# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Hegen Zheng' _publ_contact_author_email zhenghg@nju.edu.cn _publ_section_title ; The rational synthesize of (10,3)-type MOFs based on tetraunclear [W(Mo)OS3Cu3]+ secondary building units ; loop_ _publ_author_name 'Xiaoqiang Yao' 'Zhao-Rui Pan' 'Jinsong Hu' 'Yizhi Li' 'Zijian Guo' ; Hegen Zheng ; # Attachment '- cluster1.cif' data_cluster1 _database_code_depnum_ccdc_archive 'CCDC 824342' #TrackingRef '- cluster1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H35 Cu3 Mo N10 O S3, I' _chemical_formula_sum 'C45 H35 Cu3 I Mo N10 O S3' _chemical_formula_weight 1241.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.004(5) _cell_length_b 12.215(5) _cell_length_c 16.157(7) _cell_angle_alpha 74.739(6) _cell_angle_beta 76.360(5) _cell_angle_gamma 80.407(5) _cell_volume 2207.1(16) _cell_formula_units_Z 2 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 1672 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 23.37 _exptl_crystal_description rhombic _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.868 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1226 _exptl_absorpt_coefficient_mu 2.595 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.51 _exptl_absorpt_correction_T_max 0.60 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11934 _diffrn_reflns_av_R_equivalents 0.0304 _diffrn_reflns_av_sigmaI/netI 0.0825 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 26.00 _reflns_number_total 8459 _reflns_number_gt 5934 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.05P)^2^+1.99P] 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 8459 _refine_ls_number_parameters 577 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0867 _refine_ls_R_factor_gt 0.0613 _refine_ls_wR_factor_ref 0.1190 _refine_ls_wR_factor_gt 0.1143 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.097 _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 C1 C 0.6427(7) 0.3908(7) 0.6178(5) 0.052(2) Uani 1 1 d . . . H1 H 0.6365 0.4698 0.5978 0.063 Uiso 1 1 calc R . . C2 C 0.6472(7) 0.3284(6) 0.7034(5) 0.0487(18) Uani 1 1 d . . . H2 H 0.6421 0.3607 0.7504 0.058 Uiso 1 1 calc R . . C3 C 0.6607(5) 0.1979(6) 0.6239(4) 0.0360(15) Uani 1 1 d . . . H3 H 0.6671 0.1288 0.6082 0.043 Uiso 1 1 calc R . . C4 C 0.6614(7) 0.1357(6) 0.7846(4) 0.0432(17) Uani 1 1 d . . . C5 C 0.7210(6) 0.1468(6) 0.8433(4) 0.0391(15) Uani 1 1 d . . . H5 H 0.7642 0.2079 0.8297 0.047 Uiso 1 1 calc R . . C6 C 0.7183(5) 0.0699(6) 0.9216(4) 0.0396(16) Uani 1 1 d . . . H6 H 0.7578 0.0802 0.9615 0.047 Uiso 1 1 calc R . . C7 C 0.6549(5) -0.0273(5) 0.9431(4) 0.0299(13) Uani 1 1 d . . . C8 C 0.5927(5) -0.0394(6) 0.8843(4) 0.0423(17) Uani 1 1 d . . . H8 H 0.5496 -0.1006 0.8980 0.051 Uiso 1 1 calc R . . C9 C 0.5952(5) 0.0405(5) 0.8048(4) 0.0335(14) Uani 1 1 d . . . H9 H 0.5544 0.0324 0.7649 0.040 Uiso 1 1 calc R . . C10 C 0.6492(5) -0.1121(5) 1.0309(4) 0.0276(12) Uani 1 1 d . . . C11 C 0.6970(5) -0.0930(7) 1.0963(4) 0.0401(16) Uani 1 1 d . . . H11 H 0.7315 -0.0265 1.0850 0.048 Uiso 1 1 calc R . . C12 C 0.6952(5) -0.1689(5) 1.1770(4) 0.0319(14) Uani 1 1 d . . . H12 H 0.7252 -0.1529 1.2201 0.038 Uiso 1 1 calc R . . C13 C 0.6474(5) -0.2691(6) 1.1913(5) 0.0395(16) Uani 1 1 d . . . C14 C 0.5977(6) -0.2907(6) 1.1294(4) 0.0354(14) Uani 1 1 d . . . H14 H 0.5628 -0.3572 1.1415 0.043 Uiso 1 1 calc R . . C15 C 0.5997(6) -0.2135(5) 1.0489(4) 0.0397(16) Uani 1 1 d . . . H15 H 0.5678 -0.2294 1.0068 0.048 Uiso 1 1 calc R . . C16 C 0.6484(5) 0.6772(5) 0.3485(4) 0.0327(14) Uani 1 1 d . . . H16 H 0.6443 0.7502 0.3572 0.039 Uiso 1 1 calc R . . C17 C 0.6526(6) 0.5736(5) 0.4137(4) 0.0378(16) Uani 1 1 d . . . H17 H 0.6522 0.5662 0.4725 0.045 Uiso 1 1 calc R . . C18 C 0.6557(6) 0.5332(5) 0.2839(5) 0.0437(17) Uani 1 1 d . . . H18 H 0.6571 0.4933 0.2419 0.052 Uiso 1 1 calc R . . C19 C 0.9879(7) 0.0855(7) 0.1334(5) 0.052(2) Uani 1 1 d . . . H19 H 1.0377 0.0407 0.1685 0.062 Uiso 1 1 calc R . . C20 C 1.0183(6) 0.1327(5) 0.0485(5) 0.048(2) Uani 1 1 d . . . H20 H 1.0914 0.1245 0.0136 0.057 Uiso 1 1 calc R . . C21 C 0.8361(6) 0.1899(6) 0.0950(4) 0.0457(18) Uani 1 1 d . . . H21 H 0.7642 0.2327 0.0987 0.055 Uiso 1 1 calc R . . C22 C 0.9143(6) 0.2758(6) -0.0617(4) 0.0387(16) Uani 1 1 d . . . C23 C 1.0099(6) 0.2685(6) -0.1272(5) 0.056(2) Uani 1 1 d . . . H23 H 1.0718 0.2134 -0.1173 0.067 Uiso 1 1 calc R . . C24 C 1.0130(6) 0.3426(6) -0.2067(5) 0.0471(18) Uani 1 1 d . . . H24 H 1.0789 0.3382 -0.2501 0.057 Uiso 1 1 calc R . . C25 C 0.9195(7) 0.4266(6) -0.2261(5) 0.0484(18) Uani 1 1 d . . . C26 C 0.8241(7) 0.4292(6) -0.1583(4) 0.0485(18) Uani 1 1 d . . . H26 H 0.7604 0.4819 -0.1681 0.058 Uiso 1 1 calc R . . C27 C 0.8209(6) 0.3555(5) -0.0763(4) 0.0358(14) Uani 1 1 d . . . H27 H 0.7564 0.3598 -0.0316 0.043 Uiso 1 1 calc R . . C28 C 0.9226(6) 0.5051(6) -0.3126(5) 0.0436(17) Uani 1 1 d . . . C29 C 1.0264(6) 0.5307(6) -0.3640(5) 0.051(2) Uani 1 1 d . . . H29 H 1.0934 0.4938 -0.3450 0.061 Uiso 1 1 calc R . . C30 C 1.0359(6) 0.6113(6) -0.4451(4) 0.0398(16) Uani 1 1 d . . . H30 H 1.1078 0.6267 -0.4798 0.048 Uiso 1 1 calc R . . C31 C 0.9368(7) 0.6662(6) -0.4714(5) 0.0456(18) Uani 1 1 d . . . C32 C 0.8292(6) 0.6435(6) -0.4223(5) 0.0412(16) Uani 1 1 d . . . H32 H 0.7625 0.6810 -0.4414 0.049 Uiso 1 1 calc R . . C33 C 0.8236(6) 0.5621(5) -0.3427(4) 0.0375(15) Uani 1 1 d . . . H33 H 0.7517 0.5454 -0.3087 0.045 Uiso 1 1 calc R . . C34 C 1.0414(6) -0.2124(6) 0.3968(5) 0.051(2) Uani 1 1 d . . . H34 H 1.1147 -0.2498 0.4008 0.061 Uiso 1 1 calc R . . C35 C 1.0183(6) -0.1170(6) 0.3335(4) 0.0435(17) Uani 1 1 d . . . H35 H 1.0724 -0.0770 0.2899 0.052 Uiso 1 1 calc R . . C36 C 0.8589(5) -0.1633(6) 0.4192(4) 0.0395(16) Uani 1 1 d . . . H36 H 0.7819 -0.1623 0.4477 0.047 Uiso 1 1 calc R . . C37 C 0.2054(6) 0.1127(6) 0.3534(5) 0.0402(15) Uani 1 1 d . . . H37 H 0.1956 0.0585 0.4064 0.048 Uiso 1 1 calc R . . C38 C 0.1220(6) 0.1536(6) 0.3098(4) 0.0381(15) Uani 1 1 d . . . H38 H 0.0470 0.1340 0.3253 0.046 Uiso 1 1 calc R . . C39 C 0.2808(6) 0.2302(4) 0.2431(4) 0.0330(14) Uani 1 1 d . . . H39 H 0.3331 0.2759 0.2026 0.040 Uiso 1 1 calc R . . C40 C 0.1219(5) 0.2990(5) 0.1683(4) 0.0307(13) Uani 1 1 d . . . C41 C 0.0063(5) 0.3425(5) 0.1838(4) 0.0319(14) Uani 1 1 d . . . H41 H -0.0405 0.3195 0.2386 0.038 Uiso 1 1 calc R . . C42 C -0.0389(6) 0.4201(5) 0.1174(4) 0.0349(14) Uani 1 1 d . . . H42 H -0.1166 0.4479 0.1288 0.042 Uiso 1 1 calc R . . C43 C 0.0262(5) 0.4580(5) 0.0349(4) 0.0313(13) Uani 1 1 d . . . C44 C 0.1436(5) 0.4104(5) 0.0193(5) 0.0367(15) Uani 1 1 d . . . H44 H 0.1898 0.4313 -0.0360 0.044 Uiso 1 1 calc R . . C45 C 0.1899(6) 0.3335(6) 0.0854(4) 0.0383(15) Uani 1 1 d . . . H45 H 0.2673 0.3044 0.0745 0.046 Uiso 1 1 calc R . . Cu1 Cu 0.64961(7) 0.31879(6) 0.42709(5) 0.03468(19) Uani 