Supplementary Material (ESI) for Journal of Materials Chemistry This journal is (C) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 1145 _publ_requested_journal 'Journal of Materials Chemistry' loop_ _publ_author_name 'Zhang, Chi' 'Song, Yinglin' 'Fung, B.M.' 'Xue,Ziling' 'Xin, Xinquan' _publ_contact_author_name 'Dr Chi Zhang' _publ_contact_author_address ; Dr Chi Zhang Department of Chemistry & Biochemistry The University of Oklahoma 620 Parrington Oval Norman OK 73019 UNITED STATES OF AMERICA ; _publ_contact_author_email 'CZhang@chemdept.chem.ou.edu' # CLUSTER 1 data_cluster_1 _database_code_CSD 156623 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H30 Cu4 I2 N6 S4 W' _chemical_formula_weight 1294.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombhic _symmetry_space_group_name_H-M 'F d d 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 22.61310(10) _cell_length_b 23.0681(3) _cell_length_c 30.8375(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 16086.1(3) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 1.42 _cell_measurement_theta_max 28.42 _exptl_crystal_description block _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.36 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.138 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 9792 _exptl_absorpt_coefficient_mu 6.703 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.1651 _exptl_absorpt_correction_T_max 0.1964 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Siemens SMART CCD area detector diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27527 _diffrn_reflns_av_R_equivalents 0.0446 _diffrn_reflns_av_sigmaI/netI 0.0449 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 28.27 _reflns_number_total 8372 _reflns_number_gt 7125 _reflns_threshold_expression '> 2\s(I)' _computing_data_collection 'SMART (Siemens, 1996a)' _computing_cell_refinement 'SAINT (Siemens, 1996b)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXTL (Sheldrick, 1997)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material ; SHELXTL, PARST (Nardelli, 1995) and PLATON (Spek, 1990) ; _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^)+(0.0314P)^2^+30.2790P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.015(8) _refine_ls_number_reflns 8372 _refine_ls_number_parameters 425 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0454 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.0811 _refine_ls_wR_factor_gt 0.0761 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.097 _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 W1 W 0.0000 0.5000 0.344318(11) 0.03382(9) Uani 1 2 d S . . W2 W 0.0000 1.0000 0.336342(12) 0.03848(10) Uani 1 2 d S . . I1 I 0.17777(2) 0.42838(2) 0.41183(2) 0.05943(15) Uani 1 1 d . . . I2 I 0.07358(2) 0.82655(2) 0.40044(2) 0.05719(14) Uani 1 1 d . . . Cu1 Cu 0.07361(4) 0.59208(4) 0.34284(4) 0.0484(2) Uani 1 1 d . . . Cu2 Cu 0.09764(4) 0.42976(4) 0.34936(3) 0.0495(2) Uani 1 1 d . . . Cu3 Cu 0.07483(4) 0.90753(4) 0.34007(4) 0.0521(2) Uani 1 1 d . . . Cu4 Cu 0.09232(4) 1.07290(4) 0.33357(4) 0.0541(3) Uani 1 1 d . . . S1 S 0.08141(9) 0.50814(8) 0.30335(7) 0.0459(5) Uani 1 1 d . . . S2 S -0.00809(8) 0.57958(9) 0.38528(7) 0.0464(5) Uani 1 1 d . . . S3 S 0.08097(10) 0.99409(8) 0.37808(7) 0.0488(5) Uani 1 1 d . . . S4 S -0.00650(8) 0.92033(10) 0.29497(8) 0.0522(5) Uani 1 1 d . . . N1 N 0.0737(3) 0.6606(3) 0.2982(2) 0.0501(15) Uani 1 1 d . . . N2 N 0.1445(3) 0.6184(3) 0.3794(2) 0.0527(16) Uani 1 1 d . . . N3 N 0.1262(3) 0.3671(3) 0.3059(2) 0.0565(17) Uani 1 1 d . . . N4 N 0.1419(3) 0.8825(3) 0.2987(3) 0.0555(17) Uani 1 1 d . . . N5 N 0.1640(3) 1.0561(3) 0.2929(2) 0.0552(16) Uani 1 1 d . . . N6 N 0.1199(3) 1.1471(3) 0.3617(3) 0.0587(18) Uani 1 1 d . . . C1 C 0.1023(4) 0.6545(4) 0.2595(3) 0.061(2) Uani 1 1 d . . . H1A H 0.1208 0.6195 0.2534 0.073 Uiso 1 1 calc R . . C2 C 0.1046(5) 0.6975(4) 0.2296(3) 0.073(3) Uani 1 1 d . . . H2A H 0.1238 0.6916 0.2033 0.088 Uiso 1 1 calc R . . C3 C 0.0789(6) 0.7489(4) 0.2382(4) 0.089(3) Uani 1 1 d . . . H3A H 0.0804 0.7785 0.2178 0.106 Uiso 1 1 calc R . . C4 C 0.0513(7) 0.7573(4) 0.2760(4) 0.096(4) Uani 1 1 d . . . H4A H 0.0337 0.7928 0.2822 0.116 Uiso 1 1 calc R . . C5 C 0.0492(5) 0.7119(4) 0.3060(3) 0.080(3) Uani 1 1 d . . . H5A H 0.0300 0.7178 0.3322 0.096 Uiso 1 1 calc R . . C6 C 0.1942(4) 0.5876(4) 0.3824(3) 0.071(2) Uani 1 1 d . . . H6A H 0.1958 0.5523 0.3679 0.085 Uiso 1 1 calc R . . C7 C 0.2437(4) 0.6045(6) 0.4056(6) 0.112(5) Uani 1 1 d . . . H7A H 0.2779 0.5822 0.4063 0.134 Uiso 1 1 calc R . . C8 C 0.2395(5) 0.6552(6) 0.4271(6) 0.121(6) Uani 1 1 d . . . H8A H 0.2721 0.6687 0.4424 0.145 Uiso 1 1 calc R . . C9 C 0.1885(7) 0.6873(5) 0.4268(6) 0.137(7) Uani 1 1 d . . . H9A H 0.1846 0.7205 0.4437 0.164 Uiso 1 1 calc R . . C10 C 0.1429(4) 0.6683(4) 0.4004(4) 0.091(3) Uani 1 1 d . . . H10A H 0.1097 0.6917 0.3973 0.109 Uiso 1 1 calc R . . C11 C 0.0891(5) 0.3450(5) 0.2768(3) 0.084(3) Uani 1 1 d . . . H11A H 0.0496 0.3563 0.2779 0.100 Uiso 1 1 calc R . . C12 C 0.1058(7) 0.3067(5) 0.2455(4) 0.108(4) Uani 