 0.56407(15) 0.74457(12) 0.0332(5) Uani 1 1 d . . . H2A H 0.1178 0.5242 0.7397 0.040 Uiso 1 1 calc R . . H2B H 0.0901 0.6058 0.7158 0.040 Uiso 1 1 calc R . . C3 C 0.06242(16) 0.65563(13) 0.83766(14) 0.0339(5) Uani 1 1 d . . . H3A H -0.0015 0.6662 0.8056 0.041 Uiso 1 1 calc R . . H3B H 0.1072 0.6908 0.8253 0.041 Uiso 1 1 calc R . . C4 C 0.06290(15) 0.66092(13) 0.91997(14) 0.0328(5) Uani 1 1 d . . . H4A H 0.0548 0.7116 0.9340 0.039 Uiso 1 1 calc R . . H4B H 0.0108 0.6320 0.9307 0.039 Uiso 1 1 calc R . . C5 C 0.16335(18) 0.63475(15) 1.04343(14) 0.0415(6) Uani 1 1 d . . . H5A H 0.1130 0.6057 1.0568 0.050 Uiso 1 1 calc R . . H5B H 0.1587 0.6847 1.0611 0.050 Uiso 1 1 calc R . . C6 C 0.25959(18) 0.60354(15) 1.08058(15) 0.0424(7) Uani 1 1 d . . . H6A H 0.2675 0.6027 1.1363 0.051 Uiso 1 1 calc R . . H6B H 0.3088 0.6356 1.0699 0.051 Uiso 1 1 calc R . . C7 C 0.20741(17) 0.46213(16) 1.10000(12) 0.0388(6) Uani 1 1 d . . . H7A H 0.2335 0.4688 1.1553 0.047 Uiso 1 1 calc R . . H7B H 0.1419 0.4807 1.0868 0.047 Uiso 1 1 calc R . . C8 C 0.20649(18) 0.38299(15) 1.08119(14) 0.0413(6) Uani 1 1 d . . . H8A H 0.2707 0.3672 1.0796 0.050 Uiso 1 1 calc R . . H8B H 0.1866 0.3547 1.1208 0.050 Uiso 1 1 calc R . . C9 C 0.15769(19) 0.30394(14) 0.97552(15) 0.0402(6) Uani 1 1 d . . . H9A H 0.1633 0.2648 1.0134 0.048 Uiso 1 1 calc R . . H9B H 0.2170 0.3059 0.9586 0.048 Uiso 1 1 calc R . . C10 C 0.07581(18) 0.28940(13) 0.90877(16) 0.0385(6) Uani 1 1 d . . . H10A H 0.0864 0.2438 0.8839 0.046 Uiso 1 1 calc R . . H10B H 0.0171 0.2845 0.9263 0.046 Uiso 1 1 calc R . . C11 C -0.00281(17) 0.33032(14) 0.78704(15) 0.0397(6) Uani 1 1 d . . . H11A H -0.0649 0.3220 0.7983 0.048 Uiso 1 1 calc R . . H11B H 0.0157 0.2858 0.7645 0.048 Uiso 1 1 calc R . . C12 C -0.01025(17) 0.39119(15) 0.73192(13) 0.0388(6) Uani 1 1 d . . . H12A H -0.0470 0.3754 0.6811 0.047 Uiso 1 1 calc R . . H12B H 0.0537 0.4049 0.7277 0.047 Uiso 1 1 calc R . . Co2 Co 0.309173(17) 0.446185(15) 0.578788(14) 0.01827(7) Uani 1 1 d . . . S3 S 0.23085(4) 0.49719(3) 0.45233(3) 0.02582(12) Uani 1 1 d . . . S4 S 0.55771(3) 0.48231(3) 0.75133(3) 0.02388(11) Uani 1 1 d . . . O4W O 0.43592(9) 0.49686(8) 0.58002(8) 0.0219(3) Uani 1 1 d . . . H4WA H 0.4721 0.4942 0.6237 0.026 Uiso 1 1 d R . . H4WB H 0.4184 0.5408 0.5710 0.026 Uiso 1 1 d R . . O5W O 0.19058(10) 0.39472(9) 0.58917(9) 0.0314(4) Uani 1 1 d . . . H5WA H 0.1894 0.3633 0.6224 0.038 Uiso 1 1 d R . . H5WB H 0.1364 0.3984 0.5596 0.038 Uiso 1 1 d R . . O6W O 0.28159(10) 0.52449(8) 0.65189(8) 0.0246(3) Uani 1 1 d . . . H6WA H 0.2279 0.5437 0.6366 0.030 Uiso 1 1 d R . . H6WB H 0.3187 0.5599 0.6653 0.030 Uiso 1 1 d R . . O5 O 0.34570(10) 0.36378(8) 0.51272(8) 0.0277(3) Uani 1 1 d . . . O6 O 0.39346(10) 0.37667(8) 0.66292(8) 0.0248(3) Uani 1 1 d . . . O8 O 0.36938(11) 0.62837(8) 0.53915(8) 0.0293(3) Uani 1 1 d . . . O7 O 0.43307(10) 0.61867(8) 0.69637(8) 0.0271(3) Uani 1 1 d . . . C13 C 0.25582(17) 0.41915(14) 0.40025(13) 0.0348(5) Uani 1 1 d . . . H13A H 0.2041 0.3838 0.3960 0.042 Uiso 1 1 calc R . . H13B H 0.2565 0.4343 0.3481 0.042 Uiso 1 1 calc R . . C14 C 0.34834(17) 0.38277(14) 0.43636(13) 0.0349(5) Uani 1 1 d . . . H14A H 0.3563 0.3391 0.4073 0.042 Uiso 1 1 calc R . . H14B H 0.4017 0.4158 0.4371 0.042 Uiso 1 1 calc R . . C15 C 0.42863(16) 0.32547(13) 0.55408(14) 0.0324(5) Uani 1 1 d . . . H15A H 0.4858 0.3556 0.5593 0.039 Uiso 1 1 calc R . . H15B H 0.4370 0.2805 0.5272 0.039 Uiso 1 1 calc R . . C16 C 0.41258(16) 0.30896(12) 0.63030(14) 0.0315(5) Uani 1 1 d . . . H16A H 0.3583 0.2758 0.6252 0.038 Uiso 1 1 calc R . . H16B H 0.4692 0.2859 0.6632 0.038 Uiso 1 1 calc R . . C17 C 0.41594(15) 0.37851(13) 0.74475(12) 0.0274(5) Uani 1 1 d . . . H17A H 0.4008 0.3313 0.7641 0.033 Uiso 1 1 calc R . . H17B H 0.3768 0.4155 0.7615 0.033 Uiso 1 1 calc R . . C18 C 0.51967(14) 0.39540(12) 0.77786(12) 0.0267(5) Uani 1 1 d . . . H18A H 0.5580 0.3576 0.7614 0.032 Uiso 1 1 calc R . . H18B H 0.5328 0.3931 0.8340 0.032 Uiso 1 1 calc R . . C19 C 0.49664(16) 0.54209(13) 0.80271(12) 0.0285(5) Uani 1 1 d . . . H19A H 0.4314 0.5247 0.7976 0.034 Uiso 1 1 calc R . . H19B H 0.5296 0.5421 0.8574 0.034 Uiso 1 1 calc R . . C20 C 0.49424(16) 0.61726(13) 0.77162(12) 0.0305(5) Uani 1 1 d . . . H20A H 0.4707 0.6511 0.8049 0.037 Uiso 1 1 calc R . . H20B H 0.5587 0.6324 0.7701 0.037 Uiso 1 1 calc R . . C21 C 0.43919(17) 0.68482(12) 0.65789(14) 0.0316(5) Uani 1 1 d . . . H21A H 0.5008 0.6878 0.6446 0.038 Uiso 1 1 calc R . . H21B H 0.4344 0.7259 0.6915 0.038 Uiso 1 1 calc R . . C22 C 0.36103(17) 0.68819(12) 0.58759(14) 0.0323(5) Uani 1 1 d . . . H22A H 0.2994 0.6861 0.6010 0.039 Uiso 1 1 calc R . . H22B H 0.3643 0.7341 0.5606 0.039 Uiso 1 1 calc R . . C23 C 0.30597(17) 0.63464(13) 0.46556(13) 0.0332(5) Uani 1 1 d . . . H23A H 0.3263 0.6745 0.4371 0.040 Uiso 1 1 calc R . . H23B H 0.2415 0.6454 0.4707 0.040 Uiso 1 1 calc R . . C24 C 0.30558(17) 0.56478(14) 0.42294(12) 0.0323(5) Uani 1 1 d . . . H24A H 0.3709 0.5462 0.4323 0.039 Uiso 1 1 calc R . . H24B H 0.2823 0.5738 0.3677 0.039 Uiso 1 1 calc R . . Cl1 Cl 0.05093(4) 0.62178(3) 0.53334(3) 0.03047(12) Uani 1 1 d . . . O9 O 0.10295(16) 0.68291(14) 0.5653(2) 0.1193(14) Uani 1 1 d . . . O10 O 0.0419(3) 0.6187(2) 0.45537(14) 0.1455(19) Uani 1 1 d . . . O11 O 0.09971(13) 0.55943(11) 0.56871(11) 0.0460(5) Uani 1 1 d . . . O12 O -0.04074(12) 0.62597(11) 0.54705(12) 0.0468(5) Uani 1 1 d . . . Cl2 Cl 0.45823(4) 0.37115(3) 0.97134(3) 0.02867(12) Uani 1 1 d . . . O13 O 0.4773(3) 0.30775(14) 0.93708(16) 0.1187(15) Uani 1 1 d . . . O14 O 0.41449(19) 0.35463(12) 1.03014(13) 0.0681(7) Uani 1 1 d . . . O15 O 0.40186(12) 0.41756(11) 0.91562(11) 0.0457(5) Uani 1 1 d . . . Cl3 Cl 0.27464(4) 0.74383(3) 0.27799(3) 0.02646(12) Uani 1 1 d . . . O16 O 0.5428(2) 0.4077(2) 1.0002(2) 0.160(2) Uani 1 1 d . . . O17 O 0.20754(11) 0.71262(10) 0.31421(10) 0.0387(4) Uani 1 1 d . . . O18 O 0.26434(17) 0.71347(12) 0.20456(11) 0.0601(6) Uani 1 1 d . . . O19 O 0.36805(12) 0.73167(13) 0.32380(12) 0.0573(6) Uani 1 1 d . . . O20 O 0.25888(13) 0.82052(9) 0.26952(10) 0.0407(4) Uani 1 1 d . . . Cl4 Cl 0.22511(4) 0.25835(3) 0.25370(3) 0.03022(12) Uani 1 1 d . . . O21 O 0.24703(19) 0.21304(17) 0.31712(18) 0.1010(11) Uani 1 1 d . . . O22 O 0.15861(13) 0.31055(11) 0.26347(12) 0.0544(5) Uani 1 1 d . . . O23 O 0.30865(13) 0.29209(12) 0.24513(13) 0.0552(5) Uani 1 1 d . . . O24 O 0.1842(2) 0.21915(17) 0.18717(18) 0.1012(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 Co1 0.01476(13) 0.01875(15) 0.02017(13) 0.00113(10) 0.00152(10) 0.00027(10) S1 0.0211(3) 0.0431(4) 0.0262(3) -0.0036(2) 0.0023(2) -0.0010(2) S2 0.0217(2) 0.0314(3) 0.0211(2) -0.0042(2) -0.00129(19) 0.0044(2) O1W 0.0201(7) 0.0241(8) 0.0301(8) -0.0028(6) 0.0061(6) -0.0003(6) O2W 0.0185(7) 0.0318(9) 0.0431(9) 0.0137(7) 0.0028(6) -0.0034(6) O3W 0.0210(7) 0.0250(8) 0.0213(7) 0.0029(6) 0.0039(5) -0.0011(6) O1 0.0221(7) 0.0280(9) 0.0250(7) 0.0083(6) 0.0001(6) 0.0023(6) O2 0.0204(7) 0.0246(9) 0.0400(9) -0.0055(7) -0.0033(6) 0.0051(6) O3 0.0350(9) 0.0304(9) 0.0326(8) 0.0094(7) 0.0043(7) 0.0025(7) O4 0.0252(8) 0.0228(8) 0.0403(9) -0.0039(7) 0.0038(6) -0.0069(6) C1 0.0288(12) 0.0512(16) 0.0238(11) 0.0081(10) -0.0039(9) 0.0001(11) C2 0.0265(11) 0.0482(16) 0.0225(10) 0.0098(10) 0.0017(8) -0.0014(10) C3 0.0246(11) 0.0262(13) 0.0479(14) 0.0147(11) 0.0035(10) 0.0062(9) C4 0.0212(10) 0.0243(13) 0.0483(14) -0.0004(10) 0.0001(9) 0.0082(9) C5 0.0390(14) 0.0398(16) 0.0385(13) -0.0205(12) -0.0039(11) 0.0114(12) C6 0.0364(13) 0.0403(15) 0.0398(13) -0.0209(12) -0.0111(10) 0.0093(11) C7 0.0325(12) 0.0664(19) 0.0175(10) 0.0002(11) 0.0063(9) 0.0024(12) C8 0.0376(13) 0.0520(17) 0.0307(12) 0.0208(12) 0.0017(10) 0.0025(12) C9 0.0466(15) 0.0268(14) 0.0496(15) 0.0128(11) 0.0163(12) 0.0064(11) C10 0.0401(14) 0.0221(13) 0.0566(16) 0.0013(11) 0.0186(12) -0.0053(11) C11 0.0291(12) 0.0357(15) 0.0490(15) -0.0186(12) 0.0000(10) -0.0062(10) C12 0.0322(12) 0.0512(17) 0.0306(12) -0.0161(11) 0.0033(10) -0.0008(11) Co2 0.01495(13) 0.01822(15) 0.01995(13) -0.00083(10) 0.00114(10) 0.00039(10) S3 0.0219(2) 0.0328(3) 0.0202(2) 0.0005(2) 0.00035(18) 0.0016(2) S4 0.0186(2) 0.0277(3) 0.0233(2) -0.0016(2) 0.00155(18) -0.0012(2) O4W 0.0198(7) 0.0218(8) 0.0226(7) 0.0009(6) 0.0024(5) 0.0006(6) O5W 0.0179(7) 0.0337(9) 0.0376(9) 0.0123(7) -0.0023(6) -0.0049(6) O6W 0.0211(7) 0.0238(8) 0.0283(7) -0.0028(6) 0.0049(6) 0.0010(6) O5 0.0250(7) 0.0265(9) 0.0289(8) -0.0066(6) 0.0018(6) 0.0038(6) O6 0.0234(7) 0.0204(8) 0.0262(7) 0.0005(6) -0.0023(6) 0.0037(6) O8 0.0359(8) 0.0226(8) 0.0268(8) 0.0042(6) 0.0027(6) 0.0047(7) O7 0.0280(8) 0.0208(8) 0.0292(8) -0.0028(6) 0.0009(6) -0.0038(6) C13 0.0351(12) 0.0422(15) 0.0231(10) -0.0101(10) -0.0002(9) -0.0008(11) C14 0.0357(12) 0.0404(15) 0.0286(11) -0.0126(10) 0.0081(9) 0.0030(11) C15 0.0254(11) 0.0257(13) 0.0437(13) -0.0067(10) 0.0041(9) 0.0081(9) C16 0.0277(11) 0.0190(12) 0.0434(13) -0.0015(10) 0.0005(9) 0.0046(9) C17 0.0220(10) 0.0314(13) 0.0261(10) 0.0067(9) 0.0004(8) -0.0017(9) C18 0.0218(10) 0.0283(12) 0.0263(10) 0.0059(9) -0.0011(8) 0.0009(9) C19 0.0287(11) 0.0326(13) 0.0221(10) -0.0054(9) 0.0024(8) 0.0023(9) C20 0.0279(11) 0.0294(13) 0.0299(11) -0.0093(10) -0.0012(9) -0.0028(9) C21 0.0342(12) 0.0201(12) 0.0400(13) -0.0019(10) 0.0082(10) -0.0035(9) C22 0.0372(13) 0.0185(12) 0.0398(13) 0.0018(10) 0.0069(10) 0.0030(10) C23 0.0352(12) 0.0319(14) 0.0299(11) 0.0111(10) 0.0029(9) 0.0022(10) C24 0.0333(12) 0.0416(15) 0.0213(10) 0.0062(10) 0.0058(9) -0.0016(11) Cl1 0.0236(2) 0.0369(3) 0.0309(3) 0.0059(2) 0.0068(2) 0.0077(2) O9 0.0348(12) 0.0436(15) 0.267(5) -0.006(2) 0.0145(19) -0.0109(11) O10 0.163(3) 0.242(5) 0.0370(13) 0.043(2) 0.0355(17) 0.134(3) O11 0.0382(10) 0.0468(12) 0.0474(11) 0.0046(9) -0.0002(8) 0.0214(9) O12 0.0279(9) 0.0442(12) 0.0724(13) 0.0071(10) 0.0201(9) 0.0065(8) Cl2 0.0213(2) 0.0315(3) 0.0322(3) 0.0042(2) 0.00490(19) 0.0000(2) O13 0.247(4) 0.0569(16) 0.091(2) 0.0354(15) 0.115(3) 0.081(2) O14 0.1061(19) 0.0527(14) 0.0661(14) 0.0074(11) 0.0605(14) 0.0125(13) O15 0.0311(9) 0.0482(12) 0.0508(11) 0.0092(9) -0.0030(8) 0.0088(8) Cl3 0.0243(2) 0.0291(3) 0.0253(2) -0.0034(2) 0.00487(19) 0.0032(2) O16 0.0736(19) 0.191(4) 0.159(3) 0.114(3) -0.079(2) -0.088(2) O17 0.0251(8) 0.0427(11) 0.0475(10) 0.0088(8) 0.0073(7) -0.0027(7) O18 0.0947(17) 0.0485(13) 0.0387(11) -0.0179(9) 0.0194(11) 0.0029(12) O19 0.0234(9) 0.0834(16) 0.0615(13) 0.0253(12) 0.0035(8) 0.0060(10) O20 0.0521(11) 0.0265(10) 0.0452(10) -0.0054(8) 0.0150(8) 0.0014(8) Cl4 0.0255(2) 0.0294(3) 0.0371(3) 0.0020(2) 0.0103(2) 0.0046(2) O21 0.0724(17) 0.122(2) 0.123(2) 0.095(2) 0.0509(16) 0.0387(16) O22 0.0364(10) 0.0509(13) 0.0717(14) -0.0177(11) 0.0058(9) 0.0174(9) O23 0.0354(10) 0.0586(14) 0.0757(15) 0.0178(11) 0.0215(10) -0.0047(9) O24 0.0834(19) 0.105(2) 0.117(2) -0.085(2) 0.0282(17) -0.0204(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O2W 2.0388(15) . ? Co1 O1W 2.0561(15) . ? Co1 O3W 2.0747(14) . ? Co1 O2 2.1067(16) . ? Co1 O1 2.1136(14) . ? Co1 S2 2.4668(6) . ? S1 C1 1.814(3) . ? S1 C12 1.817(3) . ? S2 C6 1.815(3) . ? S2 C7 1.819(3) . ? O1 C2 1.440(3) . ? O1 C3 1.444(3) . ? O2 C5 1.436(3) . ? O2 C4 1.444(2) . ? O3 C8 1.427(3) . ? O3 C9 1.433(3) . ? O4 C10 1.426(3) . ? O4 C11 1.432(3) . ? C1 C2 1.515(3) . ? C3 C4 1.496(3) . ? C5 C6 1.516(3) . ? C7 C8 1.509(4) . ? C9 C10 1.502(4) . ? C11 C12 1.496(4) . ? Co2 O5W 2.0289(15) . ? Co2 O4W 2.0732(14) . ? Co2 O6W 2.0751(15) . ? Co2 O5 2.0941(15) . ? Co2 O6 2.1414(14) . ? Co2 S3 2.4852(6) . ? S3 C13 1.817(2) . ? S3 C24 1.829(2) . ? S4 C18 1.811(2) . ? S4 C19 1.820(2) . ? O5 C14 1.440(3) . ? O5 C15 1.445(3) . ? O6 C17 1.440(2) . ? O6 C16 1.447(3) . ? O8 C23 1.430(3) . ? O8 C22 1.441(3) . ? O7 C21 1.427(3) . ? O7 C20 1.436(2) . ? C13 C14 1.508(3) . ? C15 C16 1.492(3) . ? C17 C18 1.519(3) . ? C19 C20 1.503(3) . ? C21 C22 1.488(3) . ? C23 C24 1.510(3) . ? Cl1 O10 1.390(2) . ? Cl1 O9 1.409(3) . ? Cl1 O12 1.4244(17) . ? Cl1 O11 1.4267(18) . ? Cl2 O13 1.392(2) . ? Cl2 O16 1.393(2) . ? Cl2 O14 1.408(2) . ? Cl2 O15 1.4256(18) . ? Cl3 O18 1.4208(19) . ? Cl3 O19 1.4295(18) . ? Cl3 O17 1.4320(17) . ? Cl3 O20 1.4453(19) . ? Cl4 O21 1.398(2) . ? Cl4 O24 1.410(2) . ? Cl4 O23 1.4151(19) . ? Cl4 O22 1.4152(18) . ? 