# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name 'In-Hyeok Park' 'Hyun Jee Kim' 'Shim Sung Lee' _publ_contact_author_email pihghost@nate.com _publ_contact_author_name 'In-Hyeok Park' data_L _database_code_depnum_ccdc_archive 'CCDC 863927' #TrackingRef '9181_web_deposit_cif_file_0_In-HyeokPark_1327158897.CuX.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H26 O2 S2' _chemical_formula_sum 'C25 H26 O2 S2' _chemical_formula_weight 422.58 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 5.5135(2) _cell_length_b 8.1356(3) _cell_length_c 47.2858(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2121.03(13) _cell_formula_units_Z 4 _cell_measurement_temperature 174(2) _cell_measurement_reflns_used 9817 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 31.24 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.323 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 0.270 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9114 _exptl_absorpt_correction_T_max 0.9479 _exptl_absorpt_process_details ? _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 38369 _diffrn_reflns_av_R_equivalents 0.0356 _diffrn_reflns_av_sigmaI/netI 0.0204 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -62 _diffrn_reflns_limit_l_max 62 _diffrn_reflns_theta_min 0.86 _diffrn_reflns_theta_max 28.25 _reflns_number_total 5243 _reflns_number_gt 5098 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^+1.3207P] 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 0.07(9) _refine_ls_number_reflns 5243 _refine_ls_number_parameters 281 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0490 _refine_ls_R_factor_gt 0.0477 _refine_ls_wR_factor_ref 0.1157 _refine_ls_wR_factor_gt 0.1149 _refine_ls_goodness_of_fit_ref 1.155 _refine_ls_restrained_S_all 1.163 _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 S1 S 0.70146(13) 1.03564(9) 0.053444(13) 0.04072(16) Uani 1 1 d . . . S2 S 0.71080(11) 0.95425(8) 0.204345(12) 0.03398(14) Uani 1 1 d . . . O1 O 1.0266(4) 0.6330(3) 0.16457(4) 0.0646(7) Uani 1 1 d . . . O2 O 1.0118(4) 0.6716(3) 0.07837(5) 0.0641(7) Uani 1 1 d . . . C1 C 1.2022(8) 0.5286(5) 0.14662(8) 0.0301(10) Uani 0.552(6) 1 d P A 1 H1A H 1.3613 0.5182 0.1561 0.036 Uiso 0.552(6) 1 calc PR A 1 H1B H 1.1351 0.4173 0.1434 0.036 Uiso 0.552(6) 1 calc PR A 1 C3 C 1.0115(14) 0.5867(9) 0.10050(13) 0.067(2) Uani 0.552(6) 1 d PU A 1 H3A H 1.0089 0.4692 0.0951 0.081 Uiso 0.552(6) 1 calc PR A 1 H3B H 0.8599 0.6097 0.1110 0.081 Uiso 0.552(6) 1 calc PR A 1 C1' C 1.0175(13) 0.5765(10) 0.14091(11) 0.055(2) Uani 0.448(6) 1 d P A 2 H1'A H 0.8652 0.6154 0.1321 0.066 Uiso 0.448(6) 1 calc PR A 2 H1'B H 1.0053 0.4555 0.1426 0.066 Uiso 0.448(6) 1 calc PR A 2 C3' C 1.1842(10) 0.5447(7) 0.09258(10) 0.0307(12) Uani 0.448(6) 1 d P A 2 H3'A H 1.1062 0.4354 0.0940 0.037 Uiso 0.448(6) 1 calc PR A 2 H3'B H 1.3378 0.5340 0.0819 0.037 Uiso 0.448(6) 1 calc PR A 2 C2 C 1.2262(5) 0.6149(3) 0.12046(5) 0.0343(5) Uani 1 1 d . . . H2A H 1.3772 0.5790 0.1110 0.041 Uiso 0.552(6) 1 calc PR A 1 H2B H 1.2409 0.7340 0.1244 0.041 Uiso 0.552(6) 1 calc PR A 1 H2C H 1.3795 0.5702 0.1282 0.041 Uiso 0.448(6) 1 d PR A 2 H2D H 1.2443 0.7356 0.1188 0.041 Uiso 0.448(6) 1 d PR A 2 C4 C 0.8912(5) 0.6167(4) 0.05477(5) 0.0432(6) Uani 1 1 d . A . C5 C 0.9767(5) 0.4845(4) 0.03898(6) 0.0476(7) Uani 1 1 d . . . H5A H 1.1198 0.4285 0.0447 0.057 Uiso 1 1 calc R A . C6 C 0.8550(6) 0.4346(4) 0.01513(6) 0.0481(7) Uani 1 1 d . A . H6A H 0.9146 0.3452 0.0042 0.058 Uiso 1 1 calc R . . C7 C 0.6467(6) 0.5145(3) 0.00713(6) 0.0485(7) Uani 1 1 d . . . H7A H 0.5603 0.4790 -0.0091 0.058 Uiso 1 1 calc R A . C8 C 0.5628(5) 0.6459(3) 0.02259(5) 0.0410(6) Uani 1 1 d . A . H8A H 0.4206 0.7014 0.0165 0.049 Uiso 1 1 calc R . . C9 C 0.6800(5) 0.6996(3) 0.04685(5) 0.0354(5) Uani 1 1 d . . . C10 C 0.5800(5) 0.8378(3) 0.06420(6) 0.0461(7) Uani 1 1 d . A . H10A H 0.6193 0.8186 0.0844 0.055 Uiso 1 1 calc R . . H10B H 0.4012 0.8396 0.0623 0.055 Uiso 1 1 calc R . . C11 C 0.4773(5) 1.1695(3) 0.06966(5) 0.0380(5) Uani 1 1 d . . . H11A H 0.5148 1.2849 0.0646 0.046 Uiso 1 1 calc R . . H11B H 0.3154 1.1429 0.0618 0.046 Uiso 1 1 calc R . . C12 C 0.4686(4) 1.1541(3) 0.10146(4) 0.0269(4) Uani 1 1 d . . . C13 C 0.6584(4) 1.2150(3) 0.11787(5) 0.0334(5) Uani 1 1 d . . . H13A H 0.7891 1.2705 0.1089 0.040 Uiso 1 1 calc R . . C14 C 0.2791(4) 1.0763(3) 0.11504(5) 0.0288(4) Uani 1 1 d . . . H14A H 0.1471 1.0349 0.1043 0.035 Uiso 1 1 calc R . . C15 C 0.6602(4) 1.1963(3) 0.14674(5) 0.0315(5) Uani 1 1 d . . . H15A H 0.7922 1.2383 0.1574 0.038 Uiso 1 1 calc R . . C16 C 0.2788(4) 1.0576(3) 0.14437(5) 0.0305(4) Uani 1 1 d . . . H16A H 0.1464 1.0042 0.1534 0.037 Uiso 1 1 calc R . . C17 C 0.4707(4) 1.1165(3) 0.16049(4) 0.0263(4) Uani 1 1 d . . . C18 C 0.4771(5) 1.0938(3) 0.19213(5) 0.0344(5) Uani 1 1 d . . . H18A H 0.3175 1.0519 0.1984 0.041 Uiso 1 1 calc R . . H18B H 0.5026 1.2023 0.2011 0.041 Uiso 1 1 calc R . . C19 C 0.6012(5) 0.7649(3) 0.18857(5) 0.0352(5) Uani 1 1 d . A . H19A H 0.4250 0.7533 0.1921 0.042 Uiso 1 1 calc R . . H19B H 0.6279 0.7675 0.1679 0.042 Uiso 1 1 calc R . . C20 C 0.7343(4) 0.6219(3) 0.20127(4) 0.0299(4) Uani 1 1 d . . . C21 C 0.6536(4) 0.5486(3) 0.22618(5) 0.0337(5) Uani 1 1 d . A . H21A H 0.5108 0.5886 0.2351 0.040 Uiso 1 1 calc R . . C22 C 0.7782(5) 0.4182(3) 0.23825(5) 0.0370(5) Uani 1 1 d . . . H22A H 0.7200 0.3697 0.2552 0.044 Uiso 1 1 calc R A . C23 C 0.9858(5) 0.3586(3) 0.22574(5) 0.0390(5) Uani 1 1 d . A . H23A H 1.0721 0.2701 0.2342 0.047 Uiso 1 1 calc R . . C24 C 1.0678(5) 0.4279(4) 0.20095(5) 0.0431(6) Uani 1 1 d . . . H25A H 1.2090 0.3855 0.1920 0.052 Uiso 1 1 calc R A . C25 C 0.9445(4) 0.5597(4) 0.18892(5) 0.0391(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 S1 0.0448(3) 0.0465(3) 0.0309(3) 0.0004(3) 0.0100(3) -0.0112(3) S2 0.0339(3) 0.0383(3) 0.0298(3) 0.0013(2) -0.0074(2) -0.0044(3) O1 0.0449(11) 0.1034(19) 0.0456(11) 0.0393(12) 0.0177(10) 0.0273(13) O2 0.0558(13) 0.0899(18) 0.0466(11) -0.0201(12) -0.0171(11) 0.0085(13) C1 0.031(2) 0.0265(19) 0.0323(19) -0.0048(15) -0.0055(17) -0.0015(18) C3 0.066(3) 0.077(4) 0.059(3) 0.024(3) -0.017(3) -0.030(3) C1' 0.056(4) 0.084(5) 0.026(3) -0.006(3) 0.010(3) -0.045(4) C3' 0.032(3) 0.029(2) 0.031(2) 0.004(2) 0.003(2) 0.000(2) C2 0.0332(11) 0.0324(11) 0.0373(11) -0.0032(9) 0.0034(10) -0.0019(10) C4 0.0337(12) 0.0641(18) 0.0319(12) -0.0041(12) 0.0005(10) -0.0127(12) C5 0.0366(13) 0.0582(18) 0.0479(14) -0.0003(13) 0.0062(12) 0.0027(13) C6 0.0620(18) 0.0393(14) 0.0429(14) -0.0042(12) 0.0123(12) -0.0094(14) C7 0.067(2) 0.0398(14) 0.0385(13) -0.0020(11) -0.0066(13) -0.0152(14) C8 0.0396(13) 0.0427(14) 0.0408(13) 0.0106(11) -0.0101(11) -0.0079(12) C9 0.0339(12) 0.0408(12) 0.0316(11) -0.0002(10) 0.0091(9) -0.0092(11) C10 0.0472(15) 0.0412(14) 0.0499(15) 0.0005(12) 0.0209(12) -0.0046(12) C11 0.0418(13) 0.0414(13) 0.0307(11) 0.0104(10) -0.0026(10) 0.0014(12) C12 0.0310(10) 0.0217(9) 0.0279(10) 0.0016(8) -0.0015(8) 0.0034(9) C13 0.0323(12) 0.0329(11) 0.0348(11) 0.0045(10) 0.0006(9) -0.0110(10) C14 0.0244(9) 0.0289(10) 0.0332(10) -0.0023(8) -0.0019(9) 0.0034(9) C15 0.0285(11) 0.0302(11) 0.0357(11) -0.0010(9) -0.0052(9) -0.0061(9) C16 0.0238(9) 0.0353(11) 0.0325(10) -0.0017(9) 0.0033(8) 0.0002(10) C17 0.0264(10) 0.0249(10) 0.0276(10) -0.0037(8) -0.0014(8) 0.0069(8) C18 0.0359(12) 0.0399(13) 0.0273(10) -0.0060(9) 0.0004(9) 0.0055(10) C19 0.0320(11) 0.0426(13) 0.0311(11) -0.0015(10) -0.0099(9) -0.0035(10) C20 0.0287(10) 0.0343(11) 0.0267(9) -0.0017(9) -0.0057(9) -0.0057(9) C21 0.0405(12) 0.0341(11) 0.0264(10) -0.0071(9) 0.0048(9) -0.0044(11) C22 0.0550(15) 0.0307(11) 0.0253(10) 0.0003(9) 0.0025(10) -0.0066(11) C23 0.0488(14) 0.0346(12) 0.0337(11) -0.0006(10) -0.0111(11) -0.0008(12) C24 0.0332(12) 0.0618(17) 0.0342(12) 0.0029(12) -0.0029(10) 0.0070(12) C25 0.0286(11) 0.0624(16) 0.0264(10) 0.0109(11) -0.0040(9) -0.0057(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 S1 C10 1.816(3) . ? S1 C11 1.817(3) . ? S2 C18 1.812(2) . ? S2 C19 1.815(3) . ? O1 C1' 1.210(6) . ? O1 C25 1.373(3) . ? O1 C1 1.542(5) . ? O2 C3 1.254(6) . ? O2 C4 1.374(3) . ? O2 C3' 1.556(6) . ? C1 C2 1.429(5) . ? C3 C2 1.531(6) . ? C1' C2 1.535(6) . ? C3' C2 1.456(5) . ? C4 C5 1.392(4) . ? C4 C9 1.397(4) . ? C5 C6 1.374(4) . ? C6 C7 1.373(4) . ? C7 C8 1.375(4) . ? C8 C9 1.387(3) . ? C9 C10 1.497(4) . ? C11 C12 1.510(3) . ? C12 C14 1.380(3) . ? C12 C13 1.393(3) . ? C13 C15 1.373(3) . ? C14 C16 1.395(3) . ? C15 C17 1.391(3) . ? C16 C17 1.390(3) . ? C17 C18 1.508(3) . ? C19 C20 1.501(3) . ? C20 C21 1.393(3) . ? C20 C25 1.393(3) . ? C21 C22 1.387(4) . ? C22 C23 1.377(4) . ? C23 C24 1.377(4) . ? C24 C25 1.392(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C10 S1 C11 99.34(12) . . ? C18 S2 C19 99.43(11) . . ? C1' O1 C25 126.6(4) . . ? C1' O1 C1 46.2(4) . . ? C25 O1 C1 115.4(3) . . ? C3 O2 C4 119.9(4) . . ? C3 O2 C3' 43.5(4) . . ? C4 O2 C3' 115.5(3) . . ? C2 C1 O1 105.3(3) . . ? O2 C3 C2 115.5(5) . . ? O1 C1' C2 118.3(5) . . ? C2 C3' O2 103.2(3) . . ? C1 C2 C3' 125.2(3) . . ? C1 C2 C3 112.8(3) . . ? C3' C2 C3 42.2(4) . . ? C1 C2 C1' 44.4(4) . . ? C3' C2 C1' 111.8(3) . . ? C3 C2 C1' 77.2(4) . . ? O2 C4 C5 