# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email zhangbin@iccas.ac.cn _publ_contact_author_name 'Bin Zhang' loop_ _publ_author_name 'Bin Zhang' 'Yan Zhang' 'Daoben Zhu' data_160K _database_code_depnum_ccdc_archive 'CCDC 836179' #TrackingRef '- CCDC836179.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H32 Cu2 O14 S24' _chemical_formula_weight 1609.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.6554(3) _cell_length_b 16.9210(6) _cell_length_c 20.0587(8) _cell_angle_alpha 104.959(2) _cell_angle_beta 102.301(2) _cell_angle_gamma 91.736(2) _cell_volume 2761.70(18) _cell_formula_units_Z 2 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 57309 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 25.028 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.935 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1628 _exptl_absorpt_coefficient_mu 1.741 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.6144 _exptl_absorpt_correction_T_max 0.9627 _exptl_absorpt_process_details ; Gaussian integration (Coppens, 1970) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(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 'Nonius Kappa CCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30239 _diffrn_reflns_av_R_equivalents 0.0696 _diffrn_reflns_av_sigmaI/netI 0.0938 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.42 _diffrn_reflns_theta_max 25.07 _reflns_number_total 9650 _reflns_number_gt 5639 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0494P)^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 9650 _refine_ls_number_parameters 713 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1073 _refine_ls_R_factor_gt 0.0470 _refine_ls_wR_factor_ref 0.1099 _refine_ls_wR_factor_gt 0.0938 _refine_ls_goodness_of_fit_ref 0.951 _refine_ls_restrained_S_all 0.951 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.58786(7) 0.34899(4) 0.00684(3) 0.03405(19) Uani 1 1 d . . . Cu2 Cu 0.08170(7) 0.16082(4) 0.01420(3) 0.03321(19) Uani 1 1 d . . . S1 S 0.27528(16) -0.12332(7) 0.43997(6) 0.0348(3) Uani 1 1 d . . . S2 S 0.11208(15) 0.01367(7) 0.40177(6) 0.0317(3) Uani 1 1 d . . . S3 S 0.37284(15) -0.01678(7) 0.60353(6) 0.0327(3) Uani 1 1 d . . . S4 S 0.21393(15) 0.12132(7) 0.56539(6) 0.0329(3) Uani 1 1 d . . . S5 S 0.21710(16) -0.23141(7) 0.29628(6) 0.0349(3) Uani 1 1 d . . . S6 S 0.03358(15) -0.06533(7) 0.24691(6) 0.0322(3) Uani 1 1 d . . . S7 S 0.45956(15) 0.06174(7) 0.75752(6) 0.0317(3) Uani 1 1 d . . . S8 S 0.27923(16) 0.23007(7) 0.70951(6) 0.0341(3) Uani 1 1 d . . . S9 S 1.05987(15) 0.35119(7) 0.39462(6) 0.0330(3) Uani 1 1 d . . . S10 S 0.90822(15) 0.21822(7) 0.43402(6) 0.0324(3) Uani 1 1 d . . . S11 S 1.15205(15) 0.45708(7) 0.55754(6) 0.0339(3) Uani 1 1 d . . . S12 S 0.99703(15) 0.32597(7) 0.59820(6) 0.0318(3) Uani 1 1 d . . . S13 S 1.00925(15) 0.26149(7) 0.24220(6) 0.0320(3) Uani 1 1 d . . . S14 S 0.83663(15) 0.10274(7) 0.29334(6) 0.0285(3) Uani 1 1 d . . . S15 S 1.27234(16) 0.56179(7) 0.70118(6) 0.0361(4) Uani 1 1 d . . . S16 S 1.08639(15) 0.40536(7) 0.75191(6) 0.0318(3) Uani 1 1 d . . . S17 S 0.54964(15) 0.34817(7) 0.40392(6) 0.0312(3) Uani 1 1 d . . . S18 S 0.39977(15) 0.21723(7) 0.44612(6) 0.0322(3) Uani 1 1 d . . . S19 S 0.64003(15) 0.45803(7) 0.56731(6) 0.0321(3) Uani 1 1 d . . . S20 S 0.49368(15) 0.32593(7) 0.60947(6) 0.0313(3) Uani 1 1 d . . . S21 S 0.48263(15) 0.25936(7) 0.25098(6) 0.0321(3) Uani 1 1 d . . . S22 S 0.30179(15) 0.10435(7) 0.30423(6) 0.0333(3) Uani 1 1 d . . . S23 S 0.75560(16) 0.56529(7) 0.71088(6) 0.0365(4) Uani 1 1 d . . . S24 S 0.59534(16) 0.40398(7) 0.76373(6) 0.0327(3) Uani 1 1 d . . . O1 O 0.5186(4) 0.2667(2) 0.07936(18) 0.0480(10) Uani 1 1 d . . . O2 O 0.3639(4) 0.30346(19) -0.04448(16) 0.0349(9) Uani 1 1 d . . . O3 O 0.3045(4) 0.1827(2) 0.06795(16) 0.0419(9) Uani 1 1 d . . . O4 O 0.1546(4) 0.22373(19) -0.04464(15) 0.0356(9) Uani 1 1 d . . . O5 O 0.8117(4) 0.36837(19) 0.06352(15) 0.0344(9) Uani 1 1 d . . . O6 O 0.6653(4) 0.25090(19) -0.04871(15) 0.0388(9) Uani 1 1 d . . . O7 O 1.0109(4) 0.2905(2) 0.08472(16) 0.0407(9) Uani 1 1 d . . . O8 O 0.8581(4) 0.16963(19) -0.03295(15) 0.0340(8) Uani 1 1 d . . . O9 O 0.5104(4) 0.44456(19) 0.06385(15) 0.0316(8) Uani 1 1 d . . . O10 O 0.5779(4) 0.43243(19) -0.06392(16) 0.0363(9) Uani 1 1 d . . . O11 O 0.0199(4) 0.09131(18) 0.06939(14) 0.0311(8) Uani 1 1 d . . . O12 O 0.0626(4) 0.03670(19) -0.06483(15) 0.0355(9) Uani 1 1 d . . . C1 C 0.2206(5) -0.0243(3) 0.4683(2) 0.0259(12) Uani 1 1 d . . . C2 C 0.2629(5) 0.0215(3) 0.5372(2) 0.0285(12) Uani 1 1 d . . . C3 C 0.1911(5) -0.1359(3) 0.3499(2) 0.0270(12) Uani 1 1 d . . . C4 C 0.1194(5) -0.0722(3) 0.3325(2) 0.0257(12) Uani 1 1 d . . . C5 C 0.3684(6) 0.0700(3) 0.6730(2) 0.0269(12) Uani 1 1 d . . . C6 C 0.2990(5) 0.1336(3) 0.6549(2) 0.0288(12) Uani 1 1 d . . . C7 C 0.0941(6) -0.2290(3) 0.2115(2) 0.0381(14) Uani 1 1 d . . . H7A H 0.1199 -0.2736 0.1737 0.046 Uiso 1 1 calc R . . H7B H -0.0187 -0.2399 0.2119 0.046 Uiso 1 1 calc R . . C8 C 0.1150(6) -0.1489(3) 0.1940(2) 0.0347(13) Uani 1 1 d . . . H8A H 0.0639 -0.1562 0.1435 0.042 Uiso 1 1 calc R . . H8B H 0.2298 -0.1342 0.2004 0.042 Uiso 1 1 calc R . . C9 C 0.3948(6) 0.1504(3) 0.8132(2) 0.0312(13) Uani 1 1 d . . . H9A H 0.2810 0.1393 0.8118 0.037 Uiso 