# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # 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_09acmg18 #TrackingRef 'alzuet_dalton.ccd' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H28 Cl2 Cu N6 O4 S4' _chemical_formula_sum 'C38 H28 Cl2 Cu N6 O4 S4' _chemical_formula_weight 895.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.0860(13) _cell_length_b 14.1850(18) _cell_length_c 14.815(3) _cell_angle_alpha 95.579(4) _cell_angle_beta 98.024(5) _cell_angle_gamma 103.237(10) _cell_volume 2024.6(5) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3215 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 21.036 _exptl_crystal_description prism _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.469 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 914 _exptl_absorpt_coefficient_mu 0.925 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD2000' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 9248 _diffrn_reflns_av_R_equivalents 0.0496 _diffrn_reflns_av_sigmaI/netI 0.0923 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 27.47 _reflns_number_total 9248 _reflns_number_gt 8113 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SIR97 (Altomare et Al, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2004)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0468P)^2^+1.3244P] 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 9248 _refine_ls_number_parameters 498 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0811 _refine_ls_R_factor_gt 0.0536 _refine_ls_wR_factor_ref 0.1398 _refine_ls_wR_factor_gt 0.1247 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _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 0.30304(7) 0.62476(5) 0.23534(6) 0.0536(3) Uani 1 1 d . . . Cl14 Cl 0.4003(2) 1.11797(13) 0.08849(16) 0.0935(7) Uani 1 1 d . . . Cl34 Cl 1.03288(18) 0.89086(14) 0.24346(18) 0.0942(7) Uani 1 1 d . . . S11 S 0.40450(18) 0.92258(11) 0.39303(12) 0.0603(5) Uani 1 1 d . . . S21 S 0.35024(18) 0.75803(13) 0.52949(13) 0.0663(5) Uani 1 1 d . . . S31 S 0.56431(18) 0.66183(13) 0.01782(13) 0.0675(5) Uani 1 1 d . . . S41 S 0.24221(19) 0.54440(13) -0.06273(13) 0.0692(5) Uani 1 1 d . . . O21 O 0.4639(5) 0.8409(3) 0.5675(3) 0.0788(14) Uani 1 1 d . . . O22 O 0.3442(5) 0.6702(3) 0.5726(4) 0.0819(15) Uani 1 1 d . . . O41 O 0.1318(5) 0.4573(3) -0.0758(4) 0.0855(15) Uani 1 1 d . . . O42 O 0.3513(5) 0.5449(3) -0.1160(3) 0.0754(13) Uani 1 1 d . . . N1 N 0.3181(6) 0.4897(4) 0.2514(4) 0.0582(14) Uani 1 1 d . . . N2 N 0.1196(5) 0.5731(4) 0.2687(4) 0.0546(13) Uani 1 1 d . . . N18 N 0.3183(5) 0.7648(3) 0.2729(4) 0.0521(13) Uani 1 1 d . . . N20 N 0.3412(5) 0.7270(3) 0.4222(4) 0.0564(14) Uani 1 1 d . . . N38 N 0.4583(5) 0.6553(3) 0.1683(4) 0.0529(13) Uani 1 1 d . . . N40 N 0.2971(6) 0.5713(4) 0.0442(4) 0.0631(15) Uani 1 1 d . . . C1 C 0.4259(8) 0.4526(5) 0.2361(5) 0.070(2) Uani 1 1 d . . . H1 H 0.4966 0.4897 0.2110 0.084 Uiso 1 1 calc R . . C2 C 0.4342(8) 0.3615(5) 0.2564(6) 0.081(2) Uani 1 1 d . . . H2 H 0.5106 0.3378 0.2474 0.097 Uiso 1 1 calc R . . C3 C 0.3276(10) 0.3073(6) 0.2902(6) 0.092(3) Uani 1 1 d . . . H3 H 0.3312 0.2455 0.3048 0.110 Uiso 1 1 calc R . . C4 C 0.2166(9) 0.3420(5) 0.3027(6) 0.084(2) Uani 1 1 d . . . H4 H 0.1430 0.3034 0.3241 0.101 Uiso 1 1 calc R . . C5 C 0.2123(7) 0.4357(5) 0.2836(5) 0.0616(18) Uani 1 1 d . . . C6 C 0.0979(6) 0.4822(5) 0.2923(5) 0.0589(17) Uani 1 1 d . . . C7 C -0.0233(7) 0.4396(5) 0.3221(5) 0.070(2) Uani 1 1 d . . . H7 H -0.0357 0.3775 0.3399 0.085 Uiso 1 1 calc R . . C8 C -0.1253(8) 0.4891(6) 0.3252(5) 0.076(2) Uani 1 1 d . . . H8 H -0.2069 0.4608 0.3451 0.091 Uiso 1 1 calc R . . C9 C -0.1057(7) 0.5790(5) 0.2991(5) 0.070(2) Uani 1 1 d . . . H9 H -0.1739 0.6134 0.2996 0.084 Uiso 1 1 calc R . . C10 C 0.0184(7) 0.6189(5) 0.2716(5) 0.0666(19) Uani 1 1 d . . . H10 H 0.0319 0.6812 0.2542 0.080 Uiso 1 1 calc R . . C12 C 0.3820(6) 0.9342(4) 0.2760(4) 0.0515(16) Uani 1 1 d . . . C13 C 0.4036(6) 1.0218(4) 0.2371(5) 0.0623(18) Uani 1 1 d . . . H13 H 0.4342 1.0826 0.2731 0.075 Uiso 1 1 calc R . . C14 C 0.3768(7) 1.0125(5) 0.1424(5) 0.0629(18) Uani 1 1 d . . . C15 C 0.3341(7) 0.9223(5) 0.0872(5) 0.0701(19) Uani 1 1 d . . . H15 H 0.3202 0.9194 0.0235 0.084 Uiso 1 1 calc R . . C16 C 0.3124(6) 0.8367(4) 0.1271(5) 0.0600(17) Uani 1 1 d . . . H16 H 0.2813 0.7761 0.0909 0.072 Uiso 1 1 calc R . . C17 C 0.3383(6) 0.8439(4) 0.2229(5) 0.0512(16) Uani 1 1 d . . . C19 C 0.3489(6) 0.7938(4) 0.3633(5) 0.0522(17) Uani 1 1 d . . . C22 C 0.1973(7) 0.7961(5) 0.5421(5) 0.0607(18) Uani 1 1 d . . . C23 C 0.0730(7) 0.7333(5) 0.5069(5) 0.072(2) Uani 1 1 d . . . H23 H 0.0701 0.6713 0.4784 0.086 Uiso 1 1 calc R . . C24 C -0.0501(8) 0.7606(6) 0.5129(6) 0.081(2) Uani 1 1 d . . . H24 H -0.1341 0.7175 0.4872 0.097 Uiso 1 1 calc R . . C25 C -0.0474(9) 0.8509(7) 0.5567(6) 0.080(2) Uani 1 1 d . . . C26 C 0.0782(10) 0.9125(6) 0.5921(7) 0.097(3) Uani 1 1 d . . . H26 H 0.0819 0.9739 0.6221 0.116 Uiso 1 1 calc R . . C27 C 0.2006(9) 0.8858(6) 0.5845(6) 0.083(2) Uani 1 1 d . . . H27 H 0.2849 0.9294 0.6085 0.100 Uiso 1 1 calc R . . C28 C -0.1803(9) 0.8812(7) 0.5625(7) 0.111(3) Uani 1 1 d . . . H28A H -0.1726 0.9450 0.5441 0.167 Uiso 1 1 calc R . . H28B H -0.1977 0.8827 0.6247 0.167 Uiso 1 1 calc R . . H28C H -0.2552 0.8352 0.5225 0.167 Uiso 1 1 calc R . . C32 C 0.6667(7) 0.7255(4) 0.1206(5) 0.0614(18) Uani 1 1 d . . . C33 C 0.8035(7) 0.7805(5) 0.1360(6) 0.073(2) Uani 1 1 d . . . H33 H 0.8535 0.7878 0.0879 0.088 Uiso 1 1 calc R . . C34 C 0.8630(7) 0.8240(5) 0.2245(6) 0.0654(19) Uani 1 1 d . . . C35 C 0.7898(7) 0.8130(5) 0.2957(6) 0.0682(19) Uani 1 1 d . . . H35 H 0.8313 0.8439 0.3544 0.082 Uiso 1 1 calc R . . C36 C 0.6550(7) 0.7567(5) 0.2815(6) 0.068(2) Uani 1 1 d . . . H36 H 0.6071 0.7479 0.3305 0.082 Uiso 1 1 calc R . . C37 C 0.5931(7) 0.7137(4) 0.1936(5) 0.0556(17) Uani 1 1 d . . . C39 C 0.4259(7) 0.6247(4) 0.0787(5) 0.0542(17) Uani 1 1 d . . . C42 C 0.1692(8) 0.6430(5) -0.0906(5) 0.0689(19) Uani 1 1 d . . . C43 C 0.2394(9) 0.7182(6) -0.1301(6) 0.084(2) Uani 1 1 d . . . H43 H 0.3261 0.7172 -0.1442 0.101 Uiso 1 1 calc R . . C44 C 0.1836(11) 0.7950(7) -0.1490(6) 0.099(3) Uani 1 1 d . . . H44 H 0.2318 0.8449 -0.1770 0.118 Uiso 1 1 calc R . . C45 C 0.0571(13) 0.7987(7) -0.1269(7) 0.105(3) Uani 1 1 d . . . C46 C -0.0141(10) 0.7217(9) -0.0870(7) 0.117(3) Uani 1 1 d . . . H46 H -0.0999 0.7232 -0.0714 0.140 Uiso 1 1 calc R . . C47 C 0.0413(9) 0.6433(7) -0.0703(6) 0.091(2) Uani 1 1 d . . . H47 H -0.0081 0.5912 -0.0455 0.110 Uiso 1 1 calc R . . C48 C -0.0021(13) 0.8878(8) -0.1458(9) 0.163(5) Uani 1 1 d . . . H48A H -0.0487 0.9041 -0.0965 0.244 Uiso 1 1 calc R . . H48B H -0.0662 0.8719 -0.2026 0.244 Uiso 1 1 calc R . . H48C H 0.0720 0.9425 -0.1501 0.244 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 0.0616(5) 0.0412(5) 0.0577(6) 0.0094(4) 0.0151(4) 0.0081(4) Cl14 0.1293(17) 0.0575(11) 0.0921(16) 0.0308(11) 0.0193(13) 0.0107(11) Cl34 0.0628(11) 0.0749(13) 0.137(2) 0.0084(13) 0.0133(12) 0.0060(10) S11 0.0741(11) 0.0432(9) 0.0582(12) 0.0036(8) 0.0097(9) 0.0058(8) S21 0.0719(12) 0.0635(12) 0.0608(13) 0.0140(10) 0.0071(9) 0.0110(10) S31 0.0742(11) 0.0661(11) 0.0618(13) 0.0113(10) 0.0231(10) 0.0084(9) S41 0.0764(12) 0.0659(12) 0.0603(13) 0.0032(9) 0.0163(10) 0.0062(10) O21 0.073(3) 0.086(3) 0.063(3) 0.002(3) -0.001(2) 0.001(3) O22 0.096(3) 0.073(3) 0.086(4) 0.034(3) 0.020(3) 0.027(3) O41 0.092(3) 0.073(3) 0.075(4) -0.004(3) 0.021(3) -0.011(3) O42 0.090(3) 0.078(3) 0.057(3) 0.002(3) 0.025(3) 0.015(3) N1 0.068(4) 0.051(3) 0.056(4) 0.009(3) 0.013(3) 0.014(3) N2 0.058(3) 0.045(3) 0.059(4) 0.006(3) 0.008(3) 0.011(3) N18 0.062(3) 0.040(3) 0.050(4) 0.001(3) 0.011(3) 0.006(2) N20 0.071(3) 0.041(3) 0.056(4) 0.010(3) 0.013(3) 0.009(3) N38 0.056(3) 0.046(3) 0.053(4) 0.009(3) 0.009(3) 0.005(3) N40 0.071(4) 0.061(3) 0.058(4) 0.014(3) 0.016(3) 0.011(3) C1 0.090(5) 0.061(5) 0.068(5) 0.014(4) 0.030(4) 0.022(4) C2 0.093(6) 0.070(5) 0.103(7) 0.032(5) 0.033(5) 0.045(5) C3 0.126(7) 0.063(5) 0.104(7) 0.030(5) 0.042(6) 0.037(6) C4 0.107(6) 0.065(5) 0.097(7) 0.041(5) 0.041(5) 0.027(5) C5 0.077(5) 0.047(4) 0.057(5) 0.012(3) 0.013(4) 0.004(4) C6 0.058(4) 0.050(4) 0.066(5) 0.010(4) 0.008(3) 0.008(4) C7 0.075(5) 0.048(4) 0.082(6) 0.017(4) 0.018(4) -0.003(4) C8 0.067(5) 0.072(5) 0.079(6) 0.011(4) 0.013(4) 0.000(4) C9 0.049(4) 0.072(5) 0.088(6) 0.003(4) 0.015(4) 0.016(4) C10 0.067(5) 0.057(4) 0.072(5) 0.005(4) 0.007(4) 0.013(4) C12 0.052(4) 0.042(4) 0.056(4) -0.001(3) 0.010(3) 0.006(3) C13 0.071(4) 0.042(4) 0.068(6) 0.008(4) 0.007(4) 0.005(3) C14 0.072(5) 0.043(4) 0.073(6) 0.021(4) 0.014(4) 0.007(3) C15 0.094(5) 0.056(5) 0.061(5) 0.019(4) 0.017(4) 0.013(4) C16 0.078(5) 0.043(4) 0.053(5) -0.007(3) 0.012(4) 0.009(3) C17 0.046(4) 0.038(4) 0.070(5) 0.006(4) 0.013(3) 0.008(3) C19 0.045(4) 0.038(4) 0.068(6) -0.001(4) 0.007(3) 0.004(3) C22 0.064(5) 0.055(4) 0.057(5) 0.010(4) 0.009(4) 0.002(4) C23 0.072(5) 0.073(5) 0.073(6) 0.016(4) 0.014(4) 0.019(5) C24 0.066(5) 0.088(6) 0.078(6) 0.010(5) 0.008(4) 0.004(4) C25 0.089(6) 0.084(6) 0.083(6) 0.030(5) 0.047(5) 0.023(5) C26 0.097(7) 0.065(5) 0.128(8) 0.009(5) 0.050(6) 0.003(6) C27 0.086(6) 0.066(5) 0.091(6) 0.005(5) 0.024(5) 0.002(4) C28 0.114(7) 0.123(7) 0.126(9) 0.044(7) 0.057(6) 0.053(6) C32 0.072(5) 0.049(4) 0.072(5) 0.022(4) 0.027(4) 0.019(4) C33 0.054(4) 0.065(5) 0.109(8) 0.022(5) 0.036(5) 0.015(4) C34 0.061(4) 0.059(4) 0.075(6) 0.005(4) 0.013(4) 0.014(4) C35 0.065(5) 0.059(4) 0.079(6) 0.009(4) 0.005(4) 0.016(4) C36 0.066(5) 0.069(5) 0.078(6) 0.021(4) 0.022(4) 0.022(4) C37 0.065(5) 0.045(4) 0.061(5) 0.013(4) 0.014(4) 0.017(4) C39 0.071(5) 0.041(4) 0.056(5) 0.016(3) 0.018(4) 0.016(4) C42 0.067(5) 0.076(5) 0.055(5) -0.002(4) 0.011(4) 0.006(4) C43 0.092(6) 0.082(6) 0.074(6) 0.009(5) 0.018(5) 0.012(5) C44 0.121(8) 0.088(6) 0.086(7) 0.024(5) 0.009(6) 0.023(6) C45 0.131(9) 0.101(7) 0.080(7) 0.001(6) -0.003(6) 0.043(7) C46 0.113(7) 0.149(9) 0.105(8) 0.018(8) 0.028(6) 0.061(8) C47 0.101(7) 0.113(7) 0.067(6) 0.024(5) 0.017(5) 0.032(6) C48 0.214(12) 0.156(10) 0.147(11) 0.021(9) 0.004(9) 0.121(10) _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 N38 1.957(5) . y Cu1 N18 1.975(5) . y Cu1 N2 1.977(5) . y Cu1 N1 1.991(5) . y Cu1 N40 2.848(6) . y Cu1 N20 2.929(5) . y Cl14 C14 1.747(6) . ? Cl34 C34 1.728(7) . ? S11 C12 1.746(7) . ? S11 C19 1.775(6) . ? S21 O21 1.445(5) . ? S21 O22 1.447(4) . ? S21 N20 1.592(6) . ? S21 C22 1.775(7) . ? S31 C32 1.751(7) . ? S31 C39 1.774(6) . ? S41 O41 1.438(5) . ? S41 O42 1.440(5) . ? S41 N40 1.582(6) . ? S41 C42 1.779(8) . ? N1 C5 1.339(7) . ? N1 C1 1.348(8) . ? N2 C10 1.333(8) . ? N2 C6 1.347(7) . ? N18 C19 1.334(8) . ? N18 C17 1.395(7) . ? N20 C19 1.345(8) . ? N38 C39 1.326(8) . ? N38 C37 1.399(8) . ? N40 C39 1.346(8) . ? C1 C2 1.372(9) . ? C1 H1 0.9300 . ? C2 C3 1.358(10) . ? C2 H2 0.9300 . ? C3 C4 1.351(10) . ? C3 H3 0.9300 . ? C4 C5 1.395(9) . ? C4 H4 0.9300 . ? C5 C6 1.469(9) . ? C6 C7 1.384(9) . ? C7 C8 1.376(9) . ? C7 H7 0.9300 . ? C8 C9 1.348(9) . ? C8 H8 0.9300 . ? C9 C10 1.385(9) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C12 C17 1.380(8) . ? C12 C13 1.405(8) . ? C13 C14 1.379(9) . ? C13 H13 0.9300 . ? C14 C15 1.392(9) . ? C15 C16 1.388(8) . ? C15 H15 0.9300 . ? C16 C17 1.396(9) . ? C16 H16 0.9300 . ? C22 C27 1.353(9) . ? C22 C23 1.361(9) . ? C23 C24 1.394(9) . ? C23 H23 0.9300 . ? C24 C25 1.371(10) . ? C24 H24 0.9300 . ? C25 C26 1.364(11) . ? C25 C28 1.509(10) . ? C26 C27 1.387(10) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C32 C33 1.396(9) . ? C32 C37 1.397(9) . ? C33 C34 1.383(10) . ? C33 H33 0.9300 . ? C34 C35 1.369(10) . ? C35 C36 1.386(9) . ? C35 H35 0.9300 . ? C36 C37 1.379(10) . ? C36 H36 0.9300 . ? C42 C47 1.366(10) . ? C42 C43 1.369(10) . ? C43 C44 1.371(11) . ? C43 H43 0.9300 . ? C44 C45 1.371(12) . ? C44 H44 0.9300 . ? C45 C46 1.394(13) . ? C45 C48 1.549(12) . ? C46 C47 1.382(11) . ? C46 H46 0.9300 . ? C47 H47 0.9300 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 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 N38 Cu1 N18 91.6(2) . . y N38 Cu1 N2 163.7(2) . . y N18 Cu1 N2 97.7(2) . . y N38 Cu1 N1 95.6(2) . . y N18 Cu1 N1 156.7(2) . . y N2 Cu1 N1 81.0(2) . . y N38 Cu1 N40 53.40(19) . . y N18 Cu1 N40 115.06(19) . . y N2 Cu1 N40 110.34(19) . . y N1 Cu1 N40 86.72(19) . . y N38 Cu1 N20 117.00(19) . . y N18 Cu1 N20 52.14(18) . . y N2 Cu1 N20 79.18(18) . . y N1 Cu1 N20 105.26(18) . . y N40 Cu1 N20 166.03(14) . . y C12 S11 C19 88.8(3) . . ? O21 S21 O22 116.5(3) . . ? O21 S21 N20 113.3(3) . . ? O22 S21 N20 106.8(3) . . ? O21 S21 C22 106.2(3) . . ? O22 S21 C22 107.3(3) . . ? N20 S21 C22 106.2(3) . . ? C32 S31 C39 89.4(3) . . ? O41 S41 O42 117.5(3) . . ? O41 S41 N40 107.5(3) . . ? O42 S41 N40 113.0(3) . . ? O41 S41 C42 107.9(3) . . ? O42 S41 C42 106.7(3) . . ? N40 S41 C42 103.3(3) . . ? C5 N1 C1 120.0(5) . . ? C5 N1 Cu1 114.6(4) . . ? C1 N1 Cu1 125.4(4) . . ? C10 N2 C6 117.7(5) . . ? C10 N2 Cu1 127.1(4) . . ? C6 N2 Cu1 115.2(4) . . ? C19 N18 C17 111.8(5) . . ? C19 N18 Cu1 115.2(4) . . ? C17 N18 Cu1 130.7(4) . . ? C19 N20 S21 121.1(4) . . ? C19 N20 Cu1 71.8(4) . . ? S21 N20 Cu1 166.9(3) . . ? C39 N38 C37 112.5(6) . . ? C39 N38 Cu1 114.3(4) . . ? C37 N38 Cu1 132.6(5) . . ? C39 N40 S41 122.5(5) . . ? C39 N40 Cu1 73.4(4) . . ? S41 N40 Cu1 160.7(3) . . ? N1 C1 C2 121.9(7) . . ? N1 C1 H1 119.0 . . ? C2 C1 H1 119.0 . . ? C3 C2 C1 118.0(7) . . ? C3 C2 H2 121.0 . . ? C1 C2 H2 121.0 . . ? C4 C3 C2 120.8(7) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C3 C4 C5 120.0(7) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? N1 C5 C4 119.2(7) . . ? N1 C5 C6 114.7(6) . . ? C4 C5 C6 126.0(7) . . ? N2 C6 C7 120.9(6) . . ? N2 C6 C5 114.1(6) . . ? C7 C6 C5 125.0(6) . . ? C8 C7 C6 120.0(6) . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C9 C8 C7 119.3(7) . . ? C9 C8 H8 120.4 . . ? C7 C8 H8 120.4 . . ? C8 C9 C10 118.4(7) . . ? C8 C9 H9 120.8 . . ? C10 C9 H9 120.8 . . ? N2 C10 C9 123.7(6) . . ? N2 C10 H10 118.2 . . ? C9 C10 H10 118.2 . . ? C17 C12 C13 122.2(6) . . ? C17 C12 S11 111.1(5) . . ? C13 C12 S11 126.7(5) . . ? C14 C13 C12 116.1(6) . . ? C14 C13 H13 121.9 . . ? C12 C13 H13 121.9 . . ? C13 C14 C15 122.8(6) . . ? C13 C14 Cl14 119.0(5) . . ? C15 C14 Cl14 118.2(6) . . ? C16 C15 C14 120.1(7) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C15 C16 C17 118.3(6) . . ? C15 C16 H16 120.8 . . ? C17 C16 H16 120.8 . . ? C12 C17 N18 114.6(6) . . ? C12 C17 C16 120.4(6) . . ? N18 C17 C16 125.0(6) . . ? N18 C19 N20 119.9(5) . . ? N18 C19 S11 113.7(5) . . ? N20 C19 S11 126.3(5) . . ? C27 C22 C23 119.2(7) . . ? C27 C22 S21 122.1(6) . . ? C23 C22 S21 118.7(6) . . ? C22 C23 C24 120.9(7) . . ? C22 C23 H23 119.5 . . ? C24 C23 H23 119.5 . . ? C25 C24 C23 120.1(7) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C26 C25 C24 118.0(7) . . ? C26 C25 C28 121.7(8) . . ? C24 C25 C28 120.3(8) . . ? C25 C26 C27 121.8(8) . . ? C25 C26 H26 119.1 . . ? C27 C26 H26 119.1 . . ? C22 C27 C26 120.0(7) . . ? C22 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C33 C32 C37 120.3(7) . . ? C33 C32 S31 129.3(6) . . ? C37 C32 S31 110.4(5) . . ? C34 C33 C32 118.5(7) . . ? C34 C33 H33 120.7 . . ? C32 C33 H33 120.7 . . ? C35 C34 C33 120.9(7) . . ? C35 C34 Cl34 120.8(7) . . ? C33 C34 Cl34 118.3(6) . . ? C34 C35 C36 121.1(7) . . ? C34 C35 H35 119.5 . . ? C36 C35 H35 119.5 . . ? C37 C36 C35 119.0(7) . . ? C37 C36 H36 120.5 . . ? C35 C36 H36 120.5 . . ? C36 C37 C32 120.2(6) . . ? C36 C37 N38 125.7(6) . . ? C32 C37 N38 114.1(7) . . ? N38 C39 N40 118.8(6) . . ? N38 C39 S31 113.5(5) . . ? N40 C39 S31 127.6(6) . . ? C47 C42 C43 120.0(7) . . ? C47 C42 S41 118.6(6) . . ? C43 C42 S41 121.4(6) . . ? C42 C43 C44 120.9(8) . . ? C42 C43 H43 119.6 . . ? C44 C43 H43 119.6 . . ? C43 C44 C45 120.4(9) . . ? C43 C44 H44 119.8 . . ? C45 C44 H44 119.8 . . ? C44 C45 C46 118.5(8) . . ? C44 C45 C48 119.7(11) . . ? C46 C45 C48 121.8(11) . . ? C47 C46 C45 120.7(9) . . ? C47 C46 H46 119.6 . . ? C45 C46 H46 119.6 . . ? C42 C47 C46 119.5(8) . . ? C42 C47 H47 120.3 . . ? C46 C47 H47 120.3 . . ? C45 C48 H48A 109.5 . . ? C45 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C45 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 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 N38 Cu1 N1 C5 -170.0(5) . . . . ? N18 Cu1 N1 C5 82.5(7) . . . . ? N2 Cu1 N1 C5 -6.1(5) . . . . ? N40 Cu1 N1 C5 -117.3(5) . . . . ? N20 Cu1 N1 C5 70.0(5) . . . . ? N38 Cu1 N1 C1 12.8(6) . . . . ? N18 Cu1 N1 C1 -94.8(7) . . . . ? N2 Cu1 N1 C1 176.7(6) . . . . ? N40 Cu1 N1 C1 65.5(5) . . . . ? N20 Cu1 N1 C1 -107.2(5) . . . . ? N38 Cu1 N2 C10 -96.8(8) . . . . ? N18 Cu1 N2 C10 27.4(6) . . . . ? N1 Cu1 N2 C10 -176.1(6) . . . . ? N40 Cu1 N2 C10 -93.0(6) . . . . ? N20 Cu1 N2 C10 76.4(6) . . . . ? N38 Cu1 N2 C6 84.4(8) . . . . ? N18 Cu1 N2 C6 -151.4(5) . . . . ? N1 Cu1 N2 C6 5.2(5) . . . . ? N40 Cu1 N2 C6 88.3(5) . . . . ? N20 Cu1 N2 C6 -102.4(5) . . . . ? N38 Cu1 N18 C19 -117.2(4) . . . . ? N2 Cu1 N18 C19 76.2(4) . . . . ? N1 Cu1 N18 C19 -8.9(8) . . . . ? N40 Cu1 N18 C19 -167.1(4) . . . . ? N20 Cu1 N18 C19 6.3(4) . . . . ? N38 Cu1 N18 C17 43.7(5) . . . . ? N2 Cu1 N18 C17 -122.9(5) . . . . ? N1 Cu1 N18 C17 152.0(5) . . . . ? N40 Cu1 N18 C17 -6.1(6) . . . . ? N20 Cu1 N18 C17 167.3(6) . . . . ? O21 S21 N20 C19 -48.2(6) . . . . ? O22 S21 N20 C19 -177.7(5) . . . . ? C22 S21 N20 C19 68.0(5) . . . . ? O21 S21 N20 Cu1 144.9(11) . . . . ? O22 S21 N20 Cu1 15.4(13) . . . . ? C22 S21 N20 Cu1 -98.9(12) . . . . ? N38 Cu1 N20 C19 63.2(4) . . . . ? N18 Cu1 N20 C19 -6.0(3) . . . . ? N2 Cu1 N20 C19 -114.7(4) . . . . ? N1 Cu1 N20 C19 167.8(3) . . . . ? N40 Cu1 N20 C19 19.5(8) . . . . ? N38 Cu1 N20 S21 -128.6(12) . . . . ? N18 Cu1 N20 S21 162.2(13) . . . . ? N2 Cu1 N20 S21 53.5(12) . . . . ? N1 Cu1 N20 S21 -24.0(13) . . . . ? N40 Cu1 N20 S21 -172.3(10) . . . . ? N18 Cu1 N38 C39 -118.0(4) . . . . ? N2 Cu1 N38 C39 7.0(9) . . . . ? N1 Cu1 N38 C39 84.1(4) . . . . ? N40 Cu1 N38 C39 2.4(4) . . . . ? N20 Cu1 N38 C39 -165.6(4) . . . . ? N18 Cu1 N38 C37 52.4(5) . . . . ? N2 Cu1 N38 C37 177.4(6) . . . . ? N1 Cu1 N38 C37 -105.5(5) . . . . ? N40 Cu1 N38 C37 172.9(6) . . . . ? N20 Cu1 N38 C37 4.8(6) . . . . ? O41 S41 N40 C39 155.7(5) . . . . ? O42 S41 N40 C39 24.5(6) . . . . ? C42 S41 N40 C39 -90.3(5) . . . . ? O41 S41 N40 Cu1 -61.7(9) . . . . ? O42 S41 N40 Cu1 167.1(8) . . . . ? C42 S41 N40 Cu1 52.3(10) . . . . ? N38 Cu1 N40 C39 -2.3(3) . . . . ? N18 Cu1 N40 C39 69.8(4) . . . . ? N2 Cu1 N40 C39 179.1(3) . . . . ? N1 Cu1 N40 C39 -101.8(4) . . . . ? N20 Cu1 N40 C39 47.7(7) . . . . ? N38 Cu1 N40 S41 -150.0(10) . . . . ? N18 Cu1 N40 S41 -77.9(9) . . . . ? N2 Cu1 N40 S41 31.4(9) . . . . ? N1 Cu1 N40 S41 110.5(9) . . . . ? N20 Cu1 N40 S41 -100.0(10) . . . . ? C5 N1 C1 C2 -3.0(10) . . . . ? Cu1 N1 C1 C2 174.1(6) . . . . ? N1 C1 C2 C3 2.2(12) . . . . ? C1 C2 C3 C4 0.3(13) . . . . ? C2 C3 C4 C5 -1.9(13) . . . . ? C1 N1 C5 C4 1.3(10) . . . . ? Cu1 N1 C5 C4 -176.1(6) . . . . ? C1 N1 C5 C6 -176.6(6) . . . . ? Cu1 N1 C5 C6 6.0(7) . . . . ? C3 C4 C5 N1 1.1(11) . . . . ? C3 C4 C5 C6 178.8(7) . . . . ? C10 N2 C6 C7 -2.5(9) . . . . ? Cu1 N2 C6 C7 176.4(5) . . . . ? C10 N2 C6 C5 177.7(6) . . . . ? Cu1 N2 C6 C5 -3.4(7) . . . . ? N1 C5 C6 N2 -1.7(9) . . . . ? C4 C5 C6 N2 -179.5(7) . . . . ? N1 C5 C6 C7 178.5(6) . . . . ? C4 C5 C6 C7 0.7(12) . . . . ? N2 C6 C7 C8 1.9(10) . . . . ? C5 C6 C7 C8 -178.3(7) . . . . ? C6 C7 C8 C9 0.0(11) . . . . ? C7 C8 C9 C10 -1.2(11) . . . . ? C6 N2 C10 C9 1.3(10) . . . . ? Cu1 N2 C10 C9 -177.4(5) . . . . ? C8 C9 C10 N2 0.6(11) . . . . ? C19 S11 C12 C17 -1.2(4) . . . . ? C19 S11 C12 C13 178.6(6) . . . . ? C17 C12 C13 C14 0.8(9) . . . . ? S11 C12 C13 C14 -179.0(5) . . . . ? C12 C13 C14 C15 -1.6(10) . . . . ? C12 C13 C14 Cl14 179.7(5) . . . . ? C13 C14 C15 C16 2.2(11) . . . . ? Cl14 C14 C15 C16 -179.2(5) . . . . ? C14 C15 C16 C17 -1.8(10) . . . . ? C13 C12 C17 N18 -178.2(5) . . . . ? S11 C12 C17 N18 1.7(6) . . . . ? C13 C12 C17 C16 -0.6(9) . . . . ? S11 C12 C17 C16 179.2(5) . . . . ? C19 N18 C17 C12 -1.3(7) . . . . ? Cu1 N18 C17 C12 -162.7(4) . . . . ? C19 N18 C17 C16 -178.7(5) . . . . ? Cu1 N18 C17 C16 19.8(9) . . . . ? C15 C16 C17 C12 1.1(9) . . . . ? C15 C16 C17 N18 178.4(6) . . . . ? C17 N18 C19 N20 -177.2(5) . . . . ? Cu1 N18 C19 N20 -12.6(7) . . . . ? C17 N18 C19 S11 0.3(6) . . . . ? Cu1 N18 C19 S11 164.9(3) . . . . ? S21 N20 C19 N18 -168.8(4) . . . . ? Cu1 N20 C19 N18 8.1(5) . . . . ? S21 N20 C19 S11 14.0(7) . . . . ? Cu1 N20 C19 S11 -169.1(5) . . . . ? C12 S11 C19 N18 0.5(5) . . . . ? C12 S11 C19 N20 177.8(5) . . . . ? O21 S21 C22 C27 -2.8(7) . . . . ? O22 S21 C22 C27 122.4(6) . . . . ? N20 S21 C22 C27 -123.7(6) . . . . ? O21 S21 C22 C23 176.3(5) . . . . ? O22 S21 C22 C23 -58.4(6) . . . . ? N20 S21 C22 C23 55.5(6) . . . . ? C27 C22 C23 C24 0.9(11) . . . . ? S21 C22 C23 C24 -178.3(6) . . . . ? C22 C23 C24 C25 -1.6(11) . . . . ? C23 C24 C25 C26 1.0(12) . . . . ? C23 C24 C25 C28 179.4(7) . . . . ? C24 C25 C26 C27 0.2(13) . . . . ? C28 C25 C26 C27 -178.2(8) . . . . ? C23 C22 C27 C26 0.3(11) . . . . ? S21 C22 C27 C26 179.5(6) . . . . ? C25 C26 C27 C22 -0.9(13) . . . . ? C39 S31 C32 C33 179.9(6) . . . . ? C39 S31 C32 C37 1.2(5) . . . . ? C37 C32 C33 C34 -1.0(9) . . . . ? S31 C32 C33 C34 -179.6(5) . . . . ? C32 C33 C34 C35 0.4(10) . . . . ? C32 C33 C34 Cl34 179.3(5) . . . . ? C33 C34 C35 C36 1.1(10) . . . . ? Cl34 C34 C35 C36 -177.7(5) . . . . ? C34 C35 C36 C37 -2.0(10) . . . . ? C35 C36 C37 C32 1.3(9) . . . . ? C35 C36 C37 N38 -179.8(5) . . . . ? C33 C32 C37 C36 0.2(9) . . . . ? S31 C32 C37 C36 179.0(5) . . . . ? C33 C32 C37 N38 -178.8(5) . . . . ? S31 C32 C37 N38 0.1(6) . . . . ? C39 N38 C37 C36 179.3(6) . . . . ? Cu1 N38 C37 C36 8.8(9) . . . . ? C39 N38 C37 C32 -1.8(7) . . . . ? Cu1 N38 C37 C32 -172.3(4) . . . . ? C37 N38 C39 N40 -177.1(5) . . . . ? Cu1 N38 C39 N40 -4.7(7) . . . . ? C37 N38 C39 S31 2.7(6) . . . . ? Cu1 N38 C39 S31 175.1(2) . . . . ? S41 N40 C39 N38 171.0(4) . . . . ? Cu1 N40 C39 N38 3.1(4) . . . . ? S41 N40 C39 S31 -8.8(8) . . . . ? Cu1 N40 C39 S31 -176.7(5) . . . . ? C32 S31 C39 N38 -2.2(5) . . . . ? C32 S31 C39 N40 177.5(6) . . . . ? O41 S41 C42 C47 34.9(7) . . . . ? O42 S41 C42 C47 162.0(6) . . . . ? N40 S41 C42 C47 -78.7(6) . . . . ? O41 S41 C42 C43 -146.2(6) . . . . ? O42 S41 C42 C43 -19.0(7) . . . . ? N40 S41 C42 C43 100.2(7) . . . . ? C47 C42 C43 C44 0.6(12) . . . . ? S41 C42 C43 C44 -178.3(6) . . . . ? C42 C43 C44 C45 1.3(13) . . . . ? C43 C44 C45 C46 -1.5(14) . . . . ? C43 C44 C45 C48 177.9(9) . . . . ? C44 C45 C46 C47 -0.2(15) . . . . ? C48 C45 C46 C47 -179.6(9) . . . . ? C43 C42 C47 C46 -2.3(12) . . . . ? S41 C42 C47 C46 176.6(7) . . . . ? C45 C46 C47 C42 2.1(14) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.275 _refine_diff_density_min -0.440 _refine_diff_density_rms 0.066 _database_code_depnum_ccdc_archive 'CCDC 923555' ####################################################################### # # 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_09acmg14 #TrackingRef 'alzuet_dalton.ccd' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H30 Cu N6 O4 S4' _chemical_formula_sum 'C38 H30 Cu N6 O4 S4' _chemical_formula_weight 826.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8010(9) _cell_length_b 12.6420(14) _cell_length_c 16.1080(18) _cell_angle_alpha 78.599(5) _cell_angle_beta 79.689(6) _cell_angle_gamma 73.125(5) _cell_volume 1856.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 832 _cell_measurement_theta_min 0.999 _cell_measurement_theta_max 38.441 _exptl_crystal_description prism _exptl_crystal_colour Grey _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.479 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 850 _exptl_absorpt_coefficient_mu 3.344 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD2000 _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 8492 _diffrn_reflns_av_R_equivalents 0.0554 _diffrn_reflns_av_sigmaI/netI 0.0327 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 89.85 _reflns_number_total 8492 _reflns_number_gt 6675 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SIR97 (ALtomare et AL. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2004)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1154P)^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 8492 _refine_ls_number_parameters 478 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0454 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.1825 _refine_ls_wR_factor_gt 0.1267 _refine_ls_goodness_of_fit_ref 0.943 _refine_ls_restrained_S_all 0.943 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.017 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 0.71572(6) 0.12203(5) 0.27561(4) 0.0886(2) Uani 1 1 d . . . S11 S 0.93614(9) 0.18866(7) 0.47082(6) 0.0762(2) Uani 1 1 d . . . S21 S 0.68262(9) 0.06467(7) 0.55941(6) 0.0759(2) Uani 1 1 d . . . S31 S 0.54890(9) 0.43586(7) 0.10529(5) 0.0705(2) Uani 1 1 d . . . S41 S 0.76810(8) 0.23223(6) 0.00247(5) 0.0670(2) Uani 1 1 d . . . O21 O 0.7844(3) 0.0850(2) 0.60708(16) 0.0762(5) Uani 1 1 d . . . O22 O 0.6475(3) -0.0394(2) 0.58032(16) 0.0770(5) Uani 1 1 d . . . O41 O 0.6898(2) 0.33939(19) -0.03852(15) 0.0723(5) Uani 1 1 d . . . O42 O 0.7751(2) 0.13151(19) -0.02736(15) 0.0718(5) Uani 1 1 d . . . N1 N 0.5791(3) 0.0511(2) 0.24016(18) 0.0708(6) Uani 1 1 d . . . N2 N 0.8467(3) -0.0298(3) 0.26421(19) 0.0768(7) Uani 1 1 d . . . N18 N 0.8412(3) 0.1723(2) 0.33868(17) 0.0689(6) Uani 1 1 d . . . N20 N 0.7234(3) 0.0859(2) 0.45652(18) 0.0728(6) Uani 1 1 d . . . N38 N 0.6119(3) 0.2751(2) 0.2311(2) 0.0745(6) Uani 1 1 d . . . N40 N 0.7198(3) 0.2160(2) 0.10245(17) 0.0683(6) Uani 1 1 d . . . C1 C 0.4401(4) 0.1053(3) 0.2349(2) 0.0712(7) Uani 1 1 d . . . H1 H 0.4031 0.1769 0.2533 0.085 Uiso 1 1 d R . . C2 C 0.3632(4) 0.0456(3) 0.2034(2) 0.0751(7) Uani 1 1 d . . . H2 H 0.2642 0.0855 0.2013 0.090 Uiso 1 1 d R . . C3 C 0.4254(4) -0.0574(3) 0.1792(2) 0.0696(7) Uani 1 1 d . . . H3 H 0.3607 -0.0862 0.1582 0.084 Uiso 1 1 d R . . C4 C 0.5718(3) -0.1057(3) 0.18712(19) 0.0673(6) Uani 1 1 d . . . H4 H 0.6059 -0.1782 0.1691 0.081 Uiso 1 1 d R . . C5 C 0.6461(4) -0.0474(3) 0.2178(2) 0.0722(7) Uani 1 1 d . . . C6 C 0.8031(4) -0.0997(3) 0.2284(2) 0.0745(7) Uani 1 1 d . . . C7 C 0.8843(4) -0.2009(3) 0.2059(2) 0.0717(7) Uani 1 1 d . . . H7 H 0.8315 -0.2355 0.1796 0.086 Uiso 1 1 d R . . C8 C 1.0280(4) -0.2276(3) 0.2248(2) 0.0722(7) Uani 1 1 d . . . H8 H 1.0750 -0.3000 0.2095 0.087 Uiso 1 1 d R . . C9 C 1.0786(4) -0.1622(3) 0.2592(2) 0.0731(7) Uani 1 1 d . . . H9 H 1.1782 -0.1952 0.2659 0.088 Uiso 1 1 d R . . C10 C 0.9863(3) -0.0615(3) 0.2807(2) 0.0694(7) Uani 1 1 d . . . H10 H 1.0386 -0.0239 0.3046 0.083 Uiso 1 1 d R . . C12 C 1.0026(4) 0.2486(3) 0.3692(2) 0.0740(7) Uani 1 1 d . . . C13 C 1.1073(3) 0.3062(3) 0.3540(2) 0.0726(7) Uani 1 1 d . . . H13 H 1.1640 0.3268 0.3874 0.087 Uiso 1 1 d R . . C14 C 1.1417(4) 0.3503(3) 0.2702(2) 0.0722(7) Uani 1 1 d . . . H14 H 1.2067 0.3966 0.2537 0.087 Uiso 1 1 d R . . C15 C 1.0784(4) 0.3378(3) 0.2033(2) 0.0772(8) Uani 1 1 d . . . H15 H 1.1086 0.3635 0.1442 0.093 Uiso 1 1 d R . . C16 C 0.9800(4) 0.2751(3) 0.2167(2) 0.0692(7) Uani 1 1 d . . . H16 H 0.9199 0.2524 0.1866 0.083 Uiso 1 1 d R . . C17 C 0.9329(4) 0.2347(4) 0.3018(4) 0.095(2) Uani 1 1 d . . . C19 C 0.8143(3) 0.1414(3) 0.4231(2) 0.0684(6) Uani 1 1 d . . . C22 C 0.5233(4) 0.1651(3) 0.5799(2) 0.0701(7) Uani 1 1 d . . . C23 C 0.3953(3) 0.1517(3) 0.5657(2) 0.0714(7) Uani 1 1 d . . . H23 H 0.3807 0.0895 0.5456 0.086 Uiso 1 1 d R . . C24 C 0.2693(4) 0.2307(3) 0.5763(2) 0.0727(7) Uani 1 1 d . . . H24 H 0.1756 0.2262 0.5707 0.087 Uiso 1 1 d R . . C25 C 0.2613(4) 0.3332(3) 0.5971(2) 0.0703(7) Uani 1 1 d . . . C26 C 0.3830(3) 0.3518(3) 0.6162(2) 0.0707(7) Uani 1 1 d . . . H26 H 0.4177 0.4148 0.6339 0.085 Uiso 1 1 d R . . C27 C 0.5183(4) 0.2685(3) 0.6015(2) 0.0753(7) Uani 1 1 d . . . H27 H 0.6119 0.2748 0.6056 0.090 Uiso 1 1 d R . . C28 C 0.1324(4) 0.4308(3) 0.6134(2) 0.0750(7) Uani 1 1 d . . . H28A H 0.0601 0.3996 0.6022 0.112 Uiso 1 1 d R . . H28B H 0.1331 0.4984 0.5740 0.112 Uiso 1 1 d R . . H28C H 0.1105 0.4472 0.6707 0.112 Uiso 1 1 d R . . C32 C 0.4799(3) 0.4595(3) 0.20852(19) 0.0666(6) Uani 1 1 d . . . C33 C 0.3842(4) 0.5560(3) 0.2342(2) 0.0729(7) Uani 1 1 d . . . H33 H 0.3528 0.6183 0.1910 0.087 Uiso 1 1 d R . . C34 C 0.3322(4) 0.5501(3) 0.3221(2) 0.0727(7) Uani 1 1 d . . . H34 H 0.2711 0.6234 0.3296 0.087 Uiso 1 1 d R . . C35 C 0.3769(3) 0.4563(3) 0.3815(2) 0.0676(6) Uani 1 1 d . . . H35 H 0.3287 0.4701 0.4368 0.081 Uiso 1 1 d R . . C36 C 0.4690(4) 0.3655(3) 0.3517(2) 0.0750(7) Uani 1 1 d . . . H36 H 0.4947 0.3061 0.3982 0.090 Uiso 1 1 d R . . C37 C 0.5228(4) 0.3602(3) 0.2689(2) 0.0718(7) Uani 1 1 d . . . C39 C 0.6408(3) 0.2934(3) 0.1487(2) 0.0667(6) Uani 1 1 d . . . C42 C 0.9560(4) 0.2459(3) -0.0081(2) 0.0733(7) Uani 1 1 d . . . C43 C 1.0558(3) 0.1426(3) 0.01482(19) 0.0668(6) Uani 1 1 d . . . H43 H 1.0243 0.0758 0.0309 0.080 Uiso 1 1 d R . . C44 C 1.1943(4) 0.1567(3) 0.0091(2) 0.0741(7) Uani 1 1 d . . . H44 H 1.2745 0.0933 0.0197 0.089 Uiso 1 1 d R . . C45 C 1.2246(4) 0.2601(3) -0.0122(2) 0.0706(7) Uani 1 1 d . . . C46 C 1.1217(3) 0.3545(3) -0.03377(19) 0.0690(7) Uani 1 1 d . . . H46 H 1.1475 0.4235 -0.0533 0.083 Uiso 1 1 d R . . C47 C 0.9798(3) 0.3495(3) -0.0308(2) 0.0673(6) Uani 1 1 d . . . H47 H 0.9061 0.4173 -0.0442 0.081 Uiso 1 1 d R . . C48 C 1.3814(4) 0.2599(3) -0.0110(2) 0.0750(7) Uani 1 1 d . . . H48A H 1.4358 0.1850 0.0065 0.112 Uiso 1 1 d R . . H48B H 1.3831 0.3068 0.0288 0.112 Uiso 1 1 d R . . H48C H 1.4222 0.2880 -0.0668 0.112 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0743(4) 0.0939(4) 0.0946(4) -0.0078(3) -0.0130(3) -0.0207(3) S11 0.0758(5) 0.0769(5) 0.0763(5) -0.0117(4) -0.0103(4) -0.0206(4) S21 0.0762(5) 0.0761(5) 0.0760(5) -0.0117(4) -0.0103(4) -0.0206(4) S31 0.0700(4) 0.0702(4) 0.0717(4) -0.0107(3) -0.0100(3) -0.0189(3) S41 0.0667(4) 0.0674(4) 0.0671(4) -0.0104(3) -0.0088(3) -0.0180(3) O21 0.0736(13) 0.0762(13) 0.0796(13) -0.0122(11) -0.0114(10) -0.0200(10) O22 0.0775(14) 0.0736(13) 0.0809(13) -0.0130(11) -0.0117(11) -0.0201(11) O41 0.0697(12) 0.0734(12) 0.0743(12) -0.0139(10) -0.0077(9) -0.0188(10) O42 0.0724(12) 0.0694(12) 0.0738(12) -0.0111(9) -0.0095(9) -0.0190(10) N1 0.0697(14) 0.0718(14) 0.0730(14) -0.0142(11) -0.0084(11) -0.0204(11) N2 0.0760(16) 0.0762(16) 0.0775(16) -0.0142(13) -0.0081(12) -0.0186(13) N18 0.0695(15) 0.0684(14) 0.0700(13) -0.0097(11) -0.0129(11) -0.0187(11) N20 0.0725(15) 0.0739(15) 0.0740(15) -0.0154(12) -0.0086(12) -0.0205(12) N38 0.0734(16) 0.0728(15) 0.0790(15) -0.0138(12) -0.0074(12) -0.0220(12) N40 0.0699(14) 0.0665(13) 0.0677(13) -0.0083(10) -0.0095(10) -0.0178(11) C1 0.0738(18) 0.0720(17) 0.0694(16) -0.0109(13) -0.0115(13) -0.0207(14) C2 0.0745(18) 0.0729(17) 0.0776(18) -0.0125(14) -0.0131(15) -0.0163(14) C3 0.0689(16) 0.0666(15) 0.0721(15) -0.0120(12) -0.0093(13) -0.0150(12) C4 0.0684(16) 0.0677(16) 0.0657(14) -0.0119(12) -0.0075(12) -0.0174(12) C5 0.0700(16) 0.0748(17) 0.0753(16) -0.0147(14) -0.0082(13) -0.0233(13) C6 0.0750(18) 0.0724(17) 0.0758(17) -0.0117(14) -0.0092(14) -0.0192(14) C7 0.0716(17) 0.0740(17) 0.0708(15) -0.0146(13) -0.0055(13) -0.0213(13) C8 0.0738(18) 0.0720(17) 0.0712(16) -0.0112(13) -0.0098(13) -0.0195(13) C9 0.0718(17) 0.0723(17) 0.0754(17) -0.0106(14) -0.0097(14) -0.0200(14) C10 0.0677(16) 0.0662(15) 0.0730(16) -0.0111(13) -0.0107(13) -0.0146(12) C12 0.0743(18) 0.0711(17) 