121.5(3) . . ? O2 C4 C9 117.7(3) . . ? C5 C4 C9 120.8(2) . . ? C6 C5 C4 120.2(3) . . ? C7 C6 C5 119.7(3) . . ? C6 C7 C8 120.2(3) . . ? C7 C8 C9 121.8(3) . . ? C8 C9 C4 117.3(2) . . ? C8 C9 C10 121.2(3) . . ? C4 C9 C10 121.5(2) . . ? C9 C10 S1 112.09(17) . . ? C12 C11 S1 113.10(17) . . ? C14 C12 C13 118.2(2) . . ? C14 C12 C11 121.7(2) . . ? C13 C12 C11 120.1(2) . . ? C15 C13 C12 121.3(2) . . ? C12 C14 C16 120.9(2) . . ? C13 C15 C17 120.7(2) . . ? C17 C16 C14 120.4(2) . . ? C16 C17 C15 118.5(2) . . ? C16 C17 C18 121.3(2) . . ? C15 C17 C18 120.2(2) . . ? C17 C18 S2 114.19(16) . . ? C20 C19 S2 109.32(15) . . ? C21 C20 C25 117.7(2) . . ? C21 C20 C19 120.9(2) . . ? C25 C20 C19 121.4(2) . . ? C22 C21 C20 121.2(2) . . ? C23 C22 C21 120.3(2) . . ? C22 C23 C24 119.6(2) . . ? C23 C24 C25 120.2(2) . . ? O1 C25 C24 121.1(2) . . ? O1 C25 C20 117.9(2) . . ? C24 C25 C20 121.0(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.25 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.488 _refine_diff_density_min -0.385 _refine_diff_density_rms 0.065 ############################################################ data_1 _database_code_depnum_ccdc_archive 'CCDC 863928' #TrackingRef '9181_web_deposit_cif_file_0_In-HyeokPark_1327158897.CuX.cif' _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H26 Cl2 Cu N O2 S2' _chemical_formula_sum 'C27 H26 Cl2 Cu N O2 S2' _chemical_formula_weight 595.05 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 11.6776(6) _cell_length_b 18.6014(10) _cell_length_c 13.2518(7) _cell_angle_alpha 90.00 _cell_angle_beta 108.458(3) _cell_angle_gamma 90.00 _cell_volume 2730.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9898 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 30.70 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.448 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 1.174 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.7587 _exptl_absorpt_correction_T_max 0.9557 _exptl_absorpt_process_details ? _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 49050 _diffrn_reflns_av_R_equivalents 0.1350 _diffrn_reflns_av_sigmaI/netI 0.0563 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 28.00 _reflns_number_total 6597 _reflns_number_gt 5465 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0689P)^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 6597 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0466 _refine_ls_R_factor_gt 0.0395 _refine_ls_wR_factor_ref 0.1175 _refine_ls_wR_factor_gt 0.1137 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _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 Cu1 Cu 0.306675(18) 0.085680(13) 0.754742(17) 0.01742(9) Uani 1 1 d . . . Cl1 Cl 0.30917(4) 0.05906(3) 0.92225(4) 0.03212(15) Uani 1 1 d . . . Cl2 Cl 0.30832(5) 0.02359(3) 0.60865(4) 0.03335(15) Uani 1 1 d . . . S1 S 0.51628(4) 0.10228(3) 0.79508(4) 0.01779(12) Uani 1 1 d . . . S2 S 1.09422(4) 0.09165(3) 0.70917(4) 0.01844(12) Uani 1 1 d . . . O1 O 0.90273(13) 0.21222(8) 0.60523(12) 0.0326(4) Uani 1 1 d . . . O2 O 0.69969(13) 0.23377(8) 0.85552(13) 0.0315(4) Uani 1 1 d . . . C1 C 0.85968(19) 0.26741(12) 0.65925(18) 0.0304(5) Uani 1 1 d . . . H1A H 0.8037 0.3000 0.6076 0.036 Uiso 1 1 calc R . . H1B H 0.9278 0.2961 0.7052 0.036 Uiso 1 1 calc R . . C2 C 0.79525(19) 0.22851(12) 0.72520(19) 0.0315(5) Uani 1 1 d . . . H2A H 0.8519 0.1944 0.7732 0.038 Uiso 1 1 calc R . . H2B H 0.7278 0.2003 0.6775 0.038 Uiso 1 1 calc R . . C3 C 0.7461(2) 0.27889(12) 0.79085(18) 0.0308(5) Uani 1 1 d . . . H3A H 0.8109 0.3103 0.8355 0.037 Uiso 1 1 calc R . . H3B H 0.6814 0.3095 0.7443 0.037 Uiso 1 1 calc R . . C4 C 0.62409(17) 0.26222(11) 0.90521(16) 0.0253(4) Uani 1 1 d . . . C5 C 0.60890(19) 0.33509(12) 0.91834(18) 0.0324(5) Uani 1 1 d . . . H5A H 0.6520 0.3695 0.8915 0.039 Uiso 1 1 calc R . . C6 C 0.5291(2) 0.35720(13) 0.97165(18) 0.0360(5) Uani 1 1 d . . . H6A H 0.5182 0.4071 0.9812 0.043 Uiso 1 1 calc R . . C7 C 0.4659(2) 0.30749(14) 1.01057(19) 0.0379(6) Uani 1 1 d . . . H7A H 0.4113 0.3230 1.0462 0.045 Uiso 1 1 calc R . . C8 C 0.48267(18) 0.23491(13) 0.99719(17) 0.0306(5) Uani 1 1 d . . . H8A H 0.4395 0.2007 1.0243 0.037 Uiso 1 1 calc R . . C9 C 0.56134(17) 0.21120(11) 0.94498(15) 0.0234(4) Uani 1 1 d . . . C10 C 0.58299(17) 0.13284(11) 0.93256(15) 0.0236(4) Uani 1 1 d . . . H10A H 0.5482 0.1047 0.9792 0.028 Uiso 1 1 calc R . . H10B H 0.6710 0.1237 0.9557 0.028 Uiso 1 1 calc R . . C11 C 0.58095(16) 0.01263(10) 0.80801(16) 0.0201(4) Uani 1 1 d . . . H11A H 0.5907 -0.0060 0.8802 0.024 Uiso 1 1 calc R . . H11B H 0.5249 -0.0198 0.7561 0.024 Uiso 1 1 calc R . . C12 C 0.70170(16) 0.01213(10) 0.78933(15) 0.0179(4) Uani 1 1 d . . . C13 C 0.70707(17) 0.00783(11) 0.68601(16) 0.0219(4) Uani 1 1 d . . . H13A H 0.6343 0.0078 0.6277 0.026 Uiso 1 1 calc R . . C14 C 0.81729(17) 0.00359(11) 0.66682(16) 0.0226(4) Uani 1 1 d . . . H14A H 0.8190 0.0002 0.5958 0.027 Uiso 1 1 calc R . . C15 C 0.92452(16) 0.00433(10) 0.75052(15) 0.0195(4) Uani 1 1 d . . . C16 C 0.91914(16) 0.00964(11) 0.85343(15) 0.0231(4) Uani 1 1 d . . . H16A H 0.9920 0.0110 0.9115 0.028 Uiso 1 1 calc R . . C17 C 0.80910(17) 0.01293(11) 0.87303(15) 0.0217(4) Uani 1 1 d . . . H17A H 0.8075 0.0157 0.9441 0.026 Uiso 1 1 calc R . . C18 C 1.04467(16) 0.00145(11) 0.73108(16) 0.0217(4) Uani 1 1 d . . . H18A H 1.0378 -0.0289 0.6680 0.026 Uiso 1 1 calc R . . H18B H 1.1054 -0.0207 0.7932 0.026 Uiso 1 1 calc R . . C19 C 1.02582(18) 0.09831(11) 0.56495(16) 0.0235(4) Uani 1 1 d . . . H19A H 1.0633 0.0625 0.5299 0.028 Uiso 1 1 calc R . . H19B H 0.9385 0.0874 0.5454 0.028 Uiso 1 1 calc R . . C20 C 1.04245(16) 0.17224(11) 0.52629(15) 0.0230(4) Uani 1 1 d . . . C21 C 1.12004(18) 0.18485(13) 0.46766(16) 0.0295(5) Uani 1 1 d . . . H21A H 1.1629 0.1458 0.4505 0.035 Uiso 1 1 calc R . . C22 C 1.1360(2) 0.25322(14) 0.43386(18) 0.0361(5) Uani 1 1 d . . . H22A H 1.1889 0.2611 0.3933 0.043 Uiso 1 1 calc R . . C23 C 1.0744(2) 0.30990(14) 0.45959(19) 0.0374(5) Uani 1 1 d . . . H23A H 1.0860 0.3571 0.4371 0.045 Uiso 1 1 calc R . . C24 C 0.99564(19) 0.29932(13) 0.51782(18) 0.0328(5) Uani 1 1 d . . . H24A H 0.9536 0.3388 0.5351 0.039 Uiso 1 1 calc R . . C25 C 0.97927(17) 0.23019(12) 0.55036(16) 0.0254(4) Uani 1 1 d . . . N1 N 0.29745(14) 0.20188(10) 0.72607(14) 0.0274(4) Uani 1 1 d . . . C26 C 0.30001(18) 0.26228(12) 0.71571(17) 0.0288(5) Uani 1 1 d . . . C27 C 0.3039(3) 0.34005(13) 0.7029(2) 0.0554(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01693(15) 0.01821(15) 0.01642(14) 0.00024(8) 0.00428(10) -0.00003(8) Cl1 0.0268(3) 0.0485(4) 0.0199(2) 0.0097(2) 0.0057(2) -0.0061(2) Cl2 0.0308(3) 0.0391(3) 0.0242(3) -0.0129(2) 0.0002(2) 0.0113(2) S1 0.0173(2) 0.0160(2) 0.0196(2) 0.00028(18) 0.00516(18) -0.00044(18) S2 0.0170(2) 0.0186(3) 0.0192(2) 0.00169(17) 0.00515(19) 0.00066(17) O1 0.0317(8) 0.0287(9) 0.0432(9) 0.0109(7) 0.0202(7) 0.0059(6) O2 0.0345(8) 0.0222(8) 0.0447(9) -0.0010(7) 0.0225(7) -0.0021(6) C1 0.0280(11) 0.0315(13) 0.0324(12) 0.0053(10) 0.0106(9) 0.0044(9) C2 0.0297(11) 0.0295(13) 0.0379(12) 0.0030(10) 0.0145(9) -0.0007(9) C3 0.0312(11) 0.0269(12) 0.0363(12) 0.0019(9) 0.0134(10) -0.0052(9) C4 0.0228(10) 0.0255(11) 0.0265(10) -0.0057(9) 0.0061(8) -0.0012(8) C5 0.0341(11) 0.0236(11) 0.0357(12) -0.0065(9) 0.0056(9) -0.0051(9) C6 0.0393(12) 0.0273(13) 0.0343(12) -0.0132(10) 0.0016(10) 0.0032(10) C7 0.0327(12) 0.0458(15) 0.0347(12) -0.0158(11) 0.0101(10) 0.0033(11) C8 0.0267(10) 0.0382(13) 0.0271(11) -0.0082(9) 0.0089(9) -0.0045(9) C9 0.0211(9) 0.0241(11) 0.0209(9) -0.0052(8) 0.0010(8) -0.0035(8) C10 0.0224(9) 0.0260(11) 0.0195(9) -0.0028(8) 0.0024(7) -0.0039(8) C11 0.0174(9) 0.0153(10) 0.0269(10) 0.0016(8) 0.0061(8) -0.0015(7) C12 0.0178(9) 0.0124(9) 0.0222(9) 0.0018(7) 0.0045(7) 0.0001(7) C13 0.0171(9) 0.0243(11) 0.0198(9) 0.0027(8) -0.0004(7) -0.0013(8) C14 0.0229(9) 0.0260(11) 0.0178(9) -0.0009(8) 0.0048(8) -0.0027(8) C15 0.0201(9) 0.0163(9) 0.0218(9) 0.0020(7) 0.0062(7) -0.0008(7) C16 0.0162(9) 0.0304(11) 0.0192(9) 0.0032(8) 0.0007(7) -0.0019(8) C17 0.0211(9) 0.0265(11) 0.0171(9) 0.0019(8) 0.0056(7) -0.0014(8) C18 0.0209(9) 0.0192(10) 0.0252(10) 0.0035(8) 0.0077(8) 0.0008(8) C19 0.0208(9) 0.0258(11) 0.0205(10) 0.0030(8) 0.0019(8) 0.0003(8) C20 0.0197(9) 0.0273(11) 0.0185(9) 0.0057(8) 0.0009(7) 0.0007(8) C21 0.0268(10) 0.0378(13) 0.0230(10) 0.0042(9) 0.0065(8) 0.0029(9) C22 0.0356(12) 0.0460(15) 0.0307(12) 0.0120(11) 0.0161(10) 0.0003(11) C23 0.0417(13) 0.0339(13) 0.0362(12) 0.0157(11) 0.0118(10) -0.0003(11) C24 0.0334(11) 0.0296(12) 0.0359(12) 0.0116(10) 0.0117(10) 0.0061(10) C25 0.0212(9) 0.0297(12) 0.0238(10) 0.0080(8) 0.0051(8) 0.0021(8) N1 0.0274(9) 0.0188(10) 0.0343(10) 0.0029(8) 0.0075(7) 0.0013(7) C26 0.0327(11) 0.0224(12) 0.0278(11) -0.0009(9) 0.0044(9) 0.0001(9) C27 0.0752(19) 0.0116(11) 0.0636(19) 0.0026(12) -0.0005(15) -0.0025(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 Cu1 N1 2.1914(18) . ? Cu1 Cl2 2.2596(5) . ? Cu1 Cl1 2.2655(5) . ? Cu1 S1 2.3545(5) . ? Cu1 S2 2.3630(5) 1_455 ? S1 C11 1.8163(19) . ? S1 C10 1.8305(19) . ? S2 C19 1.827(2) . ? S2 C18 1.828(2) . ? S2 Cu1 2.3629(5) 1_655 ? O1 C25 1.360(2) . ? O1 C1 1.431(3) . ? O2 C4 1.364(2) . ? O2 C3 1.424(2) . ? C1 C2 1.507(3) . ? C2 C3 1.510(3) . ? C4 C5 1.385(3) . ? C4 C9 1.400(3) . ? C5 C6 1.398(3) . ? C6 C7 1.381(3) . ? C7 C8 1.384(3) . ? C8 C9 1.385(3) . ? C9 C10 1.497(3) . ? C11 C12 1.507(2) . ? C12 C17 1.387(3) . ? C12 C13 1.393(3) . ? C13 C14 1.391(3) . ? C14 C15 1.385(3) . ? C15 C16 1.388(3) . ? C15 C18 1.505(2) . ? C16 C17 1.391(3) . ? C19 C20 1.501(3) . ? C20 C21 1.388(3) . ? C20 C25 1.399(3) . ? C21 C22 1.380(3) . ? C22 C23 1.379(3) . ? C23 C24 1.389(3) . ? C24 C25 1.389(3) . ? N1 C26 1.133(3) . ? C26 C27 1.459(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 N1 Cu1 Cl2 111.64(5) . . ? N1 Cu1 Cl1 111.73(5) . . ? Cl2 Cu1 Cl1 136.62(2) . . ? N1 Cu1 S1 84.29(4) . . ? Cl2 Cu1 S1 88.355(19) . . ? Cl1 Cu1 S1 96.678(18) . . ? N1 Cu1 S2 85.37(4) . 