1 1 calc R . . H9B H 0.4549 0.1588 0.8627 0.037 Uiso 1 1 calc R . . C10 C 0.4170(6) 0.2287(3) 0.7910(2) 0.0346(13) Uani 1 1 d . . . H10A H 0.5269 0.2350 0.7849 0.041 Uiso 1 1 calc R . . H10B H 0.4035 0.2763 0.8295 0.041 Uiso 1 1 calc R . . C11 C 1.0131(5) 0.3148(3) 0.4618(2) 0.0289(12) Uani 1 1 d . . . C12 C 1.0511(5) 0.3601(3) 0.5310(2) 0.0249(12) Uani 1 1 d . . . C13 C 0.9898(5) 0.2606(3) 0.3269(2) 0.0257(12) Uani 1 1 d . . . C14 C 0.9221(5) 0.1995(3) 0.3456(2) 0.0246(11) Uani 1 1 d . . . C15 C 1.1673(6) 0.4697(3) 0.6479(2) 0.0275(12) Uani 1 1 d . . . C16 C 1.0959(6) 0.4098(3) 0.6670(2) 0.0281(12) Uani 1 1 d . . . C17 C 0.8477(5) 0.1861(3) 0.1891(2) 0.0268(12) Uani 1 1 d . . . H17A H 0.7460 0.2072 0.1974 0.032 Uiso 1 1 calc R . . H17B H 0.8463 0.1785 0.1384 0.032 Uiso 1 1 calc R . . C18 C 0.8598(6) 0.1040(3) 0.2054(2) 0.0283(12) Uani 1 1 d . . . H18A H 0.9646 0.0850 0.2000 0.034 Uiso 1 1 calc R . . H18B H 0.7777 0.0639 0.1698 0.034 Uiso 1 1 calc R . . C19 C 1.2217(7) 0.5659(3) 0.7851(2) 0.0478(16) Uani 1 1 d . . . H19A H 1.2964 0.6078 0.8228 0.057 Uiso 1 1 calc R . . H19B H 1.1140 0.5847 0.7832 0.057 Uiso 1 1 calc R . . C20 C 1.2246(7) 0.4888(3) 0.8052(3) 0.0535(17) Uani 1 1 d . . . H20A H 1.2084 0.5007 0.8541 0.064 Uiso 1 1 calc R . . H20B H 1.3324 0.4704 0.8067 0.064 Uiso 1 1 calc R . . C21 C 0.5015(5) 0.3139(3) 0.4720(2) 0.0260(12) Uani 1 1 d . . . C22 C 0.5417(5) 0.3610(3) 0.5413(2) 0.0252(12) Uani 1 1 d . . . C23 C 0.4675(5) 0.2596(3) 0.3370(2) 0.0254(12) Uani 1 1 d . . . C24 C 0.3966(5) 0.1995(3) 0.3560(2) 0.0278(12) Uani 1 1 d . . . C25 C 0.6579(6) 0.4714(3) 0.6580(2) 0.0282(12) Uani 1 1 d . . . C26 C 0.5948(5) 0.4103(3) 0.6777(2) 0.0253(12) Uani 1 1 d . . . C27 C 0.4521(6) 0.1496(3) 0.2095(2) 0.0321(13) Uani 1 1 d . . . H27A H 0.4523 0.1395 0.1587 0.039 Uiso 1 1 calc R . . H27B H 0.5419 0.1230 0.2316 0.039 Uiso 1 1 calc R . . C28 C 0.3002(6) 0.1108(3) 0.2159(2) 0.0326(13) Uani 1 1 d . . . H28A H 0.2791 0.0548 0.1832 0.039 Uiso 1 1 calc R . . H28B H 0.2123 0.1431 0.2009 0.039 Uiso 1 1 calc R . . C29 C 0.7092(6) 0.5686(3) 0.7955(2) 0.0340(13) Uani 1 1 d . . . H29A H 0.7763 0.6143 0.8325 0.041 Uiso 1 1 calc R . . H29B H 0.5969 0.5801 0.7930 0.041 Uiso 1 1 calc R . . C30 C 0.7347(6) 0.4904(3) 0.8167(2) 0.0314(12) Uani 1 1 d . . . H30A H 0.7282 0.5003 0.8668 0.038 Uiso 1 1 calc R . . H30B H 0.8434 0.4758 0.8137 0.038 Uiso 1 1 calc R . . C31 C 0.3838(7) 0.2344(3) 0.0491(2) 0.0345(13) Uani 1 1 d . . . C32 C 0.2948(6) 0.2564(3) -0.0189(2) 0.0305(13) Uani 1 1 d . . . C33 C 0.8837(6) 0.3043(3) 0.0509(2) 0.0280(12) Uani 1 1 d . . . C34 C 0.7961(6) 0.2358(3) -0.0156(2) 0.0305(12) Uani 1 1 d . . . C35 C 0.4813(6) 0.5044(3) 0.0375(2) 0.0300(12) Uani 1 1 d . . . C36 C -0.0132(6) 0.0148(3) 0.0384(2) 0.0310(13) Uani 1 1 d . . . O13 O 0.3648(6) -0.0453(3) 0.1047(2) 0.0915(16) Uani 1 1 d . . . C37 C 0.4397(10) -0.0342(5) 0.0521(4) 0.106(3) Uani 1 1 d . . . O14 O -0.1333(8) -0.3905(4) 0.1020(3) 0.082(3) Uani 0.736(11) 1 d P . . O14A O 0.092(3) -0.3811(11) 0.0815(9) 0.092(9) Uani 0.264(11) 1 d P . . C38 C -0.0583(11) -0.4199(5) 0.0495(4) 0.083(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0315(4) 0.0336(4) 0.0316(4) 0.0010(3) 0.0047(3) 0.0060(3) Cu2 0.0362(4) 0.0350(4) 0.0287(3) 0.0099(3) 0.0063(3) 0.0043(3) S1 0.0481(9) 0.0303(7) 0.0226(7) 0.0039(6) 0.0041(6) 0.0099(7) S2 0.0419(9) 0.0278(7) 0.0219(7) 0.0031(6) 0.0036(6) 0.0082(6) S3 0.0439(9) 0.0292(7) 0.0214(7) 0.0025(6) 0.0045(6) 0.0076(6) S4 0.0454(9) 0.0288(7) 0.0227(7) 0.0051(6) 0.0054(6) 0.0077(6) S5 0.0483(9) 0.0276(7) 0.0259(7) 0.0017(6) 0.0080(6) 0.0078(7) S6 0.0376(8) 0.0318(7) 0.0221(7) 0.0034(6) 0.0008(6) 0.0039(6) S7 0.0366(8) 0.0300(7) 0.0223(7) 0.0012(6) 0.0003(6) 0.0016(6) S8 0.0465(9) 0.0269(7) 0.0260(7) 0.0016(6) 0.0086(6) 0.0075(6) S9 0.0457(9) 0.0271(7) 0.0232(7) 0.0037(6) 0.0064(6) -0.0048(6) S10 0.0415(9) 0.0304(7) 0.0233(7) 0.0028(6) 0.0094(6) -0.0041(6) S11 0.0448(9) 0.0288(7) 0.0245(7) 0.0040(6) 0.0050(6) -0.0053(6) S12 0.0415(9) 0.0280(7) 0.0219(7) 0.0016(6) 0.0061(6) -0.0043(6) S13 0.0416(9) 0.0304(7) 0.0223(7) 0.0045(6) 0.0079(6) -0.0045(6) S14 0.0345(8) 0.0244(7) 0.0232(6) 0.0028(5) 0.0046(6) -0.0016(6) S15 0.0459(9) 0.0304(8) 0.0257(7) 0.0016(6) 0.0034(6) -0.0093(7) S16 0.0440(9) 0.0263(7) 0.0232(7) 0.0025(6) 0.0092(6) 0.0013(6) S17 0.0390(8) 0.0291(7) 0.0239(7) 0.0058(6) 0.0063(6) -0.0035(6) S18 0.0396(8) 0.0296(7) 0.0256(7) 0.0051(6) 0.0076(6) -0.0049(6) S19 0.0405(9) 0.0310(8) 0.0237(7) 0.0073(6) 0.0063(6) -0.0035(6) S20 0.0386(8) 0.0292(7) 0.0251(7) 0.0059(6) 0.0076(6) -0.0032(6) S21 0.0439(9) 0.0289(7) 0.0234(7) 0.0049(6) 0.0107(6) 0.0018(6) S22 0.0376(8) 0.0321(8) 0.0271(7) 0.0034(6) 0.0071(6) -0.0048(6) S23 0.0509(9) 0.0292(8) 0.0246(7) 0.0041(6) 0.0039(6) -0.0088(7) S24 0.0476(9) 0.0267(7) 0.0249(7) 0.0057(6) 0.0125(6) 0.0021(6) O1 0.029(2) 0.057(3) 0.052(2) 0.014(2) -0.0033(18) 0.000(2) O2 0.031(2) 0.036(2) 0.036(2) 0.0084(17) 0.0073(16) -0.0027(17) O3 0.037(2) 0.050(2) 0.039(2) 0.0209(18) -0.0026(17) 0.0003(19) O4 0.027(2) 0.045(2) 0.0331(19) 0.0131(16) 0.0001(16) -0.0033(18) O5 0.030(2) 0.035(2) 0.0299(19) -0.0044(16) 0.0056(15) 0.0017(17) O6 0.032(2) 0.043(2) 0.0273(18) -0.0079(16) -0.0036(16) 0.0129(18) O7 0.032(2) 0.050(2) 0.034(2) 