# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_t _database_code_depnum_ccdc_archive 'CCDC 890819' #TrackingRef '1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C144 H132 Cu30 I16 N24 S16, 3(H3 C2 N)' _chemical_formula_sum 'C150 H141 Cu30 I16 N27 S16' _chemical_formula_weight 6771.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 31.206(6) _cell_length_b 32.079(6) _cell_length_c 20.393(4) _cell_angle_alpha 90.00 _cell_angle_beta 106.70(3) _cell_angle_gamma 90.00 _cell_volume 19554(7) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 21308 _cell_measurement_theta_min 3.0074 _cell_measurement_theta_max 27.4855 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.300 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 12816 _exptl_absorpt_coefficient_mu 5.931 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1554 _exptl_absorpt_correction_T_max 0.3834 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 49699 _diffrn_reflns_av_R_equivalents 0.0691 _diffrn_reflns_av_sigmaI/netI 0.1032 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.46 _reflns_number_total 22097 _reflns_number_gt 16417 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1000P)^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 22097 _refine_ls_number_parameters 1092 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1243 _refine_ls_R_factor_gt 0.0930 _refine_ls_wR_factor_ref 0.2540 _refine_ls_wR_factor_gt 0.2289 _refine_ls_goodness_of_fit_ref 1.171 _refine_ls_restrained_S_all 1.171 _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 0.24876(6) 0.95663(5) 0.96297(7) 0.0408(4) Uani 1 1 d . . . Cu2 Cu 0.16856(6) 0.93622(5) 0.89126(7) 0.0435(4) Uani 1 1 d . . . Cu3 Cu 0.21765(6) 0.87187(5) 0.97005(7) 0.0422(4) Uani 1 1 d . . . Cu4 Cu 0.06537(6) 0.76849(5) 1.07361(8) 0.0458(4) Uani 1 1 d . . . Cu5 Cu 0.11476(6) 0.74723(5) 1.19135(8) 0.0431(4) Uani 1 1 d . . . Cu6 Cu 0.15531(6) 0.76553(5) 1.08224(7) 0.0442(4) Uani 1 1 d . . . Cu7 Cu 0.22387(7) 0.72026(6) 0.75919(8) 0.0545(5) Uani 1 1 d . . . Cu8 Cu 0.20314(6) 0.80481(5) 0.72451(7) 0.0421(4) Uani 1 1 d . . . Cu9 Cu 0.22851(6) 0.78358(5) 0.86329(7) 0.0418(4) Uani 1 1 d . . . Cu10 Cu 0.17043(6) 0.63930(6) 0.84387(7) 0.0507(4) Uani 1 1 d . . . Cu11 Cu 0.10144(6) 0.64243(5) 0.89956(7) 0.0404(4) Uani 1 1 d . . . Cu12 Cu 0.17602(6) 0.69256(5) 0.95546(7) 0.0410(4) Uani 1 1 d . . . Cu13 Cu 0.14554(6) 0.79622(6) 0.93125(8) 0.0547(5) Uani 1 1 d . . . Cu14 Cu 0.10255(6) 0.87785(5) 1.01046(7) 0.0446(4) Uani 1 1 d . . . Cu15 Cu 0.12868(6) 0.91921(5) 1.12361(7) 0.0435(4) Uani 1 1 d . . . I1 I 0.20523(4) 1.00313(3) 0.86327(4) 0.0513(2) Uani 1 1 d . . . I2 I 0.03160(3) 0.72700(4) 1.15533(5) 0.0575(3) Uani 1 1 d . . . I3 I 0.17868(3) 0.74443(3) 0.64092(4) 0.0513(2) Uani 1 1 d . . . I4 I 0.09016(3) 0.61773(3) 0.77707(4) 0.0507(2) Uani 1 1 d . . . I5 I 0.22991(4) 0.64132(3) 0.77950(5) 0.0542(3) Uani 1 1 d . . . I6 I 0.15422(3) 0.73820(2) 0.84166(3) 0.03521(19) Uani 1 1 d . . . I7 I 0.07475(3) 0.83683(3) 0.89421(4) 0.0426(2) Uani 1 1 d . . . I8 I 0.05209(3) 0.93658(3) 1.04568(5) 0.0542(2) Uani 1 1 d . . . S1 S 0.29432(11) 0.87521(10) 1.04319(14) 0.0375(7) Uani 1 1 d . . . S2 S 0.16413(12) 0.91499(11) 0.99360(14) 0.0406(7) Uani 1 1 d . . . S3 S 0.21909(11) 0.85478(10) 0.86124(14) 0.0387(7) Uani 1 1 d . . . S4 S 0.12844(11) 0.70646(10) 1.02128(14) 0.0376(7) Uani 1 1 d . . . S5 S 0.21534(12) 0.74474(9) 1.17672(14) 0.0386(7) Uani 1 1 d . . . S6 S 0.11236(12) 0.82328(10) 1.09176(14) 0.0418(8) Uani 1 1 d . . . S7 S 0.20335(12) 0.80670(10) 1.02344(14) 0.0414(7) Uani 1 1 d . . . S8 S 0.24656(13) 0.71912(11) 1.01470(15) 0.0318(11) Uani 0.830(10) 1 d P . 1 S8A S 0.2284(5) 0.7432(5) 1.0288(8) 0.028(5) Uani 0.170(10) 1 d P . 2 N1 N 0.3079(4) 0.9345(3) 0.9596(5) 0.035(2) Uani 1 1 d . . . N2 N 0.3719(4) 0.8962(3) 1.0222(5) 0.036(2) Uani 1 1 d . . . N3 N 0.2349(4) 0.9616(3) 1.0526(4) 0.034(2) Uani 1 1 d . . . N4 N 0.1861(4) 0.9454(3) 1.1201(5) 0.037(2) Uani 1 1 d . . . N5 N 0.1454(4) 0.9001(3) 0.8086(4) 0.037(2) Uani 1 1 d . . . N6 N 0.1565(4) 0.8422(3) 0.7428(4) 0.039(3) Uani 1 1 d . . . N7 N 0.0470(4) 0.7415(3) 0.9812(5) 0.040(3) Uani 1 1 d . . . N8 N 0.0632(4) 0.6901(3) 0.9065(4) 0.041(3) Uani 1 1 d . . . N9 N 0.1559(4) 0.6985(3) 1.2168(5) 0.042(3) Uani 1 1 d . . . N10 N 0.2323(3) 0.6784(3) 1.2601(4) 0.037(2) Uani 1 1 d . . . N11 N 0.1357(4) 0.8047(3) 1.2248(5) 0.039(2) Uani 1 1 d . . . N12 N 0.1414(4) 0.8754(4) 1.1974(5) 0.044(3) Uani 1 1 d . . . C1 C 0.3287(4) 0.9049(4) 1.0053(6) 0.039(3) Uani 1 1 d . . . C2 C 0.3337(5) 0.9537(4) 0.9264(6) 0.044(3) Uani 1 1 d . . . H2 H 0.3208 0.9749 0.8962 0.053 Uiso 1 1 calc R . . C3 C 0.3770(5) 0.9442(5) 0.9340(7) 0.053(4) Uani 1 1 d . . . C4 C 0.3961(4) 0.9159(4) 0.9860(5) 0.032(2) Uani 1 1 d . . . C5 C 0.4045(7) 0.9653(7) 0.8927(10) 0.106(9) Uani 1 1 d . . . H5A H 0.4033 0.9490 0.8527 0.160 Uiso 1 1 calc R . . H5B H 0.4351 0.9677 0.9202 0.160 Uiso 1 1 calc R . . H5C H 0.3926 0.9926 0.8790 0.160 Uiso 1 1 calc R . . C6 C 0.4450(5) 0.9051(4) 1.0080(6) 0.046(3) Uani 1 1 d . . . C7 C 0.4742(5) 0.9206(6) 1.0662(8) 0.068(5) Uani 1 1 d . . . H7 H 0.4643 0.9405 1.0915 0.082 Uiso 1 1 calc R . . C8 C 0.5184(6) 0.9075(6) 1.0883(7) 0.063(4) Uani 1 1 d . . . H8 H 0.5369 0.9188 1.1284 0.076 Uiso 1 1 calc R . . C9 C 0.5355(5) 0.8797(6) 1.0552(7) 0.058(4) Uani 1 1 d . . . C10 C 0.5056(5) 0.8621(5) 0.9947(8) 0.061(4) Uani 1 1 d . . . H10 H 0.5158 0.8419 0.9702 0.073 Uiso 1 1 calc R . . C11 C 0.4619(6) 0.8752(6) 0.9729(8) 0.071(5) Uani 1 1 d . . . H11 H 0.4430 0.8636 0.9334 0.085 Uiso 1 1 calc R . . C12 C 0.5838(5) 0.8646(6) 1.0793(8) 0.070(5) Uani 1 1 d . . . H12A H 0.6031 0.8877 1.0979 0.105 Uiso 1 1 calc R . . H12B H 0.5921 0.8530 1.0413 0.105 Uiso 1 1 calc R . . H12C H 0.5867 0.8437 1.1139 0.105 Uiso 1 1 calc R . . C13 C 0.1981(4) 0.9438(4) 1.0613(5) 0.036(3) Uani 1 1 d . . . C14 C 0.2174(5) 0.9629(4) 1.1733(6) 0.043(3) Uani 1 1 d . . . H14 H 0.2100 0.9651 1.2143 0.052 Uiso 1 1 calc R . . C15 C 0.2573(5) 0.9771(5) 1.1736(6) 0.048(3) Uani 1 1 d . . . C16 C 0.2650(5) 0.9794(4) 1.1078(6) 0.041(3) Uani 1 1 d . . . C17 C 0.2906(6) 0.9931(6) 1.2382(7) 0.079(6) Uani 1 1 d . . . H17A H 0.2749 1.0047 1.2680 0.118 Uiso 1 1 calc R . . H17B H 0.3089 1.0143 1.2265 0.118 Uiso 1 1 calc R . . H17C H 0.3093 0.9706 1.2609 0.118 Uiso 1 1 calc R . . C18 C 0.3049(5) 0.9987(4) 1.0939(6) 0.044(3) Uani 1 1 d . . . C19 C 0.3466(5) 0.9845(4) 1.1305(7) 0.052(4) Uani 1 1 d . . . H19 H 0.3497 0.9644 1.1644 0.063 Uiso 1 1 calc R . . C20 C 0.3839(6) 1.0010(5) 1.1154(8) 0.060(4) Uani 1 1 d . . . H20 H 0.4123 0.9922 1.1406 0.073 Uiso 1 1 calc R . . C21 C 0.3801(7) 1.0304(5) 1.0637(10) 0.075(5) Uani 1 1 d . . . C22 C 0.3375(7) 1.0434(5) 1.0289(8) 0.064(4) Uani 1 1 d . . . H22 H 0.3340 1.0636 0.9951 0.077 Uiso 1 1 calc R . . C23 C 0.3000(6) 1.0274(4) 1.0426(6) 0.050(3) Uani 1 1 d . . . H23 H 0.2716 1.0361 1.0173 0.059 Uiso 1 1 calc R . . C24 C 0.4204(9) 1.0505(8) 1.0491(12) 0.125(10) Uani 1 1 d . . . H24A H 0.4421 1.0295 1.0482 0.188 Uiso 1 1 calc R . . H24B H 0.4334 1.0705 1.0843 0.188 Uiso 1 1 calc R . . H24C H 0.4112 1.0644 1.0056 0.188 Uiso 1 1 calc R . . C25 C 0.1691(4) 0.8664(4) 0.7986(5) 0.038(3) Uani 1 1 d . . . C26 C 0.1181(4) 0.8527(4) 0.6952(6) 0.039(3) Uani 1 1 d . . . H26 H 0.1089 0.8364 0.6559 0.047 Uiso 1 1 calc R . . C27 C 0.0923(5) 0.8852(4) 0.7010(5) 0.044(3) Uani 1 1 d . . . C28 C 0.1069(4) 0.9114(4) 0.7595(5) 0.037(3) Uani 1 1 d . . . C29 C 0.0480(5) 0.8940(5) 0.6458(7) 0.069(5) Uani 1 1 d . . . H29A H 0.0506 0.9192 0.6221 0.104 Uiso 1 1 calc R . . H29B H 0.0243 0.8968 0.6669 0.104 Uiso 1 1 calc R . . H29C H 0.0413 0.8712 0.6138 0.104 Uiso 1 1 calc R . . C30 C 0.0864(5) 0.9497(4) 0.7752(6) 0.046(3) Uani 1 1 d . . . C31 C 0.0799(5) 0.9842(5) 0.7325(7) 0.052(4) Uani 1 1 d . . . H31 H 0.0849 0.9817 0.6898 0.062 Uiso 1 1 calc R . . C32 C 0.0660(6) 1.0225(5) 0.7516(8) 0.063(4) Uani 1 1 d . . . H32 H 0.0633 1.0457 0.7232 0.076 Uiso 1 1 calc R . . C33 C 0.0565(6) 1.0253(4) 0.8123(8) 0.060(4) Uani 1 1 d . . . C34 C 0.0614(5) 0.9910(4) 0.8552(7) 0.054(4) Uani 1 1 d . . . H34 H 0.0548 0.9930 0.8967 0.065 Uiso 1 1 calc R . . C35 C 0.0760(5) 0.9548(5) 0.8358(6) 0.050(4) Uani 1 1 d . . . H35 H 0.0791 0.9320 0.8650 0.060 Uiso 1 1 calc R . . C36 C 0.0435(9) 1.0670(6) 0.8364(10) 0.098(7) Uani 1 1 d . . . H36A H 0.0624 1.0885 0.8273 0.146 Uiso 1 1 calc R . . H36B H 0.0470 1.0657 0.8847 0.146 Uiso 1 1 calc R . . H36C H 0.0128 1.0730 0.8124 0.146 Uiso 1 1 calc R . . C37 C 0.0751(4) 0.7135(4) 0.9658(6) 0.041(3) Uani 1 1 d . . . C38 C 0.0053(4) 0.7483(4) 0.9381(5) 0.036(3) Uani 1 1 d . . . C39 C -0.0068(5) 0.7267(4) 0.8749(6) 0.046(3) Uani 1 1 d . . . C40 C 0.0236(4) 0.6990(4) 0.8638(5) 0.038(3) Uani 1 1 d . . . H40 H 0.0156 0.6850 0.8221 0.045 Uiso 1 1 calc R . . C41 C -0.0501(5) 0.7379(5) 0.8210(7) 0.059(4) Uani 1 1 d . . . H41A H -0.0456 0.7624 0.7969 0.088 Uiso 1 1 calc R . . H41B H -0.0731 0.7431 0.8428 0.088 Uiso 1 1 calc R . . H41C H -0.0590 0.7152 0.7893 0.088 Uiso 1 1 calc R . . C42 C -0.0245(4) 0.7746(5) 0.9652(6) 0.044(3) Uani 1 1 d . . . C43 C -0.0102(6) 0.8123(5) 0.9923(7) 0.061(4) Uani 1 1 d . . . H43 H 0.0174 0.8223 0.9904 0.073 Uiso 1 1 calc R . . C44 C -0.0363(5) 0.8365(5) 1.0231(7) 0.056(4) Uani 1 1 d . . . H44 H -0.0264 0.8627 1.0405 0.068 Uiso 1 1 calc R . . C45 C -0.0768(6) 0.8212(5) 1.0274(7) 0.057(4) Uani 1 1 d . . . C46 C -0.0904(5) 0.7831(5) 1.0009(6) 0.054(4) Uani 1 1 d . . . H46 H -0.1172 0.7721 1.0046 0.065 Uiso 1 1 calc R . . C47 C -0.0647(5) 0.7602(5) 0.9681(7) 0.052(4) Uani 1 1 d . . . H47 H -0.0753 0.7348 0.9480 0.062 Uiso 1 1 calc R . . C48 C -0.1081(6) 0.8465(6) 1.0583(9) 0.078(5) Uani 1 1 d . . . H48A H -0.1386 0.8410 1.0331 0.117 Uiso 1 1 calc R . . H48B H -0.1020 0.8757 1.0557 0.117 Uiso 1 1 calc R . . H48C H -0.1032 0.8387 1.1053 0.117 Uiso 1 1 calc R . . C49 C 0.2008(4) 0.7036(3) 1.2220(5) 0.029(2) Uani 1 1 d . . . C50 C 0.1447(5) 0.6648(4) 1.2454(6) 0.045(3) Uani 1 1 d . . . H50 H 0.1144 0.6606 1.2397 0.054 Uiso 1 1 calc R . . C51 C 0.1738(5) 0.6353(4) 1.2827(7) 0.051(4) Uani 1 1 d . . . C52 C 0.2184(5) 0.6440(4) 1.2886(6) 0.042(3) Uani 1 1 d . . . C53 C 0.1572(6) 0.5989(4) 1.3116(9) 0.070(5) Uani 1 1 d . . . H53A H 0.1399 0.5817 1.2751 0.105 Uiso 1 1 calc R . . H53B H 0.1389 0.6080 1.3394 0.105 Uiso 1 1 calc R . . H53C H 0.1821 0.5832 1.3392 0.105 Uiso 1 1 calc R . . C54 C 0.2551(5) 0.6158(4) 1.3307(7) 0.043(3) Uani 1 1 d . . . C55 C 0.2782(5) 0.5875(5) 1.2995(7) 0.055(4) Uani 1 1 d . . . H55 H 0.2695 0.5845 1.2521 0.066 Uiso 1 1 calc R . . C56 C 0.3122(5) 0.5651(4) 1.3374(7) 0.050(3) Uani 1 1 d . . . H56 H 0.3276 0.5479 1.3151 0.060 Uiso 1 1 calc R . . C57 C 0.3260(5) 0.5660(4) 1.4081(7) 0.047(3) Uani 1 1 d . . . C58 C 0.3023(7) 0.5932(6) 1.4375(8) 0.086(7) Uani 1 1 d . . . H58 H 0.3102 0.5946 1.4850 0.104 Uiso 1 1 calc R . . C59 C 0.2681(7) 0.6182(5) 1.4016(8) 0.075(6) Uani 1 1 d . . . H59 H 0.2538 0.6364 1.4242 0.091 Uiso 1 1 calc R . . C60 C 0.3646(6) 0.5399(5) 1.4508(8) 0.074(5) Uani 1 1 d . . . H60A H 0.3565 0.5278 1.4886 0.110 Uiso 1 1 calc R . . H60B H 0.3905 0.5572 1.4678 0.110 Uiso 1 1 calc R . . H60C H 0.3713 0.5181 1.4230 0.110 Uiso 1 1 calc R . . C61 C 0.1304(5) 0.8349(4) 1.1813(6) 0.041(3) Uani 1 1 d . . . C62 C 0.1629(5) 0.8829(4) 1.2634(6) 0.048(3) Uani 1 1 d . . . H62 H 0.1706 0.9102 1.2770 0.058 Uiso 1 1 calc R . . C63 C 0.1741(5) 0.8513(5) 1.3125(6) 0.050(4) Uani 1 1 d . . . C64 C 0.1572(5) 0.8118(4) 1.2923(6) 0.045(3) Uani 1 1 d . . . C65 C 0.2038(6) 0.8624(5) 1.3827(6) 0.072(5) Uani 1 1 d . . . H65A H 0.1946 0.8470 1.4167 0.108 Uiso 1 1 calc R . . H65B H 0.2014 0.8917 1.3905 0.108 Uiso 1 1 calc R . . H65C H 0.2343 0.8557 1.3858 0.108 Uiso 1 1 calc R . . C66 C 0.1601(5) 0.7759(4) 1.3404(6) 0.046(3) Uani 1 1 d . . . C67 C 0.1215(5) 0.7548(5) 1.3397(7) 0.052(4) Uani 1 1 d . . . H67 H 0.0942 0.7635 1.3108 0.063 Uiso 1 1 calc R . . C68 C 0.1232(6) 0.7207(5) 1.3814(7) 0.064(5) Uani 1 1 d . . . H68 H 0.0969 0.7068 1.3806 0.077 Uiso 1 1 calc R . . C69 C 0.1631(7) 0.7071(5) 1.4240(7) 0.064(5) Uani 1 1 d . . . C70 C 0.2023(7) 0.7271(6) 1.4221(7) 0.076(6) Uani 1 1 d . . . H70 H 0.2297 0.7171 1.4490 0.091 Uiso 1 1 calc R . . C71 C 0.2013(6) 0.7624(5) 1.3798(6) 0.058(4) Uani 1 1 d . . . H71 H 0.2275 0.7758 1.3787 0.070 Uiso 1 1 calc R . . C72 C 0.1659(8) 0.6697(6) 1.4713(9) 0.096(8) Uani 1 1 d . . . H72A H 0.1639 0.6791 1.5150 0.144 Uiso 1 1 calc R . . H72B H 0.1939 0.6556 1.4770 0.144 Uiso 1 1 calc R . . H72C H 0.1417 0.6510 1.4515 0.144 Uiso 1 1 calc R . . C75 C 0.5165(18) 0.9996(16) 1.228(2) 0.098(14) Uiso 0.50 1 d P . . N14 N 0.5000 0.975(3) 1.2500 0.35(4) Uiso 1 2 d S . . C73 C 0.022(2) 0.6111(18) 1.233(3) 0.110(16) Uiso 0.50 1 d P . . N13 N 0.0411(19) 0.5858(17) 1.218(2) 0.151(19) Uiso 0.50 1 d P . . C76 C 0.5211(19) 1.0245(17) 1.198(3) 0.115(16) Uiso 0.50 1 d P . . C74 C -0.019(3) 0.628(2) 1.215(3) 0.16(3) Uiso 0.50 1 d P . . C78 C 0.047(2) 1.1527(19) 0.761(3) 0.122(19) Uiso 0.50 1 d P . . C77 C 0.010(3) 1.1692(15) 0.771(2) 0.118(18) Uiso 0.50 1 d P . . N16 N -0.032(2) 1.1599(18) 0.778(3) 0.15(2) 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 0.0398(9) 0.0461(9) 0.0355(7) 0.0019(6) 0.0094(6) 0.0029(8) Cu2 0.0451(10) 0.0509(9) 0.0316(7) -0.0036(6) 0.0064(6) 0.0002(8) Cu3 0.0429(10) 0.0471(9) 0.0336(7) -0.0023(6) 0.0063(6) -0.0002(8) Cu4 0.0430(10) 0.0491(9) 0.0393(8) -0.0044(6) 0.0022(7) -0.0024(8) Cu5 0.0406(10) 0.0402(8) 0.0433(8) 0.0013(6) 0.0039(7) -0.0007(8) Cu6 0.0438(10) 0.0420(9) 0.0384(8) -0.0019(6) -0.0018(7) 0.0010(8) Cu7 0.0550(12) 0.0486(10) 0.0480(9) 0.0033(7) -0.0044(8) -0.0108(9) Cu8 0.0392(9) 0.0487(9) 0.0345(7) 0.0000(6) 0.0046(6) 0.0020(8) Cu9 0.0400(10) 0.0491(9) 0.0336(7) 0.0072(6) 0.0059(6) -0.0022(8) Cu10 0.0479(11) 0.0665(11) 0.0347(8) 0.0021(7) 0.0072(7) -0.0039(9) Cu11 0.0384(9) 0.0389(8) 0.0390(7) -0.0004(6) 0.0031(6) 0.0017(7) Cu12 0.0349(9) 0.0417(8) 0.0413(8) 0.0031(6) 0.0028(6) -0.0034(7) Cu13 0.0412(11) 0.0654(12) 0.0501(9) -0.0096(8) 0.0010(7) 0.0068(9) Cu14 0.0446(10) 0.0496(9) 0.0384(8) -0.0038(6) 0.0099(7) -0.0020(8) Cu15 0.0497(11) 0.0417(9) 0.0402(8) -0.0038(6) 0.0148(7) -0.0026(8) I1 0.0555(6) 0.0483(5) 0.0449(5) 0.0114(4) 0.0059(4) 0.0005(5) I2 0.0417(6) 0.0787(7) 0.0497(5) 0.0004(4) 0.0092(4) -0.0094(5) I3 0.0485(6) 0.0599(6) 0.0376(4) -0.0071(4) -0.0003(4) 0.0001(5) I4 0.0521(6) 0.0541(5) 0.0372(4) -0.0062(3) -0.0010(4) -0.0039(5) I5 0.0624(7) 0.0450(5) 0.0634(6) -0.0007(4) 0.0308(5) 0.0035(5) I6 0.0327(4) 0.0370(4) 0.0316(4) 0.0005(3) 0.0023(3) -0.0001(3) I7 0.0379(5) 0.0478(5) 0.0393(4) -0.0027(3) 0.0066(3) 0.0000(4) I8 0.0428(6) 0.0567(6) 0.0628(6) -0.0042(4) 0.0145(4) 0.0093(5) S1 0.0306(16) 0.0399(16) 0.0381(14) 0.0012(11) 0.0037(12) -0.0045(14) S2 0.0392(18) 0.0507(18) 0.0317(14) -0.0049(12) 0.0098(12) -0.0016(16) S3 0.0375(18) 0.0477(17) 0.0284(13) 0.0009(11) 0.0055(11) 0.0005(15) S4 0.0328(17) 0.0379(16) 0.0346(14) 0.0000(11) -0.0025(11) 0.0007(14) S5 0.0373(18) 0.0360(15) 0.0359(14) 0.0068(11) 0.0002(12) -0.0029(14) S6 0.046(2) 0.0389(16) 0.0341(14) -0.0025(11) 0.0014(13) 0.0034(15) S7 0.044(2) 0.0442(17) 0.0337(14) -0.0038(12) 0.0069(12) 0.0074(15) S8 0.035(2) 0.030(2) 0.0259(15) 0.0021(12) 0.0010(13) 0.0010(16) S8A 0.015(8) 0.021(9) 0.047(9) 0.001(6) 0.009(6) 0.014(6) N1 0.033(6) 0.037(5) 0.036(5) 0.003(4) 0.011(4) 0.007(5) N2 0.033(6) 0.031(5) 0.040(5) -0.009(4) 0.002(4) 0.000(5) N3 0.049(7) 0.021(4) 0.022(4) 0.001(3) -0.006(4) -0.005(4) N4 0.033(6) 0.043(6) 0.036(5) 0.000(4) 0.011(4) -0.011(5) N5 0.044(7) 0.039(5) 0.025(4) 0.001(4) 0.005(4) 0.006(5) N6 0.050(7) 0.036(5) 0.028(5) -0.007(4) 0.006(4) -0.008(5) N7 0.030(6) 0.044(6) 0.033(5) 0.009(4) -0.009(4) -0.006(5) N8 0.037(6) 0.054(6) 0.025(4) 0.004(4) -0.004(4) -0.003(5) N9 0.051(7) 0.025(5) 0.047(6) -0.002(4) 0.010(5) 0.010(5) N10 0.031(6) 0.052(6) 0.026(4) 0.002(4) 0.005(4) 0.000(5) N11 0.035(6) 0.032(5) 0.043(5) -0.004(4) 0.000(4) 0.012(5) N12 0.038(6) 0.057(7) 0.036(5) -0.008(5) 0.010(4) 0.000(6) C1 0.037(7) 0.035(6) 0.038(6) 0.005(5) 0.002(5) -0.006(6) C2 0.038(8) 0.053(8) 0.043(7) 0.006(5) 0.016(5) 0.004(7) C3 0.046(9) 0.057(9) 0.055(8) 0.010(6) 0.012(6) 0.014(8) C4 0.030(6) 0.034(6) 0.031(5) 0.006(4) 0.010(4) -0.004(5) C5 0.079(15) 0.16(2) 0.099(14) 0.087(14) 0.048(12) 0.028(15) C6 0.058(10) 0.044(7) 0.042(7) 0.005(5) 0.026(6) 0.002(7) C7 0.040(9) 0.093(13) 0.066(10) -0.008(8) 0.006(7) 0.030(9) C8 0.056(10) 0.087(12) 0.047(8) 0.002(7) 0.017(7) 0.014(10) C9 0.030(8) 0.082(11) 0.062(9) 0.015(8) 0.010(6) 0.000(8) C10 0.033(8) 0.074(11) 0.076(10) -0.025(8) 0.015(7) -0.009(8) C11 0.046(10) 0.102(14) 0.063(9) 0.005(9) 0.010(7) -0.022(10) C12 0.038(9) 0.102(14) 0.071(10) 0.010(9) 0.016(7) 0.018(10) C13 0.041(8) 0.034(6) 0.030(5) 0.000(4) 0.005(5) 0.014(6) C14 0.043(8) 0.059(8) 0.031(6) 0.000(5) 0.015(5) -0.014(7) C15 0.046(8) 0.064(9) 0.030(6) -0.019(5) 0.003(5) 0.002(7) C16 0.059(9) 0.026(6) 0.038(6) 0.007(4) 0.014(6) 0.000(6) C17 0.070(13) 0.121(16) 0.047(8) -0.026(9) 0.022(8) -0.027(12) C18 0.040(8) 0.047(7) 0.040(6) -0.013(5) 0.005(5) 0.000(6) C19 0.052(10) 0.041(7) 0.069(9) 0.002(6) 0.023(7) 0.008(7) C20 0.054(10) 0.050(9) 0.081(10) 0.001(7) 0.025(8) -0.005(8) C21 0.075(14) 0.052(10) 0.118(14) -0.012(9) 0.063(12) -0.017(10) C22 0.077(13) 0.046(9) 0.073(10) -0.006(7) 0.028(9) -0.005(9) C23 0.061(10) 0.048(8) 0.044(7) 0.001(6) 0.022(6) 0.000(7) C24 0.11(2) 0.14(2) 0.14(2) -0.017(17) 0.077(17) -0.079(19) C25 0.040(7) 0.044(7) 0.027(5) 0.006(4) 0.006(5) 0.004(6) C26 0.035(7) 0.041(7) 0.036(6) -0.004(5) 0.003(5) 0.001(6) C27 0.049(9) 0.057(8) 0.022(5) -0.008(5) 0.005(5) 0.000(7) C28 0.033(7) 0.047(7) 0.029(5) 0.008(5) 0.006(5) 0.003(6) C29 0.052(10) 0.082(12) 0.052(8) -0.015(8) -0.019(7) 0.017(9) C30 0.040(8) 0.051(8) 0.042(7) 0.000(5) 0.005(5) 0.017(7) C31 0.047(9) 0.064(9) 0.045(7) 0.003(6) 0.016(6) 0.005(8) C32 0.067(12) 0.058(9) 0.068(10) 0.005(7) 0.024(8) 0.022(9) C33 0.070(12) 0.036(7) 0.068(9) -0.004(6) 0.008(8) 0.017(8) C34 0.063(11) 0.044(8) 0.056(8) 0.005(6) 0.019(7) 0.021(8) C35 0.038(8) 0.072(10) 0.035(6) 0.007(6) 0.002(5) 0.011(7) C36 0.14(2) 0.063(12) 0.107(15) -0.014(10) 0.061(15) 0.016(14) C37 0.031(7) 0.043(7) 0.038(6) 0.010(5) -0.006(5) -0.010(6) C38 0.030(7) 0.045(7) 0.028(5) -0.005(4) 0.000(4) -0.012(6) C39 0.035(8) 0.054(8) 0.038(6) 0.010(5) -0.009(5) -0.012(7) C40 0.024(6) 0.057(8) 0.028(5) -0.011(5) 0.003(4) 0.005(6) C41 0.045(9) 0.062(9) 0.051(8) -0.006(6) -0.014(7) -0.003(8) C42 0.027(7) 0.061(9) 0.036(6) 0.001(5) -0.006(5) -0.006(6) C43 0.046(10) 0.071(11) 0.062(9) 0.023(7) 0.010(7) 0.000(8) C44 0.049(10) 0.068(10) 0.049(8) -0.020(7) 0.008(6) 0.002(8) C45 0.055(10) 0.065(10) 0.055(8) 0.003(7) 0.025(7) 0.020(9) C46 0.043(9) 0.079(11) 0.042(7) -0.003(7) 0.012(6) -0.008(8) C47 0.041(9) 0.053(8) 0.057(8) -0.008(6) 0.009(6) -0.013(7) C48 0.070(13) 0.088(13) 0.084(12) -0.007(10) 0.034(10) 0.025(11) C49 0.025(6) 0.027(5) 0.031(5) 0.000(4) 0.002(4) 0.003(5) C50 0.047(9) 0.033(6) 0.055(7) 0.015(5) 0.013(6) -0.001(6) C51 0.049(9) 0.042(7) 0.058(8) 0.011(6) 0.006(7) -0.009(7) C52 0.059(9) 0.029(6) 0.034(6) 0.007(4) 0.009(5) 0.011(6) C53 0.070(12) 0.031(7) 0.106(12) 0.037(8) 0.019(9) -0.011(8) C54 0.042(8) 0.036(7) 0.058(8) 0.000(5) 0.024(6) 0.001(6) C55 0.057(10) 0.074(10) 0.041(7) 0.012(6) 0.024(6) 0.011(9) C56 0.037(8) 0.045(8) 0.061(8) 0.005(6) 0.004(6) 0.014(7) C57 0.043(8) 0.023(6) 0.067(8) 0.010(5) 0.003(6) -0.001(6) C58 0.105(17) 0.090(13) 0.045(8) -0.010(8) -0.009(9) 0.035(13) C59 0.082(14) 0.076(12) 0.059(9) 0.000(8) 0.005(9) 0.036(11) C60 0.061(12) 0.062(10) 0.076(10) 0.013(8) -0.016(9) 0.013(9) C61 0.046(8) 0.034(6) 0.039(6) -0.010(5) 0.004(5) -0.006(6) C62 0.049(9) 0.051(8) 0.040(6) -0.011(5) 0.006(6) -0.013(7) C63 0.056(9) 0.068(9) 0.024(5) -0.013(5) 0.011(5) -0.012(8) C64 0.040(8) 0.052(8) 0.045(7) -0.005(6) 0.014(6) -0.003(7) C65 0.104(15) 0.086(12) 0.021(6) -0.007(6) 0.010(7) -0.027(11) C66 0.057(10) 0.041(7) 0.039(6) 0.005(5) 0.013(6) -0.011(7) C67 0.042(9) 0.060(9) 0.052(8) 0.004(6) 0.009(6) -0.012(8) C68 0.076(13) 0.072(11) 0.056(9) 0.000(7) 0.038(8) -0.028(10) C69 0.100(15) 0.052(9) 0.037(7) -0.005(6) 0.017(8) -0.010(10) C70 0.088(15) 0.085(12) 0.037(8) -0.012(7) -0.008(8) 0.024(12) C71 0.062(11) 0.068(10) 0.038(7) -0.001(6) 0.003(6) -0.014(9) C72 0.14(2) 0.067(12) 