1_455 ? Cl2 Cu1 S2 95.633(19) . 1_455 ? Cl1 Cu1 S2 86.985(18) . 1_455 ? S1 Cu1 S2 169.66(2) . 1_455 ? C11 S1 C10 99.09(9) . . ? C11 S1 Cu1 105.80(6) . . ? C10 S1 Cu1 110.55(7) . . ? C19 S2 C18 99.96(9) . . ? C19 S2 Cu1 110.27(7) . 1_655 ? C18 S2 Cu1 106.01(6) . 1_655 ? C25 O1 C1 119.05(17) . . ? C4 O2 C3 119.34(17) . . ? O1 C1 C2 105.35(17) . . ? C1 C2 C3 112.75(18) . . ? O2 C3 C2 105.52(17) . . ? O2 C4 C5 124.64(19) . . ? O2 C4 C9 114.50(18) . . ? C5 C4 C9 120.86(19) . . ? C4 C5 C6 118.9(2) . . ? C7 C6 C5 120.8(2) . . ? C6 C7 C8 119.4(2) . . ? C7 C8 C9 121.2(2) . . ? C8 C9 C4 118.8(2) . . ? C8 C9 C10 121.77(19) . . ? C4 C9 C10 119.45(18) . . ? C9 C10 S1 112.22(13) . . ? C12 C11 S1 111.90(13) . . ? C17 C12 C13 118.44(17) . . ? C17 C12 C11 121.67(17) . . ? C13 C12 C11 119.84(17) . . ? C14 C13 C12 121.02(18) . . ? C15 C14 C13 120.48(18) . . ? C14 C15 C16 118.46(17) . . ? C14 C15 C18 121.18(17) . . ? C16 C15 C18 120.34(17) . . ? C15 C16 C17 121.23(17) . . ? C12 C17 C16 120.36(18) . . ? C15 C18 S2 110.70(13) . . ? C20 C19 S2 110.99(14) . . ? C21 C20 C25 118.84(19) . . ? C21 C20 C19 121.59(19) . . ? C25 C20 C19 119.57(18) . . ? C22 C21 C20 121.1(2) . . ? C23 C22 C21 119.3(2) . . ? C22 C23 C24 121.2(2) . . ? C25 C24 C23 119.0(2) . . ? O1 C25 C24 124.9(2) . . ? O1 C25 C20 114.56(18) . . ? C24 C25 C20 120.56(19) . . ? C26 N1 Cu1 175.58(17) . . ? N1 C26 C27 179.7(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.107 _refine_diff_density_min -0.778 _refine_diff_density_rms 0.099 ############################################################ data_2 _database_code_depnum_ccdc_archive 'CCDC 863929' #TrackingRef '9181_web_deposit_cif_file_0_In-HyeokPark_1327158897.CuX.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H52 Br2 Cu2 O4 S4, 4(C H2 Cl2)' _chemical_formula_sum 'C54 H60 Br2 Cl8 Cu2 O4 S4' _chemical_formula_weight 1471.76 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.2153(3) _cell_length_b 11.6948(3) _cell_length_c 12.9855(4) _cell_angle_alpha 85.0890(10) _cell_angle_beta 65.1570(10) _cell_angle_gamma 79.3950(10) _cell_volume 1519.11(7) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9971 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.90 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.609 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 744 _exptl_absorpt_coefficient_mu 2.548 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2076 _exptl_absorpt_correction_T_max 0.9050 _exptl_absorpt_process_details ? _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 24176 _diffrn_reflns_av_R_equivalents 0.0413 _diffrn_reflns_av_sigmaI/netI 0.0309 _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 -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5962 _reflns_number_gt 5511 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0387P)^2^+1.9664P] 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 5962 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0348 _refine_ls_R_factor_gt 0.0321 _refine_ls_wR_factor_ref 0.0885 _refine_ls_wR_factor_gt 0.0864 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _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 Cu1 Cu -0.05607(3) 0.51559(3) 0.41533(3) 0.02371(9) Uani 1 1 d . . . Br1 Br 0.18786(2) 0.49933(2) 0.37779(2) 0.02516(8) Uani 1 1 d . . . O1 O -0.37695(18) -0.08584(16) 0.32468(17) 0.0308(4) Uani 1 1 d . . . O2 O -0.21959(18) 0.22478(15) 0.18873(15) 0.0279(4) Uani 1 1 d . . . S1 S -0.06071(6) 0.36146(5) 0.32296(5) 0.02136(13) Uani 1 1 d . . . S2 S -0.10995(6) -0.29534(5) 0.36623(5) 0.02131(13) Uani 1 1 d . . . C1 C -0.4566(3) 0.0124(3) 0.2986(3) 0.0448(8) Uani 1 1 d . . . H1A H -0.5493 0.0214 0.3573 0.054 Uiso 1 1 calc R . . H1B H -0.4578 0.0018 0.2242 0.054 Uiso 1 1 calc R . . C2 C -0.3960(3) 0.1191(3) 0.2951(3) 0.0398(7) Uani 1 1 d . . . H2A H -0.4611 0.1900 0.2983 0.048 Uiso 1 1 calc R . . H2B H -0.3751 0.1185 0.3620 0.048 Uiso 1 1 calc R . . C3 C -0.2709(3) 0.1215(2) 0.1884(3) 0.0339(6) Uani 1 1 d . . . H3A H -0.2043 0.0518 0.1856 0.041 Uiso 1 1 calc R . . H3B H -0.2908 0.1213 0.1210 0.041 Uiso 1 1 calc R . . C4 C -0.1029(3) 0.2414(2) 0.0994(2) 0.0255(5) Uani 1 1 d . . . C5 C -0.0386(3) 0.1699(2) 0.0048(2) 0.0343(6) Uani 1 1 d . . . H5A H -0.0746 0.1043 -0.0004 0.041 Uiso 1 1 calc R . . C6 C 0.0788(3) 0.1952(3) -0.0821(2) 0.0403(7) Uani 1 1 d . . . H6A H 0.1224 0.1468 -0.1470 0.048 Uiso 1 1 calc R . . C7 C 0.1327(3) 0.2893(3) -0.0756(2) 0.0390(7) Uani 1 1 d . . . H7A H 0.2129 0.3061 -0.1353 0.047 Uiso 1 1 calc R . . C8 C 0.0686(3) 0.3594(2) 0.0193(2) 0.0316(6) Uani 1 1 d . . . H8A H 0.1060 0.4242 0.0242 0.038 Uiso 1 1 calc R . . C9 C -0.0493(3) 0.3369(2) 0.1076(2) 0.0244(5) Uani 1 1 d . . . C10 C -0.1146(3) 0.4146(2) 0.2095(2) 0.0250(5) Uani 1 1 d . . . H10A H -0.2124 0.4200 0.2392 0.030 Uiso 1 1 calc R . . H10B H -0.0930 0.4938 0.1861 0.030 Uiso 1 1 calc R . . C11 C -0.1918(2) 0.2815(2) 0.4169(2) 0.0226(5) Uani 1 1 d . . . H11A H -0.2275 0.3125 0.4946 0.027 Uiso 1 1 calc R . . H11B H -0.2653 0.2955 0.3917 0.027 Uiso 1 1 calc R . . C12 C -0.1464(2) 0.1519(2) 0.4205(2) 0.0201(5) Uani 1 1 d . . . C13 C -0.0568(3) 0.0885(2) 0.3241(2) 0.0233(5) Uani 1 1 d . . . H13A H -0.0186 0.1278 0.2537 0.028 Uiso 1 1 calc R . . C14 C -0.1972(2) 0.0923(2) 0.5226(2) 0.0238(5) Uani 1 1 d . . . H14A H -0.2563 0.1342 0.5894 0.029 Uiso 1 1 calc R . . C15 C -0.0233(3) -0.0306(2) 0.3304(2) 0.0246(5) Uani 1 1 d . . . H15A H 0.0366 -0.0726 0.2638 0.030 Uiso 1 1 calc R . . C16 C -0.1632(3) -0.0275(2) 0.5289(2) 0.0244(5) Uani 1 1 d . . . H16A H -0.1998 -0.0667 0.5996 0.029 Uiso 1 1 calc R . . C17 C -0.0762(2) -0.0903(2) 0.4330(2) 0.0230(5) Uani 1 1 d . . . C18 C -0.0396(3) -0.2202(2) 0.4396(2) 0.0269(5) Uani 1 1 d . . . H18A H -0.0727 -0.2452 0.5203 0.032 Uiso 1 1 calc R . . H18B H 0.0586 -0.2420 0.4052 0.032 Uiso 1 1 calc R . . C19 C -0.2870(2) -0.2504(2) 0.4538(2) 0.0257(5) Uani 1 1 d . . . H19A H -0.3124 -0.2917 0.5278 0.031 Uiso 1 1 calc R . . H19B H -0.3055 -0.1658 0.4680 0.031 Uiso 1 1 calc R . . C20 C -0.3672(2) -0.2781(2) 0.3941(2) 0.0241(5) Uani 1 1 d . . . C21 C -0.3963(3) -0.3895(2) 0.3998(2) 0.0297(6) Uani 1 1 d . . . H21A H -0.3660 -0.4478 0.4429 0.036 Uiso 1 1 calc R . . C22 C -0.4688(3) -0.4173(3) 0.3439(3) 0.0341(6) Uani 1 1 d . . . H22A H -0.4874 -0.4940 0.3483 0.041 Uiso 1 1 calc R . . C23 C -0.5134(3) -0.3325(3) 0.2819(2) 0.0332(6) Uani 1 1 d . . . H23A H -0.5636 -0.3510 0.2440 0.040 Uiso 1 1 calc R . . C24 C -0.4857(3) -0.2205(3) 0.2745(2) 0.0307(6) Uani 1 1 d . . . H24A H -0.5169 -0.1626 0.2316 0.037 Uiso 1 1 calc R . . C25 C -0.4122(2) -0.1932(2) 0.3300(2) 0.0250(5) Uani 1 1 d . . . C26 C 0.2487(5) 0.6023(4) 0.0854(3) 0.0686(12) Uani 1 1 d . . . H26A H 0.1547 0.6153 0.0953 0.082 Uiso 1 1 calc R . . H26B H 0.2565 0.5472 0.1454 0.082 Uiso 1 1 calc R . . Cl1 Cl 0.35087(11) 0.53982(12) -0.04812(9) 0.0725(3) Uani 1 1 d . . . Cl2 Cl 0.29003(14) 0.73526(10) 0.10251(12) 0.0777(3) Uani 1 1 d . . . C27 C 0.6457(9) 0.8260(6) 0.9283(6) 0.127(3) Uani 1 1 d . . . H27A H 0.6987 0.7831 0.9683 0.153 Uiso 1 1 calc R . . H27B H 0.5506 0.8320 0.9810 0.153 Uiso 1 1 calc R . . Cl3 Cl 0.67236(18) 0.75031(16) 0.81805(14) 0.1070(5) Uani 1 1 d . . . Cl4 Cl 0.68606(16) 0.96928(16) 0.89601(19) 0.1251(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 Cu1 0.03109(17) 0.01606(16) 0.02699(17) -0.00024(11) -0.01416(13) -0.00570(12) Br1 0.02470(14) 0.02771(14) 0.02364(14) 0.00198(10) -0.01004(10) -0.00650(10) O1 0.0291(10) 0.0244(9) 0.0453(11) 0.0057(8) -0.0211(9) -0.0081(8) O2 0.0338(10) 0.0211(9) 0.0309(9) -0.0002(7) -0.0143(8) -0.0071(7) S1 0.0272(3) 0.0149(3) 0.0237(3) -0.0002(2) -0.0115(2) -0.0051(2) S2 0.0255(3) 0.0165(3) 0.0260(3) 0.0012(2) -0.0142(2) -0.0047(2) C1 0.0305(15) 0.0282(15) 0.082(2) 0.0098(15) -0.0304(16) -0.0069(12) C2 0.0311(15) 0.0253(14) 0.063(2) 0.0050(13) -0.0203(14) -0.0056(11) C3 0.0442(16) 0.0251(14) 0.0414(16) 0.0024(11) -0.0245(13) -0.0117(12) C4 0.0336(13) 0.0223(12) 0.0224(12) 0.0025(9) -0.0148(11) -0.0018(10) C5 0.0545(18) 0.0231(14) 0.0299(14) -0.0015(11) -0.0235(13) -0.0019(12) C6 0.0567(19) 0.0315(15) 0.0226(13) -0.0046(11) -0.0126(13) 0.0093(14) C7 0.0409(16) 0.0366(16) 0.0266(14) 0.0039(12) -0.0054(12) 0.0017(13) C8 0.0343(14) 0.0292(14) 0.0287(13) 0.0033(11) -0.0118(12) -0.0039(11) C9 0.0316(13) 0.0198(12) 0.0217(12) 0.0009(9) -0.0127(10) -0.0003(10) C10 0.0356(14) 0.0163(11) 0.0235(12) 