0.0084(17) -0.0016(17) 0.0072(18) O8 0.032(2) 0.0283(19) 0.0358(19) -0.0017(16) 0.0077(16) 0.0054(17) O9 0.037(2) 0.030(2) 0.0304(18) 0.0094(16) 0.0122(15) 0.0100(17) O10 0.044(2) 0.028(2) 0.042(2) 0.0074(17) 0.0228(17) 0.0072(18) O11 0.040(2) 0.0255(19) 0.0273(18) 0.0022(16) 0.0129(15) 0.0036(16) O12 0.052(2) 0.030(2) 0.0269(19) 0.0060(16) 0.0180(17) 0.0032(18) C1 0.027(3) 0.026(3) 0.023(3) 0.005(2) 0.005(2) 0.002(2) C2 0.030(3) 0.029(3) 0.024(3) 0.004(2) 0.005(2) 0.002(2) C3 0.030(3) 0.030(3) 0.018(2) 0.000(2) 0.005(2) 0.003(2) C4 0.027(3) 0.029(3) 0.016(2) -0.001(2) 0.003(2) -0.001(2) C5 0.035(3) 0.021(3) 0.021(3) 0.000(2) 0.006(2) 0.002(2) C6 0.032(3) 0.029(3) 0.022(3) 0.000(2) 0.008(2) -0.003(2) C7 0.050(4) 0.030(3) 0.027(3) -0.003(2) 0.006(2) -0.002(3) C8 0.036(3) 0.046(3) 0.020(3) 0.004(2) 0.009(2) 0.004(3) C9 0.028(3) 0.035(3) 0.022(3) -0.003(2) -0.001(2) 0.003(2) C10 0.043(3) 0.029(3) 0.024(3) -0.002(2) 0.004(2) -0.001(3) C11 0.030(3) 0.030(3) 0.026(3) 0.006(2) 0.007(2) 0.001(2) C12 0.030(3) 0.024(3) 0.018(2) 0.002(2) 0.005(2) 0.002(2) C13 0.028(3) 0.023(3) 0.022(3) 0.001(2) 0.004(2) 0.001(2) C14 0.021(3) 0.024(3) 0.026(3) 0.002(2) 0.004(2) 0.003(2) C15 0.032(3) 0.025(3) 0.021(3) 0.000(2) 0.005(2) 0.004(2) C16 0.035(3) 0.026(3) 0.018(2) 0.001(2) 0.001(2) 0.008(2) C17 0.022(3) 0.036(3) 0.020(2) 0.005(2) 0.003(2) 0.002(2) C18 0.030(3) 0.030(3) 0.021(3) -0.002(2) 0.008(2) 0.001(2) C19 0.077(5) 0.031(3) 0.030(3) 0.000(3) 0.012(3) 0.001(3) C20 0.066(4) 0.048(4) 0.036(3) -0.005(3) 0.012(3) -0.011(3) C21 0.029(3) 0.027(3) 0.023(3) 0.007(2) 0.008(2) 0.003(2) C22 0.025(3) 0.024(3) 0.024(3) 0.005(2) 0.002(2) 0.002(2) C23 0.022(3) 0.031(3) 0.023(3) 0.008(2) 0.003(2) 0.000(2) C24 0.028(3) 0.030(3) 0.023(3) 0.005(2) 0.002(2) 0.000(2) C25 0.035(3) 0.024(3) 0.024(3) 0.004(2) 0.008(2) 0.004(2) C26 0.029(3) 0.029(3) 0.017(2) 0.006(2) 0.005(2) 0.008(2) C27 0.036(3) 0.032(3) 0.028(3) 0.007(2) 0.006(2) 0.009(3) C28 0.036(3) 0.035(3) 0.022(3) 0.006(2) 0.001(2) 0.001(3) C29 0.041(3) 0.030(3) 0.027(3) 0.002(2) 0.006(2) -0.007(3) C30 0.030(3) 0.044(3) 0.021(3) 0.009(2) 0.010(2) 0.003(3) C31 0.034(4) 0.034(3) 0.036(3) 0.008(3) 0.009(3) 0.013(3) C32 0.027(3) 0.035(3) 0.028(3) 0.003(3) 0.009(2) 0.010(3) C33 0.029(3) 0.030(3) 0.023(3) 0.004(2) 0.007(2) -0.004(3) C34 0.028(3) 0.036(3) 0.027(3) 0.003(2) 0.012(2) -0.006(3) C35 0.020(3) 0.036(3) 0.026(3) 0.001(3) -0.001(2) -0.006(3) C36 0.027(3) 0.039(3) 0.028(3) 0.008(3) 0.011(2) 0.009(3) O13 0.089(4) 0.066(3) 0.091(4) -0.004(3) -0.010(3) 0.014(3) C37 0.125(8) 0.109(7) 0.098(6) 0.041(5) 0.045(6) -0.012(6) O14 0.110(6) 0.073(5) 0.063(5) 0.032(4) 0.004(4) -0.003(4) O14A 0.12(2) 0.089(15) 0.077(13) 0.003(11) 0.054(13) 0.041(14) C38 0.076(6) 0.089(6) 0.083(6) 0.014(5) 0.027(5) 0.021(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 O9 1.952(3) . ? Cu1 O6 1.969(3) . ? Cu1 O5 1.996(3) . ? Cu1 O2 2.015(3) . ? Cu1 O10 2.237(3) . ? Cu1 O1 2.404(4) . ? Cu2 O11 1.945(3) . ? Cu2 O4 1.962(3) . ? Cu2 O3 1.971(3) . ? Cu2 O8 1.993(3) 1_455 ? Cu2 O12 2.258(3) . ? Cu2 O7 2.456(3) 1_455 ? S1 C1 1.739(4) . ? S1 C3 1.752(4) . ? S2 C1 1.738(4) . ? S2 C4 1.746(4) . ? S3 C2 1.743(4) . ? S3 C5 1.752(4) . ? S4 C2 1.733(5) . ? S4 C6 1.745(4) . ? S5 C3 1.746(4) . ? S5 C7 1.815(4) . ? S6 C4 1.754(4) . ? S6 C8 1.796(4) . ? S7 C5 1.753(4) . ? S7 C9 1.806(4) . ? S8 C6 1.751(4) . ? S8 C10 1.813(4) . ? S9 C11 1.734(5) . ? S9 C13 1.755(4) . ? S10 C11 1.740(5) . ? S10 C14 1.751(4) . ? S11 C12 1.733(4) . ? S11 C15 1.745(4) . ? S12 C12 1.740(5) . ? S12 C16 1.750(4) . ? S13 C13 1.746(5) . ? S13 C17 1.809(4) . ? S14 C14 1.742(4) . ? S14 C18 1.822(4) . ? S15 C15 1.743(4) . ? S15 C19 1.813(5) . ? S16 C16 1.743(5) . ? S16 C20 1.773(5) . ? S17 C21 1.735(5) . ? S17 C23 1.744(4) . ? S18 C21 1.732(4) . ? S18 C24 1.749(4) . ? S19 C22 1.726(4) . ? S19 C25 1.746(4) . ? S20 C22 1.744(5) . ? S20 C26 1.756(4) . ? S21 C23 1.757(4) . ? S21 C27 1.814(4) . ? S22 C24 1.742(4) . ? S22 C28 1.801(4) . ? S23 C25 1.741(4) . ? S23 C29 1.813(5) . ? S24 C26 1.755(4) . ? S24 C30 1.808(4) . ? O1 C31 1.232(6) . ? O2 C32 1.253(5) . ? O3 C31 1.274(6) . ? O4 C32 1.261(5) . ? O5 C33 1.263(5) . ? O6 C34 1.254(5) . ? O7 C33 1.227(5) . ? O8 C34 1.256(5) . ? O8 Cu2 1.993(3) 1_655 ? O9 C35 1.266(5) . ? O10 C35 1.241(5) 2_665 ? O11 C36 1.277(5) . ? O12 C36 1.240(5) 2 ? C1 C2 1.365(6) . ? C3 C4 1.346(6) . ? C5 C6 1.341(6) . ? C7 C8 1.499(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.522(6) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.364(5) . ? C13 C14 1.346(6) . ? C15 C16 1.349(6) . ? C17 C18 1.510(6) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.461(6) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.376(5) . ? C23 C24 1.349(6) . ? C25 C26 1.339(6) . ? C27 C28 1.496(6) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.499(6) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.557(7) . ? C33 C34 1.553(6) . ? C35 O10 1.241(5) 2_665 ? C35 C35 1.577(9) 2_665 ? C36 O12 1.240(5) 2 ? C36 C36 1.559(9) 2 ? O13 C37 1.399(8) . ? O14 C38 1.349(8) . ? O14A C38 1.38(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O9 Cu1 O6 178.40(14) . . ? O9 Cu1 O5 96.45(12) . . ? O6 Cu1 O5 83.31(13) . . ? O9 Cu1 O2 90.91(13) . . ? O6 Cu1 O2 89.01(13) . . ? O5 Cu1 O2 166.22(14) . . ? O9 Cu1 O10 80.17(12) . . ? O6 Cu1 O10 101.43(13) . . ? O5 Cu1 O10 104.09(13) . . ? O2 Cu1 O10 88.60(13) . . ? O9 Cu1 O1 90.36(13) . . ? O6 Cu1 O1 88.06(13) . . ? O5 Cu1 O1 90.55(12) . . ? O2 Cu1 O1 77.73(13) . . ? O10 Cu1 O1 163.29(12) . . ? O11 Cu2 O4 175.26(13) . . ? O11 Cu2 O3 94.62(14) . . ? O4 Cu2 O3 83.69(14) . . ? O11 Cu2 O8 93.48(13) . 