0.072(12) 0.002(9) 0.010(12) -0.007(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 1.997(10) . ? Cu1 N3 2.002(9) . ? Cu1 I1 2.5726(18) . ? Cu1 Cu2 2.594(2) . ? Cu1 Cu3 2.904(2) . ? Cu2 N5 2.001(9) . ? Cu2 S2 2.237(3) . ? Cu2 I1 2.573(2) . ? Cu2 Cu3 2.788(2) . ? Cu3 S3 2.299(3) . ? Cu3 S2 2.323(4) . ? Cu3 S1 2.431(4) . ? Cu3 S7 2.457(4) . ? Cu4 N7 2.003(10) . ? Cu4 S6 2.251(4) . ? Cu4 Cu5 2.545(2) . ? Cu4 I2 2.583(2) . ? Cu4 Cu6 2.763(3) . ? Cu5 N9 1.995(10) . ? Cu5 N11 2.009(10) . ? Cu5 I2 2.569(2) . ? Cu5 Cu6 2.918(3) . ? Cu6 S4 2.289(3) . ? Cu6 S6 2.327(4) . ? Cu6 S5 2.365(3) . ? Cu6 S7 2.542(4) . ? Cu7 S5 2.268(4) 7_567 ? Cu7 I3 2.540(2) . ? Cu7 I5 2.564(2) . ? Cu7 Cu8 2.831(3) . ? Cu7 Cu9 2.912(2) . ? Cu8 N6 2.001(11) . ? Cu8 N10 2.023(11) 7_567 ? Cu8 I3 2.5480(18) . ? Cu8 Cu9 2.795(2) . ? Cu9 S3 2.302(4) . ? Cu9 S5 2.320(4) 7_567 ? Cu9 S8 2.386(3) 7_567 ? Cu9 S8A 2.386(15) 7_567 ? Cu9 I6 2.6646(19) . ? Cu10 S1 2.297(3) 7_567 ? Cu10 I5 2.564(2) . ? Cu10 I4 2.578(2) . ? Cu10 Cu11 2.709(3) . ? Cu10 Cu12 2.811(2) . ? Cu11 N8 1.969(11) . ? Cu11 N2 2.003(10) 7_567 ? Cu11 I4 2.5467(17) . ? Cu11 Cu12 2.789(2) . ? Cu12 S4 2.313(4) . ? Cu12 S8 2.346(4) . ? Cu12 S1 2.360(4) 7_567 ? Cu12 S8A 2.478(17) . ? Cu12 I6 2.6618(17) . ? Cu13 S7 2.226(4) . ? Cu13 I7 2.488(2) . ? Cu13 I6 2.676(2) . ? Cu14 S2 2.369(4) . ? Cu14 S6 2.370(3) . ? Cu14 Cu15 2.582(2) . ? Cu14 I7 2.6311(17) . ? Cu14 I8 2.682(2) . ? Cu15 N4 2.000(10) . ? Cu15 N12 2.015(11) . ? Cu15 I8 2.523(2) . ? S1 C1 1.769(13) . ? S1 Cu10 2.297(3) 7_567 ? S1 Cu12 2.360(4) 7_567 ? S2 C13 1.744(12) . ? S3 C25 1.749(12) . ? S4 C37 1.737(12) . ? S5 C49 1.745(11) . ? S5 Cu7 2.268(4) 7_567 ? S5 Cu9 2.320(4) 7_567 ? S6 C61 1.788(11) . ? S7 S8 2.105(5) 7_567 ? S7 S8A 2.172(15) . ? S8 S8 2.099(7) 7_567 ? S8 S7 2.105(5) 7_567 ? S8 Cu9 2.386(3) 7_567 ? S8A S8A 2.07(3) 7_567 ? S8A Cu9 2.386(15) 7_567 ? N1 C2 1.339(16) . ? N1 C1 1.358(14) . ? N2 C1 1.323(16) . ? N2 C4 1.355(14) . ? N2 Cu11 2.003(10) 7_567 ? N3 C13 1.340(16) . ? N3 C16 1.367(15) . ? N4 C13 1.354(14) . ? N4 C14 1.355(15) . ? N5 C25 1.361(15) . ? N5 C28 1.372(14) . ? N6 C25 1.337(14) . ? N6 C26 1.352(15) . ? N7 C37 1.354(17) . ? N7 C38 1.362(15) . ? N8 C40 1.322(14) . ? N8 C37 1.381(15) . ? N9 C50 1.321(15) . ? N9 C49 1.384(16) . ? N10 C49 1.336(14) . ? N10 C52 1.374(16) . ? N10 Cu8 2.023(11) 7_567 ? N11 C61 1.292(15) . ? N11 C64 1.366(15) . ? N12 C62 1.341(15) . ? N12 C61 1.360(16) . ? C2 C3 1.352(19) . ? C3 C4 1.393(16) . ? C3 C5 1.52(2) . ? C4 C6 1.502(18) . ? C6 C7 1.37(2) . ? C6 C11 1.39(2) . ? C7 C8 1.39(2) . ? C8 C9 1.32(2) . ? C9 C10 1.43(2) . ? C9 C12 1.52(2) . ? C10 C11 1.37(2) . ? C14 C15 1.324(19) . ? C15 C16 1.433(16) . ? C15 C17 1.515(18) . ? C16 C18 1.488(19) . ? C18 C23 1.369(18) . ? C18 C19 1.378(19) . ? C19 C20 1.39(2) . ? C20 C21 1.39(2) . ? C21 C22 1.38(3) . ? C21 C24 1.52(2) . ? C22 C23 1.38(2) . ? C26 C27 1.343(18) . ? C27 C28 1.422(15) . ? C27 C29 1.538(18) . ? C28 C30 1.463(17) . ? C30 C35 1.376(17) . ? C30 C31 1.387(19) . ? C31 C32 1.40(2) . ? C32 C33 1.36(2) . ? C33 C34 1.386(19) . ? C33 C36 1.52(2) . ? C34 C35 1.348(19) . ? C38 C39 1.415(16) . ? C38 C42 1.475(19) . ? C39 C40 1.365(18) . ? C39 C41 1.519(17) . ? C42 C43 1.35(2) . ? C42 C47 1.355(19) . ? C43 C44 1.40(2) . ? C44 C45 1.38(2) . ? C45 C46 1.35(2) . ? C45 C48 1.54(2) . ? C46 C47 1.39(2) . ? C50 C51 1.379(18) . ? C51 C52 1.39(2) . ? C51 C53 1.468(17) . ? C52 C54 1.518(17) . ? C54 C59 1.388(19) . ? C54 C55 1.419(19) . ? C55 C56 1.330(18) . ? C56 C57 1.380(18) . ? C57 C58 1.39(2) . ? C57 C60 1.520(18) . ? C58 C59 1.37(2) . ? C62 C63 1.398(19) . ? C63 C64 1.388(19) . ? C63 C65 1.508(17) . ? C64 C66 1.498(17) . ? C66 C71 1.38(2) . ? C66 C67 1.378(19) . ? C67 C68 1.38(2) . ? C68 C69 1.37(2) . ? C69 C70 1.39(3) . ? C69 C72 1.53(2) . ? C70 C71 1.42(2) . ? C75 C76 1.04(6) . ? C75 N14 1.10(7) . ? C75 C75 1.55(11) 2_657 ? N14 C75 1.10(7) 2_657 ? C73 N13 1.09(6) . ? C73 C74 1.22(7) 2_557 ? C73 C74 1.36(7) . ? C74 C73 1.22(7) 2_557 ? C74 C74 1.58(13) 2_557 ? C78 N16 0.83(7) 2_556 ? C78 C77 1.32(8) . ? C77 N16 1.40(8) . ? C77 N16 1.39(10) 2_556 ? N16 C78 0.83(7) 2_556 ? N16 C77 1.39(10) 2_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N3 120.2(4) . . ? N1 Cu1 I1 117.5(3) . . ? N3 Cu1 I1 118.2(3) . . ? N1 Cu1 Cu2 130.0(3) . . ? N3 Cu1 Cu2 96.2(3) . . ? I1 Cu1 Cu2 59.73(6) . . ? N1 Cu1 Cu3 89.7(3) . . ? N3 Cu1 Cu3 82.3(3) . . ? I1 Cu1 Cu3 118.30(7) . . ? Cu2 Cu1 Cu3 60.63(6) . . ? N5 Cu2 S2 120.4(3) . . ? N5 Cu2 I1 111.8(3) . . ? S2 Cu2 I1 127.71(11) . . ? N5 Cu2 Cu1 132.7(3) . . ? S2 Cu2 Cu1 81.90(11) . . ? I1 Cu2 Cu1 59.72(6) . . ? N5 Cu2 Cu3 93.6(3) . . ? S2 Cu2 Cu3 53.70(10) . . ? I1 Cu2 Cu3 122.67(8) . . ? Cu1 Cu2 Cu3 65.20(6) . . ? S3 Cu3 S2 123.80(13) . . ? S3 Cu3 S1 108.31(14) . . ? S2 Cu3 S1 119.10(13) . . ? S3 Cu3 S7 106.34(12) . . ? S2 Cu3 S7 100.49(13) . . ? S1 Cu3 S7 92.16(12) . . ? S3 Cu3 Cu2 77.30(10) . . ? S2 Cu3 Cu2 50.92(9) . . ? S1 Cu3 Cu2 127.00(11) . . ? S7 Cu3 Cu2 138.22(12) . . ? S3 Cu3 Cu1 94.34(10) . . ? S2 Cu3 Cu1 73.94(10) . . ? S1 Cu3 Cu1 72.85(9) . . ? S7 Cu3 Cu1 157.60(9) . . ? Cu2 Cu3 Cu1 54.16(6) . . ? N7 Cu4 S6 119.3(3) . . ? N7 Cu4 Cu5 134.7(3) . . ? S6 Cu4 Cu5 82.23(10) . . ? N7 Cu4 I2 109.0(3) . . ? S6 Cu4 I2 131.59(10) . . ? Cu5 Cu4 I2 60.13(6) . . ? N7 Cu4 Cu6 93.2(3) . . ? S6 Cu4 Cu6 54.16(10) . . ? Cu5 Cu4 Cu6 66.55(7) . . ? I2 Cu4 Cu6 122.45(8) . . ? N9 Cu5 N11 120.6(4) . . ? N9 Cu5 Cu4 128.7(3) . . ? N11 Cu5 Cu4 97.1(3) . . ? N9 Cu5 I2 113.4(3) . . ? N11 Cu5 I2 122.1(3) . . ? Cu4 Cu5 I2 60.65(6) . . ? N9 Cu5 Cu6 88.2(3) . . ? N11 Cu5 Cu6 84.6(3) . . ? Cu4 Cu5 Cu6 60.30(6) . . ? I2 Cu5 Cu6 117.17(7) . . ? S4 Cu6 S6 125.07(14) . . ? S4 Cu6 S5 106.85(12) . . ? S6 Cu6 S5 119.79(12) . . ? S4 Cu6 S7 110.34(13) . . ? S6 Cu6 S7 93.30(13) . . ? S5 Cu6 S7 95.41(13) . . ? S4 Cu6 Cu4 77.71(11) . . ? S6 Cu6 Cu4 51.62(10) . . ? S5 Cu6 Cu4 127.88(12) . . ? S7 Cu6 Cu4 132.69(10) . . ? S4 Cu6 Cu5 94.37(11) . . ? S6 Cu6 Cu5 73.16(10) . . ? S5 Cu6 Cu5 74.78(10) . . ? S7 Cu6 Cu5 155.21(10) . . ? Cu4 Cu6 Cu5 53.16(6) . . ? S5 Cu7 I3 122.71(11) 7_567 . ? S5 Cu7 I5 112.66(11) 7_567 . ? I3 Cu7 I5 116.73(7) . . ? S5 Cu7 Cu8 76.29(10) 7_567 . ? I3 Cu7 Cu8 56.33(5) . . ? I5 Cu7 Cu8 170.97(9) . . ? S5 Cu7 Cu9 51.41(10) 7_567 . ? I3 Cu7 Cu9 112.15(8) . . ? I5 Cu7 Cu9 125.82(7) . . ? Cu8 Cu7 Cu9 58.24(6) . . ? N6 Cu8 N10 123.8(4) . 7_567 ? N6 Cu8 I3 119.1(3) . . ? N10 Cu8 I3 113.6(3) 7_567 . ? N6 Cu8 Cu9 88.1(3) . . ? N10 Cu8 Cu9 85.9(2) 7_567 . ? I3 Cu8 Cu9 115.82(7) . . ? N6 Cu8 Cu7 130.8(3) . . ? N10 Cu8 Cu7 94.1(3) 7_567 . ? I3 Cu8 Cu7 56.07(5) . . ? Cu9 Cu8 Cu7 62.33(6) . . ? S3 Cu9 S5 119.19(13) . 7_567 ? S3 Cu9 S8 93.25(12) . 7_567 ? S5 Cu9 S8 107.43(14) 7_567 7_567 ? S3 Cu9 S8A 114.2(4) . 7_567 ? S5 Cu9 S8A 84.3(4) 7_567 7_567 ? S8 Cu9 S8A 25.4(4) 7_567 7_567 ? S3 Cu9 I6 116.02(11) . . ? S5 Cu9 I6 115.91(10) 7_567 . ? S8 Cu9 I6 99.21(11) 7_567 . ? S8A Cu9 I6 100.9(4) 7_567 . ? S3 Cu9 Cu8 75.07(8) . . ? S5 Cu9 Cu8 76.24(9) 7_567 . ? S8 Cu9 Cu8 167.83(12) 7_567 . ? S8A Cu9 Cu8 160.5(4) 7_567 . ? I6 Cu9 Cu8 89.18(7) . . ? S3 Cu9 Cu7 134.41(9) . . ? S5 Cu9 Cu7 49.82(9) 7_567 . ? S8 Cu9 Cu7 131.92(11) 7_567 . ? S8A Cu9 Cu7 108.5(4) 7_567 . ? I6 Cu9 Cu7 68.87(6) . . ? Cu8 Cu9 Cu7 59.43(6) . . ? S1 Cu10 I5 108.05(12) 7_567 . ? S1 Cu10 I4 126.02(12) 7_567 . ? I5 Cu10 I4 118.21(7) . . ? S1 Cu10 Cu11 78.26(11) 7_567 . ? I5 Cu10 Cu11 173.28(8) . . ? I4 Cu10 Cu11 57.52(6) . . ? S1 Cu10 Cu12 53.91(9) 7_567 . ? I5 Cu10 Cu12 120.90(8) . . ? I4 Cu10 Cu12 114.56(8) . . ? Cu11 Cu10 Cu12 60.66(6) . . ? N8 Cu11 N2 123.0(4) . 7_567 ? N8 Cu11 I4 113.3(3) . . ? N2 Cu11 I4 119.9(3) 7_567 . ? N8 Cu11 Cu10 129.0(3) . . ? N2 Cu11 Cu10 96.5(3) 7_567 . ? I4 Cu11 Cu10 58.66(6) . . ? N8 Cu11 Cu12 88.6(3) . . ? N2 Cu11 Cu12 85.7(3) 7_567 . ? I4 Cu11 Cu12 116.38(8) . . ? Cu10 Cu11 Cu12 61.48(6) . . ? S4 Cu12 S8 107.16(13) . . ? S4 Cu12 S1 119.07(13) . 7_567 ? S8 Cu12 S1 91.25(13) . 7_567 ? S4 Cu12 S8A 86.8(4) . . ? S8 Cu12 S8A 24.9(4) . . ? S1 Cu12 S8A 114.1(4) 7_567 . ? S4 Cu12 I6 110.74(10) . . ? S8 Cu12 I6 102.48(10) . . ? S1 Cu12 I6 121.20(10) 7_567 . ? S8A Cu12 I6 97.1(4) . . ? S4 Cu12 Cu11 75.46(10) . . ? S8 Cu12 Cu11 165.78(11) . . ? S1 Cu12 Cu11 75.64(10) 7_567 . ? S8A Cu12 Cu11 162.3(4) . . ? I6 Cu12 Cu11 89.24(6) . . ? S4 Cu12 Cu10 133.32(11) . . ? S8 Cu12 Cu10 117.94(12) . . ? S1 Cu12 Cu10 51.85(8) 7_567 . ? S8A Cu12 Cu10 139.8(4) . . ? I6 Cu12 Cu10 71.80(6) . . ? Cu11 Cu12 Cu10 57.87(6) . . ? S7 Cu13 I7 127.66(12) . . ? S7 Cu13 I6 117.73(12) . . ? I7 Cu13 I6 114.34(7) . . ? S2 Cu14 S6 121.73(14) . . ? S2 Cu14 Cu15 79.06(9) . . ? S6 Cu14 Cu15 79.06(9) . . ? S2 Cu14 I7 101.07(9) . . ? S6 Cu14 I7 101.76(10) . . ? Cu15 Cu14 I7 178.89(9) . . ? S2 Cu14 I8 104.41(10) . . ? S6 Cu14 I8 107.42(11) . . ? Cu15 Cu14 I8 57.24(6) . . ? I7 Cu14 I8 121.71(7) . . ? N4 Cu15 N12 109.5(4) . . ? N4 Cu15 I8 125.6(3) . . ? N12 Cu15 I8 124.9(3) . . ? N4 Cu15 Cu14 103.9(3) . . ? N12 Cu15 Cu14 104.7(3) . . ? I8 Cu15 Cu14 63.37(6) . . ? Cu1 I1 Cu2 60.54(6) . . ? Cu5 I2 Cu4 59.22(6) . . ? Cu7 I3 Cu8 67.60(6) . . ? Cu11 I4 Cu10 63.82(6) . . ? Cu10 I5 Cu7 94.43(7) . . ? Cu12 I6 Cu9 99.44(6) . . ? Cu12 I6 Cu13 80.68(6) . . ? Cu9 I6 Cu13 76.18(6) . . ? Cu13 I7 Cu14 87.37(6) . . ? Cu15 I8 Cu14 59.39(5) . . ? C1 S1 Cu10 111.8(4) . 7_567 ? C1 S1 Cu12 102.5(5) . 7_567 ? Cu10 S1 Cu12 74.24(11) 7_567 7_567 ? C1 S1 Cu3 111.6(4) . . ? Cu10 S1 Cu3 135.21(16) 7_567 . ? Cu12 S1 Cu3 106.27(13) 7_567 . ? C13 S2 Cu2 113.0(4) . . ? C13 S2 Cu3 99.8(4) . . ? Cu2 S2 Cu3 75.38(11) . . ? C13 S2 Cu14 119.0(5) . . ? Cu2 S2 Cu14 123.97(15) . . ? Cu3 S2 Cu14 113.09(15) . . ? C25 S3 Cu3 113.2(4) . . ? C25 S3 Cu9 107.8(4) . . ? Cu3 S3 Cu9 104.89(13) . . ? C37 S4 Cu6 112.3(5) . . ? C37 S4 Cu12 107.5(5) . . ? Cu6 S4 Cu12 106.18(15) . . ? C49 S5 Cu7 111.8(4) . 7_567 ? C49 S5 Cu9 103.2(4) . 