1 1 d . . . Cu2 Cu 0.44812(7) 0.13777(7) 0.35632(5) 0.0363(2) Uani 1 1 d . . . Cu3 Cu 0.79048(7) 0.07283(7) 0.28695(5) 0.03649(19) Uani 1 1 d . . . I1 I 0.53504(4) 0.40887(4) 0.10667(3) 0.04589(14) Uani 1 1 d . . . Mo1 Mo 0.63090(5) 0.10544(4) 0.42535(4) 0.03226(14) Uani 1 1 d . . . N1 N 0.6496(4) 0.3077(5) 0.5666(3) 0.0353(12) Uani 1 1 d . . . N2 N 0.6605(5) 0.2104(5) 0.7087(3) 0.0365(12) Uani 1 1 d . . . N3 N 0.6517(5) 0.6503(4) 0.2685(4) 0.0367(12) Uani 1 1 d . . . N4 N 0.6572(5) 0.4835(4) 0.3725(4) 0.0414(14) Uani 1 1 d . . . N5 N 0.8703(5) 0.1133(4) 0.1619(4) 0.0377(13) Uani 1 1 d . . . N6 N 0.9181(5) 0.1982(5) 0.0208(4) 0.0530(17) Uani 1 1 d . . . N7 N 0.9454(5) -0.2440(4) 0.4511(4) 0.0375(13) Uani 1 1 d . . . N8 N 0.8940(5) -0.0898(5) 0.3471(4) 0.0407(13) Uani 1 1 d . . . N9 N 0.3088(5) 0.1570(4) 0.3138(3) 0.0360(12) Uani 1 1 d . . . N10 N 0.1702(5) 0.2339(4) 0.2341(3) 0.0319(11) Uani 1 1 d . . . O1 O 0.6346(4) 0.0056(4) 0.5214(3) 0.0373(10) Uani 1 1 d . . . S1 S 0.48110(15) 0.24183(14) 0.44385(12) 0.0384(4) Uani 1 1 d . . . S2 S 0.60799(14) 0.01959(14) 0.32190(11) 0.0357(4) Uani 1 1 d . . . S3 S 0.79468(14) 0.19004(14) 0.37745(11) 0.0354(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.065(5) 0.050(4) 0.051(4) -0.003(4) -0.041(4) -0.005(4) C2 0.064(5) 0.050(4) 0.038(4) -0.007(3) -0.018(3) -0.016(4) C3 0.033(3) 0.039(4) 0.033(3) -0.009(3) -0.013(3) 0.015(3) C4 0.058(5) 0.049(4) 0.027(3) 0.003(3) -0.022(3) -0.020(3) C5 0.046(4) 0.044(4) 0.028(3) 0.007(3) -0.012(3) -0.022(3) C6 0.031(3) 0.051(4) 0.035(4) 0.010(3) -0.018(3) -0.015(3) C7 0.030(3) 0.033(3) 0.027(3) -0.005(2) -0.009(2) -0.002(3) C8 0.028(3) 0.057(4) 0.042(4) 0.007(3) -0.020(3) -0.017(3) C9 0.030(3) 0.039(3) 0.034(3) -0.007(3) -0.017(3) 0.002(3) C10 0.032(3) 0.025(3) 0.023(3) -0.011(2) -0.001(2) 0.005(2) C11 0.018(3) 0.070(5) 0.027(3) 0.004(3) -0.014(2) -0.002(3) C12 0.039(4) 0.030(3) 0.029(3) -0.005(2) -0.021(3) 0.008(3) C13 0.024(3) 0.051(4) 0.045(4) -0.022(3) -0.003(3) 0.001(3) C14 0.040(4) 0.037(3) 0.028(3) -0.011(3) 0.005(3) -0.013(3) C15 0.042(4) 0.032(3) 0.041(4) -0.005(3) -0.003(3) -0.005(3) C16 0.038(3) 0.040(3) 0.020(3) 0.009(3) -0.018(3) -0.008(3) C17 0.048(4) 0.027(3) 0.029(3) -0.003(3) -0.012(3) 0.019(3) C18 0.055(4) 0.029(3) 0.050(4) -0.003(3) -0.033(3) 0.010(3) C19 0.053(5) 0.055(5) 0.038(4) -0.016(3) -0.003(3) 0.019(4) C20 0.035(4) 0.027(3) 0.049(4) 0.016(3) 0.015(3) 0.015(3) C21 0.037(4) 0.041(4) 0.041(4) 0.001(3) 0.001(3) 0.017(3) C22 0.036(4) 0.044(4) 0.028(3) -0.014(3) -0.001(3) 0.018(3) C23 0.037(4) 0.041(4) 0.052(5) 0.021(3) 0.019(3) 0.013(3) C24 0.043(4) 0.046(4) 0.037(4) 0.004(3) 0.000(3) 0.005(3) C25 0.042(4) 0.039(4) 0.056(5) -0.004(3) -0.003(3) -0.002(3) C26 0.050(4) 0.052(4) 0.034(4) -0.003(3) -0.010(3) 0.009(3) C27 0.033(3) 0.036(3) 0.034(3) -0.010(3) -0.005(3) 0.010(3) C28 0.027(3) 0.050(4) 0.056(4) -0.007(3) -0.019(3) -0.003(3) C29 0.032(4) 0.043(4) 0.047(4) 0.016(3) 0.005(3) 0.016(3) C30 0.035(4) 0.039(4) 0.033(3) 0.001(3) 0.008(3) -0.007(3) C31 0.053(4) 0.047(4) 0.039(4) 0.007(3) -0.021(3) -0.022(3) C32 0.049(4) 0.033(3) 0.044(4) -0.011(3) -0.016(3) 0.004(3) C33 0.030(3) 0.036(3) 0.048(4) 0.007(3) -0.018(3) -0.023(3) C34 0.025(3) 0.052(4) 0.057(5) -0.007(4) 0.007(3) 0.015(3) C35 0.034(4) 0.051(4) 0.036(4) -0.008(3) 0.009(3) -0.006(3) C36 0.017(3) 0.055(4) 0.042(4) -0.004(3) -0.001(3) -0.011(3) C37 0.035(4) 0.049(4) 0.045(4) -0.016(3) -0.015(3) -0.009(3) C38 0.036(4) 0.038(3) 0.036(4) -0.005(3) -0.009(3) 0.008(3) C39 0.042(4) 0.011(3) 0.048(4) 0.003(2) -0.026(3) -0.002(2) C40 0.029(3) 0.027(3) 0.043(4) -0.003(3) -0.017(3) -0.017(2) C41 0.021(3) 0.041(3) 0.032(3) 0.009(3) -0.010(2) -0.021(3) C42 0.032(3) 0.030(3) 0.043(4) -0.001(3) -0.014(3) -0.006(3) C43 0.026(3) 0.038(3) 0.031(3) -0.009(3) -0.010(2) 0.001(3) C44 0.019(3) 0.026(3) 0.054(4) 0.008(3) -0.002(3) -0.005(2) C45 0.029(3) 0.043(4) 0.044(4) -0.015(3) -0.009(3) 0.003(3) Cu1 0.0357(4) 0.0315(4) 0.0347(4) -0.0036(3) -0.0092(3) -0.0014(3) Cu2 0.0338(4) 0.0408(4) 0.0333(4) -0.0082(3) -0.0108(3) 0.0036(3) Cu3 0.0389(4) 0.0377(4) 0.0352(4) -0.0121(3) -0.0024(3) -0.0121(3) I1 0.0426(3) 0.0430(3) 0.0464(3) -0.0148(2) 0.0134(2) -0.0145(2) Mo1 0.0336(3) 0.0260(3) 0.0343(3) -0.0019(2) -0.0091(2) -0.0005(2) N1 0.029(3) 0.038(3) 0.035(3) -0.003(2) -0.008(2) 0.001(2) N2 0.038(3) 0.046(3) 0.024(3) 0.005(2) -0.010(2) -0.017(2) N3 0.036(3) 0.034(3) 0.043(3) -0.013(2) 0.002(2) -0.016(2) N4 0.054(4) 0.025(3) 0.043(3) -0.007(2) -0.013(3) 0.004(2) N5 0.039(3) 0.032(3) 0.039(3) -0.012(2) -0.003(2) 0.003(2) N6 0.041(3) 0.041(3) 0.052(4) 0.004(3) 0.008(3) 0.015(3) N7 0.037(3) 0.022(2) 0.050(3) -0.006(2) -0.002(2) -0.006(2) N8 0.038(3) 0.048(3) 0.031(3) -0.008(3) 0.001(2) -0.005(3) N9 0.033(3) 0.039(3) 0.036(3) -0.009(2) -0.014(2) 0.008(2) N10 0.041(3) 0.027(3) 0.033(3) -0.009(2) -0.013(2) -0.009(2) O1 0.036(2) 0.038(2) 0.038(3) -0.008(2) -0.014(2) 0.0038(19) S1 0.0344(9) 0.0347(9) 0.0501(10) -0.0146(7) -0.0142(7) 0.0008(7) S2 0.0323(8) 0.0364(8) 0.0410(9) -0.0118(7) -0.0115(7) -0.0004(7) S3 0.0340(8) 0.0365(8) 0.0388(9) -0.0129(7) -0.0073(7) -0.0064(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.400(10) . ? C1 N1 1.452(9) . ? C1 H1 0.9300 . ? C2 N2 1.405(9) . ? C2 H2 0.9300 . ? C3 N2 1.417(8) . ? C3 N1 1.421(8) . ? C3 H3 0.9300 . ? C4 N2 1.323(8) . ? C4 C5 1.359(9) . ? C4 C9 1.441(9) . ? C5 C6 1.360(8) . ? C5 H5 0.9300 . ? C6 C7 1.438(9) . ? C6 H6 0.9300 . ? C7 C8 1.387(9) . ? C7 C10 1.515(8) . ? C8 C9 1.391(9) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 C15 1.395(9) . ? C10 C11 1.399(9) . ? C11 C12 1.385(8) . ? C11 H11 0.9300 . ? C12 C13 1.379(9) . ? C12 H12 0.9300 . ? C13 N3 1.376(9) 1_546 ? C13 C14 1.379(10) . ? C14 C15 1.388(9) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 N3 1.406(8) . ? C16 C17 1.420(8) . ? C16 H16 0.9300 . ? C17 N4 1.416(8) . ? C17 H17 0.9300 . ? C18 N3 1.381(8) . ? C18 N4 1.403(9) . ? C18 H18 0.9300 . ? C19 C20 1.329(10) . ? C19 N5 1.391(9) . ? C19 H19 0.9300 . ? C20 N6 1.426(9) . ? C20 H20 0.9300 . ? C21 N5 1.328(8) . ? C21 N6 1.353(9) . ? C21 H21 0.9300 . ? C22 C23 1.373(9) . ? C22 C27 1.379(8) . ? C22 N6 1.423(9) . ? C23 C24 1.358(10) . ? C23 H23 0.9300 . ? C24 C25 1.423(10) . ? C24 H24 0.9300 . ? C25 C26 1.388(10) . ? C25 C28 1.468(10) . ? C26 C27 1.388(9) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C29 1.358(9) . ? C28 C33 1.397(9) . ? C29 C30 1.410(9) . ? C29 H29 0.9300 . ? C30 C31 1.368(10) . ? C30 H30 0.9300 . ? C31 C32 1.376(10) . ? C31 N7 1.427(8) 1_564 ? C32 C33 1.399(9) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C34 N7 1.318(9) . ? C34 C35 1.371(10) . ? C34 H34 0.9300 . ? C35 N8 1.450(9) . ? C35 H35 0.9300 . ? C36 N8 1.298(8) . ? C36 N7 1.400(8) . ? C36 H36 0.9300 . ? C37 C38 1.315(9) . ? C37 N9 1.382(9) . ? C37 H37 0.9300 . ? C38 N10 1.420(8) . ? C38 H38 0.9300 . ? C39 N9 1.326(8) . ? C39 N10 1.362(8) . ? C39 H39 0.9300 . ? C40 N10 1.339(8) . ? C40 C41 1.390(9) . ? C40 C45 1.392(9) . ? C41 C42 1.382(8) . ? C41 H41 0.9300 . ? C42 C43 1.381(9) . ? C42 H42 0.9300 . ? C43 C44 1.422(8) . ? C43 C43 1.495(12) 2_565 ? C44 C45 1.382(9) . ? C44 H44 0.9300 . ? C45 H45 0.9300 . ? Cu1 N4 1.980(5) . ? Cu1 N1 2.221(6) . ? Cu1 S3 2.2894(19) . ? Cu1 S1 2.300(2) . ? Cu1 Mo1 2.6608(14) . ? Cu2 N9 1.911(5) . ? Cu2 S2 2.2520(18) . ? Cu2 S1 2.270(2) . ? Cu2 O1 2.406(5) 2_656 ? Cu2 Mo1 2.6167(13) . ? Cu3 N5 1.990(5) . ? Cu3 N8 2.273(6) . ? Cu3 S2 2.289(2) . ? Cu3 S3 2.3133(19) . ? Cu3 Mo1 2.6500(12) . ? Mo1 O1 1.707(4) . ? Mo1 S3 2.2517(19) . ? Mo1 S1 2.2602(18) . ? Mo1 S2 2.2813(19) . ? N3 C13 1.376(9) 1_564 ? N7 C31 1.427(8) 1_546 ? O1 Cu2 2.406(5) 2_656 ? 