1_455 ? O4 Cu2 O8 89.12(13) . 1_455 ? O3 Cu2 O8 165.46(13) . 1_455 ? O11 Cu2 O12 80.29(11) . . ? O4 Cu2 O12 95.91(13) . . ? O3 Cu2 O12 106.39(13) . . ? O8 Cu2 O12 86.87(12) 1_455 . ? C1 S1 C3 95.4(2) . . ? C1 S2 C4 95.4(2) . . ? C2 S3 C5 95.3(2) . . ? C2 S4 C6 95.3(2) . . ? C3 S5 C7 101.1(2) . . ? C4 S6 C8 100.9(2) . . ? C5 S7 C9 100.9(2) . . ? C6 S8 C10 100.7(2) . . ? C11 S9 C13 95.6(2) . . ? C11 S10 C14 95.2(2) . . ? C12 S11 C15 95.1(2) . . ? C12 S12 C16 95.3(2) . . ? C13 S13 C17 99.8(2) . . ? C14 S14 C18 102.8(2) . . ? C15 S15 C19 101.1(2) . . ? C16 S16 C20 101.3(3) . . ? C21 S17 C23 95.4(2) . . ? C21 S18 C24 95.6(2) . . ? C22 S19 C25 95.6(2) . . ? C22 S20 C26 95.0(2) . . ? C23 S21 C27 99.3(2) . . ? C24 S22 C28 102.1(2) . . ? C25 S23 C29 101.7(2) . . ? C26 S24 C30 101.2(2) . . ? C31 O1 Cu1 105.5(3) . . ? C32 O2 Cu1 117.2(3) . . ? C31 O3 Cu2 112.7(3) . . ? C32 O4 Cu2 112.7(3) . . ? C33 O5 Cu1 111.3(3) . . ? C34 O6 Cu1 111.1(3) . . ? C34 O8 Cu2 119.7(3) . 1_655 ? C35 O9 Cu1 117.6(3) . . ? C35 O10 Cu1 108.5(3) 2_665 . ? C36 O11 Cu2 117.1(3) . . ? C36 O12 Cu2 107.3(3) 2 . ? C2 C1 S2 122.0(3) . . ? C2 C1 S1 122.8(3) . . ? S2 C1 S1 115.1(2) . . ? C1 C2 S4 123.1(4) . . ? C1 C2 S3 121.8(3) . . ? S4 C2 S3 115.1(2) . . ? C4 C3 S5 130.2(3) . . ? C4 C3 S1 116.8(3) . . ? S5 C3 S1 113.0(3) . . ? C3 C4 S2 117.2(3) . . ? C3 C4 S6 126.9(3) . . ? S2 C4 S6 115.9(3) . . ? C6 C5 S3 116.5(3) . . ? C6 C5 S7 128.8(3) . . ? S3 C5 S7 114.6(3) . . ? C5 C6 S4 117.6(3) . . ? C5 C6 S8 128.8(3) . . ? S4 C6 S8 113.6(3) . . ? C8 C7 S5 113.5(3) . . ? C8 C7 H7A 108.9 . . ? S5 C7 H7A 108.9 . . ? C8 C7 H7B 108.9 . . ? S5 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? C7 C8 S6 114.2(3) . . ? C7 C8 H8A 108.7 . . ? S6 C8 H8A 108.7 . . ? C7 C8 H8B 108.7 . . ? S6 C8 H8B 108.7 . . ? H8A C8 H8B 107.6 . . ? C10 C9 S7 113.4(3) . . ? C10 C9 H9A 108.9 . . ? S7 C9 H9A 108.9 . . ? C10 C9 H9B 108.9 . . ? S7 C9 H9B 108.9 . . ? H9A C9 H9B 107.7 . . ? C9 C10 S8 113.3(3) . . ? C9 C10 H10A 108.9 . . ? S8 C10 H10A 108.9 . . ? C9 C10 H10B 108.9 . . ? S8 C10 H10B 108.9 . . ? H10A C10 H10B 107.7 . . ? C12 C11 S9 122.1(4) . . ? C12 C11 S10 122.8(4) . . ? S9 C11 S10 115.0(2) . . ? C11 C12 S11 122.2(4) . . ? C11 C12 S12 122.4(4) . . ? S11 C12 S12 115.3(2) . . ? C14 C13 S13 127.4(3) . . ? C14 C13 S9 116.4(3) . . ? S13 C13 S9 116.2(3) . . ? C13 C14 S14 129.4(3) . . ? C13 C14 S10 117.4(3) . . ? S14 C14 S10 113.2(3) . . ? C16 C15 S15 129.1(3) . . ? C16 C15 S11 117.5(3) . . ? S15 C15 S11 113.4(3) . . ? C15 C16 S16 128.4(3) . . ? C15 C16 S12 116.5(3) . . ? S16 C16 S12 115.1(3) . . ? C18 C17 S13 113.1(3) . . ? C18 C17 H17A 109.0 . . ? S13 C17 H17A 109.0 . . ? C18 C17 H17B 109.0 . . ? S13 C17 H17B 109.0 . . ? H17A C17 H17B 107.8 . . ? C17 C18 S14 115.5(3) . . ? C17 C18 H18A 108.4 . . ? S14 C18 H18A 108.4 . . ? C17 C18 H18B 108.4 . . ? S14 C18 H18B 108.4 . . ? H18A C18 H18B 107.5 . . ? C20 C19 S15 115.7(4) . . ? C20 C19 H19A 108.4 . . ? S15 C19 H19A 108.4 . . ? C20 C19 H19B 108.4 . . ? S15 C19 H19B 108.4 . . ? H19A C19 H19B 107.4 . . ? C19 C20 S16 118.4(4) . . ? C19 C20 H20A 107.7 . . ? S16 C20 H20A 107.7 . . ? C19 C20 H20B 107.7 . . ? S16 C20 H20B 107.7 . . ? H20A C20 H20B 107.1 . . ? C22 C21 S18 123.0(4) . . ? C22 C21 S17 121.7(3) . . ? S18 C21 S17 115.2(2) . . ? C21 C22 S19 123.4(4) . . ? C21 C22 S20 121.5(3) . . ? S19 C22 S20 115.1(2) . . ? C24 C23 S17 117.3(3) . . ? C24 C23 S21 126.7(3) . . ? S17 C23 S21 116.0(3) . . ? C23 C24 S22 129.9(3) . . ? C23 C24 S18 116.5(3) . . ? S22 C24 S18 113.6(3) . . ? C26 C25 S23 128.7(3) . . ? C26 C25 S19 117.2(3) . . ? S23 C25 S19 114.0(3) . . ? C25 C26 S24 128.4(3) . . ? C25 C26 S20 116.7(3) . . ? S24 C26 S20 114.8(3) . . ? C28 C27 S21 113.4(3) . . ? C28 C27 H27A 108.9 . . ? S21 C27 H27A 108.9 . . ? C28 C27 H27B 108.9 . . ? S21 C27 H27B 108.9 . . ? H27A C27 H27B 107.7 . . ? C27 C28 S22 113.5(3) . . ? C27 C28 H28A 108.9 . . ? S22 C28 H28A 108.9 . . ? C27 C28 H28B 108.9 . . ? S22 C28 H28B 108.9 . . ? H28A C28 H28B 107.7 . . ? C30 C29 S23 113.2(3) . . ? C30 C29 H29A 108.9 . . ? S23 C29 H29A 108.9 . . ? C30 C29 H29B 108.9 . . ? S23 C29 H29B 108.9 . . ? H29A C29 H29B 107.7 . . ? C29 C30 S24 114.8(3) . . ? C29 C30 H30A 108.6 . . ? S24 C30 H30A 108.6 . . ? C29 C30 H30B 108.6 . . ? S24 C30 H30B 108.6 . . ? H30A C30 H30B 107.5 . . ? O1 C31 O3 126.3(5) . . ? O1 C31 C32 119.7(5) . . ? O3 C31 C32 114.0(5) . . ? O2 C32 O4 124.5(5) . . ? O2 C32 C31 119.7(5) . . ? O4 C32 C31 115.7(5) . . ? O7 C33 O5 127.9(4) . . ? O7 C33 C34 117.9(4) . . ? O5 C33 C34 114.2(4) . . ? O6 C34 O8 124.1(4) . . ? O6 C34 C33 116.7(4) . . ? O8 C34 C33 119.2(4) . . ? O10 C35 O9 126.4(4) 2_665 . ? O10 C35 C35 117.4(6) 2_665 2_665 ? O9 C35 C35 116.1(6) . 2_665 ? O12 C36 O11 125.0(4) 2 . ? O12 C36 C36 118.5(6) 2 2 ? O11 C36 C36 116.5(6) . 