7_567 ? Cu7 S5 Cu9 78.77(13) 7_567 7_567 ? C49 S5 Cu6 112.3(4) . . ? Cu7 S5 Cu6 131.74(15) 7_567 . ? Cu9 S5 Cu6 108.99(13) 7_567 . ? C61 S6 Cu4 109.2(5) . . ? C61 S6 Cu6 103.4(5) . . ? Cu4 S6 Cu6 74.22(12) . . ? C61 S6 Cu14 120.0(4) . . ? Cu4 S6 Cu14 120.98(14) . . ? Cu6 S6 Cu14 119.44(16) . . ? S8 S7 S8A 49.9(5) 7_567 . ? S8 S7 Cu13 97.82(15) 7_567 . ? S8A S7 Cu13 95.3(4) . . ? S8 S7 Cu3 85.55(16) 7_567 . ? S8A S7 Cu3 135.4(5) . . ? Cu13 S7 Cu3 87.74(12) . . ? S8 S7 Cu6 124.81(18) 7_567 . ? S8A S7 Cu6 75.0(5) . . ? Cu13 S7 Cu6 82.82(13) . . ? Cu3 S7 Cu6 149.10(16) . . ? S8 S8 S7 96.8(3) 7_567 7_567 ? S8 S8 Cu12 110.7(2) 7_567 . ? S7 S8 Cu12 110.68(17) 7_567 . ? S8 S8 Cu9 107.6(2) 7_567 7_567 ? S7 S8 Cu9 108.47(17) 7_567 7_567 ? Cu12 S8 Cu9 120.03(17) . 7_567 ? S8A S8A S7 93.3(10) 7_567 . ? S8A S8A Cu9 108.1(10) 7_567 7_567 ? S7 S8A Cu9 118.9(7) . 7_567 ? S8A S8A Cu12 102.7(10) 7_567 . ? S7 S8A Cu12 114.8(6) . . ? Cu9 S8A Cu12 114.8(6) 7_567 . ? C2 N1 C1 115.6(11) . . ? C2 N1 Cu1 123.3(9) . . ? C1 N1 Cu1 119.2(9) . . ? C1 N2 C4 116.6(10) . . ? C1 N2 Cu11 119.8(9) . 7_567 ? C4 N2 Cu11 123.6(8) . 7_567 ? C13 N3 C16 118.9(10) . . ? C13 N3 Cu1 120.4(7) . . ? C16 N3 Cu1 120.4(9) . . ? C13 N4 C14 114.0(11) . . ? C13 N4 Cu15 119.6(8) . . ? C14 N4 Cu15 126.3(8) . . ? C25 N5 C28 120.0(10) . . ? C25 N5 Cu2 120.4(8) . . ? C28 N5 Cu2 119.4(8) . . ? C25 N6 C26 116.7(11) . . ? C25 N6 Cu8 117.0(9) . . ? C26 N6 Cu8 123.9(8) . . ? C37 N7 C38 121.2(10) . . ? C37 N7 Cu4 118.5(7) . . ? C38 N7 Cu4 120.0(9) . . ? C40 N8 C37 115.1(11) . . ? C40 N8 Cu11 126.3(8) . . ? C37 N8 Cu11 117.9(8) . . ? C50 N9 C49 116.9(11) . . ? C50 N9 Cu5 121.6(10) . . ? C49 N9 Cu5 119.2(8) . . ? C49 N10 C52 117.6(11) . . ? C49 N10 Cu8 117.5(8) . 7_567 ? C52 N10 Cu8 124.8(9) . 7_567 ? C61 N11 C64 119.7(11) . . ? C61 N11 Cu5 119.3(8) . . ? C64 N11 Cu5 120.9(9) . . ? C62 N12 C61 115.7(11) . . ? C62 N12 Cu15 123.9(10) . . ? C61 N12 Cu15 120.3(8) . . ? N2 C1 N1 125.1(12) . . ? N2 C1 S1 118.3(9) . . ? N1 C1 S1 116.6(10) . . ? N1 C2 C3 124.4(13) . . ? C2 C3 C4 115.4(13) . . ? C2 C3 C5 122.8(14) . . ? C4 C3 C5 121.7(14) . . ? N2 C4 C3 122.3(12) . . ? N2 C4 C6 114.0(10) . . ? C3 C4 C6 123.6(11) . . ? C7 C6 C11 116.3(15) . . ? C7 C6 C4 122.8(12) . . ? C11 C6 C4 120.7(13) . . ? C6 C7 C8 121.6(15) . . ? C9 C8 C7 123.3(16) . . ? C8 C9 C10 116.7(15) . . ? C8 C9 C12 123.9(15) . . ? C10 C9 C12 119.4(15) . . ? C11 C10 C9 119.9(16) . . ? C10 C11 C6 122.2(16) . . ? N3 C13 N4 124.4(10) . . ? N3 C13 S2 118.0(8) . . ? N4 C13 S2 117.5(10) . . ? C15 C14 N4 127.2(11) . . ? C14 C15 C16 115.2(11) . . ? C14 C15 C17 122.0(12) . . ? C16 C15 C17 122.6(14) . . ? N3 C16 C15 119.2(12) . . ? N3 C16 C18 115.7(10) . . ? C15 C16 C18 125.1(12) . . ? C23 C18 C19 121.2(15) . . ? C23 C18 C16 120.6(13) . . ? C19 C18 C16 118.0(13) . . ? C18 C19 C20 118.3(14) . . ? C19 C20 C21 121.9(17) . . ? C22 C21 C20 117.1(17) . . ? C22 C21 C24 120.0(19) . . ? C20 C21 C24 123(2) . . ? C21 C22 C23 122.2(16) . . ? C18 C23 C22 119.2(16) . . ? N6 C25 N5 123.3(11) . . ? N6 C25 S3 118.7(10) . . ? N5 C25 S3 117.9(8) . . ? C27 C26 N6 124.1(11) . . ? C26 C27 C28 118.4(12) . . ? C26 C27 C29 120.8(11) . . ? C28 C27 C29 120.8(12) . . ? N5 C28 C27 117.3(11) . . ? N5 C28 C30 114.0(10) . . ? C27 C28 C30 128.6(11) . . ? C35 C30 C31 116.1(13) . . ? C35 C30 C28 121.8(12) . . ? C31 C30 C28 121.8(12) . . ? C30 C31 C32 121.9(13) . . ? C33 C32 C31 118.6(14) . . ? C32 C33 C34 120.8(14) . . ? C32 C33 C36 120.1(15) . . ? C34 C33 C36 119.0(15) . . ? C35 C34 C33 119.0(13) . . ? C34 C35 C30 123.5(13) . . ? N7 C37 N8 122.3(11) . . ? N7 C37 S4 119.8(9) . . ? N8 C37 S4 117.8(10) . . ? N7 C38 C39 117.7(12) . . ? N7 C38 C42 116.0(10) . . ? C39 C38 C42 126.0(12) . . ? C40 C39 C38 116.9(11) . . ? C40 C39 C41 123.3(12) . . ? C38 C39 C41 119.5(13) . . ? N8 C40 C39 126.5(11) . . ? C43 C42 C47 119.1(15) . . ? C43 C42 C38 119.8(14) . . ? C47 C42 C38 120.9(13) . . ? C42 C43 C44 121.1(16) . . ? C45 C44 C43 119.4(15) . . ? C46 C45 C44 118.8(15) . . ? C46 C45 C48 118.5(16) . . ? C44 C45 C48 122.6(16) . . ? C45 C46 C47 120.7(15) . . ? C42 C47 C46 120.8(14) . . ? N10 C49 N9 122.1(10) . . ? N10 C49 S5 120.4(9) . . ? N9 C49 S5 117.4(8) . . ? N9 C50 C51 126.1(14) . . ? C50 C51 C52 113.3(12) . . ? C50 C51 C53 121.0(15) . . ? C52 C51 C53 125.7(13) . . ? N10 C52 C51 123.6(11) . . ? N10 C52 C54 115.9(13) . . ? C51 C52 C54 120.4(12) . . ? C59 C54 C55 118.0(14) . . ? C59 C54 C52 120.1(12) . . ? C55 C54 C52 121.8(12) . . ? C56 C55 C54 120.6(13) . . ? C55 C56 C57 123.6(14) . . ? C56 C57 C58 114.8(13) . . ? C56 C57 C60 123.0(14) . . ? C58 C57 C60 122.2(14) . . ? C59 C58 C57 124.8(15) . . ? C58 C59 C54 118.2(16) . . ? N11 C61 N12 125.2(11) . . ? N11 C61 S6 119.1(9) . . ? N12 C61 S6 115.4(9) . . ? N12 C62 C63 122.6(12) . . ? C64 C63 C62 117.0(11) . . ? C64 C63 C65 125.1(13) . . ? C62 C63 C65 117.9(13) . . ? N11 C64 C63 119.1(12) . . ? N11 C64 C66 116.8(12) . . ? C63 C64 C66 124.1(11) . . ? C71 C66 C67 121.2(13) . . ? C71 C66 C64 119.6(14) . . ? C67 C66 C64 118.9(13) . . ? C68 C67 C66 120.3(15) . . ? C69 C68 C67 120.8(16) . . ? C68 C69 C70 118.8(15) . . ? C68 C69 C72 121.8(19) . . ? C70 C69 C72 119.3(19) . . ? C69 C70 C71 121.3(16) . . ? C66 C71 C70 117.3(16) . . ? C76 C75 N14 161(7) . . ? C76 C75 C75 124(5) . 2_657 ? N14 C75 C75 45(4) . 2_657 ? C75 N14 C75 90(9) 2_657 . ? N13 C73 C74 140(8) . 2_557 ? N13 C73 C74 140(8) . . ? C74 C73 C74 75(7) 2_557 . ? C73 C74 C73 84(7) 2_557 . ? C73 C74 C74 56(5) 2_557 2_557 ? C73 C74 C74 48(4) . 2_557 ? N16 C78 C77 77(8) 2_556 . ? C78 C77 N16 144(5) . . ? C78 C77 N16 36(4) . 2_556 ? N16 C77 N16 134(5) . 2_556 ? C78 N16 C77 104(9) 2_556 . ? C78 N16 C77 68(7) 2_556 2_556 ? C77 N16 C77 38(5) . 2_556 ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 2.290 _refine_diff_density_min -1.322 _refine_diff_density_rms 0.207 data_t2 _database_code_depnum_ccdc_archive 'CCDC 890820' #TrackingRef '2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C24 H22 Cu I N4 S), 2(C N0.50 H1.5)' _chemical_formula_sum 'C50 H47 Cu2 I2 N9 S2' _chemical_formula_weight 1218.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.591(3) _cell_length_b 26.495(5) _cell_length_c 7.4948(15) _cell_angle_alpha 90.00 _cell_angle_beta 96.05(3) _cell_angle_gamma 90.00 _cell_volume 2683.8(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 11916 _cell_measurement_theta_min 3.0145 _cell_measurement_theta_max 27.4778 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.508 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1212 _exptl_absorpt_coefficient_mu 2.062 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7203 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15400 _diffrn_reflns_av_R_equivalents 0.0409 _diffrn_reflns_av_sigmaI/netI 0.0560 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6051 _reflns_number_gt 4687 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0604P)^2^+4.3347P] 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 6051 _refine_ls_number_parameters 267 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0823 _refine_ls_R_factor_gt 0.0596 _refine_ls_wR_factor_ref 0.1471 _refine_ls_wR_factor_gt 0.1356 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_restrained_S_all 1.112 _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 I1 I 0.49953(3) 0.291612(15) 0.89762(5) 0.04118(14) Uani 1 1 d . . . Cu1 Cu 0.40929(5) 0.27057(3) 0.58541(10) 0.03801(19) Uani 1 1 d . . . S1 S 0.20557(11) 0.34593(5) 0.6509(2) 0.0380(3) Uani 1 1 d . . . N1 N 0.3700(3) 0.33861(16) 0.4664(6) 0.0322(10) Uani 1 1 d . . . N2 N 0.2792(4) 0.41500(17) 0.4699(6) 0.0361(10) Uani 1 1 d . . . N3 N 0.2646(3) 0.24825(16) 0.6001(6) 0.0320(10) Uani 1 1 d . . . N4 N 0.1037(3) 0.26599(16) 0.6823(6) 0.0311(9) Uani 1 1 d . . . C1 C 0.2956(4) 0.3670(2) 0.5135(7) 0.0326(11) Uani 1 1 d . . . C2 C 0.4270(4) 0.3615(2) 0.3545(8) 0.0386(13) Uani 1 1 d . A . H2 H 0.4772 0.3426 0.3119 0.046 Uiso 1 1 calc R . . C3 C 0.4167(4) 0.4111(2) 0.2980(8) 0.0405(13) Uani 1 1 d D . . C4 C 0.3394(4) 0.4379(2) 0.3651(7) 0.0357(12) Uani 1 1 d . A . C5 C 0.489(6) 0.434(4) 0.181(7) 0.059(8) Uani 0.50 1 d PD A 1 H5A H 0.5449 0.4473 0.2560 0.089 Uiso 0.50 1 calc PR A 1 H5B H 0.4574 0.4607 0.1103 0.089 Uiso 0.50 1 calc PR A 1 H5C H 0.5114 0.4085 0.1037 0.089 Uiso 0.50 1 calc PR A 1 C5A C 0.477(6) 0.428(4) 0.150(7) 0.059(8) Uani 0.50 1 d PD A 2 H5A1 H 0.5333 0.4467 0.2005 0.089 Uiso 0.50 1 calc PR A 2 H5A2 H 0.4364 0.4491 0.0672 0.089 Uiso 0.50 1 calc PR A 2 H5A3 H 0.4979 0.3990 0.0875 0.089 Uiso 0.50 1 calc PR A 2 C6 C 0.3129(5) 0.4915(2) 0.3184(8) 0.0462(6) Uani 1 1 d . . . C7 C 0.2133(5) 0.5043(2) 0.2953(8) 0.0462(6) Uani 1 1 d . A . H7 H 0.1658 0.4802 0.3145 0.055 Uiso 1 1 calc R . . C8 C 0.1844(5) 0.5526(2) 0.2439(8) 0.0462(6) Uani 1 1 d . . . H8 H 0.1174 0.5603 0.2248 0.055 Uiso 1 1 calc R A . C9 C 0.2545(5) 0.5900(2) 0.2202(9) 0.0462(6) Uani 1 1 d D A . C10 C 0.3542(5) 0.5774(2) 0.2515(8) 0.0462(6) Uani 1 1 d . . . H10 H 0.4019 0.6020 0.2406 0.055 Uiso 1 1 calc R A . C11 C 0.3835(5) 0.5285(2) 0.2988(8) 0.0462(6) Uani 1 1 d . A . H11 H 0.4505 0.5205 0.3173 0.055 Uiso 1 1 calc R . . C12 C 0.236(3) 0.6441(4) 0.158(2) 0.0462(6) Uani 0.48(8) 1 d PD A 1 H12A H 0.2069 0.6442 0.0362 0.069 Uiso 0.48(8) 1 calc PR A 1 H12B H 0.2979 0.6620 0.1671 0.069 Uiso 0.48(8) 1 calc PR A 1 H12C H 0.1922 0.6602 0.2331 0.069 Uiso 0.48(8) 1 calc PR A 1 C12A C 0.206(3) 0.6404(6) 0.165(2) 0.0462(6) Uani 0.52(8) 1 d PD A 2 H12D H 0.1818 0.6393 0.0402 0.069 Uiso 0.52(8) 1 calc PR A 2 H12E H 0.2543 0.6669 0.1849 0.069 Uiso 0.52(8) 1 calc PR A 2 H12F H 0.1524 0.6467 0.2352 0.069 Uiso 0.52(8) 1 calc PR A 2 C13 C 0.1927(4) 0.27915(19) 0.6400(7) 0.0302(11) Uani 1 1 d . . . C14 C 0.2387(4) 0.19978(19) 0.5882(7) 0.0322(11) Uani 1 1 d . . . H14 H 0.2849 0.1770 0.5528 0.039 Uiso 1 1 calc R . . C15 C 0.1487(4) 0.1810(2) 0.6244(7) 0.0348(12) Uani 1 1 d . . . C16 C 0.0810(4) 0.2165(2) 0.6810(7) 0.0310(11) Uani 1 1 d . . . C17 C 0.1251(5) 0.1251(2) 0.5923(9) 0.0442(14) Uani 1 1 d . . . H17A H 0.1733 0.1104 0.5231 0.066 Uiso 1 1 calc R . . H17B H 0.0604 0.1218 0.5282 0.066 Uiso 1 1 calc R . . H17C H 0.1267 0.1080 0.7055 0.066 Uiso 1 1 calc R . . C18 C -0.0186(4) 0.20360(19) 0.7313(7) 0.0313(11) Uani 1 1 d . . . C19 C -0.0979(4) 0.2352(2) 0.6769(7) 0.0350(12) Uani 1 1 d . . . H19 H -0.0872 0.2645 0.6132 0.042 Uiso 1 1 calc R . . C20 C -0.1928(4) 0.2236(2) 0.7164(8) 0.0385(13) Uani 1 1 d . . . H20 