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 C2 C1 N1 106.4(6) . . ? C2 C1 H1 126.8 . . ? N1 C1 H1 126.8 . . ? C1 C2 N2 110.9(6) . . ? C1 C2 H2 124.5 . . ? N2 C2 H2 124.5 . . ? N2 C3 N1 109.2(5) . . ? N2 C3 H3 125.4 . . ? N1 C3 H3 125.4 . . ? N2 C4 C5 122.4(6) . . ? N2 C4 C9 117.8(6) . . ? C5 C4 C9 119.8(6) . . ? C4 C5 C6 121.0(6) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C5 C6 C7 120.6(6) . . ? C5 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? C8 C7 C6 119.1(6) . . ? C8 C7 C10 119.8(5) . . ? C6 C7 C10 121.0(5) . . ? C7 C8 C9 119.7(6) . . ? C7 C8 H8 120.1 . . ? C9 C8 H8 120.1 . . ? C8 C9 C4 119.7(6) . . ? C8 C9 H9 120.1 . . ? C4 C9 H9 120.1 . . ? C15 C10 C11 117.4(6) . . ? C15 C10 C7 121.6(6) . . ? C11 C10 C7 121.0(6) . . ? C12 C11 C10 122.9(7) . . ? C12 C11 H11 118.5 . . ? C10 C11 H11 118.5 . . ? C13 C12 C11 117.7(6) . . ? C13 C12 H12 121.2 . . ? C11 C12 H12 121.2 . . ? N3 C13 C14 119.6(6) 1_546 . ? N3 C13 C12 119.0(6) 1_546 . ? C14 C13 C12 121.4(7) . . ? C13 C14 C15 120.2(6) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C14 C15 C10 120.4(6) . . ? C14 C15 H15 119.8 . . ? C10 C15 H15 119.8 . . ? N3 C16 C17 108.1(6) . . ? N3 C16 H16 126.0 . . ? C17 C16 H16 126.0 . . ? N4 C17 C16 107.3(6) . . ? N4 C17 H17 126.4 . . ? C16 C17 H17 126.4 . . ? N3 C18 N4 109.8(6) . . ? N3 C18 H18 125.1 . . ? N4 C18 H18 125.1 . . ? C20 C19 N5 109.7(7) . . ? C20 C19 H19 125.1 . . ? N5 C19 H19 125.1 . . ? C19 C20 N6 107.3(6) . . ? C19 C20 H20 126.4 . . ? N6 C20 H20 126.4 . . ? N5 C21 N6 112.1(6) . . ? N5 C21 H21 123.9 . . ? N6 C21 H21 123.9 . . ? C23 C22 C27 120.9(6) . . ? C23 C22 N6 116.5(6) . . ? C27 C22 N6 122.6(6) . . ? C24 C23 C22 119.4(6) . . ? C24 C23 H23 120.3 . . ? C22 C23 H23 120.3 . . ? C23 C24 C25 122.6(7) . . ? C23 C24 H24 118.7 . . ? C25 C24 H24 118.7 . . ? C26 C25 C24 115.8(7) . . ? C26 C25 C28 121.8(7) . . ? C24 C25 C28 122.3(7) . . ? C25 C26 C27 122.1(7) . . ? C25 C26 H26 119.0 . . ? C27 C26 H26 119.0 . . ? C22 C27 C26 119.2(6) . . ? C22 C27 H27 120.4 . . ? C26 C27 H27 120.4 . . ? C29 C28 C33 117.6(7) . . ? C29 C28 C25 118.9(6) . . ? C33 C28 C25 123.3(6) . . ? C28 C29 C30 122.1(6) . . ? C28 C29 H29 118.9 . . ? C30 C29 H29 118.9 . . ? C31 C30 C29 118.3(6) . . ? C31 C30 H30 120.8 . . ? C29 C30 H30 120.8 . . ? C30 C31 C32 122.2(6) . . ? C30 C31 N7 118.7(6) . 1_564 ? C32 C31 N7 119.0(6) . 1_564 ? C31 C32 C33 117.7(6) . . ? C31 C32 H32 121.2 . . ? C33 C32 H32 121.2 . . ? C28 C33 C32 122.1(6) . . ? C28 C33 H33 119.0 . . ? C32 C33 H33 119.0 . . ? N7 C34 C35 110.7(6) . . ? N7 C34 H34 124.6 . . ? C35 C34 H34 124.6 . . ? C34 C35 N8 107.4(6) . . ? C34 C35 H35 126.3 . . ? N8 C35 H35 126.3 . . ? N8 C36 N7 115.1(6) . . ? N8 C36 H36 122.5 . . ? N7 C36 H36 122.5 . . ? C38 C37 N9 114.3(7) . . ? C38 C37 H37 122.9 . . ? N9 C37 H37 122.9 . . ? C37 C38 N10 105.8(6) . . ? C37 C38 H38 127.1 . . ? N10 C38 H38 127.1 . . ? N9 C39 N10 115.3(6) . . ? N9 C39 H39 122.3 . . ? N10 C39 H39 122.3 . . ? N10 C40 C41 120.5(6) . . ? N10 C40 C45 120.0(6) . . ? C41 C40 C45 119.2(6) . . ? C42 C41 C40 119.7(6) . . ? C42 C41 H41 120.2 . . ? C40 C41 H41 120.2 . . ? C43 C42 C41 122.8(6) . . ? C43 C42 H42 118.6 . . ? C41 C42 H42 118.6 . . ? C42 C43 C44 116.8(6) . . ? C42 C43 C43 121.0(7) . 2_565 ? C44 C43 C43 122.1(7) . 2_565 ? C45 C44 C43 120.8(6) . . ? C45 C44 H44 119.6 . . ? C43 C44 H44 119.6 . . ? C44 C45 C40 120.6(6) . . ? C44 C45 H45 119.7 . . ? C40 C45 H45 119.7 . . ? N4 Cu1 N1 103.0(2) . . ? N4 Cu1 S3 118.69(18) . . ? N1 Cu1 S3 108.49(14) . . ? N4 Cu1 S1 119.15(19) . . ? N1 Cu1 S1 99.66(15) . . ? S3 Cu1 S1 105.68(7) . . ? N4 Cu1 Mo1 153.52(17) . . ? N1 Cu1 Mo1 103.38(14) . . ? S3 Cu1 Mo1 53.48(5) . . ? S1 Cu1 Mo1 53.61(5) . . ? N9 Cu2 S2 126.39(17) . . ? N9 Cu2 S1 124.24(16) . . ? S2 Cu2 S1 109.26(7) . . ? N9 Cu2 O1 88.0(2) . 2_656 ? S2 Cu2 O1 92.84(12) . 2_656 ? S1 Cu2 O1 93.01(12) . 2_656 ? N9 Cu2 Mo1 176.05(17) . . ? S2 Cu2 Mo1 55.27(5) . . ? S1 Cu2 Mo1 54.55(5) . . ? O1 Cu2 Mo1 88.33(11) 2_656 . ? N5 Cu3 N8 104.8(2) . . ? N5 Cu3 S2 119.69(18) . . ? N8 Cu3 S2 102.09(16) . . ? N5 Cu3 S3 118.95(17) . . ? N8 Cu3 S3 101.41(16) . . ? S2 Cu3 S3 106.79(7) . . ? N5 Cu3 Mo1 154.30(15) . . ? N8 Cu3 Mo1 100.86(14) . . ? S2 Cu3 Mo1 54.43(5) . . ? S3 Cu3 Mo1 53.44(5) . . ? O1 Mo1 S3 111.09(16) . . ? O1 Mo1 S1 110.35(16) . . ? S3 Mo1 S1 108.32(7) . . ? O1 Mo1 S2 109.30(16) . . ? S3 Mo1 S2 109.18(7) . . ? S1 Mo1 S2 108.55(7) . . ? O1 Mo1 Cu2 118.86(16) . . ? S3 Mo1 Cu2 130.05(6) . . ? S1 Mo1 Cu2 54.88(5) . . ? S2 Mo1 Cu2 54.22(5) . . ? O1 Mo1 Cu3 117.04(15) . . ? S3 Mo1 Cu3 55.61(5) . . ? S1 Mo1 Cu3 132.60(6) . . ? S2 Mo1 Cu3 54.69(5) . . ? Cu2 Mo1 Cu3 98.76(4) . . ? O1 Mo1 Cu1 116.32(15) . . ? S3 Mo1 Cu1 54.79(5) . . ? S1 Mo1 Cu1 55.01(5) . . ? S2 Mo1 Cu1 134.37(5) . . ? Cu2 Mo1 Cu1 100.50(3) . . ? Cu3 Mo1 Cu1 102.25(3) . . ? C3 N1 C1 107.0(5) . . ? C3 N1 Cu1 118.6(4) . . ? C1 N1 Cu1 134.5(4) . . ? C4 N2 C2 120.9(6) . . ? C4 N2 C3 132.4(6) . . ? C2 N2 C3 106.5(5) . . ? C13 N3 C18 128.6(6) 1_564 . ? C13 N3 C16 123.7(5) 1_564 . ? C18 N3 C16 107.7(5) . . ? C18 N4 C17 107.1(5) . . ? C18 N4 Cu1 124.2(4) . . ? C17 N4 Cu1 128.4(4) . . ? C21 N5 C19 105.3(6) . . ? C21 N5 Cu3 129.5(4) . . ? C19 N5 Cu3 123.3(5) . . ? C21 N6 C22 127.6(6) . . ? C21 N6 C20 104.5(6) . . ? C22 N6 C20 126.4(6) . . ? C34 N7 C36 104.0(6) . . ? C34 N7 C31 126.4(6) . 1_546 ? C36 N7 C31 129.3(6) . 1_546 ? C36 N8 C35 102.4(5) . . ? C36 N8 Cu3 126.4(4) . . ? C35 N8 Cu3 128.4(4) . . ? C39 N9 C37 101.2(5) . . ? C39 N9 Cu2 128.2(5) . . ? C37 N9 Cu2 130.0(4) . . ? C40 N10 C39 126.7(5) . . ? C40 N10 C38 129.9(5) . . ? C39 N10 C38 103.4(5) . . ? Mo1 O1 Cu2 152.8(2) . 