0.0013(9) -0.0135(11) -0.0029(10) C11 0.0242(12) 0.0167(11) 0.0242(12) -0.0002(9) -0.0075(10) -0.0031(9) C12 0.0232(11) 0.0146(11) 0.0271(12) 0.0000(9) -0.0140(10) -0.0052(9) C13 0.0294(13) 0.0197(12) 0.0218(12) 0.0011(9) -0.0118(10) -0.0042(10) C14 0.0245(12) 0.0233(12) 0.0235(12) -0.0004(10) -0.0090(10) -0.0062(10) C15 0.0291(13) 0.0192(12) 0.0275(13) -0.0031(10) -0.0137(11) -0.0024(10) C16 0.0273(12) 0.0217(12) 0.0274(12) 0.0052(10) -0.0135(10) -0.0092(10) C17 0.0272(12) 0.0148(11) 0.0353(13) 0.0023(10) -0.0210(11) -0.0050(9) C18 0.0367(14) 0.0160(12) 0.0395(14) 0.0023(10) -0.0265(12) -0.0062(10) C19 0.0256(12) 0.0250(13) 0.0270(13) -0.0032(10) -0.0118(10) -0.0018(10) C20 0.0187(11) 0.0260(13) 0.0249(12) -0.0043(10) -0.0058(10) -0.0034(10) C21 0.0258(13) 0.0267(13) 0.0335(14) -0.0018(11) -0.0087(11) -0.0049(10) C22 0.0275(13) 0.0300(14) 0.0436(16) -0.0080(12) -0.0097(12) -0.0108(11) C23 0.0227(13) 0.0417(16) 0.0383(15) -0.0105(12) -0.0126(11) -0.0076(11) C24 0.0231(12) 0.0368(15) 0.0335(14) -0.0015(11) -0.0128(11) -0.0046(11) C25 0.0170(11) 0.0269(13) 0.0290(13) -0.0024(10) -0.0062(10) -0.0058(10) C26 0.100(3) 0.068(3) 0.045(2) 0.0103(19) -0.031(2) -0.032(3) Cl1 0.0641(6) 0.0963(9) 0.0579(6) -0.0021(5) -0.0297(5) -0.0030(6) Cl2 0.1020(9) 0.0653(7) 0.0993(9) 0.0116(6) -0.0738(8) -0.0199(6) C27 0.173(7) 0.110(5) 0.095(4) -0.002(4) -0.069(5) 0.021(5) Cl3 0.1128(12) 0.1171(13) 0.0926(10) -0.0127(9) -0.0379(9) -0.0282(10) Cl4 0.0841(10) 0.0884(11) 0.1692(17) -0.0296(11) -0.0121(11) -0.0204(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 Cu1 S1 2.2689(6) . ? Cu1 S2 2.2915(6) 1_565 ? Cu1 Br1 2.4719(4) 2_566 ? Cu1 Br1 2.5421(4) . ? Cu1 Cu1 2.9271(6) 2_566 ? Br1 Cu1 2.4719(4) 2_566 ? O1 C25 1.372(3) . ? O1 C1 1.429(3) . ? O2 C4 1.370(3) . ? O2 C3 1.432(3) . ? S1 C11 1.824(2) . ? S1 C10 1.838(3) . ? S2 C19 1.826(3) . ? S2 C18 1.826(2) . ? S2 Cu1 2.2915(6) 1_545 ? C1 C2 1.515(4) . ? C2 C3 1.504(4) . ? C4 C5 1.392(4) . ? C4 C9 1.394(4) . ? C5 C6 1.390(4) . ? C6 C7 1.373(5) . ? C7 C8 1.385(4) . ? C8 C9 1.390(4) . ? C9 C10 1.503(3) . ? C11 C12 1.512(3) . ? C12 C14 1.386(3) . ? C12 C13 1.398(3) . ? C13 C15 1.379(4) . ? C14 C16 1.388(4) . ? C15 C17 1.394(4) . ? C16 C17 1.383(4) . ? C17 C18 1.505(3) . ? C19 C20 1.500(3) . ? C20 C21 1.388(4) . ? C20 C25 1.400(4) . ? C21 C22 1.388(4) . ? C22 C23 1.378(4) . ? C23 C24 1.387(4) . ? C24 C25 1.393(4) . ? C26 Cl2 1.759(4) . ? C26 Cl1 1.759(4) . ? C27 Cl3 1.638(7) . ? C27 Cl4 1.785(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 Cu1 S2 122.85(2) . 1_565 ? S1 Cu1 Br1 111.43(2) . 2_566 ? S2 Cu1 Br1 105.94(2) 1_565 2_566 ? S1 Cu1 Br1 103.99(2) . . ? S2 Cu1 Br1 103.094(19) 1_565 . ? Br1 Cu1 Br1 108.577(13) 2_566 . ? S1 Cu1 Cu1 121.23(2) . 2_566 ? S2 Cu1 Cu1 115.38(2) 1_565 2_566 ? Br1 Cu1 Cu1 55.404(11) 2_566 2_566 ? Br1 Cu1 Cu1 53.174(11) . 2_566 ? Cu1 Br1 Cu1 71.421(13) 2_566 . ? C25 O1 C1 117.9(2) . . ? C4 O2 C3 117.2(2) . . ? C11 S1 C10 103.29(12) . . ? C11 S1 Cu1 110.03(8) . . ? C10 S1 Cu1 109.22(8) . . ? C19 S2 C18 99.63(12) . . ? C19 S2 Cu1 106.66(9) . 1_545 ? C18 S2 Cu1 100.46(8) . 1_545 ? O1 C1 C2 107.8(2) . . ? C3 C2 C1 110.7(3) . . ? O2 C3 C2 108.3(2) . . ? O2 C4 C5 124.0(2) . . ? O2 C4 C9 115.7(2) . . ? C5 C4 C9 120.3(3) . . ? C6 C5 C4 119.5(3) . . ? C7 C6 C5 120.9(3) . . ? C6 C7 C8 119.2(3) . . ? C7 C8 C9 121.5(3) . . ? C8 C9 C4 118.6(2) . . ? C8 C9 C10 119.6(2) . . ? C4 C9 C10 121.7(2) . . ? C9 C10 S1 112.42(17) . . ? C12 C11 S1 113.95(17) . . ? C14 C12 C13 118.3(2) . . ? C14 C12 C11 119.1(2) . . ? C13 C12 C11 122.6(2) . . ? C15 C13 C12 120.6(2) . . ? C12 C14 C16 121.1(2) . . ? C13 C15 C17 120.9(2) . . ? C17 C16 C14 120.5(2) . . ? C16 C17 C15 118.6(2) . . ? C16 C17 C18 120.5(2) . . ? C15 C17 C18 120.8(2) . . ? C17 C18 S2 111.48(17) . . ? C20 C19 S2 109.54(17) . . ? C21 C20 C25 118.7(2) . . ? C21 C20 C19 120.4(2) . . ? C25 C20 C19 120.9(2) . . ? C20 C21 C22 121.3(3) . . ? C23 C22 C21 119.4(3) . . ? C22 C23 C24 120.6(3) . . ? C23 C24 C25 119.8(3) . . ? O1 C25 C24 123.8(2) . . ? O1 C25 C20 116.0(2) . . ? C24 C25 C20 120.2(2) . . ? Cl2 C26 Cl1 112.8(2) . . ? Cl3 C27 Cl4 114.9(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.051 _refine_diff_density_min -1.069 _refine_diff_density_rms 0.074 ############################################################ data_3a _database_code_depnum_ccdc_archive 'CCDC 863930' #TrackingRef '9181_web_deposit_cif_file_0_In-HyeokPark_1327158897.CuX.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H52 Cu4 I4 O4 S4, C H2 Cl2' _chemical_formula_sum 'C51 H54 Cl2 Cu4 I4 O4 S4' _chemical_formula_weight 1691.84 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 36.215(4) _cell_length_b 13.9659(14) _cell_length_c 28.036(5) _cell_angle_alpha 90.00 _cell_angle_beta 125.048(4) _cell_angle_gamma 90.00 _cell_volume 11609(3) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9138 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 27.58 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.936 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6544 _exptl_absorpt_coefficient_mu 3.850 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2491 _exptl_absorpt_correction_T_max 0.4584 _exptl_absorpt_process_details ? _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 51195 _diffrn_reflns_av_R_equivalents 0.0587 _diffrn_reflns_av_sigmaI/netI 0.0484 _diffrn_reflns_limit_h_min -46 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 27.00 _reflns_number_total 12638 _reflns_number_gt 11205 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0481P)^2^+25.7320P] 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 12638 _refine_ls_number_parameters 622 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0414 _refine_ls_R_factor_gt 0.0363 _refine_ls_wR_factor_ref 0.0993 _refine_ls_wR_factor_gt 0.0956 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _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 Cu1 Cu 0.100001(16) 0.30712(3) 0.47908(2) 0.02781(11) Uani 1 1 d . . . Cu2 Cu 0.090180(17) 0.50104(3) 0.47625(2) 0.03135(12) Uani 1 1 d . . . Cu3 Cu 0.156027(17) 0.42372(3) 0.47042(2) 0.02977(11) Uani 1 1 d . . . Cu4 Cu 0.160671(17) 0.41856(3) 0.57287(2) 0.03094(12) Uani 1 1 d . . . I1 I 0.076434(9) 0.395645(16) 0.541750(12) 0.02925(7) Uani 1 1 d . . . I2 I 0.070139(8) 0.398029(16) 0.379479(11) 0.02662(7) Uani 1 1 d . . . I3 I 0.171120(9) 0.583518(16) 0.531167(11) 0.02834(7) Uani 1 1 d . . . I4 I 0.190255(8) 0.275657(17) 0.543008(11) 0.03058(7) Uani 1 1 d . . . S1 S 0.07079(3) 1.15468(6) 0.45759(4) 0.0263(2) Uani 1 1 d . . . S2 S 0.04232(3) 0.62989(6) 0.43573(4) 0.0268(2) Uani 1 1 d . . . S3 S 0.18886(3) 0.45038(7) 0.42237(4) 0.0287(2) Uani 1 1 d . . . S4 S 0.20050(3) 0.55302(7) 0.17217(4) 0.0306(2) Uani 1 1 d . . . O1 O -0.04640(11) 0.75650(19) 0.36609(13) 0.0367(7) Uani 1 1 d . . . O2 O -0.03113(10) 1.04358(18) 0.42137(14) 0.0335(6) Uani 1 1 d . . . O3 O 0.28379(11) 0.5537(2) 0.30928(13) 0.0388(7) Uani 1 1 d . . . O4 O 0.26315(12) 0.5988(2) 0.43844(16) 0.0486(9) Uani 1 1 d . . . C1 C -0.05660(14) 0.8553(3) 0.36553(19) 0.0337(9) Uani 1 1 d . . . H1A H -0.0893 0.8670 0.3369 0.040 Uiso 1 1 calc R . . H1B H -0.0397 0.8954 0.3552 0.040 Uiso 1 1 calc R . . C2 C -0.04278(16) 0.8780(3) 0.4259(2) 0.0357(10) Uani 1 1 d . . . H2A H -0.0096 0.8713 0.4533 0.043 Uiso 1 1 calc R . . H2B H -0.0569 0.8312 0.4374 0.043 Uiso 1 1 calc R . . C3 C -0.05630(16) 0.9781(3) 0.4306(2) 0.0376(10) Uani 1 1 d . . . H3A H -0.0890 0.9878 0.4010 0.045 Uiso 1 1 calc R . . H3B H -0.0499 0.9881 0.4697 0.045 Uiso 1 1 calc R . . C4 C -0.04152(13) 1.1385(3) 0.41700(18) 0.0299(9) Uani 1 1 d . . . C5 C -0.07312(14) 1.1759(3) 0.4253(2) 0.0359(9) Uani 1 1 d . . . H5A H -0.0890 1.1348 0.4346 0.043 Uiso 1 1 calc R . . C6 C -0.08112(15) 1.2727(3) 0.4198(2) 0.0407(11) Uani 1 1 d . . . H6A H -0.1023 1.2980 0.4262 0.049 Uiso 1 1 calc R . . C7 C -0.05931(15) 1.3339(3) 0.4052(2) 0.0457(12) Uani 1 1 d . . . H7A H -0.0655 1.4007 0.4011 0.055 Uiso 1 1 calc R . . C8 C -0.02848(15) 1.2965(3) 0.3968(2) 0.0400(11) Uani 1 1 d . . . H8A H -0.0130 1.3383 0.3871 0.048 Uiso 1 1 calc R . . C9 C -0.01919(13) 1.1992(3) 0.40196(19) 0.0295(8) Uani 1 1 d . . . C10 C 0.01366(13) 1.1594(3) 0.39090(19) 0.0309(9) Uani 1 1 d . . . H10A H 0.0135 1.1999 0.3618 0.037 Uiso 1 1 calc R . . H10B H 0.0041 1.0941 0.3745 0.037 Uiso 1 1 calc R . . C11 C 0.09773(14) 1.0930(2) 0.4277(2) 0.0306(9) Uani 1 1 d . . . H11A H 0.0884 1.1234 0.3905 0.037 Uiso 1 1 calc R . . H11B H 0.1309 1.0993 0.4551 0.037 Uiso 1 1 calc R . . C12 C 0.08526(13) 0.9886(3) 0.41750(18) 0.0278(8) Uani 1 1 d . . . C13 C 0.05632(15) 0.9512(3) 0.36189(19) 0.0339(9) Uani 1 1 d . . . H13A H 0.0430 0.9928 0.3292 0.041 Uiso 1 1 calc R . . C14 C 0.10346(15) 0.9273(3) 0.4644(2) 0.0371(10) Uani 1 1 d . . . H14A H 0.1229 0.9518 0.5028 0.045 Uiso 1 1 calc R . . C15 C 0.04655(14) 0.8540(3) 0.35338(17) 0.0316(9) Uani 1 1 d . . . H15A H 0.0267 0.8296 0.3150 0.038 Uiso 1 1 calc R . . C16 C 0.09373(14) 0.8302(3) 0.45611(18) 0.0353(10) Uani 1 1 d . . . H16A H 0.1065 0.7891 0.4890 0.042 Uiso 1 1 calc R . . C17 C 0.06582(12) 0.7922(2) 0.40088(17) 0.0236(7) Uani 1 1 d . . . C18 C 0.05878(13) 