# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name 'In-Hyeok Park' 'Shim Sung Lee' _publ_contact_author_name 'In-Hyeok Park' _publ_contact_author_email pihghost@nate.com data_1 _database_code_depnum_ccdc_archive 'CCDC 822020' #TrackingRef '- DT18C6CuR-F.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H32 Cu2 N2 O16 S2, C12 H24 O6 S2, 2(N O3), 2(H2 O)' _chemical_formula_sum 'C24 H60 Cu2 N4 O30 S4' _chemical_formula_weight 1140.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 _symmetry_space_group_name_Hall '-p 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.0680(3) _cell_length_b 11.0147(7) _cell_length_c 20.8655(13) _cell_angle_alpha 81.306(3) _cell_angle_beta 89.114(3) _cell_angle_gamma 80.325(3) _cell_volume 1134.95(12) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9970 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 28.27 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.668 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 594 _exptl_absorpt_coefficient_mu 1.221 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7340 _exptl_absorpt_correction_T_max 0.8193 _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 31255 _diffrn_reflns_av_R_equivalents 0.0581 _diffrn_reflns_av_sigmaI/netI 0.0314 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 0.99 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4446 _reflns_number_gt 3995 _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^)+(0.0786P)^2^+1.7594P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4446 _refine_ls_number_parameters 313 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0563 _refine_ls_R_factor_gt 0.0515 _refine_ls_wR_factor_ref 0.1380 _refine_ls_wR_factor_gt 0.1338 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _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 1.20478(8) 1.01674(4) 0.254405(18) 0.02344(15) Uani 1 1 d . . . S1 S 1.28094(17) 1.01598(8) 0.40772(4) 0.0259(2) Uani 1 1 d . . . S2 S 1.24499(18) 1.40217(8) 0.08848(4) 0.0292(2) Uani 1 1 d . . . N1 N 1.6770(5) 1.0220(3) 0.18822(14) 0.0248(6) Uani 1 1 d . . . N2 N 0.8065(7) 0.6291(3) 0.29123(16) 0.0365(7) Uani 1 1 d . . . O1 O 1.1315(5) 1.2640(3) 0.44840(12) 0.0350(6) Uani 1 1 d . . . O2 O 1.3254(5) 0.7571(3) 0.47624(12) 0.0347(6) Uani 1 1 d . . . O3 O 1.1133(5) 1.0138(2) 0.34805(11) 0.0263(5) Uani 1 1 d . . . O4 O 1.3315(5) 1.2510(2) -0.01948(12) 0.0354(6) Uani 1 1 d . . . O5 O 1.7597(6) 1.3260(2) -0.08790(12) 0.0361(6) Uani 1 1 d . . . O6 O 1.3965(5) 1.3272(2) 0.14781(12) 0.0321(6) Uani 1 1 d . . . O1W O 1.1545(6) 1.1947(3) 0.24043(13) 0.0314(6) Uani 1 1 d . . . H1WA H 1.028(11) 1.230(5) 0.245(3) 0.044(16) Uiso 1 1 d . . . H1WB H 1.251(15) 1.237(7) 0.203(4) 0.11(2) Uiso 1 1 d . . . O2W O 1.2352(7) 0.8395(3) 0.25932(14) 0.0349(6) Uani 1 1 d . . . H2WA H 1.365(12) 0.799(5) 0.265(3) 0.050(17) Uiso 1 1 d . . . H2WB H 1.118(12) 0.802(5) 0.272(3) 0.058(17) Uiso 1 1 d . . . O3W O 0.6970(6) 1.3353(3) 0.26034(17) 0.0386(6) Uani 1 1 d . . . H3WA H 0.608(11) 1.344(5) 0.230(3) 0.055(17) Uiso 1 1 d . . . H3WB H 0.692(10) 1.399(5) 0.269(2) 0.047(15) Uiso 1 1 d . . . O7 O 1.4344(4) 1.0155(2) 0.17526(11) 0.0279(5) Uani 1 1 d . . . O8 O 1.7369(5) 1.0257(2) 0.24625(11) 0.0278(5) Uani 1 1 d . . . O9 O 1.8418(5) 1.0249(3) 0.14484(13) 0.0388(6) Uani 1 1 d . . . O10 O 1.0119(7) 0.5630(4) 0.3098(2) 0.0780(13) Uani 1 1 d . . . O11 O 0.6073(8) 0.5843(4) 0.2800(3) 0.0861(14) Uani 1 1 d . . . O12 O 0.7834(7) 0.7451(3) 0.28179(18) 0.0574(9) Uani 1 1 d . . . C1 C 0.9201(8) 1.3635(3) 0.4499(2) 0.0381(9) Uani 1 1 d . . . H1A H 0.7849 1.3628 0.4163 0.046 Uiso 1 1 calc R . . H1B H 0.9879 1.4436 0.4410 0.046 Uiso 1 1 calc R . . C2 C 1.2583(8) 1.2654(4) 0.38759(17) 0.0348(8) Uani 1 1 d . . . H2A H 1.3524 1.3379 0.3786 0.042 Uiso 1 1 calc R . . H2B H 1.1237 1.2719 0.3528 0.042 Uiso 1 1 calc R . . C3 C 1.4545(8) 1.1465(4) 0.38975(17) 0.0324(8) Uani 1 1 d . . . H3A H 1.5926 1.1420 0.4235 0.039 Uiso 1 1 calc R . . H3B H 1.5448 1.1444 0.3474 0.039 Uiso 1 1 calc R . . C4 C 1.5623(7) 0.8930(4) 0.40842(17) 0.0322(8) Uani 1 1 d . . . H4A H 1.6602 0.9043 0.3671 0.039 Uiso 1 1 calc R . . H4B H 1.6864 0.8952 0.4443 0.039 Uiso 1 1 calc R . . C5 C 1.4662(8) 0.7698(4) 0.41722(18) 0.0344(8) Uani 1 1 d . . . H5A H 1.3472 0.7662 0.3806 0.041 Uiso 1 1 calc R . . H5B H 1.6205 0.7012 0.4183 0.041 Uiso 1 1 calc R . . C6 C 1.2038(8) 0.6497(3) 0.4846(2) 0.0379(9) Uani 1 1 d . . . H6A H 1.3394 0.5752 0.4808 0.045 Uiso 1 1 calc R . . H6B H 1.0650 0.6572 0.4507 0.045 Uiso 1 1 calc R . . C7 C 0.9900(8) 1.5129(3) 0.11839(18) 0.0356(8) Uani 1 1 d . . . H7A H 0.8584 1.5506 