2_656 ? Mo1 S1 Cu2 70.57(6) . . ? Mo1 S1 Cu1 71.38(6) . . ? Cu2 S1 Cu1 125.24(8) . . ? Cu2 S2 Mo1 70.51(6) . . ? Cu2 S2 Cu3 123.39(8) . . ? Mo1 S2 Cu3 70.88(5) . . ? Mo1 S3 Cu1 71.73(6) . . ? Mo1 S3 Cu3 70.96(5) . . ? Cu1 S3 Cu3 127.87(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 N2 2.0(9) . . . . ? N2 C4 C5 C6 178.6(7) . . . . ? C9 C4 C5 C6 -0.7(12) . . . . ? C4 C5 C6 C7 1.9(11) . . . . ? C5 C6 C7 C8 -2.4(10) . . . . ? C5 C6 C7 C10 -178.6(6) . . . . ? C6 C7 C8 C9 1.8(10) . . . . ? C10 C7 C8 C9 178.1(6) . . . . ? C7 C8 C9 C4 -0.6(11) . . . . ? N2 C4 C9 C8 -179.2(7) . . . . ? C5 C4 C9 C8 0.0(11) . . . . ? C8 C7 C10 C15 11.4(9) . . . . ? C6 C7 C10 C15 -172.4(6) . . . . ? C8 C7 C10 C11 -170.7(6) . . . . ? C6 C7 C10 C11 5.5(9) . . . . ? C15 C10 C11 C12 -1.1(9) . . . . ? C7 C10 C11 C12 -179.1(6) . . . . ? C10 C11 C12 C13 2.3(10) . . . . ? C11 C12 C13 N3 175.5(6) . . . 1_546 ? C11 C12 C13 C14 -3.3(9) . . . . ? N3 C13 C14 C15 -175.7(6) 1_546 . . . ? C12 C13 C14 C15 3.0(10) . . . . ? C13 C14 C15 C10 -1.7(10) . . . . ? C11 C10 C15 C14 0.7(9) . . . . ? C7 C10 C15 C14 178.7(6) . . . . ? N3 C16 C17 N4 -0.5(7) . . . . ? N5 C19 C20 N6 2.6(9) . . . . ? C27 C22 C23 C24 1.5(13) . . . . ? N6 C22 C23 C24 -178.0(8) . . . . ? C22 C23 C24 C25 -1.7(14) . . . . ? C23 C24 C25 C26 0.5(13) . . . . ? C23 C24 C25 C28 -178.9(8) . . . . ? C24 C25 C26 C27 0.9(12) . . . . ? C28 C25 C26 C27 -179.7(7) . . . . ? C23 C22 C27 C26 -0.1(12) . . . . ? N6 C22 C27 C26 179.3(7) . . . . ? C25 C26 C27 C22 -1.1(12) . . . . ? C26 C25 C28 C29 154.8(8) . . . . ? C24 C25 C28 C29 -25.9(12) . . . . ? C26 C25 C28 C33 -20.1(12) . . . . ? C24 C25 C28 C33 159.2(8) . . . . ? C33 C28 C29 C30 -0.2(12) . . . . ? C25 C28 C29 C30 -175.5(7) . . . . ? C28 C29 C30 C31 1.1(12) . . . . ? C29 C30 C31 C32 -1.3(11) . . . . ? C29 C30 C31 N7 173.8(7) . . . 1_564 ? C30 C31 C32 C33 0.7(11) . . . . ? N7 C31 C32 C33 -174.4(6) 1_564 . . . ? C29 C28 C33 C32 -0.4(11) . . . . ? C25 C28 C33 C32 174.6(7) . . . . ? C31 C32 C33 C28 0.2(10) . . . . ? N7 C34 C35 N8 -3.4(9) . . . . ? N9 C37 C38 N10 -0.7(8) . . . . ? N10 C40 C41 C42 172.6(6) . . . . ? C45 C40 C41 C42 -0.8(9) . . . . ? C40 C41 C42 C43 -0.4(10) . . . . ? C41 C42 C43 C44 2.0(9) . . . . ? C41 C42 C43 C43 -180.0(7) . . . 2_565 ? C42 C43 C44 C45 -2.5(9) . . . . ? C43 C43 C44 C45 179.5(7) 2_565 . . . ? C43 C44 C45 C40 1.4(10) . . . . ? N10 C40 C45 C44 -173.1(6) . . . . ? C41 C40 C45 C44 0.3(9) . . . . ? S2 Cu2 Mo1 O1 -93.90(18) . . . . ? S1 Cu2 Mo1 O1 95.61(18) . . . . ? O1 Cu2 Mo1 O1 0.7(3) 2_656 . . . ? S2 Cu2 Mo1 S3 85.60(9) . . . . ? S1 Cu2 Mo1 S3 -84.89(9) . . . . ? O1 Cu2 Mo1 S3 -179.78(12) 2_656 . . . ? S2 Cu2 Mo1 S1 170.49(8) . . . . ? O1 Cu2 Mo1 S1 -94.89(12) 2_656 . . . ? S1 Cu2 Mo1 S2 -170.49(8) . . . . ? O1 Cu2 Mo1 S2 94.62(12) 2_656 . . . ? S2 Cu2 Mo1 Cu3 33.70(6) . . . . ? S1 Cu2 Mo1 Cu3 -136.79(6) . . . . ? O1 Cu2 Mo1 Cu3 128.32(11) 2_656 . . . ? S2 Cu2 Mo1 Cu1 138.00(6) . . . . ? S1 Cu2 Mo1 Cu1 -32.49(6) . . . . ? O1 Cu2 Mo1 Cu1 -127.38(11) 2_656 . . . ? N5 Cu3 Mo1 O1 -179.4(4) . . . . ? N8 Cu3 Mo1 O1 -1.8(2) . . . . ? S2 Cu3 Mo1 O1 95.35(18) . . . . ? S3 Cu3 Mo1 O1 -98.06(18) . . . . ? N5 Cu3 Mo1 S3 -81.3(4) . . . . ? N8 Cu3 Mo1 S3 96.23(17) . . . . ? S2 Cu3 Mo1 S3 -166.59(8) . . . . ? N5 Cu3 Mo1 S1 2.3(4) . . . . ? N8 Cu3 Mo1 S1 179.81(17) . . . . ? S2 Cu3 Mo1 S1 -83.01(9) . . . . ? S3 Cu3 Mo1 S1 83.58(9) . . . . ? N5 Cu3 Mo1 S2 85.3(4) . . . . ? N8 Cu3 Mo1 S2 -97.18(17) . . . . ? S3 Cu3 Mo1 S2 166.59(8) . . . . ? N5 Cu3 Mo1 Cu2 51.8(4) . . . . ? N8 Cu3 Mo1 Cu2 -130.66(16) . . . . ? S2 Cu3 Mo1 Cu2 -33.48(6) . . . . ? S3 Cu3 Mo1 Cu2 133.11(6) . . . . ? N5 Cu3 Mo1 Cu1 -51.0(4) . . . . ? N8 Cu3 Mo1 Cu1 126.50(16) . . . . ? S2 Cu3 Mo1 Cu1 -136.32(6) . . . . ? S3 Cu3 Mo1 Cu1 30.27(6) . . . . ? N4 Cu1 Mo1 O1 179.7(4) . . . . ? N1 Cu1 Mo1 O1 -5.1(2) . . . . ? S3 Cu1 Mo1 O1 98.18(18) . . . . ? S1 Cu1 Mo1 O1 -97.31(18) . . . . ? N4 Cu1 Mo1 S3 81.5(4) . . . . ? N1 Cu1 Mo1 S3 -103.26(15) . . . . ? S1 Cu1 Mo1 S3 164.51(8) . . . . ? N4 Cu1 Mo1 S1 -83.0(4) . . . . ? N1 Cu1 Mo1 S1 92.23(15) . . . . ? S3 Cu1 Mo1 S1 -164.51(8) . . . . ? N4 Cu1 Mo1 S2 -1.1(4) . . . . ? N1 Cu1 Mo1 S2 174.09(15) . . . . ? S3 Cu1 Mo1 S2 -82.65(9) . . . . ? S1 Cu1 Mo1 S2 81.86(9) . . . . ? N4 Cu1 Mo1 Cu2 -50.5(4) . . . . ? N1 Cu1 Mo1 Cu2 124.67(14) . . . . ? S3 Cu1 Mo1 Cu2 -132.07(6) . . . . ? S1 Cu1 Mo1 Cu2 32.43(6) . . . . ? N4 Cu1 Mo1 Cu3 50.9(4) . . . . ? N1 Cu1 Mo1 Cu3 -133.87(14) . . . . ? S3 Cu1 Mo1 Cu3 -30.60(6) . . . . ? S1 Cu1 Mo1 Cu3 133.90(7) . . . . ? N2 C3 N1 C1 0.2(7) . . . . ? N2 C3 N1 Cu1 179.1(4) . . . . ? C2 C1 N1 C3 -1.3(8) . . . . ? C2 C1 N1 Cu1 -179.9(5) . . . . ? N4 Cu1 N1 C3 -171.4(4) . . . . ? S3 Cu1 N1 C3 -44.8(5) . . . . ? S1 Cu1 N1 C3 65.4(4) . . . . ? Mo1 Cu1 N1 C3 10.7(5) . . . . ? N4 Cu1 N1 C1 7.0(7) . . . . ? S3 Cu1 N1 C1 133.6(6) . . . . ? S1 Cu1 N1 C1 -116.1(6) . . . . ? Mo1 Cu1 N1 C1 -170.8(6) . . . . ? C5 C4 N2 C2 -43.6(11) . . . . ? C9 C4 N2 C2 135.7(7) . . . . ? C5 C4 N2 C3 142.8(8) . . . . ? C9 C4 N2 C3 -37.9(11) . . . . ? C1 C2 N2 C4 -176.9(7) . . . . ? C1 C2 N2 C3 -1.8(8) . . . . ? N1 C3 N2 C4 175.2(7) . . . . ? N1 C3 N2 C2 1.0(7) . . . . ? N4 C18 N3 C13 -179.0(6) . . . 1_564 ? N4 C18 N3 C16 -1.1(8) . . . . ? C17 C16 N3 C13 179.0(6) . . . 1_564 ? C17 C16 N3 C18 1.0(7) . . . . ? N3 C18 N4 C17 0.7(8) . . . . ? N3 C18 N4 Cu1 174.6(4) . . . . ? C16 C17 N4 C18 -0.1(8) . . . . ? C16 C17 N4 Cu1 -173.7(5) . . . . ? N1 Cu1 N4 C18 -178.0(5) . . . . ? S3 Cu1 N4 C18 62.2(6) . . . . ? S1 Cu1 N4 C18 -68.9(6) . . . . ? Mo1 Cu1 N4 C18 -2.8(9) . . . . ? N1 Cu1 N4 C17 -5.4(6) . . . . ? S3 Cu1 N4 C17 -125.2(5) . . . . ? S1 Cu1 N4 C17 103.6(6) . . . . ? Mo1 Cu1 N4 C17 169.8(4) . . . . ? N6 C21 N5 C19 10.9(9) . . . . ? N6 C21 N5 Cu3 175.7(5) . . . . ? C20 C19 N5 C21 -8.2(9) . . . . ? C20 C19 N5 Cu3 -174.1(5) . . . . ? N8 Cu3 N5 C21 168.5(6) . . . . ? S2 Cu3 N5 C21 54.9(7) . . . . ? S3 Cu3 N5 C21 -79.2(7) . . . . ? Mo1 Cu3 N5 C21 -14.0(9) . . . . ? N8 Cu3 N5 C19 -29.1(6) . . . . ? S2 Cu3 N5 C19 -142.7(5) . . . . ? S3 Cu3 N5 C19 83.2(6) . . . . ? Mo1 Cu3 N5 C19 148.3(5) . . . . ? N5 C21 N6 C22 -175.8(7) . . . . ? N5 C21 N6 C20 -9.3(9) . . . . ? C23 C22 N6 C21 179.0(8) . . . . ? C27 C22 N6 C21 -0.4(13) . . . . ? C23 C22 N6 C20 15.4(12) . . . . ? C27 C22 N6 C20 -164.0(8) . . . . ? C19 C20 N6 C21 3.8(9) . . . . ? C19 C20 N6 C22 170.5(7) . . . . ? C35 C34 N7 C36 0.0(9) . . . . ? C35 C34 N7 C31 -174.7(7) . . . 1_546 ? N8 C36 N7 C34 4.1(9) . . . . ? N8 C36 N7 C31 178.5(6) . . . 1_546 ? N7 C36 N8 C35 -5.9(8) . . . . ? N7 C36 N8 Cu3 -168.0(4) . . . . ? C34 C35 N8 C36 5.5(8) . . . . ? C34 C35 N8 Cu3 167.1(5) . . . . ? N5 Cu3 N8 C36 -160.5(6) . . . . ? S2 Cu3 N8 C36 -35.0(6) . . . . ? S3 Cu3 N8 C36 75.2(6) . . . . ? Mo1 Cu3 N8 C36 20.6(6) . . . . ? N5 Cu3 N8 C35 42.1(6) . . . . ? S2 Cu3 N8 C35 167.6(5) . . . . ? S3 Cu3 N8 C35 -82.3(5) . . . . ? Mo1 Cu3 N8 C35 -136.8(5) . . . . ? N10 C39 N9 C37 -1.4(7) . . . . ? N10 C39 N9 Cu2 -172.8(4) . . . . ? C38 C37 N9 C39 1.3(8) . . . . ? C38 C37 N9 Cu2 172.5(5) . . . . ? S2 Cu2 N9 C39 -90.3(6) . . . . ? S1 Cu2 N9 C39 85.4(6) . . . . ? O1 Cu2 N9 C39 177.7(6) 2_656 . . . ? S2 Cu2 N9 C37 100.7(6) . . . . ? S1 Cu2 N9 C37 -83.6(6) . . . . ? O1 Cu2 N9 C37 8.7(6) 2_656 . . . ? C41 C40 N10 C39 -145.7(6) . . . . ? C45 C40 N10 C39 27.7(9) . . . . ? C41 C40 N10 C38 34.3(9) . . . . ? C45 C40 N10 C38 -152.3(6) . . . . ? N9 C39 N10 C40 -179.0(6) . . . . ? N9 C39 N10 C38 1.0(7) . . . . ? C37 C38 N10 C40 179.8(6) . . . . ? C37 C38 N10 C39 -0.2(7) . . . . ? S3 Mo1 O1 Cu2 178.8(5) . . . 