2 ? O14 C38 O14A 99.6(9) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.07 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.748 _refine_diff_density_min -0.715 _refine_diff_density_rms 0.099 # Attachment '- CCDC836180.cif' data_290K _database_code_depnum_ccdc_archive 'CCDC 836180' #TrackingRef '- CCDC836180.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H32 Cu2 O14 S24' _chemical_formula_weight 1609.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7501(3) _cell_length_b 16.9319(6) _cell_length_c 20.1421(8) _cell_angle_alpha 105.1270(10) _cell_angle_beta 102.346(2) _cell_angle_gamma 91.8790(10) _cell_volume 2801.70(18) _cell_formula_units_Z 2 _cell_measurement_temperature 290(2) _cell_measurement_reflns_used 45193 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 25.028 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.907 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1628 _exptl_absorpt_coefficient_mu 1.716 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.608 _exptl_absorpt_correction_T_max 0.960 _exptl_absorpt_process_details ; Gaussian integration (Coppens, 1970) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 290(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 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31941 _diffrn_reflns_av_R_equivalents 0.0660 _diffrn_reflns_av_sigmaI/netI 0.1066 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 25.01 _reflns_number_total 9821 _reflns_number_gt 4982 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 3.0' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0447P)^2^+0.0000P] 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 9821 _refine_ls_number_parameters 713 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1257 _refine_ls_R_factor_gt 0.0464 _refine_ls_wR_factor_ref 0.1049 _refine_ls_wR_factor_gt 0.0881 _refine_ls_goodness_of_fit_ref 0.914 _refine_ls_restrained_S_all 0.914 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.58561(7) 0.34866(3) 0.00724(3) 0.0437(2) Uani 1 1 d . . . Cu2 Cu 0.07797(7) 0.16155(3) 0.01343(3) 0.0441(2) Uani 1 1 d . . . S1 S 0.27674(17) -0.12217(8) 0.43988(6) 0.0541(4) Uani 1 1 d . . . S2 S 0.11249(16) 0.01344(7) 0.40213(6) 0.0483(4) Uani 1 1 d . . . S3 S 0.37184(16) -0.01521(7) 0.60305(6) 0.0497(4) Uani 1 1 d . . . S4 S 0.21317(17) 0.12171(8) 0.56518(6) 0.0511(4) Uani 1 1 d . . . S5 S 0.21937(17) -0.23022(7) 0.29675(6) 0.0553(4) Uani 1 1 d . . . S6 S 0.03254(16) -0.06666(8) 0.24792(6) 0.0500(4) Uani 1 1 d . . . S7 S 0.45937(16) 0.06471(8) 0.75654(6) 0.0495(4) Uani 1 1 d . . . S8 S 0.27787(17) 0.23098(7) 0.70871(6) 0.0535(4) Uani 1 1 d . . . S9 S 1.05789(17) 0.35018(7) 0.39422(6) 0.0497(4) Uani 1 1 d . . . S10 S 0.90809(17) 0.21759(7) 0.43322(6) 0.0488(4) Uani 1 1 d . . . S11 S 1.15154(16) 0.45612(7) 0.55689(6) 0.0500(4) Uani 1 1 d . . . S12 S 0.99752(16) 0.32566(7) 0.59711(6) 0.0480(4) Uani 1 1 d . . . S13 S 1.00300(16) 0.26186(7) 0.24196(6) 0.0491(4) Uani 1 1 d . . . S14 S 0.83161(15) 0.10302(7) 0.29243(6) 0.0436(4) Uani 1 1 d . . . S15 S 1.27170(17) 0.56119(8) 0.70024(6) 0.0525(4) Uani 1 1 d . . . S16 S 1.08572(16) 0.40576(7) 0.75036(6) 0.0472(4) Uani 1 1 d . . . S17 S 0.54872(16) 0.34727(7) 0.40438(6) 0.0491(4) Uani 1 1 d . . . S18 S 0.40141(17) 0.21658(8) 0.44611(6) 0.0501(4) Uani 1 1 d . . . S19 S 0.64058(16) 0.45722(7) 0.56741(6) 0.0487(4) Uani 1 1 d . . . S20 S 0.49468(16) 0.32569(7) 0.60898(6) 0.0476(4) Uani 1 1 d . . . S21 S 0.48113(17) 0.25870(8) 0.25183(6) 0.0490(4) Uani 1 1 d . . . S22 S 0.30263(16) 0.10373(8) 0.30442(6) 0.0517(4) Uani 1 1 d . . . S23 S 0.75446(17) 0.56518(8) 0.71029(6) 0.0551(4) Uani 1 1 d . . . S24 S 0.59295(17) 0.40494(7) 0.76281(6) 0.0483(4) Uani 1 1 d . . . O1 O 0.5127(4) 0.2666(2) 0.07970(18) 0.0632(11) Uani 1 1 d . . . O2 O 0.3633(4) 0.30247(19) -0.04351(15) 0.0457(9) Uani 1 1 d . . . O3 O 0.2985(4) 0.1838(2) 0.06822(17) 0.0588(10) Uani 1 1 d . . . O4 O 0.1544(4) 0.22378(19) -0.04431(15) 0.0488(9) Uani 1 1 d . . . O5 O 0.8068(4) 0.36748(19) 0.06419(15) 0.0475(9) Uani 1 1 d . . . O6 O 0.6630(4) 0.25078(19) -0.04813(15) 0.0519(10) Uani 1 1 d . . . O7 O 1.0056(4) 0.2903(2) 0.08422(16) 0.0566(10) Uani 1 1 d . . . O8 O 0.8570(4) 0.17092(19) -0.03462(15) 0.0484(9) Uani 1 1 d . . . O9 O 0.5119(4) 0.44496(18) 0.06412(14) 0.0428(9) Uani 1 1 d . . . O10 O 0.5745(4) 0.43145(19) -0.06396(15) 0.0480(9) Uani 1 1 d . . . O11 O 0.0161(4) 0.09186(18) 0.06825(14) 0.0426(9) Uani 1 1 d . . . O12 O 0.0610(4) 0.03617(19) -0.06469(16) 0.0513(10) Uani 1 1 d . . . C1 C 0.2212(5) -0.0239(3) 0.4681(2) 0.0426(13) Uani 1 1 d . . . C2 C 0.2624(5) 0.0221(3) 0.5370(2) 0.0407(13) Uani 1 1 d . . . C3 C 0.1923(5) -0.1353(3) 0.3500(2) 0.0388(13) Uani 1 1 d . . . C4 C 0.1203(5) -0.0721(3) 0.3328(2) 0.0360(12) Uani 1 1 d . . . C5 C 0.3681(6) 0.0715(3) 0.6722(2) 0.0396(13) Uani 1 1 d . . . C6 C 0.2989(6) 0.1348(3) 0.6544(2) 0.0405(13) Uani 1 1 d . . . C7 C 0.0993(7) -0.2281(3) 0.2120(2) 0.0698(19) Uani 1 1 d . . . H7A H 0.1301 -0.2697 0.1753 0.084 Uiso 1 1 calc R . . H7B H -0.0093 -0.2432 0.2109 0.084 Uiso 1 1 calc R . . C8 C 0.1084(7) -0.1494(3) 0.1952(2) 0.0673(18) Uani 1 1 d . . . H8A H 0.0530 -0.1577 0.1464 0.081 Uiso 1 1 calc R . . H8B H 0.2178 -0.1335 0.1985 0.081 Uiso 1 1 calc R . . C9 C 0.3967(6) 0.1522(3) 0.8118(2) 0.0558(15) Uani 1 1 d . . . H9A H 0.2878 0.1400 0.8122 0.067 Uiso 1 1 calc R . . H9B