0.6858(2) 0.39173(17) 0.0257(8) Uani 1 1 d . . . H18A H 0.0871 0.6558 0.4013 0.031 Uiso 1 1 calc R . . H18B H 0.0351 0.6732 0.3501 0.031 Uiso 1 1 calc R . . C19 C -0.01317(13) 0.5760(3) 0.38213(19) 0.0306(9) Uani 1 1 d . . . H19A H -0.0087 0.5077 0.3773 0.037 Uiso 1 1 calc R . . H19B H -0.0315 0.5785 0.3980 0.037 Uiso 1 1 calc R . . C20 C -0.03904(13) 0.6224(3) 0.32374(19) 0.0304(9) Uani 1 1 d . . . C21 C -0.04647(14) 0.5748(3) 0.2753(2) 0.0363(10) Uani 1 1 d . . . H21A H -0.0354 0.5114 0.2796 0.044 Uiso 1 1 calc R . . C22 C -0.06949(16) 0.6176(4) 0.2215(2) 0.0450(11) Uani 1 1 d . . . H22A H -0.0749 0.5834 0.1887 0.054 Uiso 1 1 calc R . . C23 C -0.08460(15) 0.7099(4) 0.2151(2) 0.0454(11) Uani 1 1 d . . . H23A H -0.0998 0.7398 0.1780 0.054 Uiso 1 1 calc R . . C24 C -0.07796(15) 0.7606(3) 0.2626(2) 0.0396(10) Uani 1 1 d . . . H24A H -0.0887 0.8244 0.2579 0.048 Uiso 1 1 calc R . . C25 C -0.05553(13) 0.7163(3) 0.31617(19) 0.0317(9) Uani 1 1 d . . . C26 C 0.29013(17) 0.5666(3) 0.3638(2) 0.0450(11) Uani 1 1 d . . . H26A H 0.3226 0.5746 0.3951 0.054 Uiso 1 1 calc R . . H26B H 0.2790 0.5098 0.3731 0.054 Uiso 1 1 calc R . . C27 C 0.26476(17) 0.6534(3) 0.3601(2) 0.0471(12) Uani 1 1 d . . . H27A H 0.2320 0.6415 0.3325 0.056 Uiso 1 1 calc R . . H27B H 0.2728 0.7076 0.3450 0.056 Uiso 1 1 calc R . . C28 C 0.27513(18) 0.6795(3) 0.4189(3) 0.0522(13) Uani 1 1 d . . . H28A H 0.3076 0.6943 0.4467 0.063 Uiso 1 1 calc R . . H28B H 0.2575 0.7364 0.4155 0.063 Uiso 1 1 calc R . . C29 C 0.27860(16) 0.5943(4) 0.4955(2) 0.0465(12) Uani 1 1 d . . . C30 C 0.29959(19) 0.6702(5) 0.5349(3) 0.0693(19) Uani 1 1 d . . . H30A H 0.3035 0.7304 0.5226 0.083 Uiso 1 1 calc R . . C31 C 0.3145(2) 0.6559(7) 0.5922(3) 0.084(3) Uani 1 1 d . . . H31A H 0.3279 0.7078 0.6188 0.101 Uiso 1 1 calc R . . C32 C 0.3107(2) 0.5716(7) 0.6111(3) 0.088(3) Uani 1 1 d . . . H32A H 0.3222 0.5631 0.6510 0.106 Uiso 1 1 calc R . . C33 C 0.28929(17) 0.4952(5) 0.5715(2) 0.0644(17) Uani 1 1 d . . . H33A H 0.2862 0.4352 0.5848 0.077 Uiso 1 1 calc R . . C34 C 0.27276(14) 0.5065(4) 0.5136(2) 0.0431(11) Uani 1 1 d . . . C35 C 0.24942(14) 0.4277(3) 0.4705(2) 0.0397(10) Uani 1 1 d . . . H35A H 0.2549 0.3664 0.4913 0.048 Uiso 1 1 calc R . . H35B H 0.2619 0.4221 0.4471 0.048 Uiso 1 1 calc R . . C36 C 0.17254(16) 0.3532(3) 0.37097(19) 0.0367(10) Uani 1 1 d . . . H36A H 0.1915 0.2966 0.3922 0.044 Uiso 1 1 calc R . . H36B H 0.1408 0.3358 0.3541 0.044 Uiso 1 1 calc R . . C37 C 0.17714(14) 0.3772(3) 0.32214(18) 0.0305(8) Uani 1 1 d . . . C38 C 0.15338(16) 0.4537(4) 0.2851(2) 0.0444(11) Uani 1 1 d . . . H38A H 0.1359 0.4934 0.2924 0.053 Uiso 1 1 calc R . . C39 C 0.20270(14) 0.3213(3) 0.31056(18) 0.0312(8) Uani 1 1 d . . . H39A H 0.2195 0.2690 0.3354 0.037 Uiso 1 1 calc R . . C40 C 0.15485(16) 0.4726(3) 0.2385(2) 0.0422(11) Uani 1 1 d . . . H40A H 0.1383 0.5254 0.2140 0.051 Uiso 1 1 calc R . . C41 C 0.20403(13) 0.3407(3) 0.26308(17) 0.0285(8) Uani 1 1 d . . . H41A H 0.2217 0.3013 0.2559 0.034 Uiso 1 1 calc R . . C42 C 0.17997(13) 0.4168(3) 0.22573(17) 0.0275(8) Uani 1 1 d . . . C43 C 0.17888(14) 0.4354(3) 0.17254(17) 0.0301(8) Uani 1 1 d . . . H43A H 0.1474 0.4296 0.1378 0.036 Uiso 1 1 calc R . . H43B H 0.1970 0.3857 0.1696 0.036 Uiso 1 1 calc R . . C44 C 0.25845(14) 0.5278(3) 0.19593(19) 0.0391(10) Uani 1 1 d . . . H44A H 0.2576 0.5067 0.1616 0.047 Uiso 1 1 calc R . . H44B H 0.2759 0.5882 0.2101 0.047 Uiso 1 1 calc R . . C45 C 0.28328(13) 0.4533(3) 0.24293(18) 0.0333(9) Uani 1 1 d . . . C46 C 0.29355(15) 0.3660(3) 0.2294(2) 0.0405(10) Uani 1 1 d . . . H46A H 0.2845 0.3544 0.1907 0.049 Uiso 1 1 calc R . . C47 C 0.31679(17) 0.2952(3) 0.2714(2) 0.0469(12) Uani 1 1 d . . . H47A H 0.3236 0.2359 0.2615 0.056 Uiso 1 1 calc R . . C48 C 0.32986(15) 0.3125(3) 0.3277(2) 0.0437(11) Uani 1 1 d . . . H48A H 0.3457 0.2645 0.3566 0.052 Uiso 1 1 calc R . . C49 C 0.32028(14) 0.3976(3) 0.3420(2) 0.0372(10) Uani 1 1 d . . . H49A H 0.3299 0.4089 0.3810 0.045 Uiso 1 1 calc R . . C50 C 0.29625(13) 0.4684(3) 0.29956(18) 0.0332(9) Uani 1 1 d . . . Cl1 Cl -0.11289(19) 1.0586(2) 0.26607(16) 0.241(3) Uani 1 1 d . . . Cl2 Cl -0.06813(14) 1.1989(5) 0.23438(16) 0.236(3) Uani 1 1 d . . . C51 C -0.1064(3) 1.1688(6) 0.2531(4) 0.105(3) Uani 1 1 d . . . H51B H -0.0973 1.2067 0.2881 0.126 Uiso 1 1 calc R . . H51A H -0.1365 1.1924 0.2211 0.126 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 0.0375(2) 0.0146(2) 0.0328(3) -0.00263(17) 0.0210(2) -0.00257(17) Cu2 0.0379(3) 0.0191(2) 0.0361(3) 0.00667(19) 0.0207(2) 0.00304(18) Cu3 0.0369(3) 0.0299(2) 0.0292(3) -0.00337(19) 0.0228(2) -0.00295(19) Cu4 0.0406(3) 0.0252(2) 0.0226(3) -0.00450(18) 0.0155(2) -0.00066(19) I1 0.04302(15) 0.02049(12) 0.03662(16) -0.00019(9) 0.03008(13) -0.00086(9) I2 0.03269(13) 0.02242(12) 0.02288(13) -0.00026(9) 0.01488(11) -0.00145(9) I3 0.03696(14) 0.01829(12) 0.02818(14) -0.00454(9) 0.01777(11) -0.00696(9) I4 0.03378(14) 0.02288(13) 0.03069(14) 0.00086(9) 0.01596(11) 0.00695(9) S1 0.0338(5) 0.0133(4) 0.0358(5) -0.0002(3) 0.0223(4) -0.0012(3) S2 0.0381(5) 0.0153(4) 0.0300(5) 0.0007(3) 0.0213(4) 0.0003(3) S3 0.0367(5) 0.0285(5) 0.0283(5) -0.0040(4) 0.0230(4) -0.0046(4) S4 0.0422(5) 0.0241(5) 0.0217(5) 0.0009(4) 0.0160(4) -0.0020(4) O1 0.0565(18) 0.0200(13) 0.0384(17) 0.0039(12) 0.0301(15) 0.0094(12) O2 0.0434(15) 0.0165(12) 0.0519(19) 0.0055(12) 0.0340(15) 0.0026(11) O3 0.0532(18) 0.0295(15) 0.0236(15) 0.0039(12) 0.0162(14) 0.0006(13) O4 0.062(2) 0.0438(19) 0.047(2) -0.0180(15) 0.0352(18) -0.0259(15) C1 0.044(2) 0.0199(18) 0.041(2) 0.0062(16) 0.026(2) 0.0044(16) C2 0.053(2) 0.0182(18) 0.043(3) 0.0029(17) 0.031(2) 0.0017(17) C3 0.053(3) 0.0214(19) 0.050(3) 0.0012(18) 0.037(2) -0.0025(17) C4 0.0348(19) 0.0173(17) 0.036(2) -0.0023(15) 0.0193(18) -0.0016(14) C5 0.042(2) 0.028(2) 0.044(3) -0.0014(18) 0.028(2) 0.0002(17) C6 0.043(2) 0.034(2) 0.050(3) 0.0020(19) 0.030(2) 0.0110(18) C7 0.046(2) 0.0172(19) 0.069(3) -0.004(2) 0.030(2) 0.0030(17) C8 0.042(2) 0.0193(18) 0.061(3) 0.0028(18) 0.031(2) -0.0004(16) C9 0.0315(19) 0.0176(17) 0.039(2) -0.0001(15) 0.0203(18) -0.0003(14) C10 0.0338(19) 0.0222(18) 0.038(2) -0.0033(16) 0.0211(18) -0.0031(15) C11 0.040(2) 0.0141(16) 0.049(3) -0.0061(16) 0.032(2) -0.0064(14) C12 0.0329(19) 0.0168(17) 0.041(2) -0.0011(15) 0.0251(18) 0.0002(14) C13 0.048(2) 0.0224(19) 0.031(2) 0.0066(16) 0.0224(19) 0.0026(17) C14 0.047(2) 0.0170(18) 0.036(2) -0.0046(16) 0.017(2) -0.0031(16) C15 0.041(2) 0.0229(18) 0.022(2) -0.0006(15) 0.0134(17) -0.0006(16) C16 0.044(2) 0.0198(18) 0.027(2) 0.0041(15) 0.0119(18) 0.0004(16) C17 0.0277(17) 0.0152(16) 0.031(2) 0.0015(14) 0.0184(16) 0.0002(13) C18 0.0358(19) 0.0174(16) 0.031(2) -0.0006(14) 0.0229(17) -0.0009(14) C19 0.035(2) 0.0191(17) 0.043(2) 0.0017(16) 0.0253(19) -0.0003(15) C20 0.0300(19) 0.0256(18) 0.036(2) -0.0026(16) 0.0191(17) -0.0048(15) C21 0.039(2) 0.032(2) 0.042(3) -0.0077(18) 0.026(2) -0.0087(17) C22 0.047(3) 0.053(3) 0.039(3) -0.013(2) 0.026(2) -0.009(2) C23 0.038(2) 0.060(3) 0.033(2) 0.005(2) 0.017(2) -0.001(2) C24 0.038(2) 0.038(2) 0.041(3) 0.0079(19) 0.021(2) 0.0054(18) C25 0.034(2) 0.0284(19) 0.035(2) 0.0011(16) 0.0209(18) 0.0005(15) C26 0.054(3) 0.043(3) 0.028(2) 0.0054(19) 0.018(2) 0.003(2) C27 0.052(3) 0.033(2) 0.050(3) 0.006(2) 0.026(2) -0.003(2) C28 0.053(3) 0.033(2) 0.075(4) -0.011(2) 0.039(3) -0.010(2) C29 0.038(2) 0.060(3) 0.045(3) -0.022(2) 0.026(2) -0.015(2) C30 0.054(3) 0.086(4) 0.078(4) -0.050(4) 0.044(3) -0.036(3) C31 0.050(3) 0.140(7) 0.069(5) -0.065(5) 0.039(3) -0.042(4) C32 0.041(3) 0.181(9) 0.040(3) -0.040(5) 0.021(3) -0.021(4) C33 0.037(3) 0.113(5) 0.041(3) 0.001(3) 0.020(2) 0.002(3) C34 0.026(2) 0.065(3) 0.036(2) -0.008(2) 0.0165(19) 0.0006(19) C35 0.037(2) 0.039(2) 0.052(3) 0.005(2) 0.030(2) 0.0062(18) C36 0.056(3) 0.034(2) 0.035(2) -0.0103(18) 0.036(2) -0.0127(19) C37 0.037(2) 0.031(2) 0.027(2) 0.0001(16) 0.0208(17) -0.0005(16) C38 0.053(3) 0.052(3) 0.038(3) 0.010(2) 0.032(2) 0.019(2) C39 0.040(2) 0.030(2) 0.025(2) 0.0053(16) 0.0197(17) 0.0029(16) C40 0.050(3) 0.045(3) 0.034(2) 0.013(2) 0.026(2) 0.018(2) C41 0.0358(19) 0.0306(19) 0.027(2) 0.0019(16) 0.0229(17) 0.0029(16) C42 0.0316(19) 0.0264(18) 0.0213(19) 0.0001(14) 0.0134(16) -0.0012(15) C43 0.044(2) 0.0259(18) 0.024(2) -0.0028(15) 0.0211(18) -0.0060(16) C44 0.040(2) 0.043(2) 0.027(2) 0.0093(18) 0.0155(19) -0.0046(19) C45 0.0291(19) 0.034(2) 0.029(2) 0.0052(17) 0.0119(17) -0.0074(16) C46 0.041(2) 0.044(2) 0.033(2) -0.0021(19) 0.020(2) -0.0046(19) C47 0.051(3) 0.038(2) 0.048(3) 0.001(2) 0.026(2) -0.001(2) C48 0.039(2) 0.037(2) 0.040(3) 0.010(2) 0.014(2) -0.0004(18) C49 0.034(2) 0.040(2) 0.026(2) 0.0070(17) 0.0103(18) -0.0030(17) C50 0.034(2) 0.031(2) 0.025(2) 0.0044(16) 0.0111(17) -0.0061(16) Cl1 0.342(6) 0.111(2) 0.108(2) 0.0064(18) 0.035(3) -0.078(3) Cl2 0.161(3) 0.416(8) 0.108(3) 0.099(4) 0.063(2) 0.042(4) C51 0.105(6) 0.099(6) 0.087(6) 0.030(5) 0.041(5) 0.019(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 Cu1 S1 2.2984(10) 1_545 ? Cu1 I1 2.6584(6) . ? Cu1 I2 2.6665(7) . ? Cu1 I4 2.7130(6) . ? Cu1 Cu3 2.7190(7) . ? Cu1 Cu2 2.7267(7) . ? Cu1 Cu4 2.7440(7) . ? Cu2 S2 2.2960(10) . ? Cu2 I1 2.6146(6) . ? Cu2 I3 