2_656 ? S1 Mo1 O1 Cu2 58.7(5) . . . 2_656 ? S2 Mo1 O1 Cu2 -60.6(5) . . . 2_656 ? Cu2 Mo1 O1 Cu2 -1.6(6) . . . 2_656 ? Cu3 Mo1 O1 Cu2 -120.0(5) . . . 2_656 ? Cu1 Mo1 O1 Cu2 118.7(5) . . . 2_656 ? O1 Mo1 S1 Cu2 -111.62(17) . . . . ? S3 Mo1 S1 Cu2 126.56(6) . . . . ? S2 Mo1 S1 Cu2 8.13(7) . . . . ? Cu3 Mo1 S1 Cu2 66.82(8) . . . . ? Cu1 Mo1 S1 Cu2 139.86(7) . . . . ? O1 Mo1 S1 Cu1 108.52(17) . . . . ? S3 Mo1 S1 Cu1 -13.29(7) . . . . ? S2 Mo1 S1 Cu1 -131.73(6) . . . . ? Cu2 Mo1 S1 Cu1 -139.86(7) . . . . ? Cu3 Mo1 S1 Cu1 -73.04(7) . . . . ? N9 Cu2 S1 Mo1 175.4(2) . . . . ? S2 Cu2 S1 Mo1 -8.27(7) . . . . ? O1 Cu2 S1 Mo1 85.80(11) 2_656 . . . ? N9 Cu2 S1 Cu1 -136.2(2) . . . . ? S2 Cu2 S1 Cu1 40.15(11) . . . . ? O1 Cu2 S1 Cu1 134.22(13) 2_656 . . . ? Mo1 Cu2 S1 Cu1 48.42(7) . . . . ? N4 Cu1 S1 Mo1 149.6(2) . . . . ? N1 Cu1 S1 Mo1 -99.57(14) . . . . ? S3 Cu1 S1 Mo1 12.88(7) . . . . ? N4 Cu1 S1 Cu2 101.4(2) . . . . ? N1 Cu1 S1 Cu2 -147.68(16) . . . . ? S3 Cu1 S1 Cu2 -35.23(11) . . . . ? Mo1 Cu1 S1 Cu2 -48.11(7) . . . . ? N9 Cu2 S2 Mo1 -175.6(2) . . . . ? S1 Cu2 S2 Mo1 8.20(7) . . . . ? O1 Cu2 S2 Mo1 -85.99(12) 2_656 . . . ? N9 Cu2 S2 Cu3 134.9(2) . . . . ? S1 Cu2 S2 Cu3 -41.30(11) . . . . ? O1 Cu2 S2 Cu3 -135.49(14) 2_656 . . . ? Mo1 Cu2 S2 Cu3 -49.50(7) . . . . ? O1 Mo1 S2 Cu2 112.21(16) . . . . ? S3 Mo1 S2 Cu2 -126.09(6) . . . . ? S1 Mo1 S2 Cu2 -8.20(7) . . . . ? Cu3 Mo1 S2 Cu2 -137.78(7) . . . . ? Cu1 Mo1 S2 Cu2 -67.00(7) . . . . ? O1 Mo1 S2 Cu3 -110.01(16) . . . . ? S3 Mo1 S2 Cu3 11.69(7) . . . . ? S1 Mo1 S2 Cu3 129.58(6) . . . . ? Cu2 Mo1 S2 Cu3 137.78(7) . . . . ? Cu1 Mo1 S2 Cu3 70.78(7) . . . . ? N5 Cu3 S2 Cu2 -100.81(19) . . . . ? N8 Cu3 S2 Cu2 144.15(16) . . . . ? S3 Cu3 S2 Cu2 38.13(11) . . . . ? Mo1 Cu3 S2 Cu2 49.35(7) . . . . ? N5 Cu3 S2 Mo1 -150.16(18) . . . . ? N8 Cu3 S2 Mo1 94.80(15) . . . . ? S3 Cu3 S2 Mo1 -11.22(6) . . . . ? O1 Mo1 S3 Cu1 -108.03(16) . . . . ? S1 Mo1 S3 Cu1 13.33(7) . . . . ? S2 Mo1 S3 Cu1 131.36(6) . . . . ? Cu2 Mo1 S3 Cu1 72.44(7) . . . . ? Cu3 Mo1 S3 Cu1 142.92(7) . . . . ? O1 Mo1 S3 Cu3 109.05(16) . . . . ? S1 Mo1 S3 Cu3 -129.59(6) . . . . ? S2 Mo1 S3 Cu3 -11.56(7) . . . . ? Cu2 Mo1 S3 Cu3 -70.48(7) . . . . ? Cu1 Mo1 S3 Cu3 -142.92(7) . . . . ? N4 Cu1 S3 Mo1 -149.8(2) . . . . ? N1 Cu1 S3 Mo1 93.21(15) . . . . ? S1 Cu1 S3 Mo1 -12.91(7) . . . . ? N4 Cu1 S3 Cu3 -103.6(2) . . . . ? N1 Cu1 S3 Cu3 139.43(17) . . . . ? S1 Cu1 S3 Cu3 33.31(11) . . . . ? Mo1 Cu1 S3 Cu3 46.22(7) . . . . ? N5 Cu3 S3 Mo1 150.66(19) . . . . ? N8 Cu3 S3 Mo1 -95.14(15) . . . . ? S2 Cu3 S3 Mo1 11.37(7) . . . . ? N5 Cu3 S3 Cu1 104.2(2) . . . . ? N8 Cu3 S3 Cu1 -141.63(16) . . . . ? S2 Cu3 S3 Cu1 -35.12(11) . . . . ? Mo1 Cu3 S3 Cu1 -46.49(8) . . . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.773 _refine_diff_density_min -0.678 _refine_diff_density_rms 0.109 # === END # Attachment '- cluster2.cif' data_cluster2 _database_code_depnum_ccdc_archive 'CCDC 824343' #TrackingRef '- cluster2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H21.60 Br Cu3 N7 O1.30 S3 W, C3 H7 N O, 0.7(H2 O)' _chemical_formula_sum 'C30 H30 Br Cu3 N8 O3 S3 W' _chemical_formula_weight 1101.18 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' Br Br -0.2901 2.4595 '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' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 37.3848(11) _cell_length_b 9.3228(13) _cell_length_c 30.230(2) _cell_angle_alpha 90.00 _cell_angle_beta 128.195(3) _cell_angle_gamma 90.00 _cell_volume 8280.3(13) _cell_formula_units_Z 8 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 5811 _cell_measurement_theta_min 2.179 _cell_measurement_theta_max 25.173 _exptl_crystal_description 'hexagonal prism' _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.767 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4272 _exptl_absorpt_coefficient_mu 5.445 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.25 _exptl_absorpt_correction_T_max 0.34 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21700 _diffrn_reflns_av_R_equivalents 0.0467 _diffrn_reflns_av_sigmaI/netI 0.0792 _diffrn_reflns_limit_h_min -46 _diffrn_reflns_limit_h_max 44 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 26.00 _reflns_number_total 8113 _reflns_number_gt 5543 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.05P)^2^+1.99P] 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 8113 _refine_ls_number_parameters 462 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0848 _refine_ls_R_factor_gt 0.0528 _refine_ls_wR_factor_ref 0.1113 _refine_ls_wR_factor_gt 0.1052 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _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 C1 C -0.1832(2) 1.1904(7) 0.7163(3) 0.0291(14) Uani 1 1 d . . . C2 C -0.1253(2) 1.0159(8) 0.7763(3) 0.0397(17) Uani 1 1 d . . . H2 H -0.1153 0.9358 0.7995 0.048 Uiso 1 1 calc R . . C3 C -0.1674(2) 1.0748(8) 0.7525(3) 0.0404(17) Uani 1 1 d . . . H3 H -0.1854 1.0363 0.7610 0.049 Uiso 1 1 calc R . . C4 C -0.15454(19) 1.2547(7) 0.7071(3) 0.0353(16) Uani 1 1 d . . . H4 H -0.1633 1.3387 0.6861 0.042 Uiso 1 1 calc R . . C5 C -0.0984(2) 1.0782(7) 0.7649(3) 0.0362(16) Uani 1 1 d . . . C6 C -0.1136(2) 1.1931(7) 0.7291(3) 0.0399(17) Uani 1 1 d . . . H6 H -0.0959 1.2293 0.7199 0.048 Uiso 1 1 calc R . . C7 C -0.0447(2) 0.8766(7) 0.7940(3) 0.0353(15) Uani 1 1 d . . . H7 H -0.0648 0.8036 0.7863 0.042 Uiso 1 1 calc R . . C8 C 0.0141(2) 0.9869(8) 0.8151(3) 0.0429(18) Uani 1 1 d . . . H8 H 0.0424 1.0049 0.8242 0.051 Uiso 1 1 calc R . . C9 C 0.1641(2) 1.1402(7) 0.4672(3) 0.0342(15) Uani 1 1 d . . . H9 H 0.1719 1.2108 0.4935 0.041 Uiso 1 1 calc R . . C10 C 0.1368(2) 1.0355(7) 0.3891(3) 0.0411(17) Uani 1 1 d . . . H10 H 0.1221 1.0202 0.3510 0.049 Uiso 1 1 calc R . . C11 C 0.1555(3) 0.9319(7) 0.4286(3) 0.0395(16) Uani 1 1 d . . . H11 H 0.1561 0.8343 0.4228 0.047 Uiso 1 1 calc R . . C12 C 0.1974(2) 0.9317(6) 0.5330(3) 0.0327(14) Uani 1 1 d . . . C13 C 0.2233(3) 0.8135(8) 0.5448(3) 0.0427(18) Uani 1 1 d . . . H13 H 0.2264 0.7791 0.5184 0.051 Uiso 1 1 calc R . . C14 C 0.1961(2) 0.9920(6) 0.5745(3) 0.0281(14) Uani 1 1 d . . . H14 H 0.1781 1.0718 0.5667 0.034 Uiso 1 1 calc R . . C15 C 0.2226(2) 0.9293(6) 0.6281(3) 0.0338(15) Uani 1 1 d . . . H15 H 0.2232 0.9715 0.6564 0.041 Uiso 1 1 calc R . . C16 C 