1 1 d . . . H12A H 0.0781 0.2925 0.2259 0.130 Uiso 1 1 calc R . . C13 C 0.1624(7) 0.2895(6) 0.2429(5) 0.116(5) Uani 1 1 d . . . H13A H 0.1746 0.2621 0.2227 0.140 Uiso 1 1 calc R . . C14 C 0.2028(7) 0.3147(6) 0.2723(6) 0.124(6) Uani 1 1 d . . . H14A H 0.2430 0.3065 0.2702 0.149 Uiso 1 1 calc R . . C15 C 0.1824(4) 0.3510(4) 0.3035(4) 0.084(3) Uani 1 1 d . . . H15A H 0.2089 0.3650 0.3241 0.101 Uiso 1 1 calc R . . C16 C 0.1849(4) 0.8472(4) 0.3114(4) 0.074(3) Uani 1 1 d . . . H16A H 0.1854 0.8342 0.3399 0.088 Uiso 1 1 calc R . . C17 C 0.2290(5) 0.8292(5) 0.2834(5) 0.095(4) Uani 1 1 d . . . H17A H 0.2591 0.8051 0.2933 0.113 Uiso 1 1 calc R . . C18 C 0.2277(6) 0.8471(6) 0.2409(4) 0.100(4) Uani 1 1 d . . . H18A H 0.2558 0.8337 0.2213 0.120 Uiso 1 1 calc R . . C19 C 0.1857(5) 0.8839(6) 0.2283(4) 0.089(3) Uani 1 1 d . . . H19A H 0.1844 0.8974 0.1999 0.106 Uiso 1 1 calc R . . C20 C 0.1446(4) 0.9012(5) 0.2583(3) 0.077(3) Uani 1 1 d . . . H20A H 0.1164 0.9282 0.2495 0.093 Uiso 1 1 calc R . . C21 C 0.2090(4) 1.0219(4) 0.3048(3) 0.065(2) Uani 1 1 d . . . H21A H 0.2093 1.0062 0.3325 0.078 Uiso 1 1 calc R . . C22 C 0.2550(5) 1.0096(7) 0.2768(6) 0.105(5) Uani 1 1 d . . . H22A H 0.2846 0.9844 0.2859 0.126 Uiso 1 1 calc R . . C23 C 0.2582(7) 1.0314(8) 0.2392(6) 0.126(6) Uani 1 1 d . . . H23A H 0.2902 1.0228 0.2214 0.151 Uiso 1 1 calc R . . C24 C 0.2159(10) 1.0665(7) 0.2252(5) 0.148(7) Uani 1 1 d . . . H24A H 0.2184 1.0835 0.1979 0.177 Uiso 1 1 calc R . . C25 C 0.1658(6) 1.0779(5) 0.2531(3) 0.088(3) Uani 1 1 d . . . H25A H 0.1348 1.1006 0.2430 0.106 Uiso 1 1 calc R . . C26 C 0.0892(4) 1.1968(4) 0.3585(4) 0.073(3) Uani 1 1 d . . . H26A H 0.0545 1.1970 0.3424 0.088 Uiso 1 1 calc R . . C27 C 0.1069(5) 1.2465(4) 0.3778(5) 0.099(4) Uani 1 1 d . . . H27A H 0.0861 1.2808 0.3732 0.119 Uiso 1 1 calc R . . C28 C 0.1548(6) 1.2460(5) 0.4037(7) 0.135(7) Uani 1 1 d . . . H28A H 0.1660 1.2798 0.4180 0.162 Uiso 1 1 calc R . . C29 C 0.1880(4) 1.1953(5) 0.4093(5) 0.106(5) Uani 1 1 d . . . H29A H 0.2213 1.1939 0.4270 0.127 Uiso 1 1 calc R . . C30 C 0.1678(4) 1.1481(4) 0.3870(4) 0.083(3) Uani 1 1 d . . . H30A H 0.1892 1.1138 0.3896 0.100 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 W1 0.03398(17) 0.03097(17) 0.0365(3) 0.000 0.000 0.00211(14) W2 0.0420(2) 0.03554(19) 0.0379(3) 0.000 0.000 0.00508(15) I1 0.0526(3) 0.0567(3) 0.0690(4) -0.0078(3) -0.0100(3) 0.0077(2) I2 0.0695(3) 0.0434(3) 0.0587(3) 0.0051(2) 0.0120(3) 0.0030(2) Cu1 0.0487(5) 0.0389(4) 0.0576(6) -0.0036(4) 0.0039(5) -0.0053(4) Cu2 0.0452(5) 0.0409(5) 0.0625(7) 0.0003(4) 0.0032(4) 0.0094(4) Cu3 0.0520(5) 0.0463(5) 0.0581(6) -0.0007(5) 0.0029(6) 0.0112(4) Cu4 0.0495(5) 0.0477(5) 0.0649(7) 0.0093(5) -0.0033(5) 0.0027(4) S1 0.0487(11) 0.0359(9) 0.0532(13) 0.0005(8) 0.0126(9) 0.0035(7) S2 0.0402(9) 0.0501(12) 0.0487(12) -0.0138(9) 0.0006(8) 0.0017(8) S3 0.0565(12) 0.0405(10) 0.0495(12) 0.0059(8) -0.0127(10) 0.0028(8) S4 0.0467(11) 0.0529(13) 0.0571(14) -0.0168(10) 0.0022(9) 0.0067(9) N1 0.064(4) 0.040(3) 0.046(4) -0.002(3) -0.006(3) -0.003(3) N2 0.047(3) 0.045(4) 0.066(5) 0.000(3) -0.003(3) -0.009(3) N3 0.072(5) 0.037(3) 0.061(4) -0.008(3) 0.003(3) 0.012(3) N4 0.047(4) 0.053(4) 0.067(5) 0.003(3) 0.014(3) 0.001(3) N5 0.056(4) 0.062(4) 0.048(4) 0.011(3) 0.006(3) 0.001(3) N6 0.050(4) 0.044(4) 0.082(5) 0.011(3) 0.005(3) -0.004(3) C1 0.071(5) 0.054(5) 0.057(5) 0.004(4) 0.017(4) 0.005(4) C2 0.098(7) 0.072(6) 0.051(5) 0.012(4) 0.008(5) -0.002(5) C3 0.128(10) 0.068(6) 0.069(7) 0.019(5) 0.010(7) -0.018(6) C4 0.142(12) 0.042(5) 0.105(10) -0.005(5) 0.021(8) 0.016(6) C5 0.123(8) 0.052(5) 0.065(6) 0.001(4) 0.027(6) 0.020(5) C6 0.058(5) 0.061(5) 0.094(7) 0.007(5) -0.011(5) 0.000(4) C7 0.054(6) 0.097(10) 0.184(16) 0.012(9) -0.028(7) -0.003(5) C8 0.088(8) 0.092(10) 0.182(17) 0.009(10) -0.075(9) -0.033(7) C9 0.141(11) 0.050(6) 0.218(18) -0.021(8) -0.100(12) -0.013(7) C10 0.076(6) 0.056(5) 0.141(10) -0.023(6) -0.039(7) -0.006(5) C11 0.093(7) 0.091(8) 0.067(7) -0.021(5) -0.019(5) 0.028(6) C12 0.138(12) 0.095(8) 0.091(9) -0.049(7) -0.037(8) 0.026(8) C13 0.139(12) 0.089(9) 0.121(12) -0.045(8) 0.025(9) 0.014(8) C14 0.108(10) 0.088(9) 0.177(16) -0.024(9) 0.053(11) 0.031(8) C15 0.062(6) 0.066(6) 0.125(10) -0.036(6) 0.010(6) 0.010(5) C16 0.059(5) 0.079(6) 0.082(7) 0.007(5) 0.021(5) 0.018(5) C17 0.068(6) 0.091(8) 0.125(11) 0.009(7) 0.030(7) 0.027(6) C18 0.100(9) 0.110(10) 0.091(10) -0.018(7) 0.054(7) -0.001(8) C19 0.079(7) 0.125(10) 0.062(6) 0.003(6) 0.033(5) -0.004(7) C20 0.067(6) 0.097(7) 0.068(6) 0.020(5) 0.008(5) -0.004(5) C21 0.049(4) 0.086(6) 0.061(5) -0.001(5) 0.000(4) 0.011(4) C22 0.064(7) 0.123(12) 0.127(14) -0.018(9) 0.028(8) 0.012(7) C23 0.133(13) 0.112(13) 0.132(16) -0.017(10) 0.068(11) -0.018(10) C24 0.26(2) 0.118(13) 0.067(9) 0.005(8) 0.074(12) -0.037(13) C25 0.126(9) 0.087(7) 0.051(6) 0.013(5) 0.008(6) 0.001(6) C26 0.067(5) 0.052(5) 0.101(8) 0.015(5) -0.010(5) 0.013(4) C27 0.071(7) 0.052(6) 0.174(14) 0.006(6) -0.002(8) 0.002(5) C28 0.086(9) 0.067(8) 0.25(2) -0.044(10) 0.008(11) -0.007(6) C29 0.046(5) 0.082(7) 