0.0735(16) -0.0084(14) -0.0090(14) -0.0166(14) C13 0.0691(16) 0.0743(17) 0.0844(19) -0.0107(14) -0.0113(13) -0.0344(14) C14 0.0698(16) 0.0771(18) 0.0721(16) -0.0115(14) -0.0101(13) -0.0222(14) C15 0.082(2) 0.0744(18) 0.0746(17) -0.0097(14) -0.0077(14) -0.0220(15) C16 0.0672(16) 0.0688(16) 0.0714(16) -0.0093(13) -0.0082(13) -0.0192(13) C17 0.0617(19) 0.102(3) 0.150(6) -0.032(4) -0.035(3) -0.046(2) C19 0.0665(16) 0.0712(16) 0.0688(15) -0.0128(13) -0.0082(12) -0.0194(13) C22 0.0691(16) 0.0724(17) 0.0703(16) -0.0112(13) -0.0125(13) -0.0188(13) C23 0.0715(17) 0.0683(16) 0.0752(17) -0.0123(13) -0.0116(13) -0.0175(13) C24 0.0688(17) 0.0693(16) 0.0787(18) -0.0108(13) -0.0100(13) -0.0164(13) C25 0.0689(17) 0.0684(15) 0.0741(16) -0.0118(13) -0.0089(13) -0.0185(13) C26 0.0700(16) 0.0704(17) 0.0720(16) -0.0092(13) -0.0102(13) -0.0196(13) C27 0.0758(19) 0.0763(18) 0.0739(17) -0.0101(14) -0.0120(14) -0.0198(15) C28 0.0755(18) 0.0734(18) 0.0745(17) -0.0111(14) -0.0065(14) -0.0197(14) C32 0.0639(15) 0.0677(15) 0.0671(15) -0.0099(12) -0.0071(12) -0.0166(12) C33 0.0734(18) 0.0712(16) 0.0738(17) -0.0115(14) -0.0104(14) -0.0181(14) C34 0.0736(17) 0.0687(16) 0.0747(17) -0.0097(13) -0.0057(13) -0.0205(13) C35 0.0666(16) 0.0687(16) 0.0664(14) -0.0090(12) -0.0099(11) -0.0167(12) C36 0.0696(17) 0.0769(18) 0.0801(18) -0.0143(15) -0.0109(14) -0.0199(14) C37 0.0676(16) 0.0709(16) 0.0773(17) -0.0128(14) -0.0098(13) -0.0178(13) C39 0.0671(16) 0.0673(16) 0.0667(14) -0.0099(12) -0.0090(12) -0.0197(12) C42 0.0737(18) 0.0711(17) 0.0745(17) -0.0100(14) -0.0118(14) -0.0175(13) C43 0.0691(16) 0.0658(15) 0.0652(14) -0.0101(12) -0.0101(12) -0.0164(12) C44 0.0721(17) 0.0774(18) 0.0706(16) -0.0111(14) -0.0069(13) -0.0179(14) C45 0.0722(17) 0.0690(16) 0.0720(16) -0.0116(13) -0.0126(13) -0.0185(13) C46 0.0700(17) 0.0690(16) 0.0646(14) -0.0091(12) -0.0077(12) -0.0148(13) C47 0.0667(16) 0.0659(15) 0.0714(15) -0.0077(12) -0.0110(12) -0.0217(12) C48 0.0728(18) 0.0765(18) 0.0753(17) -0.0118(14) -0.0119(14) -0.0178(14) _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 2.024(3) . y Cu1 N18 2.027(3) . y Cu1 N38 1.966(3) . y Cu1 N2 1.997(3) . y Cu1 N40 2.805(3) . y Cu1 N20 2.870(3) . y S11 C19 1.816(3) . ? S11 C12 1.759(4) . ? S21 O22 1.418(2) . ? S21 O21 1.467(2) . ? S21 N20 1.621(3) . ? S21 C22 1.729(4) . ? S31 C32 1.729(3) . ? S31 C39 1.824(3) . ? S41 O42 1.427(2) . ? S41 O41 1.444(2) . ? S41 N40 1.585(3) . ? S41 C42 1.874(4) . ? N1 C1 1.345(4) . ? N1 C5 1.315(4) . ? N2 C6 1.343(4) . ? N2 C10 1.369(4) . ? N18 C17 1.348(5) . ? N18 C19 1.340(4) . ? N20 C19 1.272(4) . ? N38 C39 1.295(4) . ? N38 C37 1.347(4) . ? N40 C39 1.324(4) . ? C1 C2 1.420(4) . ? C1 H1 0.9569 . ? C2 C3 1.368(5) . ? C2 H2 0.9581 . ? C3 C4 1.405(4) . ? C3 H3 0.9532 . ? C4 C5 1.379(4) . ? C4 H4 0.9635 . ? C5 C6 1.515(5) . ? C6 C7 1.376(5) . ? C7 C8 1.424(5) . ? C7 H7 0.9601 . ? C8 C9 1.324(5) . ? C8 H8 0.9563 . ? C9 C10 1.397(5) . ? C9 H9 0.9603 . ? C10 H10 0.9599 . ? C12 C17 1.445(5) . ? C12 C13 1.384(4) . ? C13 C14 1.377(5) . ? C13 H13 0.9553 . ? C14 C15 1.390(5) . ? C14 H14 0.9558 . ? C15 C16 1.381(5) . ? C15 H15 0.9655 . ? C16 C17 1.408(7) . ? C16 H16 0.9591 . ? C22 C23 1.376(4) . ? C22 C27 1.403(5) . ? C23 C24 1.352(5) . ? C23 H23 0.9623 . ? C24 C25 1.379(4) . ? C24 H24 0.9575 . ? C25 C26 1.377(4) . ? C25 C28 1.514(5) . ? C26 C27 1.449(5) . ? C26 H26 1.0550 . ? C27 H27 0.9583 . ? C28 H28A 0.9625 . ? C28 H28B 0.9596 . ? C28 H28C 0.9589 . ? C32 C33 1.391(5) . ? C32 C37 1.433(4) . ? C33 C34 1.411(5) . ? C33 H33 0.9584 . ? C34 C35 1.384(4) . ? C34 H34 0.9634 . ? C35 C36 1.350(5) . ? C35 H35 0.9540 . ? C36 C37 1.352(5) . ? C36 H36 0.9611 . ? C42 C43 1.413(5) . ? C42 C47 1.364(4) . ? C43 C44 1.405(5) . ? C43 H43 0.9549 . ? C44 C45 1.387(5) . ? C44 H44 0.9580 . ? C45 C46 1.351(4) . ? C45 C48 1.540(4) . ? C46 C47 1.403(4) . ? C46 H46 0.9564 . ? C47 H47 0.9624 . ? C48 H48A 0.9568 . ? C48 H48B 0.9606 . ? C48 H48C 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 N1 Cu1 N18 166.37(12) . . y N1 Cu1 N38 93.83(12) . . y N18 Cu1 N38 94.19(11) . . y N1 Cu1 N2 80.31(12) . . y N18 Cu1 N2 96.98(12) . . y N38 Cu1 N2 154.03(13) . . y N1 Cu1 N40 79.57(10) . . y N18 Cu1 N40 114.05(10) . . y N38 Cu1 N40 54.55(10) . . y N2 Cu1 N40 99.48(11) . . y N1 Cu1 N20 114.06(10) . . y N18 Cu1 N20 52.47(10) . . y N38 Cu1 N20 113.34(11) . . y N2 Cu1 N20 91.95(11) . . y N40 Cu1 N20 163.69(8) . . y C19 S11 C12 90.19(16) . . ? O22 S21 O21 118.73(15) . . ? O22 S21 N20 106.49(15) . . ? O21 S21 N20 114.39(15) . . ? O22 S21 C22 105.79(15) . . ? O21 S21 C22 105.44(15) . . ? N20 S21 C22 104.80(16) . . ? C32 S31 C39 88.57(15) . . ? O42 S41 O41 120.77(14) . . ? O42 S41 N40 108.00(14) . . ? O41 S41 N40 111.15(14) . . ? O42 S41 C42 107.94(15) . . ? O41 S41 C42 103.76(14) . . ? N40 S41 C42 103.79(14) . . ? C1 N1 C5 126.2(3) . . ? C1 N1 Cu1 122.0(2) . . ? C5 N1 Cu1 111.6(2) . . ? C6 N2 C10 117.4(3) . . ? C6 N2 Cu1 118.9(2) . . ? C10 N2 Cu1 123.2(2) . . ? C17 N18 C19 124.1(3) . . ? C17 N18 Cu1 125.0(3) . . ? C19 N18 Cu1 110.8(2) . . ? C19 N20 S21 119.8(2) . . ? C19 N20 Cu1 73.89(19) . . ? S21 N20 Cu1 164.28(16) . . ? C39 N38 C37 117.0(3) . . ? C39 N38 Cu1 109.9(2) . . ? C37 N38 Cu1 133.0(3) . . ? C39 N40 S41 127.3(2) . . ? C39 N40 Cu1 71.59(17) . . ? S41 N40 Cu1 160.09(15) . . ? N1 C1 C2 114.1(3) . . ? N1 C1 H1 118.7 . . ? C2 C1 H1 127.2 . . ? C1 C2 C3 123.0(3) . . ? C1 C2 H2 112.3 . . ? C3 C2 H2 124.6 . . ? C4 C3 C2 117.8(3) . . ? C4 C3 H3 128.8 . . ? C2 C3 H3 113.3 . . ? C5 C4 C3 119.0(3) . . ? C5 C4 H4 129.1 . . ? C3 C4 H4 112.0 . . ? C4 C5 C6 119.5(3) . . ? C4 C5 N1 119.9(3) . . ? C6 C5 N1 120.6(3) . . ? N2 C6 C7 127.0(3) . . ? N2 C6 C5 107.5(3) . . ? C7 C6 C5 125.5(3) . . ? C8 C7 C6 112.2(3) . . ? C8 C7 H7 135.3 . . ? C6 C7 H7 112.5 . . ? C7 C8 C9 124.1(3) . . ? C7 C8 H8 106.5 . . ? C9 C8 H8 129.3 . . ? C8 C9 C10 119.1(3) . . ? C8 C9 H9 110.8 . . ? C10 C9 H9 130.1 . . ? N2 C10 C9 120.3(3) . . ? N2 C10 H10 130.6 . . ? C9 C10 H10 109.1 . . ? C17 C12 C13 122.6(4) . . ? C17 C12 S11 112.8(3) . . ? C13 C12 S11 124.6(3) . . ? C12 C13 C14 115.9(3) . . ? C12 C13 H13 136.7 . . ? C14 C13 H13 107.3 . . ? C13 C14 C15 123.3(3) . . ? C13 C14 H14 122.3 . . ? C15 C14 H14 114.2 . . ? C16 C15 C14 121.4(3) . . ? C16 C15 H15 115.3 . . ? C14 C15 H15 122.8 . . ? C15 C16 C17 117.7(3) . . ? C15 C16 H16 141.2 . . ? C17 C16 H16 100.8 . . ? C12 C17 N18 106.7(5) . . ? C12 C17 C16 118.6(3) . . ? N18 C17 C16 134.4(4) . . ? N20 C19 N18 122.8(3) . . ? N20 C19 S11 131.1(3) . . ? N18 C19 S11 106.0(2) . . ? C23 C22 C27 116.4(3) . . ? C23 C22 S21 120.4(3) . . ? C27 C22 S21 122.7(3) . . ? C24 C23 C22 122.5(3) . . ? C24 C23 H23 110.0 . . ? C22 C23 H23 127.4 . . ? C23 C24 C25 122.2(3) . . ? C23 C24 H24 127.5 . . ? C25 C24 H24 110.3 . . ? C26 C25 C28 110.3(3) . . ? C26 C25 C24 119.0(3) . . ? C28 C25 C24 130.4(3) . . ? C25 C26 C27 117.9(3) . . ? C25 C26 H26 140.5 . . ? C27 C26 H26 101.2 . . ? C26 C27 C22 121.3(3) . . ? C26 C27 H27 126.5 . . ? C22 C27 H27 112.2 . . ? C25 C28 H28A 97.7 . . ? C25 C28 H28B 114.4 . . ? H28A C28 H28B 109.3 . . ? C25 C28 H28C 115.9 . . ? H28A C28 H28C 109.2 . . ? H28B C28 H28C 109.5 . . ? C33 C32 C37 121.2(3) . . ? C33 C32 S31 127.5(3) . . ? C37 C32 S31 111.1(2) . . ? C34 C33 C32 116.4(3) . . ? C34 C33 H33 125.3 . . ? C32 C33 H33 118.1 . . ? C35 C34 C33 123.0(3) . . ? C35 C34 H34 130.6 . . ? C33 C34 H34 106.1 . . ? C36 C35 C34 117.2(3) . . ? C36 C35 H35 133.4 . . ? C34 C35 H35 109.3 . . ? C37 C36 C35 125.0(4) . . ? C37 C36 H36 124.6 . . ? C35 C36 H36 110.3 . . ? C36 C37 N38 130.8(3) . . ? C36 C37 C32 117.1(3) . . ? N38 C37 C32 112.1(3) . . ? N38 C39 N40 123.8(3) . . ? N38 C39 S31 111.1(2) . . ? N40 C39 S31 125.0(2) . . ? C43 C42 C47 128.2(3) . . ? C43 C42 S41 112.5(2) . . ? C47 C42 S41 119.2(3) . . ? C42 C43 C44 110.9(3) . . ? C42 C43 H43 119.8 . . ? C44 C43 H43 129.3 . . ? C43 C44 C45 123.4(3) . . ? C43 C44 H44 120.5 . . ? C45 C44 H44 116.1 . . ? C46 C45 C44 121.3(3) . . ? C46 C45 C48 122.6(3) . . ? C44 C45 C48 116.1(3) . . ? C45 C46 C47 119.7(3) . . ? C45 C46 H46 119.4 . . ? C47 C46 H46 120.8 . . ? C46 C47 C42 116.3(3) . . ? C46 C47 H47 119.5 . . ? C42 C47 H47 124.1 . . ? C45 C48 H48A 109.0 . . ? C45 C48 H48B 108.9 . . ? H48A C48 H48B 109.7 . . ? C45 C48 H48C 110.2 . . ? H48A C48 H48C 109.7 . . ? H48B C48 H48C 109.3 . . ? 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 N18 Cu1 N1 C1 97.1(5) . . . . ? N38 Cu1 N1 C1 -28.8(3) . . . . ? N2 Cu1 N1 C1 176.7(3) . . . . ? N40 Cu1 N1 C1 -81.7(2) . . . . ? N20 Cu1 N1 C1 88.9(3) . . . . ? N18 Cu1 N1 C5 -87.6(5) . . . . ? N38 Cu1 N1 C5 146.5(2) . . . . ? N2 Cu1 N1 C5 -8.0(2) . . . . ? N40 Cu1 N1 C5 93.6(2) . . . . ? N20 Cu1 N1 C5 -95.8(2) . . . . ? N1 Cu1 N2 C6 10.1(3) . . . . ? N18 Cu1 N2 C6 176.6(3) . . . . ? N38 Cu1 N2 C6 -68.6(4) . . . . ? N40 Cu1 N2 C6 -67.5(3) . . . . ? N20 Cu1 N2 C6 124.2(3) . . . . ? N1 Cu1 N2 C10 -178.8(3) . . . . ? N18 Cu1 N2 C10 -12.3(3) . . . . ? N38 Cu1 N2 C10 102.5(3) . . . . ? N40 Cu1 N2 C10 103.6(3) . . . . ? N20 Cu1 N2 C10 -64.7(3) . . . . ? N1 Cu1 N18 C17 173.9(5) . . . . ? N38 Cu1 N18 C17 -60.2(3) . . . . ? N2 Cu1 N18 C17 96.3(3) . . . . ? N40 Cu1 N18 C17 -7.4(4) . . . . ? N20 Cu1 N18 C17 -176.6(4) . . . . ? N1 Cu1 N18 C19 -10.2(6) . . . . ? N38 Cu1 N18 C19 115.7(2) . . . . ? N2 Cu1 N18 C19 -87.8(2) . . . . ? N40 Cu1 N18 C19 168.6(2) . . . . ? N20 Cu1 N18 C19 -0.7(2) . . . . ? O22 S21 N20 C19 -149.6(3) . . . . ? O21 S21 N20 C19 -16.4(3) . . . . ? C22 S21 N20 C19 98.5(3) . . . . ? O22 S21 N20 Cu1 61.7(6) . . . . ? O21 S21 N20 Cu1 -165.1(5) . . . . ? C22 S21 N20 Cu1 -50.2(6) . . . . ? N1 Cu1 N20 C19 178.3(2) . . . . ? N18 Cu1 N20 C19 0.7(2) . . . . ? N38 Cu1 N20 C19 -75.9(2) . . . . ? N2 Cu1 N20 C19 98.0(2) . . . . ? N40 Cu1 N20 C19 -36.7(4) . . . . ? N1 Cu1 N20 S21 -29.7(6) . . . . ? N18 Cu1 N20 S21 152.7(6) . . . . ? N38 Cu1 N20 S21 76.1(6) . . . . ? N2 Cu1 N20 S21 -110.0(6) . . . . ? N40 Cu1 N20 S21 115.3(6) . . . . ? N1 Cu1 N38 C39 -76.7(2) . . . . ? N18 Cu1 N38 C39 114.3(2) . . . . ? N2 Cu1 N38 C39 -1.0(4) . . . . ? N40 Cu1 N38 C39 -2.37(19) . . . . ? N20 Cu1 N38 C39 165.0(2) . . . . ? N1 Cu1 N38 C37 104.4(3) . . . . ? N18 Cu1 N38 C37 -64.6(3) . . . . ? N2 Cu1 N38 C37 -179.9(3) . . . . ? N40 Cu1 N38 C37 178.7(4) . . . . ? N20 Cu1 N38 C37 -13.9(3) . . . . ? O42 S41 N40 C39 -147.2(3) . . . . ? O41 S41 N40 C39 -12.6(3) . . . . ? C42 S41 N40 C39 98.4(3) . . . . ? O42 S41 N40 Cu1 53.5(4) . . . . ? O41 S41 N40 Cu1 -171.9(4) . . . . ? C42 S41 N40 Cu1 -61.0(4) . . . . ? N1 Cu1 N40 C39 104.68(19) . . . . ? N18 Cu1 N40 C39 -75.0(2) . . . . ? N38 Cu1 N40 C39 2.30(18) . . . . ? N2 Cu1 N40 C39 -177.11(19) . . . . ? N20 Cu1 N40 C39 -43.2(4) . . . . ? N1 Cu1 N40 S41 -92.6(4) . . . . ? N18 Cu1 N40 S41 87.8(4) . . . . ? N38 Cu1 N40 S41 165.1(5) . . . . ? N2 Cu1 N40 S41 -14.3(4) . . . . ? N20 Cu1 N40 S41 119.6(4) . . . . ? C5 N1 C1 C2 1.3(5) . . . . ? Cu1 N1 C1 C2 175.9(2) . . . . ? N1 C1 C2 C3 -1.0(5) . . . . ? C1 C2 C3 C4 0.7(5) . . . . ? C2 C3 C4 C5 -0.7(5) . . . . ? C3 C4 C5 C6 178.7(3) . . . . ? C3 C4 C5 N1 0.9(5) . . . . ? C1 N1 C5 C4 -1.3(5) . . . . ? Cu1 N1 C5 C4 -176.4(2) . . . . ? C1 N1 C5 C6 -179.1(3) . . . . ? Cu1 N1 C5 C6 5.9(4) . . . . ? C10 N2 C6 C7 -0.2(5) . . . . ? Cu1 N2 C6 C7 171.4(3) . . . . ? C10 N2 C6 C5 179.2(3) . . . . ? Cu1 N2 C6 C5 -9.1(4) . . . . ? C4 C5 C6 N2 -176.0(3) . . . . ? N1 C5 C6 N2 1.8(4) . . . . ? C4 C5 C6 C7 3.5(5) . . . . ? N1 C5 C6 C7 -178.8(3) . . . . ? N2 C6 C7 C8 0.0(5) . . . . ? C5 C6 C7 C8 -179.3(3) . . . . ? C6 C7 C8 C9 -0.7(5) . . . . ? C7 C8 C9 C10 1.5(5) . . . . ? C6 N2 C10 C9 1.0(5) . . . . ? Cu1 N2 C10 C9 -170.2(2) . . . . ? C8 C9 C10 N2 -1.7(5) . . . . ? C19 S11 C12 C17 0.9(3) . . . . ? C19 S11 C12 C13 179.1(3) . . . . ? C17 C12 C13 C14 0.1(5) . . . . ? S11 C12 C13 C14 -177.9(3) . . . . ? C12 C13 C14 C15 -0.8(5) . . . . ? C13 C14 C15 C16 -3.0(6) . . . . ? C14 C15 C16 C17 7.3(6) . . . . ? C13 C12 C17 N18 178.2(3) . . . . ? S11 C12 C17 N18 -3.6(4) . . . . ? C13 C12 C17 C16 4.2(6) . . . . ? S11 C12 C17 C16 -177.5(3) . . . . ? C19 N18 C17 C12 6.0(5) . . . . ? Cu1 N18 C17 C12 -178.6(2) . . . . ? C19 N18 C17 C16 178.6(4) . . . . ? Cu1 N18 C17 C16 -6.0(7) . . . . ? C15 C16 C17 C12 -7.7(6) . . . . ? C15 C16 C17 N18 -179.6(5) . . . . ? S21 N20 C19 N18 -172.6(3) . . . . ? Cu1 N20 C19 N18 -1.0(3) . . . . ? S21 N20 C19 S11 10.9(5) . . . . ? Cu1 N20 C19 S11 -177.5(3) . . . . ? C17 N18 C19 N20 177.4(4) . . . . ? Cu1 N18 C19 N20 1.4(4) . . . . ? C17 N18 C19 S11 -5.3(4) . . . . ? Cu1 N18 C19 S11 178.70(13) . . . . ? C12 S11 C19 N20 179.0(3) . . . . ? C12 S11 C19 N18 2.0(3) . . . . ? O22 S21 C22 C23 -34.8(3) . . . . ? O21 S21 C22 C23 -161.4(3) . . . . ? N20 S21 C22 C23 77.6(3) . . . . ? O22 S21 C22 C27 152.9(3) . . . . ? O21 S21 C22 C27 26.3(3) . . . . ? N20 S21 C22 C27 -94.8(3) . . . . ? C27 C22 C23 C24 -3.5(5) . . . . ? S21 C22 C23 C24 -176.3(3) . . . . ? C22 C23 C24 C25 4.0(5) . . . . ? C23 C24 C25 C26 -6.7(5) . . . . ? C23 C24 C25 C28 -178.5(3) . . . . ? C28 C25 C26 C27 -177.8(3) . . . . ? C24 C25 C26 C27 8.8(5) . . . . ? C25 C26 C27 C22 -8.7(5) . . . . ? C23 C22 C27 C26 5.9(5) . . . . ? S21 C22 C27 C26 178.5(3) . . . . ? C39 S31 C32 C33 -176.8(3) . . . . ? C39 S31 C32 C37 -2.6(2) . . . . ? C37 C32 C33 C34 -0.2(5) . . . . ? S31 C32 C33 C34 173.4(2) . . . . ? C32 C33 C34 C35 2.8(5) . . . . ? C33 C34 C35 C36 -3.5(5) . . . . ? C34 C35 C36 C37 1.4(5) . . . . ? C35 C36 C37 N38 -178.4(3) . . . . ? C35 C36 C37 C32 1.0(5) . . . . ? C39 N38 C37 C36 177.2(3) . . . . ? Cu1 N38 C37 C36 -4.0(6) . . . . ? C39 N38 C37 C32 -2.3(4) . . . . ? Cu1 N38 C37 C32 176.6(2) . . . . ? C33 C32 C37 C36 -1.6(5) . . . . ? S31 C32 C37 C36 -176.2(2) . . . . ? C33 C32 C37 N38 177.9(3) . . . . ? S31 C32 C37 N38 3.3(4) . . . . ? C37 N38 C39 N40 -176.0(3) . . . . ? Cu1 N38 C39 N40 4.9(4) . . . . ? C37 N38 C39 S31 0.2(4) . . . . ? Cu1 N38 C39 S31 -178.88(13) . . . . ? S41 N40 C39 N38 -176.1(2) . . . . ? Cu1 N40 C39 N38 -3.4(3) . . . . ? S41 N40 C39 S31 8.2(4) . . . . ? Cu1 N40 C39 S31 -179.1(3) . . . . ? C32 S31 C39 N38 1.5(2) . . . . ? C32 S31 C39 N40 177.6(3) . . . . ? O42 S41 C42 C43 -40.2(3) . . . . ? O41 S41 C42 C43 -169.5(2) . . . . ? N40 S41 C42 C43 74.3(3) . . . . ? O42 S41 C42 C47 143.6(3) . . . . ? O41 S41 C42 C47 14.3(3) . . . . ? N40 S41 C42 C47 -102.0(3) . . . . ? C47 C42 C43 C44 -2.1(5) . . . . ? S41 C42 C43 C44 -177.9(2) . . . . ? C42 C43 C44 C45 3.0(4) . . . . ? C43 C44 C45 C46 -3.8(5) . . . . ? C43 C44 C45 C48 177.1(3) . . . . ? C44 C45 C46 C47 3.1(5) . . . . ? C48 C45 C46 C47 -177.8(3) . . . . ? C45 C46 C47 C42 -2.0(5) . . . . ? C43 C42 C47 C46 1.6(5) . . . . ? S41 C42 C47 C46 177.2(2) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 89.85 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.199 _refine_diff_density_min -0.604 _refine_diff_density_rms 0.032 _database_code_depnum_ccdc_archive 'CCDC 923556' ####################################################################### # # 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_09acmg20 #TrackingRef 'alzuet_dalton.ccd' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C42 H38 Cu N6 O4 S4), 0.5(H2 O)' _chemical_formula_sum 'C42 H39 Cu N6 O4.50 S4' _chemical_formula_weight 891.