0.2446(2) 0.7457(6) 0.5951(3) 0.0328(15) Uani 1 1 d . . . H16 H 0.2576 0.6561 0.5999 0.039 Uiso 1 1 calc R . . C17 C 0.2479(2) 0.8060(7) 0.6401(3) 0.0333(15) Uani 1 1 d . . . C18 C 0.2589(2) 0.7520(7) 0.7270(3) 0.0339(15) Uani 1 1 d . . . C19 C 0.2225(3) 0.7859(8) 0.9053(4) 0.051(2) Uani 1 1 d . . . H19 H 0.2315 0.8154 0.9402 0.061 Uiso 1 1 calc R . . C20 C 0.18556(19) 0.6829(6) 0.8240(3) 0.0281(14) Uani 1 1 d . . . H20 H 0.1644 0.6282 0.7924 0.034 Uiso 1 1 calc R . . C21 C 0.2437(3) 0.8201(9) 0.8826(3) 0.0453(19) Uani 1 1 d . . . H21 H 0.2694 0.8774 0.8992 0.054 Uiso 1 1 calc R . . C22 C 0.2320(2) 0.7551(6) 0.7947(3) 0.0281(14) Uani 1 1 d . . . C23 C 0.2026(2) 0.7098(8) 0.7397(3) 0.0388(17) Uani 1 1 d . . . H23 H 0.1738 0.6775 0.7255 0.047 Uiso 1 1 calc R . . C24 C 0.2753(3) 0.7987(8) 0.8161(3) 0.0453(18) Uani 1 1 d . . . H24 H 0.2959 0.8267 0.8535 0.054 Uiso 1 1 calc R . . C28 C 0.2879(3) 0.8006(8) 0.7819(4) 0.0454(19) Uani 1 1 d . . . H28 H 0.3165 0.8353 0.7960 0.054 Uiso 1 1 calc R . . C29 C 0.2151(2) 0.7112(7) 0.7042(3) 0.0400(17) Uani 1 1 d . . . H29 H 0.1945 0.6853 0.6665 0.048 Uiso 1 1 calc R . . C30 C -0.0165(2) 1.0865(8) 0.8018(3) 0.0423(18) Uani 1 1 d . . . H30 H -0.0130 1.1854 0.8021 0.051 Uiso 1 1 calc R . . C31 C 0.0880(2) 0.5082(8) 0.6755(3) 0.0355(16) Uani 1 1 d . . . H31 H 0.0961 0.4264 0.6974 0.043 Uiso 1 1 calc R . . C32 C 0.0535(3) 0.3334(8) 0.5974(4) 0.058(2) Uani 1 1 d . . . H32A H 0.0792 0.2732 0.6234 0.087 Uiso 1 1 calc R . . H32B H 0.0476 0.3322 0.5616 0.087 Uiso 1 1 calc R . . H32C H 0.0273 0.2983 0.5929 0.087 Uiso 1 1 calc R . . C33 C 0.0589(2) 0.6019(7) 0.5813(3) 0.0347(15) Uani 1 1 d . . . H33A H 0.0341 0.6639 0.5705 0.052 Uiso 1 1 calc R . . H33B H 0.0530 0.5607 0.5483 0.052 Uiso 1 1 calc R . . H33C H 0.0866 0.6563 0.6014 0.052 Uiso 1 1 calc R . . N1 N 0.1423(2) 1.1668(6) 0.4132(2) 0.0373(14) Uani 1 1 d . . . N2 N 0.17404(19) 0.9987(5) 0.4804(2) 0.0304(12) Uani 1 1 d . . . N3 N 0.27305(17) 0.7448(6) 0.6924(2) 0.0349(13) Uani 1 1 d . . . N4 N 0.18450(19) 0.6976(6) 0.8663(2) 0.0367(14) Uani 1 1 d . . . N5 N 0.22012(17) 0.7542(6) 0.8305(2) 0.0328(12) Uani 1 1 d . . . N6 N -0.00175(18) 0.8569(6) 0.8134(3) 0.0363(13) Uani 1 1 d . . . N7 N -0.05427(19) 1.0139(6) 0.7877(2) 0.0321(12) Uani 1 1 d . . . N8 N 0.0635(2) 0.4819(7) 0.6192(3) 0.0425(14) Uani 1 1 d . . . O1 O 0.06705(16) 0.2740(5) 0.8300(2) 0.0451(13) Uani 1 1 d . . . O2 O 0.10108(16) 0.6200(5) 0.7019(2) 0.0449(13) Uani 1 1 d . . . O3 O 0.0692(4) 0.9533(14) 0.5061(5) 0.062(4) Uani 0.40 1 d P . . H3A H 0.0630 1.0195 0.4829 0.075 Uiso 0.40 1 d PR . . H3C H 0.0620 0.8725 0.4895 0.075 Uiso 0.40 1 d PR . . O4 O 0.1071(7) 0.951(2) 0.6057(8) 0.067(6) Uani 0.30 1 d P . . H4A H 0.1351 0.9326 0.6231 0.080 Uiso 0.30 1 d PR . . H4B H 0.1044 1.0308 0.6168 0.080 Uiso 0.30 1 d PR . . O5 O 0.0821(5) 0.2361(16) 0.9634(6) 0.032(3) Uani 0.30 1 d P . . H5D H 0.0876 0.1974 0.9925 0.039 Uiso 0.30 1 d PR . . H5C H 0.0909 0.1807 0.9495 0.039 Uiso 0.30 1 d PR . . Cu1 Cu 0.10688(3) 0.51506(9) 0.95871(4) 0.0443(2) Uani 1 1 d . . . Cu2 Cu 0.13791(3) 0.64116(9) 0.87414(4) 0.0432(2) Uani 1 1 d . . . Cu3 Cu 0.02557(3) 0.67188(9) 0.82316(4) 0.0438(2) Uani 1 1 d . . . S1 S 0.15182(6) 0.46222(19) 0.93488(9) 0.0450(5) Uani 1 1 d . . . S2 S 0.06565(6) 0.60498(19) 0.79339(9) 0.0448(5) Uani 1 1 d . . . S3 S 0.03387(6) 0.49792(19) 0.88162(9) 0.0446(5) Uani 1 1 d . . . W1 W 0.078283(10) 0.44275(3) 0.857176(15) 0.04338(11) Uani 1 1 d . . . Br1 Br 0.12970(2) 0.57563(7) 1.04511(3) 0.04504(19) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.026(3) 0.045(4) 0.022(3) 0.005(3) 0.018(3) 0.006(3) C2 0.044(4) 0.042(4) 0.045(4) 0.015(3) 0.034(4) 0.001(3) C3 0.052(4) 0.046(4) 0.053(5) 0.009(4) 0.047(4) 0.001(3) C4 0.019(3) 0.036(3) 0.045(4) 0.023(3) 0.017(3) 0.004(3) C5 0.023(3) 0.039(4) 0.036(4) 0.014(3) 0.013(3) 0.005(3) C6 0.024(3) 0.045(4) 0.038(4) 0.013(3) 0.013(3) 0.008(3) C7 0.027(3) 0.042(4) 0.040(4) -0.004(3) 0.022(3) 0.001(3) C8 0.037(4) 0.050(4) 0.045(5) 0.004(4) 0.027(4) -0.007(3) C9 0.056(4) 0.028(3) 0.033(4) 0.009(3) 0.035(4) 0.004(3) C10 0.037(4) 0.046(4) 0.019(3) -0.002(3) 0.007(3) -0.007(3) C11 0.062(5) 0.032(3) 0.029(4) -0.001(3) 0.031(4) 0.003(3) C12 0.035(3) 0.026(3) 0.036(4) 0.001(3) 0.022(3) -0.007(3) C13 0.057(4) 0.053(4) 0.028(4) -0.008(3) 0.031(4) 0.008(4) C14 0.045(4) 0.008(2) 0.042(4) 0.006(3) 0.032(3) 0.003(2) C15 0.049(4) 0.023(3) 0.043(4) 0.005(3) 0.035(4) 0.005(3) C16 0.040(4) 0.020(3) 0.044(4) 0.018(3) 0.029(4) 0.016(3) C17 0.034(3) 0.041(3) 0.033(4) 0.017(3) 0.025(3) 0.007(3) C18 0.033(3) 0.040(4) 0.045(4) 0.007(3) 0.032(4) 0.013(3) C19 0.056(5) 0.045(4) 0.049(5) -0.022(4) 0.031(4) -0.004(4) C20 0.023(3) 0.026(3) 0.028(3) -0.017(3) 0.011(3) -0.007(2) C21 0.040(4) 0.065(5) 0.032(4) -0.022(4) 0.022(4) -0.013(4) C22 0.054(4) 0.013(3) 0.027(3) 0.003(2) 0.030(3) 0.003(3) C23 0.029(3) 0.051(4) 0.033(4) -0.005(3) 0.017(3) -0.011(3) C24 0.053(5) 0.052(4) 0.038(4) -0.006(3) 0.031(4) -0.016(4) C28 0.045(4) 0.056(5) 0.055(5) 0.009(4) 0.041(4) 0.005(3) C29 0.023(3) 0.047(4) 0.031(4) -0.022(3) 0.007(3) -0.010(3) C30 0.037(4) 0.051(4) 0.052(5) -0.015(4) 0.035(4) -0.011(3) C31 0.033(3) 0.051(4) 0.034(4) 0.017(3) 0.027(3) 0.014(3) C32 0.047(5) 0.045(4) 0.062(6) -0.026(4) 0.024(5) -0.031(4) C33 0.038(4) 0.035(3) 0.029(4) 0.008(3) 0.020(3) 0.005(3) N1 0.053(4) 0.031(3) 0.032(3) -0.005(2) 0.029(3) -0.016(3) N2 0.048(3) 0.023(2) 0.037(3) -0.005(2) 0.035(3) -0.009(2) N3 0.024(3) 0.053(3) 0.038(3) 0.013(3) 0.025(3) 0.019(2) N4 0.036(3) 0.047(3) 0.034(3) -0.003(3) 0.025(3) 0.013(3) N5 0.024(3) 0.033(3) 0.040(3) -0.006(3) 0.019(3) -0.005(2) N6 0.032(3) 0.032(3) 0.049(4) -0.002(3) 0.027(3) 0.008(2) N7 0.038(3) 0.032(3) 0.034(3) -0.001(2) 0.026(3) 0.000(2) N8 0.045(3) 0.050(4) 0.039(4) -0.012(3) 0.029(3) -0.006(3) O1 0.037(3) 0.037(3) 0.046(3) -0.008(2) 0.018(3) -0.008(2) O2 0.043(3) 0.032(2) 0.054(3) -0.016(2) 0.028(3) -0.012(2) O3 0.044(7) 0.040(7) 0.032(7) -0.003(6) -0.012(6) -0.010(6) O4 0.061(12) 0.056(11) 0.047(11) 0.000(9) 0.015(10) -0.040(10) O5 0.032(7) 0.046(9) 0.027(8) 0.003(7) 0.022(7) 0.003(6) Cu1 0.0362(5) 0.0349(4) 0.0515(6) -0.0047(4) 0.0219(5) -0.0052(4) Cu2 0.0378(5) 0.0346(4) 0.0491(6) -0.0049(4) 0.0228(5) -0.0049(4) Cu3 0.0376(4) 0.0341(4) 0.0499(6) -0.0042(4) 0.0221(5) -0.0044(4) S1 0.0369(9) 0.0352(9) 0.0525(12) -0.0039(8) 0.0224(9) -0.0058(7) S2 0.0374(9) 0.0355(9) 0.0520(12) -0.0044(8) 0.0229(9) -0.0054(7) S3 0.0352(9) 0.0359(9) 0.0508(12) -0.0044(8) 0.0207(9) -0.0042(7) W1 0.03627(16) 0.03432(15) 0.0488(2) -0.00443(14) 0.02091(15) -0.00482(12) Br1 0.0381(4) 0.0348(3) 0.0526(5) -0.0049(3) 0.0232(4) -0.0063(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 C1 C3 1.382(9) . ? C1 C4 1.397(8) . ? C1 N3 1.413(7) 3_455 ? C2 C3 1.376(10) . ? C2 C5 1.380(9) . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C4 C6 1.361(8) . ? C4 H4 0.9300 . ? C5 C6 1.369(9) . ? C5 N7 1.465(8) . ? C6 H6 0.9300 . ? C7 N7 1.311(8) . ? C7 N6 1.338(8) . ? C7 H7 0.9300 . ? C8 C30 1.328(10) . ? C8 N6 1.336(9) . ? C8 H8 0.9300 . ? C9 N1 1.322(9) . ? C9 N2 1.362(8) . ? C9 H9 0.9300 . ? C10 C11 1.347(10) . ? C10 N1 1.373(9) . ? C10 H10 0.9300 . ? C11 N2 1.405(8) . ? C11 H11 0.9300 . ? C12 C13 1.361(9) . ? C12 N2 1.402(8) . ? C12 C14 1.404(9) . ? C13 C16 1.359(10) . ? C13 H13 0.9300 . ? C14 C15 1.401(9) . ? C14 H14 0.9300 . ? C15 C17 1.387(8) . ? C15 H15 0.9300 . ? C16 C17 1.407(10) . ? C16 H16 0.9300 . ? C17 N3 1.367(8) . ? C18 C29 1.381(9) . ? C18 C28 1.381(11) . ? C18 N3 1.435(8) . ? C19 C21 1.370(11) . ? C19 N4 1.420(9) . ? C19 H19 0.9300 . ? C20 N4 1.310(8) . ? C20 N5 1.356(8) . ? C20 H20 0.9300 . ? C21 N5 1.384(9) . ? C21 H21 0.9300 . ? C22 C23 1.376(9) . ? C22 C24 1.382(10) . ? C22 N5 1.401(8) . ? C23 C29 1.411(10) . ? C23 H23 0.9300 . ? C24 C28 1.376(10) . ? C24 H24 0.9300 . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 N7 1.375(8) . ? C30 H30 0.9300 . ? C31 O2 1.217(9) . ? C31 N8 1.365(10) . ? C31 H31 0.9300 . ? C32 N8 1.480(9) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 N8 1.534(9) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? N1 Cu2 2.094(5) 6_575 ? N3 C1 1.413(7) 3_545 ? N4 Cu2 1.969(6) . ? N6 Cu3 1.932(5) . ? O1 W1 1.703(5) . ? O3 H3A 0.8499 . ? O3 H3C 0.8500 . ? O4 H4A 0.8502 . ? O4 H4B 0.8499 . ? O5 H5D 0.8501 . ? O5 H5C 0.8499 . ? Cu1 S3 2.245(2) . ? Cu1 S1 2.254(2) . ? Cu1 Br1 2.2613(13) . ? Cu1 W1 2.6381(11) . ? Cu2 N1 2.094(5) 6_576 ? Cu2 S2 2.284(2) . ? Cu2 S1 2.290(2) . ? Cu2 W1 2.6907(9) . ? Cu3 S2 2.260(2) . ? Cu3 S3 2.274(2) . ? Cu3 W1 2.6453(9) . ? S1 W1 2.2632(19) . ? S2 W1 2.259(2) . ? S3 W1 2.255(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 C1 C4 119.2(6) . . ? C3 C1 N3 118.5(6) . 3_455 ? C4 C1 N3 122.2(6) . 3_455 ? C3 C2 C5 118.5(6) . . ? C3 C2 H2 120.7 . . ? C5 C2 H2 120.7 . . ? C2 C3 C1 121.0(6) . . ? C2 C3 H3 119.5 . . ? C1 C3 H3 119.5 . . ? C6 C4 C1 119.2(6) . . ? C6 C4 H4 120.4 . . ? C1 C4 H4 120.4 . . ? C6 C5 C2 120.9(6) . . ? C6 C5 N7 119.4(6) . . ? C2 C5 N7 119.6(6) . . ? C4 C6 C5 120.7(7) . . ? C4 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? N7 C7 N6 110.1(6) . . ? N7 C7 H7 125.0 . . ? N6 C7 H7 125.0 . . ? C30 C8 N6 110.2(6) . . ? C30 C8 H8 124.9 . . ? N6 C8 H8 124.9 . . ? N1 C9 N2 113.0(6) . . ? N1 C9 H9 123.5 . . ? N2 C9 H9 123.5 . . ? C11 C10 N1 110.1(6) . . ? C11 C10 H10 125.0 . . ? N1 C10 H10 125.0 . . ? C10 C11 N2 107.4(6) . . ? C10 C11 H11 126.3 . . ? N2 C11 H11 126.3 . . ? C13 C12 N2 120.1(6) . . ? C13 C12 C14 120.1(6) . . ? N2 C12 C14 119.7(5) . . ? C16 C13 C12 120.0(6) . . ? C16 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C15 C14 C12 118.4(5) . . ? C15 C14 H14 120.8 . . ? C12 C14 H14 120.8 . . ? C17 C15 C14 121.9(6) . . ? C17 C15 H15 119.0 . . ? C14 C15 H15 119.0 . . ? C13 C16 C17 122.4(6) . . ? C13 C16 H16 118.8 . . ? C17 C16 H16 118.8 . . ? N3 C17 C15 121.2(6) . . ? N3 C17 C16 122.6(6) . . ? C15 C17 C16 116.1(6) . . ? C29 C18 C28 119.9(6) . . ? C29 C18 N3 118.7(7) . . ? C28 C18 N3 121.5(6) . . ? C21 C19 N4 108.1(7) . . ? C21 C19 H19 126.0 . . ? N4 C19 H19 126.0 . . ? N4 C20 N5 114.2(6) . . ? N4 C20 H20 122.9 . . ? N5 C20 H20 122.9 . . ? C19 C21 N5 107.9(6) . . ? C19 C21 H21 126.0 . . ? N5 C21 H21 126.0 . . ? C23 C22 C24 119.0(6) . . ? C23 C22 N5 122.3(6) . . ? C24 C22 N5 118.7(6) . . ? C22 C23 C29 121.6(6) . . ? C22 C23 H23 119.2 . . ? C29 C23 H23 119.2 . . ? C28 C24 C22 119.9(7) . . ? C28 C24 H24 120.1 . . ? C22 C24 H24 120.1 . . ? C24 C28 C18 121.3(7) . . ? C24 C28 H28 119.3 . . ? C18 C28 H28 119.3 . . ? C18 C29 C23 118.1(6) . . ? C18 C29 H29 120.9 . . ? C23 C29 H29 120.9 . . ? C8 C30 N7 106.0(6) . . ? C8 C30 H30 127.0 . . ? N7 C30 H30 127.0 . . ? O2 C31 N8 131.2(7) . . ? O2 C31 H31 114.4 . . ? N8 C31 H31 114.4 . . ? N8 C32 H32A 109.5 . . ? N8 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N8 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N8 C33 H33A 109.5 . . ? N8 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? N8 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C9 N1 C10 105.3(6) . . ? C9 N1 Cu2 129.1(5) . 6_575 ? C10 N1 Cu2 122.0(5) . 6_575 ? C9 N2 C12 129.0(6) . . ? C9 N2 C11 104.2(6) . . ? C12 N2 C11 126.8(5) . . ? C17 N3 C1 119.5(5) . 3_545 ? C17 N3 C18 121.6(5) . . ? C1 N3 C18 118.4(5) 3_545 . ? C20 N4 C19 104.6(6) . . ? C20 N4 Cu2 130.7(5) . . ? C19 N4 Cu2 124.1(5) . . ? C20 N5 C21 105.2(6) . . ? C20 N5 C22 128.4(6) . . ? C21 N5 C22 126.3(5) . . ? C8 N6 C7 106.0(6) . . ? C8 N6 Cu3 128.6(4) . . ? C7 N6 Cu3 124.6(5) . . ? C7 N7 C30 107.5(6) . . ? C7 N7 C5 126.5(6) . . ? C30 N7 C5 125.8(6) . . ? C31 N8 C32 121.0(7) . . ? C31 N8 C33 118.6(6) . . ? C32 N8 C33 117.9(6) . . ? H3A O3 H3C 109.5 . . ? H4A O4 H4B 109.5 . . ? H5D O5 H5C 109.5 . . ? S3 Cu1 S1 108.71(8) . . ? S3 Cu1 Br1 124.40(7) . . ? S1 Cu1 Br1 126.89(7) . . ? S3 Cu1 W1 54.28(6) . . ? S1 Cu1 W1 54.43(6) . . ? Br1 Cu1 W1 178.60(4) . . ? N4 Cu2 N1 94.1(2) . 6_576 ? N4 Cu2 S2 117.44(19) . . ? N1 Cu2 S2 110.95(17) 6_576 . ? N4 Cu2 S1 120.80(18) . . ? N1 Cu2 S1 105.74(17) 6_576 . ? S2 Cu2 S1 106.35(8) . . ? N4 Cu2 W1 148.33(17) . . ? N1 Cu2 W1 117.55(17) 6_576 . ? S2 Cu2 W1 53.25(5) . . ? S1 Cu2 W1 53.32(5) . . ? N6 Cu3 S2 127.09(19) . . ? N6 Cu3 S3 124.1(2) . . ? S2 Cu3 S3 107.88(8) . . ? N6 Cu3 W1 167.62(19) . . ? S2 Cu3 W1 54.14(5) . . ? S3 Cu3 W1 53.92(5) . . ? Cu1 S1 W1 71.47(6) . . ? Cu1 S1 Cu2 104.62(8) . . ? W1 S1 Cu2 72.45(7) . . ? W1 S2 Cu3 71.65(7) . . ? W1 S2 Cu2 72.65(7) . . ? Cu3 S2 Cu2 99.85(9) . . ? Cu1 S3 W1 71.79(6) . . ? Cu1 S3 Cu3 104.48(8) . . ? W1 S3 Cu3 71.48(7) . . ? O1 W1 S3 110.92(18) . . ? O1 W1 S2 110.33(19) . . ? S3 W1 S2 108.62(7) . . ? O1 W1 S1 110.73(17) . . ? S3 W1 S1 108.03(8) . . ? S2 W1 S1 108.12(7) . . ? O1 W1 Cu1 126.82(19) . . ? S3 W1 Cu1 53.93(5) . . ? S2 W1 Cu1 122.85(5) . . ? S1 W1 Cu1 54.10(6) . . ? O1 W1 Cu3 131.01(17) . . ? S3 W1 Cu3 54.60(5) . . ? S2 W1 Cu3 54.20(5) . . ? S1 W1 Cu3 118.26(5) . . ? Cu1 W1 Cu3 85.09(3) . . ? O1 W1 Cu2 130.92(17) . . ? S3 W1 Cu2 118.15(5) . . ? S2 W1 Cu2 54.10(5) . . ? S1 W1 Cu2 54.24(5) . . ? Cu1 W1 Cu2 84.87(3) . . ? Cu3 W1 Cu2 81.32(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 C5 C2 C3 C1 2.5(12) . . . . ? C4 C1 C3 C2 -4.9(11) . . . . ? N3 C1 C3 C2 178.9(7) 3_455 . . . ? C3 C1 C4 C6 7.0(11) . . . . ? N3 C1 C4 C6 -176.9(7) 3_455 . . . ? C3 C2 C5 C6 -2.3(12) . . . . ? C3 C2 C5 N7 -177.4(7) . . . . ? C1 C4 C6 C5 -6.9(12) . . . . ? C2 C5 C6 C4 4.6(12) . . . . ? N7 C5 C6 C4 179.7(7) . . . . ? N1 C10 C11 N2 -0.1(8) . . . . ? N2 C12 C13 C16 -177.7(6) . . . . ? C14 C12 C13 C16 6.1(11) . . . . ? C13 C12 C14 C15 1.1(9) . . . . ? N2 C12 C14 C15 -175.1(6) . . . . ? C12 C14 C15 C17 -3.4(10) . . . . ? C12 C13 C16 C17 -11.4(11) . . . . ? C14 C15 C17 N3 -179.0(6) . . . . ? C14 C15 C17 C16 -1.4(9) . . . . ? C13 C16 C17 N3 -173.5(7) . . . . ? C13 C16 C17 C15 8.9(10) . . . . ? N4 C19 C21 N5 -0.6(9) . . . . ? C24 C22 C23 C29 -2.0(10) . . . . ? N5 C22 C23 C29 -179.9(6) . . . . ? C23 C22 C24 C28 2.0(10) . . . . ? N5 C22 C24 C28 180.0(6) . . . . ? C22 C24 C28 C18 -3.7(11) . . . . ? C29 C18 C28 C24 5.2(11) . . . . ? N3 C18 C28 C24 -175.8(6) . . . . ? C28 C18 C29 C23 -5.0(10) . . . . ? N3 C18 C29 C23 175.9(6) . . . . ? C22 C23 C29 C18 3.5(11) . . . . ? N6 C8 C30 N7 -4.0(9) . . . . ? N2 C9 N1 C10 1.1(8) . . . . ? N2 C9 N1 Cu2 -157.3(5) . . . 