0.0834 0.043 Uiso 1 1 calc R . . H7B H 0.8945 1.4702 0.1545 0.043 Uiso 1 1 calc R . . C8 C 1.0337(8) 1.3014(4) 0.06330(18) 0.0355(8) Uani 1 1 d . . . H8A H 0.9332 1.2670 0.1009 0.043 Uiso 1 1 calc R . . H8B H 0.9030 1.3492 0.0302 0.043 Uiso 1 1 calc R . . C9 C 1.2047(8) 1.1973(4) 0.03566(17) 0.0354(8) Uani 1 1 d . . . H9A H 1.3400 1.1510 0.0681 0.043 Uiso 1 1 calc R . . H9B H 1.0929 1.1387 0.0235 0.043 Uiso 1 1 calc R . . C10 C 1.5213(8) 1.1643(3) -0.04582(19) 0.0357(8) Uani 1 1 d . . . H10A H 1.4343 1.0965 -0.0575 0.043 Uiso 1 1 calc R . . H10B H 1.6635 1.1271 -0.0133 0.043 Uiso 1 1 calc R . . C11 C 1.6415(8) 1.2277(4) -0.1048(2) 0.0382(9) Uani 1 1 d . . . H11A H 1.7787 1.1672 -0.1228 0.046 Uiso 1 1 calc R . . H11B H 1.5010 1.2609 -0.1383 0.046 Uiso 1 1 calc R . . C12 C 1.8863(9) 1.3872(4) -0.14170(18) 0.0388(9) Uani 1 1 d . . . H12A H 1.7533 1.4242 -0.1765 0.047 Uiso 1 1 calc R . . H12B H 2.0257 1.3271 -0.1593 0.047 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 0.0214(2) 0.0279(2) 0.0216(2) -0.00181(16) 0.00423(16) -0.00781(16) S1 0.0242(4) 0.0343(4) 0.0204(4) -0.0029(3) 0.0052(3) -0.0099(3) S2 0.0286(5) 0.0303(4) 0.0276(4) 0.0020(3) 0.0094(3) -0.0083(3) N1 0.0191(14) 0.0255(14) 0.0299(15) -0.0024(11) 0.0016(11) -0.0052(11) N2 0.0336(18) 0.0332(17) 0.0420(18) -0.0033(14) 0.0120(14) -0.0070(14) O1 0.0310(14) 0.0447(15) 0.0266(12) -0.0021(11) 0.0029(10) -0.0014(11) O2 0.0353(15) 0.0432(15) 0.0285(13) -0.0032(11) 0.0039(11) -0.0169(12) O3 0.0220(12) 0.0352(13) 0.0223(11) -0.0017(9) 0.0042(9) -0.0091(10) O4 0.0407(15) 0.0314(13) 0.0305(13) 0.0043(10) 0.0069(11) -0.0039(11) O5 0.0434(16) 0.0402(15) 0.0276(13) -0.0063(11) 0.0080(11) -0.0150(12) O6 0.0284(13) 0.0318(13) 0.0353(13) 0.0000(10) 0.0011(10) -0.0070(10) O1W 0.0307(16) 0.0293(13) 0.0328(14) 0.0004(11) 0.0070(11) -0.0058(12) O2W 0.0357(17) 0.0280(14) 0.0398(15) -0.0033(11) 0.0040(13) -0.0036(14) O3W 0.0346(16) 0.0355(16) 0.0470(18) -0.0074(13) -0.0003(13) -0.0080(12) O7 0.0156(11) 0.0436(14) 0.0264(12) -0.0051(10) 0.0025(9) -0.0111(10) O8 0.0232(12) 0.0337(13) 0.0262(12) -0.0037(10) -0.0033(10) -0.0046(10) O9 0.0222(13) 0.0565(17) 0.0397(15) -0.0082(12) 0.0165(11) -0.0126(12) O10 0.044(2) 0.062(2) 0.111(3) 0.031(2) -0.006(2) 0.0002(17) O11 0.048(2) 0.074(3) 0.149(4) -0.047(3) -0.001(2) -0.0193(19) O12 0.054(2) 0.0338(16) 0.085(2) -0.0095(15) 0.0266(18) -0.0093(14) C1 0.039(2) 0.0292(19) 0.045(2) 0.0027(16) 0.0062(17) -0.0096(16) C2 0.040(2) 0.040(2) 0.0271(17) -0.0053(15) 0.0053(15) -0.0172(17) C3 0.035(2) 0.041(2) 0.0274(17) -0.0077(15) 0.0065(15) -0.0210(16) C4 0.0251(18) 0.043(2) 0.0263(17) 0.0010(15) 0.0019(14) -0.0040(15) C5 0.032(2) 0.039(2) 0.0293(18) -0.0024(15) 0.0035(15) -0.0007(16) C6 0.036(2) 0.0260(18) 0.050(2) -0.0046(16) 0.0062(18) -0.0017(15) C7 0.033(2) 0.0343(19) 0.0338(19) 0.0071(15) 0.0122(15) -0.0019(15) C8 0.034(2) 0.047(2) 0.0265(17) 0.0029(15) 0.0022(15) -0.0178(17) C9 0.047(2) 0.037(2) 0.0248(17) 0.0025(14) -0.0010(16) -0.0187(17) C10 0.039(2) 0.0277(18) 0.043(2) -0.0081(15) -0.0005(17) -0.0084(15) C11 0.039(2) 0.039(2) 0.040(2) -0.0167(17) 0.0052(17) -0.0062(17) C12 0.043(2) 0.041(2) 0.0303(19) -0.0012(16) 0.0105(16) -0.0033(17) _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 O1W 1.912(3) . ? Cu1 O2W 1.919(3) . ? Cu1 O3 1.998(2) . ? Cu1 O7 2.006(2) . ? Cu1 O8 2.364(2) 1_455 ? S1 O3 1.524(2) . ? S1 C4 1.793(4) . ? S1 C3 1.798(4) . ? S2 O6 1.520(3) . ? S2 C7 1.795(4) . ? S2 C8 1.803(4) . ? N1 O9 1.223(4) . ? N1 O8 1.261(4) . ? N1 O7 1.279(4) . ? N2 O10 1.198(5) . ? N2 O11 1.235(5) . ? N2 O12 1.249(4) . ? O1 C1 1.402(5) . ? O1 C2 1.413(4) . ? O2 C6 1.411(5) . ? O2 C5 1.414(4) . ? O4 C10 1.404(5) . ? O4 C9 1.409(4) . ? O5 C11 1.413(5) . ? O5 C12 1.422(4) . ? O8 Cu1 2.364(2) 1_655 ? C1 C6 1.492(6) 2_776 ? C2 C3 1.500(6) . ? C4 C5 1.502(5) . ? C6 C1 1.492(6) 2_776 ? C7 C12 1.497(6) 2_885 ? C8 C9 1.499(6) . ? C10 C11 1.494(6) . ? C12 C7 1.497(6) 2_885 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1W Cu1 O2W 173.60(12) . . ? O1W Cu1 O3 91.38(11) . . ? O2W Cu1 O3 93.43(11) . . ? O1W Cu1 O7 89.20(12) . . ? O2W Cu1 O7 87.91(12) . . ? O3 Cu1 O7 158.17(10) . . ? O1W Cu1 O8 89.76(11) . 1_455 ? O2W Cu1 O8 86.81(13) . 1_455 ? O3 Cu1 O8 81.12(9) . 1_455 ? O7 Cu1 O8 120.71(9) . 1_455 ? O3 S1 C4 106.63(16) . . ? O3 S1 C3 107.10(15) . . ? C4 S1 C3 98.61(18) . . ? O6 S2 C7 106.11(17) . . ? O6 S2 C8 105.20(16) . . ? C7 S2 C8 98.5(2) . . ? O9 N1 O8 122.2(3) . . ? O9 N1 O7 119.9(3) . . ? O8 N1 O7 117.9(3) . . ? O10 N2 O11 120.8(4) . . ? O10 N2 O12 122.2(4) . . ? O11 N2 O12 117.0(4) . . ? C1 O1 C2 113.4(3) . . ? C6 O2 C5 111.8(3) . . ? S1 O3 Cu1 132.31(14) . . ? C10 O4 C9 113.0(3) . . ? C11 O5 C12 111.9(3) . . ? N1 O7 Cu1 111.71(19) . . ? N1 O8 Cu1 108.82(19) . 