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 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 23.1710(4) _cell_length_b 11.9410(3) _cell_length_c 32.0110(7) _cell_angle_alpha 90.00 _cell_angle_beta 106.5270(10) _cell_angle_gamma 90.00 _cell_volume 8491.0(3) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 6238 _cell_measurement_theta_min 0.999 _cell_measurement_theta_max 60.02 _exptl_crystal_description prism _exptl_crystal_colour Green _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.395 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3696 _exptl_absorpt_coefficient_mu 2.973 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD2000 _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 19419 _diffrn_reflns_av_R_equivalents 0.0738 _diffrn_reflns_av_sigmaI/netI 0.1150 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 89.89 _reflns_number_total 19419 _reflns_number_gt 19235 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo & Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2009)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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. The low accuracy of the structure refinement derives from the weak diffracting power on the crystals. Nevertheless, the final results can be considered satisfactory from the chemical point of view. The large discrepancy between the R and wR values is due to the high thermal vibration present in phenyl rings. The large thermal oscillations or positional disorder indicated by larger-than normal mean-square displacement parameters of other atoms also contribute to the relatively high R factors. ; _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^)+(0.0818P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 19419 _refine_ls_number_parameters 1048 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1380 _refine_ls_R_factor_gt 0.0559 _refine_ls_wR_factor_ref 0.1604 _refine_ls_wR_factor_gt 0.1219 _refine_ls_goodness_of_fit_ref 0.961 _refine_ls_restrained_S_all 0.961 _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 0.15003(5) 0.48353(11) 0.16192(4) 0.0665(5) Uani 1 1 d . . . S11 S -0.01872(11) 0.5837(2) 0.19920(9) 0.0877(9) Uani 1 1 d . . . S21 S 0.01336(12) 0.4502(3) 0.09015(10) 0.0759(9) Uani 1 1 d . . . S31 S 0.23603(14) 0.2363(3) 0.26678(11) 0.1143(12) Uani 1 1 d . . . S41 S 0.32243(14) 0.4528(4) 0.27618(12) 0.1051(11) Uani 1 1 d . . . O21 O 0.0794(2) 0.4480(5) 0.10052(18) 0.0755(19) Uani 1 1 d . . . O22 O -0.0179(2) 0.3530(6) 0.0696(2) 0.092(2) Uani 1 1 d . . . O41 O 0.3185(3) 0.4010(7) 0.3162(3) 0.117(3) Uani 1 1 d . . . O42 O 0.3430(3) 0.5675(8) 0.2784(3) 0.133(3) Uani 1 1 d . . . N1 N 0.2041(3) 0.4362(10) 0.1266(3) 0.063(2) Uani 1 1 d . . . N2 N 0.1682(4) 0.6330(8) 0.1393(3) 0.068(2) Uani 1 1 d . . . N18 N 0.0834(4) 0.5375(6) 0.1849(3) 0.060(2) Uani 1 1 d . . . N20 N -0.0082(3) 0.4754(7) 0.1318(3) 0.072(3) Uani 1 1 d . . . N38 N 0.1719(5) 0.3541(8) 0.2021(3) 0.069(3) Uani 1 1 d . . . N40 N 0.2588(4) 0.4449(8) 0.2390(3) 0.080(3) Uani 1 1 d . . . C1 C 0.2201(4) 0.3308(11) 0.1214(4) 0.079(3) Uani 1 1 d . . . H1 H 0.2133 0.2754 0.1399 0.095 Uiso 1 1 calc R . . C2 C 0.2470(5) 0.3018(10) 0.0888(5) 0.090(4) Uani 1 1 d . . . H2 H 0.2582 0.2283 0.0854 0.108 Uiso 1 1 calc R . . C3 C 0.2563(5) 0.3860(16) 0.0618(4) 0.098(4) Uani 1 1 d . . . H3 H 0.2737 0.3695 0.0397 0.118 Uiso 1 1 calc R . . C4 C 0.2401(5) 0.4920(12) 0.0677(5) 0.096(4) Uani 1 1 d . . . H4 H 0.2469 0.5493 0.0499 0.115 Uiso 1 1 calc R . . C5 C 0.2135(4) 0.5147(12) 0.0999(4) 0.063(3) Uani 1 1 d . . . C6 C 0.1945(5) 0.6304(11) 0.1071(4) 0.067(3) Uani 1 1 d . . . C7 C 0.2016(4) 0.7230(15) 0.0843(4) 0.094(4) Uani 1 1 d . . . H7 H 0.2200 0.7176 0.0621 0.113 Uiso 1 1 calc R . . C8 C 0.1811(6) 0.8249(11) 0.0947(5) 0.110(4) Uani 1 1 d . . . H8 H 0.1842 0.8889 0.0789 0.131 Uiso 1 1 calc R . . C9 C 0.1559(5) 0.8306(11) 0.1289(5) 0.090(4) Uani 1 1 d . . . H9 H 0.1432 0.8984 0.1376 0.108 Uiso 1 1 calc R . . C10 C 0.1503(4) 0.7329(13) 0.1494(3) 0.080(3) Uani 1 1 d . . . H10 H 0.1327 0.7362 0.1721 0.096 Uiso 1 1 calc R . . C12 C 0.0462(5) 0.6254(9) 0.2373(4) 0.071(3) Uani 1 1 d . . . C13 C 0.0513(6) 0.6857(10) 0.2752(5) 0.087(4) Uani 1 1 d . . . H13 H 0.0167 0.7078 0.2823 0.105 Uiso 1 1 calc R . . C14 C 0.1072(8) 0.7131(9) 0.3025(4) 0.078(3) Uani 1 1 d . . . C15 C 0.1594(5) 0.6808(9) 0.2903(4) 0.073(3) Uani 1 1 d . . . C16 C 0.1528(5) 0.6224(9) 0.2515(5) 0.069(3) Uani 1 1 d . . . H16 H 0.1868 0.6013 0.2435 0.083 Uiso 1 1 calc R . . C17 C 0.0957(6) 0.5950(8) 0.2245(4) 0.061(3) Uani 1 1 d . . . C19 C 0.0239(6) 0.5246(8) 0.1671(4) 0.061(3) Uani 1 1 d . . . C22 C -0.0097(6) 0.5678(12) 0.0561(4) 0.073(4) Uani 1 1 d . . . C23 C -0.0595(7) 0.5570(11) 0.0228(5) 0.095(4) Uani 1 1 d . . . H23 H -0.0803 0.4894 0.0183 0.115 Uiso 1 1 calc R . . C24 C -0.0803(5) 0.645(2) -0.0050(5) 0.115(5) Uani 1 1 d . . . H24 H -0.1153 0.6376 -0.0278 0.138 Uiso 1 1 calc R . . C25 C -0.0494(8) 0.7454(15) 0.0010(5) 0.095(4) Uani 1 1 d . . . C26 C -0.0004(7) 0.7548(12) 0.0354(6) 0.139(6) Uani 1 1 d . . . H26 H 0.0205 0.8223 0.0405 0.167 Uiso 1 1 calc R . . C27 C 0.0195(5) 0.6665(15) 0.0633(5) 0.130(5) Uani 1 1 d . . . H27 H 0.0531 0.6750 0.0873 0.156 Uiso 1 1 calc R . . C28 C 0.1144(4) 0.7791(9) 0.3439(4) 0.118(4) Uani 1 1 d . . . H28A H 0.1393 0.8433 0.3438 0.177 Uiso 1 1 calc R . . H28B H 0.1330 0.7327 0.3685 0.177 Uiso 1 1 calc R . . H28C H 0.0756 0.8031 0.3456 0.177 Uiso 1 1 calc R . . C29 C 0.2218(5) 0.7051(8) 0.3191(3) 0.108(4) Uani 1 1 d . . . H29A H 0.2265 0.6733 0.3474 0.162 Uiso 1 1 calc R . . H29B H 0.2277 0.7847 0.3217 0.162 Uiso 1 1 calc R . . H29C H 0.2509 0.6728 0.3065 0.162 Uiso 1 1 calc R . . C30 C -0.0686(5) 0.8464(11) -0.0304(4) 0.150(5) Uani 1 1 d . . . H30A H -0.1044 0.8275 -0.0530 0.225 Uiso 1 1 calc R . . H30B H -0.0369 0.8642 -0.0431 0.225 Uiso 1 1 calc R . . H30C H -0.0765 0.9100 -0.0144 0.225 Uiso 1 1 calc R . . C32 C 0.1711(5) 0.1778(14) 0.2335(4) 0.095(4) Uani 1 1 d . . . C33 C 0.1453(8) 0.0728(14) 0.2355(5) 0.111(5) Uani 1 1 d . . . H33 H 0.1633 0.0231 0.2578 0.133 Uiso 1 1 calc R . . C34 C 0.0923(8) 0.0429(12) 0.2038(6) 0.101(4) Uani 1 1 d . . . C35 C 0.0663(6) 0.1189(16) 0.1709(5) 0.094(4) Uani 1 1 d . . . C36 C 0.0913(7) 0.2211(12) 0.1702(4) 0.081(4) Uani 1 1 d . . . H36 H 0.0732 0.2714 0.1482 0.097 Uiso 1 1 calc R . . C37 C 0.1434(7) 0.2518(12) 0.2016(5) 0.076(3) Uani 1 1 d . . . C39 C 0.2226(6) 0.3549(10) 0.2338(4) 0.079(3) Uani 1 1 d . . . C42 C 0.3724(6) 0.3696(14) 0.2578(6) 0.144(7) Uani 1 1 d . . . C43 C 0.4145(13) 0.317(3) 0.2840(6) 0.60(4) Uani 1 1 d . . . H43 H 0.4178 0.3196 0.3136 0.717 Uiso 1 1 calc R . . C44 C 0.4570(14) 0.255(4) 0.2693(8) 0.71(5) Uani 1 1 d . . . H44 H 0.4888 0.2218 0.2902 0.846 Uiso 1 1 calc R . . C45 C 0.4544(10) 0.242(2) 0.2305(8) 0.266(14) Uani 1 1 d . . . C46 C 0.4106(10) 0.2869(15) 0.2047(5) 0.146(5) Uani 1 1 d . . . H46 H 0.4055 0.2785 0.1750 0.175 Uiso 1 1 calc R . . C47 C 0.3684(6) 0.3495(13) 0.2180(7) 0.130(5) Uani 1 1 d . . . H47 H 0.3357 0.3784 0.1967 0.156 Uiso 1 1 calc R . . C48 C 0.0668(5) -0.0746(10) 0.2086(4) 0.140(5) Uani 1 1 d . . . H48A H 0.0975 -0.1191 0.2280 0.210 Uiso 1 1 calc R . . H48B H 0.0541 -0.1102 0.1806 0.210 Uiso 1 1 calc R . . H48C H 0.0331 -0.0675 0.2202 0.210 Uiso 1 1 calc R . . C49 C 0.0103(5) 0.0841(9) 0.1364(4) 0.119(4) Uani 1 1 d . . . H49A H -0.0197 0.0607 0.1500 0.178 Uiso 1 1 calc R . . H49B H 0.0195 0.0231 0.1199 0.178 Uiso 1 1 calc R . . H49C H -0.0047 0.1462 0.1174 0.178 Uiso 1 1 calc R . . C50 C 0.4996(8) 0.1655(17) 0.2157(6) 0.352(16) Uani 1 1 d . . . H50A H 0.5116 0.1043 0.2358 0.528 Uiso 1 1 calc R . . H50B H 0.5344 0.2084 0.2152 0.528 Uiso 1 1 calc R . . H50C H 0.4806 0.1367 0.1871 0.528 Uiso 1 1 calc R . . Cu2 Cu 0.38495(6) 0.76720(12) 0.02448(5) 0.0817(6) Uani 1 1 d . . . S61 S 0.18727(11) 0.7992(2) -0.03310(9) 0.0778(9) Uani 1 1 d . . . S71 S 0.24645(19) 1.0362(3) 0.00336(13) 0.1147(12) Uani 1 1 d . . . S81 S 0.38300(12) 0.5581(3) 0.13742(11) 0.1045(10) Uani 1 1 d . . . S91 S 0.43633(13) 0.4319(3) 0.06527(13) 0.0988(10) Uani 1 1 d . . . O71 O 0.2007(4) 1.0204(6) 0.0259(3) 0.146(3) Uani 1 1 d . . . O72 O 0.2877(4) 1.1281(6) 0.0179(2) 0.151(3) Uani 1 1 d . . . O91 O 0.4339(3) 0.3867(6) 0.0230(3) 0.122(3) Uani 1 1 d . . . O92 O 0.4098(3) 0.3670(6) 0.0936(3) 0.112(3) Uani 1 1 d . . . N3 N 0.4717(4) 0.8056(8) 0.0478(5) 0.091(3) Uani 1 1 d . . . N4 N 0.4026(7) 0.8066(7) -0.0321(5) 0.090(4) Uani 1 1 d . . . N68 N 0.2996(3) 0.7403(8) -0.0051(2) 0.065(2) Uani 1 1 d . . . N70 N 0.2881(3) 0.9288(9) 0.0058(3) 0.092(3) Uani 1 1 d . . . N88 N 0.3768(4) 0.7180(10) 0.0815(3) 0.079(3) Uani 1 1 d . . . N90 N 0.4095(4) 0.5562(9) 0.0579(3) 0.089(3) Uani 1 1 d . . . C51 C 0.5037(7) 0.8006(11) 0.0893(6) 0.142(6) Uani 1 1 d . . . H51 H 0.4835 0.7857 0.1100 0.171 Uiso 1 1 calc R . . C52 C 0.5654(8) 0.8164(14) 0.1037(6) 0.166(7) Uani 1 1 d . . . H52 H 0.5864 0.8110 0.1330 0.199 Uiso 1 1 calc R . . C53 C 0.5937(7) 0.8396(13) 0.0738(8) 0.139(7) Uani 1 1 d . . . H53 H 0.6349 0.8535 0.0824 0.167 Uiso 1 1 calc R . . C54 C 0.5623(9) 0.8431(11) 0.0300(7) 0.131(5) Uani 1 1 d . . . H54 H 0.5830 0.8549 0.0095 0.157 Uiso 1 1 calc R . . C55 C 0.4988(7) 0.8289(8) 0.0160(7) 0.089(4) Uani 1 1 d . . . C56 C 0.4588(10) 0.8287(10) -0.0279(6) 0.089(4) Uani 1 1 d . . . C57 C 0.4820(8) 0.8632(11) -0.0622(8) 0.121(5) Uani 1 1 d . . . H57 H 0.5223 0.8820 -0.0578 0.145 Uiso 1 1 calc R . . C58 C 0.4404(11) 0.8667(12) -0.1024(7) 0.141(6) Uani 1 1 d . . . H58 H 0.4528 0.8877 -0.1264 0.169 Uiso 1 1 calc R . . C59 C 0.3820(10) 0.8407(12) -0.1082(5) 0.134(6) Uani 1 1 d . . . H59 H 0.3544 0.8445 -0.1356 0.160 Uiso 1 1 calc R . . C60 C 0.3642(6) 0.8086(11) -0.0724(8) 0.115(5) Uani 1 1 d . . . H60 H 0.3244 0.7875 -0.0763 0.138 Uiso 1 1 calc R . . C62 C 0.2062(6) 0.6624(8) -0.0418(3) 0.060(3) Uani 1 1 d . . . C63 C 0.1702(4) 0.5785(11) -0.0637(3) 0.070(3) Uani 1 1 d . . . H63 H 0.1292 0.5916 -0.0756 0.084 Uiso 1 1 calc R . . C64 C 0.1936(5) 0.4735(10) -0.0684(3) 0.066(3) Uani 1 1 d . . . C65 C 0.2556(6) 0.4557(9) -0.0499(4) 0.067(3) Uani 1 1 d . . . C66 C 0.2920(4) 0.5398(11) -0.0276(3) 0.071(3) Uani 1 1 d . . . H66 H 0.3328 0.5264 -0.0147 0.085 Uiso 1 1 calc R . . C67 C 0.2680(5) 0.6442(11) -0.0243(3) 0.060(3) Uani 1 1 d . . . C69 C 0.2637(5) 0.8274(12) -0.0080(3) 0.075(3) Uani 1 1 d . . . C72 C 0.2078(9) 1.0606(8) -0.0525(4) 0.076(3) Uani 1 1 d . . . C73 C 0.1469(9) 1.0844(9) -0.0661(7) 0.100(5) Uani 1 1 d . . . H73 H 0.1249 1.0847 -0.0458 0.121 Uiso 1 1 calc R . . C74 C 0.1188(6) 1.1073(9) -0.1084(7) 0.098(4) Uani 1 1 d . . . H74 H 0.0786 1.1290 -0.1161 0.118 Uiso 1 1 calc R . . C75 C 0.1474(8) 1.0998(9) -0.1406(6) 0.087(4) Uani 1 1 d . . . C76 C 0.2075(9) 1.0722(10) -0.1270(6) 0.099(4) Uani 1 1 d . . . H76 H 0.2283 1.0661 -0.1479 0.119 Uiso 1 1 calc R . . C77 C 0.2381(5) 1.0534(8) -0.0843(7) 0.085(4) Uani 1 1 d . . . H77 H 0.2789 1.0360 -0.0765 0.102 Uiso 1 1 calc R . . C78 C 0.1539(4) 0.3815(8) -0.0936(3) 0.101(4) Uani 1 1 d . . . H78A H 0.1682 0.3590 -0.1176 0.151 Uiso 1 1 calc R . . H78B H 0.1133 0.4085 -0.1043 0.151 Uiso 1 1 calc R . . H78C H 0.1549 0.3186 -0.0747 0.151 Uiso 1 1 calc R . . C79 C 0.2818(4) 0.3433(8) -0.0525(3) 0.089(3) Uani 1 1 d . . . H79A H 0.2760 0.3237 -0.0825 0.133 Uiso 1 1 calc R . . H79B H 0.2624 0.2890 -0.0390 0.133 Uiso 1 1 calc R . . H79C H 0.3241 0.3448 -0.0377 0.133 Uiso 1 1 calc R . . C80 C 0.1160(5) 1.1240(10) -0.1872(4) 0.125(5) Uani 1 1 d . . . H80A H 0.1399 1.0967 -0.2051 0.188 Uiso 1 1 calc R . . H80B H 0.1105 1.2033 -0.1912 0.188 Uiso 1 1 calc R . . H80C H 0.0775 1.0875 -0.1953 0.188 Uiso 1 1 calc R . . C82 C 0.3576(5) 0.6903(11) 0.1488(6) 0.094(4) Uani 1 1 d . . . C83 C 0.3380(6) 0.7208(16) 0.1844(5) 0.114(4) Uani 1 1 d . . . H83 H 0.3374 0.6687 0.2059 0.137 Uiso 1 1 calc R . . C84 C 0.3196(6) 0.8297(18) 0.1874(6) 0.111(5) Uani 1 1 d . . . C85 C 0.3197(6) 0.9043(14) 0.1539(7) 0.110(4) Uani 1 1 d . . . C86 C 0.3395(5) 0.8732(14) 0.1187(4) 0.094(4) Uani 1 1 d . . . H86 H 0.3406 0.9251 0.0973 0.113 Uiso 1 1 calc R . . C87 C 0.3576(4) 0.7630(15) 0.1159(5) 0.076(3) Uani 1 1 d . . . C89 C 0.3913(4) 0.6105(14) 0.0886(4) 0.082(4) Uani 1 1 d . . . C92 C 0.5133(5) 0.4496(9) 0.0936(5) 0.077(3) Uani 1 1 d . . . C93 C 0.5545(9) 0.4866(10) 0.0738(4) 0.117(5) Uani 1 1 d . . . H93 H 0.5430 0.5000 0.0439 0.140 Uiso 1 1 calc R . . C94 C 0.6135(7) 0.5044(11) 0.0981(8) 0.137(6) Uani 1 1 d . . . H94 H 0.6401 0.5324 0.0837 0.164 Uiso 1 1 calc R . . C95 C 0.6348(7) 0.4843(11) 0.1403(6) 0.104(5) Uani 1 1 d . . . C96 C 0.5941(9) 0.4477(13) 0.1600(5) 0.158(6) Uani 1 1 d . . . H96 H 0.6066 0.4337 0.1898 0.189 Uiso 1 1 calc R . . C97 C 0.5329(7) 0.4297(11) 0.1369(6) 0.125(5) Uani 1 1 d . . . H97 H 0.5062 0.4041 0.1516 0.150 Uiso 1 1 calc R . . C98 C 0.2956(5) 0.8665(12) 0.2256(4) 0.159(6) Uani 1 1 d . . . H98A H 0.2948 0.8033 0.2440 0.238 Uiso 1 1 calc R . . H98B H 0.2556 0.8958 0.2144 0.238 Uiso 1 1 calc R . . H98C H 0.3214 0.9234 0.2423 0.238 Uiso 1 1 calc R . . C99 C 0.3004(6) 1.0245(11) 0.1567(4) 0.150(5) Uani 1 1 d . . . H99A H 0.3097 1.0678 0.1342 0.225 Uiso 1 1 calc R . . H99B H 0.3216 1.0549 0.1847 0.225 Uiso 1 1 calc R . . H99C H 0.2579 1.0271 0.1532 0.225 Uiso 1 1 calc R . . C100 C 0.7009(5) 0.5065(9) 0.1629(4) 0.145(5) Uani 1 1 d . . . H10A H 0.7244 0.4890 0.1434 0.217 Uiso 1 1 calc R . . H10B H 0.7138 0.4604 0.1885 0.217 Uiso 1 1 calc R . . H10C H 0.7063 0.5839 0.1711 0.217 Uiso 1 1 calc R . . O1 O 0.3939(3) 0.1289(7) 0.0843(4) 0.225(5) Uani 1 1 d . . . H1A H 0.3504 0.1280 0.0741 0.338 Uiso 1 1 d R . . H1B H 0.4034 0.1958 0.0799 0.338 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0660(8) 0.0696(10) 0.0707(11) 0.0069(8) 0.0304(7) 0.0059(7) S11 0.0734(18) 0.114(2) 0.085(2) -0.0035(19) 0.0383(18) 0.0094(16) S21 0.068(2) 0.086(2) 0.073(3) -0.009(2) 0.0197(17) -0.0005(17) S31 0.113(2) 0.117(3) 0.110(3) 0.047(2) 0.028(2) 0.031(2) S41 0.080(2) 0.148(4) 0.086(3) 0.007(3) 0.022(2) 0.024(2) O21 0.047(4) 0.099(5) 0.078(5) 0.002(4) 0.014(3) 0.008(3) O22 0.082(4) 0.091(6) 0.107(6) -0.018(5) 0.032(4) -0.008(4) O41 0.091(5) 0.185(8) 0.075(6) 0.035(6) 0.025(4) 0.039(5) O42 0.107(6) 0.164(9) 0.116(7) -0.003(7) 0.014(5) -0.008(6) N1 0.060(5) 0.077(7) 0.062(7) 0.002(6) 0.033(5) 0.009(5) N2 0.071(6) 0.051(7) 0.081(8) 0.003(6) 0.023(5) 0.008(5) N18 0.060(6) 0.060(6) 0.072(8) -0.005(5) 0.036(5) 0.005(5) N20 0.070(6) 0.100(7) 0.046(7) -0.009(6) 0.019(5) -0.006(5) N38 0.074(6) 0.070(7) 0.065(8) 0.023(6) 0.023(5) 0.020(6) N40 0.066(6) 0.099(8) 0.070(7) 0.020(6) 0.012(5) 0.022(5) C1 0.084(8) 0.076(11) 0.082(11) 0.001(8) 0.031(7) 0.014(7) C2 0.088(8) 0.102(11) 0.081(11) -0.019(10) 0.027(7) 0.040(7) C3 0.098(8) 0.143(14) 0.071(11) 0.025(11) 0.053(7) -0.006(10) C4 0.103(9) 0.073(11) 0.123(14) 0.010(9) 0.050(9) -0.001(8) C5 0.049(6) 0.108(13) 0.042(9) 0.001(9) 0.029(6) 0.003(7) C6 0.061(7) 0.084(12) 0.060(10) 0.007(9) 0.025(7) 0.000(7) C7 0.114(9) 0.098(11) 0.095(11) 0.027(10) 0.067(8) -0.014(9) C8 0.142(11) 0.063(11) 0.112(14) 0.017(10) 0.017(10) -0.009(9) C9 0.127(9) 0.074(11) 0.086(11) -0.001(9) 0.058(8) 0.006(7) C10 0.093(8) 0.074(9) 0.077(10) 0.036(9) 0.031(6) -0.012(8) C12 0.089(10) 0.060(8) 0.081(11) 0.010(7) 0.048(9) 0.014(7) C13 0.091(11) 0.081(9) 0.102(13) 0.011(9) 0.047(10) 0.012(8) C14 0.116(11) 0.066(8) 0.062(11) 0.003(7) 0.042(10) 0.003(8) C15 0.091(10) 0.072(8) 0.059(11) -0.001(7) 0.024(9) -0.007(7) C16 0.082(10) 0.068(8) 0.062(10) 0.011(7) 0.027(8) 0.016(6) C17 0.080(9) 0.050(7) 0.056(10) 0.001(7) 0.026(10) 0.011(7) C19 0.080(9) 0.067(8) 0.053(10) 0.011(7) 0.045(7) 0.011(6) C22 0.043(7) 0.121(13) 0.043(9) 0.004(8) -0.004(6) 0.015(8) C23 0.098(12) 0.122(12) 0.078(12) 0.035(10) 0.044(10) 0.010(9) C24 0.064(9) 0.193(18) 0.086(13) 0.000(14) 0.018(8) -0.007(12) C25 0.083(10) 0.149(16) 0.060(12) 0.021(11) 0.031(9) 0.046(10) C26 0.138(13) 0.090(12) 0.154(15) 0.039(11) -0.016(12) -0.002(10) C27 0.097(10) 0.108(12) 0.149(15) 0.007(12) -0.023(9) -0.039(11) C28 0.150(10) 0.127(11) 0.080(10) -0.037(9) 0.039(8) -0.007(8) C29 0.113(9) 0.107(10) 0.097(10) -0.008(8) 0.019(8) -0.003(7) C30 0.179(12) 0.161(13) 0.122(12) 0.050(11) 0.062(9) 0.079(10) C32 0.112(11) 0.080(11) 0.108(12) 0.051(10) 0.057(9) 0.030(10) C33 