H -0.2450 0.2449 0.6781 0.046 Uiso 1 1 calc R . . C21 C -0.2107(4) 0.1799(2) 0.8135(7) 0.0352(12) Uani 1 1 d . . . C22 C -0.1299(4) 0.1498(2) 0.8718(7) 0.0382(13) Uani 1 1 d . . . H22 H -0.1395 0.1214 0.9408 0.046 Uiso 1 1 calc R . . C23 C -0.0350(4) 0.1609(2) 0.8298(8) 0.0372(12) Uani 1 1 d . . . H23 H 0.0175 0.1397 0.8681 0.045 Uiso 1 1 calc R . . C24 C -0.3137(5) 0.1663(3) 0.8496(9) 0.0517(16) Uani 1 1 d . . . H24A H -0.3136 0.1332 0.9020 0.078 Uiso 1 1 calc R . . H24B H -0.3563 0.1665 0.7390 0.078 Uiso 1 1 calc R . . H24C H -0.3371 0.1904 0.9309 0.078 Uiso 1 1 calc R . . N5 N 0.1322(12) 0.5065(7) 0.772(2) 0.099(3) Uiso 0.50 1 d PD . . C25 C 0.2150(12) 0.5077(8) 0.788(3) 0.099(3) Uiso 0.50 1 d PD . . C26 C 0.3165(13) 0.4855(8) 0.820(3) 0.099(3) Uiso 0.50 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.0413(2) 0.0425(2) 0.0395(2) -0.00009(16) 0.00263(16) -0.00981(17) Cu1 0.0333(4) 0.0340(4) 0.0465(4) 0.0034(3) 0.0029(3) 0.0024(3) S1 0.0405(8) 0.0289(7) 0.0468(8) -0.0004(6) 0.0152(6) -0.0006(6) N1 0.031(2) 0.032(2) 0.034(2) 0.0019(19) 0.0011(19) 0.0044(19) N2 0.041(3) 0.029(2) 0.040(2) -0.0012(19) 0.012(2) 0.000(2) N3 0.030(2) 0.029(2) 0.037(2) 0.0030(19) 0.0016(19) 0.0010(19) N4 0.027(2) 0.032(2) 0.034(2) 0.0022(19) 0.0025(18) -0.0020(19) C1 0.034(3) 0.034(3) 0.030(3) -0.002(2) 0.003(2) -0.001(2) C2 0.037(3) 0.037(3) 0.043(3) -0.002(3) 0.010(2) 0.002(2) C3 0.042(3) 0.036(3) 0.045(3) 0.005(3) 0.014(3) 0.001(3) C4 0.041(3) 0.030(3) 0.037(3) -0.001(2) 0.006(2) 0.000(2) C5 0.074(16) 0.039(18) 0.070(14) 0.008(15) 0.037(15) 0.000(8) C5A 0.074(16) 0.039(18) 0.070(14) 0.008(15) 0.037(15) 0.000(8) C6 0.0577(16) 0.0299(11) 0.0531(14) 0.0030(10) 0.0152(13) 0.0011(11) C7 0.0577(16) 0.0299(11) 0.0531(14) 0.0030(10) 0.0152(13) 0.0011(11) C8 0.0577(16) 0.0299(11) 0.0531(14) 0.0030(10) 0.0152(13) 0.0011(11) C9 0.0577(16) 0.0299(11) 0.0531(14) 0.0030(10) 0.0152(13) 0.0011(11) C10 0.0577(16) 0.0299(11) 0.0531(14) 0.0030(10) 0.0152(13) 0.0011(11) C11 0.0577(16) 0.0299(11) 0.0531(14) 0.0030(10) 0.0152(13) 0.0011(11) C12 0.0577(16) 0.0299(11) 0.0531(14) 0.0030(10) 0.0152(13) 0.0011(11) C12A 0.0577(16) 0.0299(11) 0.0531(14) 0.0030(10) 0.0152(13) 0.0011(11) C13 0.034(3) 0.026(3) 0.030(3) 0.003(2) 0.003(2) 0.001(2) C14 0.031(3) 0.027(3) 0.038(3) 0.000(2) 0.002(2) 0.001(2) C15 0.040(3) 0.033(3) 0.031(3) 0.003(2) -0.002(2) 0.000(2) C16 0.032(3) 0.035(3) 0.025(2) 0.003(2) 0.000(2) -0.003(2) C17 0.044(3) 0.035(3) 0.054(4) 0.002(3) 0.011(3) -0.002(3) C18 0.036(3) 0.029(3) 0.029(3) 0.000(2) 0.004(2) -0.003(2) C19 0.037(3) 0.027(3) 0.041(3) 0.000(2) 0.004(2) -0.003(2) C20 0.036(3) 0.038(3) 0.040(3) 0.000(2) 0.000(2) 0.001(2) C21 0.031(3) 0.039(3) 0.036(3) -0.003(2) 0.003(2) -0.008(2) C22 0.043(3) 0.035(3) 0.037(3) 0.004(2) 0.003(2) -0.006(3) C23 0.033(3) 0.037(3) 0.042(3) 0.003(2) 0.010(2) 0.003(2) C24 0.039(3) 0.059(4) 0.057(4) 0.005(3) 0.009(3) -0.004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag I1 Cu1 2.5619(9) 4_566 ? I1 Cu1 2.5856(11) . ? Cu1 N1 2.057(4) . ? Cu1 N3 2.067(4) . ? Cu1 I1 2.5619(9) 4_565 ? S1 C1 1.770(6) . ? S1 C13 1.779(5) . ? N1 C1 1.338(7) . ? N1 C2 1.345(7) . ? N2 C1 1.326(7) . ? N2 C4 1.338(7) . ? N3 C14 1.332(7) . ? N3 C13 1.333(7) . ? N4 C13 1.329(7) . ? N4 C16 1.346(7) . ? C2 C3 1.382(8) . ? C3 C4 1.405(8) . ? C3 C5 1.512(10) . ? C3 C5A 1.512(10) . ? C4 C6 1.498(8) . ? C6 C7 1.388(9) . ? C6 C11 1.390(9) . ? C7 C8 1.382(8) . ? C8 C9 1.400(8) . ? C9 C10 1.392(9) . ? C9 C12 1.517(9) . ? C9 C12A 1.524(8) . ? C10 C11 1.389(8) . ? C14 C15 1.373(8) . ? C15 C16 1.412(8) . ? C15 C17 1.529(8) . ? C16 C18 1.484(8) . ? C18 C23 1.381(7) . ? C18 C19 1.392(8) . ? C19 C20 1.387(8) . ? C20 C21 1.402(8) . ? C21 C22 1.390(8) . ? C21 C24 1.497(8) . ? C22 C23 1.392(8) . ? N5 C25 1.120(9) . ? C25 C26 1.495(10) . ? 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 Cu1 I1 Cu1 98.61(3) 4_566 . ? N1 Cu1 N3 93.95(18) . . ? N1 Cu1 I1 116.30(13) . 4_565 ? N3 Cu1 I1 111.00(13) . 4_565 ? N1 Cu1 I1 106.27(12) . . ? N3 Cu1 I1 112.12(13) . . ? I1 Cu1 I1 115.27(3) 4_565 . ? C1 S1 C13 111.0(3) . . ? C1 N1 C2 114.3(5) . . ? C1 N1 Cu1 123.2(4) . . ? C2 N1 Cu1 121.7(4) . . ? C1 N2 C4 118.8(5) . . ? C14 N3 C13 114.4(5) . . ? C14 N3 Cu1 121.2(4) . . ? C13 N3 Cu1 124.1(4) . . ? C13 N4 C16 117.8(5) . . ? N2 C1 N1 125.9(5) . . ? N2 C1 S1 109.7(4) . . ? N1 C1 S1 124.3(4) . . ? N1 C2 C3 125.0(5) . . ? C2 C3 C4 115.2(5) . . ? C2 C3 C5 121(5) . . ? C4 C3 C5 124(5) . . ? C2 C3 C5A 118(5) . . ? C4 C3 C5A 126(5) . . ? C5 C3 C5A 12(5) . . ? N2 C4 C3 120.5(5) . . ? N2 C4 C6 114.9(5) . . ? C3 C4 C6 124.5(5) . . ? C7 C6 C11 119.4(6) . . ? C7 C6 C4 117.8(5) . . ? C11 C6 C4 122.8(6) . . ? C8 C7 C6 120.3(6) . . ? C7 C8 C9 121.0(6) . . ? C10 C9 C8 118.1(5) . . ? C10 C9 C12 113.9(18) . . ? C8 C9 C12 128.0(18) . . ? C10 C9 C12A 129.8(16) . . ? C8 C9 C12A 112.1(16) . . ? C12 C9 C12A 16.1(8) . . ? C11 C10 C9 121.1(6) . . ? C10 C11 C6 120.0(6) . . ? N4 C13 N3 126.8(5) . . ? N4 C13 S1 109.7(4) . . ? N3 C13 S1 123.4(4) . . ? N3 C14 C15 124.8(5) . . ? C14 C15 C16 116.1(5) . . ? C14 C15 C17 119.8(5) . . ? C16 C15 C17 124.0(5) . . ? N4 C16 C15 119.7(5) . . ? N4 C16 C18 115.9(5) . . ? C15 C16 C18 124.3(5) . . ? C23 C18 C19 119.1(5) . . ? C23 C18 C16 121.8(5) . . ? C19 C18 C16 119.1(5) . . ? C20 C19 C18 120.8(5) . . ? C19 C20 C21 120.7(5) . . ? C22 C21 C20 117.5(5) . . ? C22 C21 C24 121.8(5) . . ? C20 C21 C24 120.7(5) . . ? C21 C22 C23 121.8(5) . . ? C18 C23 C22 120.0(5) . . ? N5 C25 C26 155(2) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.291 _refine_diff_density_min -0.769 _refine_diff_density_rms 0.120 data_shelxl _database_code_depnum_ccdc_archive 'CCDC 890821' #TrackingRef '3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H44 Cu4 I4 N8 S4, C2 H3 N' _chemical_formula_sum 'C50 H47 Cu4 I4 N9 S4' _chemical_formula_weight 1663.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 9.2606(19) _cell_length_b 11.579(2) _cell_length_c 14.140(3) _cell_angle_alpha 83.58(3) _cell_angle_beta 80.89(3) _cell_angle_gamma 78.86(3) _cell_volume 1463.7(5) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4721 _cell_measurement_theta_min 3.1339 _cell_measurement_theta_max 25.3491 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.2500 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.1000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.888 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 802 _exptl_absorpt_coefficient_mu 3.727 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.7328 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13952 _diffrn_reflns_av_R_equivalents 0.0393 _diffrn_reflns_av_sigmaI/netI 0.0506 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 25.36 _reflns_number_total 5294 _reflns_number_gt 3880 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0664P)^2^+5.7313P] 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 5294 _refine_ls_number_parameters 333 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0869 _refine_ls_R_factor_gt 0.0598 _refine_ls_wR_factor_ref 0.1584 _refine_ls_wR_factor_gt 0.1416 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _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 I1 I 0.24817(7) 0.50979(6) 0.51779(4) 0.0591(2) Uani 1 1 d . . . I2 I 0.56159(9) 0.20488(6) 0.40795(5) 0.0675(2) Uani 1 1 d . . . Cu1 Cu 0.38408(15) 0.40095(11) 0.37231(8) 0.0623(3) Uani 1 1 d . . . Cu2 Cu 0.48160(15) 0.62563(11) 0.46960(8) 0.0643(4) Uani 1 1 d . . . S1 S 0.5052(2) 0.4577(2) 0.13706(15) 0.0473(5) Uani 1 1 d . . . S2 S 0.5439(2) 0.51010(19) 0.26213(15) 0.0454(5) Uani 1 1 d . . . N1 N 0.2747(8) 0.3897(6) 0.2598(5) 0.0485(17) Uani 1 1 d . . . N2 N 0.2768(7) 0.3916(6) 0.0916(5) 0.0439(16) Uani 1 1 d . . . N3 N 0.4603(8) 0.7167(6) 0.3353(5) 0.0492(17) Uani 1 1 d . . . N4 N 0.4298(7) 0.7180(6) 0.1722(5) 0.0441(16) Uani 1 1 d . . . C1 C 0.3306(9) 0.4091(7) 0.1690(6) 0.0433(19) Uani 1 1 d . . . C2 C 0.1441(10) 0.3513(8) 0.2716(6) 0.052(2) Uani 1 1 d . . . H2 H 0.0972 0.3388 0.3341 0.063 Uiso 1 1 calc R . . C3 C 0.0754(10) 0.3293(8) 0.1984(7) 0.052(2) Uani 1 1 d . . . C5 C -0.0682(12) 0.2814(11) 0.2237(8) 0.080(3) Uani 1 1 d . . . H5A H -0.0767 0.2482 0.2892 0.120 Uiso 1 1 calc R . . H5B H -0.0680 0.2213 0.1820 0.120 Uiso 1 1 calc R . . H5C H -0.1508 0.3442 0.2159 0.120 Uiso 1 1 calc R . . C4 C 0.1452(9) 0.3543(7) 0.1027(6) 0.0428(19) Uani 1 1 d . . . C6 C 0.0900(9) 0.3441(7) 0.0137(6) 0.0446(19) Uani 1 1 d . . . C7 C -0.0570(9) 0.3423(8) 0.0044(7) 0.050(2) Uani 1 1 d . . . H7 H -0.1276 0.3445 0.0592 0.060 Uiso 1 1 calc R . . C8 C -0.1014(10) 0.3374(8) -0.0841(7) 0.054(2) Uani 1 1 d . . . H8 H -0.2013 0.3388 -0.0874 0.065 Uiso 1 1 calc R . . C9 C -0.0013(10) 0.3305(7) -0.1667(7) 0.051(2) Uani 1 1 d . . . C10 C 0.1456(10) 0.3346(8) -0.1583(6) 0.055(2) Uani 1 1 d . . . H10 H 0.2150 0.3338 -0.2136 0.066 Uiso 1 1 calc R . . C11 C 0.1907(10) 0.3396(8) -0.0731(7) 0.057(2) Uani 1 1 d . . . H11 H 0.2904 0.3402 -0.0711 0.069 Uiso 1 1 calc R . . C12 C -0.0493(11) 0.3235(10) -0.2601(7) 0.066(3) Uani 1 1 d . . . H12A H -0.0712 0.2463 -0.2629 0.098 Uiso 1 1 calc R . . H12B H 0.0287 0.3377 -0.3110 0.098 Uiso 1 1 calc R . . H12C H -0.1367 0.3818 -0.2674 0.098 Uiso 1 1 calc R . . C13 C 0.4678(8) 0.6651(7) 0.2544(6) 0.0399(18) Uani 1 1 d . . . C14 C 0.4204(10) 0.8324(8) 0.3279(6) 0.052(2) Uani 1 1 d . . . H14 H 0.4198 0.8721 0.3817 0.063 Uiso 1 1 calc R . . C15 C 0.3789(11) 0.9002(8) 0.2447(6) 0.051(2) Uani 1 1 d . . . C17 C 0.3424(14) 1.0327(9) 0.2457(8) 0.076(3) Uani 1 1 d . . . H17A H 0.3628 1.0684 0.1816 0.114 Uiso 1 1 calc R . . H17B H 0.4020 1.0578 0.2864 0.114 Uiso 1 1 calc R . . H17C H 0.2390 1.0561 0.2697 0.114 Uiso 1 1 calc R . . C16 C 0.3827(8) 0.8351(7) 0.1676(6) 0.0408(18) Uani 1 1 d . . . C18 C 0.3350(9) 0.8859(7) 0.0726(6) 0.0421(19) Uani 1 1 d . . . C19 C 0.2243(11) 0.9843(8) 0.0641(7) 0.058(2) Uani 1 1 d . . . H19 H 0.1785 1.0224 0.1184 0.070 Uiso 1 1 calc R . . C20 C 0.1820(11) 1.0257(9) -0.0239(7) 0.065(3) Uani 1 1 d . . . H20 H 0.1083 1.0924 -0.0282 0.078 Uiso 1 1 calc R . . C21 C 0.2456(11) 0.9714(8) -0.1059(7) 0.058(2) Uani 1 1 d . . . C22 C 0.3526(11) 0.8708(8) -0.0972(7) 