1_655 ? O1 C1 C6 108.7(3) . 2_776 ? O1 C2 C3 108.0(3) . . ? C2 C3 S1 109.5(3) . . ? C5 C4 S1 109.4(3) . . ? O2 C5 C4 108.4(3) . . ? O2 C6 C1 108.7(3) . 2_776 ? C12 C7 S2 109.9(3) 2_885 . ? C9 C8 S2 109.1(3) . . ? O4 C9 C8 107.4(3) . . ? O4 C10 C11 109.7(3) . . ? O5 C11 C10 109.3(3) . . ? O5 C12 C7 107.6(3) . 2_885 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.220 _refine_diff_density_min -0.569 _refine_diff_density_rms 0.109 ############################################################ data_2 _database_code_depnum_ccdc_archive 'CCDC 822021' #TrackingRef '6248_web_deposit_cif_file_0_In-HyeokPark_1310473525.DT18C6Cu-R.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H48 Cu4 I4 O8 S4' _chemical_formula_sum 'C24 H48 Cu4 I4 O8 S4' _chemical_formula_weight 1354.62 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P1 _symmetry_space_group_name_Hall 'P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 8.3361(7) _cell_length_b 10.7845(9) _cell_length_c 12.6902(16) _cell_angle_alpha 104.841(5) _cell_angle_beta 104.913(6) _cell_angle_gamma 105.793(4) _cell_volume 993.40(17) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6960 _cell_measurement_theta_min 2.67 _cell_measurement_theta_max 28.24 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.264 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 648 _exptl_absorpt_coefficient_mu 5.469 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3305 _exptl_absorpt_correction_T_max 0.6108 _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 14902 _diffrn_reflns_av_R_equivalents 0.0654 _diffrn_reflns_av_sigmaI/netI 0.0821 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6856 _reflns_number_gt 5923 _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. We used 12 restraint. Due to the disorder, C10 and C11 atoms have large anisotropic displacement parameters. So ISOR command was used in final refinement. ; _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^)+(0.0416P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.07(3) _refine_ls_number_reflns 6856 _refine_ls_number_parameters 422 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0533 _refine_ls_R_factor_gt 0.0402 _refine_ls_wR_factor_ref 0.1051 _refine_ls_wR_factor_gt 0.0906 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.030 _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 0.36247(18) 0.24658(13) 0.32154(13) 0.0360(3) Uani 1 1 d . . . Cu2 Cu 0.55898(18) 0.43463(13) 0.26204(13) 0.0336(3) Uani 1 1 d . . . Cu3 Cu 0.36822(18) 0.18575(13) 0.10064(12) 0.0336(3) Uani 1 1 d . . . Cu4 Cu 0.18070(18) 0.33695(13) 0.16100(13) 0.0369(3) Uani 1 1 d . . . I1 I 0.34927(8) 0.49734(6) 0.38379(6) 0.03311(18) Uani 1 1 d . . . I2 I 0.65903(8) 0.22635(6) 0.27661(6) 0.03000(17) Uani 1 1 d . . . I3 I 0.39999(8) 0.40850(6) 0.04166(6) 0.02922(16) Uani 1 1 d . . . I4 I 0.06924(8) 0.07310(6) 0.14009(6) 0.03242(17) Uani 1 1 d . . . S1 S 0.3622(4) 0.1632(3) 0.4712(3) 0.0320(6) Uani 1 1 d . A . S2 S 0.9437(4) 0.4007(3) 1.0922(3) 0.0343(6) Uani 1 1 d . . . S3 S 0.7986(4) 0.6388(3) 0.3332(2) 0.0294(6) Uani 1 1 d . . . S4 S 1.3826(4) 1.0130(3) 0.9587(3) 0.0305(6) Uani 1 1 d . . . O1 O 0.4953(10) -0.0609(8) 0.5624(7) 0.0340(18) Uani 1 1 d . . . O2 O 0.6830(12) 0.0995(9) 0.7910(8) 0.049(2) Uani 1 1 d . . . O3 O 0.8964(12) 0.6114(8) 0.9426(8) 0.043(2) Uani 1 1 d . A . O4 O 0.747(3) 0.477(2) 0.708(2) 0.050(9) Uani 0.44(3) 1 d P A 1 O4' O 0.623(3) 0.4434(19) 0.7108(19) 0.051(6) Uani 0.56(3) 1 d P A 2 O5 O 1.0695(10) 0.6349(7) 0.6376(7) 0.0314(17) Uani 1 1 d . . . O6 O 1.3806(9) 0.7167(7) 0.8450(7) 0.0317(17) Uani 1 1 d . . . O7 O 1.0507(10) 1.0120(7) 0.6729(7) 0.0347(18) Uani 1 1 d . . . O8 O 0.9490(9) 0.9700(7) 0.4318(7) 0.0314(17) Uani 1 1 d . . . C1 C 0.3448(17) -0.0108(12) 0.4047(12) 0.041(3) Uani 1 1 d . . . H1A H 0.2399 -0.0546 0.3317 0.049 Uiso 1 1 calc R . . H1B H 0.4514 -0.0080 0.3831 0.049 Uiso 1 1 calc R . . C2 C 0.3283(15) -0.0988(12) 0.4760(12) 0.040(3) Uani 1 1 d . . . H2A H 0.2394 -0.0875 0.5129 0.048 Uiso 1 1 calc R . . H2B H 0.2876 -0.1966 0.4263 0.048 Uiso 1 1 calc R . . C3 C 0.4869(16) -0.1144(12) 0.6503(11) 0.040(3) Uani 1 1 d . . . H3A H 0.4645 -0.2141 0.6208 0.048 Uiso 1 1 calc R . . H3B H 0.3877 -0.1020 0.6756 0.048 Uiso 1 1 calc R . . C4 C 0.6582(17) -0.0422(12) 0.7506(12) 0.039(3) Uani 1 1 d . . . H4A H 0.6543 -0.0802 0.8135 0.047 Uiso 1 1 calc R . . H4B H 0.7579 -0.0546 0.7259 0.047 Uiso 1 1 calc R . . C5 C 0.8097(18) 0.1664(13) 0.9043(12) 