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 O2W Co1 O1W 87.99(6) . . ? O2W Co1 O3W 173.47(6) . . ? O1W Co1 O3W 89.47(6) . . ? O2W Co1 O2 91.95(7) . . ? O1W Co1 O2 173.91(6) . . ? O3W Co1 O2 89.94(6) . . ? O2W Co1 O1 92.38(6) . . ? O1W Co1 O1 96.57(6) . . ? O3W Co1 O1 81.94(6) . . ? O2 Co1 O1 77.35(6) . . ? O2W Co1 S2 92.74(5) . . ? O1W Co1 S2 102.56(4) . . ? O3W Co1 S2 93.68(4) . . ? O2 Co1 S2 83.53(4) . . ? O1 Co1 S2 160.35(5) . . ? C1 S1 C12 101.66(13) . . ? C6 S2 C7 99.92(14) . . ? C6 S2 Co1 93.78(8) . . ? C7 S2 Co1 110.32(8) . . ? C2 O1 C3 115.29(17) . . ? C2 O1 Co1 127.04(14) . . ? C3 O1 Co1 113.96(13) . . ? C5 O2 C4 113.22(18) . . ? C5 O2 Co1 116.04(14) . . ? C4 O2 Co1 111.25(13) . . ? C8 O3 C9 112.74(19) . . ? C10 O4 C11 110.64(19) . . ? C2 C1 S1 114.53(16) . . ? O1 C2 C1 111.34(19) . . ? O1 C3 C4 107.84(18) . . ? O2 C4 C3 106.93(18) . . ? O2 C5 C6 107.4(2) . . ? C5 C6 S2 113.89(17) . . ? C8 C7 S2 111.59(17) . . ? O3 C8 C7 108.89(19) . . ? O3 C9 C10 108.8(2) . . ? O4 C10 C9 109.52(19) . . ? O4 C11 C12 109.61(19) . . ? C11 C12 S1 111.31(17) . . ? O5W Co2 O4W 174.11(6) . . ? O5W Co2 O6W 87.99(6) . . ? O4W Co2 O6W 89.40(6) . . ? O5W Co2 O5 93.08(7) . . ? O4W Co2 O5 89.09(6) . . ? O6W Co2 O5 175.19(6) . . ? O5W Co2 O6 90.18(6) . . ? O4W Co2 O6 84.93(6) . . ? O6W Co2 O6 97.77(6) . . ? O5 Co2 O6 77.55(6) . . ? O5W Co2 S3 93.27(5) . . ? O4W Co2 S3 92.44(4) . . ? O6W Co2 S3 101.86(4) . . ? O5 Co2 S3 82.76(4) . . ? O6 Co2 S3 160.16(4) . . ? C13 S3 C24 100.64(12) . . ? C13 S3 Co2 94.05(8) . . ? C24 S3 Co2 111.08(7) . . ? C18 S4 C19 100.70(11) . . ? C14 O5 C15 113.67(17) . . ? C14 O5 Co2 116.35(14) . . ? C15 O5 Co2 111.26(12) . . ? C17 O6 C16 115.16(17) . . ? C17 O6 Co2 131.70(13) . . ? C16 O6 Co2 111.57(12) . . ? C23 O8 C22 111.97(17) . . ? C21 O7 C20 112.44(17) . . ? C14 C13 S3 113.93(16) . . ? O5 C14 C13 107.03(19) . . ? O5 C15 C16 106.18(18) . . ? O6 C16 C15 106.97(18) . . ? O6 C17 C18 111.29(17) . . ? C17 C18 S4 114.90(15) . . ? C20 C19 S4 110.07(16) . . ? O7 C20 C19 108.98(17) . . ? O7 C21 C22 109.15(19) . . ? O8 C22 C21 109.13(19) . . ? O8 C23 C24 109.15(18) . . ? C23 C24 S3 111.55(16) . . ? O10 Cl1 O9 111.0(3) . . ? O10 Cl1 O12 108.94(18) . . ? O9 Cl1 O12 108.60(15) . . ? O10 Cl1 O11 109.59(17) . . ? O9 Cl1 O11 108.10(15) . . ? O12 Cl1 O11 110.63(12) . . ? O13 Cl2 O16 108.9(3) . . ? O13 Cl2 O14 109.47(15) . . ? O16 Cl2 O14 110.4(2) . . ? O13 Cl2 O15 109.82(16) . . ? O16 Cl2 O15 105.95(15) . . ? O14 Cl2 O15 112.26(14) . . ? O18 Cl3 O19 110.29(14) . . ? O18 Cl3 O17 110.18(13) . . ? O19 Cl3 O17 109.45(11) . . ? O18 Cl3 O20 108.33(12) . . ? O19 Cl3 O20 108.77(13) . . ? O17 Cl3 O20 109.80(11) . . ? O21 Cl4 O24 110.9(2) . . ? O21 Cl4 O23 109.24(15) . . ? O24 Cl4 O23 109.21(16) . . ? O21 Cl4 O22 109.49(16) . . ? O24 Cl4 O22 107.61(15) . . ? O23 Cl4 O22 110.39(13) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1WA O15 0.83 1.96 2.767(2) 161.1 . O1W H1WB O4 0.87 1.91 2.754(2) 163.3 . O2W H2WA O20 0.86 1.92 2.766(2) 166.5 4_576 O2W H2WB O16 0.88 1.82 2.680(3) 166.4 3_667 O3W H3WA O3 0.84 1.89 2.695(2) 161.7 . O3W H3WA O4 0.84 2.61 3.013(2) 110.7 . O4W H4WB O8 0.86 1.81 2.666(2) 171.5 . O5W H5WA O24 0.84 1.94 2.781(3) 171.7 4_566 O5W H5WB O12 0.84 2.14 2.894(3) 149.5 3_566 O6W H6WA O11 0.84 1.99 2.789(2) 157.0 . O6W H6WB O7 0.85 1.96 2.780(2) 162.3 . _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.967 _refine_diff_density_min -0.844 _refine_diff_density_rms 0.077 ############################################################ data_compound2b _database_code_depnum_ccdc_archive 'CCDC 769789' #TrackingRef '- IHDT-F.cif' _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H24 Co N4 O2, 2(Cl O4)' _chemical_formula_sum 'C28 H24 Cl2 Co N4 O10' _chemical_formula_weight 706.34 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' 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' _cell_length_a 10.455(2) _cell_length_b 14.087(3) _cell_length_c 11.199(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.144(4) _cell_angle_gamma 90.00 _cell_volume 1584.3(6) _cell_formula_units_Z 2 _cell_measurement_temperature 174(2) _cell_measurement_reflns_used 5987 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 27.36 _exptl_crystal_description block _exptl_crystal_colour yellow-orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.481 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 722 _exptl_absorpt_coefficient_mu 0.771 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7479 _exptl_absorpt_correction_T_max 0.8674 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 174(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 14571 _diffrn_reflns_av_R_equivalents 0.0315 _diffrn_reflns_av_sigmaI/netI 0.0278 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 27.49 _reflns_number_total 3632 _reflns_number_gt 3104 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker APEX2' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0447P)^2^+0.5283P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3632 _refine_ls_number_parameters 233 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0404 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.0893 _refine_ls_wR_factor_gt 0.0845 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.5000 0.0000 0.0000 0.02948(10) Uani 1 2 d S . . Cl1 Cl 0.08826(4) 0.21338(3) 0.74787(4) 0.04291(13) Uani 1 1 d . . . O1 O 0.1684(3) 0.1359(2) 0.7985(2) 0.0629(11) Uani 0.570(4) 1 d P A 1 O2 O 0.1622(3) 0.30069(19) 0.8177(3) 0.0612(9) Uani 0.570(4) 1 d P A 1 O3 O -0.0299(3) 0.2125(3) 0.7783(4) 0.0751(13) Uani 0.570(4) 1 d P A 1 O1' O 0.0146(8) 0.2705(5) 0.7919(5) 0.110(3) Uani 0.430(4) 1 d P A 2 O2' O 0.0547(5) 0.1097(3) 0.7756(4) 0.0697(14) Uani 0.430(4) 1 d P A 2 O3' O 0.2191(3) 0.2146(3) 0.7715(4) 0.0732(16) Uani 0.430(4) 1 d P A 2 O4 O 0.0564(2) 0.22024(13) 0.61506(15) 0.0868(7) Uani 1 1 d . A . N1 N 0.68974(14) 0.05633(11) 0.08483(13) 0.0401(3) Uani 1 1 d . . . C1 C 0.79204(17) 0.08992(12) 0.11771(15) 0.0356(4) Uani 1 1 d . . . C2 C 0.92128(16) 0.13367(12) 0.15628(16) 0.0354(4) Uani 1 1 d . . . C3 C 0.96986(17) 0.16743(13) 0.27684(18) 0.0418(4) Uani 1 1 d . . . H3A H 0.9190 0.1604 0.3347 0.050 Uiso 1 1 calc R . . C4 C 1.09282(19) 0.21131(15) 0.3120(2) 0.0523(5) Uani 1 1 d . . . H4A H 1.1275 0.2341 0.3945 0.063 Uiso 1 1 calc R . . C5 C 1.1645(2) 0.22186(16) 0.2276(2) 0.0589(6) Uani 1 1 d . . . H5A H 1.2484 0.2529 0.2520 0.071 Uiso 1 1 calc R . . C6 C 1.1173(2) 0.1885(2) 0.1087(2) 0.0680(7) Uani 1 1 d . . . H6A H 1.1689 0.1960 0.0516 0.082 Uiso 1 1 calc R . . C7 C 0.9945(2) 0.14396(18) 0.07144(19) 0.0552(5) Uani 1 1 d . . . H7A H 0.9611 0.1208 -0.0111 0.066 Uiso 1 1 calc R . . N2 N 0.44539(16) 0.01111(11) 0.16823(14) 0.0410(4) Uani 1 1 d . . . C8 C 0.40215(18) 0.02032(13) 0.25017(15) 0.0372(4) Uani 1 1 d . . . C9 C 0.34651(18) 0.02833(13) 0.35351(15) 0.0377(4) Uani 1 1 d . . . C10 C 0.4007(2) 0.09192(13) 0.44960(16) 0.0425(4) Uani 1 1 d . . . H10A H 0.4729 0.1319 0.4466 0.051 Uiso 1 1 calc R . . C11 C 0.3471(2) 0.09556(15) 0.54934(17) 0.0511(5) Uani 1 1 d . . . H11A H 0.3823 0.1388 0.6154 0.061 Uiso 1 1 calc R . . C12 C 0.2428(3) 0.03687(17) 0.55346(19) 0.0588(6) Uani 1 1 d . . . H12A H 0.2079 0.0392 0.6231 0.071 Uiso 1 1 calc R . . C13 C 0.1889(3) -0.02524(17) 0.4573(2) 0.0590(6) Uani 1 1 d . . . H13A H 0.1165 -0.0650 0.4607 0.071 Uiso 1 1 calc R . . C14 C 0.2401(2) -0.02967(14) 0.35601(18) 0.0465(4) Uani 1 1 d . . . H14A H 0.2029 -0.0718 0.2892 0.056 Uiso 1 1 calc R . . O1W O 0.42902(12) 0.13477(8) -0.04289(11) 0.0422(3) Uani 1 1 d . . . H1WA H 0.4571 0.1844 0.0063 0.051 Uiso 1 1 d R . . H1WB H 0.3600 0.1510 -0.0920 0.051 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 Co1 0.02927(17) 0.03448(18) 0.02516(15) -0.00053(11) 0.00834(11) 0.00051(12) Cl1 0.0354(2) 0.0542(3) 0.0432(2) 0.01414(19) 0.01778(17) 0.01384(19) O1 0.073(2) 0.0544(17) 0.0499(15) -0.0016(12) -0.0026(13) 0.0304(16) O2 0.073(2) 0.0521(16) 0.0662(17) -0.0202(13) 0.0328(14) -0.0244(14) O3 0.0365(14) 0.117(4) 0.079(2) -0.022(2) 0.0275(14) -0.0095(19) O1' 0.141(7) 0.125(5) 0.071(3) -0.003(4) 0.041(4) 0.099(5) O2' 0.080(3) 0.061(2) 0.061(2) 0.0221(18) 0.008(2) -0.025(2) O3' 0.0284(16) 0.108(4) 0.076(3) 0.040(2) 0.0028(16) -0.0060(19) O4 0.1530(19) 0.0693(11) 0.0470(9) 0.0216(8) 0.0427(10) 0.0490(12) N1 0.0358(8) 0.0450(9) 0.0384(7) -0.0023(6) 0.0087(6) -0.0016(7) C1 0.0351(9) 0.0383(9) 0.0334(8) 0.0010(7) 0.0095(7) 0.0042(7) C2 0.0287(8) 0.0380(9) 0.0398(9) 0.0055(7) 0.0100(7) 0.0026(7) C3 0.0347(9) 0.0455(10) 0.0458(10) -0.0048(8) 0.0121(7) 0.0024(8) C4 0.0366(10) 0.0488(11) 0.0651(13) -0.0079(9) 0.0037(9) 0.0014(8) C5 0.0336(10) 0.0515(12) 0.0855(16) 0.0190(11) 0.0065(10) -0.0043(9) C6 0.0452(12) 0.0950(19) 0.0713(15) 0.0323(14) 0.0286(11) -0.0003(12) C7 0.0456(11) 0.0826(16) 0.0395(10) 0.0098(10) 0.0155(8) -0.0010(10) N2 0.0439(8) 0.0493(9) 0.0317(7) -0.0012(6) 0.0137(6) 0.0020(7) C8 0.0415(9) 0.0405(9) 0.0300(8) 0.0007(7) 0.0106(7) 0.0053(7) C9 0.0478(10) 0.0376(9) 0.0309(8) 0.0038(7) 0.0160(7) 0.0120(8) C10 0.0513(10) 0.0423(10) 0.0331(8) 0.0018(7) 0.0104(7) 0.0100(8) C11 0.0747(14) 0.0476(11) 0.0318(9) -0.0010(8) 0.0163(9) 0.0217(10) C12 0.0910(17) 0.0547(12) 0.0440(11) 0.0090(9) 0.0408(11) 0.0238(12) C13 0.0776(16) 0.0519(12) 0.0624(13) 0.0063(10) 0.0442(12) 0.0044(11) C14 0.0608(12) 0.0408(10) 0.0448(10) -0.0026(8) 0.0260(9) 0.0031(9) O1W 0.0436(7) 0.0368(6) 0.0407(7) -0.0002(5) 0.0024(5) 0.0042(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1W 2.0463(12) . ? Co1 O1W 2.0464(12) 3_655 ? Co1 N1 2.1022(15) . ? Co1 N1 2.1023(15) 3_655 ? Co1 N2 2.1208(16) 3_655 ? Co1 N2 2.1209(16) . ? Cl1 O1' 1.302(4) . ? Cl1 O3' 1.319(3) . ? Cl1 O3 1.370(3) . ? Cl1 O1 1.397(2) . ? Cl1 O4 1.4342(16) . ? Cl1 O2 1.545(3) . ? Cl1 O2' 1.554(4) . ? N1 C1 1.133(2) . ? C1 C2 1.438(2) . ? C2 C7 1.384(3) . ? C2 C3 1.388(2) . ? C3 C4 1.381(3) . ? C4 C5 1.367(3) . ? C5 C6 1.368(4) . ? C6 C7 1.385(3) . ? N2 C8 1.137(2) . ? C8 C9 1.437(2) . ? C9 C14 1.387(3) . ? C9 C10 1.394(3) . ? C10 C11 1.383(3) . ? C11 C12 1.379(3) . ? C12 C13 1.380(3) . ? C13 C14 1.385(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1W Co1 O1W 180.0 . 3_655 ? O1W Co1 N1 89.48(6) . . ? O1W Co1 N1 90.52(6) 3_655 . ? O1W Co1 N1 90.52(6) . 3_655 ? O1W Co1 N1 89.48(6) 3_655 3_655 ? N1 Co1 N1 180.0 . 3_655 ? O1W Co1 N2 91.69(6) . 3_655 ? O1W Co1 N2 88.31(6) 3_655 3_655 ? N1 Co1 N2 88.63(6) . 3_655 ? N1 Co1 N2 91.37(6) 3_655 3_655 ? O1W Co1 N2 88.31(6) . . ? O1W Co1 N2 91.69(6) 3_655 . ? N1 Co1 N2 91.37(6) . . ? N1 Co1 N2 88.63(6) 3_655 . ? N2 Co1 N2 180.0 3_655 . ? O1' Cl1 O3' 127.3(5) . . ? O1' Cl1 O3 40.7(4) . . ? O3' Cl1 O3 155.1(3) . . ? O1' Cl1 O1 132.9(3) . . ? O3' Cl1 O1 57.1(2) . . ? O3 Cl1 O1 111.9(3) . . ? O1' Cl1 O4 111.1(3) . . ? O3' Cl1 O4 97.8(2) . . ? O3 Cl1 O4 107.0(2) . . ? O1 Cl1 O4 114.45(13) . . ? O1' Cl1 O2 65.2(4) . . ? O3' Cl1 O2 62.8(2) . . ? O3 Cl1 O2 103.9(2) . . ? O1 Cl1 O2 104.91(18) . . ? O4 Cl1 O2 114.25(14) . . ? O1' Cl1 O2' 108.4(4) . . ? O3' Cl1 O2' 104.5(3) . . ? O3 Cl1 O2' 70.9(3) . . ? O1 Cl1 O2' 47.7(2) . . ? O4 Cl1 O2' 105.69(17) . . ? O2 Cl1 O2' 139.15(19) . . ? C1 N1 Co1 172.36(14) . . ? N1 C1 C2 178.50(19) . . ? C7 C2 C3 120.62(17) . . ? C7 C2 C1 119.47(17) . . ? C3 C2 C1 119.88(16) . . ? C4 C3 C2 119.36(19) . . ? C5 C4 C3 119.8(2) . . ? C4 C5 C6 121.13(19) . . ? C5 C6 C7 120.1(2) . . ? C2 C7 C6 119.0(2) . . ? C8 N2 Co1 172.11(15) . . ? N2 C8 C9 177.9(2) . . ? C14 C9 C10 121.27(17) . . ? C14 C9 C8 118.47(17) . . ? C10 C9 C8 120.25(17) . . ? C11 C10 C9 118.60(19) . . ? C12 C11 C10 120.42(19) . . ? C11 C12 C13 120.64(19) . . ? C12 C13 C14 120.0(2) . . ? C13 C14 C9 119.04(19) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.322 _refine_diff_density_min -0.407 _refine_diff_density_rms 0.066 ############################################################ data_compound3 _database_code_depnum_ccdc_archive 'CCDC 769790' #TrackingRef '- IHDT-F.cif' _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H24 Cl2 Cu O12 S2, 2(C7 H5 N)' _chemical_formula_sum 'C26 H34 Cl2 Cu N2 O12 S2' _chemical_formula_weight 765.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' 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' _cell_length_a 24.822(5) _cell_length_b 7.9670(17) _cell_length_c 16.866(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.299(8) _cell_angle_gamma 90.00 _cell_volume 3270.6(11) _cell_formula_units_Z 4 _cell_measurement_temperature 172(2) _cell_measurement_reflns_used 7482 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 27.44 _exptl_crystal_description plate _exptl_crystal_colour dark-green _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.554 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1580 _exptl_absorpt_coefficient_mu 1.021 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6036 _exptl_absorpt_correction_T_max 0.9603 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 172(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 24911 _diffrn_reflns_av_R_equivalents 0.0630 _diffrn_reflns_av_sigmaI/netI 0.0658 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 0.84 _diffrn_reflns_theta_max 27.49 _reflns_number_total 7246 _reflns_number_gt 4796 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker APEX2' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1080P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7246 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0812 _refine_ls_R_factor_gt 0.0474 _refine_ls_wR_factor_ref 0.1723 _refine_ls_wR_factor_gt 0.1388 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.216266(15) 0.51064(5) 0.004983(19) 0.02394(15) Uani 1 1 d . . . Cl1 Cl 0.16381(3) 0.73309(11) -0.17482(4) 0.0259(2) Uani 1 1 d . . . Cl2 Cl 0.25892(4) 0.28387(12) 0.19492(4) 0.0328(2) Uani 1 1 d . . . S1 S 0.22706(4) 0.78503(12) 0.04733(4) 0.0299(2) Uani 1 1 d . . . S2 S 0.30066(3) 0.42582(13) -0.01854(4) 0.0280(2) Uani 1 1 d . . . O2 O 0.19117(8) 0.2780(3) -0.02549(11) 0.0244(5) Uani 1 1 d . . . O1 O 0.13859(9) 0.5340(3) 0.02136(12) 0.0290(5) Uani 1 1 d . . . O5 O 0.17750(10) 0.5741(3) -0.13363(12) 0.0328(6) Uani 1 1 d . . . O6 O 0.13960(9) 0.8432(3) -0.12369(13) 0.0354(6) Uani 1 1 d . . . O7 O 0.21246(11) 0.8078(4) -0.19187(16) 0.0492(7) Uani 1 1 d . . . O8 O 0.12506(11) 0.7009(4) -0.24875(12) 0.0426(7) Uani 1 1 d . . . O9 O 0.23297(14) 0.4161(4) 0.14250(14) 0.0632(10) Uani 1 1 d . . . O3 O 0.38532(10) 0.6785(4) -0.05127(17) 0.0491(7) Uani 1 1 d . . . O10 O 0.21663(11) 0.1779(4) 0.21429(17) 0.0549(8) Uani 1 1 d . . . O4 O 0.34252(11) 0.8347(4) 0.07987(15) 0.0519(8) Uani 1 1 d . . . O11 O 0.29273(13) 0.1906(4) 0.15146(19) 0.0636(9) Uani 1 1 d . . . O12 O 0.28982(12) 0.3592(5) 0.26600(13) 0.0596(9) Uani 1 1 d . . . C1 C 0.15837(16) 0.8085(5) 0.0712(2) 0.0380(9) Uani 1 1 d . . . H1A H 0.1609 0.8824 0.1190 0.046 Uiso 1 1 calc R . . H1B H 0.1339 0.8635 0.0252 0.046 Uiso 1 1 calc R . . C2 C 0.13337(16) 0.6429(5) 0.08844(19) 0.0380(9) Uani 1 1 d . . . H2A H 0.1533 0.5952 0.1402 0.046 Uiso 1 1 calc R . . H2B H 0.0943 0.6576 0.0917 0.046 Uiso 1 1 calc R . . C3 C 0.11421(14) 0.3684(5) 0.02392(19) 0.0349(8) Uani 1 1 d . . . H3A H 0.0737 0.3764 0.0148 0.042 Uiso 1 1 calc R . . H3B H 0.1277 0.3143 0.0769 0.042 Uiso 1 1 calc R . . C4 C 0.13183(13) 0.2702(5) -0.04282(19) 0.0313(8) Uani 1 1 d . . . H4A H 0.1191 0.1525 -0.0429 0.038 Uiso 1 1 calc R . . H4B H 0.1168 0.3210 -0.0961 0.038 Uiso 1 1 calc R . . C5 C 0.21865(13) 0.1994(4) -0.08475(16) 0.0269(7) Uani 1 1 d . . . H5A H 0.2100 0.2595 -0.1371 0.032 Uiso 1 1 calc R . . H5B H 0.2073 0.0806 -0.0935 0.032 Uiso 1 1 calc R . . C6 C 0.27930(13) 0.2117(5) -0.04844(17) 