0.059(2) Uani 1 1 d . . . H22 H 0.3953 0.8311 -0.1513 0.071 Uiso 1 1 calc R . . C23 C 0.3971(10) 0.8285(8) -0.0083(6) 0.054(2) Uani 1 1 d . . . H23 H 0.4693 0.7609 -0.0035 0.065 Uiso 1 1 calc R . . C24 C 0.2000(14) 1.0181(10) -0.2023(7) 0.078(3) Uani 1 1 d . . . H24A H 0.0976 1.0133 -0.2018 0.117 Uiso 1 1 calc R . . H24B H 0.2607 0.9720 -0.2511 0.117 Uiso 1 1 calc R . . H24C H 0.2125 1.0990 -0.2154 0.117 Uiso 1 1 calc R . . N5 N -0.031(2) 0.0377(17) 0.6240(13) 0.072(5) Uani 0.50 1 d P . . C25 C 0.045(3) 0.0855(19) 0.5754(14) 0.065(4) Uani 0.50 1 d P . . C26 C 0.162(2) 0.1314(18) 0.5245(13) 0.065(4) Uani 0.50 1 d P . . H26A H 0.2211 0.1511 0.5681 0.098 Uiso 0.50 1 calc PR . . H26B H 0.1251 0.2012 0.4859 0.098 Uiso 0.50 1 calc PR . . H26C H 0.2214 0.0741 0.4836 0.098 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.0558(4) 0.0738(4) 0.0502(4) -0.0120(3) -0.0050(3) -0.0158(3) I2 0.0994(6) 0.0554(4) 0.0498(4) -0.0119(3) -0.0168(3) -0.0098(4) Cu1 0.0770(8) 0.0708(8) 0.0432(6) -0.0058(6) -0.0132(6) -0.0191(6) Cu2 0.0840(9) 0.0661(8) 0.0460(6) -0.0053(6) -0.0168(6) -0.0143(7) S1 0.0482(12) 0.0566(13) 0.0408(11) -0.0122(10) -0.0053(9) -0.0149(10) S2 0.0499(12) 0.0461(12) 0.0431(11) -0.0058(9) -0.0129(10) -0.0095(10) N1 0.058(5) 0.048(4) 0.040(4) -0.005(3) -0.005(3) -0.015(4) N2 0.046(4) 0.045(4) 0.045(4) -0.010(3) -0.012(3) -0.008(3) N3 0.059(5) 0.055(5) 0.036(4) -0.003(3) -0.008(3) -0.016(4) N4 0.042(4) 0.052(4) 0.037(4) -0.011(3) -0.005(3) -0.004(3) C1 0.051(5) 0.036(4) 0.041(5) -0.005(4) -0.008(4) -0.002(4) C2 0.064(6) 0.057(6) 0.035(4) 0.000(4) 0.005(4) -0.019(5) C3 0.048(5) 0.053(5) 0.055(5) 0.004(4) -0.003(4) -0.015(4) C5 0.067(7) 0.112(9) 0.069(7) 0.011(6) -0.007(6) -0.047(7) C4 0.038(4) 0.036(4) 0.055(5) -0.010(4) -0.010(4) -0.002(3) C6 0.046(5) 0.036(4) 0.052(5) -0.002(4) -0.012(4) -0.006(4) C7 0.037(5) 0.058(5) 0.056(5) -0.011(4) -0.007(4) -0.007(4) C8 0.034(5) 0.057(6) 0.071(6) -0.003(5) -0.014(4) -0.004(4) C9 0.057(6) 0.039(5) 0.060(6) -0.003(4) -0.019(5) -0.009(4) C10 0.055(6) 0.073(6) 0.041(5) -0.008(4) -0.007(4) -0.020(5) C11 0.048(5) 0.068(6) 0.060(6) -0.004(5) -0.007(5) -0.022(5) C12 0.060(6) 0.079(7) 0.063(6) -0.013(5) -0.018(5) -0.012(5) C13 0.035(4) 0.049(5) 0.038(4) -0.003(4) -0.005(3) -0.016(4) C14 0.063(6) 0.053(6) 0.048(5) -0.020(4) -0.006(4) -0.020(5) C15 0.072(6) 0.046(5) 0.039(4) -0.008(4) -0.004(4) -0.019(4) C17 0.118(9) 0.057(6) 0.062(6) -0.013(5) -0.018(6) -0.029(6) C16 0.037(4) 0.040(5) 0.046(5) -0.004(4) 0.001(4) -0.012(4) C18 0.050(5) 0.036(4) 0.041(4) -0.007(4) -0.001(4) -0.011(4) C19 0.066(6) 0.054(6) 0.052(5) -0.013(5) -0.009(5) 0.002(5) C20 0.063(6) 0.054(6) 0.070(7) -0.005(5) -0.017(5) 0.016(5) C21 0.072(6) 0.047(5) 0.057(6) 0.001(5) -0.021(5) -0.006(5) C22 0.070(6) 0.048(5) 0.050(5) -0.007(4) 0.004(5) 0.001(5) C23 0.060(6) 0.055(5) 0.046(5) 0.002(4) -0.019(4) 0.001(4) C24 0.111(9) 0.066(7) 0.057(6) 0.008(5) -0.031(6) -0.007(6) N5 0.086(13) 0.086(13) 0.055(10) -0.019(10) -0.016(10) -0.033(11) C25 0.095(12) 0.066(9) 0.039(7) -0.016(7) -0.001(7) -0.028(8) C26 0.095(12) 0.066(9) 0.039(7) -0.016(7) -0.001(7) -0.028(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag I1 Cu1 2.5593(16) . ? I1 Cu2 2.7046(17) 2_666 ? I1 Cu2 2.7177(17) . ? I2 Cu1 2.5837(17) . ? I2 Cu2 2.6919(15) 2_666 ? Cu1 N1 2.045(7) . ? Cu1 S2 2.402(3) . ? Cu1 Cu2 2.6866(18) 2_666 ? Cu2 N3 2.085(7) . ? Cu2 Cu1 2.6866(17) 2_666 ? Cu2 I2 2.6919(15) 2_666 ? Cu2 I1 2.7046(17) 2_666 ? Cu2 Cu2 2.910(3) 2_666 ? S1 C1 1.789(9) . ? S1 S2 2.037(3) . ? S2 C13 1.795(8) . ? N1 C1 1.318(10) . ? N1 C2 1.348(11) . ? N2 C1 1.322(10) . ? N2 C4 1.351(10) . ? N3 C14 1.316(11) . ? N3 C13 1.336(10) . ? N4 C13 1.318(10) . ? N4 C16 1.339(10) . ? C2 C3 1.367(13) . ? C2 H2 0.9300 . ? C3 C4 1.429(12) . ? C3 C5 1.515(13) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C4 C6 1.456(12) . ? C6 C7 1.392(11) . ? C6 C11 1.418(12) . ? C7 C8 1.388(13) . ? C7 H7 0.9300 . ? C8 C9 1.370(13) . ? C8 H8 0.9300 . ? C9 C10 1.395(12) . ? C9 C12 1.475(13) . ? C10 C11 1.347(12) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C14 C15 1.403(12) . ? C14 H14 0.9300 . ? C15 C16 1.385(11) . ? C15 C17 1.507(12) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C16 C18 1.503(11) . ? C18 C23 1.376(12) . ? C18 C19 1.385(12) . ? C19 C20 1.372(13) . ? C19 H19 0.9300 . ? C20 C21 1.375(14) . ? C20 H20 0.9300 . ? C21 C22 1.383(13) . ? C21 C24 1.502(13) . ? C22 C23 1.393(12) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? N5 C25 1.09(2) . ? C25 C26 1.36(3) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? 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 Cu1 I1 Cu2 61.31(5) . 2_666 ? Cu1 I1 Cu2 80.24(5) . . ? Cu2 I1 Cu2 64.92(5) 2_666 . ? Cu1 I2 Cu2 61.19(4) . 2_666 ? N1 Cu1 S2 87.6(2) . . ? N1 Cu1 I1 120.4(2) . . ? S2 Cu1 I1 114.59(7) . . ? N1 Cu1 I2 110.7(2) . . ? S2 Cu1 I2 102.00(8) . . ? I1 Cu1 I2 116.56(5) . . ? N1 Cu1 Cu2 169.2(2) . 2_666 ? S2 Cu1 Cu2 100.97(7) . 2_666 ? I1 Cu1 Cu2 62.02(4) . 2_666 ? I2 Cu1 Cu2 61.39(5) . 2_666 ? N3 Cu2 Cu1 146.4(2) . 2_666 ? N3 Cu2 I2 104.9(2) . 2_666 ? Cu1 Cu2 I2 57.42(4) 2_666 2_666 ? N3 Cu2 I1 114.3(2) . 2_666 ? Cu1 Cu2 I1 56.68(5) 2_666 2_666 ? I2 Cu2 I1 108.32(5) 2_666 2_666 ? N3 Cu2 I1 107.2(2) . . ? Cu1 Cu2 I1 105.38(6) 2_666 . ? I2 Cu2 I1 106.28(5) 2_666 . ? I1 Cu2 I1 115.08(5) 2_666 . ? N3 Cu2 Cu2 131.2(2) . 2_666 ? Cu1 Cu2 Cu2 74.76(6) 2_666 2_666 ? I2 Cu2 Cu2 123.63(7) 2_666 2_666 ? I1 Cu2 Cu2 57.76(5) 2_666 2_666 ? I1 Cu2 Cu2 57.32(5) . 2_666 ? C1 S1 S2 103.7(3) . . ? C13 S2 S1 103.1(3) . . ? C13 S2 Cu1 111.2(3) . . ? S1 S2 Cu1 98.54(11) . . ? C1 N1 C2 113.5(7) . . ? C1 N1 Cu1 123.5(6) . . ? C2 N1 Cu1 122.7(6) . . ? C1 N2 C4 118.8(7) . . ? C14 N3 C13 115.0(7) . . ? C14 N3 Cu2 120.1(6) . . ? C13 N3 Cu2 124.4(6) . . ? C13 N4 C16 117.7(7) . . ? N1 C1 N2 128.0(8) . . ? N1 C1 S1 120.9(6) . . ? N2 C1 S1 111.0(6) . . ? N1 C2 C3 124.8(8) . . ? N1 C2 H2 117.6 . . ? C3 C2 H2 117.6 . . ? C2 C3 C4 116.9(8) . . ? C2 C3 C5 118.4(8) . . ? C4 C3 C5 124.6(8) . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C4 C3 117.8(7) . . ? N2 C4 C6 115.2(7) . . ? C3 C4 C6 127.1(8) . . ? C7 C6 C11 115.5(8) . . ? C7 C6 C4 125.7(8) . . ? C11 C6 C4 118.8(8) . . ? C8 C7 C6 122.0(9) . . ? C8 C7 H7 119.0 . . ? C6 C7 H7 119.0 . . ? C9 C8 C7 121.4(8) . . ? C9 C8 H8 119.3 . . ? C7 C8 H8 119.3 . . ? C8 C9 C10 116.9(8) . . ? C8 C9 C12 121.0(8) . . ? C10 C9 C12 122.1(9) . . ? C11 C10 C9 122.4(9) . . ? C11 C10 H10 118.8 . . ? C9 C10 H10 118.8 . . ? C10 C11 C6 121.7(9) . . ? C10 C11 H11 119.2 . . ? C6 C11 H11 119.2 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N4 C13 N3 126.1(7) . . ? N4 C13 S2 119.5(6) . . ? N3 C13 S2 114.3(6) . . ? N3 C14 C15 124.7(8) . . ? N3 C14 H14 117.6 . . ? C15 C14 H14 117.6 . . ? C16 C15 C14 114.4(8) . . ? C16 C15 C17 126.9(8) . . ? C14 C15 C17 118.7(8) . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N4 C16 C15 121.8(8) . . ? N4 C16 C18 113.5(7) . . ? C15 C16 C18 124.7(7) . . ? C23 C18 C19 118.7(8) . . ? C23 C18 C16 118.8(7) . . ? C19 C18 C16 122.5(7) . . ? C20 C19 C18 120.3(8) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C19 C20 C21 121.8(8) . . ? C19 C20 H20 119.1 . . ? C21 C20 H20 119.1 . . ? C20 C21 C22 117.9(9) . . ? C20 C21 C24 121.5(9) . . ? C22 C21 C24 120.5(9) . . ? C21 C22 C23 120.6(9) . . ? C21 C22 H22 119.7 . . ? C23 C22 H22 119.7 . . ? C18 C23 C22 120.5(8) . . ? C18 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N5 C25 C26 168(3) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.36 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.901 _refine_diff_density_min -0.939 _refine_diff_density_rms 0.131 data_t3 _database_code_depnum_ccdc_archive 'CCDC 890822' #TrackingRef '4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H66 Cu6 N12 S6' _chemical_formula_sum 'C72 H66 Cu6 N12 S6' _chemical_formula_weight 1673.09 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.694(4) _cell_length_b 13.3920(18) _cell_length_c 18.751(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.182(2) _cell_angle_gamma 90.00 _cell_volume 6954.3(16) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 10892 _cell_measurement_theta_min 3.0423 _cell_measurement_theta_max 27.4855 _exptl_crystal_description Prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.598 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3408 _exptl_absorpt_coefficient_mu 2.035 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3300 _exptl_absorpt_correction_T_max 0.6864 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 16294 _diffrn_reflns_av_R_equivalents 0.0286 _diffrn_reflns_av_sigmaI/netI 0.0525 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 27.49 _reflns_number_total 7893 _reflns_number_gt 6222 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0358P)^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 7893 _refine_ls_number_parameters 434 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0526 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.0843 _refine_ls_wR_factor_gt 0.0775 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.996 _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 0.241759(12) 0.64923(3) 0.09471(2) 0.02951(10) Uani 1 1 d . . . Cu2 Cu 0.178624(12) 0.79606(2) 0.046528(19) 0.02809(10) Uani 1 1 d . . . Cu3 Cu 0.276384(12) 0.89471(3) 0.049360(19) 0.02895(10) Uani 1 1 d . . . S1 S 0.15410(2) 0.64931(5) 0.00214(4) 0.02424(15) Uani 1 1 d . . . S2 S 0.26295(2) 0.79641(5) 0.14518(4) 0.02616(16) Uani 1 1 d . . . S3 S 0.18958(2) 0.90660(5) -0.04310(4) 0.02537(15) Uani 1 1 d . . . N1 N 0.18517(7) 0.56317(16) 0.12235(12) 0.0250(5) Uani 1 1 d . . . N2 N 0.10796(7) 0.51416(16) 0.07913(12) 0.0248(5) Uani 1 1 d . . . N4 N 0.21876(9) 0.90272(19) 0.24515(14) 0.0395(6) Uani 1 1 d . . . N3 N 0.17059(8) 0.85111(16) 0.14634(12) 0.0253(5) Uani 1 1 d . . . N5 N 0.24152(7) 1.02776(16) 0.04077(12) 0.0248(5) Uani 1 1 d . . . N6 N 0.16653(8) 1.09017(18) -0.00258(16) 0.0423(7) Uani 1 1 d . . . C1 C 0.14797(9) 0.56776(19) 0.07496(14) 0.0233(6) Uani 1 1 d . . . C2 C 0.17775(9) 0.5057(2) 0.17937(15) 0.0270(6) Uani 1 1 d . . . H2B H 0.2025 0.5020 0.2137 0.032 Uiso 1 1 calc