H 0.4584 0.1613 0.8597 0.067 Uiso 1 1 calc R . . C10 C 0.4103(7) 0.2298(3) 0.7903(2) 0.0589(16) Uani 1 1 d . . . H10A H 0.5172 0.2394 0.7860 0.071 Uiso 1 1 calc R . . H10B H 0.3920 0.2751 0.8278 0.071 Uiso 1 1 calc R . . C11 C 1.0115(5) 0.3137(3) 0.4611(2) 0.0414(13) Uani 1 1 d . . . C12 C 1.0508(5) 0.3595(3) 0.5304(2) 0.0395(13) Uani 1 1 d . . . C13 C 0.9848(5) 0.2607(3) 0.3264(2) 0.0375(13) Uani 1 1 d . . . C14 C 0.9178(5) 0.1995(3) 0.3449(2) 0.0363(12) Uani 1 1 d . . . C15 C 1.1671(6) 0.4693(3) 0.6468(2) 0.0387(13) Uani 1 1 d . . . C16 C 1.0955(5) 0.4103(3) 0.6656(2) 0.0375(13) Uani 1 1 d . . . C17 C 0.8447(5) 0.1858(3) 0.1890(2) 0.0399(13) Uani 1 1 d . . . H17A H 0.7458 0.2061 0.1967 0.048 Uiso 1 1 calc R . . H17B H 0.8440 0.1781 0.1395 0.048 Uiso 1 1 calc R . . C18 C 0.8564(6) 0.1037(3) 0.2052(2) 0.0444(14) Uani 1 1 d . . . H18A H 0.9583 0.0853 0.2004 0.053 Uiso 1 1 calc R . . H18B H 0.7773 0.0641 0.1700 0.053 Uiso 1 1 calc R . . C19 C 1.2299(7) 0.5642(3) 0.7844(2) 0.0699(19) Uani 1 1 d . . . H19A H 1.3131 0.5998 0.8207 0.084 Uiso 1 1 calc R . . H19B H 1.1335 0.5904 0.7866 0.084 Uiso 1 1 calc R . . C20 C 1.2139(9) 0.4912(4) 0.8024(3) 0.103(3) Uani 1 1 d . . . H20A H 1.1870 0.5056 0.8480 0.124 Uiso 1 1 calc R . . H20B H 1.3179 0.4721 0.8099 0.124 Uiso 1 1 calc R . . C21 C 0.5024(5) 0.3133(3) 0.4721(2) 0.0399(13) Uani 1 1 d . . . C22 C 0.5424(5) 0.3602(3) 0.5413(2) 0.0382(13) Uani 1 1 d . . . C23 C 0.4670(5) 0.2586(3) 0.3370(2) 0.0359(12) Uani 1 1 d . . . C24 C 0.3982(5) 0.1987(3) 0.3561(2) 0.0382(13) Uani 1 1 d . . . C25 C 0.6573(6) 0.4712(3) 0.6577(2) 0.0395(13) Uani 1 1 d . . . C26 C 0.5945(6) 0.4104(3) 0.6775(2) 0.0372(13) Uani 1 1 d . . . C27 C 0.4452(6) 0.1494(3) 0.2092(2) 0.0562(16) Uani 1 1 d . . . H27A H 0.4418 0.1405 0.1593 0.067 Uiso 1 1 calc R . . H27B H 0.5331 0.1226 0.2288 0.067 Uiso 1 1 calc R . . C28 C 0.2993(6) 0.1099(3) 0.2162(2) 0.0505(15) Uani 1 1 d . . . H28A H 0.2801 0.0548 0.1844 0.061 Uiso 1 1 calc R . . H28B H 0.2124 0.1404 0.2015 0.061 Uiso 1 1 calc R . . C29 C 0.7125(6) 0.5687(3) 0.7952(2) 0.0542(15) Uani 1 1 d . . . H29A H 0.7821 0.6121 0.8313 0.065 Uiso 1 1 calc R . . H29B H 0.6056 0.5828 0.7943 0.065 Uiso 1 1 calc R . . C30 C 0.7304(6) 0.4913(3) 0.8152(2) 0.0520(15) Uani 1 1 d . . . H30A H 0.7224 0.5015 0.8640 0.062 Uiso 1 1 calc R . . H30B H 0.8356 0.4761 0.8132 0.062 Uiso 1 1 calc R . . C31 C 0.3787(7) 0.2346(3) 0.0498(3) 0.0450(14) Uani 1 1 d . . . C32 C 0.2927(7) 0.2560(3) -0.0178(2) 0.0388(13) Uani 1 1 d . . . C33 C 0.8793(6) 0.3043(3) 0.0507(2) 0.0383(13) Uani 1 1 d . . . C34 C 0.7944(6) 0.2356(3) -0.0164(2) 0.0366(13) Uani 1 1 d . . . C35 C 0.4821(5) 0.5049(3) 0.0377(2) 0.0366(13) Uani 1 1 d . . . C36 C -0.0129(6) 0.0156(3) 0.0381(2) 0.0385(13) Uani 1 1 d . . . O13 O 0.3721(7) -0.0433(3) 0.1013(3) 0.150(2) Uani 1 1 d . . . C37 C 0.4552(16) -0.0387(7) 0.0487(6) 0.224(7) Uani 1 1 d . . . O14 O -0.1320(9) -0.3889(4) 0.1034(4) 0.100(4) Uani 0.719(15) 1 d P . . O14A O 0.064(5) -0.3886(15) 0.0805(14) 0.178(16) Uani 0.281(15) 1 d P . . C38 C -0.0634(15) -0.4220(7) 0.0492(6) 0.122(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0454(4) 0.0418(4) 0.0374(4) 0.0022(3) 0.0059(3) 0.0062(3) Cu2 0.0498(5) 0.0449(4) 0.0380(4) 0.0141(3) 0.0078(3) 0.0023(3) S1 0.0800(11) 0.0455(8) 0.0302(7) 0.0057(6) 0.0031(7) 0.0153(8) S2 0.0694(10) 0.0407(8) 0.0290(7) 0.0041(6) 0.0048(7) 0.0100(7) S3 0.0737(11) 0.0416(8) 0.0271(7) 0.0028(6) 0.0046(7) 0.0088(7) S4 0.0746(11) 0.0444(8) 0.0299(7) 0.0062(6) 0.0067(7) 0.0106(7) S5 0.0845(12) 0.0396(8) 0.0355(7) 0.0017(6) 0.0097(7) 0.0122(8) S6 0.0647(10) 0.0452(8) 0.0309(7) 0.0050(6) -0.0015(7) 0.0028(7) S7 0.0625(10) 0.0447(8) 0.0301(7) 0.0025(6) -0.0029(7) 0.0011(7) S8 0.0800(12) 0.0406(8) 0.0361(7) 0.0028(6) 0.0140(7) 0.0124(8) S9 0.0746(11) 0.0399(8) 0.0293(7) 0.0039(6) 0.0095(7) -0.0077(7) S10 0.0693(10) 0.0431(8) 0.0295(7) 0.0033(6) 0.0121(7) -0.0097(7) S11 0.0722(11) 0.0444(8) 0.0292(7) 0.0069(6) 0.0088(7) -0.0091(7) S12 0.0687(10) 0.0402(8) 0.0292(7) 0.0026(6) 0.0094(7) -0.0085(7) S13 0.0688(11) 0.0456(8) 0.0297(7) 0.0050(6) 0.0127(7) -0.0074(7) S14 0.0571(10) 0.0374(8) 0.0313(7) 0.0041(6) 0.0071(6) -0.0022(7) S15 0.0709(11) 0.0437(8) 0.0339(7) 0.0029(6) 0.0058(7) -0.0156(7) S16 0.0721(11) 0.0378(8) 0.0298(7) 0.0040(6) 0.0149(7) -0.0004(7) S17 0.0678(11) 0.0451(8) 0.0316(7) 0.0093(6) 0.0096(7) -0.0090(7) S18 0.0682(10) 0.0461(8) 0.0334(7) 0.0088(6) 0.0112(7) -0.0099(7) S19 0.0664(10) 0.0449(8) 0.0326(7) 0.0104(6) 0.0091(7) -0.0077(7) S20 0.0650(10) 0.0432(8) 0.0321(7) 0.0083(6) 0.0101(7) -0.0075(7) S21 0.0712(11) 0.0433(8) 0.0329(7) 0.0077(6) 0.0169(7) 0.0006(7) S22 0.0626(10) 0.0469(8) 0.0387(8) 0.0031(6) 0.0104(7) -0.0127(7) S23 0.0820(12) 0.0421(8) 0.0345(8) 0.0067(6) 0.0070(7) -0.0137(8) S24 0.0739(11) 0.0404(8) 0.0326(7) 0.0087(6) 0.0186(7) 0.0017(7) O1 0.042(3) 0.072(3) 0.067(2) 0.022(2) -0.005(2) -0.007(2) O2 0.046(2) 0.047(2) 0.043(2) 0.0125(17) 0.0083(17) -0.0020(18) O3 0.048(3) 0.070(3) 0.061(2) 0.037(2) -0.0048(19) -0.002(2) O4 0.043(2) 0.061(2) 0.042(2) 0.0223(17) 0.0004(18) -0.0062(19) O5 0.044(2) 0.043(2) 0.044(2) -0.0072(17) 0.0080(17) 0.0025(18) O6 0.045(2) 0.056(2) 0.0387(19) -0.0067(17) -0.0019(17) 0.0131(19) O7 0.042(2) 0.071(2) 0.043(2) 