0.190(14) -0.030(8) -0.016(7) -0.011(5) C30 0.040(4) 0.066(6) 0.144(11) -0.021(6) 0.000(5) -0.009(4) _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 W1 S2 2.236(2) . ? W1 S2 2.236(2) 2_565 ? W1 S1 2.2405(19) 2_565 ? W1 S1 2.240(2) . ? W1 Cu1 2.6990(8) 2_565 ? W1 Cu1 2.6990(8) . ? W1 Cu2 2.7431(9) . ? W1 Cu2 2.7431(8) 2_565 ? W2 S4 2.242(2) . ? W2 S4 2.242(2) 2_575 ? W2 S3 2.242(2) . ? W2 S3 2.242(2) 2_575 ? W2 Cu4 2.6820(9) 2_575 ? W2 Cu4 2.6820(9) . ? W2 Cu3 2.7252(9) . ? W2 Cu3 2.7252(9) 2_575 ? I1 Cu2 2.6448(11) . ? I2 Cu3 2.6373(12) . ? Cu1 N2 2.051(7) . ? Cu1 N1 2.096(6) . ? Cu1 S2 2.282(2) . ? Cu1 S1 2.294(2) . ? Cu2 N3 2.073(6) . ? Cu2 S2 2.318(2) 2_565 ? Cu2 S1 2.327(2) . ? Cu3 N4 2.064(7) . ? Cu3 S3 2.320(2) . ? Cu3 S4 2.325(2) . ? Cu4 N6 2.018(7) . ? Cu4 N5 2.087(7) . ? Cu4 S4 2.282(2) 2_575 ? Cu4 S3 2.292(2) . ? S2 Cu2 2.318(2) 2_565 ? S4 Cu4 2.282(2) 2_575 ? N1 C5 1.329(10) . ? N1 C1 1.364(10) . ? N2 C10 1.321(11) . ? N2 C6 1.333(10) . ? N3 C15 1.328(11) . ? N3 C11 1.330(12) . ? N4 C20 1.319(12) . ? N4 C16 1.327(11) . ? N5 C25 1.328(12) . ? N5 C21 1.337(10) . ? N6 C30 1.337(12) . ? N6 C26 1.342(10) . ? C1 C2 1.355(12) . ? C2 C3 1.346(14) . ? C3 C4 1.337(16) . ? C4 C5 1.398(14) . ? C6 C7 1.384(14) . ? C7 C8 1.35(2) . ? C8 C9 1.373(18) . ? C9 C10 1.385(15) . ? C11 C12 1.364(14) . ? C12 C13 1.342(18) . ? C13 C14 1.41(2) . ? C14 C15 1.357(16) . ? C16 C17 1.381(14) . ? C17 C18 1.375(17) . ? C18 C19 1.331(17) . ? C19 C20 1.373(13) . ? C21 C22 1.381(15) . ? C22 C23 1.27(2) . ? C23 C24 1.32(2) . ? C24 C25 1.45(2) . ? C26 C27 1.353(14) . ? C27 C28 1.35(2) . ? C28 C29 1.401(16) . ? C29 C30 1.367(14) . ? 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 S2 W1 S2 111.21(12) . 2_565 ? S2 W1 S1 108.67(7) . 2_565 ? S2 W1 S1 108.47(7) 2_565 2_565 ? S2 W1 S1 108.47(7) . . ? S2 W1 S1 108.67(7) 2_565 . ? S1 W1 S1 111.36(12) 2_565 . ? S2 W1 Cu1 127.25(5) . 2_565 ? S2 W1 Cu1 54.12(6) 2_565 2_565 ? S1 W1 Cu1 54.39(5) 2_565 2_565 ? S1 W1 Cu1 124.28(5) . 2_565 ? S2 W1 Cu1 54.12(5) . . ? S2 W1 Cu1 127.25(5) 2_565 . ? S1 W1 Cu1 124.28(5) 2_565 . ? S1 W1 Cu1 54.39(5) . . ? Cu1 W1 Cu1 178.06(5) 2_565 . ? S2 W1 Cu2 121.25(5) . . ? S2 W1 Cu2 54.35(5) 2_565 . ? S1 W1 Cu2 130.07(5) 2_565 . ? S1 W1 Cu2 54.56(5) . . ? Cu1 W1 Cu2 91.86(3) 2_565 . ? Cu1 W1 Cu2 88.25(3) . . ? S2 W1 Cu2 54.35(5) . 2_565 ? S2 W1 Cu2 121.25(5) 2_565 2_565 ? S1 W1 Cu2 54.56(5) 2_565 2_565 ? S1 W1 Cu2 130.07(5) . 2_565 ? Cu1 W1 Cu2 88.25(3) 2_565 2_565 ? Cu1 W1 Cu2 91.86(3) . 2_565 ? Cu2 W1 Cu2 173.50(5) . 2_565 ? S4 W2 S4 110.63(13) . 2_575 ? S4 W2 S3 109.29(7) . . ? S4 W2 S3 108.84(7) 2_575 . ? S4 W2 S3 108.84(7) . 2_575 ? S4 W2 S3 109.29(7) 2_575 2_575 ? S3 W2 S3 109.94(12) . 2_575 ? S4 W2 Cu4 54.33(5) . 2_575 ? S4 W2 Cu4 123.15(6) 2_575 2_575 ? S3 W2 Cu4 128.01(6) . 2_575 ? S3 W2 Cu4 54.61(6) 2_575 2_575 ? S4 W2 Cu4 123.15(6) . . ? S4 W2 Cu4 54.33(5) 2_575 . ? S3 W2 Cu4 54.61(6) . . ? S3 W2 Cu4 128.01(6) 2_575 . ? Cu4 W2 Cu4 176.35(5) 2_575 . ? S4 W2 Cu3 54.77(6) . . ? S4 W2 Cu3 128.68(6) 2_575 . ? S3 W2 Cu3 54.63(5) . . ? S3 W2 Cu3 122.03(6) 2_575 . ? Cu4 W2 Cu3 89.65(3) 2_575 . ? Cu4 W2 Cu3 90.51(3) . . ? S4 W2 Cu3 128.68(6) . 2_575 ? S4 W2 Cu3 54.77(6) 2_575 2_575 ? S3 W2 Cu3 122.03(6) . 2_575 ? S3 W2 Cu3 54.63(5) 2_575 2_575 ? Cu4 W2 Cu3 90.51(3) 2_575 2_575 ? Cu4 W2 Cu3 89.65(3) . 2_575 ? Cu3 W2 Cu3 175.16(5) . 2_575 ? N2 Cu1 N1 97.9(2) . . ? N2 Cu1 S2 110.7(2) . . ? N1 Cu1 S2 118.2(2) . . ? N2 Cu1 S1 118.8(2) . . ? N1 Cu1 S1 106.72(19) . . ? S2 Cu1 S1 105.06(7) . . ? N2 Cu1 W1 134.83(19) . . ? N1 Cu1 W1 127.25(18) . . ? S2 Cu1 W1 52.53(5) . . ? S1 Cu1 W1 52.56(5) . . ? N3 Cu2 S2 121.1(2) . 2_565 ? N3 Cu2 S1 101.3(2) . . ? S2 Cu2 S1 103.04(7) 2_565 . ? N3 Cu2 I1 104.4(2) . . ? S2 Cu2 I1 104.44(6) 2_565 . ? S1 Cu2 I1 124.15(6) . . ? N3 Cu2 W1 128.7(2) . . ? S2 Cu2 W1 51.60(5) 2_565 . ? S1 Cu2 W1 51.65(5) . . ? I1 Cu2 W1 126.86(4) . . ? N4 Cu3 S3 120.6(2) . . ? N4 Cu3 S4 104.3(2) . . ? S3 Cu3 S4 103.90(8) . . ? N4 Cu3 I2 104.23(19) . . ? S3 Cu3 I2 104.70(7) . . ? S4 Cu3 I2 120.26(7) . . ? N4 Cu3 W2 130.5(2) . . ? S3 Cu3 W2 52.02(5) . . ? S4 Cu3 W2 51.98(5) . . ? I2 Cu3 W2 125.28(4) . . ? N6 Cu4 N5 100.2(3) . . ? N6 Cu4 S4 115.4(2) . 2_575 ? N5 Cu4 S4 111.1(2) . 2_575 ? N6 Cu4 S3 116.7(2) . . ? N5 Cu4 S3 107.43(19) . . ? S4 Cu4 S3 105.75(8) 2_575 . ? N6 Cu4 W2 139.3(2) . . ? N5 Cu4 W2 120.5(2) . . ? S4 Cu4 W2 52.96(6) 2_575 . ? S3 Cu4 W2 52.88(6) . . ? W1 S1 Cu1 73.05(6) . . ? W1 S1 Cu2 73.78(6) . . ? Cu1 S1 Cu2 110.14(10) . . ? W1 S2 Cu1 73.35(6) . . ? W1 S2 Cu2 74.05(6) . 2_565 ? Cu1 S2 Cu2 116.42(10) . 2_565 ? W2 S3 Cu4 72.51(6) . . ? W2 S3 Cu3 73.35(7) . . ? Cu4 S3 Cu3 112.76(10) . . ? W2 S4 Cu4 72.71(6) . 