0.0297(8) Uani 1 1 d . . . H6A H 0.3007 0.1712 -0.0884 0.036 Uiso 1 1 calc R . . H6B H 0.2878 0.1377 -0.0005 0.036 Uiso 1 1 calc R . . C7 C 0.30965(14) 0.5160(5) -0.11469(18) 0.0337(9) Uani 1 1 d . . . H7A H 0.3355 0.4461 -0.1384 0.040 Uiso 1 1 calc R . . H7B H 0.2740 0.5182 -0.1531 0.040 Uiso 1 1 calc R . . C8 C 0.33183(14) 0.6913(5) -0.1009(2) 0.0386(9) Uani 1 1 d . . . H8A H 0.3340 0.7451 -0.1531 0.046 Uiso 1 1 calc R . . H8B H 0.3076 0.7598 -0.0736 0.046 Uiso 1 1 calc R . . C9 C 0.40525(16) 0.8284(6) -0.0110(3) 0.0529(11) Uani 1 1 d . . . H9A H 0.3843 0.9253 -0.0379 0.064 Uiso 1 1 calc R . . H9B H 0.4444 0.8440 -0.0140 0.064 Uiso 1 1 calc R . . C10 C 0.39961(17) 0.8213(7) 0.0753(3) 0.0627(14) Uani 1 1 d . . . H10A H 0.4147 0.7140 0.0997 0.075 Uiso 1 1 calc R . . H10B H 0.4205 0.9144 0.1058 0.075 Uiso 1 1 calc R . . C11 C 0.32830(18) 0.7482(6) 0.1455(2) 0.0517(12) Uani 1 1 d . . . H11A H 0.3529 0.7826 0.1964 0.062 Uiso 1 1 calc R . . H11B H 0.3325 0.6258 0.1385 0.062 Uiso 1 1 calc R . . C12 C 0.26985(17) 0.7884(5) 0.14918(18) 0.0423(10) Uani 1 1 d . . . H12A H 0.2680 0.9008 0.1735 0.051 Uiso 1 1 calc R . . H12B H 0.2558 0.7052 0.1837 0.051 Uiso 1 1 calc R . . N1 N 0.42930(17) 0.2307(5) -0.0486(2) 0.0618(11) Uani 1 1 d . . . C13 C 0.43995(16) 0.2822(6) 0.0167(3) 0.0474(10) Uani 1 1 d . . . C14 C 0.45315(15) 0.3459(6) 0.0984(2) 0.0436(10) Uani 1 1 d . . . C15 C 0.50339(16) 0.4266(6) 0.1253(3) 0.0552(12) Uani 1 1 d . . . H15A H 0.5291 0.4365 0.0906 0.066 Uiso 1 1 calc R . . C16 C 0.5153(2) 0.4913(7) 0.2020(4) 0.0731(17) Uani 1 1 d . . . H16A H 0.5491 0.5476 0.2203 0.088 Uiso 1 1 calc R . . C17 C 0.4778(2) 0.4748(7) 0.2532(3) 0.0683(15) Uani 1 1 d . . . H17A H 0.4862 0.5206 0.3062 0.082 Uiso 1 1 calc R . . C18 C 0.42851(18) 0.3921(7) 0.2271(2) 0.0611(14) Uani 1 1 d . . . H18A H 0.4032 0.3802 0.2623 0.073 Uiso 1 1 calc R . . C19 C 0.41603(15) 0.3266(6) 0.1498(2) 0.0481(11) Uani 1 1 d . . . H19A H 0.3824 0.2688 0.1318 0.058 Uiso 1 1 calc R . . N2 N 0.00388(16) -0.1544(5) 0.0850(2) 0.0567(10) Uani 1 1 d . . . C20 C 0.01369(16) -0.0238(6) 0.1122(2) 0.0399(9) Uani 1 1 d . . . C21 C 0.02480(13) 0.1423(5) 0.14477(17) 0.0308(8) Uani 1 1 d . . . C22 C 0.07362(14) 0.1774(5) 0.19998(18) 0.0349(9) Uani 1 1 d . . . H22A H 0.1001 0.0915 0.2160 0.042 Uiso 1 1 calc R . . C23 C 0.08289(14) 0.3368(5) 0.23074(18) 0.0363(9) Uani 1 1 d . . . H23A H 0.1160 0.3613 0.2677 0.044 Uiso 1 1 calc R . . C24 C 0.04478(15) 0.4600(5) 0.2084(2) 0.0370(9) Uani 1 1 d . . . H24A H 0.0516 0.5696 0.2303 0.044 Uiso 1 1 calc R . . C25 C -0.00372(15) 0.4275(6) 0.1543(2) 0.0420(10) Uani 1 1 d . . . H25A H -0.0300 0.5144 0.1397 0.050 Uiso 1 1 calc R . . C26 C -0.01386(14) 0.2696(6) 0.1215(2) 0.0401(10) Uani 1 1 d . . . H26A H -0.0468 0.2474 0.0836 0.048 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0304(2) 0.0219(3) 0.0196(2) -0.00314(16) 0.00508(15) -0.00083(18) Cl1 0.0317(4) 0.0265(5) 0.0189(3) 0.0038(3) 0.0032(3) -0.0027(4) Cl2 0.0491(5) 0.0276(5) 0.0243(3) 0.0058(3) 0.0135(3) 0.0039(4) S1 0.0481(5) 0.0220(5) 0.0204(3) -0.0006(3) 0.0086(3) -0.0013(4) S2 0.0275(4) 0.0338(6) 0.0207(3) -0.0033(4) 0.0000(3) -0.0004(4) O2 0.0294(11) 0.0234(14) 0.0200(9) -0.0019(9) 0.0040(8) -0.0017(10) O1 0.0393(12) 0.0248(14) 0.0261(10) 0.0001(10) 0.0144(9) 0.0007(11) O5 0.0485(13) 0.0263(15) 0.0222(9) 0.0068(10) 0.0037(9) 0.0034(12) O6 0.0416(13) 0.0287(16) 0.0368(11) -0.0067(12) 0.0100(10) 0.0028(12) O7 0.0449(14) 0.049(2) 0.0591(15) 0.0071(15) 0.0237(12) -0.0125(15) O8 0.0575(15) 0.0374(18) 0.0251(10) 0.0003(11) -0.0106(10) -0.0019(14) O9 0.119(3) 0.0343(19) 0.0276(12) 0.0072(13) -0.0066(14) 0.0077(19) O3 0.0328(13) 0.0379(19) 0.0737(17) -0.0185(16) 0.0032(12) -0.0040(13) O10 0.0528(16) 0.055(2) 0.0647(16) 0.0078(17) 0.0296(13) -0.0051(16) O4 0.0513(15) 0.057(2) 0.0470(13) 0.0005(15) 0.0079(12) 0.0150(16) O11 0.0674(19) 0.046(2) 0.089(2) -0.0118(18) 0.0450(17) -0.0005(17) O12 0.0705(18) 0.072(3) 0.0301(12) 0.0056(15) -0.0053(12) -0.0040(19) C1 0.054(2) 0.031(2) 0.0344(16) -0.0006(17) 0.0217(15) 0.0077(19) C2 0.055(2) 0.029(2) 0.0368(16) -0.0030(17) 0.0260(15) 0.007(2) C3 0.0384(17) 0.033(2) 0.0378(16) 0.0053(17) 0.0176(14) -0.0055(18) C4 0.0327(16) 0.028(2) 0.0338(15) -0.0029(15) 0.0084(13) -0.0079(16) C5 0.0421(17) 0.0184(19) 0.0198(12) -0.0064(13) 0.0053(12) -0.0027(16) C6 0.0385(17) 0.028(2) 0.0231(13) 0.0029(14) 0.0073(12) 0.0094(17) C7 0.0334(16) 0.043(3) 0.0261(14) -0.0004(16) 0.0080(13) -0.0029(17) C8 0.0344(17) 0.040(3) 0.0425(17) 0.0000(18) 0.0113(14) -0.0034(18) C9 0.0312(18) 0.047(3) 0.081(3) -0.014(3) 0.0141(18) -0.015(2) C10 0.043(2) 0.062(4) 0.073(3) -0.023(3) -0.011(2) 0.008(2) C11 0.074(3) 0.038(3) 0.0322(17) -0.0047(18) -0.0153(18) 0.001(2) C12 0.073(3) 0.029(2) 0.0232(15) -0.0092(15) 0.0044(15) -0.005(2) N1 0.072(3) 0.044(3) 0.070(2) -0.001(2) 0.014(2) -0.010(2) C13 0.043(2) 0.034(3) 0.066(3) 0.006(2) 0.0129(19) 0.000(2) C14 0.0359(18) 0.035(3) 0.058(2) 0.009(2) 0.0046(16) 0.0018(19) C15 0.037(2) 0.043(3) 0.086(3) -0.004(3) 0.012(2) 0.001(2) C16 0.042(2) 0.065(4) 0.104(4) -0.017(3) -0.005(3) 0.002(3) C17 0.063(3) 0.065(4) 0.068(3) -0.007(3) -0.010(2) 0.021(3) C18 0.051(2) 0.077(4) 0.054(2) 0.017(3) 0.0081(19) 0.027(3) C19 0.0343(18) 0.049(3) 0.058(2) 0.015(2) 0.0003(16) 0.007(2) N2 0.074(2) 0.038(2) 0.0548(19) -0.010(2) 0.0061(17) -0.009(2) C20 0.043(2) 0.041(3) 0.0364(17) -0.0008(19) 0.0077(15) -0.004(2) C21 0.0332(16) 0.031(2) 0.0308(14) -0.0008(16) 0.0123(12) -0.0072(17) C22 0.0336(17) 0.040(3) 0.0302(15) 0.0109(17) 0.0047(13) 0.0029(18) C23 0.0376(18) 0.043(3) 0.0266(14) 0.0027(17) 0.0016(13) -0.0083(19) C24 0.047(2) 0.031(2) 0.0366(17) -0.0074(17) 0.0178(15) -0.0097(19) C25 0.0345(18) 0.037(3) 0.056(2) 0.001(2) 0.0130(16) 0.0061(19) C26 0.0243(16) 0.047(3) 0.0471(19) 0.002(2) 0.0025(14) -0.0027(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 O2 1.991(2) . ? Cu1 O1 2.009(2) . ? Cu1 S1 2.2991(11) . ? Cu1 S2 2.3083(9) . ? Cu1 O9 2.396(2) . ? Cu1 O5 2.401(2) . ? Cl1 O7 1.425(3) . ? Cl1 O8 1.441(2) . ? Cl1 O6 1.442(2) . ? Cl1 O5 1.453(3) . ? Cl2 O12 1.423(3) . ? Cl2 O11 1.426(3) . ? Cl2 O10 1.434(3) . ? Cl2 O9 1.443(3) . ? S1 C12 1.834(3) . ? S1 C1 1.837(4) . ? S2 C7 1.827(3) . ? S2 C6 1.828(4) . ? O2 C4 1.446(4) . ? O2 C5 1.457(4) . ? O1 C2 1.451(4) . ? O1 C3 1.456(4) . ? O3 C9 1.414(5) . ? O3 C8 1.428(4) . ? O4 C11 1.406(5) . ? O4 C10 1.438(5) . ? C1 C2 1.510(6) . ? C3 C4 1.504(5) . ? C5 C6 1.513(4) . ? C7 C8 1.503(5) . ? C9 C10 1.489(6) . ? C11 C12 1.499(6) . ? N1 C13 1.156(5) . ? C13 C14 1.445(6) . ? C14 C19 1.391(5) . ? C14 C15 1.397(5) . ? C15 C16 1.369(7) . ? C16 C17 1.394(8) . ? C17 C18 1.384(7) . ? C18 C19 1.382(6) . ? N2 C20 1.144(5) . ? C20 C21 1.439(6) . ? C21 C26 1.399(5) . ? C21 C22 1.404(4) . ? C22 C23 1.374(6) . ? C23 C24 1.364(6) . ? C24 C25 1.385(5) . ? C25 C26 1.377(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Cu1 O1 82.05(9) . . ? O2 Cu1 S1 167.72(6) . . ? O1 Cu1 S1 85.74(8) . . ? O2 Cu1 S2 86.08(7) . . ? O1 Cu1 S2 168.07(8) . . ? S1 Cu1 S2 106.10(4) . . ? O2 Cu1 O9 86.75(10) . . ? O1 Cu1 O9 83.38(10) . . ? S1 Cu1 O9 90.61(8) . . ? S2 Cu1 O9 94.80(9) . . ? O2 Cu1 O5 84.22(9) . . ? O1 Cu1 O5 84.38(8) . . ? S1 Cu1 O5 95.87(7) . . ? S2 Cu1 O5 95.65(6) . . ? O9 Cu1 O5 165.68(10) . . ? O7 Cl1 O8 110.37(16) . . ? O7 Cl1 O6 109.60(17) . . ? O8 Cl1 O6 109.89(15) . . ? O7 Cl1 O5 109.42(16) . . ? O8 Cl1 O5 108.22(16) . . ? O6 Cl1 O5 109.30(14) . . ? O12 Cl2 O11 112.2(2) . . ? O12 Cl2 O10 110.75(17) . . ? O11 Cl2 O10 109.9(2) . . ? O12 Cl2 O9 108.1(2) . . ? O11 Cl2 O9 107.60(19) . . ? O10 Cl2 O9 108.1(2) . . ? C12 S1 C1 100.67(17) . . ? C12 S1 Cu1 108.41(14) . . ? C1 S1 Cu1 96.21(13) . . ? C7 S2 C6 101.61(16) . . ? C7 S2 Cu1 108.08(12) . . ? C6 S2 Cu1 95.55(11) . . ? C4 O2 C5 116.0(2) . . ? C4 O2 Cu1 110.3(2) . . ? C5 O2 Cu1 114.35(18) . . ? C2 O1 C3 114.7(2) . . ? C2 O1 Cu1 113.4(2) . . ? C3 O1 Cu1 109.6(2) . . ? Cl1 O5 Cu1 131.36(15) . . ? Cl2 O9 Cu1 142.57(19) . . ? C9 O3 C8 114.8(3) . . ? C11 O4 C10 114.1(3) . . ? C2 C1 S1 112.8(3) . . ? O1 C2 C1 105.6(3) . . ? O1 C3 C4 105.4(3) . . ? O2 C4 C3 105.1(3) . . ? O2 C5 C6 104.9(2) . . ? C5 C6 S2 112.6(2) . . ? C8 C7 S2 109.4(2) . . ? O3 C8 C7 107.2(3) . . ? O3 C9 C10 110.3(4) . . ? O4 C10 C9 109.4(3) . . ? O4 C11 C12 108.8(3) . . ? C11 C12 S1 110.2(2) . . ? N1 C13 C14 179.7(6) . . ? C19 C14 C15 120.5(4) . . ? C19 C14 C13 120.1(4) . . ? C15 C14 C13 119.5(4) . . ? C16 C15 C14 119.5(5) . . ? C15 C16 C17 120.3(5) . . ? C18 C17 C16 120.2(5) . . ? C19 C18 C17 120.1(4) . . ? C18 C19 C14 119.5(4) . . ? N2 C20 C21 178.4(5) . . ? C26 C21 C22 119.8(4) . . ? C26 C21 C20 119.4(3) . . ? C22 C21 C20 120.8(4) . . ? C23 C22 C21 119.6(4) . . ? C24 C23 C22 120.3(3) . . ? C23 C24 C25 120.9(4) . . ? C26 C25 C24 120.1(4) . . ? C25 C26 C21 119.3(3) . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 0.835 _refine_diff_density_min -0.647 _refine_diff_density_rms 0.129 ############################################################ data_compound4 _database_code_depnum_ccdc_archive 'CCDC 769791' #TrackingRef '- IHDT-F.cif' _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H30 O7 S2 Zn, 2(Cl O4)' _chemical_formula_sum 'C12 H30 Cl2 O15 S2 Zn' _chemical_formula_weight 614.75 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' 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' _cell_length_a 14.5666(11) _cell_length_b 18.5451(13) _cell_length_c 18.2069(12) _cell_angle_alpha 90.00 _cell_angle_beta 104.593(4) _cell_angle_gamma 90.00 _cell_volume 4759.7(6) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9982 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 27.43 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.716 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2544 _exptl_absorpt_coefficient_mu 1.500 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6143 _exptl_absorpt_correction_T_max 0.7242 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 39117 _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_sigmaI/netI 0.0381 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 27.00 _reflns_number_total 10383 _reflns_number_gt 8203 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker APEX2' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0374P)^2^+4.3741P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10383 _refine_ls_number_parameters 579 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0500 _refine_ls_R_factor_gt 0.0363 _refine_ls_wR_factor_ref 0.0939 _refine_ls_wR_factor_gt 0.0872 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.189007(19) 0.532858(16) 0.916982(16) 0.02036(8) Uani 1 1 d . . . S1 S -0.06656(5) 0.46939(4) 0.76120(4) 0.03204(17) Uani 1 1 d . . . S2 S 0.27825(5) 0.51363(4) 1.04978(4) 0.02729(15) Uani 1 1 d . . . O1W O 0.20952(13) 0.44241(10) 0.86017(10) 0.0262(4) Uani 1 1 d . . . H1WA H 0.2642 0.4257 0.8706 0.031 Uiso 1 1 d R . . H1WB H 0.1717 0.4056 0.8562 0.031 Uiso 1 1 d R . . O2W O 0.30176(13) 0.57842(10) 0.88572(11) 0.0325(5) Uani 1 1 d . . . H2WA H 0.2959 0.6134 0.8539 0.039 Uiso 1 1 d R . . H2WB H 0.3573 0.5852 0.9170 0.039 Uiso 1 1 d R . . O3W O 0.06250(12) 0.49035(10) 0.93391(10) 0.0239(4) Uani 1 1 d . . . H3WA H 0.0743 0.4504 0.9555 0.029 Uiso 1 1 d R . . H3WB H 0.0236 0.4856 0.8914 0.029 Uiso 1 1 d R . . O1 O 0.09306(12) 0.58345(10) 0.82455(10) 0.0272(4) Uani 1 1 d . . . O2 O 0.15514(13) 0.63566(10) 0.96286(12) 0.0321(5) Uani 1 1 d . . . O3 O 0.14245(14) 0.37153(11) 1.00820(11) 0.0353(5) Uani 1 1 d . . . O4 O 0.06573(13) 0.34683(10) 0.85612(12) 0.0315(4) Uani 1 1 d . . . C1 C -0.0242(2) 0.54125(18) 0.71146(17) 0.0371(7) Uani 1 1 d . . . H1A H -0.0304 0.5259 0.6584 0.045 Uiso 1 1 calc R . . H1B H -0.0655 0.5839 0.7102 0.045 Uiso 1 1 calc R . . C2 C 0.0780(2) 0.56360(17) 0.74578(15) 0.0331(7) Uani 1 1 d . . . H2A H 0.1207 0.5232 0.7415 0.040 Uiso 1 1 calc R . . H2B H 0.0940 0.6050 0.7170 0.040 Uiso 1 1 calc R . . C3 C 0.0648(2) 0.65584(15) 0.83784(18) 0.0349(7) Uani 1 1 d . . . H3A H 0.0008 0.6661 0.8052 0.042 Uiso 1 1 calc R . . H3B H 0.1099 0.6911 0.8257 0.042 Uiso 1 1 calc R . . C4 C 0.06427(19) 0.66180(16) 0.91953(18) 0.0345(7) Uani 1 1 d . . . H4A H 0.0550 0.7126 0.9328 0.041 Uiso 1 1 calc R . . H4B H 0.0124 0.6324 0.9301 0.041 Uiso 1 1 calc R . . C5 C 0.1637(2) 0.63516(18) 1.04291(18) 0.0420(8) Uani 1 1 d . . . H5A H 0.1127 0.6054 1.0546 0.050 Uiso 1 1 calc R . . H5B H 0.1583 0.6848 1.0613 0.050 Uiso 1 1 calc R . . C6 C 0.2597(2) 0.60386(17) 1.08086(19) 0.0425(8) Uani 1 1 d . . . H6A H 0.2670 0.6032 1.1364 0.051 Uiso 1 1 calc R . . H6B H 0.3095 0.6358 1.0707 0.051 Uiso 1 1 calc R . . C7 C 0.2063(2) 0.46244(18) 1.09971(17) 0.0392(8) Uani 1 1 d . . . H7A H 0.2316 0.4690 1.1551 0.047 Uiso 1 1 calc R . . H7B H 0.1405 0.4810 1.0856 0.047 Uiso 1 1 calc R . . C8 C 0.2057(2) 0.38331(18) 1.08089(18) 0.0425(8) Uani 1 1 d . . . H8A H 0.2705 0.3675 1.0804 0.051 Uiso 1 1 calc R . . H8B H 0.1849 0.3549 1.1198 0.051 Uiso 1 1 calc R . . C9 C 0.1570(2) 0.30353(17) 0.97580(19) 0.0422(8) Uani 1 1 d . . . H9A H 0.1619 0.2648 1.0140 0.051 Uiso 1 1 calc R . . H9B H 0.2168 0.3046 0.9593 0.051 Uiso 1 1 calc R . . C10 C 0.0752(2) 0.28903(16) 0.90930(19) 0.0401(8) Uani 1 1 d . . . H10A H 0.0858 0.2432 0.8847 0.048 Uiso 1 1 calc R . . H10B H 0.0163 0.2843 0.9265 0.048 Uiso 1 1 calc R . . C11 C -0.0035(2) 0.33038(17) 0.78701(18) 0.0405(8) Uani 1 1 d . . . H11A H -0.0661 0.3226 0.7977 0.049 Uiso 1 1 calc R . . H11B H 0.0146 0.2856 0.7647 0.049 Uiso 1 1 calc R . . C12 C -0.0098(2) 0.39111(18) 0.73222(18) 0.0402(8) Uani 1 1 d . . . H12A H -0.0465 0.3753 0.6813 0.048 Uiso 1 1 calc R . . H12B H 0.0547 0.4043 0.7286 0.048 Uiso 1 1 calc R . . Zn2 Zn 0.307299(19) 0.449533(16) 0.579913(17) 0.02050(8) Uani 1 1 d . . . S3 S 0.22971(5) 0.49745(4) 0.45164(4) 0.02784(15) Uani 1 1 d . . . S4 S 0.55754(4) 0.48273(4) 0.75185(4) 0.02518(15) Uani 1 1 d . . . O4W O 0.43779(12) 0.49697(9) 0.58006(10) 