R . . C3 C 0.13593(9) 0.4507(2) 0.19147(15) 0.0270(6) Uani 1 1 d . . . C4 C 0.10170(9) 0.4528(2) 0.13590(15) 0.0255(6) Uani 1 1 d . . . C5 C 0.13020(10) 0.3963(2) 0.26114(16) 0.0382(8) Uani 1 1 d . . . H5A H 0.0994 0.3617 0.2616 0.057 Uiso 1 1 calc R . . H5B H 0.1314 0.4438 0.3001 0.057 Uiso 1 1 calc R . . H5C H 0.1561 0.3482 0.2666 0.057 Uiso 1 1 calc R . . C6 C 0.05709(9) 0.3917(2) 0.13319(15) 0.0280(6) Uani 1 1 d . . . C7 C 0.05496(10) 0.2961(2) 0.16125(17) 0.0366(7) Uani 1 1 d . . . H7A H 0.0821 0.2695 0.1848 0.044 Uiso 1 1 calc R . . C8 C 0.01353(10) 0.2397(2) 0.15500(17) 0.0385(7) Uani 1 1 d . . . H8A H 0.0129 0.1754 0.1751 0.046 Uiso 1 1 calc R . . C9 C -0.02726(10) 0.2747(2) 0.12013(16) 0.0334(7) Uani 1 1 d . . . C10 C -0.02492(10) 0.3702(2) 0.09188(18) 0.0365(7) Uani 1 1 d . . . H10A H -0.0520 0.3963 0.0680 0.044 Uiso 1 1 calc R . . C11 C 0.01614(10) 0.4280(2) 0.09780(17) 0.0350(7) Uani 1 1 d . . . H11A H 0.0166 0.4924 0.0779 0.042 Uiso 1 1 calc R . . C12 C -0.07198(11) 0.2111(2) 0.1126(2) 0.0485(9) Uani 1 1 d . . . H12A H -0.0966 0.2482 0.0870 0.073 Uiso 1 1 calc R . . H12B H -0.0839 0.1935 0.1596 0.073 Uiso 1 1 calc R . . H12C H -0.0642 0.1508 0.0864 0.073 Uiso 1 1 calc R . . C13 C 0.21255(10) 0.8556(2) 0.18299(15) 0.0281(6) Uani 1 1 d . . . C14 C 0.17859(12) 0.9411(3) 0.27399(18) 0.0485(9) Uani 1 1 d . . . H14A H 0.1815 0.9733 0.3183 0.058 Uiso 1 1 calc R . . C15 C 0.13326(11) 0.9368(2) 0.24341(18) 0.0432(8) Uani 1 1 d . . . C16 C 0.13084(10) 0.8913(2) 0.17674(15) 0.0292(6) Uani 1 1 d . . . C17 C 0.08951(14) 0.9741(3) 0.2835(2) 0.0751(13) Uani 1 1 d . . . H17A H 0.0609 0.9658 0.2541 0.113 Uiso 1 1 calc R . . H17B H 0.0937 1.0443 0.2948 0.113 Uiso 1 1 calc R . . H17C H 0.0859 0.9363 0.3273 0.113 Uiso 1 1 calc R . . C18 C 0.08462(10) 0.8794(2) 0.13635(16) 0.0308(7) Uani 1 1 d . . . C19 C 0.07016(10) 0.7851(2) 0.11463(16) 0.0338(7) Uani 1 1 d . . . H19A H 0.0901 0.7298 0.1237 0.041 Uiso 1 1 calc R . . C20 C 0.02640(10) 0.7719(2) 0.07956(17) 0.0395(8) Uani 1 1 d . . . H20A H 0.0170 0.7076 0.0649 0.047 Uiso 1 1 calc R . . C21 C -0.00352(10) 0.8527(3) 0.06605(17) 0.0441(9) Uani 1 1 d . . . C22 C 0.01129(11) 0.9468(3) 0.08680(19) 0.0454(9) Uani 1 1 d . . . H22A H -0.0084 1.0023 0.0772 0.054 Uiso 1 1 calc R . . C23 C 0.05512(11) 0.9601(2) 0.12176(18) 0.0431(8) Uani 1 1 d . . . H23A H 0.0648 1.0245 0.1356 0.052 Uiso 1 1 calc R . . C24 C -0.05201(11) 0.8375(3) 0.0300(2) 0.0593(11) Uani 1 1 d . . . H24A H -0.0681 0.9015 0.0249 0.089 Uiso 1 1 calc R . . H24B H -0.0717 0.7934 0.0588 0.089 Uiso 1 1 calc R . . H24C H -0.0472 0.8081 -0.0167 0.089 Uiso 1 1 calc R . . C25 C 0.20014(9) 1.0193(2) 0.00261(16) 0.0284(6) Uani 1 1 d . . . C26 C 0.25062(10) 1.1156(2) 0.07474(15) 0.0271(6) Uani 1 1 d . . . C27 C 0.21710(10) 1.1934(2) 0.07175(17) 0.0345(7) Uani 1 1 d . . . C28 C 0.17576(11) 1.1741(2) 0.03308(19) 0.0442(9) Uani 1 1 d . . . H28A H 0.1521 1.2243 0.0318 0.053 Uiso 1 1 calc R . . C29 C 0.22447(12) 1.2941(2) 0.10608(19) 0.0476(9) Uani 1 1 d . . . H29A H 0.1965 1.3359 0.0969 0.071 Uiso 1 1 calc R . . H29B H 0.2530 1.3254 0.0863 0.071 Uiso 1 1 calc R . . H29C H 0.2286 1.2857 0.1571 0.071 Uiso 1 1 calc R . . C30 C 0.29851(10) 1.12433(19) 0.10976(15) 0.0262(6) Uani 1 1 d . . . C31 C 0.33967(10) 1.0966(2) 0.07295(16) 0.0301(6) Uani 1 1 d . . . H31A H 0.3367 1.0715 0.0263 0.036 Uiso 1 1 calc R . . C32 C 0.38503(10) 1.1050(2) 0.10330(17) 0.0332(7) Uani 1 1 d . . . H32A H 0.4124 1.0857 0.0771 0.040 Uiso 1 1 calc R . . C33 C 0.39067(10) 1.1415(2) 0.17203(18) 0.0353(7) Uani 1 1 d . . . C34 C 0.34958(11) 1.1706(2) 0.20921(17) 0.0362(7) Uani 1 1 d . . . H34A H 0.3528 1.1962 0.2556 0.043 Uiso 1 1 calc R . . C35 C 0.30384(10) 1.1624(2) 0.17891(16) 0.0315(7) Uani 1 1 d . . . H35A H 0.2765 1.1825 0.2048 0.038 Uiso 1 1 calc R . . C36 C 0.43995(11) 1.1478(3) 0.20664(19) 0.0530(10) Uani 1 1 d . . . H36A H 0.4643 1.1249 0.1733 0.079 Uiso 1 1 calc R . . H36B H 0.4406 1.1062 0.2489 0.079 Uiso 1 1 calc R . . H36C H 0.4466 1.2165 0.2199 0.079 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 0.02317(17) 0.0300(2) 0.0353(2) -0.00238(16) -0.00221(14) -0.00158(15) Cu2 0.03242(19) 0.02559(19) 0.02624(19) -0.00138(15) -0.00155(14) -0.00207(15) Cu3 0.02630(18) 0.0287(2) 0.0319(2) 0.00294(16) 0.00251(14) 0.00487(15) S1 0.0226(3) 0.0230(3) 0.0271(4) -0.0006(3) 0.0000(3) 0.0000(3) S2 0.0230(3) 0.0267(4) 0.0287(4) 0.0003(3) -0.0030(3) -0.0009(3) S3 0.0221(3) 0.0245(4) 0.0295(4) 0.0009(3) -0.0018(3) -0.0011(3) N1 0.0208(11) 0.0244(12) 0.0299(13) -0.0019(10) -0.0010(9) 0.0003(9) N2 0.0218(11) 0.0242(12) 0.0286(13) -0.0015(10) 0.0026(9) -0.0002(10) N4 0.0421(15) 0.0440(16) 0.0322(15) -0.0156(13) -0.0046(12) 0.0013(13) N3 0.0268(11) 0.0239(12) 0.0253(12) -0.0015(10) -0.0005(10) 0.0005(10) N5 0.0233(11) 0.0228(12) 0.0282(13) -0.0015(10) -0.0008(9) 0.0019(9) N6 0.0284(13) 0.0302(14) 0.068(2) -0.0060(14) -0.0087(13) 0.0072(11) C1 0.0207(13) 0.0212(14) 0.0281(15) -0.0049(12) 0.0020(11) 0.0025(11) C2 0.0277(14) 0.0258(15) 0.0276(15) -0.0026(12) -0.0042(12) 0.0041(12) C3 0.0279(14) 0.0255(15) 0.0276(15) 0.0020(12) 0.0007(12) 0.0011(12) C4 0.0248(13) 0.0225(14) 0.0293(15) -0.0005(12) 0.0036(11) 0.0022(11) C5 0.0366(16) 0.0449(19) 0.0330(17) 0.0074(15) -0.0061(14) -0.0054(15) C6 0.0276(14) 0.0258(15) 0.0306(16) 0.0025(12) 0.0017(12) -0.0013(12) C7 0.0323(15) 0.0342(17) 0.0433(19) 0.0072(15) -0.0045(14) 0.0003(14) C8 0.0430(17) 0.0290(17) 0.0433(19) 0.0081(15) -0.0003(14) -0.0055(14) C9 0.0313(15) 0.0317(17) 0.0370(17) 0.0023(14) 0.0035(13) -0.0056(13) C10 0.0276(15) 0.0336(17) 0.048(2) 0.0063(15) -0.0057(14) -0.0020(13) C11 0.0296(15) 0.0288(16) 0.047(2) 0.0105(14) -0.0036(13) -0.0018(13) C12 0.0401(18) 0.0385(19) 0.067(3) 0.0134(18) -0.0053(17) -0.0133(15) C13 0.0304(14) 0.0266(15) 0.0274(15) 0.0004(12) -0.0008(12) -0.0033(12) C14 0.055(2) 0.054(2) 0.037(2) -0.0224(17) -0.0049(16) 0.0052(18) C15 0.0438(18) 0.046(2) 0.040(2) -0.0143(16) 0.0023(15) 0.0109(16) C16 0.0318(15) 0.0266(15) 0.0293(16) -0.0016(12) 0.0028(12) 0.0040(12) C17 0.066(3) 0.106(4) 0.054(3) -0.039(3) 0.013(2) 0.021(2) C18 0.0258(14) 0.0359(17) 0.0308(16) 0.0006(13) 0.0048(12) 0.0051(13) C19 0.0316(15) 0.0363(17) 0.0336(17) -0.0030(14) 0.0034(13) 0.0039(13) C20 0.0356(16) 0.0429(19) 0.0401(19) -0.0026(15) 0.0020(14) -0.0032(15) C21 0.0268(15) 0.072(3) 0.0339(18) 0.0064(17) 0.0034(13) -0.0028(17) C22 0.0330(17) 0.050(2) 0.053(2) 0.0072(18) 0.0000(15) 0.0160(16) C23 0.0397(17) 0.0393(19) 0.050(2) -0.0032(16) -0.0006(15) 0.0067(15) C24 0.0329(18) 0.087(3) 0.057(3) 0.008(2) -0.0080(17) -0.0014(19) C25 0.0262(14) 0.0232(14) 0.0359(17) 0.0016(13) -0.0018(12) 0.0028(12) C26 0.0303(14) 0.0239(14) 0.0272(15) -0.0014(12) 0.0017(12) -0.0017(12) C27 0.0345(16) 0.0264(16) 0.0427(19) -0.0045(14) -0.0011(14) 0.0048(13) C28 0.0328(16) 0.0341(18) 0.066(3) -0.0056(17) -0.0034(16) 0.0128(14) C29 0.057(2) 0.0279(17) 0.058(2) -0.0108(16) -0.0051(18) 0.0140(16) C30 0.0300(14) 0.0178(13) 0.0306(16) -0.0016(12) -0.0015(12) 0.0019(11) C31 0.0352(15) 0.0254(15) 0.0297(16) -0.0038(12) -0.0007(12) -0.0005(13) C32 0.0305(15) 0.0308(16) 0.0383(18) -0.0035(14) 0.0024(13) 0.0000(13) C33 0.0337(16) 0.0294(16) 0.0428(19) -0.0011(14) -0.0038(14) -0.0034(13) C34 0.0450(18) 0.0331(17) 0.0304(17) -0.0042(13) -0.0037(14) -0.0038(14) C35 0.0365(16) 0.0281(16) 0.0298(16) -0.0031(13) 0.0023(13) 0.0044(13) C36 0.0380(18) 0.069(3) 0.051(2) -0.006(2) -0.0104(17) -0.0062(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 N1 2.015(2) . ? Cu1 S2 2.2630(8) . ? Cu1 S3 2.2635(8) 7_565 ? Cu1 Cu2 2.7802(5) . ? Cu1 Cu3 2.8085(6) 7_565 ? Cu2 N3 2.024(2) . ? Cu2 S1 2.2389(8) . ? Cu2 S3 2.2607(8) . ? Cu2 Cu3 3.0128(6) . ? Cu3 N5 2.033(2) . ? Cu3 S1 2.2356(8) 7_565 ? Cu3 S2 2.2592(8) . ? Cu3 Cu1 2.8085(6) 7_565 ? S1 C1 1.757(3) . ? S1 Cu3 2.2356(8) 7_565 ? S2 C13 1.756(3) . ? S3 C25 1.759(3) . ? S3 Cu1 2.2635(8) 7_565 ? N1 C2 1.334(3) . ? N1 C1 1.360(3) . ? N2 C1 1.323(3) . ? N2 C4 1.356(3) . ? N4 C13 1.336(4) . ? N4 C14 1.341(4) . ? N3 C13 1.350(3) . ? N3 C16 1.353(3) . ? N5 C25 1.354(3) . ? N5 C26 1.361(3) . ? N6 C28 1.332(4) . ? N6 C25 1.333(3) . ? C2 C3 1.392(4) . ? C2 H2B 0.9400 . ? C3 C4 1.407(3) . ? C3 C5 1.505(4) . ? C4 C6 1.483(4) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 H5C 0.9700 . ? C6 C7 1.385(4) . ? C6 C11 1.399(4) . ? C7 C8 1.378(4) . ? C7 H7A 0.9400 . ? C8 C9 1.385(4) . ? C8 H8A 0.9400 . ? C9 C10 1.386(4) . ? C9 C12 1.509(4) . ? C10 C11 1.380(4) . ? C10 H10A 0.9400 . ? C11 H11A 0.9400 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 H12C 0.9700 . ? C14 C15 1.380(4) . ? C14 H14A 0.9400 . ? C15 C16 1.392(4) . ? C15 C17 1.513(5) . ? C16 C18 1.494(4) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 C23 1.382(4) . ? C18 C19 1.385(4) . ? C19 C20 1.388(4) . ? C19 H19A 0.9400 . ? C20 C21 1.385(4) . ? C20 H20A 0.9400 . ? C21 C22 1.381(5) . ? C21 C24 1.515(4) . ? C22 C23 1.389(4) . ? C22 H22A 0.9400 . ? C23 H23A 0.9400 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? C26 C27 1.396(4) . ? C26 C30 1.483(4) . ? C27 C28 1.378(4) . ? C27 C29 1.508(4) . ? C28 H28A 0.9400 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C29 H29C 0.9700 . ? C30 C31 1.385(4) . ? C30 C35 1.401(4) . ? C31 C32 1.382(4) . ? C31 H31A 0.9400 . ? C32 C33 1.387(4) . ? C32 H32A 0.9400 . ? C33 C34 1.392(4) . ? C33 C36 1.512(4) . ? C34 C35 1.391(4) . ? C34 H34A 0.9400 . ? C35 H35A 0.9400 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C36 H36C 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 S2 126.27(7) . . ? N1 Cu1 S3 125.19(7) . 7_565 ? S2 Cu1 S3 104.45(3) . 7_565 ? N1 Cu1 Cu2 89.96(6) . . ? S2 Cu1 Cu2 71.45(2) . . ? S3 Cu1 Cu2 128.54(2) 7_565 . ? N1 Cu1 Cu3 89.47(7) . 7_565 ? S2 Cu1 Cu3 129.06(2) . 7_565 ? S3 Cu1 Cu3 70.58(2) 7_565 7_565 ? Cu2 Cu1 Cu3 74.052(14) . 7_565 ? N3 Cu2 S1 128.99(7) . . ? N3 Cu2 S3 117.66(7) . . ? S1 Cu2 S3 109.86(3) . . ? N3 Cu2 Cu1 91.60(6) . . ? S1 Cu2 Cu1 71.92(2) . . ? S3 Cu2 Cu1 128.24(2) . . ? N3 Cu2 Cu3 85.72(6) . . ? S1 Cu2 Cu3 131.53(2) . . ? S3 Cu2 Cu3 66.627(19) . . ? Cu1 Cu2 Cu3 74.944(15) . . ? N5 Cu3 S1 127.33(7) . 7_565 ? N5 Cu3 S2 119.63(7) . . ? S1 Cu3 S2 109.52(3) 7_565 . ? N5 Cu3 Cu1 91.37(6) . 