2_575 ? W2 S4 Cu3 73.25(7) . . ? Cu4 S4 Cu3 111.67(11) 2_575 . ? C5 N1 C1 116.5(7) . . ? C5 N1 Cu1 123.5(6) . . ? C1 N1 Cu1 119.8(5) . . ? C10 N2 C6 116.9(8) . . ? C10 N2 Cu1 120.4(6) . . ? C6 N2 Cu1 122.7(6) . . ? C15 N3 C11 117.3(8) . . ? C15 N3 Cu2 122.0(6) . . ? C11 N3 Cu2 120.4(6) . . ? C20 N4 C16 116.5(8) . . ? C20 N4 Cu3 121.7(6) . . ? C16 N4 Cu3 121.9(6) . . ? C25 N5 C21 117.0(9) . . ? C25 N5 Cu4 120.6(7) . . ? C21 N5 Cu4 122.4(6) . . ? C30 N6 C26 116.6(8) . . ? C30 N6 Cu4 121.0(6) . . ? C26 N6 Cu4 122.2(6) . . ? C2 C1 N1 122.6(8) . . ? C3 C2 C1 119.6(10) . . ? C4 C3 C2 120.1(9) . . ? C3 C4 C5 118.9(9) . . ? N1 C5 C4 122.3(9) . . ? N2 C6 C7 124.7(10) . . ? C8 C7 C6 116.2(10) . . ? C7 C8 C9 121.7(10) . . ? C8 C9 C10 117.2(12) . . ? N2 C10 C9 123.0(10) . . ? N3 C11 C12 123.5(11) . . ? C13 C12 C11 119.9(12) . . ? C12 C13 C14 117.2(11) . . ? C15 C14 C13 119.3(12) . . ? N3 C15 C14 122.5(12) . . ? N4 C16 C17 122.0(10) . . ? C18 C17 C16 119.3(11) . . ? C19 C18 C17 119.0(10) . . ? C18 C19 C20 118.2(11) . . ? N4 C20 C19 124.9(10) . . ? N5 C21 C22 121.5(11) . . ? C23 C22 C21 122.2(14) . . ? C22 C23 C24 119.9(14) . . ? C23 C24 C25 119.0(13) . . ? N5 C25 C24 120.3(12) . . ? N6 C26 C27 122.6(9) . . ? C28 C27 C26 119.4(10) . . ? C27 C28 C29 120.8(12) . . ? C30 C29 C28 115.1(12) . . ? N6 C30 C29 125.3(9) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.632 _refine_diff_density_min -1.122 _refine_diff_density_rms 0.146 #======END # CLUSTER 3 data_cluster_3 _database_code_CSD 156624 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H30 Br2 Cu4 N6 S4 W' _chemical_formula_weight 1200.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 '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 orthorhombic _symmetry_space_group_name_H-M 'F d d 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 22.58970(10) _cell_length_b 22.8053(3) _cell_length_c 30.1995(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 15557.7(3) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6421 _cell_measurement_theta_min 1.44 _cell_measurement_theta_max 28.35 _exptl_crystal_description block _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.050 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 9216 _exptl_absorpt_coefficient_mu 7.397 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.1137 _exptl_absorpt_correction_T_max 0.2698 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ; Siemens SMART CCD area detector diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26507 _diffrn_reflns_av_R_equivalents 0.0593 _diffrn_reflns_av_sigmaI/netI 0.0653 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 28.27 _reflns_number_total 9516 _reflns_number_gt 6696 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1996)' _computing_cell_refinement 'SAINT (Siemens, 1996)' _computing_data_reduction 'SAINT (Siemens, 1996)' _computing_structure_solution 'SHELXTL (Sheldrick, 1997)' _computing_structure_refinement 'SHELXTL (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material ; SHELXTL (Sheldrick, 1997) PARST (Nardelli, 1983) ; _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^)+(0.0431P)^2^+40.3481P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000051(4) _refine_ls_extinction_expression 'Fc^*^==kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00 _refine_ls_number_reflns 9516 _refine_ls_number_parameters 426 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0747 _refine_ls_R_factor_gt 0.0432 _refine_ls_wR_factor_ref 0.1114 _refine_ls_wR_factor_gt 0.0977 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.074 _refine_ls_shift/su_mean 0.009 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 W1 W 0.0000 0.5000 0.345920(13) 0.04024(15) Uani 1 2 d S . . W2 W 0.0000 1.0000 0.335220(15) 0.04696(19) Uani 1 2 d S . . Br1 Br 0.17585(5) 0.42802(5) 0.40723(5) 0.0757(3) Uani 1 1 d . . . Br2 Br 0.07157(6) 0.82871(5) 0.39695(4) 0.0736(3) Uani 1 1 d . . . Cu1 Cu 0.07244(6) 0.59349(5) 0.34469(5) 0.0572(3) Uani 1 1 d . . . Cu2 Cu 0.09774(5) 0.42983(5) 0.35023(5) 0.0580(4) Uani 1 1 d . . . Cu3 Cu 0.07260(6) 0.90541(5) 0.33986(5) 0.0612(3) Uani 1 1 d . . . Cu4 Cu 0.09373(6) 1.07194(6) 0.33192(5) 0.0670(4) Uani 1 1 d . . . S1 S 0.08140(13) 0.50896(10) 0.30400(10) 0.0511(7) Uani 1 1 d . . . S2 S -0.00949(11) 0.58013(13) 0.38775(10) 0.0535(7) Uani 1 1 d . . . S3 S 0.08022(15) 0.99299(12) 0.37790(11) 0.0609(8) Uani 1 1 d . . . S4 S -0.00780(12) 0.91949(14) 0.29246(11) 0.0622(9) Uani 1 1 d . . . N1 N 0.0743(4) 0.6622(4) 0.2980(3) 0.067(2) Uani 1 1 d . . . N2 N 0.1432(4) 0.6207(4) 0.3820(3) 0.061(2) Uani 1 1 d . . . N3 N 0.1253(4) 0.3653(4) 0.3068(3) 0.064(2) Uani 1 1 d . . . N4 N 0.1412(4) 0.8808(4) 0.2983(3) 0.067(3) Uani 1 1 d . . . N5 N 0.1669(4) 1.0525(4) 0.2910(3) 0.074(3) Uani 1 1 d . . . N6 N 0.1213(4) 1.1465(4) 0.3617(3) 0.067(2) Uani 1 1 d . . . C1 C 0.1022(5) 0.6533(5) 0.2599(3) 0.069(3) Uani 1 1 d . . . H1A H 0.1202 0.6171 0.2551 0.083 Uiso 1 1 calc R . . C2 C 0.1056(6) 0.6944(6) 0.2279(4) 0.090(4) Uani 1 1 d . . . H2A H 0.1228 0.6859 0.2007 0.108 Uiso 1 1 calc R . . C3 C 0.0833(7) 0.7484(6) 0.2362(4) 0.097(4) Uani 1 1 d . . . H3A H 0.0883 0.7783 0.2155 0.116 Uiso 1 1 calc R . . C4 C 0.0545(8) 0.7592(5) 0.2738(5) 0.121(6) Uani 1 1 d . . . H4A H 0.0363 0.7952 0.2788 0.145 Uiso 1 1 calc R . . C5 C 0.0523(6) 0.7137(5) 0.3061(5) 0.098(4) Uani 1 1 d . . . H5A H 0.0349 0.7210 0.3334 0.118 Uiso 1 1 calc R . . C6 C 