0.140(13) 0.089(13) 0.129(15) 0.062(11) 0.081(12) 0.047(10) C34 0.123(12) 0.092(13) 0.118(15) 0.009(12) 0.083(11) 0.012(11) C35 0.109(11) 0.092(13) 0.097(13) 0.024(11) 0.054(10) 0.024(11) C36 0.100(11) 0.049(10) 0.115(13) 0.032(8) 0.066(11) 0.006(7) C37 0.081(10) 0.068(12) 0.090(12) -0.002(11) 0.041(9) 0.013(10) C39 0.093(10) 0.084(10) 0.072(10) 0.021(9) 0.045(8) 0.027(8) C42 0.130(12) 0.238(18) 0.045(12) 0.004(12) -0.005(10) 0.088(10) C43 0.47(4) 1.23(9) 0.087(17) 0.10(3) 0.072(19) 0.67(5) C44 0.56(5) 1.47(12) 0.10(2) 0.13(4) 0.11(3) 0.80(7) C45 0.233(19) 0.48(4) 0.11(2) 0.09(2) 0.088(17) 0.24(2) C46 0.149(14) 0.178(16) 0.129(16) 0.010(13) 0.067(14) 0.009(12) C47 0.092(10) 0.161(14) 0.138(19) 0.007(13) 0.035(12) 0.033(9) C48 0.168(11) 0.080(10) 0.211(16) 0.024(10) 0.117(10) 0.003(8) C49 0.129(10) 0.098(10) 0.142(13) -0.022(9) 0.059(9) -0.022(8) C50 0.33(2) 0.51(4) 0.28(2) 0.10(2) 0.20(2) 0.32(3) Cu2 0.0842(10) 0.0823(11) 0.0791(13) -0.0039(9) 0.0240(8) -0.0199(8) S61 0.0915(19) 0.0576(19) 0.087(2) -0.0012(16) 0.0301(16) 0.0019(15) S71 0.202(4) 0.059(3) 0.094(4) -0.005(2) 0.059(3) -0.004(3) S81 0.115(2) 0.101(3) 0.095(3) 0.020(2) 0.0270(19) -0.0024(19) S91 0.091(2) 0.094(3) 0.103(3) -0.001(3) 0.014(2) -0.002(2) O71 0.271(10) 0.098(6) 0.109(7) 0.029(5) 0.120(7) 0.055(6) O72 0.282(10) 0.053(5) 0.104(7) -0.018(5) 0.033(6) -0.037(6) O91 0.111(6) 0.131(7) 0.107(7) -0.022(6) 0.004(5) 0.006(5) O92 0.098(5) 0.095(6) 0.139(7) 0.021(5) 0.028(5) -0.013(4) N3 0.087(8) 0.110(8) 0.073(9) -0.015(7) 0.019(8) -0.025(6) N4 0.085(8) 0.089(7) 0.111(13) -0.014(7) 0.054(9) -0.024(6) N68 0.070(6) 0.061(6) 0.062(6) -0.002(5) 0.014(5) -0.008(6) N70 0.125(7) 0.077(7) 0.071(7) -0.020(6) 0.026(5) -0.017(7) N88 0.093(6) 0.084(8) 0.064(9) 0.009(7) 0.030(6) -0.007(6) N90 0.080(6) 0.095(9) 0.082(9) 0.003(7) 0.009(5) -0.007(6) C51 0.075(11) 0.215(16) 0.123(16) -0.041(12) 0.008(9) -0.056(9) C52 0.107(15) 0.241(19) 0.138(17) -0.052(14) 0.014(12) -0.065(12) C53 0.079(12) 0.141(13) 0.19(2) -0.041(15) 0.027(14) -0.026(9) C54 0.104(15) 0.111(11) 0.19(2) -0.039(12) 0.066(12) 0.001(10) C55 0.088(13) 0.060(8) 0.139(18) -0.014(9) 0.067(13) -0.014(7) C56 0.129(17) 0.067(9) 0.071(15) -0.016(9) 0.027(14) 0.013(9) C57 0.145(15) 0.106(11) 0.137(18) 0.005(12) 0.083(16) 0.013(10) C58 0.156(17) 0.159(14) 0.15(2) 0.036(13) 0.107(16) 0.026(13) C59 0.178(19) 0.165(14) 0.080(13) 0.035(11) 0.073(14) 0.046(12) C60 0.105(11) 0.140(12) 0.092(14) -0.013(11) 0.015(13) -0.003(9) C62 0.075(9) 0.052(8) 0.057(8) -0.002(6) 0.024(6) -0.016(7) C63 0.065(7) 0.063(8) 0.087(9) 0.021(7) 0.029(6) 0.000(8) C64 0.066(8) 0.055(9) 0.076(9) 0.010(7) 0.018(6) -0.006(7) C65 0.088(9) 0.037(8) 0.080(9) -0.009(7) 0.030(7) 0.003(7) C66 0.081(8) 0.062(9) 0.069(9) 0.002(7) 0.019(6) 0.004(8) C67 0.061(9) 0.066(10) 0.056(8) 0.010(7) 0.020(6) -0.023(8) C69 0.095(9) 0.074(10) 0.064(9) -0.009(7) 0.037(7) -0.005(8) C72 0.151(13) 0.029(6) 0.063(11) -0.001(6) 0.054(12) -0.018(7) C73 0.130(14) 0.057(8) 0.148(18) 0.003(10) 0.093(12) -0.008(8) C74 0.133(12) 0.056(8) 0.111(14) -0.003(10) 0.045(14) 0.000(7) C75 0.110(13) 0.049(8) 0.117(16) -0.024(8) 0.055(13) -0.013(8) C76 0.141(15) 0.089(10) 0.082(15) -0.016(9) 0.056(10) -0.016(9) C77 0.110(9) 0.058(8) 0.100(12) -0.018(9) 0.050(12) -0.008(6) C78 0.091(7) 0.061(8) 0.144(11) -0.019(8) 0.024(7) -0.010(6) C79 0.089(7) 0.075(9) 0.099(9) -0.008(7) 0.021(6) -0.003(6) C80 0.153(11) 0.129(12) 0.082(11) -0.008(9) 0.016(9) -0.010(8) C82 0.107(9) 0.109(13) 0.067(12) 0.024(12) 0.025(8) -0.017(8) C83 0.110(10) 0.143(17) 0.083(14) 0.014(12) 0.019(9) -0.014(10) C84 0.118(10) 0.115(15) 0.090(15) -0.005(13) 0.015(9) -0.018(10) C85 0.134(10) 0.102(14) 0.098(15) -0.032(13) 0.042(10) -0.002(9) C86 0.123(9) 0.078(12) 0.086(13) -0.003(9) 0.038(8) -0.008(8) C87 0.072(7) 0.092(13) 0.063(13) -0.002(11) 0.016(7) -0.017(8) C89 0.067(7) 0.102(12) 0.070(12) 0.016(10) 0.008(7) -0.007(8) C92 0.087(9) 0.086(8) 0.053(10) 0.009(7) 0.009(9) 0.005(7) C93 0.139(13) 0.142(12) 0.088(12) 0.009(8) 0.061(13) -0.019(9) C94 0.064(10) 0.168(14) 0.18(2) -0.008(14) 0.041(11) -0.024(9) C95 0.131(16) 0.093(10) 0.086(14) 0.008(10) 0.027(13) 0.022(9) C96 0.111(13) 0.251(19) 0.094(14) 0.031(12) 0.001(12) -0.014(12) C97 0.102(12) 0.180(14) 0.094(14) 0.043(11) 0.031(9) -0.007(9) C98 0.177(12) 0.236(17) 0.082(11) -0.035(11) 0.067(10) 0.006(11) C99 0.211(13) 0.132(13) 0.119(13) -0.037(10) 0.066(10) -0.014(11) C100 0.072(8) 0.163(13) 0.171(14) -0.034(10) -0.012(8) 0.001(8) O1 0.141(7) 0.152(8) 0.403(16) 0.040(9) 0.110(8) -0.012(6) _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 N38 1.981(8) . y Cu1 N1 1.993(7) . y Cu1 N18 1.999(7) . y Cu1 N2 2.015(8) . y Cu1 O21 2.212(5) . y Cu1 N40 3.019(8) . y Cu1 N20 3.517(7) . y Cu1 Cu2 8.6073(17) . y S11 C12 1.719(11) . ? S11 C19 1.761(9) . ? S21 O22 1.427(6) . ? S21 O21 1.471(5) . ? S21 N20 1.579(8) . ? S21 C22 1.765(11) . ? S31 C32 1.725(13) . ? S31 C39 1.741(11) . ? S41 O42 1.446(9) . ? S41 O41 1.447(7) . ? S41 N40 1.613(8) . ? S41 C42 1.750(15) . ? N1 C5 1.329(11) . ? N1 C1 1.336(11) . ? N2 C10 1.332(12) . ? N2 C6 1.337(11) . ? N18 C19 1.343(11) . ? N18 C17 1.396(11) . ? N20 C19 1.304(11) . ? N38 C39 1.317(12) . ? N38 C37 1.388(13) . ? N40 C39 1.344(12) . ? C1 C2 1.404(12) . ? C1 H1 0.9300 . ? C2 C3 1.381(13) . ? C2 H2 0.9300 . ? C3 C4 1.349(13) . ? C3 H3 0.9300 . ? C4 C5 1.371(13) . ? C4 H4 0.9300 . ? C5 C6 1.488(13) . ? C6 C7 1.361(13) . ? C7 C8 1.381(13) . ? C7 H7 0.9300 . ? C8 C9 1.383(14) . ? C8 H8 0.9300 . ? C9 C10 1.362(12) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C12 C17 1.372(12) . ? C12 C13 1.387(12) . ? C13 C14 1.380(12) . ? C13 H13 0.9300 . ? C14 C15 1.426(13) . ? C14 C28 1.508(12) . ? C15 C16 1.393(11) . ? C15 C29 1.505(11) . ? C16 C17 1.397(11) . ? C16 H16 0.9300 . ? C22 C23 1.337(13) . ? C22 C27 1.345(13) . ? C23 C24 1.375(15) . ? C23 H23 0.9300 . ? C24 C25 1.378(15) . ? C24 H24 0.9300 . ? C25 C26 1.343(15) . ? C25 C30 1.552(14) . ? C26 C27 1.374(14) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C32 C37 1.365(13) . ? C32 C33 1.398(14) . ? C33 C34 1.399(14) . ? C33 H33 0.9300 . ? C34 C35 1.391(15) . ? C34 C48 1.547(15) . ? C35 C36 1.353(14) . ? C35 C49 1.504(13) . ? C36 C37 1.383(13) . ? C36 H36 0.9300 . ? C42 C43 1.257(19) . ? C42 C47 1.274(15) . ? C43 C44 1.42(2) . ? C43 H43 0.9300 . ? C44 C45 1.24(2) . ? C44 H44 0.9300 . ? C45 C46 1.236(17) . ? C45 C50 1.56(2) . ? C46 C47 1.388(17) . ? C46 H46 0.9300 . ? C47 H47 0.9300 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? Cu2 N68 1.960(7) . y Cu2 N88 1.978(10) . y Cu2 N3 1.989(9) . y Cu2 N4 2.022(11) . y Cu2 N90 2.733(10) . y Cu2 N70 2.890(9) . y S61 C62 1.735(9) . ? S61 C69 1.756(10) . ? S71 O72 1.443(7) . ? S71 O71 1.455(8) . ? S71 N70 1.593(9) . ? S71 C72 1.781(11) . ? S81 C89 1.746(12) . ? S81 C82 1.759(14) . ? S91 O91 1.444(7) . ? S91 O92 1.456(7) . ? S91 N90 1.600(10) . ? S91 C92 1.769(10) . ? N3 C51 1.327(13) . ? N3 C55 1.366(13) . ? N4 C56 1.297(16) . ? N4 C60 1.343(14) . ? N68 C69 1.320(11) . ? N68 C67 1.405(11) . ? N70 C69 1.355(11) . ? N88 C89 1.330(13) . ? N88 C87 1.405(13) . ? N90 C89 1.341(12) . ? C51 C52 1.386(15) . ? C51 H51 0.9300 . ? C52 C53 1.334(17) . ? C52 H52 0.9300 . ? C53 C54 1.383(16) . ? C53 H53 0.9300 . ? C54 C55 1.420(16) . ? C54 H54 0.9300 . ? C55 C56 1.447(15) . ? C56 C57 1.414(17) . ? C57 C58 1.372(16) . ? C57 H57 0.9300 . ? C58 C59 1.347(16) . ? C58 H58 0.9300 . ? C59 C60 1.378(15) . ? C59 H59 0.9300 . ? C60 H60 0.9300 . ? C62 C63 1.363(11) . ? C62 C67 1.398(11) . ? C63 C64 1.392(11) . ? C63 H63 0.9300 . ? C64 C65 1.404(11) . ? C64 C78 1.510(11) . ? C65 C66 1.375(11) . ? C65 C79 1.486(11) . ? C66 C67 1.382(11) . ? C66 H66 0.9300 . ? C72 C73 1.384(13) . ? C72 C77 1.394(12) . ? C73 C74 1.355(14) . ? C73 H73 0.9300 . ? C74 C75 1.377(14) . ? C74 H74 0.9300 . ? C75 C76 1.377(14) . ? C75 C80 1.489(14) . ? C76 C77 1.369(13) . ? C76 H76 0.9300 . ? C77 H77 0.9300 . ? C78 H78A 0.9600 . ? C78 H78B 0.9600 . ? C78 H78C 0.9600 . ? C79 H79A 0.9600 . ? C79 H79B 0.9600 . ? C79 H79C 0.9600 . ? C80 H80A 0.9600 . ? C80 H80B 0.9600 . ? C80 H80C 0.9600 . ? C82 C87 1.365(13) . ? C82 C83 1.391(15) . ? C83 C84 1.381(15) . ? C83 H83 0.9300 . ? C84 C85 1.395(16) . ? C84 C98 1.544(16) . ? C85 C86 1.384(15) . ? C85 C99 1.513(15) . ? C86 C87 1.392(14) . ? C86 H86 0.9300 . ? C92 C97 1.351(13) . ? C92 C93 1.363(13) . ? C93 C94 1.383(14) . ? C93 H93 0.9300 . ? C94 C95 1.322(16) . ? C94 H94 0.9300 . ? C95 C96 1.348(16) . ? C95 C100 1.519(16) . ? C96 C97 1.416(15) . ? C96 H96 0.9300 . ? C97 H97 0.9300 . ? C98 H98A 0.9600 . ? C98 H98B 0.9600 . ? C98 H98C 0.9600 . ? C99 H99A 0.9600 . ? C99 H99B 0.9600 . ? C99 H99C 0.9600 . ? C100 H10A 0.9600 . ? C100 H10B 0.9600 . ? C100 H10C 0.9600 . ? O1 H1A 0.9672 . ? O1 H1B 0.8499 . ? 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 N38 Cu1 N1 93.5(4) . . y N38 Cu1 N18 95.4(3) . . y N1 Cu1 N18 167.8(4) . . y N38 Cu1 N2 152.0(4) . . y N1 Cu1 N2 79.5(5) . . y N18 Cu1 N2 96.2(4) . . y N38 Cu1 O21 114.5(4) . . y N1 Cu1 O21 82.4(3) . . y N18 Cu1 O21 86.3(3) . . y N2 Cu1 O21 91.6(3) . . y N38 Cu1 N40 49.5(3) . . y N1 Cu1 N40 84.6(3) . . y N18 Cu1 N40 107.6(3) . . y N2 Cu1 N40 102.6(3) . . y O21 Cu1 N40 158.7(2) . . y N38 Cu1 N20 102.2(3) . . y N1 Cu1 N20 127.7(3) . . y N18 Cu1 N20 41.9(3) . . y N2 Cu1 N20 103.5(3) . . y O21 Cu1 N20 45.6(2) . . y N40 Cu1 N20 141.6(2) . . y N38 Cu1 Cu2 123.8(3) . . ? N1 Cu1 Cu2 39.7(4) . . ? N18 Cu1 Cu2 136.8(2) . . ? N2 Cu1 Cu2 40.6(3) . . ? O21 Cu1 Cu2 92.12(14) . . ? N40 Cu1 Cu2 88.57(17) . . ? N20 Cu1 Cu2 129.20(14) . . ? C12 S11 C19 90.4(7) . . ? O22 S21 O21 116.7(4) . . ? O22 S21 N20 107.6(5) . . ? O21 S21 N20 111.8(4) . . ? O22 S21 C22 109.7(6) . . ? O21 S21 C22 105.4(5) . . ? N20 S21 C22 104.9(4) . . ? C32 S31 C39 89.0(8) . . ? O42 S41 O41 117.6(6) . . ? O42 S41 N40 108.2(5) . . ? O41 S41 N40 110.7(5) . . ? O42 S41 C42 108.3(7) . . ? O41 S41 C42 105.6(7) . . ? N40 S41 C42 105.7(6) . . ? S21 O21 Cu1 131.0(3) . . ? C5 N1 C1 118.8(9) . . ? C5 N1 Cu1 114.2(9) . . ? C1 N1 Cu1 125.4(10) . . ? C10 N2 C6 116.7(10) . . ? C10 N2 Cu1 126.5(9) . . ? C6 N2 Cu1 116.3(9) . . ? C19 N18 C17 111.3(9) . . ? C19 N18 Cu1 127.9(7) . . ? C17 N18 Cu1 120.8(8) . . ? C19 N20 S21 125.4(7) . . ? C19 N20 Cu1 57.1(5) . . ? S21 N20 Cu1 71.4(3) . . ? C39 N38 C37 109.3(10) . . ? C39 N38 Cu1 120.2(8) . . ? C37 N38 Cu1 130.4(10) . . ? C39 N40 S41 123.0(9) . . ? C39 N40 Cu1 71.0(6) . . ? S41 N40 Cu1 165.9(5) . . ? N1 C1 C2 121.5(10) . . ? N1 C1 H1 119.2 . . ? C2 C1 H1 119.2 . . ? C3 C2 C1 117.8(11) . . ? C3 C2 H2 121.1 . . ? C1 C2 H2 121.1 . . ? C4 C3 C2 119.8(12) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C3 C4 C5 119.5(12) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? N1 C5 C4 122.5(12) . . ? N1 C5 C6 116.3(12) . . ? C4 C5 C6 121.2(14) . . ? N2 C6 C7 123.0(11) . . ? N2 C6 C5 111.3(13) . . ? C7 C6 C5 125.7(14) . . ? C6 C7 C8 119.0(11) . . ? C6 C7 H7 120.5 . . ? C8 C7 H7 120.5 . . ? C7 C8 C9 119.0(12) . . ? C7 C8 H8 120.5 . . ? C9 C8 H8 120.5 . . ? C10 C9 C8 117.3(11) . . ? C10 C9 H9 121.3 . . ? C8 C9 H9 121.3 . . ? N2 C10 C9 124.8(11) . . ? N2 C10 H10 117.6 . . ? C9 C10 H10 117.6 . . ? C17 C12 C13 122.0(11) . . ? C17 C12 S11 110.4(12) . . ? C13 C12 S11 127.5(11) . . ? C14 C13 C12 120.5(11) . . ? C14 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? C13 C14 C15 118.6(11) . . ? C13 C14 C28 122.0(14) . . ? C15 C14 C28 119.4(14) . . ? C16 C15 C14 119.5(10) . . ? C16 C15 C29 119.0(12) . . ? C14 C15 C29 121.5(14) . . ? C15 C16 C17 121.0(10) . . ? C15 C16 H16 119.5 . . ? C17 C16 H16 119.5 . . ? C12 C17 N18 115.3(12) . . ? C12 C17 C16 118.5(11) . . ? N18 C17 C16 126.2(12) . . ? N20 C19 N18 133.1(9) . . ? N20 C19 S11 114.3(9) . . ? N18 C19 S11 112.6(8) . . ? C23 C22 C27 120.0(12) . . ? C23 C22 S21 117.2(13) . . ? C27 C22 S21 122.8(13) . . ? C22 C23 C24 120.4(13) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C23 C24 C25 120.2(13) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C26 C25 C24 118.1(14) . . ? C26 C25 C30 119.2(18) . . ? C24 C25 C30 122.8(18) . . ? C25 C26 C27 121.2(13) . . ? C25 C26 H26 119.4 . . ? C27 C26 H26 119.4 . . ? C22 C27 C26 120.1(12) . . ? C22 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? C14 C28 H28A 109.5 . . ? C14 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C14 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C15 C29 H29A 109.5 . . ? C15 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C15 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C37 C32 C33 119.9(13) . . ? C37 C32 S31 109.9(13) . . ? C33 C32 S31 130.1(15) . . ? C32 C33 C34 119.6(13) . . ? C32 C33 H33 120.2 . . ? C34 C33 H33 120.2 . . ? C35 C34 C33 119.0(14) . . ? C35 C34 C48 124.9(18) . . ? C33 C34 C48 116.1(18) . . ? C36 C35 C34 120.4(13) . . ? C36 C35 C49 121.4(16) . . ? C34 C35 C49 118.2(17) . . ? C35 C36 C37 121.0(12) . . ? C35 C36 H36 119.5 . . ? C37 C36 H36 119.5 . . ? C32 C37 C36 120.0(13) . . ? C32 C37 N38 116.3(14) . . ? C36 C37 N38 123.7(14) . . ? N38 C39 N40 119.3(11) . . ? N38 C39 S31 115.4(9) . . ? N40 C39 S31 125.4(11) . . ? C43 C42 C47 113.3(18) . . ? C43 C42 S41 121.3(17) . . ? C47 C42 S41 125.3(14) . . ? C42 C43 C44 121.3(18) . . ? C42 C43 H43 119.3 . . ? C44 C43 H43 119.3 . . ? C45 C44 C43 124(2) . . ? C45 C44 H44 118.0 . . ? C43 C44 H44 118.0 . . ? C46 C45 C44 114(2) . . ? C46 C45 C50 123(2) . . ? C44 C45 C50 122(2) . . ? C45 C46 C47 123.2(19) . . ? C45 C46 H46 118.4 . . ? C47 C46 H46 118.4 . . ? C42 C47 C46 123.4(17) . . ? C42 C47 H47 118.3 . . ? C46 C47 H47 118.3 . . ? C34 C48 H48A 109.5 . . ? C34 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C34 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C35 C49 H49A 109.5 . . ? C35 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C35 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C45 C50 H50A 109.5 . . ? C45 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C45 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? N68 Cu2 N88 92.8(3) . . y N68 Cu2 N3 172.7(5) . . y N88 Cu2 N3 94.3(5) . . y N68 Cu2 N4 92.3(5) . . y N88 Cu2 N4 173.1(5) . . y N3 Cu2 N4 80.8(6) . . y N68 Cu2 N90 96.1(3) . . y N88 Cu2 N90 55.2(4) . . y N3 Cu2 N90 89.4(3) . . y N4 Cu2 N90 119.5(4) . . y N68 Cu2 N70 52.6(3) . . y N88 Cu2 N70 96.7(4) . . y N3 Cu2 N70 124.5(3) . . y N4 Cu2 N70 90.1(4) . . y N90 Cu2 N70 139.4(3) . . y N68 Cu2 Cu1 59.0(2) . . ? N88 Cu2 Cu1 34.0(2) . . ? N3 Cu2 Cu1 128.2(4) . . ? N4 Cu2 Cu1 150.2(5) . . ? N90 Cu2 Cu1 61.9(2) . . ? N70 Cu2 Cu1 78.56(17) . . ? C62 S61 C69 89.2(6) . . ? O72 S71 O71 116.6(6) . . ? O72 S71 N70 105.1(5) . . ? O71 S71 N70 112.8(5) . . ? O72 S71 C72 107.3(5) . . ? O71 S71 C72 106.8(8) . . ? N70 S71 C72 107.8(6) . . ? C89 S81 C82 89.5(8) . . ? O91 S91 O92 118.3(5) . . ? O91 S91 N90 107.3(6) . . ? O92 S91 N90 111.8(5) . . ? O91 S91 C92 106.9(6) . . ? O92 S91 C92 106.7(6) . . ? N90 S91 C92 104.9(5) . . ? C51 N3 C55 120.8(13) . . ? C51 N3 Cu2 125.5(11) . . ? C55 N3 Cu2 113.4(11) . . ? C56 N4 C60 117.7(13) . . ? C56 N4 Cu2 114.1(14) . . ? C60 N4 Cu2 128.1(13) . . ? C69 N68 C67 111.9(9) . . ? C69 N68 Cu2 115.7(7) . . ? C67 N68 Cu2 132.4(8) . . ? C69 N70 S71 120.8(8) . . ? C69 N70 Cu2 72.5(6) . . ? S71 N70 Cu2 166.2(5) . . ? C89 N88 C87 111.0(12) . . ? C89 N88 Cu2 110.9(9) . . ? C87 N88 Cu2 138.1(11) . . ? C89 N90 S91 122.0(10) . . ? C89 N90 Cu2 76.5(7) . . ? S91 N90 Cu2 160.4(6) . . ? N3 C51 C52 123.7(14) . . ? N3 C51 H51 118.1 . . ? C52 C51 H51 118.1 . . ? C53 C52 C51 117.5(17) . . ? C53 C52 H52 121.2 . . ? C51 C52 H52 121.2 . . ? C52 C53 C54 120.5(18) . . ? C52 C53 H53 119.8 . . ? C54 C53 H53 119.8 . . ? C53 C54 C55 121.1(16) . . ? C53 C54 H54 119.4 . . ? C55 C54 H54 119.4 . . ? N3 C55 C54 116.2(15) . . ? N3 