2.6658(6) . ? Cu2 Cu4 2.6906(8) . ? Cu2 Cu3 2.7068(8) . ? Cu2 I2 2.7741(7) . ? Cu3 S3 2.2820(11) . ? Cu3 I4 2.6564(6) . ? Cu3 I3 2.6665(6) . ? Cu3 I2 2.6826(6) . ? Cu3 Cu4 2.7800(9) . ? Cu4 S4 2.3188(12) 6_566 ? Cu4 I4 2.6196(6) . ? Cu4 I1 2.6671(7) . ? Cu4 I3 2.7066(6) . ? S1 C11 1.826(4) . ? S1 C10 1.827(4) . ? S1 Cu1 2.2983(10) 1_565 ? S2 C18 1.825(4) . ? S2 C19 1.843(4) . ? S3 C36 1.814(4) . ? S3 C35 1.826(4) . ? S4 C43 1.823(4) . ? S4 C44 1.835(5) . ? S4 Cu4 2.3186(12) 6_565 ? O1 C25 1.361(5) . ? O1 C1 1.426(4) . ? O2 C4 1.365(4) . ? O2 C3 1.416(5) . ? O3 C50 1.355(5) . ? O3 C26 1.422(6) . ? O4 C29 1.360(7) . ? O4 C28 1.426(6) . ? C1 C2 1.498(6) . ? C2 C3 1.513(6) . ? C4 C5 1.393(6) . ? C4 C9 1.394(6) . ? C5 C6 1.371(6) . ? C6 C7 1.376(7) . ? C7 C8 1.371(7) . ? C8 C9 1.387(5) . ? C9 C10 1.498(6) . ? C11 C12 1.505(5) . ? C12 C14 1.379(6) . ? C12 C13 1.387(6) . ? C13 C15 1.388(6) . ? C14 C16 1.387(5) . ? C15 C17 1.392(5) . ? C16 C17 1.379(5) . ? C17 C18 1.505(5) . ? C19 C20 1.489(6) . ? C20 C21 1.392(6) . ? C20 C25 1.406(5) . ? C21 C22 1.374(7) . ? C22 C23 1.371(7) . ? C23 C24 1.403(7) . ? C24 C25 1.378(6) . ? C26 C27 1.488(7) . ? C27 C28 1.509(8) . ? C29 C34 1.388(7) . ? C29 C30 1.400(7) . ? C30 C31 1.383(10) . ? C31 C32 1.330(12) . ? C32 C33 1.408(10) . ? C33 C34 1.380(7) . ? C34 C35 1.487(7) . ? C36 C37 1.509(6) . ? C37 C39 1.385(6) . ? C37 C38 1.391(6) . ? C38 C40 1.366(7) . ? C39 C41 1.386(6) . ? C40 C42 1.391(6) . ? C41 C42 1.391(5) . ? C42 C43 1.492(6) . ? C44 C45 1.505(6) . ? C45 C50 1.389(6) . ? C45 C46 1.389(7) . ? C46 C47 1.390(7) . ? C47 C48 1.384(7) . ? C48 C49 1.362(7) . ? C49 C50 1.401(6) . ? Cl1 C51 1.630(9) . ? Cl2 C51 1.790(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 Cu1 I1 109.26(3) 1_545 . ? S1 Cu1 I2 108.53(3) 1_545 . ? I1 Cu1 I2 112.31(2) . . ? S1 Cu1 I4 102.81(3) 1_545 . ? I1 Cu1 I4 111.16(2) . . ? I2 Cu1 I4 112.28(2) . . ? S1 Cu1 Cu3 141.83(3) 1_545 . ? I1 Cu1 Cu3 108.64(2) . . ? I2 Cu1 Cu3 59.741(17) . . ? I4 Cu1 Cu3 58.553(17) . . ? S1 Cu1 Cu2 151.60(3) 1_545 . ? I1 Cu1 Cu2 58.077(16) . . ? I2 Cu1 Cu2 61.899(16) . . ? I4 Cu1 Cu2 105.522(19) . . ? Cu3 Cu1 Cu2 59.611(18) . . ? S1 Cu1 Cu4 140.47(3) 1_545 . ? I1 Cu1 Cu4 59.141(19) . . ? I2 Cu1 Cu4 110.70(2) . . ? I4 Cu1 Cu4 57.374(16) . . ? Cu3 Cu1 Cu4 61.18(2) . . ? Cu2 Cu1 Cu4 58.919(18) . . ? S2 Cu2 I1 113.25(3) . . ? S2 Cu2 I3 102.37(3) . . ? I1 Cu2 I3 115.30(2) . . ? S2 Cu2 Cu4 147.55(4) . . ? I1 Cu2 Cu4 60.34(2) . . ? I3 Cu2 Cu4 60.701(17) . . ? S2 Cu2 Cu3 136.35(4) . . ? I1 Cu2 Cu3 110.33(2) . . ? I3 Cu2 Cu3 59.507(18) . . ? Cu4 Cu2 Cu3 62.00(2) . . ? S2 Cu2 Cu1 147.32(3) . . ? I1 Cu2 Cu1 59.653(16) . . ? I3 Cu2 Cu1 109.30(2) . . ? Cu4 Cu2 Cu1 60.860(18) . . ? Cu3 Cu2 Cu1 60.053(18) . . ? S2 Cu2 I2 102.90(3) . . ? I1 Cu2 I2 110.28(2) . . ? I3 Cu2 I2 111.86(2) . . ? Cu4 Cu2 I2 109.07(2) . . ? Cu3 Cu2 I2 58.592(17) . . ? Cu1 Cu2 I2 57.984(16) . . ? S3 Cu3 I4 114.03(3) . . ? S3 Cu3 I3 104.79(3) . . ? I4 Cu3 I3 109.14(2) . . ? S3 Cu3 I2 99.99(3) . . ? I4 Cu3 I2 113.60(2) . . ? I3 Cu3 I2 114.80(2) . . ? S3 Cu3 Cu2 138.27(3) . . ? I4 Cu3 Cu2 107.70(2) . . ? I3 Cu3 Cu2 59.481(17) . . ? I2 Cu3 Cu2 61.96(2) . . ? S3 Cu3 Cu1 144.97(3) . . ? I4 Cu3 Cu1 60.611(17) . . ? I3 Cu3 Cu1 109.52(2) . . ? I2 Cu3 Cu1 59.158(19) . . ? Cu2 Cu3 Cu1 60.337(19) . . ? S3 Cu3 Cu4 150.62(3) . . ? I4 Cu3 Cu4 57.561(17) . . ? I3 Cu3 Cu4 59.552(17) . . ? I2 Cu3 Cu4 109.13(2) . . ? Cu2 Cu3 Cu4 58.712(19) . . ? Cu1 Cu3 Cu4 59.855(18) . . ? S4 Cu4 I4 115.32(3) 6_566 . ? S4 Cu4 I1 102.66(4) 6_566 . ? I4 Cu4 I1 113.886(19) . . ? S4 Cu4 Cu2 135.39(3) 6_566 . ? I4 Cu4 Cu2 109.28(2) . . ? I1 Cu4 Cu2 58.418(18) . . ? S4 Cu4 I3 103.19(3) 6_566 . ? I4 Cu4 I3 109.03(2) . . ? I1 Cu4 I3 112.224(19) . . ? Cu2 Cu4 I3 59.197(17) . . ? S4 Cu4 Cu1 148.36(4) 6_566 . ? I4 Cu4 Cu1 60.720(17) . . ? I1 Cu4 Cu1 58.831(17) . . ? Cu2 Cu4 Cu1 60.22(2) . . ? I3 Cu4 Cu1 107.60(2) . . ? S4 Cu4 Cu3 149.65(4) 6_566 . ? I4 Cu4 Cu3 58.850(17) . . ? I1 Cu4 Cu3 106.61(2) . . ? Cu2 Cu4 Cu3 59.29(2) . . ? I3 Cu4 Cu3 58.138(16) . . ? Cu1 Cu4 Cu3 58.97(2) . . ? Cu2 I1 Cu1 62.271(19) . . ? Cu2 I1 Cu4 61.241(17) . . ? Cu1 I1 Cu4 62.028(17) . . ? Cu1 I2 Cu3 61.101(17) . . ? Cu1 I2 Cu2 60.117(19) . . ? Cu3 I2 Cu2 59.450(18) . . ? Cu2 I3 Cu3 61.012(17) . . ? Cu2 I3 Cu4 60.102(16) . . ? Cu3 I3 Cu4 62.31(2) . . ? Cu4 I4 Cu3 63.59(2) . . ? Cu4 I4 Cu1 61.906(17) . . ? Cu3 I4 Cu1 60.835(16) . . ? C11 S1 C10 97.9(2) . . ? C11 S1 Cu1 105.68(12) . 1_565 ? C10 S1 Cu1 108.36(13) . 1_565 ? C18 S2 C19 104.49(19) . . ? C18 S2 Cu2 102.88(12) . . ? C19 S2 Cu2 104.06(12) . . ? C36 S3 C35 99.4(2) . . ? C36 S3 Cu3 107.72(14) . . ? C35 S3 Cu3 110.29(17) . . ? C43 S4 C44 103.3(2) . . ? C43 S4 Cu4 100.84(13) . 6_565 ? C44 S4 Cu4 105.18(15) . 6_565 ? C25 O1 C1 118.6(3) . . ? C4 O2 C3 118.1(3) . . ? C50 O3 C26 117.5(3) . . ? C29 O4 C28 118.6(4) . . ? O1 C1 C2 106.0(3) . . ? C1 C2 C3 112.3(4) . . ? O2 C3 C2 107.8(4) . . ? O2 C4 C5 124.1(4) . . ? O2 C4 C9 116.1(4) . . ? C5 C4 C9 119.8(4) . . ? C6 C5 C4 119.4(4) . . ? C5 C6 C7 121.7(4) . . ? C8 C7 C6 118.5(4) . . ? C7 C8 C9 121.9(4) . . ? C8 C9 C4 118.7(4) . . ? C8 C9 C10 121.0(4) . . ? C4 C9 C10 120.3(3) . . ? C9 C10 S1 111.6(3) . . ? C12 C11 S1 111.3(3) . . ? C14 C12 C13 118.5(3) . . ? C14 C12 C11 119.6(4) . . ? C13 C12 C11 121.9(4) . . ? C12 C13 C15 120.9(4) . . ? C12 C14 C16 120.7(4) . . ? C13 C15 C17 120.2(4) . . ? C17 C16 C14 121.1(4) . . ? C16 C17 C15 118.5(3) . . ? C16 C17 C18 120.9(3) . . ? C15 C17 C18 120.4(3) . . ? C17 C18 S2 113.3(3) . . ? C20 C19 S2 114.9(3) . . ? C21 C20 C25 118.1(4) . . ? C21 C20 C19 120.8(4) . . ? C25 C20 C19 121.1(4) . . ? C22 C21 C20 121.3(4) . . ? C23 C22 C21 119.8(5) . . ? C22 C23 C24 120.9(5) . . ? C25 C24 C23 118.7(4) . . ? O1 C25 C24 125.4(4) . . ? O1 C25 C20 113.5(4) . . ? C24 C25 C20 121.1(4) . . ? O3 C26 C27 108.5(4) . . ? C26 C27 C28 111.4(4) . . ? O4 C28 C27 106.8(4) . . ? O4 C29 C34 115.2(4) . . ? O4 C29 C30 124.3(5) . . ? C34 C29 C30 120.5(6) . . ? C31 C30 C29 118.7(7) . . ? C32 C31 C30 122.0(6) . . ? C31 C32 C33 119.5(7) . . ? C34 C33 C32 120.7(7) . . ? C33 C34 C29 118.5(5) . . ? C33 C34 C35 122.1(5) . . ? C29 C34 C35 119.5(5) . . ? C34 C35 S3 110.7(3) . . ? C37 C36 S3 113.5(3) . . ? C39 C37 C38 117.9(4) . . ? C39 C37 C36 121.7(4) . . ? C38 C37 C36 120.3(4) . . ? C40 C38 C37 121.1(4) . . ? C37 C39 C41 120.8(4) . . ? C38 C40 C42 121.9(4) . . ? C39 C41 C42 121.3(4) . . ? C41 C42 C40 117.0(4) . . ? C41 C42 C43 122.1(4) . . ? C40 C42 C43 120.9(4) . . ? C42 C43 S4 113.4(3) . . ? C45 C44 S4 115.7(3) . . ? C50 C45 C46 118.5(4) . . ? C50 C45 C44 122.4(4) . . ? C46 C45 C44 119.1(4) . . ? C45 C46 C47 121.4(5) . . ? C48 C47 C46 119.0(5) . . ? C49 C48 C47 120.7(4) . . ? C48 C49 C50 120.3(5) . . ? O3 C50 C45 115.5(4) . . ? O3 C50 C49 124.5(4) . . ? C45 C50 C49 120.1(4) . . ? Cl1 C51 Cl2 121.5(7) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.579 _refine_diff_density_min -1.212 _refine_diff_density_rms 0.168 ############################################################ data_3b _database_code_depnum_ccdc_archive 'CCDC 863931' #TrackingRef '9181_web_deposit_cif_file_0_In-HyeokPark_1327158897.CuX.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H52 Cu4 I4 O4 S4, C H2 Cl2' _chemical_formula_sum 'C51 H54 Cl2 Cu4 I4 O4 S4' _chemical_formula_weight 1691.84 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' I I -0.4742 1.8119 '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 17.0726(15) _cell_length_b 21.8272(18) _cell_length_c 16.3027(14) _cell_angle_alpha 90.00 _cell_angle_beta 110.571(4) _cell_angle_gamma 90.00 _cell_volume 5687.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9830 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 30.88 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.976 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3272 _exptl_absorpt_coefficient_mu 3.929 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4400 _exptl_absorpt_correction_T_max 0.6210 _exptl_absorpt_process_details ? _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 53038 _diffrn_reflns_av_R_equivalents 0.1450 _diffrn_reflns_av_sigmaI/netI 0.0782 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 28.00 _reflns_number_total 13702 _reflns_number_gt 10454 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0696P)^2^+8.0950P] 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 13702 _refine_ls_number_parameters 622 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0675 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.1403 _refine_ls_wR_factor_gt 0.1272 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _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 Cu1 Cu 0.15502(4) 0.82617(3) 0.69219(4) 0.02967(16) Uani 1 1 d . . . Cu2 Cu 0.28215(4) 0.90789(3) 0.70214(4) 0.02944(16) Uani 1 1 d . . . Cu3 Cu 0.30164(4) 0.82004(3) 0.82214(5) 0.02850(16) Uani 1 1 d . . . Cu4 Cu 0.20217(4) 0.91410(3) 0.82164(5) 0.02976(16) Uani 1 1 d . . . I1 I 0.12214(2) 0.945122(16) 0.65141(2) 0.02880(10) Uani 1 1 d . . . I2 I 0.28618(2) 0.792538(17) 0.65157(2) 0.02989(10) Uani 1 1 d . . . I3 I 0.37099(2) 0.928632(16) 0.87134(2) 0.02772(10) Uani 1 1 d . . . I4 