0.047(3) Uani 1 1 d . . . H5A H 0.9198 0.1468 0.9077 0.057 Uiso 1 1 calc R . . H5B H 0.7624 0.1334 0.9601 0.057 Uiso 1 1 calc R . . C6 C 0.8493(19) 0.3193(12) 0.9350(12) 0.046(3) Uani 1 1 d . . . H6A H 0.7384 0.3360 0.9044 0.055 Uiso 1 1 calc R . . H6B H 0.9345 0.3584 0.8997 0.055 Uiso 1 1 calc R . . C7 C 1.0529(17) 0.5798(12) 1.1125(12) 0.039(3) Uani 1 1 d . . . H7A H 1.1150 0.6326 1.1968 0.047 Uiso 1 1 calc R . . H7B H 1.1441 0.5864 1.0752 0.047 Uiso 1 1 calc R . . C8 C 0.9255(17) 0.6454(13) 1.0622(11) 0.043(3) Uani 1 1 d . . . H8A H 0.8114 0.6106 1.0743 0.052 Uiso 1 1 calc R . . H8B H 0.9777 0.7466 1.1016 0.052 Uiso 1 1 calc R . . C9 C 0.7502(17) 0.6376(12) 0.8829(11) 0.043(3) Uani 1 1 d . . . H9A H 0.7593 0.7325 0.9226 0.051 Uiso 0.44(3) 1 calc PR A 1 H9B H 0.6378 0.5723 0.8797 0.051 Uiso 0.44(3) 1 calc PR A 1 H9C H 0.6483 0.5978 0.9057 0.051 Uiso 0.56(3) 1 d PR A 2 H9D H 0.7791 0.7383 0.9071 0.051 Uiso 0.56(3) 1 d PR A 2 C10 C 0.7537(17) 0.6207(12) 0.7696(11) 0.044(12) Uani 0.44(3) 1 d PRU A 1 H10A H 0.8637 0.6902 0.7743 0.053 Uiso 0.44(3) 1 calc PR A 1 H10B H 0.6506 0.6364 0.7235 0.053 Uiso 0.44(3) 1 calc PR A 1 C11 C 0.574(5) 0.391(4) 0.651(4) 0.050(11) Uani 0.44(3) 1 d PU A 1 H11A H 0.5090 0.4288 0.5986 0.060 Uiso 0.44(3) 1 calc PR A 1 H11B H 0.5137 0.3767 0.7072 0.060 Uiso 0.44(3) 1 calc PR A 1 C10' C 0.697(5) 0.582(3) 0.751(3) 0.058(8) Uani 0.56(3) 1 d P A 2 H10C H 0.6104 0.6203 0.7154 0.069 Uiso 0.56(3) 1 calc PR A 2 H10D H 0.8032 0.6113 0.7291 0.069 Uiso 0.56(3) 1 calc PR A 2 C11' C 0.681(3) 0.387(2) 0.616(2) 0.049(8) Uani 0.56(3) 1 d P A 2 H11C H 0.6497 0.4246 0.5533 0.059 Uiso 0.56(3) 1 calc PR A 2 H11D H 0.8112 0.4096 0.6446 0.059 Uiso 0.56(3) 1 calc PR A 2 C12 C 0.5880(16) 0.2410(13) 0.5742(11) 0.042(3) Uani 1 1 d . . . H12A H 0.6145 0.1859 0.6233 0.050 Uiso 0.44(3) 1 calc PR A 1 H12B H 0.6767 0.2575 0.5355 0.050 Uiso 0.44(3) 1 calc PR A 1 H12C H 0.6609 0.1969 0.5394 0.050 Uiso 0.56(3) 1 d PR A 2 H12D H 0.5859 0.2150 0.6433 0.050 Uiso 0.56(3) 1 d PR A 2 C13 C 0.8843(15) 0.6824(11) 0.4892(10) 0.028(2) Uani 1 1 d . . . H13A H 0.9605 0.7811 0.5271 0.033 Uiso 1 1 calc R . . H13B H 0.7846 0.6654 0.5189 0.033 Uiso 1 1 calc R . . C14 C 0.9914(16) 0.5953(11) 0.5170(10) 0.034(3) Uani 1 1 d . . . H14A H 0.9130 0.4971 0.4839 0.041 Uiso 1 1 calc R . . H14B H 1.0851 0.6069 0.4818 0.041 Uiso 1 1 calc R . . C15 C 1.1598(16) 0.5481(11) 0.6685(11) 0.038(3) Uani 1 1 d . . . H15A H 1.2591 0.5561 0.6383 0.045 Uiso 1 1 calc R . . H15B H 1.0768 0.4511 0.6334 0.045 Uiso 1 1 calc R . . C16 C 1.2311(16) 0.5892(11) 0.7987(10) 0.036(3) Uani 1 1 d . . . H16A H 1.1375 0.6008 0.8308 0.043 Uiso 1 1 calc R . . H16B H 1.2686 0.5170 0.8206 0.043 Uiso 1 1 calc R . . C17 C 1.4426(16) 0.7770(12) 0.9667(10) 0.037(3) Uani 1 1 d . . . H17A H 1.5713 0.8325 0.9951 0.044 Uiso 1 1 calc R . . H17B H 1.4276 0.7035 1.0008 0.044 Uiso 1 1 calc R . . C18 C 1.3439(17) 0.8689(12) 1.0078(12) 0.041(3) Uani 1 1 d . . . H18A H 1.3846 0.9027 1.0939 0.049 Uiso 1 1 calc R . . H18B H 1.2146 0.8145 0.9774 0.049 Uiso 1 1 calc R . . C19 C 1.1839(15) 0.9532(11) 0.8327(11) 0.031(3) Uani 1 1 d . . . H19A H 1.1766 0.8686 0.7747 0.038 Uiso 1 1 calc R . . H19B H 1.0773 0.9315 0.8554 0.038 Uiso 1 1 calc R . . C20 C 1.1908(16) 1.0654(11) 0.7808(10) 0.035(3) Uani 1 1 d . . . H20A H 1.1788 1.1446 0.8339 0.042 Uiso 1 1 calc R . . H20B H 1.3064 1.0975 0.7698 0.042 Uiso 1 1 calc R . . C21 C 1.0359(16) 1.1169(11) 0.6288(10) 0.034(3) Uani 1 1 d . . . H21A H 1.1509 1.1664 0.6237 0.041 Uiso 1 1 calc R . . H21B H 1.0041 1.1838 0.6811 0.041 Uiso 1 1 calc R . . C22 C 0.8938(16) 1.0528(13) 0.5101(11) 0.038(3) Uani 1 1 d . . . H22A H 0.7821 0.9958 0.5144 0.046 Uiso 1 1 calc R . . H22B H 0.8703 1.1258 0.4817 0.046 Uiso 1 1 calc R . . C23 C 0.8160(16) 0.8947(12) 0.3225(10) 0.037(3) Uani 1 1 d . . . H23A H 0.8725 0.8752 0.2636 0.045 Uiso 1 1 calc R . . H23B H 0.7458 0.9513 0.3020 0.045 Uiso 1 1 calc R . . C24 C 0.6921(15) 0.7609(11) 0.3179(10) 0.031(2) Uani 1 1 d . . . H24A H 0.5914 0.7197 0.2426 0.037 Uiso 1 1 calc R . . H24B H 0.6427 0.7799 0.3808 0.037 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 0.0401(8) 0.0317(7) 0.0394(9) 0.0175(6) 0.0141(7) 0.0128(6) Cu2 0.0346(7) 0.0249(6) 0.0376(8) 0.0119(6) 0.0092(6) 0.0076(6) Cu3 0.0406(8) 0.0280(6) 0.0321(8) 0.0097(6) 0.0114(6) 0.0144(6) Cu4 0.0383(8) 0.0311(7) 0.0427(9) 0.0154(6) 0.0110(7) 0.0155(6) I1 0.0376(4) 0.0285(3) 0.0367(4) 0.0097(3) 0.0171(3) 0.0150(3) I2 0.0302(3) 0.0295(3) 0.0345(4) 0.0147(3) 0.0108(3) 0.0144(3) I3 0.0329(4) 0.0257(3) 0.0298(4) 0.0136(3) 0.0102(3) 0.0089(3) I4 0.0296(3) 0.0258(3) 0.0407(4) 