C55 C56 114.8(16) . . ? C54 C55 C56 128.8(18) . . ? N4 C56 C57 124.9(14) . . ? N4 C56 C55 116.5(19) . . ? C57 C56 C55 118(2) . . ? C58 C57 C56 114.5(17) . . ? C58 C57 H57 122.8 . . ? C56 C57 H57 122.8 . . ? C59 C58 C57 122.2(18) . . ? C59 C58 H58 118.9 . . ? C57 C58 H58 118.9 . . ? C58 C59 C60 118.4(16) . . ? C58 C59 H59 120.8 . . ? C60 C59 H59 120.8 . . ? N4 C60 C59 122.1(14) . . ? N4 C60 H60 119.0 . . ? C59 C60 H60 119.0 . . ? C63 C62 C67 120.0(9) . . ? C63 C62 S61 128.9(10) . . ? C67 C62 S61 111.0(10) . . ? C62 C63 C64 121.1(9) . . ? C62 C63 H63 119.4 . . ? C64 C63 H63 119.4 . . ? C63 C64 C65 118.3(9) . . ? C63 C64 C78 121.0(10) . . ? C65 C64 C78 120.7(11) . . ? C66 C65 C64 120.8(9) . . ? C66 C65 C79 119.2(11) . . ? C64 C65 C79 119.9(11) . . ? C65 C66 C67 119.8(9) . . ? C65 C66 H66 120.1 . . ? C67 C66 H66 120.1 . . ? C66 C67 C62 119.9(9) . . ? C66 C67 N68 126.8(11) . . ? C62 C67 N68 113.3(11) . . ? N68 C69 N70 119.0(10) . . ? N68 C69 S61 114.5(8) . . ? N70 C69 S61 126.4(9) . . ? C73 C72 C77 117.7(12) . . ? C73 C72 S71 121.7(16) . . ? C77 C72 S71 120.6(17) . . ? C74 C73 C72 120.8(13) . . ? C74 C73 H73 119.6 . . ? C72 C73 H73 119.6 . . ? C73 C74 C75 122.7(15) . . ? C73 C74 H74 118.7 . . ? C75 C74 H74 118.7 . . ? C74 C75 C76 116.0(14) . . ? C74 C75 C80 122.3(17) . . ? C76 C75 C80 121.6(17) . . ? C77 C76 C75 123.0(13) . . ? C77 C76 H76 118.5 . . ? C75 C76 H76 118.5 . . ? C76 C77 C72 119.6(12) . . ? C76 C77 H77 120.2 . . ? C72 C77 H77 120.2 . . ? C64 C78 H78A 109.5 . . ? C64 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C64 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C65 C79 H79A 109.5 . . ? C65 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C65 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? C75 C80 H80A 109.5 . . ? C75 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C75 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? C87 C82 C83 122.5(14) . . ? C87 C82 S81 109.8(14) . . ? C83 C82 S81 127.7(16) . . ? C84 C83 C82 118.9(15) . . ? C84 C83 H83 120.5 . . ? C82 C83 H83 120.5 . . ? C83 C84 C85 118.7(16) . . ? C83 C84 C98 120.8(19) . . ? C85 C84 C98 120.4(18) . . ? C86 C85 C84 121.9(14) . . ? C86 C85 C99 118.3(19) . . ? C84 C85 C99 119.7(17) . . ? C85 C86 C87 118.8(13) . . ? C85 C86 H86 120.6 . . ? C87 C86 H86 120.6 . . ? C82 C87 C86 119.0(13) . . ? C82 C87 N88 115.5(15) . . ? C86 C87 N88 125.5(16) . . ? N88 C89 N90 117.4(13) . . ? N88 C89 S81 114.2(11) . . ? N90 C89 S81 128.4(12) . . ? C97 C92 C93 117.3(11) . . ? C97 C92 S91 120.1(13) . . ? C93 C92 S91 122.5(14) . . ? C92 C93 C94 119.9(12) . . ? C92 C93 H93 120.0 . . ? C94 C93 H93 120.0 . . ? C95 C94 C93 124.7(15) . . ? C95 C94 H94 117.7 . . ? C93 C94 H94 117.7 . . ? C94 C95 C96 115.5(16) . . ? C94 C95 C100 119.2(16) . . ? C96 C95 C100 125.3(16) . . ? C95 C96 C97 122.3(15) . . ? C95 C96 H96 118.9 . . ? C97 C96 H96 118.9 . . ? C92 C97 C96 120.3(12) . . ? C92 C97 H97 119.9 . . ? C96 C97 H97 119.9 . . ? C84 C98 H98A 109.5 . . ? C84 C98 H98B 109.5 . . ? H98A C98 H98B 109.5 . . ? C84 C98 H98C 109.5 . . ? H98A C98 H98C 109.5 . . ? H98B C98 H98C 109.5 . . ? C85 C99 H99A 109.5 . . ? C85 C99 H99B 109.5 . . ? H99A C99 H99B 109.5 . . ? C85 C99 H99C 109.5 . . ? H99A C99 H99C 109.5 . . ? H99B C99 H99C 109.5 . . ? C95 C100 H10A 109.5 . . ? C95 C100 H10B 109.5 . . ? H10A C100 H10B 109.5 . . ? C95 C100 H10C 109.5 . . ? H10A C100 H10C 109.5 . . ? H10B C100 H10C 109.5 . . ? H1A O1 H1B 104.3 . . ? 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 O22 S21 O21 Cu1 -128.8(5) . . . . ? N20 S21 O21 Cu1 -4.3(6) . . . . ? C22 S21 O21 Cu1 109.2(6) . . . . ? N38 Cu1 O21 S21 85.5(5) . . . . ? N1 Cu1 O21 S21 175.8(6) . . . . ? N18 Cu1 O21 S21 -8.8(5) . . . . ? N2 Cu1 O21 S21 -104.9(6) . . . . ? N40 Cu1 O21 S21 122.9(6) . . . . ? N20 Cu1 O21 S21 2.5(4) . . . . ? Cu2 Cu1 O21 S21 -145.6(4) . . . . ? N38 Cu1 N1 C5 -166.4(7) . . . . ? N18 Cu1 N1 C5 57(2) . . . . ? N2 Cu1 N1 C5 -13.7(7) . . . . ? O21 Cu1 N1 C5 79.3(7) . . . . ? N40 Cu1 N1 C5 -117.6(7) . . . . ? N20 Cu1 N1 C5 85.3(7) . . . . ? Cu2 Cu1 N1 C5 -23.3(5) . . . . ? N38 Cu1 N1 C1 28.0(8) . . . . ? N18 Cu1 N1 C1 -109(2) . . . . ? N2 Cu1 N1 C1 -179.3(8) . . . . ? O21 Cu1 N1 C1 -86.2(8) . . . . ? N40 Cu1 N1 C1 76.8(8) . . . . ? N20 Cu1 N1 C1 -80.2(9) . . . . ? Cu2 Cu1 N1 C1 171.1(10) . . . . ? N38 Cu1 N2 C10 -98.4(10) . . . . ? N1 Cu1 N2 C10 -175.9(9) . . . . ? N18 Cu1 N2 C10 15.6(9) . . . . ? O21 Cu1 N2 C10 102.1(8) . . . . ? N40 Cu1 N2 C10 -93.9(8) . . . . ? N20 Cu1 N2 C10 57.6(8) . . . . ? Cu2 Cu1 N2 C10 -166.5(10) . . . . ? N38 Cu1 N2 C6 90.2(11) . . . . ? N1 Cu1 N2 C6 12.7(7) . . . . ? N18 Cu1 N2 C6 -155.7(7) . . . . ? O21 Cu1 N2 C6 -69.3(7) . . . . ? N40 Cu1 N2 C6 94.7(7) . . . . ? N20 Cu1 N2 C6 -113.8(7) . . . . ? Cu2 Cu1 N2 C6 22.1(5) . . . . ? N38 Cu1 N18 C19 -102.5(8) . . . . ? N1 Cu1 N18 C19 34(2) . . . . ? N2 Cu1 N18 C19 103.0(7) . . . . ? O21 Cu1 N18 C19 11.8(7) . . . . ? N40 Cu1 N18 C19 -151.7(7) . . . . ? N20 Cu1 N18 C19 -0.3(6) . . . . ? Cu2 Cu1 N18 C19 100.9(7) . . . . ? N38 Cu1 N18 C17 76.3(7) . . . . ? N1 Cu1 N18 C17 -147.1(19) . . . . ? N2 Cu1 N18 C17 -78.1(7) . . . . ? O21 Cu1 N18 C17 -169.4(7) . . . . ? N40 Cu1 N18 C17 27.2(7) . . . . ? N20 Cu1 N18 C17 178.6(8) . . . . ? Cu2 Cu1 N18 C17 -80.2(7) . . . . ? O22 S21 N20 C19 151.2(8) . . . . ? O21 S21 N20 C19 21.8(10) . . . . ? C22 S21 N20 C19 -91.9(10) . . . . ? O22 S21 N20 Cu1 131.5(3) . . . . ? O21 S21 N20 Cu1 2.1(3) . . . . ? C22 S21 N20 Cu1 -111.7(6) . . . . ? N38 Cu1 N20 C19 84.8(7) . . . . ? N1 Cu1 N20 C19 -171.1(7) . . . . ? N18 Cu1 N20 C19 0.3(6) . . . . ? N2 Cu1 N20 C19 -83.9(7) . . . . ? O21 Cu1 N20 C19 -162.7(7) . . . . ? N40 Cu1 N20 C19 47.5(7) . . . . ? Cu2 Cu1 N20 C19 -119.7(6) . . . . ? N38 Cu1 N20 S21 -114.3(4) . . . . ? N1 Cu1 N20 S21 -10.2(6) . . . . ? N18 Cu1 N20 S21 161.2(5) . . . . ? N2 Cu1 N20 S21 76.9(5) . . . . ? O21 Cu1 N20 S21 -1.8(3) . . . . ? N40 Cu1 N20 S21 -151.6(3) . . . . ? Cu2 Cu1 N20 S21 41.2(4) . . . . ? N1 Cu1 N38 C39 79.4(8) . . . . ? N18 Cu1 N38 C39 -108.9(8) . . . . ? N2 Cu1 N38 C39 5.3(13) . . . . ? O21 Cu1 N38 C39 162.6(7) . . . . ? N40 Cu1 N38 C39 -0.5(6) . . . . ? N20 Cu1 N38 C39 -150.8(7) . . . . ? Cu2 Cu1 N38 C39 51.9(8) . . . . ? N1 Cu1 N38 C37 -96.1(8) . . . . ? N18 Cu1 N38 C37 75.6(9) . . . . ? N2 Cu1 N38 C37 -170.2(9) . . . . ? O21 Cu1 N38 C37 -12.8(9) . . . . ? N40 Cu1 N38 C37 -175.9(10) . . . . ? N20 Cu1 N38 C37 33.7(8) . . . . ? Cu2 Cu1 N38 C37 -123.6(7) . . . . ? O42 S41 N40 C39 -168.0(8) . . . . ? O41 S41 N40 C39 -37.8(10) . . . . ? C42 S41 N40 C39 76.1(10) . . . . ? O42 S41 N40 Cu1 19.1(19) . . . . ? O41 S41 N40 Cu1 149.3(16) . . . . ? C42 S41 N40 Cu1 -96.8(18) . . . . ? N38 Cu1 N40 C39 0.4(6) . . . . ? N1 Cu1 N40 C39 -98.8(6) . . . . ? N18 Cu1 N40 C39 82.4(6) . . . . ? N2 Cu1 N40 C39 -176.8(6) . . . . ? O21 Cu1 N40 C39 -46.2(9) . . . . ? N20 Cu1 N40 C39 51.5(7) . . . . ? Cu2 Cu1 N40 C39 -138.4(6) . . . . ? N38 Cu1 N40 S41 174.1(19) . . . . ? N1 Cu1 N40 S41 74.9(18) . . . . ? N18 Cu1 N40 S41 -103.9(17) . . . . ? N2 Cu1 N40 S41 -3.1(18) . . . . ? O21 Cu1 N40 S41 127.5(17) . . . . ? N20 Cu1 N40 S41 -134.8(16) . . . . ? Cu2 Cu1 N40 S41 35.3(17) . . . . ? C5 N1 C1 C2 0.6(14) . . . . ? Cu1 N1 C1 C2 165.5(7) . . . . ? N1 C1 C2 C3 -0.3(15) . . . . ? C1 C2 C3 C4 0.6(16) . . . . ? C2 C3 C4 C5 -1.2(17) . . . . ? C1 N1 C5 C4 -1.2(14) . . . . ? Cu1 N1 C5 C4 -167.8(7) . . . . ? C1 N1 C5 C6 179.7(8) . . . . ? Cu1 N1 C5 C6 13.1(10) . . . . ? C3 C4 C5 N1 1.6(16) . . . . ? C3 C4 C5 C6 -179.4(10) . . . . ? C10 N2 C6 C7 -2.0(14) . . . . ? Cu1 N2 C6 C7 170.2(8) . . . . ? C10 N2 C6 C5 178.6(8) . . . . ? Cu1 N2 C6 C5 -9.1(10) . . . . ? N1 C5 C6 N2 -2.6(12) . . . . ? C4 C5 C6 N2 178.3(9) . . . . ? N1 C5 C6 C7 178.0(9) . . . . ? C4 C5 C6 C7 -1.0(15) . . . . ? N2 C6 C7 C8 0.3(16) . . . . ? C5 C6 C7 C8 179.5(10) . . . . ? C6 C7 C8 C9 2.2(17) . . . . ? C7 C8 C9 C10 -2.8(17) . . . . ? C6 N2 C10 C9 1.4(15) . . . . ? Cu1 N2 C10 C9 -170.0(8) . . . . ? C8 C9 C10 N2 1.1(16) . . . . ? C19 S11 C12 C17 0.5(7) . . . . ? C19 S11 C12 C13 177.8(10) . . . . ? C17 C12 C13 C14 -2.8(15) . . . . ? S11 C12 C13 C14 -179.8(8) . . . . ? C12 C13 C14 C15 1.7(15) . . . . ? C12 C13 C14 C28 179.7(9) . . . . ? C13 C14 C15 C16 -0.3(14) . . . . ? C28 C14 C15 C16 -178.4(9) . . . . ? C13 C14 C15 C29 -178.3(9) . . . . ? C28 C14 C15 C29 3.7(14) . . . . ? C14 C15 C16 C17 0.0(14) . . . . ? C29 C15 C16 C17 178.0(8) . . . . ? C13 C12 C17 N18 -178.2(9) . . . . ? S11 C12 C17 N18 -0.6(10) . . . . ? C13 C12 C17 C16 2.4(14) . . . . ? S11 C12 C17 C16 179.9(7) . . . . ? C19 N18 C17 C12 0.4(11) . . . . ? Cu1 N18 C17 C12 -178.6(6) . . . . ? C19 N18 C17 C16 179.9(8) . . . . ? Cu1 N18 C17 C16 0.9(12) . . . . ? C15 C16 C17 C12 -1.0(13) . . . . ? C15 C16 C17 N18 179.6(9) . . . . ? S21 N20 C19 N18 -22.8(16) . . . . ? Cu1 N20 C19 N18 -0.4(8) . . . . ? S21 N20 C19 S11 159.1(5) . . . . ? Cu1 N20 C19 S11 -178.5(8) . . . . ? C17 N18 C19 N20 -178.2(10) . . . . ? Cu1 N18 C19 N20 0.7(15) . . . . ? C17 N18 C19 S11 0.0(9) . . . . ? Cu1 N18 C19 S11 178.9(4) . . . . ? C12 S11 C19 N20 178.3(8) . . . . ? C12 S11 C19 N18 -0.3(7) . . . . ? O22 S21 C22 C23 14.4(9) . . . . ? O21 S21 C22 C23 140.8(8) . . . . ? N20 S21 C22 C23 -101.0(9) . . . . ? O22 S21 C22 C27 -168.1(10) . . . . ? O21 S21 C22 C27 -41.7(11) . . . . ? N20 S21 C22 C27 76.6(11) . . . . ? C27 C22 C23 C24 2.0(17) . . . . ? S21 C22 C23 C24 179.6(9) . . . . ? C22 C23 C24 C25 0.9(18) . . . . ? C23 C24 C25 C26 -2.7(19) . . . . ? C23 C24 C25 C30 177.0(10) . . . . ? C24 C25 C26 C27 2(2) . . . . ? C30 C25 C26 C27 -178.0(12) . . . . ? C23 C22 C27 C26 -3(2) . . . . ? S21 C22 C27 C26 179.6(10) . . . . ? C25 C26 C27 C22 1(2) . . . . ? C39 S31 C32 C37 -2.2(8) . . . . ? C39 S31 C32 C33 178.5(11) . . . . ? C37 C32 C33 C34 2.2(17) . . . . ? S31 C32 C33 C34 -178.6(9) . . . . ? C32 C33 C34 C35 0.0(18) . . . . ? C32 C33 C34 C48 -179.9(9) . . . . ? C33 C34 C35 C36 -1.5(17) . . . . ? C48 C34 C35 C36 178.3(10) . . . . ? C33 C34 C35 C49 178.4(10) . . . . ? C48 C34 C35 C49 -1.8(16) . . . . ? C34 C35 C36 C37 0.9(16) . . . . ? C49 C35 C36 C37 -179.0(9) . . . . ? C33 C32 C37 C36 -2.8(16) . . . . ? S31 C32 C37 C36 177.8(8) . . . . ? C33 C32 C37 N38 179.9(9) . . . . ? S31 C32 C37 N38 0.5(12) . . . . ? C35 C36 C37 C32 1.3(16) . . . . ? C35 C36 C37 N38 178.4(9) . . . . ? C39 N38 C37 C32 2.2(12) . . . . ? Cu1 N38 C37 C32 178.1(7) . . . . ? C39 N38 C37 C36 -175.0(10) . . . . ? Cu1 N38 C37 C36 0.9(14) . . . . ? C37 N38 C39 N40 177.3(9) . . . . ? Cu1 N38 C39 N40 0.9(13) . . . . ? C37 N38 C39 S31 -4.0(10) . . . . ? Cu1 N38 C39 S31 179.7(4) . . . . ? S41 N40 C39 N38 -178.7(7) . . . . ? Cu1 N40 C39 N38 -0.5(8) . . . . ? S41 N40 C39 S31 2.7(13) . . . . ? Cu1 N40 C39 S31 -179.2(9) . . . . ? C32 S31 C39 N38 3.7(8) . . . . ? C32 S31 C39 N40 -177.6(9) . . . . ? O42 S41 C42 C43 96(3) . . . . ? O41 S41 C42 C43 -30(3) . . . . ? N40 S41 C42 C43 -148(3) . . . . ? O42 S41 C42 C47 -88.2(17) . . . . ? O41 S41 C42 C47 145.0(16) . . . . ? N40 S41 C42 C47 27.6(19) . . . . ? C47 C42 C43 C44 8(5) . . . . ? S41 C42 C43 C44 -176(3) . . . . ? C42 C43 C44 C45 -4(8) . . . . ? C43 C44 C45 C46 -1(7) . . . . ? C43 C44 C45 C50 -176(4) . . . . ? C44 C45 C46 C47 2(5) . . . . ? C50 C45 C46 C47 176.2(18) . . . . ? C43 C42 C47 C46 -7(3) . . . . ? S41 C42 C47 C46 177.1(11) . . . . ? C45 C46 C47 C42 3(3) . . . . ? N38 Cu1 Cu2 N68 135.6(5) . . . . ? N1 Cu1 Cu2 N68 89.4(5) . . . . ? N18 Cu1 Cu2 N68 -72.9(6) . . . . ? N2 Cu1 Cu2 N68 -76.1(5) . . . . ? O21 Cu1 Cu2 N68 13.9(4) . . . . ? N40 Cu1 Cu2 N68 172.6(4) . . . . ? N20 Cu1 Cu2 N68 -15.3(4) . . . . ? N38 Cu1 Cu2 N88 -50.5(8) . . . . ? N1 Cu1 Cu2 N88 -96.7(8) . . . . ? N18 Cu1 Cu2 N88 101.0(8) . . . . ? N2 Cu1 Cu2 N88 97.8(8) . . . . ? O21 Cu1 Cu2 N88 -172.2(7) . . . . ? N40 Cu1 Cu2 N88 -13.5(7) . . . . ? N20 Cu1 Cu2 N88 158.6(7) . . . . ? N38 Cu1 Cu2 N3 -46.3(5) . . . . ? N1 Cu1 Cu2 N3 -92.5(5) . . . . ? N18 Cu1 Cu2 N3 105.3(6) . . . . ? N2 Cu1 Cu2 N3 102.1(5) . . . . ? O21 Cu1 Cu2 N3 -167.9(4) . . . . ? N40 Cu1 Cu2 N3 -9.2(4) . . . . ? N20 Cu1 Cu2 N3 162.9(4) . . . . ? N38 Cu1 Cu2 N4 119.0(7) . . . . ? N1 Cu1 Cu2 N4 72.8(7) . . . . ? N18 Cu1 Cu2 N4 -89.5(7) . . . . ? N2 Cu1 Cu2 N4 -92.6(7) . . . . ? O21 Cu1 Cu2 N4 -2.6(6) . . . . ? N40 Cu1 Cu2 N4 156.0(6) . . . . ? N20 Cu1 Cu2 N4 -31.9(6) . . . . ? N38 Cu1 Cu2 N90 18.0(4) . . . . ? N1 Cu1 Cu2 N90 -28.2(4) . . . . ? N18 Cu1 Cu2 N90 169.5(5) . . . . ? N2 Cu1 Cu2 N90 166.4(4) . . . . ? O21 Cu1 Cu2 N90 -103.6(3) . . . . ? N40 Cu1 Cu2 N90 55.1(3) . . . . ? N20 Cu1 Cu2 N90 -132.8(3) . . . . ? N38 Cu1 Cu2 N70 -171.4(4) . . . . ? N1 Cu1 Cu2 N70 142.4(4) . . . . ? N18 Cu1 Cu2 N70 -19.9(5) . . . . ? N2 Cu1 Cu2 N70 -23.1(4) . . . . ? O21 Cu1 Cu2 N70 67.0(2) . . . . ? N40 Cu1 Cu2 N70 -134.4(2) . . . . ? N20 Cu1 Cu2 N70 37.7(3) . . . . ? N68 Cu2 N3 C51 162(3) . . . . ? N88 Cu2 N3 C51 -3.7(11) . . . . ? N4 Cu2 N3 C51 -178.7(11) . . . . ? N90 Cu2 N3 C51 -58.7(11) . . . . ? N70 Cu2 N3 C51 97.5(11) . . . . ? Cu1 Cu2 N3 C51 -6.1(12) . . . . ? N68 Cu2 N3 C55 -24(4) . . . . ? N88 Cu2 N3 C55 170.4(8) . . . . ? N4 Cu2 N3 C55 -4.6(7) . . . . ? N90 Cu2 N3 C55 115.4(8) . . . . ? N70 Cu2 N3 C55 -88.4(8) . . . . ? Cu1 Cu2 N3 C55 168.0(6) . . . . ? N68 Cu2 N4 C56 -177.8(8) . . . . ? N88 Cu2 N4 C56 -41(4) . . . . ? N3 Cu2 N4 C56 4.6(8) . . . . ? N90 Cu2 N4 C56 -79.5(8) . . . . ? N70 Cu2 N4 C56 129.6(8) . . . . ? Cu1 Cu2 N4 C56 -163.7(6) . . . . ? N68 Cu2 N4 C60 -0.3(11) . . . . ? N88 Cu2 N4 C60 136(4) . . . . ? N3 Cu2 N4 C60 -177.9(11) . . . . ? N90 Cu2 N4 C60 98.0(11) . . . . ? N70 Cu2 N4 C60 -52.9(10) . . . . ? Cu1 Cu2 N4 C60 13.8(14) . . . . ? N88 Cu2 N68 C69 93.5(8) . . . . ? N3 Cu2 N68 C69 -72(3) . . . . ? N4 Cu2 N68 C69 -91.3(7) . . . . ? N90 Cu2 N68 C69 148.7(7) . . . . ? N70 Cu2 N68 C69 -2.8(6) . . . . ? Cu1 Cu2 N68 C69 96.9(7) . . . . ? N88 Cu2 N68 C67 -86.4(9) . . . . ? N3 Cu2 N68 C67 108(3) . . . . ? N4 Cu2 N68 C67 88.8(8) . . . . ? N90 Cu2 N68 C67 -31.1(8) . . . . ? N70 Cu2 N68 C67 177.3(9) . . . . ? Cu1 Cu2 N68 C67 -83.0(8) . . . . ? O72 S71 N70 C69 -176.4(8) . . . . ? O71 S71 N70 C69 55.5(10) . . . . ? C72 S71 N70 C69 -62.2(10) . . . . ? O72 S71 N70 Cu2 20(2) . . . . ? O71 S71 N70 Cu2 -108(2) . . . . ? C72 S71 N70 Cu2 134.6(19) . . . . ? N68 Cu2 N70 C69 2.6(6) . . . . ? N88 Cu2 N70 C69 -85.8(6) . . . . ? N3 Cu2 N70 C69 174.3(7) . . . . ? N4 Cu2 N70 C69 95.4(7) . . . . ? N90 Cu2 N70 C69 -44.0(7) . . . . ? Cu1 Cu2 N70 C69 -56.9(5) . . . . ? N68 Cu2 N70 S71 167(2) . . . . ? N88 Cu2 N70 S71 79(2) . . . . ? N3 Cu2 N70 S71 -21(2) . . . . ? N4 Cu2 N70 S71 -100(2) . . . . ? N90 Cu2 N70 S71 121(2) . . . . ? Cu1 Cu2 N70 S71 108(2) . . . . ? N68 Cu2 N88 C89 94.8(7) . . . . ? N3 Cu2 N88 C89 -87.1(7) . . . . ? N4 Cu2 N88 C89 -42(4) . . . . ? N90 Cu2 N88 C89 -0.8(6) . . . . ? N70 Cu2 N88 C89 147.4(7) . . . . ? Cu1 Cu2 N88 C89 89.5(8) . . . . ? N68 Cu2 N88 C87 -81.8(10) . . . . ? N3 Cu2 N88 C87 96.4(10) . . . . ? N4 Cu2 N88 C87 141(4) . . . . ? N90 Cu2 N88 C87 -177.3(11) . . . . ? N70 Cu2 N88 C87 -29.1(10) . . . . ? Cu1 Cu2 N88 C87 -87.0(11) . . . . ? O91 S91 N90 C89 162.7(8) . . . . ? O92 S91 N90 C89 31.4(10) . . . . ? C92 S91 N90 C89 -83.8(10) . . . . ? O91 S91 N90 Cu2 -38.5(14) . . . . ? O92 S91 N90 Cu2 -169.8(12) . . . . ? C92 S91 N90 Cu2 75.0(15) . . . . ? N68 Cu2 N90 C89 -88.4(6) . . . . ? N88 Cu2 N90 C89 0.7(6) . . . . ? N3 Cu2 N90 C89 96.3(7) . . . . ? N4 Cu2 N90 C89 175.5(7) . . . . ? N70 Cu2 N90 C89 -52.9(7) . . . . ? Cu1 Cu2 N90 C89 -38.6(5) . . . . ? N68 Cu2 N90 S91 110.0(13) . . . . ? N88 Cu2 N90 S91 -160.9(15) . . . . ? N3 Cu2 N90 S91 -65.3(14) . . . . ? N4 Cu2 N90 S91 13.9(15) . . . . ? N70 Cu2 N90 S91 145.5(12) . . . . ? Cu1 Cu2 N90 S91 159.8(14) . . . . ? C55 N3 C51 C52 -1(2) . . . . ? Cu2 N3 C51 C52 172.7(10) . . . . ? N3 C51 C52 C53 1(2) . . . . ? C51 C52 C53 C54 -2(3) . . . . ? C52 C53 C54 C55 4(3) . . . . ? C51 N3 C55 C54 2.1(16) . . . . ? Cu2 N3 C55 C54 -172.3(7) . . . . ? C51 N3 C55 C56 178.4(11) . . . . ? Cu2 N3 C55 C56 4.0(12) . . . . ? C53 C54 C55 N3 -3.6(18) . . . . ? C53 C54 C55 C56 -179.2(13) . . . . ? C60 N4 C56 C57 5.1(17) . . . . ? Cu2 N4 C56 C57 -177.1(9) . . . . ? C60 N4 C56 C55 178.4(10) . . . . ? Cu2 N4 C56 C55 -3.8(12) . . . . ? N3 C55 C56 N4 -0.1(15) . . . . ? C54 C55 C56 N4 175.6(10) . . . . ? N3 C55 C56 C57 173.6(10) . . . . ? C54 C55 C56 C57 -10.6(18) . . . . ? N4 C56 C57 C58 -3.3(19) . . . . ? C55 C56 C57 C58 -176.5(12) . . . . ? C56 C57 C58 C59 1(2) . . . . ? C57 C58 C59 C60 -1(2) . . . . ? C56 N4 C60 C59 -4.7(18) . . . . ? Cu2 N4 C60 C59 177.8(9) . . . . ? C58 C59 C60 N4 3(2) . . . . ? C69 S61 C62 C63 -175.6(9) . . . . ? C69 S61 C62 C67 2.0(7) . . . . ? C67 C62 C63 C64 0.9(14) . . . . ? S61 C62 C63 C64 178.3(7) . . . . ? C62 C63 C64 C65 0.4(14) . . . . ? C62 C63 C64 C78 -178.6(9) . . . . ? C63 C64 C65 C66 0.0(14) . . . . ? C78 C64 C65 C66 179.0(9) . . . . ? C63 C64 C65 C79 177.2(9) . . . . ? C78 C64 C65 C79 -3.8(14) . . . . ? C64 C65 C66 C67 -1.8(15) . . . . ? C79 C65 C66 C67 -179.0(8) . . . . ? C65 C66 C67 C62 3.1(14) . . . . ? C65 C66 C67 N68 -175.8(8) . . . . ? C63 C62 C67 C66 -2.6(13) . . . . ? S61 C62 C67 C66 179.5(7) . . . . ? C63 C62 C67 N68 176.4(8) . . . . ? S61 C62 C67 N68 -1.5(10) . . . . ? C69 N68 C67 C66 178.7(9) . . . . ? Cu2 N68 C67 C66 -1.4(14) . . . . ? C69 N68 C67 C62 -0.2(11) . . . . ? Cu2 N68 C67 C62 179.7(6) . . . . ? C67 N68 C69 N70 -174.6(8) . . . . ? Cu2 N68 C69 N70 5.5(12) . . . . ? C67 N68 C69 S61 1.9(10) . . . . ? Cu2 N68 C69 S61 -178.1(4) . . . . ? S71 N70 C69 N68 -179.4(7) . . . . ? Cu2 N70 C69 N68 -3.5(8) . . . . ? S71 N70 C69 S61 4.7(13) . . . . ? Cu2 N70 C69 S61 -179.5(8) . . . . ? C62 S61 C69 N68 -2.3(8) . . . . ? C62 S61 C69 N70 173.8(9) . . . . ? O72 S71 C72 C73 -112.6(9) . . . . ? O71 S71 C72 C73 13.2(10) . . . . ? N70 S71 C72 C73 134.7(9) . . . . ? O72 S71 C72 C77 69.0(9) . . . . ? O71 S71 C72 C77 -165.2(8) . . . . ? N70 S71 C72 C77 -43.7(9) . . . . ? C77 C72 C73 C74 -4.4(16) . . . . ? S71 C72 C73 C74 177.2(9) . . . . ? C72 C73 C74 C75 5.2(19) . . . . ? C73 C74 C75 C76 -2.8(17) . . . . ? C73 C74 C75 C80 179.3(11) . . . . ? C74 C75 C76 C77 -0.3(17) . . . . ? C80 C75 C76 C77 177.6(11) . . . . ? C75 C76 C77 C72 0.9(17) . . . . ? C73 C72 C77 C76 1.4(15) . . . . ? S71 C72 C77 C76 179.8(8) . . . . ? C89 S81 C82 C87 -0.5(8) . . . . ? C89 S81 C82 C83 177.7(11) . . . . ? C87 C82 C83 C84 -1.9(18) . . . . ? S81 C82 C83 C84 -179.9(9) . . . . ? C82 C83 C84 C85 1.7(19) . . . . ? C82 C83 C84 C98 178.0(10) . . . . ? C83 C84 C85 C86 -2.1(19) . . . . ? C98 C84 C85 C86 -178.4(10) . . . . ? C83 C84 C85 C99 -179.2(11) . . . . ? C98 C84 C85 C99 4.5(18) . . . . ? C84 C85 C86 C87 2.5(18) . . . . ? C99 C85 C86 C87 179.6(10) . . . . ? C83 C82 C87 C86 2.4(16) . . . . ? S81 C82 C87 C86 -179.4(8) . . . . ? C83 C82 C87 N88 -177.9(10) . . . . ? S81 C82 C87 N88 0.4(11) . . . . ? C85 C86 C87 C82 -2.6(16) . . . . ? C85 C86 C87 N88 177.7(10) . . . . ? C89 N88 C87 C82 0.0(12) . . . . ? Cu2 N88 C87 C82 176.5(7) . . . . ? C89 N88 C87 C86 179.7(10) . . . . ? Cu2 N88 C87 C86 -3.7(16) . . . . ? C87 N88 C89 N90 178.9(8) . . . . ? Cu2 N88 C89 N90 1.4(12) . . . . ? C87 N88 C89 S81 -0.4(11) . . . . ? Cu2 N88 C89 S81 -177.9(4) . . . . ? S91 N90 C89 N88 171.8(7) . . . . ? Cu2 N90 C89 N88 -1.0(8) . . . . ? S91 N90 C89 S81 -8.9(14) . . . . ? Cu2 N90 C89 S81 178.2(9) . . . . ? C82 S81 C89 N88 0.5(8) . . . . ? C82 S81 C89 N90 -178.7(10) . . . . ? O91 S91 C92 C97 -143.1(10) . . . . ? O92 S91 C92 C97 -15.7(11) . . . . ? N90 S91 C92 C97 103.1(11) . . . . ? O91 S91 C92 C93 39.1(11) . . . . ? O92 S91 C92 C93 166.5(9) . . . . ? N90 S91 C92 C93 -74.7(11) . . . . ? C97 C92 C93 C94 -1.2(17) . . . . ? S91 C92 C93 C94 176.7(9) . . . . ? C92 C93 C94 C95 2(2) . . . . ? C93 C94 C95 C96 -2(2) . . . . ? C93 C94 C95 C100 179.4(10) . . . . ? C94 C95 C96 C97 1(2) . . . . ? C100 C95 C96 C97 179.4(11) . . . . ? C93 C92 C97 C96 0.2(18) . . . . ? S91 C92 C97 C96 -177.7(10) . . . . ? C95 C96 C97 C92 0(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1A O72 0.97 1.96 2.756(12) 137.5 1_545 O1 H1B O92 0.85 2.09 2.871(11) 153.1 . _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 89.89 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.459 _refine_diff_density_min -0.392 _refine_diff_density_rms 0.063 _database_code_depnum_ccdc_archive 'CCDC 923557' ####################################################################### # # 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_09acmg13 #TrackingRef 'alzuet_dalton.ccd' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H34 Cu N6 O4 S4' _chemical_formula_sum 'C40 H34 Cu N6 O4 S4' _chemical_formula_weight 854.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 2/c' _symmetry_Int_Tables_number 15 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 23.234(5) _cell_length_b 16.908(5) _cell_length_c 22.099(5) _cell_angle_alpha 90.00 _cell_angle_beta 116.953(5) _cell_angle_gamma 90.00 _cell_volume 7738(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5532 _cell_measurement_theta_min 0.999 _cell_measurement_theta_max 70.076 _exptl_crystal_description prism _exptl_crystal_colour 'light grey' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.467 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3528 _exptl_absorpt_coefficient_mu 3.228 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD2000 _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 10149 _diffrn_reflns_av_R_equivalents 0.0384 _diffrn_reflns_av_sigmaI/netI 0.0447 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.37 _diffrn_reflns_theta_max 89.23 _reflns_number_total 8852 _reflns_number_gt 8328 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2009)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0944P)^2^+1.8348P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00018(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8852 _refine_ls_number_parameters 498 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0800 _refine_ls_R_factor_gt 0.0518 _refine_ls_wR_factor_ref 0.1615 _refine_ls_wR_factor_gt 0.1391 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.0000 0.03050(4) 0.2500 0.0594(3) Uani 1 2 d S . . S11 S 0.15291(5) -0.10677(7) 0.40970(6) 0.0794(4) Uani 1 1 d . . . S21 S 0.18810(5) -0.04142(7) 0.28950(6) 0.0764(4) Uani 1 1 d . . . O21 O 0.23177(13) -0.09122(18) 0.34331(18) 0.0894(9) Uani 1 1 d . . . O22 O 0.18383(14) -0.0533(2) 0.22308(17) 0.1014(11) Uani 1 1 d . . . N1 N -0.04565(15) 0.1220(2) 0.18711(18) 0.0661(9) Uani 1 1 d . . . N18 N 0.04310(14) -0.04762(17) 0.32313(16) 0.0606(8) Uani 1 1 d . . . N20 N 0.11580(14) -0.0443(2) 0.28027(18) 0.0714(9) Uani 1 1 d . . . C1 C -0.0935(2) 0.1176(3) 0.1239(2) 0.0753(12) Uani 1 1 d . . . H1 H -0.1077 0.0679 0.1051 0.090 Uiso 1 1 d R . . C2 C -0.1229(2) 0.1835(3) 0.0851(2) 0.0831(13) Uani 1 1 d . . . H2 H -0.1564 0.1782 0.0414 0.100 Uiso 1 1 d R . . C3 C -0.1016(3) 0.2567(3) 0.1125(3) 0.0887(15) Uani 1 1 d . . . H3 H -0.1201 0.3021 0.0873 0.106 Uiso 1 1 d R . . C4 C -0.0527(2) 0.2629(3) 0.1777(3) 0.0829(14) Uani 1 1 d . . . H4 H -0.0380 0.3124 0.1968 0.099 Uiso 1 1 d R . . C5 C -0.02548(18) 0.1951(3) 0.2146(2) 0.0687(11) Uani 1 1 d . . . C12 C 0.08949(19) -0.1051(2) 0.4314(2) 0.0689(11) Uani 1 1 d . . . C13 C 0.0880(2) -0.1319(3) 0.4898(2) 0.0817(13) Uani 1 1 d . . . H13 H 0.1249 -0.1543 0.5243 0.098 Uiso 1 1 d R . . C14 C 0.0325(2) -0.1259(3) 0.4974(2) 0.0791(12) Uani 1 1 d . . . C15 C -0.0230(2) -0.0919(3) 0.4455(2) 0.0729(11) Uani 1 1 d . . . C16 C -0.02149(19) -0.0642(2) 0.3866(2) 0.0666(10) Uani 1 1 d . . . H16 H -0.0580 -0.0409 0.3525 0.080 Uiso 1 1 d R . . C17 C 0.03432(18) -0.0715(2) 0.3791(2) 0.0607(9) Uani 1 1 d . . . C19 C 0.10253(18) -0.0635(2) 0.3307(2) 0.0643(10) Uani 1 1 d . . . C22 C 0.21012(19) 0.0571(3) 0.3126(2) 0.0695(11) Uani 1 1 d . . . C23 C 0.1810(3) 0.1152(4) 0.2649(3) 0.0986(15) Uani 1 1 d . . . H23 H 0.1528 0.1012 0.2205 0.118 Uiso 1 1 d R . . C24 C 0.1928(3) 0.1913(4) 0.2815(4) 0.1154(19) Uani 1 1 d . . . H24 H 0.1720 0.2298 0.2488 0.138 Uiso 1 1 d R . . C25 C 0.2349(3) 0.2136(3) 0.3460(4) 0.1006(17) Uani 1 1 d . . . H25 H 0.2434 0.2668 0.3570 0.121 Uiso 1 1 d R . . C26 C 0.2647(2) 0.1562(3) 0.3945(3) 0.0950(15) Uani 1 1 d . . . H26 H 0.2934 0.1708 0.4385 0.114 Uiso 1 1 d R . . C27 C 0.2524(2) 0.0770(3) 0.3782(3) 0.0783(12) Uani 1 1 d . . . H27 H 0.2723 0.0382 0.4108 0.094 Uiso 1 1 d R . . C28 C 0.0322(3) -0.1562(3) 0.5617(3) 0.1078(17) Uani 1 1 d . . . H28A H 0.0749 -0.1727 0.5931 0.162 Uiso 1 1 d R . . H28B H 0.0031 -0.2002 0.5510 0.162 Uiso 1 1 d R . . H28C H 0.0183 -0.1148 0.5818 0.162 Uiso 1 1 d R . . C29 C -0.0849(2) -0.0850(3) 0.4516(3) 0.0948(15) Uani 1 1 d . . . H29A H -0.1168 -0.0584 0.4124 0.142 Uiso 1 1 d R . . H29B H -0.0771 -0.0552 0.4916 0.142 Uiso 1 1 d R . . H29C H -0.1001 -0.1368 0.4548 0.142 Uiso 1 1 d R . . Cu2 Cu 0.5000 0.02703(4) 0.2500 0.0599(3) Uani 1 2 d S . . S31 S 0.33608(5) -0.09833(7) 0.25216(6) 0.0741(3) Uani 1 1 d . . . S41 S 0.31007(5) -0.04265(7) 0.09976(6) 0.0793(4) Uani 1 1 d . . . O41 O 0.26466(14) -0.09315(18) 0.10955(18) 0.0952(10) Uani 1 1 d . . . O42 O 0.31767(16) -0.0554(2) 0.03977(17) 0.1094(12) Uani 1 1 d . . . N2 N 0.54445(15) 0.11908(19) 0.22927(16) 0.0653(8) Uani 1 1 d . . . N38 N 0.45081(14) -0.05045(18) 0.27551(16) 0.0600(8) Uani 1 1 d . . . N40 N 0.38091(15) -0.0448(2) 0.16185(19) 0.0739(10) Uani 1 1 d . . . C6 C 0.52530(18) 0.1922(2) 0.2383(2) 0.0662(10) Uani 1 1 d . . . C7 C 0.5518(2) 0.2601(3) 0.2269(2) 0.0837(13) Uani 1 1 d . . . H7 H 0.5376 0.3094 0.2332 0.100 Uiso 1 1 d R . . C8 C 0.5992(2) 0.2545(3) 0.2060(2) 0.0860(13) Uani 1 1 d . . . H8 H 0.6171 0.2997 0.1975 0.103 Uiso 1 1 d R . . C9 C 0.6194(2) 0.1814(3) 0.1982(2) 0.0823(13) Uani 1 1 d . . . H9 H 0.6522 0.1762 0.1853 0.099 Uiso 1 1 d R . . C10 C 0.5910(2) 0.1151(3) 0.2094(2) 0.0771(12) Uani 1 1 d . . . H10 H 0.6048 0.0655 0.2030 0.092 Uiso 1 1 d R . . C32 C 0.39689(18) -0.1000(2) 0.3353(2) 0.0665(11) Uani 1 1 d . . . C33 C 0.3941(2) -0.1241(2) 0.3940(2) 0.0753(12) Uani 1 1 d . . . H33 H 0.3553 -0.1420 0.3917 0.090 Uiso 1 1 d R . . C34 C 0.4485(2) -0.1217(3) 0.4554(2) 0.0758(12) Uani 1 1 d . . . C35 C 0.5074(2) -0.0946(2) 0.4591(2) 0.0714(11) Uani 1 1 d . . . C36 C 0.50992(18) -0.0704(2) 0.4003(2) 0.0654(10) Uani 1 1 d . . . H36 H 0.5487 -0.0525 0.4025 0.078 Uiso 1 1 d R . . C37 C 0.45535(18) -0.0726(2) 0.3386(2) 0.0603(10) Uani 1 1 d . . . C39 C 0.39197(18) -0.0624(2) 0.2251(2) 0.0650(10) Uani 1 1 d . . . C42 C 0.28691(19) 0.0555(3) 0.1004(2) 0.0703(11) Uani 1 1 d . . . C43 C 0.2538(2) 0.0781(3) 0.1355(2) 0.0846(13) Uani 1 1 d . . . H43 H 0.2386 0.0406 0.1556 0.102 Uiso 1 1 d R . . C44 C 0.2434(2) 0.1592(4) 0.1405(3) 0.0998(16) Uani 1 1 d . . . H44 H 0.2208 0.1763 0.1637 0.120 Uiso 1 1 d R . . C45 C 0.2669(3) 0.2129(3) 0.1109(3) 0.1094(18) Uani 1 1 d . . . H45 H 0.2623 0.2668 0.1159 0.131 Uiso 1 1 d R . . C46 C 0.2965(3) 0.1876(4) 0.0744(4) 0.137(2) Uani 1 1 d . . . H46 H 0.3098 0.2244 0.0520 0.164 Uiso 1 1 d R . . C47 C 0.3073(3) 0.1108(3) 0.0695(3) 0.1094(18) Uani 1 1 d . . . H47 H 0.3288 0.0950 0.0450 0.131 Uiso 1 1 d R . . C48 C 0.4448(3) -0.1478(3) 0.5193(3) 0.1011(16) Uani 1 1 d . . . H48A H 0.4766 -0.1880 0.5418 0.152 Uiso 1 1 d R . . H48B H 0.4026 -0.1686 0.5074 0.152 Uiso 1 1 d R . . H48C H 0.4529 -0.1033 0.5491 0.152 Uiso 1 1 d R . . C49 C 0.5676(2) -0.0929(3) 0.5256(2) 0.0944(15) Uani 1 1 d . . . H49A H 0.5608 -0.0599 0.5570 0.142 Uiso 1 1 d R . . H49B H 0.6027 -0.0723 0.5187 0.142 Uiso 1 1 d R . . H49C H 0.5778 -0.1456 0.5435 0.142 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0555(4) 0.0637(5) 0.0597(5) 0.000 0.0267(4) 0.000 S11 0.0636(6) 0.0969(9) 0.0730(8) 0.0082(6) 0.0269(6) 0.0198(5) S21 0.0555(6) 0.0967(8) 0.0803(9) -0.0050(6) 0.0336(6) 0.0005(5) O21 0.0577(16) 0.091(2) 0.115(3) 0.0087(19) 0.0362(18) 0.0103(15) O22 0.0739(19) 0.153(3) 0.090(3) -0.037(2) 0.0486(19) -0.0136(19) N1 0.065(2) 0.072(2) 0.069(2) 0.0028(18) 0.0372(19) 0.0011(16) N18 0.0529(17) 0.068(2) 0.060(2) -0.0016(16) 0.0253(16) 0.0006(14) N20 0.0497(18) 0.100(3) 0.066(2) 0.0018(19) 0.0278(17) -0.0001(16) C1 0.074(3) 0.086(3) 0.067(3) 0.007(2) 0.033(3) 0.002(2) C2 0.083(3) 0.091(4) 0.080(3) 0.026(3) 0.041(3) 0.020(3) C3 0.097(4) 0.082(4) 0.102(4) 0.030(3) 0.058(3) 0.025(3) C4 0.092(3) 0.066(3) 0.107(4) 0.015(3) 0.059(3) 0.012(2) C5 0.070(3) 0.067(3) 0.084(3) 0.003(2) 0.048(2) 0.003(2) C12 0.066(2) 0.077(3) 0.056(3) 0.004(2) 0.022(2) 0.0139(19) C13 0.088(3) 0.091(3) 0.059(3) 0.011(2) 0.028(3) 0.021(2) C14 0.091(3) 0.085(3) 0.065(3) 0.003(2) 0.039(3) 0.010(2) C15 0.078(3) 0.082(3) 0.062(3) 0.003(2) 0.035(2) 0.002(2) C16 0.061(2) 0.081(3) 0.054(3) 0.000(2) 0.022(2) 0.0050(19) C17 0.058(2) 0.065(2) 0.055(3) -0.0033(19) 0.023(2) 0.0003(18) C19 0.055(2) 0.072(3) 0.065(3) -0.005(2) 0.026(2) 0.0013(18) C22 0.059(2) 0.086(3) 0.069(3) 0.014(2) 0.033(2) 0.006(2) C23 0.109(4) 0.104(4) 0.075(4) 0.013(3) 0.035(3) 0.016(3) C24 0.142(5) 0.101(5) 0.107(5) 0.025(4) 0.061(5) 0.025(4) C25 0.108(4) 0.075(3) 0.139(6) -0.002(4) 0.074(4) 0.004(3) C26 0.078(3) 0.101(4) 0.103(4) -0.015(3) 0.038(3) -0.003(3) C27 0.065(3) 0.082(3) 0.080(4) 0.004(3) 0.026(3) 0.002(2) C28 0.129(4) 0.129(4) 0.078(4) 0.024(3) 0.058(3) 0.027(3) C29 0.090(3) 0.122(4) 0.088(4) 0.008(3) 0.054(3) 0.004(3) Cu2 0.0575(5) 0.0643(5) 0.0596(6) 0.000 0.0280(4) 0.000 S31 0.0571(6) 0.0832(7) 0.0804(8) -0.0020(6) 0.0298(6) -0.0064(5) S41 0.0687(7) 0.0938(8) 0.0662(8) -0.0032(6) 0.0227(6) 0.0091(6) O41 0.0720(19) 0.085(2) 0.108(3) 0.0032(18) 0.0229(18) -0.0116(16) O42 0.102(2) 0.154(3) 0.065(2) -0.016(2) 0.0308(19) 0.026(2) N2 0.0666(19) 0.073(2) 0.055(2) 0.0003(16) 0.0261(17) -0.0020(16) N38 0.0528(18) 0.067(2) 0.057(2) -0.0015(16) 0.0226(16) 0.0033(14) N40 0.0553(19) 0.099(3) 0.062(2) 0.0056(19) 0.0220(18) 0.0114(17) C6 0.071(3) 0.067(3) 0.051(3) 0.002(2) 0.020(2) -0.004(2) C7 0.102(3) 0.064(3) 0.082(4) -0.001(2) 0.039(3) -0.009(2) C8 0.097(3) 0.078(3) 0.079(4) 0.007(3) 0.037(3) -0.015(3) C9 0.083(3) 0.093(4) 0.075(3) 0.000(3) 0.039(3) -0.017(3) C10 0.078(3) 0.079(3) 0.078(3) 0.001(2) 0.039(3) -0.007(2) C32 0.059(2) 0.064(2) 0.081(3) 0.003(2) 0.035(2) 0.0009(18) C33 0.073(3) 0.078(3) 0.090(4) 0.005(3) 0.050(3) -0.002(2) C34 0.079(3) 0.082(3) 0.076(3) 0.006(2) 0.044(3) 0.004(2) C35 0.072(3) 0.079(3) 0.066(3) 0.007(2) 0.034(2) 0.010(2) C36 0.054(2) 0.076(3) 0.067(3) 0.001(2) 0.029(2) 0.0014(19) C37 0.060(2) 0.062(2) 0.063(3) 0.0026(19) 0.031(2) 0.0030(18) C39 0.059(2) 0.068(3) 0.067(3) -0.002(2) 0.027(2) 0.0059(18) C42 0.060(2) 0.083(3) 0.063(3) 0.009(2) 0.023(2) -0.002(2) C43 0.078(3) 0.100(4) 0.078(3) 0.009(3) 0.038(3) 0.014(3) C44 0.095(4) 0.107(4) 0.093(4) -0.001(3) 0.038(3) 0.019(3) C45 0.108(4) 0.078(4) 0.126(5) -0.007(3) 0.038(4) 0.001(3) C46 0.165(6) 0.097(5) 0.185(7) 0.002(5) 0.112(6) -0.016(4) C47 0.119(4) 0.092(4) 0.142(5) 0.017(4) 0.081(4) 0.000(3) C48 0.120(4) 0.115(4) 0.093(4) 0.011(3) 0.071(4) 0.002(3) C49 0.081(3) 0.127(4) 0.071(3) 0.010(3) 0.031(3) 0.010(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N18 1.973(3) 2 y Cu1 N18 1.973(3) . y Cu1 N1 2.028(3) 2 y Cu1 N1 2.028(3) . y Cu1 N20 2.767(3) 2 y Cu1 N20 2.767(3) . y Cu1 Cu2 11.617(3) . y S11 C12 1.744(4) . ? S11 C19 1.760(4) . ? S21 O21 1.435(3) . ? S21 O22 1.440(3) . ? S21 N20 1.598(3) . ? S21 C22 1.749(5) . ? N1 C1 1.336(5) . ? N1 C5 1.364(5) . ? N18 C19 1.341(4) . ? N18 C17 1.400(5) . ? N20 C19 1.325(5) . ? C1 C2 1.384(6) . ? C1 H1 0.9300 . ? C2 C3 1.368(6) . ? C2 H2 0.9300 . ? C3 C4 1.376(7) . ? C3 H3 0.9300 . ? C4 C5 1.382(6) . ? C4 H4 0.9300 . ? C5 C5 1.473(8) 2 ? C12 C13 1.383(6) . ? C12 C17 1.400(5) . ? C13 C14 1.378(6) . ? C13 H13 0.9300 . ? C14 C15 1.402(6) . ? C14 C28 1.514(6) . ? C15 C16 1.397(5) . ? C15 C29 1.509(6) . ? C16 C17 1.386(5) . ? C16 H16 0.9300 . ? C22 C27 1.374(6) . ? C22 C23 1.374(6) . ? C23 C24 1.332(8) . ? C23 H23 0.9300 . ? C24 C25 1.366(8) . ? C24 H24 0.9300 . ? C25 C26 1.377(7) . ? C25 H25 0.9300 . ? C26 C27 1.381(7) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? Cu2 N38 1.981(3) . y Cu2 N38 1.981(3) 2_655 y Cu2 N2 2.032(3) . y Cu2 N2 2.032(3) 2_655 y Cu2 N40 2.835(3) . y Cu2 N40 2.835(3) 2_655 y S31 C32 1.737(4) . ? S31 C39 1.766(4) . ? S41 O42 1.431(3) . ? S41 O41 1.448(3) . ? S41 N40 1.595(3) . ? S41 C42 1.746(4) . ? N2 C10 1.341(5) . ? N2 C6 1.360(5) . ? N38 C39 1.331(5) . ? N38 C37 1.400(5) . ? N40 C39 1.335(5) . ? C6 C7 1.378(5) . ? C6 C6 1.483(7) 2_655 ? C7 C8 1.377(6) . ? C7 H7 0.9300 . ? C8 C9 1.360(6) . ? C8 H8 0.9300 . ? C9 C10 1.380(6) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C32 C33 1.389(5) . ? C32 C37 1.405(5) . ? C33 C34 1.373(6) . ? C33 H33 0.9300 . ? C34 C35 1.411(6) . ? C34 C48 1.518(6) . ? C35 C36 1.389(5) . ? C35 C49 1.501(6) . ? C36 C37 1.379(5) . ? C36 H36 0.9300 . ? C42 C47 1.363(6) . ? C42 C43 1.372(6) . ? C43 C44 1.406(7) . ? C43 H43 0.9300 . ? C44 C45 1.369(7) . ? C44 H44 0.9300 . ? C45 C46 1.346(8) . ? C45 H45 0.9300 . ? C46 C47 1.335(8) . ? C46 H46 0.9300 . ? C47 H47 0.9300 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 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 N18 Cu1 N18 95.94(18) 2 . y N18 Cu1 N1 170.28(13) 2 2 y N18 Cu1 N1 92.04(14) . 