I 0.16160(2) 0.802109(16) 0.85677(2) 0.02718(10) Uani 1 1 d . . . O1 O -0.1071(3) 0.55949(19) 0.4493(3) 0.0432(11) Uani 1 1 d . . . O2 O -0.0833(2) 0.72272(18) 0.3906(2) 0.0315(9) Uani 1 1 d . . . O3 O 0.7176(4) 0.5533(2) 1.0512(3) 0.0598(15) Uani 1 1 d . . . O4 O 0.5754(3) 0.7318(2) 1.0463(3) 0.0467(12) Uani 1 1 d . . . S1 S 0.04193(8) 0.77224(6) 0.59809(9) 0.0257(3) Uani 1 1 d . . . S2 S -0.16249(8) 0.49795(6) 0.61656(9) 0.0272(3) Uani 1 1 d . . . S3 S 0.39212(8) 0.74204(6) 0.88239(8) 0.0241(3) Uani 1 1 d . . . S4 S 0.65237(8) 0.47008(6) 0.86737(9) 0.0266(3) Uani 1 1 d . . . C1 C -0.0404(4) 0.5940(3) 0.4336(4) 0.0411(15) Uani 1 1 d . . . H1A H 0.0071 0.5662 0.4390 0.049 Uiso 1 1 calc R . . H1B H -0.0201 0.6266 0.4783 0.049 Uiso 1 1 calc R . . C2 C -0.0709(4) 0.6220(3) 0.3447(4) 0.0373(14) Uani 1 1 d . . . H2A H -0.0222 0.6368 0.3307 0.045 Uiso 1 1 calc R . . H2B H -0.0993 0.5901 0.3012 0.045 Uiso 1 1 calc R . . C3 C -0.1296(4) 0.6739(3) 0.3359(4) 0.0386(14) Uani 1 1 d . . . H3A H -0.1530 0.6876 0.2742 0.046 Uiso 1 1 calc R . . H3B H -0.1764 0.6611 0.3546 0.046 Uiso 1 1 calc R . . C4 C -0.1245(4) 0.7757(3) 0.3927(3) 0.0282(12) Uani 1 1 d . . . C5 C -0.2083(4) 0.7852(3) 0.3482(4) 0.0380(14) Uani 1 1 d . . . H5A H -0.2417 0.7534 0.3133 0.046 Uiso 1 1 calc R . . C6 C -0.2439(5) 0.8414(4) 0.3542(4) 0.0509(19) Uani 1 1 d . . . H6A H -0.3021 0.8474 0.3241 0.061 Uiso 1 1 calc R . . C7 C -0.1964(5) 0.8888(3) 0.4030(4) 0.0504(18) Uani 1 1 d . . . H7A H -0.2213 0.9271 0.4067 0.060 Uiso 1 1 calc R . . C8 C -0.1110(5) 0.8791(3) 0.4468(4) 0.0412(15) Uani 1 1 d . . . H8A H -0.0775 0.9117 0.4795 0.049 Uiso 1 1 calc R . . C9 C -0.0741(4) 0.8232(2) 0.4436(3) 0.0295(12) Uani 1 1 d . . . C10 C 0.0168(4) 0.8136(3) 0.4928(4) 0.0338(13) Uani 1 1 d . . . H10A H 0.0447 0.8541 0.5046 0.041 Uiso 1 1 calc R . . H10B H 0.0408 0.7904 0.4550 0.041 Uiso 1 1 calc R . . C11 C -0.0436(3) 0.7906(2) 0.6383(3) 0.0246(11) Uani 1 1 d . . . H11A H -0.0205 0.8097 0.6970 0.030 Uiso 1 1 calc R . . H11B H -0.0827 0.8200 0.5980 0.030 Uiso 1 1 calc R . . C12 C -0.0896(3) 0.7323(2) 0.6434(3) 0.0222(10) Uani 1 1 d . . . C13 C -0.1592(4) 0.7135(3) 0.5739(4) 0.0326(13) Uani 1 1 d . . . H13A H -0.1793 0.7380 0.5225 0.039 Uiso 1 1 calc R . . C14 C -0.0611(4) 0.6958(3) 0.7168(3) 0.0293(12) Uani 1 1 d . . . H14A H -0.0135 0.7082 0.7650 0.035 Uiso 1 1 calc R . . C15 C -0.1009(4) 0.6410(3) 0.7212(4) 0.0314(12) Uani 1 1 d . . . H15A H -0.0805 0.6163 0.7724 0.038 Uiso 1 1 calc R . . C16 C -0.2000(4) 0.6595(3) 0.5784(4) 0.0324(13) Uani 1 1 d . . . H16A H -0.2488 0.6481 0.5309 0.039 Uiso 1 1 calc R . . C17 C -0.1707(3) 0.6219(2) 0.6510(4) 0.0259(11) Uani 1 1 d . . . C18 C -0.2110(4) 0.5612(2) 0.6563(4) 0.0302(12) Uani 1 1 d . . . H18A H -0.2713 0.5632 0.6207 0.036 Uiso 1 1 calc R . . H18B H -0.2056 0.5532 0.7178 0.036 Uiso 1 1 calc R . . C19 C -0.2235(4) 0.5029(3) 0.4996(4) 0.0378(14) Uani 1 1 d . . . H19A H -0.2799 0.4854 0.4884 0.045 Uiso 1 1 calc R . . H19B H -0.2304 0.5465 0.4816 0.045 Uiso 1 1 calc R . . C20 C -0.1820(4) 0.4693(3) 0.4469(4) 0.0296(12) Uani 1 1 d . . . C21 C -0.1986(4) 0.4088(3) 0.4246(4) 0.0418(15) Uani 1 1 d . . . H21A H -0.2384 0.3874 0.4424 0.050 Uiso 1 1 calc R . . C22 C -0.1570(4) 0.3778(3) 0.3753(4) 0.0436(16) Uani 1 1 d . . . H22A H -0.1691 0.3360 0.3592 0.052 Uiso 1 1 calc R . . C23 C -0.0985(5) 0.4096(3) 0.3511(4) 0.0459(16) Uani 1 1 d . . . H23A H -0.0700 0.3890 0.3185 0.055 Uiso 1 1 calc R . . C24 C -0.0804(4) 0.4700(3) 0.3729(4) 0.0389(14) Uani 1 1 d . . . H24A H -0.0402 0.4910 0.3552 0.047 Uiso 1 1 calc R . . C25 C -0.1212(4) 0.4999(3) 0.4208(4) 0.0328(13) Uani 1 1 d . . . C26 C 0.7364(5) 0.6107(4) 1.0969(5) 0.061(2) Uani 1 1 d . . . H26A H 0.7860 0.6302 1.0899 0.073 Uiso 1 1 calc R . . H26B H 0.7468 0.6052 1.1602 0.073 Uiso 1 1 calc R . . C27 C 0.6622(5) 0.6468(4) 1.0557(6) 0.079(3) Uani 1 1 d . . . H27A H 0.6135 0.6224 1.0563 0.095 Uiso 1 1 calc R . . H27B H 0.6562 0.6526 0.9935 0.095 Uiso 1 1 calc R . . C28 C 0.6562(5) 0.7102(4) 1.0942(5) 0.059(2) Uani 1 1 d . . . H28A H 0.6642 0.7069 1.1572 0.070 Uiso 1 1 calc R . . H28B H 0.6992 0.7382 1.0875 0.070 Uiso 1 1 calc R . . C29 C 0.5439(4) 0.7818(3) 1.0759(4) 0.0323(13) Uani 1 1 d . . . C30 C 0.5931(4) 0.8288(3) 1.1249(4) 0.0407(15) Uani 1 1 d . . . H30A H 0.6522 0.8277 1.1405 0.049 Uiso 1 1 calc R . . C31 C 0.5552(5) 0.8772(3) 1.1506(4) 0.0482(17) Uani 1 1 d . . . H31A H 0.5887 0.9094 1.1844 0.058 Uiso 1 1 calc R . . C32 C 0.4703(4) 0.8796(3) 1.1283(4) 0.0472(17) Uani 1 1 d . . . H32A H 0.4451 0.9130 1.1473 0.057 Uiso 1 1 calc R . . C33 C 0.4207(4) 0.8330(3) 1.0778(4) 0.0405(15) Uani 1 1 d . . . H33A H 0.3616 0.8349 1.0614 0.049 Uiso 1 1 calc R . . C34 C 0.4581(3) 0.7834(3) 1.0509(3) 0.0281(12) Uani 1 1 d . . . C35 C 0.4055(3) 0.7326(3) 0.9973(3) 0.0310(12) Uani 1 1 d . . . H35A H 0.3501 0.7326 1.0040 0.037 Uiso 1 1 calc R . . H35B H 0.4326 0.6927 1.0185 0.037 Uiso 1 1 calc R . . C36 C 0.3361(4) 0.6724(2) 0.8361(4) 0.0317(12) Uani 1 1 d . . . H36A H 0.2987 0.6618 0.8687 0.038 Uiso 1 1 calc R . . H36B H 0.3004 0.6805 0.7746 0.038 Uiso 1 1 calc R . . C37 C 0.3918(3) 0.6175(2) 0.8382(3) 0.0245(11) Uani 1 1 d . . . C38 C 0.4779(3) 0.6213(3) 0.8670(4) 0.0390(15) Uani 1 1 d . . . H38A H 0.5049 0.6589 0.8899 0.047 Uiso 1 1 calc R . . C39 C 0.3546(3) 0.5617(3) 0.8062(4) 0.0332(13) Uani 1 1 d . . . H39A H 0.2954 0.5577 0.7872 0.040 Uiso 1 1 calc R . . C40 C 0.4029(4) 0.5119(3) 0.8018(4) 0.0343(13) Uani 1 1 d . . . H40A H 0.3761 0.4741 0.7798 0.041 Uiso 1 1 calc R . . C41 C 0.5252(4) 0.5710(3) 0.8628(5) 0.0430(16) Uani 1 1 d . . . H41A H 0.5845 0.5746 0.8840 0.052 Uiso 1 1 calc R . . C42 C 0.4896(3) 0.5154(2) 0.8288(3) 0.0262(11) Uani 1 1 d . . . C43 C 0.5395(3) 0.4625(3) 0.8158(4) 0.0306(12) Uani 1 1 d . . . H43A H 0.5260 0.4566 0.7521 0.037 Uiso 1 1 calc R . . H43B H 0.5217 0.4252 0.8388 0.037 Uiso 1 1 calc R . . C44 C 0.6661(3) 0.4416(3) 0.9771(4) 0.0308(12) Uani 1 1 d . . . H44A H 0.6256 0.4621 0.9990 0.037 Uiso 1 1 calc R . . H44B H 0.6549 0.3970 0.9744 0.037 Uiso 1 1 calc R . . C45 C 0.7538(4) 0.4538(3) 1.0390(4) 0.0355(14) Uani 1 1 d . . . C46 C 0.8124(4) 0.4071(4) 1.0601(4) 0.0483(17) Uani 1 1 d . . . H46A H 0.7961 0.3681 1.0337 0.058 Uiso 1 1 calc R . . C47 C 0.8937(5) 0.4144(4) 1.1180(4) 0.058(2) Uani 1 1 d . . . H47A H 0.9312 0.3807 1.1348 0.069 Uiso 1 1 calc R . . C48 C 0.9173(5) 0.4706(4) 1.1493(5) 0.0518(18) Uani 1 1 d . . . H48A H 0.9741 0.4764 1.1853 0.062 Uiso 1 1 calc R . . C49 C 0.8665(5) 0.5191(3) 1.1336(4) 0.0511(19) Uani 1 1 d . . . H49A H 0.8863 0.5579 1.1587 0.061 Uiso 1 1 calc R . . C50 C 0.7777(5) 0.5103(3) 1.0753(4) 0.0472(17) Uani 1 1 d . . . C51 C 0.5572(6) 0.6775(4) 0.3511(6) 0.070(2) Uani 1 1 d . . . H51A H 0.5010 0.6591 0.3376 0.084 Uiso 1 1 calc R . . H51B H 0.5716 0.6995 0.4076 0.084 Uiso 1 1 calc R . . Cl1 Cl 0.6314(2) 0.61840(16) 0.3613(2) 0.1374(16) Uani 1 1 d . . . Cl2 Cl 0.5546(3) 0.7278(2) 0.2713(3) 0.1523(16) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0252(3) 0.0340(4) 0.0293(4) -0.0007(3) 0.0089(3) -0.0034(3) Cu2 0.0291(3) 0.0309(4) 0.0311(4) 0.0029(3) 0.0141(3) -0.0036(3) Cu3 0.0263(3) 0.0248(3) 0.0338(4) 0.0032(3) 0.0098(3) 0.0056(3) Cu4 0.0340(4) 0.0254(4) 0.0340(4) -0.0031(3) 0.0171(3) 0.0031(3) I1 0.02677(19) 0.02583(19) 0.03085(19) 0.00088(14) 0.00643(15) 0.00325(13) I2 0.0377(2) 0.0288(2) 0.0307(2) -0.00053(14) 0.02134(16) 0.00341(15) I3 0.02549(18) 0.02740(19) 0.02990(19) -0.00380(14) 0.00924(14) -0.00181(13) I4 0.02695(18) 0.0295(2) 0.02849(19) 0.00287(14) 0.01401(15) -0.00120(14) O1 0.059(3) 0.027(2) 0.057(3) 0.006(2) 0.037(2) -0.001(2) O2 0.031(2) 0.028(2) 0.030(2) -0.0013(16) 0.0052(17) -0.0009(17) O3 0.086(4) 0.038(3) 0.041(3) -0.015(2) 0.005(3) 0.001(3) O4 0.033(2) 0.049(3) 0.049(3) -0.021(2) 0.003(2) 0.013(2) S1 0.0260(6) 0.0250(7) 0.0285(7) -0.0010(5) 0.0126(5) -0.0040(5) S2 0.0282(7) 0.0249(7) 0.0336(7) 0.0039(5) 0.0174(6) -0.0011(5) S3 0.0230(6) 0.0235(7) 0.0267(7) 0.0018(5) 0.0098(5) 0.0042(5) S4 0.0246(6) 0.0268(7) 0.0279(7) -0.0047(5) 0.0087(5) 0.0027(5) C1 0.043(4) 0.040(4) 0.042(4) 0.000(3) 0.016(3) -0.009(3) C2 0.047(4) 0.031(3) 0.040(3) 0.000(3) 0.022(3) -0.008(3) C3 0.042(4) 0.037(3) 0.036(3) -0.005(3) 0.012(3) -0.010(3) C4 0.035(3) 0.024(3) 0.026(3) 0.001(2) 0.011(2) 0.000(2) C5 0.036(3) 0.044(4) 0.029(3) 0.003(3) 0.006(3) -0.001(3) C6 0.045(4) 0.074(5) 0.032(3) 0.014(3) 0.011(3) 0.023(4) C7 0.071(5) 0.045(4) 0.035(4) 0.006(3) 0.018(3) 0.027(4) C8 0.069(5) 0.023(3) 0.033(3) 0.002(2) 0.020(3) 0.003(3) C9 0.042(3) 0.026(3) 0.020(3) 0.000(2) 0.011(2) -0.005(2) C10 0.043(3) 0.036(3) 0.028(3) -0.003(2) 0.018(3) -0.012(3) C11 0.028(3) 0.024(3) 0.026(3) -0.003(2) 0.015(2) -0.002(2) C12 0.024(2) 0.022(3) 0.024(3) 0.002(2) 0.013(2) 0.001(2) C13 0.032(3) 0.031(3) 0.033(3) 0.011(2) 0.008(2) -0.002(2) C14 0.030(3) 0.034(3) 0.023(3) 0.000(2) 0.009(2) 0.001(2) C15 0.042(3) 0.028(3) 0.025(3) 0.003(2) 0.013(2) -0.005(2) C16 0.028(3) 0.034(3) 0.030(3) 0.003(2) 0.004(2) -0.010(2) C17 0.028(3) 0.023(3) 0.035(3) 0.003(2) 0.021(2) 0.001(2) C18 0.036(3) 0.021(3) 0.040(3) -0.001(2) 0.022(3) -0.004(2) C19 0.033(3) 0.045(4) 0.040(3) 0.013(3) 0.018(3) 