0.1918(5) 0.5873(5) 0.3872(4) 0.078(3) Uani 1 1 d . . . H6A H 0.1922 0.5503 0.3741 0.093 Uiso 1 1 calc R . . C7 C 0.2399(6) 0.6044(8) 0.4102(6) 0.122(6) Uani 1 1 d . . . H7A H 0.2729 0.5801 0.4122 0.146 Uiso 1 1 calc R . . C8 C 0.2399(8) 0.6568(9) 0.4303(8) 0.153(10) Uani 1 1 d . . . H8A H 0.2727 0.6691 0.4465 0.184 Uiso 1 1 calc R . . C9 C 0.1905(8) 0.6923(7) 0.4268(7) 0.146(7) Uani 1 1 d . . . H9A H 0.1892 0.7287 0.4407 0.175 Uiso 1 1 calc R . . C10 C 0.1417(6) 0.6717(5) 0.4012(5) 0.099(4) Uani 1 1 d . . . H10A H 0.1082 0.6951 0.3983 0.118 Uiso 1 1 calc R . . C11 C 0.0871(6) 0.3402(6) 0.2779(4) 0.093(4) Uani 1 1 d . . . H11A H 0.0473 0.3505 0.2788 0.112 Uiso 1 1 calc R . . C12 C 0.1056(9) 0.3004(7) 0.2476(5) 0.125(6) Uani 1 1 d . . . H12A H 0.0783 0.2841 0.2281 0.149 Uiso 1 1 calc R . . C13 C 0.1638(9) 0.2838(7) 0.2452(6) 0.129(6) Uani 1 1 d . . . H13A H 0.1766 0.2543 0.2262 0.154 Uiso 1 1 calc R . . C14 C 0.2014(10) 0.3127(8) 0.2722(8) 0.155(9) Uani 1 1 d . . . H14A H 0.2419 0.3058 0.2699 0.186 Uiso 1 1 calc R . . C15 C 0.1811(5) 0.3517(5) 0.3030(6) 0.107(5) Uani 1 1 d . . . H15A H 0.2082 0.3693 0.3220 0.129 Uiso 1 1 calc R . . C16 C 0.1840(4) 0.8452(5) 0.3121(4) 0.083(3) Uani 1 1 d . . . H16A H 0.1826 0.8304 0.3408 0.099 Uiso 1 1 calc R . . C17 C 0.2304(7) 0.8297(7) 0.2849(6) 0.110(5) Uani 1 1 d . . . H17A H 0.2619 0.8077 0.2957 0.132 Uiso 1 1 calc R . . C18 C 0.2290(8) 0.8472(8) 0.2423(6) 0.111(6) Uani 1 1 d . . . H18A H 0.2577 0.8337 0.2227 0.133 Uiso 1 1 calc R . . C19 C 0.1868(6) 0.8840(8) 0.2279(5) 0.107(5) Uani 1 1 d . . . H19A H 0.1865 0.8982 0.1991 0.129 Uiso 1 1 calc R . . C20 C 0.1454(5) 0.8989(6) 0.2571(4) 0.086(4) Uani 1 1 d . . . H20A H 0.1164 0.9248 0.2473 0.104 Uiso 1 1 calc R . . C21 C 0.2102(5) 1.0185(6) 0.3055(4) 0.080(3) Uani 1 1 d . . . H21A H 0.2080 1.0047 0.3344 0.096 Uiso 1 1 calc R . . C22 C 0.2578(6) 1.0025(8) 0.2807(6) 0.105(5) Uani 1 1 d . . . H22A H 0.2858 0.9771 0.2926 0.126 Uiso 1 1 calc R . . C23 C 0.2647(9) 1.0212(9) 0.2421(7) 0.131(6) Uani 1 1 d . . . H23A H 0.2979 1.0103 0.2259 0.157 Uiso 1 1 calc R . . C24 C 0.2248(11) 1.0568(9) 0.2241(5) 0.143(8) Uani 1 1 d . . . H24A H 0.2295 1.0702 0.1952 0.172 Uiso 1 1 calc R . . C25 C 0.1700(8) 1.0755(7) 0.2519(5) 0.120(6) Uani 1 1 d . . . H25A H 0.1415 1.1013 0.2413 0.143 Uiso 1 1 calc R . . C26 C 0.0879(5) 1.1952(5) 0.3604(4) 0.087(3) Uani 1 1 d . . . H26A H 0.0511 1.1945 0.3466 0.104 Uiso 1 1 calc R . . C27 C 0.1081(8) 1.2461(5) 0.3797(7) 0.120(6) Uani 1 1 d . . . H27A H 0.0869 1.2805 0.3752 0.144 Uiso 1 1 calc R . . C28 C 0.1574(10) 1.2480(6) 0.4048(9) 0.147(8) Uani 1 1 d . . . H28A H 0.1686 1.2825 0.4190 0.176 Uiso 1 1 calc R . . C29 C 0.1922(6) 1.1956(7) 0.4091(7) 0.126(7) Uani 1 1 d . . . H29A H 0.2266 1.1940 0.4260 0.152 Uiso 1 1 calc R . . C30 C 0.1707(6) 1.1487(6) 0.3867(5) 0.090(4) Uani 1 1 d . . . H30A H 0.1925 1.1142 0.3888 0.108 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 W1 0.0421(3) 0.0346(3) 0.0441(4) 0.000 0.000 0.0009(2) W2 0.0509(4) 0.0401(3) 0.0498(5) 0.000 0.000 0.0057(2) Br1 0.0667(7) 0.0705(7) 0.0900(9) -0.0088(6) -0.0143(6) 0.0150(6) Br2 0.0939(8) 0.0494(6) 0.0776(8) 0.0090(5) 0.0212(6) 0.0049(6) Cu1 0.0603(7) 0.0461(6) 0.0654(8) -0.0056(7) 0.0029(7) -0.0100(6) Cu2 0.0540(7) 0.0467(7) 0.0733(10) 0.0021(7) 0.0061(7) 0.0101(5) Cu3 0.0624(8) 0.0490(7) 0.0722(8) -0.0001(8) 0.0066(8) 0.0113(6) Cu4 0.0593(8) 0.0543(8) 0.0873(12) 0.0139(8) -0.0106(7) 0.0024(6) S1 0.0587(19) 0.0367(13) 0.0578(17) 0.0025(12) 0.0139(14) -0.0008(11) S2 0.0522(17) 0.0515(18) 0.0567(18) -0.0163(14) -0.0001(12) 0.0023(12) S3 0.071(2) 0.0498(17) 0.0623(19) 0.0067(13) -0.0154(16) 0.0047(13) S4 0.0567(19) 0.063(2) 0.067(2) -0.0188(17) 0.0056(14) 0.0041(14) N1 0.079(6) 0.043(5) 0.079(6) -0.007(4) -0.002(5) -0.002(4) N2 0.060(6) 0.050(5) 0.072(6) -0.006(5) 0.003(5) -0.016(5) N3 0.069(6) 0.052(5) 0.071(5) 0.004(4) 0.009(4) 0.012(4) N4 0.060(6) 0.069(7) 0.073(7) 0.001(5) 0.013(5) -0.002(5) N5 0.076(7) 0.064(6) 0.081(6) 0.022(5) -0.008(5) -0.019(5) N6 0.055(5) 0.050(5) 0.096(7) 0.009(5) -0.006(5) -0.008(4) C1 0.070(7) 0.073(7) 0.063(6) 0.003(5) 0.015(5) 0.002(5) C2 0.095(9) 0.088(9) 0.087(8) 0.028(7) 0.025(7) -0.002(7) C3 0.139(13) 0.078(9) 0.073(8) 0.017(7) 0.001(8) -0.026(8) C4 0.192(19) 0.037(7) 0.132(13) 0.001(7) 0.034(12) 0.001(8) C5 0.129(12) 0.067(8) 0.099(9) 0.001(7) 0.035(8) 0.016(8) C6 0.091(9) 0.061(7) 0.081(8) 0.004(5) -0.009(6) -0.013(6) C7 0.078(10) 0.114(14) 0.173(16) 0.030(12) -0.061(10) -0.019(8) C8 0.109(14) 0.110(16) 0.24(3) 0.033(16) -0.094(15) -0.057(12) C9 0.135(15) 0.102(12) 0.20(2) -0.053(12) -0.057(14) -0.021(11) C10 0.091(9) 0.069(8) 0.135(12) -0.019(8) -0.010(8) -0.013(7) C11 0.097(10) 0.095(10) 0.087(9) -0.025(7) -0.023(7) 0.037(8) C12 0.175(18) 0.111(12) 0.088(10) -0.042(9) -0.024(10) 0.027(12) C13 0.151(17) 0.088(12) 0.148(15) -0.042(11) 0.024(12) 0.035(11) C14 0.147(18) 0.098(13) 0.22(2) -0.055(14) 0.073(16) 0.010(12) C15 0.055(8) 0.079(9) 0.187(15) -0.061(10) 0.025(9) 0.011(6) C16 0.056(7) 0.082(8) 0.111(9) 0.012(7) 0.019(6) 0.019(6) C17 