0.0160(3) 0.0102(3) 0.0064(3) S1 0.0316(14) 0.0275(12) 0.0402(17) 0.0160(12) 0.0153(13) 0.0092(11) S2 0.0312(14) 0.0300(13) 0.0470(18) 0.0201(13) 0.0161(13) 0.0109(11) S3 0.0293(13) 0.0279(13) 0.0301(15) 0.0123(11) 0.0083(12) 0.0089(11) S4 0.0344(14) 0.0298(13) 0.0317(16) 0.0126(12) 0.0133(12) 0.0151(11) O1 0.028(4) 0.046(4) 0.032(5) 0.022(4) 0.009(3) 0.011(3) O2 0.052(5) 0.036(4) 0.042(5) 0.014(4) -0.003(4) 0.008(4) O3 0.052(5) 0.049(5) 0.061(6) 0.034(5) 0.031(5) 0.041(4) O4 0.039(14) 0.025(11) 0.068(17) 0.003(11) 0.006(11) 0.009(9) O4' 0.072(17) 0.043(11) 0.053(14) 0.020(10) 0.043(12) 0.021(11) O5 0.036(4) 0.030(4) 0.031(5) 0.015(3) 0.011(4) 0.013(3) O6 0.027(4) 0.035(4) 0.033(4) 0.013(3) 0.008(3) 0.012(3) O7 0.038(4) 0.029(4) 0.031(4) 0.009(3) 0.004(4) 0.011(3) O8 0.027(4) 0.029(4) 0.044(5) 0.020(4) 0.015(4) 0.010(3) C1 0.035(6) 0.031(6) 0.051(9) 0.016(6) 0.005(6) 0.011(5) C2 0.034(6) 0.032(6) 0.054(8) 0.025(6) 0.008(6) 0.011(5) C3 0.042(7) 0.037(6) 0.044(8) 0.021(6) 0.018(6) 0.012(6) C4 0.048(7) 0.032(6) 0.041(7) 0.023(5) 0.011(6) 0.015(5) C5 0.043(7) 0.040(7) 0.060(10) 0.027(7) 0.025(7) 0.002(6) C6 0.054(8) 0.034(6) 0.043(8) 0.023(6) 0.003(6) 0.008(6) C7 0.038(6) 0.029(6) 0.053(9) 0.016(6) 0.018(6) 0.013(5) C8 0.049(7) 0.044(7) 0.054(9) 0.024(6) 0.029(7) 0.026(6) C9 0.053(8) 0.040(7) 0.050(8) 0.025(6) 0.025(7) 0.023(6) C10 0.046(13) 0.041(13) 0.045(13) 0.016(6) 0.012(6) 0.017(6) C11 0.047(12) 0.051(12) 0.052(12) 0.016(6) 0.017(6) 0.020(6) C10' 0.09(2) 0.027(14) 0.054(18) 0.007(13) 0.017(16) 0.031(17) C11' 0.039(13) 0.040(14) 0.051(17) 0.005(12) 0.006(12) 0.008(11) C12 0.039(7) 0.043(7) 0.029(7) 0.014(6) 0.006(5) -0.001(6) C13 0.032(6) 0.028(5) 0.021(6) 0.009(5) 0.008(5) 0.010(5) C14 0.047(7) 0.028(5) 0.030(7) 0.013(5) 0.008(5) 0.020(5) C15 0.039(6) 0.022(5) 0.048(8) 0.012(5) 0.013(6) 0.008(5) C16 0.047(7) 0.031(6) 0.031(7) 0.018(5) 0.004(5) 0.020(5) C17 0.035(6) 0.042(6) 0.029(7) 0.014(5) -0.002(5) 0.018(5) C18 0.052(8) 0.040(7) 0.041(8) 0.020(6) 0.022(6) 0.023(6) C19 0.031(6) 0.026(5) 0.036(7) 0.013(5) 0.011(5) 0.008(5) C20 0.043(7) 0.029(5) 0.029(7) 0.010(5) 0.009(5) 0.011(5) C21 0.049(7) 0.034(5) 0.032(6) 0.027(5) 0.014(5) 0.020(5) C22 0.039(7) 0.043(7) 0.039(7) 0.019(6) 0.011(6) 0.022(6) C23 0.043(7) 0.037(6) 0.033(7) 0.017(5) 0.012(6) 0.013(5) C24 0.031(6) 0.037(6) 0.016(6) 0.015(5) -0.006(5) 0.006(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 2.299(3) . ? Cu1 Cu2 2.6419(18) . ? Cu1 I1 2.6574(14) . ? Cu1 I4 2.6804(16) . ? Cu1 Cu3 2.7268(19) . ? Cu1 I2 2.7276(14) . ? Cu1 Cu4 2.762(2) . ? Cu2 S3 2.305(3) . ? Cu2 I2 2.6321(15) . ? Cu2 Cu3 2.6668(18) . ? Cu2 I3 2.6725(17) . ? Cu2 I1 2.7202(15) . ? Cu2 Cu4 2.8489(19) . ? Cu3 S4 2.290(3) 1_444 ? Cu3 Cu4 2.6557(18) . ? Cu3 I3 2.6604(15) . ? Cu3 I2 2.6815(16) . ? Cu3 I4 2.6915(15) . ? Cu4 S2 2.302(3) 1_454 ? Cu4 I4 2.6604(15) . ? Cu4 I1 2.6621(17) . ? Cu4 I3 2.7361(16) . ? S1 C1 1.798(12) . ? S1 C12 1.807(12) . ? S2 C6 1.813(14) . ? S2 C7 1.815(12) . ? S2 Cu4 2.302(3) 1_656 ? S3 C24 1.800(12) . ? S3 C13 1.806(12) . ? S4 C18 1.798(13) . ? S4 C19 1.801(12) . ? S4 Cu3 2.290(3) 1_666 ? O1 C3 1.388(14) . ? O1 C2 1.408(14) . ? O2 C5 1.405(16) . ? O2 C4 1.419(15) . ? O3 C9 1.401(15) . ? O3 C8 1.405(15) . ? O4 C11 1.36(5) . ? O4 C10 1.52(2) . ? O4' C10' 1.35(4) . ? O4' C11' 1.46(3) . ? O5 C14 1.396(14) . ? O5 C15 1.420(13) . ? O6 C17 1.402(14) . ? O6 C16 1.437(13) . ? O7 C20 1.405(14) . ? O7 C21 1.406(13) . ? O8 C23 1.398(14) . ? O8 C22 1.414(13) . ? C1 C2 1.475(18) . ? C3 C4 1.489(17) . ? C5 C6 1.513(17) . ? C7 C8 1.526(18) . ? C9 C10 1.4117 . ? C9 C10' 1.52(3) . ? C11 C12 1.72(4) . ? C11' C12 1.43(2) . ? C13 C14 1.507(15) . ? C15 C16 1.502(17) . ? C17 C18 1.526(16) . ? C19 C20 1.513(16) . ? C21 C22 1.501(17) . ? C23 C24 1.505(16) . ? 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 Cu2 142.48(10) . . ? S1 Cu1 I1 109.46(9) . . ? Cu2 Cu1 I1 61.77(4) . . ? S1 Cu1 I4 106.12(9) . . ? Cu2 Cu1 I4 111.07(6) . . ? I1 Cu1 I4 110.22(6) . . ? S1 Cu1 Cu3 144.00(9) . . ? Cu2 Cu1 Cu3 59.54(5) . . ? I1 Cu1 Cu3 106.54(6) . . ? I4 Cu1 Cu3 59.70(4) . . ? S1 Cu1 I2 104.02(9) . . ? Cu2 Cu1 I2 58.68(4) . . ? I1 Cu1 I2 116.36(5) . . ? I4 Cu1 I2 110.03(5) . . ? Cu3 Cu1 I2 58.89(4) . . ? S1 Cu1 Cu4 146.81(10) . . ? Cu2 Cu1 Cu4 63.59(5) . . ? I1 Cu1 Cu4 58.80(4) . . ? I4 Cu1 Cu4 58.51(4) . . ? Cu3 Cu1 Cu4 57.87(5) . . ? I2 Cu1 Cu4 108.90(6) . . ? S3 Cu2 I2 111.92(9) . . ? S3 Cu2 Cu1 144.14(10) . . ? I2 Cu2 Cu1 62.29(4) . . ? S3 Cu2 Cu3 150.05(9) . . ? I2 Cu2 Cu3 60.80(4) . . ? Cu1 Cu2 Cu3 61.81(5) . . ? S3 Cu2 I3 103.70(9) . . ? I2 Cu2 I3 112.29(5) . . ? Cu1 Cu2 