0.008(3) C20 0.031(3) 0.030(3) 0.028(3) 0.007(2) 0.012(2) 0.004(2) C21 0.037(3) 0.041(4) 0.041(4) 0.010(3) 0.006(3) 0.000(3) C22 0.038(3) 0.031(3) 0.049(4) -0.005(3) -0.001(3) 0.002(3) C23 0.065(5) 0.039(4) 0.037(3) -0.001(3) 0.022(3) 0.014(3) C24 0.048(4) 0.037(4) 0.039(3) 0.006(3) 0.025(3) 0.003(3) C25 0.040(3) 0.032(3) 0.032(3) 0.006(2) 0.019(3) 0.006(3) C26 0.049(4) 0.062(5) 0.059(5) -0.019(4) 0.005(4) 0.006(4) C27 0.047(4) 0.097(7) 0.067(5) -0.050(5) -0.012(4) 0.034(4) C28 0.040(4) 0.059(5) 0.060(5) -0.030(4) -0.003(3) 0.013(3) C29 0.036(3) 0.030(3) 0.031(3) -0.003(2) 0.013(3) 0.010(2) C30 0.036(3) 0.040(4) 0.041(4) -0.010(3) 0.008(3) 0.001(3) C31 0.057(4) 0.040(4) 0.042(4) -0.013(3) 0.011(3) 0.004(3) C32 0.058(4) 0.042(4) 0.041(4) -0.011(3) 0.016(3) 0.019(3) C33 0.036(3) 0.052(4) 0.035(3) -0.001(3) 0.013(3) 0.014(3) C34 0.031(3) 0.035(3) 0.021(3) 0.003(2) 0.012(2) 0.006(2) C35 0.027(3) 0.040(3) 0.028(3) 0.005(2) 0.012(2) 0.001(2) C36 0.028(3) 0.027(3) 0.038(3) 0.002(2) 0.010(2) 0.003(2) C37 0.028(3) 0.022(3) 0.025(3) 0.002(2) 0.011(2) 0.005(2) C38 0.022(3) 0.023(3) 0.066(4) -0.011(3) 0.007(3) -0.001(2) C39 0.020(3) 0.032(3) 0.049(4) -0.003(3) 0.014(3) 0.000(2) C40 0.029(3) 0.025(3) 0.050(4) -0.009(3) 0.016(3) -0.006(2) C41 0.022(3) 0.037(3) 0.059(4) -0.011(3) 0.001(3) 0.003(2) C42 0.026(3) 0.026(3) 0.028(3) -0.001(2) 0.010(2) -0.003(2) C43 0.027(3) 0.029(3) 0.032(3) -0.011(2) 0.006(2) 0.001(2) C44 0.027(3) 0.035(3) 0.032(3) -0.001(2) 0.011(2) 0.000(2) C45 0.034(3) 0.053(4) 0.023(3) -0.002(3) 0.014(2) -0.006(3) C46 0.036(4) 0.074(5) 0.034(3) -0.006(3) 0.011(3) 0.002(3) C47 0.053(5) 0.085(6) 0.036(4) -0.002(4) 0.017(3) 0.014(4) C48 0.042(4) 0.056(5) 0.061(5) 0.000(4) 0.022(4) 0.001(3) C49 0.074(5) 0.052(4) 0.032(3) -0.012(3) 0.024(3) -0.023(4) C50 0.066(5) 0.049(4) 0.025(3) 0.003(3) 0.013(3) -0.012(4) C51 0.059(5) 0.070(6) 0.079(6) -0.004(5) 0.023(5) 0.008(4) Cl1 0.098(2) 0.126(3) 0.127(3) -0.057(2) -0.0360(19) 0.060(2) Cl2 0.133(3) 0.179(4) 0.184(4) 0.083(3) 0.103(3) 0.039(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 Cu1 S1 2.3206(15) . ? Cu1 I2 2.6521(8) . ? Cu1 Cu3 2.6543(10) . ? Cu1 I1 2.6901(8) . ? Cu1 I4 2.6973(8) . ? Cu1 Cu4 2.7553(10) . ? Cu1 Cu2 2.7698(9) . ? Cu2 S4 2.2949(15) 2_656 ? Cu2 I2 2.6576(8) . ? Cu2 Cu3 2.6752(10) . ? Cu2 I3 2.6785(8) . ? Cu2 I1 2.6871(8) . ? Cu2 Cu4 2.7474(10) . ? Cu3 S3 2.2767(14) . ? Cu3 I3 2.6450(8) . ? Cu3 Cu4 2.6624(9) . ? Cu3 I4 2.6715(8) . ? Cu3 I2 2.7653(8) . ? Cu4 S2 2.3029(15) 2_556 ? Cu4 I4 2.6574(8) . ? Cu4 I1 2.7135(8) . ? Cu4 I3 2.7245(8) . ? O1 C25 1.375(7) . ? O1 C1 1.461(7) . ? O2 C4 1.360(7) . ? O2 C3 1.434(7) . ? O3 C50 1.343(9) . ? O3 C26 1.436(8) . ? O4 C29 1.378(7) . ? O4 C28 1.406(8) . ? S1 C11 1.842(5) . ? S1 C10 1.851(6) . ? S2 C19 1.826(6) . ? S2 C18 1.841(6) . ? S2 Cu4 2.3029(15) 2_546 ? S3 C36 1.812(6) . ? S3 C35 1.817(5) . ? S4 C43 1.819(6) . ? S4 C44 1.829(6) . ? S4 Cu2 2.2949(15) 2_646 ? C1 C2 1.488(8) . ? C2 C3 1.486(9) . ? C4 C5 1.373(8) . ? C4 C9 1.415(7) . ? C5 C6 1.388(9) . ? C6 C7 1.380(11) . ? C7 C8 1.396(10) . ? C8 C9 1.383(8) . ? C9 C10 1.491(8) . ? C11 C12 1.513(7) . ? C12 C14 1.377(7) . ? C12 C13 1.386(8) . ? C13 C16 1.384(8) . ? C14 C15 1.391(8) . ? C15 C17 1.394(8) . ? C16 C17 1.380(7) . ? C17 C18 1.509(7) . ? C19 C20 1.487(8) . ? C20 C21 1.372(8) . ? C20 C25 1.419(8) . ? C21 C22 1.416(9) . ? C22 C23 1.383(10) . ? C23 C24 1.373(9) . ? C24 C25 1.379(8) . ? C26 C27 1.443(10) . ? C27 C28 1.538(10) . ? C29 C34 1.375(8) . ? C29 C30 1.388(8) . ? C30 C31 1.378(9) . ? C31 C32 1.366(10) . ? C32 C33 1.393(9) . ? C33 C34 1.404(8) . ? C34 C35 1.500(8) . ? C36 C37 1.523(7) . ? C37 C38 1.380(7) . ? C37 C39 1.390(8) . ? C38 C41 1.380(8) . ? C39 C40 1.381(8) . ? C40 C42 1.391(7) . ? C41 C42 1.382(8) . ? C42 C43 1.493(7) . ? C44 C45 1.506(8) . ? C45 C50 1.366(9) . ? C45 C46 1.386(9) . ? C46 C47 1.387(10) . ? C47 C48 1.334(11) . ? C48 C49 1.336(10) . ? C49 C50 1.492(10) . ? C51 Cl2 1.692(9) . ? C51 Cl1 1.774(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 Cu1 I2 105.90(4) . . ? S1 Cu1 Cu3 146.54(5) . . ? I2 Cu1 Cu3 62.82(2) . . ? S1 Cu1 I1 105.86(4) . . ? I2 Cu1 I1 109.06(3) . . ? Cu3 Cu1 I1 107.59(3) . . ? S1 Cu1 I4 107.04(4) . . ? I2 Cu1 I4 116.79(3) . . ? Cu3 Cu1 I4 59.89(2) . . ? I1 Cu1 I4 111.46(3) . . ? S1 Cu1 Cu4 144.19(5) . . ? I2 Cu1 Cu4 109.81(3) . . ? Cu3 Cu1 Cu4 58.93(2) . . ? I1 Cu1 Cu4 59.76(2) . . ? I4 Cu1 Cu4 58.32(2) . . ? S1 Cu1 Cu2 144.91(5) . . ? I2 Cu1 Cu2 58.66(2) . . ? Cu3 Cu1 Cu2 59.06(2) . . ? I1 Cu1 Cu2 58.94(2) . . ? I4 Cu1 Cu2 108.01(3) . . ? Cu4 Cu1 Cu2 59.64(3) . . ? S4 Cu2 I2 109.70(4) 2_656 . ? S4 Cu2 Cu3 145.90(5) 2_656 . ? I2 Cu2 Cu3 62.47(2) . . ? S4 Cu2 I3 102.16(4) 2_656 . ? I2 Cu2 I3 114.37(3) . . ? Cu3 Cu2 I3 59.21(2) . . ? S4 Cu2 I1 106.74(4) 2_656 . ? I2 Cu2 I1 108.99(3) . . ? Cu3 Cu2 I1 107.07(3) . . ? I3 Cu2 I1 114.36(3) . . ? S4 Cu2 Cu4 140.41(5) 2_656 . ? I2 Cu2 Cu4 109.89(3) . . ? Cu3 Cu2 Cu4 58.79(2) . . ? I3 Cu2 Cu4 60.27(2) . . ? I1 Cu2 Cu4 59.90(2) . . ? S4 Cu2 Cu1 149.28(5) 2_656 . ? I2 Cu2 Cu1 58.46(2) . . ? Cu3 Cu2 Cu1 58.32(3) . . ? I3 Cu2 Cu1 108.52(3) . . ? I1 Cu2 Cu1 59.05(2) . . ? Cu4 Cu2 Cu1 59.92(2) . . ? S3 Cu3 I3 112.07(4) . . ? S3 Cu3 Cu1 133.52(5) . . ? I3 Cu3 Cu1 113.15(3) . . ? S3 Cu3 Cu4 155.96(5) . . ? I3 Cu3 Cu4 61.77(2) . . ? Cu1 Cu3 Cu4 62.43(3) . . ? S3 Cu3 I4 108.73(4) . . ? I3 Cu3 I4 113.94(3) . . ? Cu1 Cu3 I4 60.86(2) . . ? Cu4 Cu3 I4 59.76(2) . . ? S3 Cu3 Cu2 137.96(5) . . ? I3 Cu3 Cu2 60.46(2) . . ? Cu1 Cu3 Cu2 62.62(3) . . ? Cu4 Cu3 Cu2 61.96(3) . . ? I4 Cu3 Cu2 111.65(3) . . ? S3 Cu3 I2 94.71(4) . . ? I3 Cu3 I2 111.96(3) . . ? Cu1 Cu3 I2 58.55(2) . . ? Cu4 Cu3 I2 109.20(3) . . ? I4 Cu3 I2 113.85(3) . . ? Cu2 Cu3 I2 58.45(2) . . ? S2 Cu4 I4 119.85(4) 2_556 . ? S2 Cu4 Cu3 153.75(5) 2_556 . ? I4 Cu4 Cu3 60.29(2) . . ? S2 Cu4 I1 97.43(4) 2_556 . ? I4 Cu4 I1 111.98(3) . . ? Cu3 Cu4 I1 106.68(3) . . ? S2 Cu4 I3 102.74(4) 2_556 . ? I4 Cu4 I3 111.82(3) . . ? Cu3 Cu4 I3 58.80(2) . . ? I1 Cu4 I3 112.03(3) . . ? S2 Cu4 Cu2 130.19(5) 2_556 . ? I4 Cu4 Cu2 109.85(3) . . ? Cu3 Cu4 Cu2 59.25(3) . . ? I1 Cu4 Cu2 58.95(2) . . ? I3 Cu4 Cu2 58.61(2) . . ? S2 Cu4 Cu1 146.82(5) 2_556 . ? I4 Cu4 Cu1 59.75(2) . . ? Cu3 Cu4 Cu1 58.64(3) . . ? I1 Cu4 Cu1 58.92(2) . . ? I3 Cu4 Cu1 107.62(3) . . ? Cu2 Cu4 Cu1 60.44(2) . . ? Cu2 I1 Cu1 62.01(2) . . ? Cu2 I1 Cu4 61.15(2) . . ? Cu1 I1 Cu4 61.31(2) . . ? Cu1 I2 Cu2 62.89(2) . . ? Cu1 I2 Cu3 58.63(2) . . ? Cu2 I2 Cu3 59.08(2) . . ? Cu3 I3 Cu2 60.33(2) . . ? Cu3 I3 Cu4 59.43(2) . . ? Cu2 I3 Cu4 61.12(2) . . ? Cu4 I4 Cu3 59.95(2) . . ? Cu4 I4 Cu1 61.93(2) . . ? Cu3 I4 Cu1 59.26(2) . . ? C25 O1 C1 118.9(5) . . ? C4 O2 C3 118.1(4) . . ? C50 O3 C26 116.7(6) . . ? C29 O4 C28 119.9(5) . . ? C11 S1 C10 105.6(3) . . ? C11 S1 Cu1 103.51(18) . . ? C10 S1 Cu1 103.49(19) . . ? C19 S2 C18 99.2(3) . . ? C19 S2 Cu4 110.8(2) . 2_546 ? C18 S2 Cu4 101.81(18) . 2_546 ? C36 S3 C35 101.0(3) . . ? C36 S3 Cu3 105.58(18) . . ? C35 S3 Cu3 110.5(2) . . ? C43 S4 C44 99.9(3) . . ? C43 S4 Cu2 109.79(18) . 2_646 ? C44 S4 Cu2 111.38(19) . 2_646 ? O1 C1 C2 110.8(5) . . ? C3 C2 C1 113.6(5) . . ? O2 C3 C2 107.5(5) . . ? O2 C4 C5 124.4(5) . . ? O2 C4 C9 115.1(5) . . ? C5 C4 C9 120.4(5) . . ? C4 C5 C6 119.7(6) . . ? C7 C6 C5 121.3(7) . . ? C6 C7 C8 118.6(6) . . ? C9 C8 C7 121.5(6) . . ? C8 C9 C4 118.5(6) . . ? C8 C9 C10 120.4(5) . . ? C4 C9 C10 121.1(5) . . ? C9 C10 S1 115.2(4) . . ? C12 C11 S1 109.1(3) . . ? C14 C12 C13 118.6(5) . . ? C14 C12 C11 120.2(5) . . ? C13 C12 C11 121.2(5) . . ? C16 C13 C12 120.8(5) . . ? C12 C14 C15 120.9(5) . . ? C14 C15 C17 120.4(5) . . ? C17 C16 C13 121.0(5) . . ? C16 C17 C15 118.3(5) . . ? C16 C17 C18 122.4(5) . . ? C15 C17 C18 119.3(5) . . ? C17 C18 S2 111.6(4) . . ? C20 C19 S2 111.2(4) . . ? C21 C20 C25 118.6(6) . . ? C21 C20 C19 122.2(6) . . ? C25 C20 C19 119.3(5) . . ? C20 C21 C22 120.8(6) . . ? C23 C22 C21 118.5(6) . . ? C24 C23 C22 121.9(6) . . ? C23 C24 C25 119.1(6) . . ? O1 C25 C24 125.1(5) . . ? O1 C25 C20 113.8(5) . . ? C24 C25 C20 121.0(6) . . ? O3 C26 C27 103.6(6) . . ? C26 C27 C28 118.3(6) . . ? O4 C28 C27 105.5(5) . . ? C34 C29 O4 115.0(5) . . ? C34 C29 C30 121.3(5) . . ? O4 C29 C30 123.7(5) . . ? C31 C30 C29 119.1(6) . . ? C32 C31 C30 121.1(6) . . ? C31 C32 C33 119.8(6) . . ? C32 C33 C34 120.0(6) . . ? C29 C34 C33 118.7(6) . . ? C29 C34 C35 120.8(5) . . ? C33 C34 C35 120.5(5) . . ? C34 C35 S3 110.5(4) . . ? C37 C36 S3 114.6(4) . . ? C38 C37 C39 118.2(5) . . ? C38 C37 C36 122.9(5) . . ? C39 C37 C36 118.9(5) . . ? C41 C38 C37 120.5(5) . . ? C40 C39 C37 120.5(5) . . ? C39 C40 C42 121.9(5) . . ? C38 C41 C42 122.4(5) . . ? C41 C42 C40 116.4(5) . . ? C41 C42 C43 122.9(5) . . ? C40 C42 C43 120.6(5) . . ? C42 C43 S4 115.4(4) . . ? C45 C44 S4 110.6(4) . . ? C50 C45 C46 118.5(6) . . ? C50 C45 C44 121.7(6) . . ? C46 C45 C44 119.8(6) . . ? C45 C46 C47 123.2(7) . . ? C48 C47 C46 117.5(8) . . ? C47 C48 C49 124.6(7) . . ? C48 C49 C50 117.8(7) . . ? O3 C50 C45 115.0(6) . . ? O3 C50 C49 126.6(6) . . ? C45 C50 C49 118.3(7) . . ? Cl2 C51 Cl1 111.6(5) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.644 _refine_diff_density_min -1.482 _refine_diff_density_rms 0.221