0.0043(18) -0.0069(18) 0.007(2) O8 0.047(2) 0.034(2) 0.054(2) -0.0053(17) 0.0104(17) 0.0082(18) O9 0.059(2) 0.038(2) 0.0358(18) 0.0139(16) 0.0158(16) 0.0132(18) O10 0.066(3) 0.037(2) 0.049(2) 0.0106(17) 0.0303(18) 0.0118(19) O11 0.061(2) 0.0309(19) 0.0369(19) 0.0043(16) 0.0201(16) 0.0030(17) O12 0.077(3) 0.038(2) 0.046(2) 0.0099(17) 0.0317(19) 0.0045(19) C1 0.050(4) 0.043(3) 0.033(3) 0.005(2) 0.011(2) 0.000(3) C2 0.049(4) 0.041(3) 0.030(3) 0.007(2) 0.008(2) 0.002(3) C3 0.046(3) 0.038(3) 0.026(3) 0.003(2) 0.003(2) 0.003(3) C4 0.042(3) 0.039(3) 0.022(2) 0.004(2) 0.004(2) 0.000(3) C5 0.053(4) 0.038(3) 0.022(3) 0.000(2) 0.007(2) -0.004(3) C6 0.051(4) 0.037(3) 0.031(3) 0.002(2) 0.013(2) -0.002(3) C7 0.110(5) 0.045(4) 0.039(3) -0.004(3) 0.004(3) 0.002(4) C8 0.085(5) 0.078(4) 0.028(3) 0.000(3) 0.007(3) 0.015(4) C9 0.062(4) 0.061(4) 0.035(3) 0.003(3) 0.004(3) 0.005(3) C10 0.098(5) 0.041(3) 0.030(3) 0.001(3) 0.012(3) -0.007(3) C11 0.051(4) 0.041(3) 0.031(3) 0.008(2) 0.010(2) 0.001(3) C12 0.055(4) 0.034(3) 0.023(3) 0.000(2) 0.007(2) 0.000(2) C13 0.044(3) 0.039(3) 0.027(3) 0.005(2) 0.007(2) 0.004(3) C14 0.039(3) 0.038(3) 0.027(3) 0.003(2) 0.006(2) 0.004(3) C15 0.050(4) 0.038(3) 0.025(3) 0.003(2) 0.010(2) 0.001(3) C16 0.046(3) 0.036(3) 0.023(3) -0.001(2) 0.001(2) 0.003(3) C17 0.047(3) 0.049(3) 0.025(3) 0.013(2) 0.008(2) 0.010(3) C18 0.049(4) 0.046(3) 0.032(3) 0.001(2) 0.009(2) -0.010(3) C19 0.127(6) 0.046(4) 0.028(3) 0.001(3) 0.014(3) -0.013(4) C20 0.179(8) 0.077(5) 0.036(3) -0.004(3) 0.024(4) -0.063(5) C21 0.049(3) 0.040(3) 0.032(3) 0.011(2) 0.010(2) 0.003(3) C22 0.039(3) 0.043(3) 0.031(3) 0.012(2) 0.004(2) 0.000(2) C23 0.035(3) 0.041(3) 0.029(3) 0.011(2) 0.003(2) 0.003(2) C24 0.040(3) 0.043(3) 0.032(3) 0.008(2) 0.011(2) 0.003(3) C25 0.043(3) 0.038(3) 0.035(3) 0.006(2) 0.007(2) 0.006(3) C26 0.053(4) 0.033(3) 0.026(3) 0.008(2) 0.010(2) 0.008(3) C27 0.070(5) 0.062(4) 0.033(3) 0.006(3) 0.011(3) 0.012(3) C28 0.044(4) 0.061(4) 0.039(3) 0.007(3) 0.002(3) -0.002(3) C29 0.071(4) 0.044(3) 0.038(3) 0.000(3) 0.009(3) -0.009(3) C30 0.051(4) 0.070(4) 0.031(3) 0.009(3) 0.008(3) 0.002(3) C31 0.045(4) 0.045(4) 0.044(3) 0.014(3) 0.005(3) 0.006(3) C32 0.039(4) 0.039(3) 0.040(3) 0.010(3) 0.013(3) 0.011(3) C33 0.044(4) 0.040(3) 0.029(3) 0.007(3) 0.010(3) -0.003(3) C34 0.033(4) 0.043(3) 0.034(3) 0.008(3) 0.010(3) -0.005(3) C35 0.028(3) 0.039(3) 0.035(3) 0.002(3) 0.002(2) -0.008(3) C36 0.038(3) 0.045(4) 0.040(3) 0.016(3) 0.016(3) 0.007(3) O13 0.154(5) 0.082(4) 0.144(5) -0.023(3) -0.046(4) 0.013(3) C37 0.358(19) 0.196(11) 0.175(10) 0.065(8) 0.168(11) -0.006(10) O14 0.135(7) 0.097(6) 0.075(6) 0.044(4) 0.012(4) 0.014(4) O14A 0.32(5) 0.12(2) 0.11(2) 0.003(15) 0.11(2) 0.06(2) C38 0.119(9) 0.125(9) 0.114(9) 0.015(7) 0.032(7) 0.033(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O9 1.949(3) . ? Cu1 O6 1.970(3) . ? Cu1 O5 1.995(3) . ? Cu1 O2 2.018(3) . ? Cu1 O10 2.243(3) . ? Cu1 O1 2.423(4) . ? Cu2 O11 1.949(3) . ? Cu2 O4 1.959(3) . ? Cu2 O3 1.977(3) . ? Cu2 O8 2.000(3) 1_455 ? Cu2 O12 2.267(3) . ? Cu2 O7 2.458(3) 1_455 ? S1 C1 1.734(5) . ? S1 C3 1.756(4) . ? S2 C1 1.734(5) . ? S2 C4 1.745(4) . ? S3 C2 1.737(4) . ? S3 C5 1.747(4) . ? S4 C2 1.734(4) . ? S4 C6 1.746(4) . ? S5 C3 1.739(4) . ? S5 C7 1.813(5) . ? S6 C4 1.745(4) . ? S6 C8 1.766(5) . ? S7 C5 1.750(4) . ? S7 C9 1.786(5) . ? S8 C6 1.749(4) . ? S8 C10 1.803(4) . ? S9 C11 1.736(5) . ? S9 C13 1.747(4) . ? S10 C11 1.730(5) . ? S10 C14 1.746(4) . ? S11 C12 1.728(4) . ? S11 C15 1.741(4) . ? S12 C12 1.732(5) . ? S12 C16 1.753(4) . ? S13 C13 1.748(5) . ? S13 C17 1.803(4) . ? S14 C14 1.741(4) . ? S14 C18 1.819(4) . ? S15 C15 1.741(4) . ? S15 C19 1.798(5) . ? S16 C20 1.746(5) . ? S16 C16 1.748(5) . ? S17 C21 1.729(5) . ? S17 C23 1.749(4) . ? S18 C21 1.730(5) . ? S18 C24 1.753(4) . ? S19 C22 1.726(4) . ? S19 C25 1.744(4) . ? S20 C22 1.736(5) . ? S20 C26 1.759(4) . ? S21 C23 1.746(5) . ? S21 C27 1.810(5) . ? S22 C24 1.742(5) . ? S22 C28 1.801(5) . ? S23 C25 1.739(5) . ? S23 C29 1.812(5) . ? S24 C26 1.747(4) . ? S24 C30 1.799(5) . ? O1 C31 1.231(6) . ? O2 C32 1.259(5) . ? O3 C31 1.268(6) . ? O4 C32 1.256(5) . ? O5 C33 1.260(5) . ? O6 C34 1.260(5) . ? O7 C33 1.231(5) . ? O8 C34 1.246(5) . ? O8 Cu2 2.000(3) 1_655 ? O9 C35 1.274(5) . ? O10 C35 1.239(5) 2_665 ? O11 C36 1.266(5) . ? O12 C36 1.245(5) 2 ? C1 C2 1.366(5) . ? C3 C4 1.345(6) . ? C5 C6 1.339(6) . ? C7 C8 1.462(6) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.496(6) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.371(5) . ? C13 C14 1.345(6) . ? C15 C16 1.339(6) . ? C17 C18 1.510(6) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.387(6) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.376(5) . ? C23 C24 1.342(6) . ? C25 C26 1.339(6) . ? C27 C28 1.472(6) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.471(6) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.546(7) . ? C33 C34 1.557(6) . ? C35 O10 1.239(5) 2_665 ? C35 C35 1.583(9) 2_665 ? C36 O12 1.245(5) 2 ? C36 C36 1.556(9) 2 ? O13 C37 1.424(10) . ? O14 C38 1.359(12) . ? O14A C38 1.20(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O9 Cu1 O6 178.60(13) . . ? O9 Cu1 O5 96.05(13) . . ? O6 Cu1 O5 82.91(13) . . ? O9 Cu1 O2 91.46(13) . . ? O6 Cu1 O2 89.34(13) . . ? O5 Cu1 O2 165.39(14) . . ? O9 Cu1 O10 80.02(12) . . ? O6 Cu1 O10 101.14(13) . . ? O5 Cu1 O10 104.98(13) . . ? O2 Cu1 O10 88.62(13) . . ? O9 Cu1 O1 90.32(13) . . ? O6 Cu1 O1 88.75(13) . . ? O5 Cu1 O1 90.73(13) . . ? O2 Cu1 O1 76.69(13) . . ? O10 Cu1 O1 162.26(12) . . ? O11 Cu2 O4 174.45(13) . . ? O11 Cu2 O3 94.27(14) . . ? O4 Cu2 O3 83.15(15) . . ? O11 Cu2 O8 94.12(13) . 