0.0236(4) Uani 1 1 d . . . H4WA H 0.4740 0.4943 0.6237 0.028 Uiso 1 1 d R . . H4WB H 0.4202 0.5409 0.5710 0.028 Uiso 1 1 d R . . O5W O 0.18849(13) 0.39759(11) 0.59274(12) 0.0341(5) Uani 1 1 d . . . H5WA H 0.1873 0.3662 0.6260 0.041 Uiso 1 1 d R . . H5WB H 0.1343 0.4012 0.5632 0.041 Uiso 1 1 d R . . O6W O 0.28329(13) 0.52647(10) 0.65369(10) 0.0262(4) Uani 1 1 d . . . H6WA H 0.2296 0.5457 0.6384 0.031 Uiso 1 1 d R . . H6WB H 0.3204 0.5619 0.6671 0.031 Uiso 1 1 d R . . O5 O 0.34253(13) 0.36220(10) 0.51269(11) 0.0311(4) Uani 1 1 d . . . O6 O 0.39133(12) 0.37779(9) 0.66233(10) 0.0258(4) Uani 1 1 d . . . O8 O 0.36918(14) 0.62847(10) 0.53927(11) 0.0318(5) Uani 1 1 d . . . O7 O 0.43364(13) 0.61983(10) 0.69575(11) 0.0290(4) Uani 1 1 d . . . C13 C 0.2541(2) 0.41892(17) 0.40078(17) 0.0366(7) Uani 1 1 d . . . H13A H 0.2017 0.3839 0.3965 0.044 Uiso 1 1 calc R . . H13B H 0.2551 0.4336 0.3487 0.044 Uiso 1 1 calc R . . C14 C 0.3464(2) 0.38190(17) 0.43725(17) 0.0368(7) Uani 1 1 d . . . H14A H 0.3545 0.3384 0.4079 0.044 Uiso 1 1 calc R . . H14B H 0.4005 0.4148 0.4391 0.044 Uiso 1 1 calc R . . C15 C 0.4263(2) 0.32478(16) 0.55500(18) 0.0355(7) Uani 1 1 d . . . H15A H 0.4833 0.3552 0.5598 0.043 Uiso 1 1 calc R . . H15B H 0.4352 0.2793 0.5292 0.043 Uiso 1 1 calc R . . C16 C 0.4103(2) 0.30955(14) 0.63096(18) 0.0338(7) Uani 1 1 d . . . H16A H 0.3557 0.2765 0.6262 0.041 Uiso 1 1 calc R . . H16B H 0.4672 0.2867 0.6642 0.041 Uiso 1 1 calc R . . C17 C 0.41348(19) 0.38051(15) 0.74370(16) 0.0287(6) Uani 1 1 d . . . H17A H 0.3969 0.3338 0.7633 0.034 Uiso 1 1 calc R . . H17B H 0.3747 0.4184 0.7596 0.034 Uiso 1 1 calc R . . C18 C 0.51759(19) 0.39617(15) 0.77788(16) 0.0291(6) Uani 1 1 d . . . H18A H 0.5557 0.3578 0.7619 0.035 Uiso 1 1 calc R . . H18B H 0.5300 0.3939 0.8339 0.035 Uiso 1 1 calc R . . C19 C 0.4967(2) 0.54339(15) 0.80241(16) 0.0304(6) Uani 1 1 d . . . H19A H 0.4310 0.5264 0.7971 0.036 Uiso 1 1 calc R . . H19B H 0.5297 0.5436 0.8571 0.036 Uiso 1 1 calc R . . C20 C 0.4952(2) 0.61832(16) 0.77091(17) 0.0343(7) Uani 1 1 d . . . H20A H 0.4722 0.6527 0.8039 0.041 Uiso 1 1 calc R . . H20B H 0.5601 0.6328 0.7694 0.041 Uiso 1 1 calc R . . C21 C 0.4409(2) 0.68563(15) 0.65729(17) 0.0341(7) Uani 1 1 d . . . H21A H 0.5028 0.6880 0.6442 0.041 Uiso 1 1 calc R . . H21B H 0.4366 0.7271 0.6906 0.041 Uiso 1 1 calc R . . C22 C 0.3620(2) 0.68908(15) 0.58657(18) 0.0362(7) Uani 1 1 d . . . H22A H 0.3001 0.6881 0.5997 0.043 Uiso 1 1 calc R . . H22B H 0.3662 0.7345 0.5591 0.043 Uiso 1 1 calc R . . C23 C 0.3065(2) 0.63474(16) 0.46479(17) 0.0364(7) Uani 1 1 d . . . H23A H 0.3282 0.6742 0.4366 0.044 Uiso 1 1 calc R . . H23B H 0.2416 0.6463 0.4688 0.044 Uiso 1 1 calc R . . C24 C 0.3060(2) 0.56458(17) 0.42319(16) 0.0342(7) Uani 1 1 d . . . H24A H 0.3715 0.5456 0.4335 0.041 Uiso 1 1 calc R . . H24B H 0.2835 0.5733 0.3679 0.041 Uiso 1 1 calc R . . Cl1 Cl 0.05156(5) 0.62101(4) 0.53399(4) 0.03096(16) Uani 1 1 d . . . O9 O 0.1042(2) 0.68194(16) 0.5668(3) 0.1174(16) Uani 1 1 d . . . O10 O 0.0429(3) 0.6182(3) 0.45628(17) 0.141(2) Uani 1 1 d . . . O11 O 0.09972(15) 0.55824(12) 0.56951(13) 0.0452(6) Uani 1 1 d . . . O12 O -0.04051(15) 0.62547(12) 0.54671(15) 0.0481(6) Uani 1 1 d . . . Cl2 Cl 0.45704(5) 0.37171(4) 0.97014(4) 0.02999(15) Uani 1 1 d . . . O13 O 0.4711(3) 0.30715(16) 0.93501(19) 0.1181(17) Uani 1 1 d . . . O14 O 0.4147(2) 0.35674(14) 1.02946(16) 0.0692(9) Uani 1 1 d . . . O15 O 0.40148(15) 0.41918(13) 0.91496(14) 0.0486(6) Uani 1 1 d . . . Cl3 Cl 0.27649(5) 0.74312(4) 0.27841(4) 0.02880(15) Uani 1 1 d . . . O16 O 0.5445(2) 0.4048(3) 0.9971(2) 0.156(2) Uani 1 1 d . . . O17 O 0.20900(14) 0.71136(12) 0.31357(13) 0.0418(5) Uani 1 1 d . . . O18 O 0.2665(2) 0.71346(14) 0.20526(14) 0.0672(8) Uani 1 1 d . . . O19 O 0.36995(16) 0.73125(16) 0.32473(15) 0.0638(8) Uani 1 1 d . . . O20 O 0.26043(17) 0.81978(11) 0.27040(13) 0.0439(5) Uani 1 1 d . . . Cl4 Cl 0.22339(5) 0.25913(4) 0.25296(4) 0.03148(16) Uani 1 1 d . . . O21 O 0.2443(2) 0.2127(2) 0.3153(2) 0.1014(13) Uani 1 1 d . . . O22 O 0.15736(17) 0.31156(14) 0.26321(15) 0.0592(7) Uani 1 1 d . . . O23 O 0.30759(16) 0.29263(14) 0.24573(15) 0.0561(7) Uani 1 1 d . . . O24 O 0.1825(2) 0.22133(19) 0.1859(2) 0.0954(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.01642(14) 0.02149(16) 0.02179(16) 0.00113(12) 0.00226(11) 0.00045(11) S1 0.0222(3) 0.0445(4) 0.0276(4) -0.0036(3) 0.0031(3) -0.0005(3) S2 0.0226(3) 0.0329(4) 0.0230(3) -0.0044(3) -0.0005(3) 0.0045(3) O1W 0.0216(9) 0.0252(10) 0.0321(11) -0.0032(8) 0.0075(8) -0.0003(7) O2W 0.0198(9) 0.0328(11) 0.0432(12) 0.0130(9) 0.0045(8) -0.0021(8) O3W 0.0219(9) 0.0257(10) 0.0232(10) 0.0017(8) 0.0042(7) -0.0001(7) O1 0.0219(9) 0.0307(10) 0.0261(10) 0.0086(8) 0.0010(8) 0.0043(8) O2 0.0223(9) 0.0265(10) 0.0432(12) -0.0052(9) 0.0001(9) 0.0053(8) O3 0.0372(11) 0.0315(11) 0.0352(12) 0.0080(9) 0.0054(9) 0.0022(9) O4 0.0265(10) 0.0244(10) 0.0422(12) -0.0037(9) 0.0058(9) -0.0057(8) C1 0.0285(15) 0.053(2) 0.0242(15) 0.0087(14) -0.0043(12) -0.0005(14) C2 0.0289(14) 0.0481(18) 0.0205(14) 0.0102(13) 0.0033(12) -0.0001(13) C3 0.0248(14) 0.0276(15) 0.050(2) 0.0158(13) 0.0059(13) 0.0065(12) C4 0.0230(14) 0.0281(15) 0.0485(19) 0.0006(13) 0.0015(13) 0.0080(11) C5 0.0406(17) 0.0405(18) 0.0395(19) -0.0187(15) -0.0001(14) 0.0115(14) C6 0.0371(17) 0.0386(18) 0.0420(19) -0.0200(15) -0.0082(14) 0.0080(14) C7 0.0358(16) 0.061(2) 0.0209(15) 0.0010(14) 0.0078(13) 0.0002(15) C8 0.0410(17) 0.053(2) 0.0307(17) 0.0196(15) 0.0044(14) 0.0033(15) C9 0.0473(19) 0.0303(16) 0.052(2) 0.0129(15) 0.0180(16) 0.0075(14) C10 0.0440(18) 0.0220(15) 0.059(2) 0.0017(14) 0.0221(16) -0.0054(13) C11 0.0300(15) 0.0386(18) 0.048(2) -0.0202(15) 0.0010(14) -0.0063(13) C12 0.0338(16) 0.051(2) 0.0338(18) -0.0190(15) 0.0054(14) -0.0021(14) Zn2 0.01720(14) 0.02060(15) 0.02208(16) -0.00071(12) 0.00191(12) 0.00034(11) S3 0.0232(3) 0.0363(4) 0.0215(3) 0.0001(3) 0.0011(3) 0.0026(3) S4 0.0195(3) 0.0296(4) 0.0247(3) -0.0020(3) 0.0025(3) -0.0014(3) O4W 0.0222(9) 0.0226(9) 0.0243(10) 0.0010(7) 0.0027(7) 0.0006(7) O5W 0.0192(9) 0.0357(11) 0.0419(12) 0.0142(9) -0.0025(8) -0.0051(8) O6W 0.0229(9) 0.0255(10) 0.0296(10) -0.0035(8) 0.0055(8) 0.0003(8) O5 0.0261(10) 0.0297(11) 0.0350(11) -0.0071(9) 0.0029(8) 0.0041(8) O6 0.0240(9) 0.0212(9) 0.0276(10) 0.0009(8) -0.0019(8) 0.0037(7) O8 0.0387(11) 0.0256(10) 0.0283(11) 0.0043(8) 0.0032(9) 0.0045(9) O7 0.0312(10) 0.0226(10) 0.0309(11) -0.0028(8) 0.0035(8) -0.0044(8) C13 0.0369(16) 0.0446(18) 0.0246(15) -0.0110(13) 0.0008(13) 0.0011(14) C14 0.0386(16) 0.0416(18) 0.0305(16) -0.0129(14) 0.0090(13) 0.0042(14) C15 0.0298(15) 0.0264(15) 0.0477(19) -0.0074(13) 0.0053(14) 0.0101(12) C16 0.0314(15) 0.0174(13) 0.0486(19) 0.0014(12) 0.0029(13) 0.0049(11) C17 0.0258(13) 0.0297(15) 0.0285(15) 0.0064(12) 0.0029(11) -0.0028(11) C18 0.0257(13) 0.0291(15) 0.0300(15) 0.0058(12) 0.0021(12) 0.0015(11) C19 0.0284(14) 0.0370(16) 0.0234(14) -0.0085(12) 0.0023(11) 0.0020(12) C20 0.0301(15) 0.0334(16) 0.0345(17) -0.0110(13) -0.0011(13) -0.0033(12) C21 0.0369(16) 0.0231(14) 0.0421(18) -0.0025(13) 0.0093(14) -0.0043(12) C22 0.0441(17) 0.0209(14) 0.0426(19) 0.0015(13) 0.0089(14) 0.0031(13) C23 0.0387(16) 0.0356(16) 0.0321(17) 0.0123(13) 0.0035(13) 0.0011(13) C24 0.0366(16) 0.0430(18) 0.0243(15) 0.0075(13) 0.0100(13) -0.0005(13) Cl1 0.0243(3) 0.0361(4) 0.0328(4) 0.0060(3) 0.0079(3) 0.0075(3) O9 0.0385(16) 0.0429(17) 0.257(5) -0.007(2) 0.011(2) -0.0118(13) O10 0.169(4) 0.224(5) 0.0394(18) 0.047(2) 0.043(2) 0.133(4) O11 0.0390(12) 0.0464(14) 0.0456(14) 0.0057(11) 0.0022(10) 0.0184(10) O12 0.0289(11) 0.0431(13) 0.0766(18) 0.0067(12) 0.0212(11) 0.0064(10) Cl2 0.0231(3) 0.0325(4) 0.0335(4) 0.0038(3) 0.0055(3) -0.0003(3) O13 0.251(5) 0.0540(18) 0.087(2) 0.0309(17) 0.113(3) 0.075(3) O14 0.112(2) 0.0516(16) 0.0661(18) 0.0069(14) 0.0638(18) 0.0133(16) O15 0.0333(12) 0.0496(14) 0.0570(15) 0.0115(12) 0.0000(11) 0.0098(10) Cl3 0.0273(3) 0.0309(3) 0.0277(3) -0.0030(3) 0.0060(3) 0.0039(3) O16 0.070(2) 0.200(5) 0.146(4) 0.112(3) -0.068(2) -0.086(3) O17 0.0266(10) 0.0464(13) 0.0510(14) 0.0090(11) 0.0071(10) -0.0034(9) O18 0.115(2) 0.0499(16) 0.0415(15) -0.0184(12) 0.0283(16) -0.0004(16) O19 0.0265(12) 0.093(2) 0.0679(18) 0.0336(16) 0.0048(11) 0.0046(13) O20 0.0574(14) 0.0286(11) 0.0485(14) -0.0069(10) 0.0187(11) 0.0013(10) Cl4 0.0266(3) 0.0306(4) 0.0390(4) 0.0019(3) 0.0115(3) 0.0045(3) O21 0.077(2) 0.118(3) 0.122(3) 0.091(2) 0.050(2) 0.035(2) O22 0.0392(13) 0.0579(16) 0.0758(19) -0.0226(14) 0.0060(12) 0.0173(12) O23 0.0381(13) 0.0610(16) 0.0735(18) 0.0151(14) 0.0220(12) -0.0076(12) O24 0.087(2) 0.093(2) 0.108(3) -0.072(2) 0.027(2) -0.0176(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1W 2.0319(18) . ? Zn1 O2W 2.0510(19) . ? Zn1 O3W 2.0973(17) . ? Zn1 O1 2.1167(17) . ? Zn1 O2 2.1870(19) . ? Zn1 S2 2.4656(7) . ? S1 C1 1.805(3) . ? S1 C12 1.813(3) . ? S2 C6 1.809(3) . ? S2 C7 1.819(3) . ? O1 C3 1.442(3) . ? O1 C2 1.443(3) . ? O2 C5 1.431(4) . ? O2 C4 1.443(3) . ? O3 C8 1.426(4) . ? O3 C9 1.431(4) . ? O4 C10 1.428(4) . ? O4 C11 1.433(3) . ? C1 C2 1.520(4) . ? C3 C4 1.494(4) . ? C5 C6 1.511(4) . ? C7 C8 1.506(5) . ? C9 C10 1.494(5) . ? C11 C12 1.492(5) . ? Zn2 O5W 2.0448(18) . ? Zn2 O6W 2.0492(18) . ? Zn2 O4W 2.0939(17) . ? Zn2 O6 2.1436(17) . ? Zn2 O5 2.1681(19) . ? Zn2 S3 2.4882(7) . ? S3 C13 1.809(3) . ? S3 C24 1.828(3) . ? S4 C18 1.811(3) . ? S4 C19 1.819(3) . ? O5 C14 1.436(4) . ? O5 C15 1.445(3) . ? O6 C17 1.435(3) . ? O6 C16 1.443(3) . ? O8 C22 1.436(3) . ? O8 C23 1.436(3) . ? O7 C21 1.424(3) . ? O7 C20 1.435(3) . ? C13 C14 1.507(4) . ? C15 C16 1.486(4) . ? C17 C18 1.515(4) . ? C19 C20 1.501(4) . ? C21 C22 1.496(4) . ? C23 C24 1.505(4) . ? Cl1 O10 1.389(3) . ? Cl1 O9 1.411(3) . ? Cl1 O12 1.420(2) . ? Cl1 O11 1.427(2) . ? Cl2 O16 1.388(3) . ? Cl2 O13 1.396(3) . ? Cl2 O14 1.400(3) . ? Cl2 O15 1.425(2) . ? Cl3 O18 1.414(2) . ? Cl3 O19 1.426(2) . ? Cl3 O17 1.428(2) . ? Cl3 O20 1.442(2) . ? Cl4 O21 1.396(3) . ? Cl4 O24 1.404(3) . ? Cl4 O23 1.410(2) . ? Cl4 O22 1.413(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1W Zn1 O2W 88.17(8) . . ? O1W Zn1 O3W 90.68(7) . . ? O2W Zn1 O3W 172.04(7) . . ? O1W Zn1 O1 96.52(7) . . ? O2W Zn1 O1 90.65(7) . . ? O3W Zn1 O1 81.65(7) . . ? O1W Zn1 O2 172.01(7) . . ? O2W Zn1 O2 91.17(8) . . ? O3W Zn1 O2 88.88(7) . . ? O1 Zn1 O2 75.52(7) . . ? O1W Zn1 S2 105.72(6) . . ? O2W Zn1 S2 94.04(6) . . ? O3W Zn1 S2 93.86(5) . . ? O1 Zn1 S2 157.39(6) . . ? O2 Zn1 S2 82.27(5) . . ? C1 S1 C12 101.92(16) . . ? C6 S2 C7 100.14(17) . . ? C6 S2 Zn1 95.13(11) . . ? C7 S2 Zn1 109.74(10) . . ? C3 O1 C2 115.2(2) . . ? C3 O1 Zn1 115.99(16) . . ? C2 O1 Zn1 125.57(16) . . ? C5 O2 C4 113.0(2) . . ? C5 O2 Zn1 114.40(17) . . ? C4 O2 Zn1 110.38(16) . . ? C8 O3 C9 112.9(2) . . ? C10 O4 C11 111.2(2) . . ? C2 C1 S1 114.7(2) . . ? O1 C2 C1 111.5(2) . . ? O1 C3 C4 108.0(2) . . ? O2 C4 C3 106.6(2) . . ? O2 C5 C6 107.5(3) . . ? C5 C6 S2 114.0(2) . . ? C8 C7 S2 111.4(2) . . ? O3 C8 C7 109.0(2) . . ? O3 C9 C10 108.8(2) . . ? O4 C10 C9 109.6(2) . . ? O4 C11 C12 109.7(2) . . ? C11 C12 S1 111.5(2) . . ? O5W Zn2 O6W 87.94(8) . . ? O5W Zn2 O4W 172.72(7) . . ? O6W Zn2 O4W 90.65(7) . . ? O5W Zn2 O6 88.74(7) . . ? O6W Zn2 O6 97.76(7) . . ? O4W Zn2 O6 84.37(7) . . ? O5W Zn2 O5 92.30(8) . . ? O6W Zn2 O5 173.67(7) . . ? O4W Zn2 O5 88.32(7) . . ? O6 Zn2 O5 75.93(7) . . ? O5W Zn2 S3 94.48(6) . . ? O6W Zn2 S3 104.74(5) . . ? O4W Zn2 S3 92.79(5) . . ? O6 Zn2 S3 157.36(5) . . ? O5 Zn2 S3 81.55(6) . . ? C13 S3 C24 101.03(15) . . ? C13 S3 Zn2 95.26(10) . . ? C24 S3 Zn2 110.15(10) . . ? C18 S4 C19 100.74(14) . . ? C14 O5 C15 113.6(2) . . ? C14 O5 Zn2 114.95(16) . . ? C15 O5 Zn2 110.23(16) . . ? C17 O6 C16 115.1(2) . . ? C17 O6 Zn2 129.86(16) . . ? C16 O6 Zn2 113.55(16) . . ? C22 O8 C23 112.2(2) . . ? C21 O7 C20 112.3(2) . . ? C14 C13 S3 114.2(2) . . ? O5 C14 C13 106.9(2) . . ? O5 C15 C16 106.2(2) . . ? O6 C16 C15 107.0(2) . . ? O6 C17 C18 111.9(2) . . ? C17 C18 S4 114.63(19) . . ? C20 C19 S4 110.0(2) . . ? O7 C20 C19 109.1(2) . . ? O7 C21 C22 108.9(2) . . ? O8 C22 C21 109.1(2) . . ? O8 C23 C24 109.1(2) . . ? C23 C24 S3 111.9(2) . . ? O10 Cl1 O9 111.2(3) . . ? O10 Cl1 O12 108.7(2) . . ? O9 Cl1 O12 108.61(18) . . ? O10 Cl1 O11 109.81(19) . . ? O9 Cl1 O11 107.98(18) . . ? O12 Cl1 O11 110.50(14) . . ? O16 Cl2 O13 108.2(3) . . ? O16 Cl2 O14 111.0(2) . . ? O13 Cl2 O14 109.09(18) . . ? O16 Cl2 O15 106.52(18) . . ? O13 Cl2 O15 109.24(19) . . ? O14 Cl2 O15 112.61(17) . . ? O18 Cl3 O19 110.70(18) . . ? O18 Cl3 O17 110.02(16) . . ? O19 Cl3 O17 109.49(14) . . ? O18 Cl3 O20 108.21(15) . . ? O19 Cl3 O20 108.56(16) . . ? O17 Cl3 O20 109.84(14) . . ? O21 Cl4 O24 110.9(3) . . ? O21 Cl4 O23 109.33(18) . . ? O24 Cl4 O23 109.12(19) . . ? O21 Cl4 O22 109.5(2) . . ? O24 Cl4 O22 107.73(18) . . ? O23 Cl4 O22 110.25(16) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1WA O15 0.83 1.96 2.756(3) 159.4 . O1W H1WB O4 0.87 1.89 2.731(3) 162.6 . O2W H2WA O20 0.86 1.93 2.775(3) 168.0 4_576 O2W H2WB O16 0.87 1.84 2.694(4) 163.8 3_667 O3W H3WA O3 0.84 1.89 2.692(3) 160.9 . O3W H3WA O4 0.84 2.62 3.021(3) 110.9 . O4W H4WB O8 0.86 1.82 2.669(3) 171.1 . O5W H5WA O24 0.84 1.97 2.797(3) 168.0 4_566 O5W H5WB O12 0.84 2.18 2.919(3) 147.5 3_566 O6W H6WA O11 0.84 2.00 2.790(3) 155.5 . O6W H6WB O7 0.85 1.93 2.745(3) 162.0 . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.981 _refine_diff_density_min -0.884 _refine_diff_density_rms 0.081 ############################################################ data_compound5 _database_code_depnum_ccdc_archive 'CCDC 769792' #TrackingRef '- IHDT-F.cif' _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H24 Cd Cl2 O12 S2' _chemical_formula_sum 'C12 H24 Cd Cl2 O12 S2' _chemical_formula_weight 607.73 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' 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' 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' _cell_length_a 11.2071(10) _cell_length_b 13.5832(13) _cell_length_c 13.9936(13) _cell_angle_alpha 90.00 _cell_angle_beta 103.817(4) _cell_angle_gamma 90.00 _cell_volume 2068.