I3 111.14(6) . . ? Cu3 Cu2 I3 59.77(4) . . ? S3 Cu2 I1 102.37(8) . . ? I2 Cu2 I1 117.49(5) . . ? Cu1 Cu2 I1 59.40(4) . . ? Cu3 Cu2 I1 106.47(5) . . ? I3 Cu2 I1 107.78(5) . . ? S3 Cu2 Cu4 138.99(9) . . ? I2 Cu2 Cu4 109.09(5) . . ? Cu1 Cu2 Cu4 60.26(5) . . ? Cu3 Cu2 Cu4 57.45(5) . . ? I3 Cu2 Cu4 59.31(4) . . ? I1 Cu2 Cu4 57.06(4) . . ? S4 Cu3 Cu4 146.68(10) 1_444 . ? S4 Cu3 I3 110.59(9) 1_444 . ? Cu4 Cu3 I3 61.95(4) . . ? S4 Cu3 Cu2 143.21(10) 1_444 . ? Cu4 Cu3 Cu2 64.72(5) . . ? I3 Cu3 Cu2 60.22(4) . . ? S4 Cu3 I2 99.46(9) 1_444 . ? Cu4 Cu3 I2 113.61(6) . . ? I3 Cu3 I2 111.11(5) . . ? Cu2 Cu3 I2 58.96(4) . . ? S4 Cu3 I4 105.57(9) 1_444 . ? Cu4 Cu3 I4 59.67(4) . . ? I3 Cu3 I4 117.37(5) . . ? Cu2 Cu3 I4 109.96(5) . . ? I2 Cu3 I4 111.10(5) . . ? S4 Cu3 Cu1 140.11(10) 1_444 . ? Cu4 Cu3 Cu1 61.73(5) . . ? I3 Cu3 Cu1 108.90(5) . . ? Cu2 Cu3 Cu1 58.64(5) . . ? I2 Cu3 Cu1 60.57(4) . . ? I4 Cu3 Cu1 59.29(4) . . ? S2 Cu4 Cu3 144.54(11) 1_454 . ? S2 Cu4 I4 110.85(9) 1_454 . ? Cu3 Cu4 I4 60.83(4) . . ? S2 Cu4 I1 106.55(9) 1_454 . ? Cu3 Cu4 I1 108.49(6) . . ? I4 Cu4 I1 110.69(6) . . ? S2 Cu4 I3 104.78(9) 1_454 . ? Cu3 Cu4 I3 59.11(4) . . ? I4 Cu4 I3 115.82(5) . . ? I1 Cu4 I3 107.62(5) . . ? S2 Cu4 Cu1 149.02(10) 1_454 . ? Cu3 Cu4 Cu1 60.40(5) . . ? I4 Cu4 Cu1 59.21(4) . . ? I1 Cu4 Cu1 58.64(4) . . ? I3 Cu4 Cu1 105.74(5) . . ? S2 Cu4 Cu2 143.61(9) 1_454 . ? Cu3 Cu4 Cu2 57.83(5) . . ? I4 Cu4 Cu2 105.55(5) . . ? I1 Cu4 Cu2 59.04(4) . . ? I3 Cu4 Cu2 57.13(4) . . ? Cu1 Cu4 Cu2 56.15(5) . . ? Cu1 I1 Cu4 62.56(5) . . ? Cu1 I1 Cu2 58.84(4) . . ? Cu4 I1 Cu2 63.91(4) . . ? Cu2 I2 Cu3 60.24(4) . . ? Cu2 I2 Cu1 59.03(4) . . ? Cu3 I2 Cu1 60.54(4) . . ? Cu3 I3 Cu2 60.01(4) . . ? Cu3 I3 Cu4 58.94(4) . . ? Cu2 I3 Cu4 63.56(5) . . ? Cu4 I4 Cu1 62.28(5) . . ? Cu4 I4 Cu3 59.50(4) . . ? Cu1 I4 Cu3 61.01(4) . . ? C1 S1 C12 102.3(6) . . ? C1 S1 Cu1 101.7(5) . . ? C12 S1 Cu1 106.2(4) . . ? C6 S2 C7 102.8(6) . . ? C6 S2 Cu4 108.6(5) . 1_656 ? C7 S2 Cu4 102.4(4) . 1_656 ? C24 S3 C13 102.4(5) . . ? C24 S3 Cu2 102.2(4) . . ? C13 S3 Cu2 106.2(4) . . ? C18 S4 C19 101.0(6) . . ? C18 S4 Cu3 104.5(4) . 1_666 ? C19 S4 Cu3 108.1(4) . 1_666 ? C3 O1 C2 113.5(9) . . ? C5 O2 C4 110.7(10) . . ? C9 O3 C8 112.5(9) . . ? C11 O4 C10 109(2) . . ? C10' O4' C11' 109(2) . . ? C14 O5 C15 111.6(8) . . ? C17 O6 C16 113.9(9) . . ? C20 O7 C21 110.8(8) . . ? C23 O8 C22 113.2(8) . . ? C2 C1 S1 116.0(10) . . ? O1 C2 C1 108.9(10) . . ? O1 C3 C4 109.5(10) . . ? O2 C4 C3 107.7(10) . . ? O2 C5 C6 107.9(12) . . ? C5 C6 S2 108.6(9) . . ? C8 C7 S2 113.6(9) . . ? O3 C8 C7 108.1(9) . . ? O3 C9 C10 106.5(6) . . ? O3 C9 C10' 114.1(15) . . ? C10 C9 C10' 18.6(16) . . ? C9 C10 O4 111.5(12) . . ? O4 C11 C12 104(3) . . ? O4' C10' C9 110(2) . . ? C12 C11' O4' 105.5(19) . . ? C11' C12 C11 39.6(14) . . ? C11' C12 S1 120.9(14) . . ? C11 C12 S1 98.0(15) . . ? C14 C13 S3 108.8(7) . . ? O5 C14 C13 109.5(8) . . ? O5 C15 C16 109.5(9) . . ? O6 C16 C15 108.3(10) . . ? O6 C17 C18 112.2(10) . . ? C17 C18 S4 111.0(9) . . ? C20 C19 S4 108.5(8) . . ? O7 C20 C19 108.7(9) . . ? O7 C21 C22 108.5(9) . . ? O8 C22 C21 109.9(9) . . ? O8 C23 C24 113.0(9) . . ? C23 C24 S3 113.2(8) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.304 _refine_diff_density_min -1.134 _refine_diff_density_rms 0.183 ############################################################ data_3 _database_code_depnum_ccdc_archive 'CCDC 822022' #TrackingRef '6248_web_deposit_cif_file_0_In-HyeokPark_1310473525.DT18C6Cu-R.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C12 H24 Cu I O4 S2), Co H12 O6, 2(Cl O4), 2(H O0.50)' _chemical_formula_sum 'C24 H62 Cl2 Co Cu2 I2 O23 S4' _chemical_formula_weight 1357.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 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 9.3053(4) _cell_length_b 10.1770(4) _cell_length_c 13.6897(6) _cell_angle_alpha 86.972(2) _cell_angle_beta 89.543(2) _cell_angle_gamma 64.397(2) _cell_volume 1167.33(9) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9857 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 28.29 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.931 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 679 _exptl_absorpt_coefficient_mu 2.945 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3781 _exptl_absorpt_correction_T_max 0.6046 _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 20842 _diffrn_reflns_av_R_equivalents 0.0280 _diffrn_reflns_av_sigmaI/netI 0.0221 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 28.00 _reflns_number_total 5615 _reflns_number_gt 5289 _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^)+(0.0265P)^2^+0.7839P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5615 _refine_ls_number_parameters 328 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0227 _refine_ls_R_factor_gt 0.0208 _refine_ls_wR_factor_ref 0.0549 _refine_ls_wR_factor_gt 0.0534 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.43994(3) 0.16618(3) 0.489204(17) 0.02679(6) Uani 1 1 d . . . I1 I 0.260947(14) 0.017528(13) 0.484041(8) 0.02495(4) Uani 1 1 d . . . Co1 Co 0.5000 0.5000 0.0000 0.02103(7) Uani 1 2 d S . . O1W O 0.74331(19) 0.4414(2) -0.02135(13) 0.0332(3) Uani 1 1 d . . . H1WA H 0.779(4) 0.416(4) -0.067(3) 0.061(11) Uiso 1 1 d . . . H1WB H 0.791(4) 0.480(4) 0.001(2) 0.054(9) Uiso 1 1 d . . . O2W O 0.5381(2) 0.48932(19) 0.14705(10) 0.0282(3) Uani 1 1 d . . . H2WA H 0.481(4) 0.549(3) 0.179(2) 0.041(8) Uiso 1 1 d . . . H2WB H 0.592(4) 0.423(3) 0.175(2) 0.039(8) Uiso 1 1 d . . . O3W O 0.5676(2) 0.27542(19) 0.00061(13) 0.0328(3) Uani 1 1 d . . . H3WA H 0.503(4) 0.242(4) -0.009(3) 0.059(10) Uiso 1 1 d . . . H3WB H 0.634(6) 0.225(5) 0.020(3) 0.094(17) Uiso 1 1 d . . . S1 S 0.39098(5) 0.31347(5) 0.34545(3) 0.02136(9) Uani 1 1 d . . . S2 S 0.70608(5) 0.65556(5) 0.40143(3) 0.02178(9) Uani 1 1 d . . . O1 O 0.18086(16) 0.59352(15) 0.22117(9) 0.0246(3) Uani 1 1 d . . . O2 O 0.38944(16) 0.71833(15) 0.26924(10) 0.0257(3) Uani 1 1 d . . . O3 O 0.8140(2) 0.36630(17) 0.28998(12) 0.0411(4) Uani 1 1 d . . . O4 O 0.68351(19) 0.19565(18) 0.21682(17) 0.0519(5) Uani 1 1 d . . . C1 C 0.1748(2) 0.4057(2) 0.34013(14) 0.0277(4) Uani 1 1 d . . . H1A H 0.1326 0.3316 0.3467 0.033 Uiso 1 1 calc R . . H1B H 0.1369 0.4684 0.3965 0.033 Uiso 1 1 calc R . . C2 C 0.1073(2) 0.4991(2) 0.24650(14) 0.0276(4) Uani 1 1 d . . . H2A H 0.1211 0.4343 0.1922 0.033 Uiso 1 1 calc R . . H2B H -0.0085 0.5589 0.2542 0.033 Uiso 1 1 calc R . . C3 C 0.1368(2) 0.7129(2) 0.28262(15) 0.0296(4) Uani 1 1 d . . . H3A H 0.1652 0.6762 0.3515 0.035 Uiso 1 1 calc R . . H3B H 0.0201 0.7734 0.2780 0.035 Uiso 1 1 calc R . . C4 C 0.2222(2) 0.8027(2) 0.25103(16) 0.0306(4) Uani 1 1 d . . . H4A H 0.2020 0.8316 0.1805 0.037 Uiso 1 1 calc R . . H4B H 0.1829 0.8925 0.2879 0.037 Uiso 1 1 calc R . . C5 C 0.4743(2) 0.8058(2) 0.25371(14) 0.0251(4) Uani 1 1 d . . . H5A H 0.4333 0.8880 0.2976 0.030 Uiso 1 1 calc R . . H5B H 0.4579 0.8467 0.1853 0.030 Uiso 1 1 calc R . . C6 C 0.6497(2) 0.7140(2) 0.27403(13) 0.0237(3) Uani 1 1 d . . . H6A H 0.7084 0.7702 0.2501 0.028 Uiso 1 1 calc R . . H6B H 0.6850 0.6260 0.2355 0.028 Uiso 1 1 calc R . . C7 C 0.6611(2) 0.4995(2) 0.42089(14) 0.0249(4) Uani 1 1 d . . . H7A H 0.6376 0.4905 0.4909 0.030 Uiso 1 1 calc R . . H7B H 0.5637 0.5180 0.3827 0.030 Uiso 1 1 calc R . . C8 C 0.7931(3) 0.3558(2) 0.39255(16) 0.0317(4) Uani 1 1 d . . . H8A H 0.8932 0.3366 0.4279 0.038 Uiso 1 1 calc R . . H8B H 0.7639 0.2748 0.4096 0.038 Uiso 1 1 calc R . . C9 C 0.9128(3) 0.2356(3) 0.24447(19) 0.0417(5) Uani 1 1 d . . . H9A H 1.0193 0.1926 0.2767 0.050 Uiso 1 1 calc R . . H9B H 0.9266 0.2599 0.1751 0.050 Uiso 1 1 calc R . . C10 C 0.8471(3) 0.1246(2) 0.24889(19) 0.0385(5) Uani 1 1 d . . . H10A H 0.9087 0.0444 0.2061 0.046 Uiso 1 1 calc R . . H10B H 0.8548 0.0829 0.3167 0.046 Uiso 1 1 calc R . . C11 C 0.6033(3) 0.1069(2) 0.23197(15) 0.0306(4) Uani 1 1 d . . . H11A H 0.6428 0.0449 0.2930 0.037 Uiso 1 1 calc R . . H11B H 0.6225 0.0425 0.1768 0.037 Uiso 1 1 calc R . . C12 C 0.4274(2) 0.2048(2) 0.23920(14) 0.0283(4) Uani 1 1 d . . . H12A H 0.3674 0.1448 0.2446 0.034 Uiso 1 1 calc R . . H12B H 0.3898 0.2699 0.1793 0.034 Uiso 1 1 calc R . . Cl1 Cl 0.2021(6) 0.1945(6) -0.0118(4) 0.0356(7) Uani 0.497(12) 1 d P A 1 Cl2 Cl 0.1840(5) 0.2348(5) -0.0281(3) 0.0292(6) Uani 0.503(12) 1 d P A 2 O5 O 0.3577(2) 0.1521(3) -0.03912(18) 0.0611(6) Uani 1 1 d . . . O6 O 0.1105(3) 0.1714(3) -0.08786(16) 0.0622(6) Uani 1 1 d . . . O7 O 0.1296(8) 0.3449(11) 0.0088(12) 0.113(5) Uani 0.497(12) 1 d P A 1 O8 O 0.1881(11) 0.1196(17) 0.0726(5) 0.115(4) Uani 0.503(12) 1 d P A 1 O7' O 0.1389(7) 0.3798(5) -0.0628(4) 0.0519(15) Uani 0.503(12) 1 d P A 2 O8' O 0.1476(8) 0.2275(11) 0.0719(3) 0.062(2) Uani 0.497(12) 1 d P A 2 O4W O 0.8710(5) 0.0889(5) -0.0019(4) 0.0637(13) Uani 0.50 1 d P . . H4WA H 0.904(10) -0.007(11) 0.017(6) 0.08(2) Uiso 0.50 1 d P . . H4WB H 0.956(17) 0.106(13) -0.004(9) 0.14(4) Uiso 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.02888(12) 0.02703(13) 0.02195(11) -0.00106(9) -0.00160(9) -0.00972(10) I1 0.02487(7) 0.02335(7) 0.02642(7) 0.00119(5) -0.00215(5) -0.01046(5) Co1 0.02306(17) 0.02415(17) 0.01652(15) -0.00089(12) -0.00076(12) -0.01081(14) O1W 0.0280(7) 0.0475(10) 0.0289(8) -0.0068(7) 