0.083(9) 0.107(12) 0.140(14) 0.013(10) 0.042(9) 0.029(8) C18 0.087(11) 0.125(15) 0.121(13) -0.043(11) 0.047(10) -0.009(10) C19 0.088(10) 0.147(15) 0.087(9) -0.014(9) 0.023(8) -0.007(10) C20 0.080(8) 0.112(10) 0.067(7) 0.007(7) 0.018(6) -0.015(7) C21 0.056(7) 0.107(9) 0.076(7) 0.001(7) 0.001(5) 0.004(6) C22 0.082(10) 0.127(14) 0.105(12) -0.001(9) 0.025(8) -0.023(9) C23 0.149(17) 0.129(16) 0.115(15) 0.000(12) 0.042(13) -0.024(13) C24 0.23(2) 0.136(16) 0.068(9) 0.010(10) 0.026(12) -0.070(16) C25 0.149(15) 0.105(12) 0.105(12) 0.036(10) -0.013(11) -0.029(10) C26 0.072(8) 0.060(7) 0.128(10) 0.007(7) -0.021(7) 0.009(6) C27 0.112(14) 0.053(8) 0.193(18) -0.009(9) -0.002(12) 0.001(8) C28 0.125(17) 0.081(13) 0.23(2) 0.002(13) 0.004(16) -0.017(10) C29 0.059(8) 0.086(10) 0.23(2) -0.028(12) 0.000(10) -0.027(7) C30 0.062(8) 0.083(9) 0.125(11) -0.004(8) 0.018(7) -0.005(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 W1 S2 2.232(3) . ? W1 S2 2.232(3) 2_565 ? W1 S1 2.242(3) 2_565 ? W1 S1 2.242(3) . ? W1 Cu1 2.6879(12) 2_565 ? W1 Cu1 2.6879(12) . ? W1 Cu2 2.7300(11) . ? W1 Cu2 2.7300(11) 2_565 ? W2 S3 2.230(3) . ? W2 S3 2.230(3) 2_575 ? W2 S4 2.252(3) . ? W2 S4 2.252(3) 2_575 ? W2 Cu4 2.6805(13) 2_575 ? W2 Cu4 2.6805(13) . ? W2 Cu3 2.7134(12) . ? W2 Cu3 2.7134(12) 2_575 ? Br1 Cu2 2.4653(17) . ? Br2 Cu3 2.4560(17) . ? Cu1 N2 2.051(9) . ? Cu1 N1 2.109(9) . ? Cu1 S2 2.282(3) . ? Cu1 S1 2.295(3) . ? Cu2 N3 2.066(9) . ? Cu2 S2 2.304(3) 2_565 ? Cu2 S1 2.311(3) . ? Cu3 N4 2.071(9) . ? Cu3 S3 2.310(3) . ? Cu3 S4 2.335(4) . ? Cu4 N6 2.021(9) . ? Cu4 N5 2.111(10) . ? Cu4 S4 2.286(3) 2_575 ? Cu4 S3 2.294(3) . ? S2 Cu2 2.304(3) 2_565 ? S4 Cu4 2.286(3) 2_575 ? N1 C5 1.298(13) . ? N1 C1 1.328(14) . ? N2 C10 1.299(13) . ? N2 C6 1.346(14) . ? N3 C15 1.304(13) . ? N3 C11 1.355(15) . ? N4 C20 1.314(14) . ? N4 C16 1.330(13) . ? N5 C25 1.292(16) . ? N5 C21 1.322(14) . ? N6 C26 1.342(13) . ? N6 C30 1.349(14) . ? C1 C2 1.350(14) . ? C2 C3 1.354(17) . ? C3 C4 1.331(19) . ? C4 C5 1.425(17) . ? C6 C7 1.349(16) . ? C7 C8 1.34(3) . ? C8 C9 1.38(2) . ? C9 C10 1.427(18) . ? C11 C12 1.354(17) . ? C12 C13 1.37(2) . ? C13 C14 1.35(2) . ? C14 C15 1.366(19) . ? C16 C17 1.377(16) . ? C17 C18 1.35(2) . ? C18 C19 1.34(2) . ? C19 C20 1.329(16) . ? C21 C22 1.360(17) . ? C22 C23 1.25(2) . ? C23 C24 1.33(3) . ? C24 C25 1.56(3) . ? C26 C27 1.377(17) . ? C27 C28 1.35(3) . ? C28 C29 1.44(2) . ? C29 C30 1.357(18) . ? 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 S2 W1 S2 111.05(16) . 2_565 ? S2 W1 S1 108.39(9) . 2_565 ? S2 W1 S1 108.89(10) 2_565 2_565 ? S2 W1 S1 108.89(10) . . ? S2 W1 S1 108.39(9) 2_565 . ? S1 W1 S1 111.23(16) 2_565 . ? S2 W1 Cu1 126.78(8) . 2_565 ? S2 W1 Cu1 54.33(8) 2_565 2_565 ? S1 W1 Cu1 54.59(7) 2_565 2_565 ? S1 W1 Cu1 124.32(7) . 2_565 ? S2 W1 Cu1 54.33(8) . . ? S2 W1 Cu1 126.78(8) 2_565 . ? S1 W1 Cu1 124.32(7) 2_565 . ? S1 W1 Cu1 54.59(7) . . ? Cu1 W1 Cu1 178.42(7) 2_565 . ? S2 W1 Cu2 122.05(8) . . ? S2 W1 Cu2 54.22(7) 2_565 . ? S1 W1 Cu2 129.56(8) 2_565 . ? S1 W1 Cu2 54.34(7) . . ? Cu1 W1 Cu2 91.61(4) 2_565 . ? Cu1 W1 Cu2 88.47(4) . . ? S2 W1 Cu2 54.22(7) . 2_565 ? S2 W1 Cu2 122.05(8) 2_565 2_565 ? S1 W1 Cu2 54.34(7) 2_565 2_565 ? S1 W1 Cu2 129.56(8) . 2_565 ? Cu1 W1 Cu2 88.47(4) 2_565 2_565 ? Cu1 W1 Cu2 91.61(4) . 2_565 ? Cu2 W1 Cu2 174.53(6) . 2_565 ? S3 W2 S3 109.36(18) . 2_575 ? S3 W2 S4 109.68(11) . . ? S3 W2 S4 109.05(10) 2_575 . ? S3 W2 S4 109.05(10) . 2_575 ? S3 W2 S4 109.68(11) 2_575 2_575 ? S4 W2 S4 110.01(18) . 2_575 ? S3 W2 Cu4 128.29(9) . 2_575 ? S3 W2 Cu4 54.78(8) 2_575 2_575 ? S4 W2 Cu4 54.39(8) . 2_575 ? S4 W2 Cu4 122.66(8) 2_575 2_575 ? S3 W2 Cu4 54.78(8) . . ? S3 W2 Cu4 128.29(9) 2_575 . ? S4 W2 Cu4 122.66(8) . . ? S4 W2 Cu4 54.39(8) 2_575 . ? Cu4 W2 Cu4 175.74(7) 2_575 . ? S3 W2 Cu3 54.68(8) . . ? S3 W2 Cu3 121.22(8) 2_575 . ? S4 W2 Cu3 55.16(9) . . ? S4 W2 Cu3 129.10(8) 2_575 . ? Cu4 W2 Cu3 89.59(4) 2_575 . ? Cu4 W2 Cu3 90.63(4) . . ? S3 W2 Cu3 121.22(8) . 2_575 ? S3 W2 Cu3 54.68(8) 2_575 2_575 ? S4 W2 Cu3 129.09(8) . 2_575 ? S4 W2 Cu3 55.16(9) 2_575 2_575 ? Cu4 W2 Cu3 90.63(4) 2_575 2_575 ? Cu4 W2 Cu3 89.59(4) . 2_575 ? Cu3 W2 Cu3 174.08(7) . 2_575 ? N2 Cu1 N1 97.2(3) . . ? N2 Cu1 S2 111.1(3) . . ? N1 Cu1 S2 119.8(3) . . ? N2 Cu1 S1 118.7(3) . . ? N1 Cu1 S1 105.3(3) . . ? S2 Cu1 S1 105.33(10) . . ? N2 Cu1 W1 135.0(2) . . ? N1 Cu1 W1 127.7(3) . . ? S2 Cu1 W1 52.59(7) . . ? S1 Cu1 W1 52.76(7) . . ? N3 Cu2 S2 120.2(3) . 2_565 ? N3 Cu2 S1 102.7(3) . . ? S2 Cu2 S1 103.64(10) 2_565 . ? N3 Cu2 Br1 102.5(3) . . ? S2 Cu2 Br1 105.92(10) 2_565 . ? S1 Cu2 Br1 123.31(9) . . ? N3 Cu2 W1 129.1(3) . . ? S2 Cu2 W1 51.79(7) 2_565 . ? S1 Cu2 W1 52.00(7) . . ? Br1 Cu2 W1 128.46(6) . . ? N4 Cu3 S3 118.7(3) . . ? N4 Cu3 S4 104.3(3) . . ? S3 Cu3 S4 104.12(11) . . ? N4 Cu3 Br2 103.8(3) . . ? S3 Cu3 Br2 105.51(10) . . ? S4 Cu3 Br2 121.39(10) . . ? N4 Cu3 W2 129.5(3) . . ? S3 Cu3 W2 51.94(8) . . ? S4 Cu3 W2 52.32(8) . . ? Br2 Cu3 W2 126.64(6) . . ? N6 Cu4 N5 101.3(4) . . ? N6 Cu4 S4 114.9(3) . 2_575 ? N5 Cu4 S4 112.2(3) . 