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9910 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 27.46 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.951 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 1.575 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7436 _exptl_absorpt_correction_T_max 0.8978 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 18715 _diffrn_reflns_av_R_equivalents 0.0360 _diffrn_reflns_av_sigmaI/netI 0.0315 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 27.49 _reflns_number_total 4708 _reflns_number_gt 4266 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker APEX2' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0292P)^2^+1.2549P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4708 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0296 _refine_ls_R_factor_gt 0.0260 _refine_ls_wR_factor_ref 0.0637 _refine_ls_wR_factor_gt 0.0619 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.893981(13) 0.702636(11) 0.185764(11) 0.01706(6) Uani 1 1 d . . . S1 S 0.70041(5) 0.80433(4) 0.20205(4) 0.02205(12) Uani 1 1 d . . . S2 S 1.11546(5) 0.66373(4) 0.29420(4) 0.02235(12) Uani 1 1 d . . . O1 O 0.72939(14) 0.62032(11) 0.07251(11) 0.0228(3) Uani 1 1 d . . . O2 O 0.91420(13) 0.51944(11) 0.18849(10) 0.0206(3) Uani 1 1 d . . . O3 O 1.02684(14) 0.68258(11) 0.07119(11) 0.0219(3) Uani 1 1 d . . . O4 O 0.84010(15) 0.82003(11) 0.04643(11) 0.0224(3) Uani 1 1 d . . . C1 C 0.5862(2) 0.71640(17) 0.14036(18) 0.0252(5) Uani 1 1 d . . . H1A H 0.5801 0.6628 0.1869 0.030 Uiso 1 1 calc R . . H1B H 0.5053 0.7496 0.1219 0.030 Uiso 1 1 calc R . . C2 C 0.6139(2) 0.67170(18) 0.04884(17) 0.0262(5) Uani 1 1 d . . . H2A H 0.5475 0.6254 0.0184 0.031 Uiso 1 1 calc R . . H2B H 0.6169 0.7244 0.0006 0.031 Uiso 1 1 calc R . . C3 C 0.7159(2) 0.51671(16) 0.08513(17) 0.0256(5) Uani 1 1 d . . . H3A H 0.6614 0.4877 0.0255 0.031 Uiso 1 1 calc R . . H3B H 0.6799 0.5038 0.1420 0.031 Uiso 1 1 calc R . . C4 C 0.8417(2) 0.47334(16) 0.10257(16) 0.0238(5) Uani 1 1 d . . . H4A H 0.8384 0.4013 0.1126 0.029 Uiso 1 1 calc R . . H4B H 0.8773 0.4858 0.0454 0.029 Uiso 1 1 calc R . . C5 C 1.0354(2) 0.47955(17) 0.21665(17) 0.0252(5) Uani 1 1 d . . . H5A H 1.0777 0.4885 0.1627 0.030 Uiso 1 1 calc R . . H5B H 1.0314 0.4082 0.2299 0.030 Uiso 1 1 calc R . . C6 C 1.1050(2) 0.53169(17) 0.30746(16) 0.0233(5) Uani 1 1 d . . . H6A H 1.1892 0.5043 0.3265 0.028 Uiso 1 1 calc R . . H6B H 1.0646 0.5178 0.3617 0.028 Uiso 1 1 calc R . . C7 C 1.2080(2) 0.6710(2) 0.20375(19) 0.0320(6) Uani 1 1 d . . . H7A H 1.2865 0.7043 0.2340 0.038 Uiso 1 1 calc R . . H7B H 1.2276 0.6034 0.1859 0.038 Uiso 1 1 calc R . . C8 C 1.1461(2) 0.72550(19) 0.11125(17) 0.0262(5) Uani 1 1 d . . . H8A H 1.1369 0.7959 0.1265 0.031 Uiso 1 1 calc R . . H8B H 1.1969 0.7211 0.0625 0.031 Uiso 1 1 calc R . . C9 C 0.9681(2) 0.72234(17) -0.02407(16) 0.0252(5) Uani 1 1 d . . . H9A H 0.8977 0.6801 -0.0554 0.030 Uiso 1 1 calc R . . H9B H 1.0272 0.7221 -0.0666 0.030 Uiso 1 1 calc R . . C10 C 0.9237(2) 0.82535(17) -0.01573(16) 0.0233(5) Uani 1 1 d . . . H10A H 0.9935 0.8693 0.0133 0.028 Uiso 1 1 calc R . . H10B H 0.8819 0.8511 -0.0814 0.028 Uiso 1 1 calc R . . C11 C 0.7951(2) 0.91414(16) 0.06672(17) 0.0244(5) Uani 1 1 d . . . H11A H 0.7727 0.9535 0.0055 0.029 Uiso 1 1 calc R . . H11B H 0.8597 0.9500 0.1147 0.029 Uiso 1 1 calc R . . C12 C 0.6837(2) 0.89969(17) 0.10822(18) 0.0274(5) Uani 1 1 d . . . H12A H 0.6127 0.8829 0.0535 0.033 Uiso 1 1 calc R . . H12B H 0.6649 0.9628 0.1368 0.033 Uiso 1 1 calc R . . Cl1 Cl 0.81340(5) 0.67458(4) 0.42737(4) 0.02006(11) Uani 1 1 d . . . O5 O 0.8725(2) 0.64221(14) 0.35214(14) 0.0485(6) Uani 1 1 d . . . O6 O 0.83683(17) 0.77669(12) 0.44615(13) 0.0325(4) Uani 1 1 d . . . O7 O 0.68501(17) 0.65840(15) 0.39401(15) 0.0449(5) Uani 1 1 d . . . O8 O 0.86140(18) 0.61914(13) 0.51478(13) 0.0370(4) Uani 1 1 d . . . Cl2 Cl 1.08876(5) 0.94140(4) 0.27860(4) 0.02419(12) Uani 1 1 d . . . O9 O 0.98874(16) 0.87189(13) 0.26657(13) 0.0344(4) Uani 1 1 d . . . O10 O 1.0711(2) 1.01672(15) 0.34476(15) 0.0473(5) Uani 1 1 d . . . O11 O 1.08995(17) 0.98304(15) 0.18457(13) 0.0424(5) Uani 1 1 d . . . O12 O 1.20233(17) 0.89243(15) 0.31738(16) 0.0459(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.01533(10) 0.01547(9) 0.02084(9) 0.00153(5) 0.00523(7) 0.00153(6) S1 0.0216(3) 0.0207(3) 0.0244(3) -0.0012(2) 0.0067(2) 0.0028(2) S2 0.0205(3) 0.0215(3) 0.0236(3) 0.0036(2) 0.0022(2) -0.0005(2) O1 0.0206(8) 0.0167(8) 0.0288(8) -0.0007(6) 0.0016(6) 0.0001(6) O2 0.0187(8) 0.0178(8) 0.0245(8) -0.0025(6) 0.0039(6) 0.0024(6) O3 0.0206(8) 0.0219(8) 0.0249(8) 0.0028(6) 0.0086(6) 0.0007(6) O4 0.0248(8) 0.0178(7) 0.0268(8) 0.0028(6) 0.0108(7) 0.0024(6) C1 0.0157(11) 0.0265(12) 0.0324(12) 0.0028(9) 0.0036(9) -0.0009(9) C2 0.0184(12) 0.0261(12) 0.0301(12) -0.0012(10) -0.0019(9) 0.0018(9) C3 0.0249(12) 0.0172(11) 0.0327(12) -0.0016(9) 0.0030(10) -0.0034(9) C4 0.0262(12) 0.0181(11) 0.0262(11) -0.0040(9) 0.0044(9) -0.0008(9) C5 0.0216(12) 0.0203(11) 0.0340(12) -0.0002(9) 0.0072(10) 0.0070(9) C6 0.0216(12) 0.0204(11) 0.0273(11) 0.0060(9) 0.0044(9) 0.0046(9) C7 0.0175(12) 0.0413(15) 0.0390(13) 0.0154(12) 0.0101(10) 0.0031(11) C8 0.0173(11) 0.0320(13) 0.0307(12) 0.0076(10) 0.0087(9) -0.0003(10) C9 0.0281(13) 0.0289(12) 0.0205(10) -0.0015(9) 0.0098(9) 0.0013(10) C10 0.0243(12) 0.0267(12) 0.0195(10) 0.0054(9) 0.0062(9) 0.0005(9) C11 0.0269(12) 0.0157(10) 0.0299(11) 0.0044(9) 0.0049(9) 0.0035(9) C12 0.0270(12) 0.0191(11) 0.0360(12) 0.0072(9) 0.0072(10) 0.0091(9) Cl1 0.0207(3) 0.0188(2) 0.0225(2) 0.00109(19) 0.0088(2) 0.0011(2) O5 0.0782(15) 0.0337(10) 0.0500(11) 0.0125(9) 0.0480(11) 0.0252(10) O6 0.0384(11) 0.0176(8) 0.0387(10) 0.0007(7) 0.0034(8) -0.0015(7) O7 0.0259(10) 0.0448(12) 0.0607(13) -0.0046(10) 0.0038(9) -0.0077(9) O8 0.0474(11) 0.0283(9) 0.0310(9) 0.0107(7) 0.0008(8) -0.0026(8) Cl2 0.0212(3) 0.0224(3) 0.0278(3) -0.0002(2) 0.0034(2) -0.0039(2) O9 0.0280(9) 0.0268(9) 0.0457(10) 0.0034(8) 0.0036(8) -0.0097(7) O10 0.0551(13) 0.0383(11) 0.0518(12) -0.0183(9) 0.0196(10) -0.0092(10) O11 0.0398(11) 0.0520(12) 0.0342(10) 0.0116(9) 0.0064(8) -0.0120(9) O12 0.0239(10) 0.0471(12) 0.0625(13) 0.0121(10) 0.0021(9) 0.0041(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O1 2.4016(15) . ? Cd1 O3 2.4500(15) . ? Cd1 O4 2.4792(15) . ? Cd1 O2 2.4982(15) . ? Cd1 O5 2.5339(17) . ? Cd1 S1 2.6273(6) . ? Cd1 S2 2.6351(6) . ? S1 C1 1.812(2) . ? S1 C12 1.822(2) . ? S2 C6 1.810(2) . ? S2 C7 1.820(2) . ? O1 C3 1.431(3) . ? O1 C2 1.437(3) . ? O2 C4 1.425(3) . ? O2 C5 1.427(3) . ? O3 C8 1.443(3) . ? O3 C9 1.443(3) . ? O4 C10 1.425(3) . ? O4 C11 1.427(3) . ? C1 C2 1.515(3) . ? C3 C4 1.493(3) . ? C5 C6 1.500(3) . ? C7 C8 1.509(3) . ? C9 C10 1.499(3) . ? C11 C12 1.510(3) . ? Cl1 O7 1.4198(19) . ? Cl1 O6 1.4243(17) . ? Cl1 O8 1.4278(17) . ? Cl1 O5 1.4396(17) . ? Cl2 O12 1.4237(19) . ? Cl2 O10 1.4249(19) . ? Cl2 O11 1.4353(18) . ? Cl2 O9 1.4444(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cd1 O3 90.43(5) . . ? O1 Cd1 O4 77.06(5) . . ? O3 Cd1 O4 68.21(5) . . ? O1 Cd1 O2 66.35(5) . . ? O3 Cd1 O2 80.34(5) . . ? O4 Cd1 O2 131.06(5) . . ? O1 Cd1 O5 103.23(7) . . ? O3 Cd1 O5 140.48(6) . . ? O4 Cd1 O5 150.71(5) . . ? O2 Cd1 O5 72.03(5) . . ? O1 Cd1 S1 77.41(4) . . ? O3 Cd1 S1 139.35(4) . . ? O4 Cd1 S1 71.28(4) . . ? O2 Cd1 S1 126.60(4) . . ? O5 Cd1 S1 80.14(4) . . ? O1 Cd1 S2 139.11(4) . . ? O3 Cd1 S2 73.65(4) . . ? O4 Cd1 S2 126.93(4) . . ? O2 Cd1 S2 73.85(4) . . ? O5 Cd1 S2 71.89(5) . . ? S1 Cd1 S2 137.667(19) . . ? C1 S1 C12 100.72(11) . . ? C1 S1 Cd1 96.67(8) . . ? C12 S1 Cd1 104.83(8) . . ? C6 S2 C7 100.77(12) . . ? C6 S2 Cd1 100.51(7) . . ? C7 S2 Cd1 101.73(8) . . ? C3 O1 C2 112.95(17) . . ? C3 O1 Cd1 117.63(13) . . ? C2 O1 Cd1 115.67(12) . . ? C4 O2 C5 112.30(16) . . ? C4 O2 Cd1 113.17(12) . . ? C5 O2 Cd1 117.33(12) . . ? C8 O3 C9 112.54(16) . . ? C8 O3 Cd1 110.61(13) . . ? C9 O3 Cd1 110.40(12) . . ? C10 O4 C11 113.03(16) . . ? C10 O4 Cd1 116.14(12) . . ? C11 O4 Cd1 116.80(12) . . ? C2 C1 S1 113.74(16) . . ? O1 C2 C1 110.80(18) . . ? O1 C3 C4 106.52(18) . . ? O2 C4 C3 106.89(17) . . ? O2 C5 C6 108.81(17) . . ? C5 C6 S2 114.47(15) . . ? C8 C7 S2 113.68(17) . . ? O3 C8 C7 109.18(19) . . ? O3 C9 C10 111.35(18) . . ? O4 C10 C9 106.21(18) . . ? O4 C11 C12 108.89(18) . . ? C11 C12 S1 114.69(16) . . ? O7 Cl1 O6 109.83(12) . . ? O7 Cl1 O8 110.18(12) . . ? O6 Cl1 O8 109.90(11) . . ? O7 Cl1 O5 108.61(13) . . ? O6 Cl1 O5 109.61(12) . . ? O8 Cl1 O5 108.68(12) . . ? Cl1 O5 Cd1 137.24(11) . . ? O12 Cl2 O10 109.76(13) . . ? O12 Cl2 O11 109.29(12) . . ? O10 Cl2 O11 110.24(13) . . ? O12 Cl2 O9 109.71(12) . . ? O10 Cl2 O9 108.71(12) . . ? O11 Cl2 O9 109.12(11) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.765 _refine_diff_density_min -0.508 _refine_diff_density_rms 0.088 ############################################################ data_compound6 _database_code_depnum_ccdc_archive 'CCDC 769793' #TrackingRef '- IHDT-F.cif' _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ;2(C12 H24 Cd N O7 S2), Cd N4 O12 ; _chemical_formula_sum 'C24 H48 Cd3 N6 O26 S4' _chemical_formula_weight 1302.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma _symmetry_space_group_name_Hall '-P 2ac 2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 15.887(5) _cell_length_b 26.686(9) _cell_length_c 10.632(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4507(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9897 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 28.23 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.919 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2600 _exptl_absorpt_coefficient_mu 1.680 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5185 _exptl_absorpt_correction_T_max 0.7298 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 40491 _diffrn_reflns_av_R_equivalents 0.0366 _diffrn_reflns_av_sigmaI/netI 0.0203 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 27.00 _reflns_number_total 5030 _reflns_number_gt 4558 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker APEX2' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0274P)^2^+2.5224P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5030 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0272 _refine_ls_R_factor_gt 0.0236 _refine_ls_wR_factor_ref 0.0585 _refine_ls_wR_factor_gt 0.0567 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.009100(10) 0.596609(6) 0.704991(14) 0.02801(6) Uani 1 1 d . . . Cd2 Cd 0.222518(15) 0.2500 0.68668(2) 0.03025(7) Uani 1 2 d S . . S1 S 0.05578(5) 0.68101(2) 0.79654(7) 0.04535(17) Uani 1 1 d . . . S2 S -0.12187(3) 0.60696(2) 0.55916(5) 0.03117(12) Uani 1 1 d . . . O1 O 0.19473(11) 0.62176(6) 0.66523(16) 0.0403(4) Uani 1 1 d . . . O2 O 0.06155(10) 0.62211(6) 0.48634(14) 0.0376(4) Uani 1 1 d . . . O3 O -0.08304(10) 0.52339(6) 0.75409(15) 0.0331(3) Uani 1 1 d . . . O4 O -0.06718(11) 0.60339(6) 0.91278(16) 0.0384(4) Uani 1 1 d . . . C1 C 0.16228(16) 0.66763(9) 0.8496(2) 0.0422(6) Uani 1 1 d . . . H1A H 0.1819 0.6944 0.9071 0.051 Uiso 1 1 calc R . . H1B H 0.1636 0.6353 0.8954 0.051 Uiso 1 1 calc R . . C2 C 0.21796(17) 0.66506(10) 0.7364(2) 0.0444(6) Uani 1 1 d . . . H2A H 0.2110 0.6956 0.6847 0.053 Uiso 1 1 calc R . . H2B H 0.2776 0.6627 0.7626 0.053 Uiso 1 1 calc R . . C3 C 0.20682(16) 0.62794(11) 0.5332(2) 0.0468(6) Uani 1 1 d . . . H3A H 0.2142 0.5946 0.4937 0.056 Uiso 1 1 calc R . . H3B H 0.2588 0.6476 0.5184 0.056 Uiso 1 1 calc R . . C4 C 0.13403(16) 0.65411(11) 0.4730(2) 0.0465(7) Uani 1 1 d . . . H4A H 0.1238 0.6867 0.5147 0.056 Uiso 1 1 calc R . . H4B H 0.1458 0.6603 0.3829 0.056 Uiso 1 1 calc R . . C5 C 0.00043(14) 0.63097(9) 0.3912(2) 0.0352(5) Uani 1 1 d . . . H5A H 0.0258 0.6263 0.3069 0.042 Uiso 1 1 calc R . . H5B H -0.0211 0.6657 0.3973 0.042 Uiso 1 1 calc R . . C6 C -0.06995(14) 0.59416(8) 0.4107(2) 0.0325(5) Uani 1 1 d . . . H6A H -0.0472 0.5596 0.4110 0.039 Uiso 1 1 calc R . . H6B H -0.1110 0.5969 0.3410 0.039 Uiso 1 1 calc R . . C7 C -0.17962(14) 0.54910(9) 0.5854(2) 0.0375(5) Uani 1 1 d . . . H7A H -0.2280 0.5561 0.6415 0.045 Uiso 1 1 calc R . . H7B H -0.2023 0.5372 0.5041 0.045 Uiso 1 1 calc R . . C8 C -0.12655(15) 0.50766(8) 0.6436(2) 0.0364(5) Uani 1 1 d . . . H8A H -0.1635 0.4790 0.6650 0.044 Uiso 1 1 calc R . . H8B H -0.0850 0.4959 0.5808 0.044 Uiso 1 1 calc R . . C9 C -0.13651(16) 0.52747(10) 0.8630(2) 0.0424(6) Uani 1 1 d . . . H9A H -0.1523 0.4937 0.8937 0.051 Uiso 1 1 calc R . . H9B H -0.1886 0.5459 0.8416 0.051 Uiso 1 1 calc R . . C10 C -0.08816(17) 0.55513(10) 0.9620(2) 0.0438(6) Uani 1 1 d . . . H10A H -0.1227 0.5587 1.0390 0.053 Uiso 1 1 calc R . . H10B H -0.0363 0.5365 0.9839 0.053 Uiso 1 1 calc R . . C11 C -0.02057(17) 0.63293(12) 1.0009(3) 0.0506(7) Uani 1 1 d . . . H11A H 0.0329 0.6159 1.0224 0.061 Uiso 1 1 calc R . . H11B H -0.0536 0.6374 1.0791 0.061 Uiso 1 1 calc R . . C12 C -0.00259(18) 0.68323(11) 0.9422(3) 0.0588(9) Uani 1 1 d . . . H12A H 0.0294 0.7037 1.0033 0.071 Uiso 1 1 calc R . . H12B H -0.0568 0.7004 0.9265 0.071 Uiso 1 1 calc R . . N1 N 0.12307(11) 0.52028(6) 0.75015(18) 0.0285(4) Uani 1 1 d . . . O5 O 0.08918(10) 0.52968(5) 0.64379(14) 0.0323(3) Uani 1 1 d . . . O6 O 0.10066(10) 0.54685(6) 0.84268(15) 0.0322(3) Uani 1 1 d . . . O7 O 0.17532(10) 0.48684(6) 0.76101(18) 0.0403(4) Uani 1 1 d . . . N2 N 0.12697(19) 0.2500 0.4671(3) 0.0431(7) Uani 1 2 d S . . O8 O 0.09360(16) 0.2500 0.5745(3) 0.0513(7) Uani 1 2 d S . . O9 O 0.20610(15) 0.2500 0.4628(2) 0.0417(6) Uani 1 2 d S . . O10 O 0.0848(2) 0.2500 0.3723(3) 0.0893(12) Uani 1 2 d S . . N3 N 0.19222(17) 0.2500 0.9444(2) 0.0308(6) Uani 1 2 d S . . O11 O 0.13153(14) 0.2500 0.8686(2) 0.0464(6) Uani 1 2 d S . . O12 O 0.26555(13) 0.2500 0.8989(2) 0.0307(5) Uani 1 2 d S . . O13 O 0.18075(15) 0.2500 1.0589(2) 0.0440(6) Uani 