0.0031(6) -0.0202(7) O2W 0.0355(8) 0.0258(7) 0.0191(6) -0.0008(6) -0.0040(6) -0.0093(6) O3W 0.0369(9) 0.0274(8) 0.0357(8) -0.0013(6) -0.0030(7) -0.0152(7) S1 0.0231(2) 0.0217(2) 0.0205(2) -0.00001(16) -0.00185(16) -0.01096(17) S2 0.0228(2) 0.0222(2) 0.0220(2) -0.00331(16) 0.00038(16) -0.01107(17) O1 0.0247(6) 0.0251(7) 0.0226(6) -0.0002(5) -0.0001(5) -0.0095(5) O2 0.0229(6) 0.0224(6) 0.0312(7) -0.0013(5) -0.0033(5) -0.0091(5) O3 0.0481(9) 0.0266(8) 0.0386(8) -0.0064(6) 0.0144(7) -0.0065(7) O4 0.0219(7) 0.0270(8) 0.0979(15) 0.0208(9) 0.0035(8) -0.0048(6) C1 0.0230(9) 0.0319(10) 0.0282(9) 0.0032(8) 0.0005(7) -0.0123(8) C2 0.0235(9) 0.0308(10) 0.0294(9) 0.0027(8) -0.0042(7) -0.0132(8) C3 0.0242(9) 0.0314(10) 0.0307(9) -0.0069(8) 0.0015(7) -0.0093(8) C4 0.0243(9) 0.0250(9) 0.0387(11) -0.0020(8) -0.0061(8) -0.0068(7) C5 0.0301(9) 0.0225(9) 0.0235(8) -0.0004(7) -0.0008(7) -0.0122(7) C6 0.0281(9) 0.0256(9) 0.0199(8) -0.0010(7) 0.0031(7) -0.0140(7) C7 0.0260(9) 0.0257(9) 0.0260(9) -0.0010(7) 0.0045(7) -0.0143(7) C8 0.0333(10) 0.0238(9) 0.0367(11) 0.0020(8) 0.0046(8) -0.0117(8) C9 0.0343(11) 0.0346(12) 0.0504(14) -0.0116(10) 0.0123(10) -0.0087(9) C10 0.0285(10) 0.0282(11) 0.0492(13) -0.0010(9) 0.0028(9) -0.0033(8) C11 0.0401(11) 0.0220(9) 0.0265(9) -0.0015(7) 0.0031(8) -0.0102(8) C12 0.0347(10) 0.0339(10) 0.0226(9) -0.0061(7) 0.0014(7) -0.0202(9) Cl1 0.0326(11) 0.0471(19) 0.0330(16) -0.0095(12) 0.0016(10) -0.0219(14) Cl2 0.0272(9) 0.0404(16) 0.0236(10) -0.0026(9) -0.0021(7) -0.0180(11) O5 0.0391(10) 0.0714(14) 0.0802(15) -0.0240(12) 0.0124(10) -0.0288(10) O6 0.0667(13) 0.0736(14) 0.0578(12) -0.0111(10) -0.0210(10) -0.0400(12) O7 0.063(3) 0.091(6) 0.204(13) -0.095(8) 0.029(5) -0.041(4) O8 0.141(7) 0.164(11) 0.060(4) 0.026(5) 0.023(4) -0.088(7) O7' 0.063(3) 0.041(2) 0.052(3) -0.0054(19) -0.017(2) -0.0213(19) O8' 0.083(4) 0.103(5) 0.025(2) -0.006(2) 0.011(2) -0.064(4) O4W 0.038(2) 0.041(2) 0.110(4) 0.020(2) 0.003(2) -0.0175(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 S1 2.3324(5) . ? Cu1 S2 2.3459(5) 2_666 ? Cu1 I1 2.6121(3) 2_656 ? Cu1 I1 2.6942(3) . ? I1 Cu1 2.6121(3) 2_656 ? Co1 O2W 2.0359(14) . ? Co1 O2W 2.0360(14) 2_665 ? Co1 O3W 2.0917(17) 2_665 ? Co1 O3W 2.0917(17) . ? Co1 O1W 2.0995(16) 2_665 ? Co1 O1W 2.0996(16) . ? S1 C12 1.8142(19) . ? S1 C1 1.816(2) . ? S2 C7 1.8158(19) . ? S2 C6 1.8182(19) . ? S2 Cu1 2.3459(5) 2_666 ? O1 C3 1.423(2) . ? O1 C2 1.429(2) . ? O2 C5 1.431(2) . ? O2 C4 1.432(2) . ? O3 C8 1.421(3) . ? O3 C9 1.422(3) . ? O4 C11 1.406(3) . ? O4 C10 1.435(3) . ? C1 C2 1.519(3) . ? C3 C4 1.495(3) . ? C5 C6 1.509(3) . ? C7 C8 1.516(3) . ? C9 C10 1.497(4) . ? C11 C12 1.510(3) . ? Cl1 O5 1.375(5) . ? Cl1 O8 1.387(11) . ? Cl1 O7 1.424(7) . ? Cl1 O6 1.441(5) . ? Cl2 O7' 1.406(6) . ? Cl2 O6 1.413(5) . ? Cl2 O8' 1.414(6) . ? Cl2 O5 1.476(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 Cu1 S2 99.460(18) . 2_666 ? S1 Cu1 I1 113.632(15) . 2_656 ? S2 Cu1 I1 124.029(15) 2_666 2_656 ? S1 Cu1 I1 108.296(14) . . ? S2 Cu1 I1 100.485(14) 2_666 . ? I1 Cu1 I1 109.388(10) 2_656 . ? Cu1 I1 Cu1 70.612(10) 2_656 . ? O2W Co1 O2W 179.999(1) . 2_665 ? O2W Co1 O3W 88.32(7) . 2_665 ? O2W Co1 O3W 91.68(7) 2_665 2_665 ? O2W Co1 O3W 91.68(7) . . ? O2W Co1 O3W 88.32(7) 2_665 . ? O3W Co1 O3W 180.0 2_665 . ? O2W Co1 O1W 90.75(7) . 2_665 ? O2W Co1 O1W 89.25(7) 2_665 2_665 ? O3W Co1 O1W 84.52(7) 2_665 2_665 ? O3W Co1 O1W 95.48(7) . 2_665 ? O2W Co1 O1W 89.25(7) . . ? O2W Co1 O1W 90.75(7) 2_665 . ? O3W Co1 O1W 95.48(7) 2_665 . ? O3W Co1 O1W 84.52(7) . . ? O1W Co1 O1W 180.0 2_665 . ? C12 S1 C1 99.78(9) . . ? C12 S1 Cu1 110.58(7) . . ? C1 S1 Cu1 102.38(7) . . ? C7 S2 C6 103.61(9) . . ? C7 S2 Cu1 109.44(6) . 2_666 ? C6 S2 Cu1 113.31(6) . 2_666 ? C3 O1 C2 113.48(15) . . ? C5 O2 C4 111.09(15) . . ? C8 O3 C9 117.28(18) . . ? C11 O4 C10 112.83(17) . . ? C2 C1 S1 114.00(14) . . ? O1 C2 C1 113.33(15) . . ? O1 C3 C4 109.09(16) . . ? O2 C4 C3 108.84(16) . . ? O2 C5 C6 109.73(15) . . ? C5 C6 S2 115.83(13) . . ? C8 C7 S2 114.54(13) . . ? O3 C8 C7 107.66(16) . . ? O3 C9 C10 113.3(2) . . ? O4 C10 C9 108.16(18) . . ? O4 C11 C12 108.16(16) . . ? C11 C12 S1 109.98(14) . . ? O5 Cl1 O8 112.9(7) . . ? O5 Cl1 O7 110.6(4) . . ? O8 Cl1 O7 105.9(11) . . ? O5 Cl1 O6 111.1(3) . . ? O8 Cl1 O6 107.4(6) . . ? O7 Cl1 O6 108.7(4) . . ? O7' Cl2 O6 108.7(3) . . ? O7' Cl2 O8' 111.1(7) . . ? O6 Cl2 O8' 112.8(4) . . ? O7' Cl2 O5 108.6(3) . . ? O6 Cl2 O5 107.0(3) . . ? O8' Cl2 O5 108.5(5) . . ? Cl1 O5 Cl2 16.5(2) . . ? Cl2 O6 Cl1 16.92(18) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.941 _refine_diff_density_min -0.432 _refine_diff_density_rms 0.078