2 y N18 Cu1 N1 92.04(14) 2 . y N18 Cu1 N1 170.28(13) . . y N1 Cu1 N1 80.6(2) 2 . y N18 Cu1 N20 54.47(11) 2 2 y N18 Cu1 N20 88.21(11) . 2 y N1 Cu1 N20 131.58(11) 2 2 y N1 Cu1 N20 91.94(12) . 2 y N18 Cu1 N20 88.21(11) 2 . y N18 Cu1 N20 54.47(11) . . y N1 Cu1 N20 91.94(12) 2 . y N1 Cu1 N20 131.58(11) . . y N20 Cu1 N20 125.58(14) 2 . y N18 Cu1 Cu2 97.64(8) 2 . ? N18 Cu1 Cu2 81.97(8) . . ? N1 Cu1 Cu2 77.96(8) 2 . ? N1 Cu1 Cu2 102.49(8) . . ? N20 Cu1 Cu2 149.37(7) 2 . ? N20 Cu1 Cu2 30.10(7) . . ? C12 S11 C19 90.04(18) . . ? O21 S21 O22 117.3(2) . . ? O21 S21 N20 113.28(18) . . ? O22 S21 N20 106.44(18) . . ? O21 S21 C22 108.3(2) . . ? O22 S21 C22 107.8(2) . . ? N20 S21 C22 102.59(18) . . ? C1 N1 C5 118.1(4) . . ? C1 N1 Cu1 127.1(3) . . ? C5 N1 Cu1 114.8(3) . . ? C19 N18 C17 112.7(3) . . ? C19 N18 Cu1 110.4(3) . . ? C17 N18 Cu1 133.9(2) . . ? C19 N20 S21 122.1(3) . . ? C19 N20 Cu1 75.2(2) . . ? S21 N20 Cu1 150.1(2) . . ? N1 C1 C2 123.2(5) . . ? N1 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? C3 C2 C1 118.4(5) . . ? C3 C2 H2 120.8 . . ? C1 C2 H2 120.8 . . ? C2 C3 C4 119.5(5) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C3 C4 C5 119.7(5) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? N1 C5 C4 121.0(4) . . ? N1 C5 C5 114.9(2) . 2 ? C4 C5 C5 124.0(3) . 2 ? C13 C12 C17 120.2(4) . . ? C13 C12 S11 129.2(3) . . ? C17 C12 S11 110.5(3) . . ? C14 C13 C12 120.6(4) . . ? C14 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? C13 C14 C15 119.7(4) . . ? C13 C14 C28 119.5(4) . . ? C15 C14 C28 120.8(4) . . ? C16 C15 C14 119.8(4) . . ? C16 C15 C29 119.0(4) . . ? C14 C15 C29 121.3(4) . . ? C17 C16 C15 120.1(4) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C16 C17 N18 126.9(3) . . ? C16 C17 C12 119.5(4) . . ? N18 C17 C12 113.6(3) . . ? N20 C19 N18 117.7(4) . . ? N20 C19 S11 129.2(3) . . ? N18 C19 S11 113.1(3) . . ? C27 C22 C23 120.1(5) . . ? C27 C22 S21 121.1(3) . . ? C23 C22 S21 118.7(4) . . ? C24 C23 C22 120.7(6) . . ? C24 C23 H23 119.6 . . ? C22 C23 H23 119.6 . . ? C23 C24 C25 121.0(6) . . ? C23 C24 H24 119.5 . . ? C25 C24 H24 119.5 . . ? C24 C25 C26 119.1(5) . . ? C24 C25 H25 120.4 . . ? C26 C25 H25 120.5 . . ? C25 C26 C27 120.5(5) . . ? C25 C26 H26 119.7 . . ? C27 C26 H26 119.7 . . ? C22 C27 C26 118.6(5) . . ? C22 C27 H27 120.7 . . ? C26 C27 H27 120.7 . . ? C14 C28 H28A 109.5 . . ? C14 C28 H28B 109.4 . . ? H28A C28 H28B 109.5 . . ? C14 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C15 C29 H29A 109.5 . . ? C15 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C15 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N38 Cu2 N38 97.20(17) . 2_655 y N38 Cu2 N2 171.33(13) . . y N38 Cu2 N2 91.41(13) 2_655 . y N38 Cu2 N2 91.41(13) . 2_655 y N38 Cu2 N2 171.33(13) 2_655 2_655 y N2 Cu2 N2 80.00(19) . 2_655 y N38 Cu2 N40 53.35(12) . . y N38 Cu2 N40 91.75(11) 2_655 . y N2 Cu2 N40 127.64(12) . . y N2 Cu2 N40 92.60(11) 2_655 . y N38 Cu2 N40 91.75(11) . 2_655 y N38 Cu2 N40 53.35(12) 2_655 2_655 y N2 Cu2 N40 92.60(11) . 2_655 y N2 Cu2 N40 127.64(12) 2_655 2_655 y N40 Cu2 N40 129.29(14) . 2_655 y N38 Cu2 Cu1 45.37(8) . . ? N38 Cu2 Cu1 135.17(8) 2_655 . ? N2 Cu2 Cu1 127.35(9) . . ? N2 Cu2 Cu1 52.09(9) 2_655 . ? N40 Cu2 Cu1 48.52(7) . . ? N40 Cu2 Cu1 131.81(7) 2_655 . ? C32 S31 C39 89.64(19) . . ? O42 S41 O41 117.0(2) . . ? O42 S41 N40 106.32(19) . . ? O41 S41 N40 113.31(19) . . ? O42 S41 C42 108.5(2) . . ? O41 S41 C42 108.12(19) . . ? N40 S41 C42 102.48(19) . . ? C10 N2 C6 117.4(3) . . ? C10 N2 Cu2 127.1(3) . . ? C6 N2 Cu2 115.5(2) . . ? C39 N38 C37 112.2(3) . . ? C39 N38 Cu2 111.6(3) . . ? C37 N38 Cu2 131.9(3) . . ? C39 N40 S41 122.6(3) . . ? C39 N40 Cu2 73.2(2) . . ? S41 N40 Cu2 152.4(2) . . ? N2 C6 C7 121.8(4) . . ? N2 C6 C6 114.5(2) . 2_655 ? C7 C6 C6 123.7(3) . 2_655 ? C8 C7 C6 119.7(4) . . ? C8 C7 H7 120.1 . . ? C6 C7 H7 120.1 . . ? C9 C8 C7 118.7(4) . . ? C9 C8 H8 120.6 . . ? C7 C8 H8 120.6 . . ? C8 C9 C10 119.6(4) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? N2 C10 C9 122.7(4) . . ? N2 C10 H10 118.6 . . ? C9 C10 H10 118.6 . . ? C33 C32 C37 120.0(4) . . ? C33 C32 S31 129.3(3) . . ? C37 C32 S31 110.7(3) . . ? C34 C33 C32 120.2(4) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? C33 C34 C35 120.0(4) . . ? C33 C34 C48 119.7(4) . . ? C35 C34 C48 120.2(4) . . ? C36 C35 C34 119.5(4) . . ? C36 C35 C49 119.7(4) . . ? C34 C35 C49 120.7(4) . . ? C37 C36 C35 120.5(4) . . ? C37 C36 H36 119.8 . . ? C35 C36 H36 119.7 . . ? C36 C37 N38 126.7(3) . . ? C36 C37 C32 119.6(4) . . ? N38 C37 C32 113.7(3) . . ? N38 C39 N40 118.7(4) . . ? N38 C39 S31 113.7(3) . . ? N40 C39 S31 127.5(3) . . ? C47 C42 C43 120.2(5) . . ? C47 C42 S41 118.1(4) . . ? C43 C42 S41 121.5(3) . . ? C42 C43 C44 118.4(5) . . ? C42 C43 H43 120.8 . . ? C44 C43 H43 120.8 . . ? C45 C44 C43 119.4(5) . . ? C45 C44 H44 120.3 . . ? C43 C44 H44 120.3 . . ? C46 C45 C44 119.9(5) . . ? C46 C45 H45 120.1 . . ? C44 C45 H45 120.1 . . ? C47 C46 C45 121.5(6) . . ? C47 C46 H46 119.3 . . ? C45 C46 H46 119.2 . . ? C46 C47 C42 120.5(6) . . ? C46 C47 H47 119.7 . . ? C42 C47 H47 119.7 . . ? C34 C48 H48A 109.5 . . ? C34 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C34 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C35 C49 H49A 109.5 . . ? C35 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C35 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 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 N18 Cu1 N1 C1 8.7(3) 2 . . . ? N18 Cu1 N1 C1 -136.5(7) . . . . ? N1 Cu1 N1 C1 -177.7(4) 2 . . . ? N20 Cu1 N1 C1 -45.8(3) 2 . . . ? N20 Cu1 N1 C1 98.1(3) . . . . ? Cu2 Cu1 N1 C1 107.0(3) . . . . ? N18 Cu1 N1 C5 -173.4(2) 2 . . . ? N18 Cu1 N1 C5 41.4(8) . . . . ? N1 Cu1 N1 C5 0.21(18) 2 . . . ? N20 Cu1 N1 C5 132.1(2) 2 . . . ? N20 Cu1 N1 C5 -84.0(3) . . . . ? Cu2 Cu1 N1 C5 -75.1(2) . . . . ? N18 Cu1 N18 C19 92.7(3) 2 . . . ? N1 Cu1 N18 C19 -81.8(3) 2 . . . ? N1 Cu1 N18 C19 -122.3(7) . . . . ? N20 Cu1 N18 C19 146.7(3) 2 . . . ? N20 Cu1 N18 C19 9.2(2) . . . . ? Cu2 Cu1 N18 C19 -4.2(2) . . . . ? N18 Cu1 N18 C17 -109.2(4) 2 . . . ? N1 Cu1 N18 C17 76.4(3) 2 . . . ? N1 Cu1 N18 C17 35.9(9) . . . . ? N20 Cu1 N18 C17 -55.2(3) 2 . . . ? N20 Cu1 N18 C17 167.3(4) . . . . ? Cu2 Cu1 N18 C17 153.9(3) . . . . ? O21 S21 N20 C19 25.0(4) . . . . ? O22 S21 N20 C19 155.4(4) . . . . ? C22 S21 N20 C19 -91.4(4) . . . . ? O21 S21 N20 Cu1 144.2(4) . . . . ? O22 S21 N20 Cu1 -85.4(4) . . . . ? C22 S21 N20 Cu1 27.7(4) . . . . ? N18 Cu1 N20 C19 -107.6(2) 2 . . . ? N18 Cu1 N20 C19 -9.0(2) . . . . ? N1 Cu1 N20 C19 82.1(2) 2 . . . ? N1 Cu1 N20 C19 161.3(2) . . . . ? N20 Cu1 N20 C19 -65.1(2) 2 . . . ? Cu2 Cu1 N20 C19 143.8(3) . . . . ? N18 Cu1 N20 S21 122.3(4) 2 . . . ? N18 Cu1 N20 S21 -139.1(4) . . . . ? N1 Cu1 N20 S21 -48.0(4) 2 . . . ? N1 Cu1 N20 S21 31.2(5) . . . . ? N20 Cu1 N20 S21 164.8(4) 2 . . . ? Cu2 Cu1 N20 S21 13.7(3) . . . . ? C5 N1 C1 C2 0.7(5) . . . . ? Cu1 N1 C1 C2 178.5(3) . . . . ? N1 C1 C2 C3 0.6(6) . . . . ? C1 C2 C3 C4 -1.0(6) . . . . ? C2 C3 C4 C5 0.2(6) . . . . ? C1 N1 C5 C4 -1.5(5) . . . . ? Cu1 N1 C5 C4 -179.6(3) . . . . ? C1 N1 C5 C5 177.5(4) . . . 2 ? Cu1 N1 C5 C5 -0.6(5) . . . 2 ? C3 C4 C5 N1 1.1(6) . . . . ? C3 C4 C5 C5 -177.8(4) . . . 2 ? C19 S11 C12 C13 178.7(4) . . . . ? C19 S11 C12 C17 -0.8(3) . . . . ? C17 C12 C13 C14 -0.1(7) . . . . ? S11 C12 C13 C14 -179.5(4) . . . . ? C12 C13 C14 C15 -0.2(7) . . . . ? C12 C13 C14 C28 179.6(4) . . . . ? C13 C14 C15 C16 -0.3(7) . . . . ? C28 C14 C15 C16 179.9(4) . . . . ? C13 C14 C15 C29 179.4(4) . . . . ? C28 C14 C15 C29 -0.4(7) . . . . ? C14 C15 C16 C17 1.1(6) . . . . ? C29 C15 C16 C17 -178.6(4) . . . . ? C15 C16 C17 N18 179.2(4) . . . . ? C15 C16 C17 C12 -1.4(6) . . . . ? C19 N18 C17 C16 -179.3(4) . . . . ? Cu1 N18 C17 C16 23.0(6) . . . . ? C19 N18 C17 C12 1.3(5) . . . . ? Cu1 N18 C17 C12 -156.5(3) . . . . ? C13 C12 C17 C16 0.9(6) . . . . ? S11 C12 C17 C16 -179.6(3) . . . . ? C13 C12 C17 N18 -179.6(4) . . . . ? S11 C12 C17 N18 -0.1(4) . . . . ? S21 N20 C19 N18 165.5(3) . . . . ? Cu1 N20 C19 N18 12.2(3) . . . . ? S21 N20 C19 S11 -13.3(6) . . . . ? Cu1 N20 C19 S11 -166.6(4) . . . . ? C17 N18 C19 N20 179.1(3) . . . . ? Cu1 N18 C19 N20 -17.8(4) . . . . ? C17 N18 C19 S11 -1.9(4) . . . . ? Cu1 N18 C19 S11 161.16(18) . . . . ? C12 S11 C19 N20 -179.6(4) . . . . ? C12 S11 C19 N18 1.6(3) . . . . ? O21 S21 C22 C27 -13.5(4) . . . . ? O22 S21 C22 C27 -141.4(3) . . . . ? N20 S21 C22 C27 106.5(3) . . . . ? O21 S21 C22 C23 170.8(3) . . . . ? O22 S21 C22 C23 42.9(4) . . . . ? N20 S21 C22 C23 -69.2(4) . . . . ? C27 C22 C23 C24 -0.6(7) . . . . ? S21 C22 C23 C24 175.1(4) . . . . ? C22 C23 C24 C25 1.2(9) . . . . ? C23 C24 C25 C26 -0.9(9) . . . . ? C24 C25 C26 C27 0.2(8) . . . . ? C23 C22 C27 C26 -0.1(6) . . . . ? S21 C22 C27 C26 -175.8(3) . . . . ? C25 C26 C27 C22 0.3(7) . . . . ? N18 Cu1 Cu2 N38 -68.34(16) 2 . . . ? N18 Cu1 Cu2 N38 26.63(16) . . . . ? N1 Cu1 Cu2 N38 120.46(17) 2 . . . ? N1 Cu1 Cu2 N38 -162.16(17) . . . . ? N20 Cu1 Cu2 N38 -45.92(19) 2 . . . ? N20 Cu1 Cu2 N38 4.56(19) . . . . ? N18 Cu1 Cu2 N38 -26.36(16) 2 . . 2_655 ? N18 Cu1 Cu2 N38 68.61(16) . . . 2_655 ? N1 Cu1 Cu2 N38 162.44(17) 2 . . 2_655 ? N1 Cu1 Cu2 N38 -120.18(17) . . . 2_655 ? N20 Cu1 Cu2 N38 -3.94(19) 2 . . 2_655 ? N20 Cu1 Cu2 N38 46.5(2) . . . 2_655 ? N18 Cu1 Cu2 N2 117.90(14) 2 . . . ? N18 Cu1 Cu2 N2 -147.13(14) . . . . ? N1 Cu1 Cu2 N2 -53.30(16) 2 . . . ? N1 Cu1 Cu2 N2 24.09(15) . . . . ? N20 Cu1 Cu2 N2 140.33(19) 2 . . . ? N20 Cu1 Cu2 N2 -169.19(18) . . . . ? N18 Cu1 Cu2 N2 147.30(15) 2 . . 2_655 ? N18 Cu1 Cu2 N2 -117.73(14) . . . 2_655 ? N1 Cu1 Cu2 N2 -23.89(15) 2 . . 2_655 ? N1 Cu1 Cu2 N2 53.49(16) . . . 2_655 ? N20 Cu1 Cu2 N2 169.73(18) 2 . . 2_655 ? N20 Cu1 Cu2 N2 -139.79(19) . . . 2_655 ? N18 Cu1 Cu2 N40 7.37(13) 2 . . . ? N18 Cu1 Cu2 N40 102.34(14) . . . . ? N1 Cu1 Cu2 N40 -163.83(14) 2 . . . ? N1 Cu1 Cu2 N40 -86.44(14) . . . . ? N20 Cu1 Cu2 N40 29.80(17) 2 . . . ? N20 Cu1 Cu2 N40 80.28(18) . . . . ? N18 Cu1 Cu2 N40 -102.70(14) 2 . . 2_655 ? N18 Cu1 Cu2 N40 -7.74(13) . . . 2_655 ? N1 Cu1 Cu2 N40 86.10(15) 2 . . 2_655 ? N1 Cu1 Cu2 N40 163.48(14) . . . 2_655 ? N20 Cu1 Cu2 N40 -80.28(18) 2 . . 2_655 ? N20 Cu1 Cu2 N40 -29.80(17) . . . 2_655 ? N38 Cu2 N2 C10 170.7(7) . . . . ? N38 Cu2 N2 C10 -2.7(3) 2_655 . . . ? N2 Cu2 N2 C10 178.4(4) 2_655 . . . ? N40 Cu2 N2 C10 -96.0(3) . . . . ? N40 Cu2 N2 C10 50.6(3) 2_655 . . . ? Cu1 Cu2 N2 C10 -158.4(3) . . . . ? N38 Cu2 N2 C6 -7.7(10) . . . . ? N38 Cu2 N2 C6 178.9(3) 2_655 . . . ? N2 Cu2 N2 C6 0.1(2) 2_655 . . . ? N40 Cu2 N2 C6 85.6(3) . . . . ? N40 Cu2 N2 C6 -127.7(3) 2_655 . . . ? Cu1 Cu2 N2 C6 23.2(3) . . . . ? N38 Cu2 N38 C39 -97.5(3) 2_655 . . . ? N2 Cu2 N38 C39 89.1(9) . . . . ? N2 Cu2 N38 C39 81.5(3) 2_655 . . . ? N40 Cu2 N38 C39 -10.7(2) . . . . ? N40 Cu2 N38 C39 -150.8(3) 2_655 . . . ? Cu1 Cu2 N38 C39 54.1(2) . . . . ? N38 Cu2 N38 C37 108.1(3) 2_655 . . . ? N2 Cu2 N38 C37 -65.3(9) . . . . ? N2 Cu2 N38 C37 -72.9(3) 2_655 . . . ? N40 Cu2 N38 C37 -165.1(4) . . . . ? N40 Cu2 N38 C37 54.8(3) 2_655 . . . ? Cu1 Cu2 N38 C37 -100.3(3) . . . . ? O42 S41 N40 C39 -156.1(4) . . . . ? O41 S41 N40 C39 -26.2(4) . . . . ? C42 S41 N40 C39 90.1(4) . . . . ? O42 S41 N40 Cu2 84.8(4) . . . . ? O41 S41 N40 Cu2 -145.2(4) . . . . ? C42 S41 N40 Cu2 -29.0(4) . . . . ? N38 Cu2 N40 C39 10.4(2) . . . . ? N38 Cu2 N40 C39 108.1(2) 2_655 . . . ? N2 Cu2 N40 C39 -158.8(2) . . . . ? N2 Cu2 N40 C39 -79.4(2) 2_655 . . . ? N40 Cu2 N40 C39 66.4(2) 2_655 . . . ? Cu1 Cu2 N40 C39 -48.9(2) . . . . ? N38 Cu2 N40 S41 140.2(5) . . . . ? N38 Cu2 N40 S41 -122.2(4) 2_655 . . . ? N2 Cu2 N40 S41 -29.0(5) . . . . ? N2 Cu2 N40 S41 50.3(4) 2_655 . . . ? N40 Cu2 N40 S41 -163.9(4) 2_655 . . . ? Cu1 Cu2 N40 S41 80.9(4) . . . . ? C10 N2 C6 C7 0.8(6) . . . . ? Cu2 N2 C6 C7 179.3(3) . . . . ? C10 N2 C6 C6 -178.7(4) . . . 2_655 ? Cu2 N2 C6 C6 -0.2(5) . . . 2_655 ? N2 C6 C7 C8 -0.4(6) . . . . ? C6 C6 C7 C8 179.1(5) 2_655 . . . ? C6 C7 C8 C9 -0.9(7) . . . . ? C7 C8 C9 C10 1.6(7) . . . . ? C6 N2 C10 C9 0.0(6) . . . . ? Cu2 N2 C10 C9 -178.3(3) . . . . ? C8 C9 C10 N2 -1.2(7) . . . . ? C39 S31 C32 C33 -178.7(4) . . . . ? C39 S31 C32 C37 0.9(3) . . . . ? C37 C32 C33 C34 -0.3(6) . . . . ? S31 C32 C33 C34 179.2(3) . . . . ? C32 C33 C34 C35 0.1(6) . . . . ? C32 C33 C34 C48 179.7(4) . . . . ? C33 C34 C35 C36 0.1(6) . . . . ? C48 C34 C35 C36 -179.6(4) . . . . ? C33 C34 C35 C49 -178.8(4) . . . . ? C48 C34 C35 C49 1.5(6) . . . . ? C34 C35 C36 C37 0.0(6) . . . . ? C49 C35 C36 C37 179.0(4) . . . . ? C35 C36 C37 N38 -179.8(4) . . . . ? C35 C36 C37 C32 -0.3(6) . . . . ? C39 N38 C37 C36 177.6(4) . . . . ? Cu2 N38 C37 C36 -28.2(6) . . . . ? C39 N38 C37 C32 -1.9(5) . . . . ? Cu2 N38 C37 C32 152.3(3) . . . . ? C33 C32 C37 C36 0.5(6) . . . . ? S31 C32 C37 C36 -179.2(3) . . . . ? C33 C32 C37 N38 180.0(3) . . . . ? S31 C32 C37 N38 0.4(4) . . . . ? C37 N38 C39 N40 -179.2(3) . . . . ? Cu2 N38 C39 N40 21.2(4) . . . . ? C37 N38 C39 S31 2.6(4) . . . . ? Cu2 N38 C39 S31 -157.01(18) . . . . ? S41 N40 C39 N38 -169.2(3) . . . . ? Cu2 N40 C39 N38 -14.2(3) . . . . ? S41 N40 C39 S31 8.8(5) . . . . ? Cu2 N40 C39 S31 163.7(4) . . . . ? C32 S31 C39 N38 -2.1(3) . . . . ? C32 S31 C39 N40 179.9(4) . . . . ? O42 S41 C42 C47 -29.7(5) . . . . ? O41 S41 C42 C47 -157.6(4) . . . . ? N40 S41 C42 C47 82.5(4) . . . . ? O42 S41 C42 C43 155.7(4) . . . . ? O41 S41 C42 C43 27.8(4) . . . . ? N40 S41 C42 C43 -92.1(4) . . . . ? C47 C42 C43 C44 -1.9(7) . . . . ? S41 C42 C43 C44 172.6(4) . . . . ? C42 C43 C44 C45 -0.5(7) . . . . ? C43 C44 C45 C46 3.5(9) . . . . ? C44 C45 C46 C47 -4.1(11) . . . . ? C45 C46 C47 C42 1.6(11) . . . . ? C43 C42 C47 C46 1.5(9) . . . . ? S41 C42 C47 C46 -173.2(5) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 89.23 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.352 _refine_diff_density_min -0.574 _refine_diff_density_rms 0.060 #============================================================================== # End of Crystallographic Information File _database_code_depnum_ccdc_archive 'CCDC 923558'