1 2 d S . . N4 N 0.28786(16) 0.34713(9) 0.6688(2) 0.0486(6) Uani 1 1 d . . . O14 O 0.33324(12) 0.30963(7) 0.64745(17) 0.0472(4) Uani 1 1 d . . . O15 O 0.21371(13) 0.33888(7) 0.70619(19) 0.0541(5) Uani 1 1 d . . . O16 O 0.31477(17) 0.39000(8) 0.6550(2) 0.0767(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.03121(10) 0.02419(9) 0.02864(9) -0.00089(6) -0.00401(6) -0.00241(6) Cd2 0.02990(12) 0.03614(13) 0.02470(11) 0.000 0.00009(8) 0.000 S1 0.0539(4) 0.0225(3) 0.0596(4) -0.0052(3) -0.0220(3) 0.0023(3) S2 0.0286(3) 0.0307(3) 0.0343(3) 0.0003(2) -0.0020(2) 0.0027(2) O1 0.0417(10) 0.0379(9) 0.0412(9) 0.0031(7) -0.0076(8) -0.0122(8) O2 0.0340(9) 0.0476(9) 0.0313(8) 0.0124(7) -0.0070(7) -0.0162(7) O3 0.0303(8) 0.0333(8) 0.0358(8) 0.0031(7) 0.0020(7) -0.0027(6) O4 0.0366(9) 0.0435(9) 0.0352(8) -0.0052(7) -0.0025(7) 0.0060(7) C1 0.0483(15) 0.0357(12) 0.0426(13) -0.0021(10) -0.0173(11) -0.0118(11) C2 0.0473(15) 0.0405(13) 0.0454(14) 0.0070(11) -0.0166(12) -0.0191(12) C3 0.0331(13) 0.0607(17) 0.0466(15) -0.0045(12) 0.0052(11) -0.0153(12) C4 0.0449(15) 0.0615(17) 0.0332(12) 0.0146(11) -0.0021(11) -0.0270(13) C5 0.0378(13) 0.0390(12) 0.0288(11) 0.0074(9) -0.0039(9) -0.0005(10) C6 0.0317(12) 0.0354(12) 0.0304(11) -0.0022(9) -0.0057(9) 0.0016(9) C7 0.0260(11) 0.0430(13) 0.0434(13) 0.0020(10) -0.0036(10) -0.0062(10) C8 0.0358(12) 0.0300(11) 0.0433(13) -0.0021(10) 0.0006(10) -0.0065(9) C9 0.0385(13) 0.0481(14) 0.0405(13) 0.0085(11) 0.0089(11) -0.0054(11) C10 0.0435(14) 0.0537(15) 0.0342(12) 0.0078(11) 0.0045(10) 0.0050(12) C11 0.0453(15) 0.0685(19) 0.0380(14) -0.0223(13) -0.0030(11) 0.0102(14) C12 0.0529(17) 0.0487(16) 0.075(2) -0.0368(15) -0.0131(15) 0.0160(13) N1 0.0243(9) 0.0237(8) 0.0376(10) -0.0016(8) 0.0011(8) -0.0061(7) O5 0.0367(9) 0.0286(8) 0.0316(8) -0.0025(6) 0.0007(7) -0.0039(6) O6 0.0328(8) 0.0298(8) 0.0341(8) -0.0056(6) 0.0010(7) -0.0006(6) O7 0.0309(8) 0.0326(8) 0.0575(10) -0.0043(8) -0.0015(8) 0.0062(7) N2 0.0410(17) 0.0518(18) 0.0366(16) 0.000 -0.0113(13) 0.000 O8 0.0350(14) 0.0702(18) 0.0488(16) 0.000 0.0033(12) 0.000 O9 0.0344(13) 0.0540(15) 0.0367(13) 0.000 0.0000(10) 0.000 O10 0.069(2) 0.143(4) 0.056(2) 0.000 -0.0375(17) 0.000 N3 0.0315(14) 0.0330(13) 0.0280(13) 0.000 0.0003(11) 0.000 O11 0.0259(12) 0.0817(19) 0.0317(12) 0.000 -0.0036(10) 0.000 O12 0.0224(10) 0.0360(11) 0.0336(11) 0.000 0.0015(9) 0.000 O13 0.0394(13) 0.0673(17) 0.0252(12) 0.000 0.0024(10) 0.000 N4 0.0624(16) 0.0422(13) 0.0412(12) 0.0096(10) -0.0149(11) -0.0059(11) O14 0.0535(11) 0.0471(10) 0.0409(10) 0.0025(8) 0.0023(8) -0.0051(9) O15 0.0518(12) 0.0469(11) 0.0636(13) 0.0113(9) -0.0098(10) 0.0088(9) O16 0.104(2) 0.0393(11) 0.0865(17) 0.0137(11) -0.0077(15) -0.0200(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O5 2.2874(16) . ? Cd1 O6 2.4540(16) . ? Cd1 O3 2.4966(16) . ? Cd1 O4 2.5263(18) . ? Cd1 O2 2.5616(17) . ? Cd1 S1 2.5633(9) . ? Cd1 S2 2.6096(8) . ? Cd2 O12 2.358(2) . ? Cd2 O8 2.370(3) . ? Cd2 O15 2.385(2) . ? Cd2 O15 2.385(2) 7_565 ? Cd2 O9 2.395(2) . ? Cd2 O14 2.4083(19) . ? Cd2 O14 2.4084(19) 7_565 ? Cd2 O11 2.415(2) . ? S1 C12 1.806(3) . ? S1 C1 1.819(3) . ? S2 C6 1.814(2) . ? S2 C7 1.818(2) . ? O1 C3 1.426(3) . ? O1 C2 1.430(3) . ? O2 C5 1.422(3) . ? O2 C4 1.441(3) . ? O3 C8 1.426(3) . ? O3 C9 1.440(3) . ? O4 C10 1.430(3) . ? O4 C11 1.431(3) . ? C1 C2 1.495(4) . ? C3 C4 1.495(4) . ? C5 C6 1.503(3) . ? C7 C8 1.522(3) . ? C9 C10 1.498(4) . ? C11 C12 1.508(5) . ? N1 O7 1.224(2) . ? N1 O6 1.264(2) . ? N1 O5 1.277(2) . ? N2 O10 1.210(4) . ? N2 O9 1.258(4) . ? N2 O8 1.259(4) . ? N3 O13 1.231(3) . ? N3 O11 1.256(3) . ? N3 O12 1.261(3) . ? N4 O16 1.230(3) . ? N4 O14 1.254(3) . ? N4 O15 1.262(3) . ? 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 O5 Cd1 O6 54.37(5) . . ? O5 Cd1 O3 76.97(6) . . ? O6 Cd1 O3 78.42(5) . . ? O5 Cd1 O4 124.86(5) . . ? O6 Cd1 O4 78.55(6) . . ? O3 Cd1 O4 65.92(5) . . ? O5 Cd1 O2 76.61(6) . . ? O6 Cd1 O2 119.49(5) . . ? O3 Cd1 O2 126.05(5) . . ? O4 Cd1 O2 158.54(6) . . ? O5 Cd1 S1 129.29(5) . . ? O6 Cd1 S1 94.44(4) . . ? O3 Cd1 S1 141.07(4) . . ? O4 Cd1 S1 75.15(4) . . ? O2 Cd1 S1 90.98(4) . . ? O5 Cd1 S2 110.92(4) . . ? O6 Cd1 S2 152.17(4) . . ? O3 Cd1 S2 74.90(4) . . ? O4 Cd1 S2 97.44(5) . . ? O2 Cd1 S2 72.07(4) . . ? S1 Cd1 S2 111.31(2) . . ? O12 Cd2 O8 137.07(8) . . ? O12 Cd2 O15 86.20(5) . . ? O8 Cd2 O15 89.60(5) . . ? O12 Cd2 O15 86.20(5) . 7_565 ? O8 Cd2 O15 89.60(5) . 7_565 ? O15 Cd2 O15 167.96(10) . 7_565 ? O12 Cd2 O9 169.40(8) . . ? O8 Cd2 O9 53.54(9) . . ? O15 Cd2 O9 94.59(5) . . ? O15 Cd2 O9 94.59(5) 7_565 . ? O12 Cd2 O14 87.36(6) . . ? O8 Cd2 O14 122.96(6) . . ? O15 Cd2 O14 53.19(7) . . ? O15 Cd2 O14 135.64(7) 7_565 . ? O9 Cd2 O14 84.69(6) . . ? O12 Cd2 O14 87.36(6) . 7_565 ? O8 Cd2 O14 122.96(6) . 7_565 ? O15 Cd2 O14 135.64(7) . 7_565 ? O15 Cd2 O14 53.19(7) 7_565 7_565 ? O9 Cd2 O14 84.69(6) . 7_565 ? O14 Cd2 O14 82.71(10) . 7_565 ? O12 Cd2 O11 53.63(7) . . ? O8 Cd2 O11 83.44(9) . . ? O15 Cd2 O11 83.99(5) . . ? O15 Cd2 O11 83.99(5) 7_565 . ? O9 Cd2 O11 136.97(8) . . ? O14 Cd2 O11 125.17(6) . . ? O14 Cd2 O11 125.17(6) 7_565 . ? C12 S1 C1 102.60(13) . . ? C12 S1 Cd1 101.88(10) . . ? C1 S1 Cd1 102.38(8) . . ? C6 S2 C7 101.74(11) . . ? C6 S2 Cd1 97.74(8) . . ? C7 S2 Cd1 102.78(8) . . ? C3 O1 C2 113.14(19) . . ? C5 O2 C4 112.16(17) . . ? C5 O2 Cd1 117.88(13) . . ? C4 O2 Cd1 120.45(13) . . ? C8 O3 C9 113.49(18) . . ? C8 O3 Cd1 110.02(13) . . ? C9 O3 Cd1 117.05(13) . . ? C10 O4 C11 112.1(2) . . ? C10 O4 Cd1 111.57(14) . . ? C11 O4 Cd1 111.33(15) . . ? C2 C1 S1 108.05(18) . . ? O1 C2 C1 108.08(19) . . ? O1 C3 C4 111.8(2) . . ? O2 C4 C3 107.4(2) . . ? O2 C5 C6 107.53(18) . . ? C5 C6 S2 109.59(16) . . ? C8 C7 S2 113.58(16) . . ? O3 C8 C7 112.91(19) . . ? O3 C9 C10 107.5(2) . . ? O4 C10 C9 107.8(2) . . ? O4 C11 C12 108.5(2) . . ? C11 C12 S1 115.03(18) . . ? O7 N1 O6 121.77(19) . . ? O7 N1 O5 120.83(19) . . ? O6 N1 O5 117.41(17) . . ? N1 O5 Cd1 97.81(12) . . ? N1 O6 Cd1 90.35(12) . . ? O10 N2 O9 121.6(3) . . ? O10 N2 O8 121.5(3) . . ? O9 N2 O8 117.0(3) . . ? N2 O8 Cd2 95.31(19) . . ? N2 O9 Cd2 94.16(19) . . ? O13 N3 O11 121.4(3) . . ? O13 N3 O12 121.0(3) . . ? O11 N3 O12 117.6(2) . . ? N3 O11 Cd2 93.10(17) . . ? N3 O12 Cd2 95.68(16) . . ? O16 N4 O14 121.4(3) . . ? O16 N4 O15 121.6(3) . . ? O14 N4 O15 117.0(2) . . ? N4 O14 Cd2 94.36(15) . . ? N4 O15 Cd2 95.24(15) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.336 _refine_diff_density_min -0.751 _refine_diff_density_rms 0.084 ############################################################ data_compound7 _database_code_depnum_ccdc_archive 'CCDC 769794' #TrackingRef '- IHDT-F.cif' _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H72 Hg2 O12 S6, 4(Cl O4)' _chemical_formula_sum 'C36 H72 Cl4 Hg2 O28 S6' _chemical_formula_weight 1688.28 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' 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' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' 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' _cell_length_a 12.7113(19) _cell_length_b 10.0162(15) _cell_length_c 22.698(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.226(2) _cell_angle_gamma 90.00 _cell_volume 2852.4(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7060 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 28.42 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.38 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.966 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1672 _exptl_absorpt_coefficient_mu 5.867 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1691 _exptl_absorpt_correction_T_max 0.2140 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 27911 _diffrn_reflns_av_R_equivalents 0.0846 _diffrn_reflns_av_sigmaI/netI 0.0813 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 28.00 _reflns_number_total 6877 _reflns_number_gt 5597 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker APEX2' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0418P)^2^+2.0579P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6877 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0588 _refine_ls_R_factor_gt 0.0469 _refine_ls_wR_factor_ref 0.1148 _refine_ls_wR_factor_gt 0.1088 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hg1 Hg 0.781155(15) 1.05718(2) 0.638440(9) 0.02802(9) Uani 1 1 d . . . S1 S 0.82470(11) 1.03430(14) 0.75051(6) 0.0293(3) Uani 1 1 d . . . S2 S 0.89761(13) 1.25599(18) 0.62271(7) 0.0427(4) Uani 1 1 d . . . O1 O 0.5820(3) 1.0530(3) 0.67981(18) 0.0293(9) Uani 1 1 d . . . O2 O 0.6572(3) 1.2749(4) 0.62464(17) 0.0328(9) Uani 1 1 d . . . O3 O 0.9584(3) 0.9751(5) 0.5859(2) 0.0451(11) Uani 1 1 d . . . O4 O 0.8809(3) 0.8068(4) 0.66724(17) 0.0361(9) Uani 1 1 d . . . C1 C 0.7003(5) 1.0710(6) 0.7760(3) 0.0324(13) Uani 1 1 d . . . H1A H 0.7060 1.0410 0.8180 0.039 Uiso 1 1 calc R . . H1B H 0.6906 1.1691 0.7756 0.039 Uiso 1 1 calc R . . C2 C 0.6014(5) 1.0085(6) 0.7405(3) 0.0327(13) Uani 1 1 d . . . H2A H 0.6095 0.9102 0.7412 0.039 Uiso 1 1 calc R . . H2B H 0.5390 1.0308 0.7597 0.039 Uiso 1 1 calc R . . C3 C 0.5237(5) 1.1773(6) 0.6715(3) 0.0373(14) Uani 1 1 d . . . H3A H 0.5455 1.2366 0.7062 0.045 Uiso 1 1 calc R . . H3B H 0.4463 1.1599 0.6682 0.045 Uiso 1 1 calc R . . C4 C 0.5466(5) 1.2426(6) 0.6161(3) 0.0381(14) Uani 1 1 d . . . H4A H 0.5286 1.1814 0.5817 0.046 Uiso 1 1 calc R . . H4B H 0.5032 1.3246 0.6080 0.046 Uiso 1 1 calc R . . C5 C 0.6917(6) 1.3374(6) 0.5753(3) 0.0417(15) Uani 1 1 d . . . H5A H 0.6446 1.4135 0.5613 0.050 Uiso 1 1 calc R . . H5B H 0.6902 1.2732 0.5420 0.050 Uiso 1 1 calc R . . C6 C 0.8035(6) 1.3853(6) 0.5960(3) 0.0467(17) Uani 1 1 d . . . H6A H 0.8023 1.4512 0.6284 0.056 Uiso 1 1 calc R . . H6B H 0.8288 1.4319 0.5624 0.056 Uiso 1 1 calc R . . C7 C 0.9482(5) 1.2016(8) 0.5559(3) 0.0476(18) Uani 1 1 d . . . H7A H 0.8881 1.1759 0.5246 0.057 Uiso 1 1 calc R . . H7B H 0.9877 1.2754 0.5403 0.057 Uiso 1 1 calc R . . C8 C 1.0198(5) 1.0860(8) 0.5712(3) 0.054(2) Uani 1 1 d . . . H8A H 1.0556 1.0629 0.5369 0.065 Uiso 1 1 calc R . . H8B H 1.0753 1.1085 0.6056 0.065 Uiso 1 1 calc R . . C9 C 1.0235(5) 0.8673(9) 0.6131(3) 0.054(2) Uani 1 1 d . . . H9A H 1.0702 0.8991 0.6495 0.065 Uiso 1 1 calc R . . H9B H 1.0690 0.8324 0.5851 0.065 Uiso 1 1 calc R . . C10 C 0.9508(5) 0.7597(7) 0.6288(3) 0.0442(16) Uani 1 1 d . . . H10A H 0.9082 0.7246 0.5917 0.053 Uiso 1 1 calc R . . H10B H 0.9942 0.6854 0.6485 0.053 Uiso 1 1 calc R . . C11 C 0.9225(5) 0.7980(7) 0.7298(3) 0.0377(14) Uani 1 1 d . . . H11A H 0.9903 0.8482 0.7388 0.045 Uiso 1 1 calc R . . H11B H 0.9366 0.7036 0.7414 0.045 Uiso 1 1 calc R . . C12 C 0.8407(5) 0.8567(6) 0.7640(3) 0.0362(14) Uani 1 1 d . . . H12A H 0.8634 0.8409 0.8072 0.043 Uiso 1 1 calc R . . H12B H 0.7715 0.8114 0.7518 0.043 Uiso 1 1 calc R . . S3 S 0.65307(10) 0.93246(12) 0.56484(6) 0.0234(3) Uani 1 1 d . . . O5 O 0.7275(3) 1.0987(4) 0.46665(18) 0.0302(8) Uani 1 1 d . . . O6 O 0.5409(3) 1.2543(4) 0.44720(16) 0.0274(8) Uani 1 1 d . . . C13 C 0.7187(5) 0.8788(6) 0.5032(3) 0.0302(12) Uani 1 1 d . . . H13A H 0.7969 0.8815 0.5156 0.036 Uiso 1 1 calc R . . H13B H 0.6980 0.7858 0.4922 0.036 Uiso 1 1 calc R . . C14 C 0.6873(5) 0.9692(5) 0.4501(3) 0.0296(12) Uani 1 1 d . . . H14A H 0.7179 0.9359 0.4154 0.035 Uiso 1 1 calc R . . H14B H 0.6087 0.9720 0.4390 0.035 Uiso 1 1 calc R . . C15 C 0.7075(4) 1.1923(6) 0.4192(3) 0.0323(13) Uani 1 1 d . . . H15A H 0.7409 1.1593 0.3854 0.039 Uiso 1 1 calc R . . H15B H 0.7424 1.2778 0.4327 0.039 Uiso 1 1 calc R . . C17 C 0.4409(4) 1.3154(5) 0.4300(3) 0.0302(12) Uani 1 1 d . . . H17A H 0.4501 1.3941 0.4049 0.036 Uiso 1 1 calc R . . H17B H 0.4146 1.3477 0.4662 0.036 Uiso 1 1 calc R . . C18 C 0.3580(4) 1.2252(5) 0.3959(2) 0.0268(11) Uani 1 1 d . . . H18A H 0.3770 1.2065 0.3561 0.032 Uiso 1 1 calc R . . H18B H 0.2882 1.2712 0.3900 0.032 Uiso 1 1 calc R . . C16 C 0.5909(4) 1.2183(6) 0.3971(2) 0.0295(12) Uani 1 1 d . . . H16A H 0.5829 1.2917 0.3674 0.035 Uiso 1 1 calc R . . H16B H 0.5569 1.1373 0.3776 0.035 Uiso 1 1 calc R . . Cl1 Cl 0.27398(11) 1.51050(14) 0.24409(6) 0.0319(3) Uani 1 1 d . . . O7 O 0.3563(4) 1.5922(5) 0.2262(2) 0.0539(13) Uani 1 1 d . . . O8 O 0.2345(5) 1.4235(5) 0.1952(2) 0.0620(16) Uani 1 1 d . . . O9 O 0.3181(6) 1.4356(5) 0.2948(3) 0.0682(17) Uani 1 1 d . . . O10 O 0.1929(4) 1.5989(7) 0.2573(2) 0.0660(15) Uani 1 1 d . . . Cl2 Cl 0.19994(14) 1.42650(13) 0.56274(7) 0.0372(3) Uani 1 1 d . . . O11 O 0.2099(5) 1.3102(5) 0.5987(2) 0.0677(16) Uani 1 1 d . . . O12 O 0.1378(5) 1.3927(6) 0.5055(2) 0.0668(16) Uani 1 1 d . . . O13 O 0.1455(4) 1.5265(5) 0.5907(2) 0.0547(13) Uani 1 1 d . . . O14 O 0.3002(4) 1.4727(5) 0.5531(3) 0.0700(17) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hg1 0.02433(13) 0.03363(14) 0.02628(14) 0.00247(9) 0.00458(9) -0.00491(8) S1 0.0287(7) 0.0339(7) 0.0251(7) 0.0004(6) 0.0032(6) -0.0054(5) S2 0.0449(9) 0.0591(10) 0.0234(8) -0.0009(7) 0.0036(6) -0.0310(8) O1 0.029(2) 0.028(2) 0.032(2) -0.0039(16) 0.0064(17) -0.0019(15) O2 0.040(2) 0.029(2) 0.027(2) -0.0005(17) -0.0008(17) -0.0055(17) O3 0.025(2) 0.073(3) 0.038(3) 0.001(2) 0.0043(19) -0.005(2) O4 0.024(2) 0.056(3) 0.027(2) -0.0020(19) 0.0012(16) 0.0098(18) C1 0.034(3) 0.040(3) 0.023(3) 0.001(2) 0.006(2) 0.003(2) C2 0.031(3) 0.037(3) 0.033(3) -0.001(3) 0.015(3) -0.002(2) C3 0.029(3) 0.037(3) 0.044(4) -0.008(3) 0.001(3) 0.006(2) C4 0.039(3) 0.029(3) 0.043(4) -0.005(3) -0.002(3) 0.002(2) C5 0.064(4) 0.027(3) 0.033(3) 0.009(3) 0.004(3) 0.006(3) C6 0.080(5) 0.031(3) 0.031(3) 0.000(3) 0.016(3) -0.022(3) C7 0.041(4) 0.077(5) 0.025(3) 0.001(3) 0.004(3) -0.032(4) C8 0.026(3) 0.098(6) 0.039(4) -0.006(4) 0.010(3) -0.025(4) C9 0.022(3) 0.102(6) 0.038(4) -0.005(4) 0.004(3) 0.019(4) C10 0.036(3) 0.060(4) 0.035(4) -0.013(3) 0.000(3) 0.023(3) C11 0.031(3) 0.053(4) 0.026(3) 0.007(3) -0.003(2) 0.014(3) C12 0.037(3) 0.038(3) 0.034(3) 0.011(3) 0.007(3) 0.008(3) S3 0.0224(6) 0.0241(6) 0.0233(7) 0.0011(5) 0.0028(5) 0.0007(5) O5 