1_455 ? O4 Cu2 O8 89.47(14) . 1_455 ? O3 Cu2 O8 165.05(14) . 1_455 ? O11 Cu2 O12 79.77(11) . . ? O4 Cu2 O12 96.18(13) . . ? O3 Cu2 O12 106.03(13) . . ? O8 Cu2 O12 87.63(12) 1_455 . ? C1 S1 C3 95.3(2) . . ? C1 S2 C4 95.6(2) . . ? C2 S3 C5 95.5(2) . . ? C2 S4 C6 95.3(2) . . ? C3 S5 C7 101.1(2) . . ? C4 S6 C8 101.4(2) . . ? C5 S7 C9 101.6(2) . . ? C6 S8 C10 100.8(2) . . ? C11 S9 C13 95.7(2) . . ? C11 S10 C14 95.4(2) . . ? C12 S11 C15 95.2(2) . . ? C12 S12 C16 95.0(2) . . ? C13 S13 C17 99.9(2) . . ? C14 S14 C18 102.9(2) . . ? C15 S15 C19 101.7(2) . . ? C20 S16 C16 100.8(3) . . ? C21 S17 C23 95.9(2) . . ? C21 S18 C24 95.6(2) . . ? C22 S19 C25 95.6(2) . . ? C22 S20 C26 95.3(2) . . ? C23 S21 C27 99.4(2) . . ? C24 S22 C28 102.2(2) . . ? C25 S23 C29 102.1(2) . . ? C26 S24 C30 100.9(2) . . ? C31 O1 Cu1 106.1(3) . . ? C32 O2 Cu1 118.1(3) . . ? C31 O3 Cu2 113.1(3) . . ? C32 O4 Cu2 112.8(3) . . ? C33 O5 Cu1 111.9(3) . . ? C34 O6 Cu1 112.3(3) . . ? C34 O8 Cu2 120.1(3) . 1_655 ? C35 O9 Cu1 117.9(3) . . ? C35 O10 Cu1 108.8(3) 2_665 . ? C36 O11 Cu2 117.3(3) . . ? C36 O12 Cu2 107.8(3) 2 . ? C2 C1 S1 122.8(4) . . ? C2 C1 S2 122.0(4) . . ? S1 C1 S2 115.2(2) . . ? C1 C2 S4 123.1(4) . . ? C1 C2 S3 121.9(4) . . ? S4 C2 S3 115.0(2) . . ? C4 C3 S5 130.3(3) . . ? C4 C3 S1 116.8(3) . . ? S5 C3 S1 112.9(3) . . ? C3 C4 S6 126.7(3) . . ? C3 C4 S2 117.0(3) . . ? S6 C4 S2 116.3(3) . . ? C6 C5 S3 116.7(3) . . ? C6 C5 S7 128.2(3) . . ? S3 C5 S7 115.1(3) . . ? C5 C6 S4 117.4(3) . . ? C5 C6 S8 129.1(3) . . ? S4 C6 S8 113.5(3) . . ? C8 C7 S5 115.4(3) . . ? C8 C7 H7A 108.4 . . ? S5 C7 H7A 108.4 . . ? C8 C7 H7B 108.4 . . ? S5 C7 H7B 108.4 . . ? H7A C7 H7B 107.5 . . ? C7 C8 S6 116.9(4) . . ? C7 C8 H8A 108.1 . . ? S6 C8 H8A 108.1 . . ? C7 C8 H8B 108.1 . . ? S6 C8 H8B 108.1 . . ? H8A C8 H8B 107.3 . . ? C10 C9 S7 114.9(4) . . ? C10 C9 H9A 108.6 . . ? S7 C9 H9A 108.6 . . ? C10 C9 H9B 108.6 . . ? S7 C9 H9B 108.6 . . ? H9A C9 H9B 107.5 . . ? C9 C10 S8 115.2(3) . . ? C9 C10 H10A 108.5 . . ? S8 C10 H10A 108.5 . . ? C9 C10 H10B 108.5 . . ? S8 C10 H10B 108.5 . . ? H10A C10 H10B 107.5 . . ? C12 C11 S10 123.2(4) . . ? C12 C11 S9 121.8(4) . . ? S10 C11 S9 115.0(2) . . ? C11 C12 S11 122.3(4) . . ? C11 C12 S12 122.2(4) . . ? S11 C12 S12 115.4(2) . . ? C14 C13 S9 116.4(3) . . ? C14 C13 S13 127.4(3) . . ? S9 C13 S13 116.2(3) . . ? C13 C14 S14 129.3(3) . . ? C13 C14 S10 117.3(3) . . ? S14 C14 S10 113.3(3) . . ? C16 C15 S11 117.3(3) . . ? C16 C15 S15 128.8(3) . . ? S11 C15 S15 113.8(3) . . ? C15 C16 S16 128.6(3) . . ? C15 C16 S12 116.7(3) . . ? S16 C16 S12 114.7(3) . . ? C18 C17 S13 113.5(3) . . ? C18 C17 H17A 108.9 . . ? S13 C17 H17A 108.9 . . ? C18 C17 H17B 108.9 . . ? S13 C17 H17B 108.9 . . ? H17A C17 H17B 107.7 . . ? C17 C18 S14 115.2(3) . . ? C17 C18 H18A 108.5 . . ? S14 C18 H18A 108.5 . . ? C17 C18 H18B 108.5 . . ? S14 C18 H18B 108.5 . . ? H18A C18 H18B 107.5 . . ? C20 C19 S15 119.0(4) . . ? C20 C19 H19A 107.6 . . ? S15 C19 H19A 107.6 . . ? C20 C19 H19B 107.6 . . ? S15 C19 H19B 107.6 . . ? H19A C19 H19B 107.0 . . ? C19 C20 S16 124.4(5) . . ? C19 C20 H20A 106.2 . . ? S16 C20 H20A 106.2 . . ? C19 C20 H20B 106.2 . . ? S16 C20 H20B 106.2 . . ? H20A C20 H20B 106.4 . . ? C22 C21 S17 122.2(4) . . ? C22 C21 S18 122.8(4) . . ? S17 C21 S18 115.0(2) . . ? C21 C22 S19 123.0(4) . . ? C21 C22 S20 121.8(3) . . ? S19 C22 S20 115.1(2) . . ? C24 C23 S21 127.2(3) . . ? C24 C23 S17 116.6(3) . . ? S21 C23 S17 116.2(3) . . ? C23 C24 S22 129.8(3) . . ? C23 C24 S18 116.8(3) . . ? S22 C24 S18 113.4(3) . . ? C26 C25 S23 128.6(3) . . ? C26 C25 S19 117.5(3) . . ? S23 C25 S19 113.9(3) . . ? C25 C26 S24 128.7(3) . . ? C25 C26 S20 116.2(3) . . ? S24 C26 S20 115.1(3) . . ? C28 C27 S21 115.0(4) . . ? C28 C27 H27A 108.5 . . ? S21 C27 H27A 108.5 . . ? C28 C27 H27B 108.5 . . ? S21 C27 H27B 108.5 . . ? H27A C27 H27B 107.5 . . ? C27 C28 S22 114.0(3) . . ? C27 C28 H28A 108.8 . . ? S22 C28 H28A 108.8 . . ? C27 C28 H28B 108.8 . . ? S22 C28 H28B 108.8 . . ? H28A C28 H28B 107.6 . . ? C30 C29 S23 114.1(3) . . ? C30 C29 H29A 108.7 . . ? S23 C29 H29A 108.7 . . ? C30 C29 H29B 108.7 . . ? S23 C29 H29B 108.7 . . ? H29A C29 H29B 107.6 . . ? C29 C30 S24 116.7(3) . . ? C29 C30 H30A 108.1 . . ? S24 C30 H30A 108.1 . . ? C29 C30 H30B 108.1 . . ? S24 C30 H30B 108.1 . . ? H30A C30 H30B 107.3 . . ? O1 C31 O3 127.0(5) . . ? O1 C31 C32 119.3(5) . . ? O3 C31 C32 113.7(5) . . ? O4 C32 O2 124.1(5) . . ? O4 C32 C31 116.2(5) . . ? O2 C32 C31 119.6(5) . . ? O7 C33 O5 128.3(4) . . ? O7 C33 C34 117.1(5) . . ? O5 C33 C34 114.6(4) . . ? O8 C34 O6 124.8(4) . . ? O8 C34 C33 119.7(5) . . ? O6 C34 C33 115.5(4) . . ? O10 C35 O9 127.0(4) 2_665 . ? O10 C35 C35 117.2(6) 2_665 2_665 ? O9 C35 C35 115.8(6) . 2_665 ? O12 C36 O11 125.0(4) 2 . ? O12 C36 C36 117.5(6) 2 2 ? O11 C36 C36 117.4(6) . 2 ? O14A C38 O14 93.8(16) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.727 _refine_diff_density_min -0.566 _refine_diff_density_rms 0.079