6_575 ? C11 C10 N1 C9 -0.6(8) . . . . ? C11 C10 N1 Cu2 159.7(5) . . . 6_575 ? N1 C9 N2 C12 178.7(6) . . . . ? N1 C9 N2 C11 -1.1(8) . . . . ? C13 C12 N2 C9 -147.4(7) . . . . ? C14 C12 N2 C9 28.8(10) . . . . ? C13 C12 N2 C11 32.4(10) . . . . ? C14 C12 N2 C11 -151.4(6) . . . . ? C10 C11 N2 C9 0.7(8) . . . . ? C10 C11 N2 C12 -179.1(6) . . . . ? C15 C17 N3 C1 -139.2(7) . . . 3_545 ? C16 C17 N3 C1 43.3(10) . . . 3_545 ? C15 C17 N3 C18 32.0(10) . . . . ? C16 C17 N3 C18 -145.4(7) . . . . ? C29 C18 N3 C17 51.1(9) . . . . ? C28 C18 N3 C17 -127.9(7) . . . . ? C29 C18 N3 C1 -137.6(7) . . . 3_545 ? C28 C18 N3 C1 43.4(9) . . . 3_545 ? N5 C20 N4 C19 -0.9(7) . . . . ? N5 C20 N4 Cu2 170.4(4) . . . . ? C21 C19 N4 C20 0.9(8) . . . . ? C21 C19 N4 Cu2 -171.2(5) . . . . ? N4 C20 N5 C21 0.6(8) . . . . ? N4 C20 N5 C22 176.7(6) . . . . ? C19 C21 N5 C20 0.0(8) . . . . ? C19 C21 N5 C22 -176.2(6) . . . . ? C23 C22 N5 C20 16.9(10) . . . . ? C24 C22 N5 C20 -161.0(6) . . . . ? C23 C22 N5 C21 -167.8(7) . . . . ? C24 C22 N5 C21 14.3(10) . . . . ? C30 C8 N6 C7 5.1(9) . . . . ? C30 C8 N6 Cu3 175.0(6) . . . . ? N7 C7 N6 C8 -4.2(9) . . . . ? N7 C7 N6 Cu3 -174.6(5) . . . . ? N6 C7 N7 C30 1.8(8) . . . . ? N6 C7 N7 C5 176.8(6) . . . . ? C8 C30 N7 C7 1.3(9) . . . . ? C8 C30 N7 C5 -173.7(7) . . . . ? C6 C5 N7 C7 -139.2(8) . . . . ? C2 C5 N7 C7 36.0(11) . . . . ? C6 C5 N7 C30 34.9(11) . . . . ? C2 C5 N7 C30 -149.9(7) . . . . ? O2 C31 N8 C32 177.0(7) . . . . ? O2 C31 N8 C33 15.6(10) . . . . ? C20 N4 Cu2 N1 -137.0(6) . . . 6_576 ? C19 N4 Cu2 N1 32.9(6) . . . 6_576 ? C20 N4 Cu2 S2 -20.8(6) . . . . ? C19 N4 Cu2 S2 149.1(5) . . . . ? C20 N4 Cu2 S1 111.9(6) . . . . ? C19 N4 Cu2 S1 -78.2(6) . . . . ? C20 N4 Cu2 W1 42.9(8) . . . . ? C19 N4 Cu2 W1 -147.2(5) . . . . ? C8 N6 Cu3 S2 -37.0(8) . . . . ? C7 N6 Cu3 S2 131.2(5) . . . . ? C8 N6 Cu3 S3 130.8(6) . . . . ? C7 N6 Cu3 S3 -61.0(7) . . . . ? C8 N6 Cu3 W1 54.1(13) . . . . ? C7 N6 Cu3 W1 -137.7(7) . . . . ? S3 Cu1 S1 W1 -0.52(7) . . . . ? Br1 Cu1 S1 W1 179.43(6) . . . . ? S3 Cu1 S1 Cu2 64.88(9) . . . . ? Br1 Cu1 S1 Cu2 -115.17(8) . . . . ? W1 Cu1 S1 Cu2 65.40(7) . . . . ? N4 Cu2 S1 Cu1 153.0(2) . . . . ? N1 Cu2 S1 Cu1 48.20(19) 6_576 . . . ? S2 Cu2 S1 Cu1 -69.83(10) . . . . ? W1 Cu2 S1 Cu1 -64.72(6) . . . . ? N4 Cu2 S1 W1 -142.3(2) . . . . ? N1 Cu2 S1 W1 112.91(17) 6_576 . . . ? S2 Cu2 S1 W1 -5.11(8) . . . . ? N6 Cu3 S2 W1 164.7(2) . . . . ? S3 Cu3 S2 W1 -4.70(7) . . . . ? N6 Cu3 S2 Cu2 96.8(2) . . . . ? S3 Cu3 S2 Cu2 -72.59(9) . . . . ? W1 Cu3 S2 Cu2 -67.88(6) . . . . ? N4 Cu2 S2 W1 144.01(18) . . . . ? N1 Cu2 S2 W1 -109.40(18) 6_576 . . . ? S1 Cu2 S2 W1 5.12(8) . . . . ? N4 Cu2 S2 Cu3 -148.88(19) . . . . ? N1 Cu2 S2 Cu3 -42.29(19) 6_576 . . . ? S1 Cu2 S2 Cu3 72.23(9) . . . . ? W1 Cu2 S2 Cu3 67.11(6) . . . . ? S1 Cu1 S3 W1 0.52(7) . . . . ? Br1 Cu1 S3 W1 -179.43(5) . . . . ? S1 Cu1 S3 Cu3 -63.99(9) . . . . ? Br1 Cu1 S3 Cu3 116.06(8) . . . . ? W1 Cu1 S3 Cu3 -64.51(7) . . . . ? N6 Cu3 S3 Cu1 -100.3(2) . . . . ? S2 Cu3 S3 Cu1 69.44(10) . . . . ? W1 Cu3 S3 Cu1 64.73(6) . . . . ? N6 Cu3 S3 W1 -165.0(2) . . . . ? S2 Cu3 S3 W1 4.72(7) . . . . ? Cu1 S3 W1 O1 121.01(19) . . . . ? Cu3 S3 W1 O1 -126.16(19) . . . . ? Cu1 S3 W1 S2 -117.56(7) . . . . ? Cu3 S3 W1 S2 -4.74(7) . . . . ? Cu1 S3 W1 S1 -0.52(7) . . . . ? Cu3 S3 W1 S1 112.31(6) . . . . ? Cu3 S3 W1 Cu1 112.82(6) . . . . ? Cu1 S3 W1 Cu3 -112.82(6) . . . . ? Cu1 S3 W1 Cu2 -58.99(7) . . . . ? Cu3 S3 W1 Cu2 53.83(7) . . . . ? Cu3 S2 W1 O1 126.55(18) . . . . ? Cu2 S2 W1 O1 -126.45(17) . . . . ? Cu3 S2 W1 S3 4.77(7) . . . . ? Cu2 S2 W1 S3 111.77(7) . . . . ? Cu3 S2 W1 S1 -112.23(7) . . . . ? Cu2 S2 W1 S1 -5.23(8) . . . . ? Cu3 S2 W1 Cu1 -53.77(6) . . . . ? Cu2 S2 W1 Cu1 53.23(7) . . . . ? Cu2 S2 W1 Cu3 107.00(7) . . . . ? Cu3 S2 W1 Cu2 -107.00(7) . . . . ? Cu1 S1 W1 O1 -121.1(2) . . . . ? Cu2 S1 W1 O1 126.2(2) . . . . ? Cu1 S1 W1 S3 0.52(7) . . . . ? Cu2 S1 W1 S3 -112.15(7) . . . . ? Cu1 S1 W1 S2 117.89(7) . . . . ? Cu2 S1 W1 S2 5.22(8) . . . . ? Cu2 S1 W1 Cu1 -112.67(6) . . . . ? Cu1 S1 W1 Cu3 59.41(7) . . . . ? Cu2 S1 W1 Cu3 -53.26(7) . . . . ? Cu1 S1 W1 Cu2 112.67(7) . . . . ? S3 Cu1 W1 O1 -90.4(2) . . . . ? S1 Cu1 W1 O1 90.2(2) . . . . ? Br1 Cu1 W1 O1 -70.7(19) . . . . ? S1 Cu1 W1 S3 -179.39(9) . . . . ? Br1 Cu1 W1 S3 19.7(19) . . . . ? S3 Cu1 W1 S2 89.99(8) . . . . ? S1 Cu1 W1 S2 -89.40(8) . . . . ? Br1 Cu1 W1 S2 109.7(19) . . . . ? S3 Cu1 W1 S1 179.39(9) . . . . ? Br1 Cu1 W1 S1 -160.9(19) . . . . ? S3 Cu1 W1 Cu3 48.94(6) . . . . ? S1 Cu1 W1 Cu3 -130.45(6) . . . . ? Br1 Cu1 W1 Cu3 68.6(19) . . . . ? S3 Cu1 W1 Cu2 130.65(6) . . . . ? S1 Cu1 W1 Cu2 -48.75(6) . . . . ? Br1 Cu1 W1 Cu2 150.3(19) . . . . ? N6 Cu3 W1 O1 173.1(9) . . . . ? S2 Cu3 W1 O1 -86.6(2) . . . . ? S3 Cu3 W1 O1 87.9(3) . . . . ? N6 Cu3 W1 S3 85.3(9) . . . . ? S2 Cu3 W1 S3 -174.46(9) . . . . ? N6 Cu3 W1 S2 -100.3(9) . . . . ? S3 Cu3 W1 S2 174.46(9) . . . . ? N6 Cu3 W1 S1 -7.5(9) . . . . ? S2 Cu3 W1 S1 92.73(9) . . . . ? S3 Cu3 W1 S1 -92.82(9) . . . . ? N6 Cu3 W1 Cu1 36.9(9) . . . . ? S2 Cu3 W1 Cu1 137.15(6) . . . . ? S3 Cu3 W1 Cu1 -48.40(6) . . . . ? N6 Cu3 W1 Cu2 -48.7(9) . . . . ? S2 Cu3 W1 Cu2 51.60(6) . . . . ? S3 Cu3 W1 Cu2 -133.95(6) . . . . ? N4 Cu2 W1 O1 3.2(4) . . . . ? N1 Cu2 W1 O1 -176.9(3) 6_576 . . . ? S2 Cu2 W1 O1 86.6(2) . . . . ? S1 Cu2 W1 O1 -87.3(2) . . . . ? N4 Cu2 W1 S3 -176.8(3) . . . . ? N1 Cu2 W1 S3 3.12(19) 6_576 . . . ? S2 Cu2 W1 S3 -93.42(9) . . . . ? S1 Cu2 W1 S3 92.71(9) . . . . ? N4 Cu2 W1 S2 -83.4(3) . . . . ? N1 Cu2 W1 S2 96.53(19) 6_576 . . . ? S1 Cu2 W1 S2 -173.87(9) . . . . ? N4 Cu2 W1 S1 90.5(3) . . . . ? N1 Cu2 W1 S1 -89.59(19) 6_576 . . . ? S2 Cu2 W1 S1 173.87(9) . . . . ? N4 Cu2 W1 Cu1 139.1(3) . . . . ? N1 Cu2 W1 Cu1 -40.96(18) 6_576 . . . ? S2 Cu2 W1 Cu1 -137.49(7) . . . . ? S1 Cu2 W1 Cu1 48.64(7) . . . . ? N4 Cu2 W1 Cu3 -135.1(3) . . . . ? N1 Cu2 W1 Cu3 44.85(18) 6_576 . . . ? S2 Cu2 W1 Cu3 -51.69(7) . . . . ? S1 Cu2 W1 Cu3 134.44(7) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.025 _refine_diff_density_min -1.059 _refine_diff_density_rms 0.134 # === END