2_575 ? N6 Cu4 S3 115.6(3) . . ? N5 Cu4 S3 107.1(3) . . ? S4 Cu4 S3 105.64(12) 2_575 . ? N6 Cu4 W2 137.9(3) . . ? N5 Cu4 W2 120.8(3) . . ? S4 Cu4 W2 53.20(8) 2_575 . ? S3 Cu4 W2 52.56(8) . . ? W1 S1 Cu1 72.65(9) . . ? W1 S1 Cu2 73.66(9) . . ? Cu1 S1 Cu2 110.27(13) . . ? W1 S2 Cu1 73.08(9) . . ? W1 S2 Cu2 73.99(9) . 2_565 ? Cu1 S2 Cu2 115.76(14) . 2_565 ? W2 S3 Cu4 72.66(9) . . ? W2 S3 Cu3 73.38(10) . . ? Cu4 S3 Cu3 112.79(15) . . ? W2 S4 Cu4 72.41(9) . 2_575 ? W2 S4 Cu3 72.52(10) . . ? Cu4 S4 Cu3 110.65(15) 2_575 . ? C5 N1 C1 118.9(10) . . ? C5 N1 Cu1 122.6(9) . . ? C1 N1 Cu1 118.4(7) . . ? C10 N2 C6 118.4(10) . . ? C10 N2 Cu1 119.7(9) . . ? C6 N2 Cu1 121.8(7) . . ? C15 N3 C11 117.2(11) . . ? C15 N3 Cu2 121.1(9) . . ? C11 N3 Cu2 121.3(8) . . ? C20 N4 C16 115.8(11) . . ? C20 N4 Cu3 122.9(9) . . ? C16 N4 Cu3 121.3(8) . . ? C25 N5 C21 120.0(13) . . ? C25 N5 Cu4 119.4(11) . . ? C21 N5 Cu4 120.6(8) . . ? C26 N6 C30 116.7(10) . . ? C26 N6 Cu4 120.7(8) . . ? C30 N6 Cu4 122.4(8) . . ? N1 C1 C2 122.8(11) . . ? C1 C2 C3 118.5(12) . . ? C4 C3 C2 120.6(12) . . ? C3 C4 C5 117.7(12) . . ? N1 C5 C4 121.2(12) . . ? N2 C6 C7 123.6(13) . . ? C8 C7 C6 119.4(15) . . ? C7 C8 C9 119.2(14) . . ? C8 C9 C10 118.2(15) . . ? N2 C10 C9 121.1(13) . . ? C12 C11 N3 121.6(13) . . ? C11 C12 C13 121.0(15) . . ? C14 C13 C12 116.0(15) . . ? C13 C14 C15 121.2(18) . . ? N3 C15 C14 122.7(16) . . ? N4 C16 C17 121.6(13) . . ? C18 C17 C16 118.4(15) . . ? C19 C18 C17 120.7(14) . . ? C20 C19 C18 116.5(15) . . ? N4 C20 C19 126.8(14) . . ? N5 C21 C22 124.1(13) . . ? C23 C22 C21 121.3(18) . . ? C22 C23 C24 120.3(19) . . ? C23 C24 C25 119.1(15) . . ? N5 C25 C24 115.1(15) . . ? N6 C26 C27 120.0(12) . . ? C28 C27 C26 122.6(14) . . ? C27 C28 C29 118.5(17) . . ? C30 C29 C28 114.5(16) . . ? N6 C30 C29 127.2(13) . . ? 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 S2 W1 Cu1 N2 82.8(4) . . . . ? S2 W1 Cu1 N2 -8.0(4) 2_565 . . . ? S1 W1 Cu1 N2 171.7(4) 2_565 . . . ? S1 W1 Cu1 N2 -95.3(4) . . . . ? Cu1 W1 Cu1 N2 -142.2(4) 2_565 . . . ? Cu2 W1 Cu1 N2 -49.4(4) . . . . ? Cu2 W1 Cu1 N2 125.1(4) 2_565 . . . ? S2 W1 Cu1 N1 -101.5(4) . . . . ? S2 W1 Cu1 N1 167.6(3) 2_565 . . . ? S1 W1 Cu1 N1 -12.6(4) 2_565 . . . ? S1 W1 Cu1 N1 80.4(4) . . . . ? Cu1 W1 Cu1 N1 33.5(3) 2_565 . . . ? Cu2 W1 Cu1 N1 126.2(3) . . . . ? Cu2 W1 Cu1 N1 -59.3(3) 2_565 . . . ? S2 W1 Cu1 S2 -90.88(19) 2_565 . . . ? S1 W1 Cu1 S2 88.86(13) 2_565 . . . ? S1 W1 Cu1 S2 -178.12(14) . . . . ? Cu1 W1 Cu1 S2 134.97(9) 2_565 . . . ? Cu2 W1 Cu1 S2 -132.27(10) . . . . ? Cu2 W1 Cu1 S2 42.26(10) 2_565 . . . ? S2 W1 Cu1 S1 178.12(14) . . . . ? S2 W1 Cu1 S1 87.24(13) 2_565 . . . ? S1 W1 Cu1 S1 -93.02(19) 2_565 . . . ? Cu1 W1 Cu1 S1 -46.91(10) 2_565 . . . ? Cu2 W1 Cu1 S1 45.85(10) . . . . ? Cu2 W1 Cu1 S1 -139.62(10) 2_565 . . . ? S2 W1 Cu2 N3 -165.3(3) . . . . ? S2 W1 Cu2 N3 100.6(3) 2_565 . . . ? S1 W1 Cu2 N3 15.1(3) 2_565 . . . ? S1 W1 Cu2 N3 -74.1(3) . . . . ? Cu1 W1 Cu2 N3 58.3(3) 2_565 . . . ? Cu1 W1 Cu2 N3 -120.1(3) . . . . ? Cu2 W1 Cu2 N3 149.0(3) 2_565 . . . ? S2 W1 Cu2 S2 94.1(2) . . . 2_565 ? S1 W1 Cu2 S2 -85.55(14) 2_565 . . 2_565 ? S1 W1 Cu2 S2 -174.71(14) . . . 2_565 ? Cu1 W1 Cu2 S2 -42.33(11) 2_565 . . 2_565 ? Cu1 W1 Cu2 S2 139.25(11) . . . 2_565 ? Cu2 W1 Cu2 S2 48.39(10) 2_565 . . 2_565 ? S2 W1 Cu2 S1 -91.20(13) . . . . ? S2 W1 Cu2 S1 174.71(14) 2_565 . . . ? S1 W1 Cu2 S1 89.16(19) 2_565 . . . ? Cu1 W1 Cu2 S1 132.39(10) 2_565 . . . ? Cu1 W1 Cu2 S1 -46.03(10) . . . . ? Cu2 W1 Cu2 S1 -136.90(9) 2_565 . . . ? S2 W1 Cu2 Br1 14.43(13) . . . . ? S2 W1 Cu2 Br1 -79.66(12) 2_565 . . . ? S1 W1 Cu2 Br1 -165.21(11) 2_565 . . . ? S1 W1 Cu2 Br1 105.63(12) . . . . ? Cu1 W1 Cu2 Br1 -121.98(8) 2_565 . . . ? Cu1 W1 Cu2 Br1 59.59(8) . . . . ? Cu2 W1 Cu2 Br1 -31.27(7) 2_565 . . . ? S3 W2 Cu3 N4 -98.3(4) . . . . ? S3 W2 Cu3 N4 169.1(4) 2_575 . . . ? S4 W2 Cu3 N4 76.6(4) . . . . ? S4 W2 Cu3 N4 -11.8(4) 2_575 . . . ? Cu4 W2 Cu3 N4 121.8(4) 2_575 . . . ? Cu4 W2 Cu3 N4 -53.9(4) . . . . ? Cu3 W2 Cu3 N4 -146.0(4) 2_575 . . . ? S3 W2 Cu3 S3 -92.6(2) 2_575 . . . ? S4 W2 Cu3 S3 174.92(16) . . . . ? S4 W2 Cu3 S3 86.54(15) 2_575 . . . ? Cu4 W2 Cu3 S3 -139.87(12) 2_575 . . . ? Cu4 W2 Cu3 S3 44.39(11) . . . . ? Cu3 W2 Cu3 S3 -47.71(11) 2_575 . . . ? S3 W2 Cu3 S4 -174.92(16) . . . . ? S3 W2 Cu3 S4 92.47(14) 2_575 . . . ? S4 W2 Cu3 S4 -88.4(2) 2_575 . . . ? Cu4 W2 Cu3 S4 45.21(11) 2_575 . . . ? Cu4 W2 Cu3 S4 -130.53(11) . . . . ? Cu3 W2 Cu3 S4 137.37(10) 2_575 . . . ? S3 W2 Cu3 Br2 80.84(14) . . . . ? S3 W2 Cu3 Br2 -11.77(14) 2_575 . . . ? S4 W2 Cu3 Br2 -104.24(12) . . . . ? S4 W2 Cu3 Br2 167.39(13) 2_575 . . . ? Cu4 W2 Cu3 Br2 -59.02(9) 2_575 . . . ? Cu4 W2 Cu3 Br2 125.23(9) . . . . ? Cu3 W2 Cu3 Br2 33.13(8) 2_575 . . . ? S3 W2 Cu4 N6 -88.0(4) . . . . ? S3 W2 Cu4 N6 -0.3(4) 2_575 . . . ? S4 W2 Cu4 N6 179.9(4) . . . . ? S4 W2 Cu4 N6 87.6(4) 2_575 . . . ? Cu4 W2 Cu4 N6 134.8(4) 2_575 . . . ? Cu3 W2 Cu4 N6 -132.3(4) . . . . ? Cu3 W2 Cu4 N6 41.8(4) 2_575 . . . ? S3 W2 Cu4 N5 88.5(3) . . . . ? S3 W2 Cu4 N5 176.2(3) 2_575 . . . ? S4 W2 Cu4 N5 -3.6(3) . . . . ? S4 W2 Cu4 N5 -95.9(3) 2_575 . . . ? Cu4 W2 Cu4 N5 -48.7(3) 2_575 . . . ? Cu3 W2 Cu4 N5 44.2(3) . . . . ? Cu3 W2 Cu4 N5 -141.7(3) 2_575 . . . ? S3 W2 Cu4 S4 -175.53(15) . . . 