7_565 ? S1 Cu3 Cu1 71.39(2) 7_565 7_565 ? S2 Cu3 Cu1 127.84(2) . 7_565 ? N5 Cu3 Cu2 87.50(6) . . ? S1 Cu3 Cu2 130.67(2) 7_565 . ? S2 Cu3 Cu2 66.94(2) . . ? Cu1 Cu3 Cu2 74.524(13) 7_565 . ? C1 S1 Cu3 104.91(9) . 7_565 ? C1 S1 Cu2 106.66(9) . . ? Cu3 S1 Cu2 97.55(3) 7_565 . ? C13 S2 Cu3 101.03(10) . . ? C13 S2 Cu1 110.88(9) . . ? Cu3 S2 Cu1 102.59(3) . . ? C25 S3 Cu2 102.82(10) . . ? C25 S3 Cu1 110.67(9) . 7_565 ? Cu2 S3 Cu1 102.50(3) . 7_565 ? C2 N1 C1 115.6(2) . . ? C2 N1 Cu1 131.17(18) . . ? C1 N1 Cu1 113.23(18) . . ? C1 N2 C4 119.0(2) . . ? C13 N4 C14 115.4(2) . . ? C13 N3 C16 117.9(2) . . ? C13 N3 Cu2 112.94(18) . . ? C16 N3 Cu2 128.78(18) . . ? C25 N5 C26 118.4(2) . . ? C25 N5 Cu3 111.67(17) . . ? C26 N5 Cu3 129.31(17) . . ? C28 N6 C25 115.6(2) . . ? N2 C1 N1 124.7(3) . . ? N2 C1 S1 117.79(19) . . ? N1 C1 S1 117.46(19) . . ? N1 C2 C3 124.5(2) . . ? N1 C2 H2B 117.7 . . ? C3 C2 H2B 117.7 . . ? C2 C3 C4 115.3(3) . . ? C2 C3 C5 119.2(2) . . ? C4 C3 C5 125.4(2) . . ? N2 C4 C3 120.4(2) . . ? N2 C4 C6 114.6(2) . . ? C3 C4 C6 125.0(3) . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C11 117.8(3) . . ? C7 C6 C4 122.2(2) . . ? C11 C6 C4 119.9(3) . . ? C8 C7 C6 120.7(3) . . ? C8 C7 H7A 119.7 . . ? C6 C7 H7A 119.7 . . ? C7 C8 C9 122.2(3) . . ? C7 C8 H8A 118.9 . . ? C9 C8 H8A 118.9 . . ? C8 C9 C10 116.9(3) . . ? C8 C9 C12 121.4(3) . . ? C10 C9 C12 121.6(3) . . ? C11 C10 C9 121.8(3) . . ? C11 C10 H10A 119.1 . . ? C9 C10 H10A 119.1 . . ? C10 C11 C6 120.6(3) . . ? C10 C11 H11A 119.7 . . ? C6 C11 H11A 119.7 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N4 C13 N3 125.0(3) . . ? N4 C13 S2 117.7(2) . . ? N3 C13 S2 117.3(2) . . ? N4 C14 C15 124.8(3) . . ? N4 C14 H14A 117.6 . . ? C15 C14 H14A 117.6 . . ? C14 C15 C16 115.6(3) . . ? C14 C15 C17 120.6(3) . . ? C16 C15 C17 123.7(3) . . ? N3 C16 C15 121.0(3) . . ? N3 C16 C18 116.2(2) . . ? C15 C16 C18 122.7(3) . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C23 C18 C19 119.0(3) . . ? C23 C18 C16 121.5(3) . . ? C19 C18 C16 119.5(2) . . ? C18 C19 C20 120.5(3) . . ? C18 C19 H19A 119.8 . . ? C20 C19 H19A 119.8 . . ? C21 C20 C19 120.5(3) . . ? C21 C20 H20A 119.7 . . ? C19 C20 H20A 119.7 . . ? C22 C21 C20 118.9(3) . . ? C22 C21 C24 120.6(3) . . ? C20 C21 C24 120.4(3) . . ? C21 C22 C23 120.6(3) . . ? C21 C22 H22A 119.7 . . ? C23 C22 H22A 119.7 . . ? C18 C23 C22 120.6(3) . . ? C18 C23 H23A 119.7 . . ? C22 C23 H23A 119.7 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N6 C25 N5 124.6(3) . . ? N6 C25 S3 117.4(2) . . ? N5 C25 S3 117.95(19) . . ? N5 C26 C27 120.3(2) . . ? N5 C26 C30 116.0(2) . . ? C27 C26 C30 123.6(2) . . ? C28 C27 C26 115.6(3) . . ? C28 C27 C29 120.2(3) . . ? C26 C27 C29 124.1(3) . . ? N6 C28 C27 125.5(3) . . ? N6 C28 H28A 117.3 . . ? C27 C28 H28A 117.3 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C31 C30 C35 118.3(3) . . ? C31 C30 C26 119.6(3) . . ? C35 C30 C26 122.0(3) . . ? C32 C31 C30 121.4(3) . . ? C32 C31 H31A 119.3 . . ? C30 C31 H31A 119.3 . . ? C31 C32 C33 120.7(3) . . ? C31 C32 H32A 119.6 . . ? C33 C32 H32A 119.6 . . ? C32 C33 C34 118.3(3) . . ? C32 C33 C36 121.2(3) . . ? C34 C33 C36 120.5(3) . . ? C35 C34 C33 121.2(3) . . ? C35 C34 H34A 119.4 . . ? C33 C34 H34A 119.4 . . ? C34 C35 C30 120.0(3) . . ? C34 C35 H35A 120.0 . . ? C30 C35 H35A 120.0 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Cu1 Cu2 N3 83.25(9) . . . . ? S2 Cu1 Cu2 N3 -45.37(7) . . . . ? S3 Cu1 Cu2 N3 -139.34(7) 7_565 . . . ? Cu3 Cu1 Cu2 N3 172.71(6) 7_565 . . . ? N1 Cu1 Cu2 S1 -47.51(7) . . . . ? S2 Cu1 Cu2 S1 -176.14(3) . . . . ? S3 Cu1 Cu2 S1 89.90(4) 7_565 . . . ? Cu3 Cu1 Cu2 S1 41.94(2) 7_565 . . . ? N1 Cu1 Cu2 S3 -148.92(7) . . . . ? S2 Cu1 Cu2 S3 82.46(4) . . . . ? S3 Cu1 Cu2 S3 -11.51(5) 7_565 . . . ? Cu3 Cu1 Cu2 S3 -59.46(3) 7_565 . . . ? N1 Cu1 Cu2 Cu3 168.39(7) . . . . ? S2 Cu1 Cu2 Cu3 39.77(2) . . . . ? S3 Cu1 Cu2 Cu3 -54.20(3) 7_565 . . . ? Cu3 Cu1 Cu2 Cu3 -102.152(13) 7_565 . . . ? N3 Cu2 Cu3 N5 -72.31(9) . . . . ? S1 Cu2 Cu3 N5 146.74(7) . . . . ? S3 Cu2 Cu3 N5 50.33(7) . . . . ? Cu1 Cu2 Cu3 N5 -165.13(7) . . . . ? N3 Cu2 Cu3 S1 147.98(7) . . . 7_565 ? S1 Cu2 Cu3 S1 7.04(6) . . . 7_565 ? S3 Cu2 Cu3 S1 -89.37(4) . . . 7_565 ? Cu1 Cu2 Cu3 S1 55.17(3) . . . 7_565 ? N3 Cu2 Cu3 S2 51.50(6) . . . . ? S1 Cu2 Cu3 S2 -89.45(4) . . . . ? S3 Cu2 Cu3 S2 174.15(3) . . . . ? Cu1 Cu2 Cu3 S2 -41.32(2) . . . . ? N3 Cu2 Cu3 Cu1 -164.43(6) . . . 7_565 ? S1 Cu2 Cu3 Cu1 54.62(3) . . . 7_565 ? S3 Cu2 Cu3 Cu1 -41.78(2) . . . 7_565 ? Cu1 Cu2 Cu3 Cu1 102.753(14) . . . 7_565 ? N3 Cu2 S1 C1 -23.36(12) . . . . ? S3 Cu2 S1 C1 178.61(9) . . . . ? Cu1 Cu2 S1 C1 53.56(9) . . . . ? Cu3 Cu2 S1 C1 102.71(9) . . . . ? N3 Cu2 S1 Cu3 -131.44(8) . . . 7_565 ? S3 Cu2 S1 Cu3 70.52(3) . . . 7_565 ? Cu1 Cu2 S1 Cu3 -54.53(2) . . . 7_565 ? Cu3 Cu2 S1 Cu3 -5.38(4) . . . 7_565 ? N5 Cu3 S2 C13 11.56(12) . . . . ? S1 Cu3 S2 C13 171.91(9) 7_565 . . . ? Cu1 Cu3 S2 C13 -106.91(9) 7_565 . . . ? Cu2 Cu3 S2 C13 -61.18(9) . . . . ? N5 Cu3 S2 Cu1 126.11(7) . . . . ? S1 Cu3 S2 Cu1 -73.54(3) 7_565 . . . ? Cu1 Cu3 S2 Cu1 7.64(4) 7_565 . . . ? Cu2 Cu3 S2 Cu1 53.38(2) . . . . ? N1 Cu1 S2 C13 -26.11(13) . . . . ? S3 Cu1 S2 C13 175.90(10) 7_565 . . . ? Cu2 Cu1 S2 C13 49.59(10) . . . . ? Cu3 Cu1 S2 C13 99.38(10) 7_565 . . . ? N1 Cu1 S2 Cu3 -133.26(8) . . . . ? S3 Cu1 S2 Cu3 68.74(3) 7_565 . . . ? Cu2 Cu1 S2 Cu3 -57.57(2) . . . . ? Cu3 Cu1 S2 Cu3 -7.77(4) 7_565 . . . ? N3 Cu2 S3 C25 11.23(11) . . . . ? S1 Cu2 S3 C25 172.07(9) . . . . ? Cu1 Cu2 S3 C25 -105.72(9) . . . . ? Cu3 Cu2 S3 C25 -60.22(9) . . . . ? N3 Cu2 S3 Cu1 126.15(7) . . . 7_565 ? S1 Cu2 S3 Cu1 -73.02(3) . . . 7_565 ? Cu1 Cu2 S3 Cu1 9.20(4) . . . 7_565 ? Cu3 Cu2 S3 Cu1 54.70(2) . . . 7_565 ? S2 Cu1 N1 C2 -72.6(3) . . . . ? S3 Cu1 N1 C2 81.0(3) 7_565 . . . ? Cu2 Cu1 N1 C2 -139.3(2) . . . . ? Cu3 Cu1 N1 C2 146.6(2) 7_565 . . . ? S2 Cu1 N1 C1 105.31(18) . . . . ? S3 Cu1 N1 C1 -101.05(17) 7_565 . . . ? Cu2 Cu1 N1 C1 38.58(18) . . . . ? Cu3 Cu1 N1 C1 -35.48(17) 7_565 . . . ? S1 Cu2 N3 C13 109.81(18) . . . . ? S3 Cu2 N3 C13 -93.60(18) . . . . ? Cu1 Cu2 N3 C13 41.94(18) . . . . ? Cu3 Cu2 N3 C13 -32.83(18) . . . . ? S1 Cu2 N3 C16 -77.2(2) . . . . ? S3 Cu2 N3 C16 79.4(2) . . . . ? Cu1 Cu2 N3 C16 -145.0(2) . . . . ? Cu3 Cu2 N3 C16 140.2(2) . . . . ? S1 Cu3 N5 C25 110.12(18) 7_565 . . . ? S2 Cu3 N5 C25 -93.37(19) . . . . ? Cu1 Cu3 N5 C25 42.65(19) 7_565 . . . ? Cu2 Cu3 N5 C25 -31.79(18) . . . . ? S1 Cu3 N5 C26 -79.5(3) 7_565 . . . ? S2 Cu3 N5 C26 77.0(2) . . . . ? Cu1 Cu3 N5 C26 -147.0(2) 7_565 . . . ? Cu2 Cu3 N5 C26 138.6(2) . . . . ? C4 N2 C1 N1 3.1(4) . . . . ? C4 N2 C1 S1 -178.1(2) . . . . ? C2 N1 C1 N2 -5.6(4) . . . . ? Cu1 N1 C1 N2 176.2(2) . . . . ? C2 N1 C1 S1 175.6(2) . . . . ? Cu1 N1 C1 S1 -2.7(3) . . . . ? Cu3 S1 C1 N2 -124.57(19) 7_565 . . . ? Cu2 S1 C1 N2 132.62(19) . . . . ? Cu3 S1 C1 N1 54.3(2) 7_565 . . . ? Cu2 S1 C1 N1 -48.5(2) . . . . ? C1 N1 C2 C3 1.4(4) . . . . ? Cu1 N1 C2 C3 179.3(2) . . . . ? N1 C2 C3 C4 4.6(4) . . . . ? N1 C2 C3 C5 -174.4(3) . . . . ? C1 N2 C4 C3 3.7(4) . . . . ? C1 N2 C4 C6 -176.5(2) . . . . ? C2 C3 C4 N2 -7.2(4) . . . . ? C5 C3 C4 N2 171.8(3) . . . . ? C2 C3 C4 C6 173.0(3) . . . . ? C5 C3 C4 C6 -8.0(5) . . . . ? N2 C4 C6 C7 146.5(3) . . . . ? C3 C4 C6 C7 -33.6(4) . . . . ? N2 C4 C6 C11 -29.7(4) . . . . ? C3 C4 C6 C11 150.1(3) . . . . ? C11 C6 C7 C8 -0.8(5) . . . . ? C4 C6 C7 C8 -177.1(3) . . . . ? C6 C7 C8 C9 0.8(5) . . . . ? C7 C8 C9 C10 -0.5(5) . . . . ? C7 C8 C9 C12 178.8(3) . . . . ? C8 C9 C10 C11 0.3(5) . . . . ? C12 C9 C10 C11 -179.1(3) . . . . ? C9 C10 C11 C6 -0.3(5) . . . . ? C7 C6 C11 C10 0.5(5) . . . . ? C4 C6 C11 C10 176.9(3) . . . . ? C14 N4 C13 N3 5.2(5) . . . . ? C14 N4 C13 S2 -175.9(2) . . . . ? C16 N3 C13 N4 -4.8(4) . . . . ? Cu2 N3 C13 N4 169.0(2) . . . . ? C16 N3 C13 S2 176.2(2) . . . . ? Cu2 N3 C13 S2 -9.9(3) . . . . ? Cu3 S2 C13 N4 -110.8(2) . . . . ? Cu1 S2 C13 N4 141.0(2) . . . . ? Cu3 S2 C13 N3 68.3(2) . . . . ? Cu1 S2 C13 N3 -39.9(2) . . . . ? C13 N4 C14 C15 -1.5(5) . . . . ? N4 C14 C15 C16 -2.0(5) . . . . ? N4 C14 C15 C17 174.4(4) . . . . ? C13 N3 C16 C15 0.7(4) . . . . ? Cu2 N3 C16 C15 -172.1(2) . . . . ? C13 N3 C16 C18 -176.5(2) . . . . ? Cu2 N3 C16 C18 10.8(4) . . . . ? C14 C15 C16 N3 2.5(5) . . . . ? C17 C15 C16 N3 -173.9(3) . . . . ? C14 C15 C16 C18 179.4(3) . . . . ? C17 C15 C16 C18 3.1(5) . . . . ? N3 C16 C18 C23 -128.7(3) . . . . ? C15 C16 C18 C23 54.2(4) . . . . ? N3 C16 C18 C19 53.1(4) . . . . ? C15 C16 C18 C19 -124.0(3) . . . . ? C23 C18 C19 C20 -0.8(5) . . . . ? C16 C18 C19 C20 177.4(3) . . . . ? C18 C19 C20 C21 -0.3(5) . . . . ? C19 C20 C21 C22 1.2(5) . . . . ? C19 C20 C21 C24 -177.9(3) . . . . ? C20 C21 C22 C23 -1.1(5) . . . . ? C24 C21 C22 C23 178.0(3) . . . . ? C19 C18 C23 C22 0.9(5) . . . . ? C16 C18 C23 C22 -177.2(3) . . . . ? C21 C22 C23 C18 0.0(5) . . . . ? C28 N6 C25 N5 0.0(5) . . . . ? C28 N6 C25 S3 179.7(3) . . . . ? C26 N5 C25 N6 -2.1(4) . . . . ? Cu3 N5 C25 N6 169.4(3) . . . . ? C26 N5 C25 S3 178.3(2) . . . . ? Cu3 N5 C25 S3 -10.2(3) . . . . ? Cu2 S3 C25 N6 -111.9(2) . . . . ? Cu1 S3 C25 N6 139.2(2) 7_565 . . . ? Cu2 S3 C25 N5 67.7(2) . . . . ? Cu1 S3 C25 N5 -41.1(2) 7_565 . . . ? C25 N5 C26 C27 2.0(4) . . . . ? Cu3 N5 C26 C27 -167.9(2) . . . . ? C25 N5 C26 C30 -174.2(2) . . . . ? Cu3 N5 C26 C30 15.9(4) . . . . ? N5 C26 C27 C28 0.1(5) . . . . ? C30 C26 C27 C28 176.0(3) . . . . ? N5 C26 C27 C29 -178.4(3) . . . . ? C30 C26 C27 C29 -2.5(5) . . . . ? C25 N6 C28 C27 2.3(5) . . . . ? C26 C27 C28 N6 -2.3(5) . . . . ? C29 C27 C28 N6 176.2(3) . . . . ? N5 C26 C30 C31 47.2(4) . . . . ? C27 C26 C30 C31 -128.9(3) . . . . ? N5 C26 C30 C35 -134.5(3) . . . . ? C27 C26 C30 C35 49.4(4) . . . . ? C35 C30 C31 C32 0.6(4) . . . . ? C26 C30 C31 C32 179.0(3) . . . . ? C30 C31 C32 C33 0.1(4) . . . . ? C31 C32 C33 C34 -0.8(4) . . . . ? C31 C32 C33 C36 178.0(3) . . . . ? C32 C33 C34 C35 0.7(4) . . . . ? C36 C33 C34 C35 -178.1(3) . . . . ? C33 C34 C35 C30 0.0(4) . . . . ? C31 C30 C35 C34 -0.7(4) . . . . ? C26 C30 C35 C34 -179.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.453 _refine_diff_density_min -0.507 _refine_diff_density_rms 0.071