0.027(2) 0.0264(18) 0.035(2) 0.0024(17) -0.0035(16) -0.0046(15) O6 0.0267(19) 0.031(2) 0.024(2) 0.0004(16) 0.0029(15) -0.0029(15) C13 0.034(3) 0.029(3) 0.029(3) -0.001(2) 0.010(2) 0.004(2) C14 0.033(3) 0.034(3) 0.022(3) -0.007(2) 0.004(2) -0.007(2) C15 0.026(3) 0.033(3) 0.038(3) 0.008(3) 0.004(2) -0.009(2) C17 0.030(3) 0.021(2) 0.041(3) 0.002(2) 0.007(2) 0.000(2) C18 0.032(3) 0.022(2) 0.027(3) 0.008(2) 0.004(2) 0.002(2) C16 0.029(3) 0.037(3) 0.023(3) 0.002(2) 0.007(2) -0.005(2) Cl1 0.0353(7) 0.0333(7) 0.0255(7) -0.0005(6) -0.0001(6) -0.0010(6) O7 0.051(3) 0.053(3) 0.059(3) 0.001(2) 0.013(3) -0.014(2) O8 0.095(5) 0.048(3) 0.036(3) -0.012(2) -0.008(3) -0.020(3) O9 0.102(5) 0.055(3) 0.042(3) 0.020(2) -0.009(3) 0.005(3) O10 0.047(3) 0.102(4) 0.049(3) -0.013(3) 0.007(2) 0.022(3) Cl2 0.0573(10) 0.0251(7) 0.0313(8) -0.0033(6) 0.0139(7) -0.0084(6) O11 0.121(5) 0.040(3) 0.047(3) 0.012(2) 0.030(3) 0.007(3) O12 0.106(5) 0.055(3) 0.036(3) -0.004(3) 0.003(3) -0.018(3) O13 0.058(3) 0.047(3) 0.061(3) -0.012(2) 0.015(3) 0.002(2) O14 0.053(3) 0.055(3) 0.108(5) -0.001(3) 0.033(3) -0.006(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg1 S3 2.4758(14) . ? Hg1 S1 2.5255(15) . ? Hg1 S2 2.5404(15) . ? Hg1 O2 2.679(4) . ? Hg1 O3 2.835(4) . ? Hg1 O1 2.837(4) . ? Hg1 O4 2.838(4) . ? S1 C1 1.807(6) . ? S1 C12 1.811(6) . ? S2 C6 1.801(8) . ? S2 C7 1.824(7) . ? O1 C2 1.431(7) . ? O1 C3 1.446(7) . ? O2 C5 1.413(7) . ? O2 C4 1.426(7) . ? O3 C8 1.427(8) . ? O3 C9 1.438(9) . ? O4 C10 1.423(7) . ? O4 C11 1.436(7) . ? C1 C2 1.516(8) . ? C3 C4 1.486(9) . ? C5 C6 1.502(10) . ? C7 C8 1.480(11) . ? C9 C10 1.499(10) . ? C11 C12 1.513(8) . ? S3 C13 1.821(5) . ? S3 C18 1.830(5) 3_676 ? O5 C15 1.420(7) . ? O5 C14 1.423(6) . ? O6 C17 1.408(6) . ? O6 C16 1.435(6) . ? C13 C14 1.509(8) . ? C15 C16 1.510(8) . ? C17 C18 1.503(8) . ? C18 S3 1.830(5) 3_676 ? Cl1 O9 1.412(5) . ? Cl1 O10 1.426(5) . ? Cl1 O8 1.437(5) . ? Cl1 O7 1.437(5) . ? Cl2 O14 1.406(5) . ? Cl2 O11 1.416(5) . ? Cl2 O13 1.423(5) . ? Cl2 O12 1.449(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S3 Hg1 S1 130.40(4) . . ? S3 Hg1 S2 129.47(5) . . ? S1 Hg1 S2 100.03(5) . . ? S3 Hg1 O2 91.20(9) . . ? S1 Hg1 O2 102.79(9) . . ? S2 Hg1 O2 71.98(10) . . ? S3 Hg1 O3 92.92(10) . . ? S1 Hg1 O3 109.68(10) . . ? S2 Hg1 O3 69.37(11) . . ? O2 Hg1 O3 132.76(13) . . ? S3 Hg1 O1 72.00(9) . . ? S1 Hg1 O1 74.24(9) . . ? S2 Hg1 O1 128.96(8) . . ? O2 Hg1 O1 60.76(11) . . ? O3 Hg1 O1 161.14(12) . . ? S3 Hg1 O4 86.03(9) . . ? S1 Hg1 O4 70.74(9) . . ? S2 Hg1 O4 118.43(9) . . ? O2 Hg1 O4 168.12(12) . . ? O3 Hg1 O4 59.01(13) . . ? O1 Hg1 O4 107.45(11) . . ? C1 S1 C12 103.1(3) . . ? C1 S1 Hg1 104.0(2) . . ? C12 S1 Hg1 105.1(2) . . ? C6 S2 C7 103.8(3) . . ? C6 S2 Hg1 103.9(2) . . ? C7 S2 Hg1 100.0(2) . . ? C2 O1 C3 113.6(4) . . ? C2 O1 Hg1 107.3(3) . . ? C3 O1 Hg1 114.2(3) . . ? C5 O2 C4 114.7(5) . . ? C5 O2 Hg1 101.6(3) . . ? C4 O2 Hg1 112.3(3) . . ? C8 O3 C9 112.7(5) . . ? C8 O3 Hg1 112.0(4) . . ? C9 O3 Hg1 118.6(3) . . ? C10 O4 C11 114.8(4) . . ? C10 O4 Hg1 116.8(4) . . ? C11 O4 Hg1 111.2(3) . . ? C2 C1 S1 116.1(4) . . ? O1 C2 C1 112.6(5) . . ? O1 C3 C4 108.9(5) . . ? O2 C4 C3 107.9(5) . . ? O2 C5 C6 107.0(5) . . ? C5 C6 S2 114.8(4) . . ? C8 C7 S2 108.9(5) . . ? O3 C8 C7 109.0(5) . . ? O3 C9 C10 107.9(5) . . ? O4 C10 C9 112.1(5) . . ? O4 C11 C12 108.0(4) . . ? C11 C12 S1 111.3(4) . . ? C13 S3 C18 101.5(3) . 3_676 ? C13 S3 Hg1 109.5(2) . . ? C18 S3 Hg1 101.59(18) 3_676 . ? C15 O5 C14 112.9(4) . . ? C17 O6 C16 112.5(4) . . ? C14 C13 S3 110.0(4) . . ? O5 C14 C13 107.3(5) . . ? O5 C15 C16 114.4(4) . . ? O6 C17 C18 114.1(4) . . ? C17 C18 S3 111.8(4) . 3_676 ? O6 C16 C15 108.4(4) . . ? O9 Cl1 O10 111.4(4) . . ? O9 Cl1 O8 110.6(3) . . ? O10 Cl1 O8 111.3(4) . . ? O9 Cl1 O7 108.7(4) . . ? O10 Cl1 O7 106.8(4) . . ? O8 Cl1 O7 107.9(3) . . ? O14 Cl2 O11 111.2(4) . . ? O14 Cl2 O13 110.8(3) . . ? O11 Cl2 O13 109.1(3) . . ? O14 Cl2 O12 108.4(4) . . ? O11 Cl2 O12 108.1(3) . . ? O13 Cl2 O12 109.3(4) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.845 _refine_diff_density_min -2.274 _refine_diff_density_rms 0.195 ############################################################ data_compound8 _database_code_depnum_ccdc_archive 'CCDC 769795' #TrackingRef '- IHDT-F.cif' _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H24 Hg N2 O10 S2, 2(H2 O)' _chemical_formula_sum 'C12 H28 Hg N2 O12 S2' _chemical_formula_weight 657.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' 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' _cell_length_a 9.2913(6) _cell_length_b 7.7909(5) _cell_length_c 15.0248(11) _cell_angle_alpha 90.00 _cell_angle_beta 107.267(3) _cell_angle_gamma 90.00 _cell_volume 1038.59(12) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6572 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 31.49 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.101 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 644 _exptl_absorpt_coefficient_mu 7.674 _exptl_absorpt_correction_type 'multi-scan (SADABS)' _exptl_absorpt_correction_T_min 0.1743 _exptl_absorpt_correction_T_max 0.3388 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 9633 _diffrn_reflns_av_R_equivalents 0.0456 _diffrn_reflns_av_sigmaI/netI 0.0405 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 28.00 _reflns_number_total 2506 _reflns_number_gt 2170 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker APEX2' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0324P)^2^+0.3174P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2506 _refine_ls_number_parameters 133 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0288 _refine_ls_R_factor_gt 0.0246 _refine_ls_wR_factor_ref 0.0654 _refine_ls_wR_factor_gt 0.0626 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hg1 Hg 0.5000 0.5000 0.0000 0.01554(7) Uani 1 2 d S . . S1 S 0.47267(7) 0.20637(8) 0.04372(5) 0.01556(14) Uani 1 1 d . . . O1 O 0.1923(2) 0.4053(2) -0.00657(13) 0.0205(4) Uani 1 1 d . . . O2 O 0.2490(2) 0.5591(3) -0.16013(13) 0.0179(4) Uani 1 1 d . . . C1 C 0.3371(4) 0.2198(4) 0.1092(2) 0.0219(7) Uani 1 1 d . . . H1A H 0.3378 0.1125 0.1447 0.026 Uiso 1 1 calc R . . H1B H 0.3622 0.3167 0.1538 0.026 Uiso 1 1 calc R . . C2 C 0.1845(3) 0.2469(4) 0.0394(2) 0.0237(6) Uani 1 1 d . . . H2A H 0.1604 0.1515 -0.0062 0.028 Uiso 1 1 calc R . . H2B H 0.1054 0.2524 0.0713 0.028 Uiso 1 1 calc R . . C3 C 0.0773(3) 0.4235(4) -0.0929(2) 0.0213(6) Uani 1 1 d . . . H3A H -0.0227 0.4320 -0.0823 0.026 Uiso 1 1 calc R . . H3B H 0.0768 0.3231 -0.1334 0.026 Uiso 1 1 calc R . . C4 C 0.1110(3) 0.5842(4) -0.1378(2) 0.0202(6) Uani 1 1 d . . . H4A H 0.0280 0.6092 -0.1951 0.024 Uiso 1 1 calc R . . H4B H 0.1210 0.6825 -0.0946 0.024 Uiso 1 1 calc R . . C5 C 0.2921(3) 0.7054(3) -0.20333(19) 0.0210(6) Uani 1 1 d . . . H5A H 0.2029 0.7491 -0.2522 0.025 Uiso 1 1 calc R . . H5B H 0.3681 0.6702 -0.2340 0.025 Uiso 1 1 calc R . . C6 C 0.3568(3) 0.8487(3) -0.13468(19) 0.0197(6) Uani 1 1 d . . . H6A H 0.2794 0.8846 -0.1052 0.024 Uiso 1 1 calc R . . H6B H 0.3781 0.9484 -0.1696 0.024 Uiso 1 1 calc R . . N1 N 0.3337(3) 0.7354(3) 0.13420(18) 0.0215(6) Uani 1 1 d . . . O3 O 0.4438(2) 0.6324(3) 0.15093(14) 0.0272(5) Uani 1 1 d . . . O4 O 0.2737(3) 0.7629(3) 0.19619(15) 0.0420(6) Uani 1 1 d . . . O5 O 0.2887(3) 0.8086(3) 0.05746(16) 0.0333(5) Uani 1 1 d . . . O1W O 0.4886(4) 0.4901(2) 0.3370(3) 0.0341(8) Uani 1 1 d . . . H1WA H 0.4641 0.5548 0.2908 0.041 Uiso 1 1 d R . . H1WB H 0.4093 0.4320 0.3394 0.041 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 Hg1 0.01678(11) 0.01115(11) 0.01994(11) 0.00184(5) 0.00738(8) 0.00140(5) S1 0.0159(3) 0.0099(3) 0.0223(3) -0.0008(3) 0.0080(3) 0.0015(3) O1 0.0165(9) 0.0153(10) 0.0291(10) 0.0039(8) 0.0062(8) -0.0021(8) O2 0.0154(10) 0.0159(10) 0.0238(10) 0.0010(9) 0.0078(8) 0.0027(9) C1 0.0247(15) 0.0157(15) 0.0289(16) 0.0026(13) 0.0134(13) 0.0022(13) C2 0.0183(14) 0.0161(14) 0.0411(17) 0.0049(12) 0.0157(14) 0.0003(11) C3 0.0132(13) 0.0212(15) 0.0309(16) -0.0030(13) 0.0088(12) -0.0019(12) C4 0.0152(13) 0.0216(15) 0.0248(14) 0.0011(13) 0.0075(11) 0.0042(12) C5 0.0202(14) 0.0218(14) 0.0204(13) 0.0045(12) 0.0053(11) 0.0010(12) C6 0.0184(13) 0.0140(13) 0.0267(14) 0.0054(11) 0.0070(12) 0.0041(11) N1 0.0186(12) 0.0215(13) 0.0234(13) -0.0044(10) 0.0046(10) -0.0032(10) O3 0.0253(11) 0.0267(11) 0.0295(11) -0.0040(9) 0.0080(9) 0.0089(9) O4 0.0326(13) 0.0674(18) 0.0309(13) -0.0029(12) 0.0169(11) 0.0166(12) O5 0.0409(14) 0.0279(12) 0.0299(12) 0.0079(10) 0.0088(11) 0.0052(11) O1W 0.0318(17) 0.0289(17) 0.0389(19) 0.0077(9) 0.0065(15) -0.0004(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg1 S1 2.4142(7) 3_665 ? Hg1 S1 2.4142(7) . ? Hg1 O3 2.680(2) . ? Hg1 O2 2.8474(19) . ? Hg1 O1 2.9260(18) . ? S1 C6 1.810(3) 3_665 ? S1 C1 1.818(3) . ? O1 C3 1.422(3) . ? O1 C2 1.426(3) . ? O2 C5 1.426(3) . ? O2 C4 1.432(3) . ? C1 C2 1.507(4) . ? C3 C4 1.499(5) . ? C5 C6 1.518(4) . ? C6 S1 1.810(3) 3_665 ? N1 O4 1.238(3) . ? N1 O5 1.242(3) . ? N1 O3 1.266(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 Hg1 S1 180.0 3_665 . ? S1 Hg1 O3 85.88(5) 3_665 . ? S1 Hg1 O3 94.12(5) . . ? S1 Hg1 O2 75.09(5) 3_665 . ? S1 Hg1 O2 104.91(5) . . ? O3 Hg1 O2 109.65(6) . . ? S1 Hg1 O1 114.23(4) 3_665 . ? S1 Hg1 O1 65.77(4) . . ? O3 Hg1 O1 72.04(6) . . ? O2 Hg1 O1 57.68(6) . . ? C6 S1 C1 101.35(14) 3_665 . ? C6 S1 Hg1 106.90(9) 3_665 . ? C1 S1 Hg1 103.81(11) . . ? C3 O1 C2 113.3(2) . . ? C3 O1 Hg1 117.88(16) . . ? C2 O1 Hg1 113.04(15) . . ? C5 O2 C4 112.9(2) . . ? C5 O2 Hg1 104.11(14) . . ? C4 O2 Hg1 112.93(15) . . ? C2 C1 S1 106.9(2) . . ? O1 C2 C1 106.6(2) . . ? O1 C3 C4 107.0(2) . . ? O2 C4 C3 108.2(2) . . ? O2 C5 C6 112.7(2) . . ? C5 C6 S1 114.85(19) . 3_665 ? O4 N1 O5 121.1(3) . . ? O4 N1 O3 118.6(3) . . ? O5 N1 O3 120.3(3) . . ? N1 O3 Hg1 115.16(17) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1WA O3 0.83 2.14 2.921(4) 155.8 . O1W H1WB O4 0.87 2.09 2.933(4) 161.2 2_545 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.012 _refine_diff_density_min -2.073 _refine_diff_density_rms 0.163 ############################################################ data_compound9 _database_code_depnum_ccdc_archive 'CCDC 769796' #TrackingRef '- IHDT-F.cif' _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H24 Cl2 O12 Pb S2' _chemical_formula_sum 'C12 H24 Cl2 O12 Pb S2' _chemical_formula_weight 702.52 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' 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' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' 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' _cell_length_a 8.4360(3) _cell_length_b 10.3907(3) _cell_length_c 12.0754(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.4210(10) _cell_angle_gamma 90.00 _cell_volume 1029.57(6) _cell_formula_units_Z 2 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used 5953 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 27.59 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.266 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 680 _exptl_absorpt_coefficient_mu 8.715 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2103 _exptl_absorpt_correction_T_max 0.4211 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 9350 _diffrn_reflns_av_R_equivalents 0.0330 _diffrn_reflns_av_sigmaI/netI 0.0278 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 27.59 _reflns_number_total 2383 _reflns_number_gt 2147 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker APEX2' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0311P)^2^+0.3870P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0098(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2383 _refine_ls_number_parameters 134 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0240 _refine_ls_R_factor_gt 0.0209 _refine_ls_wR_factor_ref 0.0551 _refine_ls_wR_factor_gt 0.0534 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.163 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Pb1 Pb 0.5000 0.0000 0.0000 0.01434(9) Uani 1 2 d S . . S1 S 0.44904(9) 0.28820(8) 0.04471(7) 0.01919(18) Uani 1 1 d . . . O1 O 0.7513(2) 0.16026(19) 0.06122(19) 0.0210(5) Uani 1 1 d . . . O2 O 0.8012(2) -0.10084(19) 0.09575(17) 0.0178(4) Uani 1 1 d . . . C1 C 0.5861(4) 0.3227(3) -0.0478(3) 0.0199(7) Uani 1 1 d . . . H1A H 0.5529 0.2732 -0.1194 0.024 Uiso 1 1 calc R . . H1B H 0.5821 0.4155 -0.0668 0.024 Uiso 1 1 calc R . . C2 C 0.7566(4) 0.2853(3) 0.0143(3) 0.0243(7) Uani 1 1 d . . . H2A H 0.8297 0.2853 -0.0391 0.029 Uiso 1 1 calc R . . H2B H 0.7994 0.3479 0.0758 0.029 Uiso 1 1 calc R . . C3 C 0.9116(3) 0.1098(3) 0.1090(3) 0.0213(6) Uani 1 1 d . . . H3A H 0.9772 0.1739 0.1607 0.026 Uiso 1 1 calc R . . H3B H 0.9678 0.0901 0.0476 0.026 Uiso 1 1 calc R . . C4 C 0.8933(5) -0.0104(2) 0.1736(4) 0.0198(8) Uani 1 1 d . . . H4A H 1.0019 -0.0465 0.2090 0.024 Uiso 1 1 calc R . . H4B H 0.8365 0.0091 0.2348 0.024 Uiso 1 1 calc R . . C5 C 0.8059(3) -0.2284(3) 0.1424(2) 0.0199(6) Uani 1 1 d . . . H5A H 0.7349 -0.2331 0.1970 0.024 Uiso 1 1 calc R . . H5B H 0.9186 -0.2499 0.1834 0.024 Uiso 1 1 calc R . . C6 C 0.7480(4) -0.3225(3) 0.0467(3) 0.0223(7) Uani 1 1 d . . . H6A H 0.7443 -0.4092 0.0799 0.027 Uiso 1 1 calc R . . H6B H 0.8294 -0.3251 -0.0006 0.027 Uiso 1 1 calc R . . Cl1 Cl 0.37703(9) -0.03220(8) 0.25093(7) 0.01743(16) Uani 1 1 d . . . O3 O 0.5333(3) -0.0529(3) 0.2214(2) 0.0359(6) Uani 1 1 d . . . O4 O 0.3027(3) -0.1536(2) 0.2617(2) 0.0440(7) Uani 1 1 d . . . O5 O 0.2811(4) 0.0366(4) 0.1622(3) 0.0600(9) Uani 1 1 d U . . O6 O 0.4029(6) 0.0339(4) 0.3537(4) 0.0761(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 Pb1 0.01612(12) 0.01285(13) 0.01348(13) 0.00157(5) 0.00227(7) -0.00153(4) S1 0.0218(4) 0.0191(4) 0.0163(4) -0.0017(3) 0.0037(3) 0.0020(3) O1 0.0140(10) 0.0151(11) 0.0327(13) 0.0046(9) 0.0035(9) -0.0017(8) O2 0.0167(10) 0.0166(11) 0.0181(11) 0.0000(8) 0.0002(8) -0.0002(8) C1 0.0238(15) 0.0141(15) 0.0212(16) 0.0042(12) 0.0042(13) -0.0003(12) C2 0.0236(15) 0.0166(16) 0.0321(19) 0.0038(14) 0.0054(13) -0.0049(12) C3 0.0112(13) 0.0214(16) 0.0310(18) -0.0009(13) 0.0040(12) 0.0004(11) C4 0.0137(16) 0.0230(19) 0.021(2) -0.0024(11) 0.0004(14) -0.0002(10) C5 0.0216(15) 0.0161(15) 0.0205(15) 0.0040(12) 0.0021(12) 0.0054(11) C6 0.0230(15) 0.0193(16) 0.0235(17) -0.0021(13) 0.0032(13) 0.0056(12) Cl1 0.0155(3) 0.0210(3) 0.0176(4) 0.0004(3) 0.0074(3) 0.0013(3) O3 0.0222(12) 0.0548(16) 0.0355(15) 0.0066(14) 0.0167(11) 0.0074(12) O4 0.0548(17) 0.0227(13) 0.0653(19) 0.0054(12) 0.0360(14) -0.0048(11) O5 0.0430(15) 0.0724(15) 0.0640(18) 0.0363(15) 0.0114(13) 0.0079(14) O6 0.090(3) 0.089(2) 0.067(3) -0.053(2) 0.055(3) -0.043(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Pb1 O1 2.6621(19) 3_655 ? Pb1 O1 2.6622(19) . ? Pb1 O3 2.680(2) . ? Pb1 O3 2.680(2) 3_655 ? Pb1 O2 2.744(2) . ? Pb1 O2 2.744(2) 3_655 ? Pb1 S1 3.0906(8) . ? Pb1 S1 3.0906(8) 3_655 ? S1 C6 1.805(3) 3_655 ? S1 C1 1.820(3) . ? O1 C2 1.422(4) . ? O1 C3 1.440(3) . ? O2 C4 1.425(4) . ? O2 C5 1.437(3) . ? C1 C2 1.511(4) . ? C3 C4 1.499(4) . ? C5 C6 1.505(4) . ? C6 S1 1.805(3) 3_655 ? Cl1 O5 1.382(3) . ? Cl1 O6 1.391(4) . ? Cl1 O4 1.428(2) . ? Cl1 O3 1.459(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Pb1 O1 180.0 3_655 . ? O1 Pb1 O3 92.35(7) 3_655 . ? O1 Pb1 O3 87.65(7) . . ? O1 Pb1 O3 87.65(7) 3_655 3_655 ? O1 Pb1 O3 92.35(7) . 3_655 ? O3 Pb1 O3 180.0 . 3_655 ? O1 Pb1 O2 118.56(5) 3_655 . ? O1 Pb1 O2 61.44(5) . . ? O3 Pb1 O2 68.21(6) . . ? O3 Pb1 O2 111.79(6) 3_655 . ? O1 Pb1 O2 61.44(5) 3_655 3_655 ? O1 Pb1 O2 118.56(5) . 3_655 ? O3 Pb1 O2 111.79(6) . 3_655 ? O3 Pb1 O2 68.21(6) 3_655 3_655 ? O2 Pb1 O2 180.0 . 3_655 ? O1 Pb1 S1 121.37(5) 3_655 . ? O1 Pb1 S1 58.63(5) . . ? O3 Pb1 S1 90.64(7) . . ? O3 Pb1 S1 89.36(7) 3_655 . ? O2 Pb1 S1 116.69(4) . . ? O2 Pb1 S1 63.31(4) 3_655 . ? O1 Pb1 S1 58.63(5) 3_655 3_655 ? O1 Pb1 S1 121.37(5) . 3_655 ? O3 Pb1 S1 89.36(7) . 3_655 ? O3 Pb1 S1 90.64(7) 3_655 3_655 ? O2 Pb1 S1 63.31(4) . 3_655 ? O2 Pb1 S1 116.69(4) 3_655 3_655 ? S1 Pb1 S1 180.0 . 3_655 ? C6 S1 C1 102.22(16) 3_655 . ? C6 S1 Pb1 103.29(11) 3_655 . ? C1 S1 Pb1 87.14(10) . . ? C2 O1 C3 112.3(2) . . ? C2 O1 Pb1 123.89(18) . . ? C3 O1 Pb1 119.76(16) . . ? C4 O2 C5 112.8(2) . . ? C4 O2 Pb1 109.64(17) . . ? C5 O2 Pb1 117.14(16) . . ? C2 C1 S1 108.2(2) . . ? O1 C2 C1 108.6(2) . . ? O1 C3 C4 108.2(2) . . ? O2 C4 C3 108.2(3) . . ? O2 C5 C6 108.9(2) . . ? C5 C6 S1 115.5(2) . 3_655 ? O5 Cl1 O6 112.3(3) . . ? O5 Cl1 O4 109.7(2) . . ? O6 Cl1 O4 109.6(2) . . ? O5 Cl1 O3 106.65(18) . . ? O6 Cl1 O3 109.1(2) . . ? O4 Cl1 O3 109.42(16) . . ? Cl1 O3 Pb1 108.78(13) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.59 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.087 _refine_diff_density_min -1.581 _refine_diff_density_rms 0.131 ########################################################### data_compound10 _database_code_depnum_ccdc_archive 'CCDC 769797' #TrackingRef '- IHDT-F.cif' _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H24 N2 O10 Pb S2' _chemical_formula_sum 'C12 H24 N2 O10 Pb S2' _chemical_formula_weight 627.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Cc _symmetry_space_group_name_Hall 'C -2yc' 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' _cell_length_a 10.9492(12) _cell_length_b 11.6596(13) _cell_length_c 15.2396(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.114(5) _cell_angle_gamma 90.00 _cell_volume 1945.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9959 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 32.88 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.143 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1216 _exptl_absorpt_coefficient_mu 8.940 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1745 _exptl_absorpt_correction_T_max 0.3118 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 15377 _diffrn_reflns_av_R_equivalents 0.0694 _diffrn_reflns_av_sigmaI/netI 0.0585 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 26.99 _reflns_number_total 4163 _reflns_number_gt 3954 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker APEX2' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0666P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.487(16) _refine_ls_number_reflns 4163 _refine_ls_number_parameters 283 _refine_ls_number_restraints 57 _refine_ls_R_factor_all 0.0406 _refine_ls_R_factor_gt 0.0392 _refine_ls_wR_factor_ref 0.1008 _refine_ls_wR_factor_gt 0.0995 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Pb1 Pb 0.3265(3) 0.380172(14) 0.3302(2) 0.02402(10) Uani 1 1 d . . . S1 S 0.6072(4) 0.3534(4) 0.3049(3) 0.0332(12) Uani 1 1 d . A . S2 S 0.0441(4) 0.3531(4) 0.3547(3) 0.0370(13) Uani 1 1 d . . . O1 O 0.4823(10) 0.5311(11) 0.4276(7) 0.034(2) Uani 1 1 d . A . O2 O 0.2282(11) 0.5251(11) 0.4541(7) 0.035(3) Uani 1 1 d . A . O3 O 0.1612(9) 0.5242(10) 0.2329(6) 0.029(2) Uani 1 1 d . A . O4 O 0.4203(10) 0.5336(10) 0.2144(7) 0.024(2) Uani 1 1 d . A . C1 C 0.6210(15) 0.4445(14) 0.2137(11) 0.030(3) Uani 1 1 d . . . H1A H 0.7083 0.4649 0.2072 0.035 Uiso 1 1 calc R A . H1B H 0.5971 0.4006 0.1608 0.035 Uiso 1 1 calc R . . C2 C 0.5460(14) 0.5573(15) 0.2150(11) 0.034(4) Uani 1 1 d . A . H2A H 0.5670 0.6020 0.2682 0.040 Uiso 1 1 calc R . . H2B H 0.5671 0.6042 0.1630 0.040 Uiso 1 1 calc R . . C3 C 0.347(3) 0.6330(14) 0.2084(16) 0.026(4) Uani 1 1 d . . . H3A H 0.3876 0.6910 0.1709 0.031 Uiso 1 1 calc R A . H3B H 0.3346 0.6665 0.2674 0.031 Uiso 1 1 calc R . . C4 C 0.2184(15) 0.5952(16) 0.1661(13) 0.031(4) Uani 1 1 d . A . H4A H 0.1674 0.6632 0.1529 0.037 Uiso 1 1 calc R . . H4B H 0.2310 0.5511 0.1114 0.037 Uiso 1 1 calc R . . C5 C 0.0581(16) 0.4678(17) 0.2000(10) 0.038(4) Uani 1 1 d . . . H5A H 0.0189 0.5164 0.1548 0.046 Uiso 1 1 calc R A . H5B H 0.0838 0.3954 0.1716 0.046 Uiso 1 1 calc R . . C6 C -0.0249(17) 0.4438(19) 0.2644(10) 0.048(4) Uani 1 1 d . A . H6A H -0.0952 0.4026 0.2383 0.058 Uiso 1 1 calc R . . H6B H -0.0554 0.5165 0.2897 0.058 Uiso 1 1 calc R . . C7 C 0.030(2) 0.4536(18) 0.4510(12) 0.048(5) Uani 1 1 d . A . H7A H -0.0571 0.4737 0.4586 0.057 Uiso 1 1 calc R . . H7B H 0.0567 0.4126 0.5046 0.057 Uiso 1 1 calc R . . C8 C 0.0998(15) 0.5583(16) 0.4434(11) 0.036(4) Uani 1 1 d U . . H8A H 0.0755 0.6135 0.4895 0.043 Uiso 1 1 calc R A . H8B H 0.0864 0.5941 0.3853 0.043 Uiso 1 1 calc R . . C9 C 0.304(3) 0.6293(13) 0.4681(16) 0.028(5) Uani 1 1 d . . . H9A H 0.3056 0.6757 0.4138 0.033 Uiso 1 1 calc R A . H9B H 0.2678 0.6767 0.5155 0.033 Uiso 1 1 calc R . . C10 C 0.4196(17) 0.5962(16) 0.4908(11) 0.037(5) Uani 1 1 d . A . H10A H 0.4152 0.5510 0.5456 0.045 Uiso 1 1 calc R . . H10B H 0.4681 0.6659 0.5035 0.045 Uiso 1 1 calc R . . C11 C 0.5910(14) 0.4801(18) 0.4646(12) 0.043(4) Uani 1 1 d . . . H11A H 0.5688 0.4144 0.5025 0.052 Uiso 1 1 calc R A . H11B H 0.6352 0.5372 0.5009 0.052 Uiso 1 1 calc R . . C12 C 0.6774(13) 0.4370(16) 0.3847(10) 0.034(3) Uani 1 1 d . A . H12A H 0.7461 0.3926 0.4100 0.040 Uiso 1 1 calc R . . H12B H 0.7127 0.5054 0.3558 0.040 Uiso 1 1 calc R . . N1 N 0.3227(12) 0.2089(12) 0.1733(8) 0.034(3) Uani 1 1 d . . . O5 O 0.2723(16) 0.3077(12) 0.1679(8) 0.034(3) Uani 0.54(2) 1 d PU A 1 O6 O 0.3079(17) 0.1764(13) 0.2621(10) 0.047(5) Uani 0.54(2) 1 d PU A 1 O5' O 0.2353(13) 0.2748(12) 0.1860(9) 0.020(3) Uani 0.46(2) 1 d PU A 2 O6' O 0.4207(16) 0.2188(15) 0.2159(12) 0.034(4) Uani 0.46(2) 1 d PU A 2 O7 O 0.3172(16) 0.1404(9) 0.1125(12) 0.049(4) Uani 1 1 d . A . N2 N 0.3300(11) 0.2119(11) 0.4852(10) 0.037(3) Uani 1 1 d . . . O8 O 0.2249(15) 0.2525(14) 0.4742(12) 0.046(4) Uani 0.54(2) 1 d PU A 1 O9 O 0.4104(18) 0.2429(16) 0.4461(12) 0.062(5) Uani 0.54(2) 1 d PU A 1 O8' O 0.306(2) 0.1800(14) 0.4035(11) 0.049(6) Uani 0.46(2) 1 d PDU A 2 O9' O 0.3185(17) 0.3106(12) 0.4893(9) 0.042(4) Uani 0.46(2) 1 d PDU A 2 O10 O 0.3320(19) 0.1453(12) 0.5476(12) 0.068(6) Uani 1 1 d . A . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.02392(16) 0.02307(13) 0.02506(14) 0.0017(3) -0.00343(10) -0.0055(2) S1 0.033(3) 0.038(2) 0.029(3) 0.0008(19) 0.001(2) 0.0197(17) S2 0.031(3) 0.035(2) 0.046(4) -0.007(2) 0.001(2) 0.0132(17) O1 0.029(6) 0.046(6) 0.027(6) -0.002(5) -0.008(4) 0.003(4) O2 0.024(5) 0.044(6) 0.038(6) -0.012(5) -0.003(4) -0.012(4) O3 0.022(5) 0.046(6) 0.019(5) 0.004(4) -0.003(3) 0.008(4) O4 0.028(5) 0.022(4) 0.023(4) -0.002(3) 0.003(3) -0.005(3) C1 0.025(7) 0.032(6) 0.032(8) 0.007(5) 0.009(6) 0.006(5) C2 0.026(5) 0.040(6) 0.035(6) 0.018(4) -0.004(4) -0.019(4) C3 0.039(9) 0.030(6) 0.009(7) 0.002(4) 0.001(5) -0.006(5) C4 0.019(6) 0.037(7) 0.035(9) 0.007(6) -0.007(5) 0.001(5) C5 0.045(9) 0.052(8) 0.017(6) -0.008(5) -0.004(6) -0.011(6) C6 0.057(10) 0.062(10) 0.025(6) -0.003(6) -0.023(6) 0.009(7) C7 0.040(10) 0.078(13) 0.025(8) -0.013(8) -0.002(7) 0.009(9) C8 0.034(5) 0.038(5) 0.037(5) -0.001(3) -0.003(3) 0.001(3) C9 0.048(10) 0.025(6) 0.010(8) 0.000(4) 0.005(6) -0.013(5) C10 0.051(10) 0.045(8) 0.017(7) -0.005(6) 0.009(7) -0.028(7) C11 0.021(7) 0.070(10) 0.039(8) -0.015(7) -0.005(6) -0.019(7) C12 0.015(6) 0.049(7) 0.036(7) -0.004(5) 0.002(5) 0.006(5) N1 0.037(8) 0.033(8) 0.034(7) -0.012(6) -0.007(6) -0.009(5) O5 0.034(4) 0.033(4) 0.033(4) 0.0011(19) -0.0010(19) 0.002(2) O6 0.049(5) 0.045(5) 0.047(5) -0.0003(19) 0.003(2) -0.001(2) O5' 0.018(4) 0.020(4) 0.021(4) -0.0002(19) -0.0002(19) 0.0003(19) O6' 0.034(5) 0.034(5) 0.035(5) -0.002(2) -0.001(2) 0.001(2) O7 0.051(8) 0.040(7) 0.058(10) -0.014(6) -0.016(6) -0.014(5) N2 0.025(7) 0.017(6) 0.069(10) 0.000(6) -0.006(6) -0.006(5) O8 0.045(5) 0.046(4) 0.046(5) 0.001(2) 0.001(2) 0.002(2) O9 0.061(6) 0.062(6) 0.062(6) 0.003(2) 0.000(2) 0.001(2) O8' 0.050(6) 0.048(6) 0.050(6) 0.000(2) -0.001(2) 0.000(2) O9' 0.044(5) 0.041(5) 0.041(5) 0.0010(19) -0.002(2) 0.002(2) O10 0.103(13) 0.042(7) 0.060(11) 0.029(7) 0.030(9) -0.021(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Pb1 O9 2.553(17) . ? Pb1 O9' 2.558(14) . ? Pb1 O8' 2.597(19) . ? Pb1 O6 2.601(16) . ? Pb1 O5 2.680(12) . ? Pb1 O5' 2.707(12) . ? Pb1 O4 2.716(10) . ? Pb1 O2 2.755(12) . ? Pb1 O1 2.863(12) . ? Pb1 O8 2.877(16) . ? Pb1 O3 2.879(11) . ? Pb1 S1 3.114(6) . ? S1 C12 1.737(17) . ? S1 C1 1.756(16) . ? S2 C7 1.885(19) . ? S2 C6 1.892(18) . ? O1 C10 1.41(2) . ? O1 C11 1.45(2) . ? O2 C8 1.47(2) . ? O2 C9 1.48(2) . ? O3 C5 1.398(18) . ? O3 C4 1.45(2) . ? O4 C2 1.404(19) . ? O4 C3 1.41(3) . ? C1 C2 1.55(2) . ? C3 C4 1.61(3) . ? C5 C6 1.37(3) . ? C7 C8 1.44(3) . ? C9 C10 1.37(4) . ? C11 C12 1.62(2) . ? N1 O7 1.224(18) . ? N1 O5' 1.244(18) . ? N1 O6' 1.26(2) . ? N1 O5 1.281(19) . ? N1 O6 1.416(19) . ? N2 O9 1.12(2) . ? N2 O9' 1.160(19) . ? N2 O10 1.23(2) . ? N2 O8 1.26(2) . ? N2 O8' 1.33(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O9 Pb1 O9' 32.7(5) . . ? O9 Pb1 O8' 34.0(6) . . ? O9' Pb1 O8' 45.9(2) . . ? O9 Pb1 O6 74.4(6) . . ? O9' Pb1 O6 94.9(4) . . ? O8' Pb1 O6 49.0(3) . . ? O9 Pb1 O5 121.3(5) . . ? O9' Pb1 O5 140.1(4) . . ? O8' Pb1 O5 95.4(4) . . ? O6 Pb1 O5 47.7(4) . . ? O9 Pb1 O5' 114.1(6) . . ? O9' Pb1 O5' 127.7(4) . . ? O8' Pb1 O5' 84.8(5) . . ? O6 Pb1 O5' 39.9(5) . . ? O5 Pb1 O5' 13.3(3) . . ? O9 Pb1 O4 136.6(5) . . ? O9' Pb1 O4 147.0(4) . . ? O8' Pb1 O4 154.8(5) . . ? O6 Pb1 O4 111.8(4) . . ? O5 Pb1 O4 72.0(4) . . ? O5' Pb1 O4 84.9(4) . . ? O9 Pb1 O2 92.9(5) . . ? O9' Pb1 O2 62.0(4) . . ? O8' Pb1 O2 102.8(4) . . ? O6 Pb1 O2 143.5(4) . . ? O5 Pb1 O2 137.7(4) . . ? O5' Pb1 O2 133.7(4) . . ? O4 Pb1 O2 101.0(2) . . ? O9 Pb1 O1 79.3(5) . . ? O9' Pb1 O1 74.1(4) . . ? O8' Pb1 O1 112.4(4) . . ? O6 Pb1 O1 144.5(5) . . ? O5 Pb1 O1 143.4(5) . . ? O5' Pb1 O1 156.6(4) . . ? O4 Pb1 O1 72.9(3) . . ? O2 Pb1 O1 60.1(3) . . ? O9 Pb1 O8 44.6(5) . . ? O9' Pb1 O8 25.7(5) . . ? O8' Pb1 O8 34.2(5) . . ? O6 Pb1 O8 78.6(5) . . ? O5 Pb1 O8 117.1(5) . . ? O5' Pb1 O8 104.0(5) . . ? O4 Pb1 O8 169.6(4) . . ? O2 Pb1 O8 69.0(5) . . ? O1 Pb1 O8 98.8(4) . . ? O9 Pb1 O3 161.3(5) . . ? O9' Pb1 O3 130.6(5) . . ? O8' Pb1 O3 133.7(5) . . ? O6 Pb1 O3 106.2(4) . . ? O5 Pb1 O3 64.5(4) . . ? O5' Pb1 O3 67.4(4) . . ? O4 Pb1 O3 61.3(3) . . ? O2 Pb1 O3 75.5(4) . . ? O1 Pb1 O3 106.36(14) . . ? O8 Pb1 O3 116.8(4) . . ? O9 Pb1 S1 70.7(5) . . ? O9' Pb1 S1 97.0(4) . . ? O8' Pb1 S1 92.9(5) . . ? O6 Pb1 S1 86.3(4) . . ? O5 Pb1 S1 94.1(4) . . ? O5' Pb1 S1 102.5(3) . . ? O4 Pb1 S1 67.1(3) . . ? O2 Pb1 S1 122.3(3) . . ? O1 Pb1 S1 62.5(3) . . ? O8 Pb1 S1 115.2(3) . . ? O3 Pb1 S1 127.9(2) . . ? C12 S1 C1 100.1(8) . . ? C12 S1 Pb1 107.0(5) . . ? C1 S1 Pb1 97.1(6) . . ? C7 S2 C6 100.7(9) . . ? C7 S2 Pb1 96.5(7) . . ? C6 S2 Pb1 104.5(7) . . ? C10 O1 C11 110.9(13) . . ? C10 O1 Pb1 113.3(9) . . ? C11 O1 Pb1 116.1(10) . . ? C8 O2 C9 109.5(15) . . ? C8 O2 Pb1 117.5(9) . . ? C9 O2 Pb1 112.5(12) . . ? C5 O3 C4 111.5(12) . . ? C5 O3 Pb1 114.6(10) . . ? C4 O3 Pb1 114.9(8) . . ? C2 O4 C3 113.2(14) . . ? C2 O4 Pb1 119.9(9) . . ? C3 O4 Pb1 111.6(11) . . ? C2 C1 S1 117.2(11) . . ? O4 C2 C1 110.6(13) . . ? O4 C3 C4 107.3(14) . . ? O3 C4 C3 104.7(14) . . ? C6 C5 O3 112.1(12) . . ? C5 C6 S2 111.8(14) . . ? C8 C7 S2 114.8(13) . . ? C7 C8 O2 106.0(16) . . ? C10 C9 O2 108.7(15) . . ? C9 C10 O1 115.6(17) . . ? O1 C11 C12 108.4(13) . . ? C11 C12 S1 116.2(10) . . ? O7 N1 O5' 119.0(13) . . ? O7 N1 O6' 119.4(14) . . ? O5' N1 O6' 121.2(13) . . ? O7 N1 O5 121.2(14) . . ? O5' N1 O5 28.5(8) . . ? O6' N1 O5 108.5(14) . . ? O7 N1 O6 122.9(15) . . ? O5' N1 O6 85.8(12) . . ? O6' N1 O6 68.3(14) . . ? O5 N1 O6 104.6(12) . . ? N1 O5 Pb1 97.5(9) . . ? N1 O6 Pb1 97.4(9) . . ? N1 O5' Pb1 97.2(8) . . ? O9 N2 O9' 78.1(14) . . ? O9 N2 O10 127.0(18) . . ? O9' N2 O10 126.0(16) . . ? O9 N2 O8 121.7(16) . . ? O9' N2 O8 62.1(13) . . ? O10 N2 O8 110.9(16) . . ? O9 N2 O8' 75.3(16) . . ? O9' N2 O8' 107.9(14) . . ? O10 N2 O8' 123.6(15) . . ? O8 N2 O8' 78.4(15) . . ? N2 O8 Pb1 86.7(10) . . ? N2 O9 Pb1 106.7(13) . . ? N2 O8' Pb1 97.8(10) . . ? N2 O9' Pb1 105.1(10) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.163 _refine_diff_density_min -2.680 _refine_diff_density_rms 0.207