2_575 ? S3 W2 Cu4 S4 -87.84(16) 2_575 . . 2_575 ? S4 W2 Cu4 S4 92.3(2) . . . 2_575 ? Cu4 W2 Cu4 S4 47.22(11) 2_575 . . 2_575 ? Cu3 W2 Cu4 S4 140.16(12) . . . 2_575 ? Cu3 W2 Cu4 S4 -45.76(12) 2_575 . . 2_575 ? S3 W2 Cu4 S3 87.7(2) 2_575 . . . ? S4 W2 Cu4 S3 -92.13(15) . . . . ? S4 W2 Cu4 S3 175.53(15) 2_575 . . . ? Cu4 W2 Cu4 S3 -137.26(11) 2_575 . . . ? Cu3 W2 Cu4 S3 -44.32(11) . . . . ? Cu3 W2 Cu4 S3 129.76(11) 2_575 . . . ? S2 W1 S1 Cu1 -1.61(12) . . . . ? S2 W1 S1 Cu1 -122.54(10) 2_565 . . . ? S1 W1 S1 Cu1 117.78(9) 2_565 . . . ? Cu1 W1 S1 Cu1 178.60(6) 2_565 . . . ? Cu2 W1 S1 Cu1 -118.02(11) . . . . ? Cu2 W1 S1 Cu1 57.14(12) 2_565 . . . ? S2 W1 S1 Cu2 116.41(10) . . . . ? S2 W1 S1 Cu2 -4.52(12) 2_565 . . . ? S1 W1 S1 Cu2 -124.21(9) 2_565 . . . ? Cu1 W1 S1 Cu2 -63.38(10) 2_565 . . . ? Cu1 W1 S1 Cu2 118.02(11) . . . . ? Cu2 W1 S1 Cu2 175.16(6) 2_565 . . . ? N2 Cu1 S1 W1 126.6(3) . . . . ? N1 Cu1 S1 W1 -126.0(3) . . . . ? S2 Cu1 S1 W1 1.55(12) . . . . ? N2 Cu1 S1 Cu2 62.1(3) . . . . ? N1 Cu1 S1 Cu2 169.5(3) . . . . ? S2 Cu1 S1 Cu2 -63.02(15) . . . . ? W1 Cu1 S1 Cu2 -64.56(9) . . . . ? N3 Cu2 S1 W1 130.1(3) . . . . ? S2 Cu2 S1 W1 4.27(11) 2_565 . . . ? Br1 Cu2 S1 W1 -115.53(9) . . . . ? N3 Cu2 S1 Cu1 -166.0(3) . . . . ? S2 Cu2 S1 Cu1 68.20(14) 2_565 . . . ? Br1 Cu2 S1 Cu1 -51.60(15) . . . . ? W1 Cu2 S1 Cu1 63.93(10) . . . . ? S2 W1 S2 Cu1 120.90(9) 2_565 . . . ? S1 W1 S2 Cu1 -119.53(9) 2_565 . . . ? S1 W1 S2 Cu1 1.62(12) . . . . ? Cu1 W1 S2 Cu1 -178.60(6) 2_565 . . . ? Cu2 W1 S2 Cu1 60.77(11) . . . . ? Cu2 W1 S2 Cu1 -124.05(11) 2_565 . . . ? S2 W1 S2 Cu2 -115.05(10) 2_565 . . 2_565 ? S1 W1 S2 Cu2 4.52(12) 2_565 . . 2_565 ? S1 W1 S2 Cu2 125.67(10) . . . 2_565 ? Cu1 W1 S2 Cu2 -54.55(11) 2_565 . . 2_565 ? Cu1 W1 S2 Cu2 124.05(11) . . . 2_565 ? Cu2 W1 S2 Cu2 -175.18(6) . . . 2_565 ? N2 Cu1 S2 W1 -131.2(3) . . . . ? N1 Cu1 S2 W1 116.7(3) . . . . ? S1 Cu1 S2 W1 -1.55(12) . . . . ? N2 Cu1 S2 Cu2 166.6(3) . . . 2_565 ? N1 Cu1 S2 Cu2 54.5(3) . . . 2_565 ? S1 Cu1 S2 Cu2 -63.71(16) . . . 2_565 ? W1 Cu1 S2 Cu2 -62.16(10) . . . 2_565 ? S3 W2 S3 Cu4 -123.77(10) 2_575 . . . ? S4 W2 S3 Cu4 116.68(11) . . . . ? S4 W2 S3 Cu4 -3.85(13) 2_575 . . . ? Cu4 W2 S3 Cu4 176.32(7) 2_575 . . . ? Cu3 W2 S3 Cu4 121.11(12) . . . . ? Cu3 W2 S3 Cu4 -64.01(11) 2_575 . . . ? S3 W2 S3 Cu3 115.12(10) 2_575 . . . ? S4 W2 S3 Cu3 -4.43(14) . . . . ? S4 W2 S3 Cu3 -124.96(11) 2_575 . . . ? Cu4 W2 S3 Cu3 55.21(13) 2_575 . . . ? Cu4 W2 S3 Cu3 -121.11(12) . . . . ? Cu3 W2 S3 Cu3 174.88(6) 2_575 . . . ? N6 Cu4 S3 W2 132.0(3) . . . . ? N5 Cu4 S3 W2 -116.1(3) . . . . ? S4 Cu4 S3 W2 3.72(13) 2_575 . . . ? N6 Cu4 S3 Cu3 -165.2(3) . . . . ? N5 Cu4 S3 Cu3 -53.2(3) . . . . ? S4 Cu4 S3 Cu3 66.58(17) 2_575 . . . ? W2 Cu4 S3 Cu3 62.86(11) . . . . ? N4 Cu3 S3 W2 119.5(3) . . . . ? S4 Cu3 S3 W2 4.14(13) . . . . ? Br2 Cu3 S3 W2 -124.70(8) . . . . ? N4 Cu3 S3 Cu4 57.1(3) . . . . ? S4 Cu3 S3 Cu4 -58.29(17) . . . . ? Br2 Cu3 S3 Cu4 172.87(11) . . . . ? W2 Cu3 S3 Cu4 -62.43(11) . . . . ? S3 W2 S4 Cu4 123.60(12) . . . 2_575 ? S3 W2 S4 Cu4 3.87(13) 2_575 . . 2_575 ? S4 W2 S4 Cu4 -116.46(11) 2_575 . . 2_575 ? Cu4 W2 S4 Cu4 -176.29(7) . . . 2_575 ? Cu3 W2 S4 Cu4 119.20(12) . . . 2_575 ? Cu3 W2 S4 Cu4 -55.64(13) 2_575 . . 2_575 ? S3 W2 S4 Cu3 4.40(13) . . . . ? S3 W2 S4 Cu3 -115.33(11) 2_575 . . . ? S4 W2 S4 Cu3 124.35(10) 2_575 . . . ? Cu4 W2 S4 Cu3 -119.20(12) 2_575 . . . ? Cu4 W2 S4 Cu3 64.52(11) . . . . ? Cu3 W2 S4 Cu3 -174.83(6) 2_575 . . . ? N4 Cu3 S4 W2 -129.2(3) . . . . ? S3 Cu3 S4 W2 -4.12(13) . . . . ? Br2 Cu3 S4 W2 114.33(9) . . . . ? N4 Cu3 S4 Cu4 168.0(3) . . . 2_575 ? S3 Cu3 S4 Cu4 -66.91(17) . . . 2_575 ? Br2 Cu3 S4 Cu4 51.54(17) . . . 2_575 ? W2 Cu3 S4 Cu4 -62.79(11) . . . 2_575 ? N2 Cu1 N1 C5 -79.9(11) . . . . ? S2 Cu1 N1 C5 39.5(11) . . . . ? S1 Cu1 N1 C5 157.7(10) . . . . ? W1 Cu1 N1 C5 103.2(10) . . . . ? N2 Cu1 N1 C1 96.1(9) . . . . ? S2 Cu1 N1 C1 -144.6(8) . . . . ? S1 Cu1 N1 C1 -26.3(9) . . . . ? W1 Cu1 N1 C1 -80.8(9) . . . . ? N1 Cu1 N2 C10 60.3(10) . . . . ? S2 Cu1 N2 C10 -65.6(10) . . . . ? S1 Cu1 N2 C10 172.2(9) . . . . ? W1 Cu1 N2 C10 -123.2(9) . . . . ? N1 Cu1 N2 C6 -119.6(9) . . . . ? S2 Cu1 N2 C6 114.6(8) . . . . ? S1 Cu1 N2 C6 -7.7(10) . . . . ? W1 Cu1 N2 C6 57.0(10) . . . . ? S2 Cu2 N3 C15 -143.8(10) 2_565 . . . ? S1 Cu2 N3 C15 102.0(10) . . . . ? Br1 Cu2 N3 C15 -26.8(11) . . . . ? W1 Cu2 N3 C15 152.9(10) . . . . ? S2 Cu2 N3 C11 43.5(10) 2_565 . . . ? S1 Cu2 N3 C11 -70.7(9) . . . . ? Br1 Cu2 N3 C11 160.5(9) . . . . ? W1 Cu2 N3 C11 -19.7(10) . . . . ? S3 Cu3 N4 C20 -84.8(10) . . . . ? S4 Cu3 N4 C20 30.5(10) . . . . ? Br2 Cu3 N4 C20 158.5(9) . . . . ? W2 Cu3 N4 C20 -22.2(11) . . . . ? S3 Cu3 N4 C16 95.2(9) . . . . ? S4 Cu3 N4 C16 -149.5(9) . . . . ? Br2 Cu3 N4 C16 -21.4(9) . . . . ? W2 Cu3 N4 C16 157.9(8) . . . . ? N6 Cu4 N5 C25 -86.9(10) . . . . ? S4 Cu4 N5 C25 36.2(10) 2_575 . . . ? S3 Cu4 N5 C25 151.7(10) . . . . ? W2 Cu4 N5 C25 95.5(10) . . . . ? N6 Cu4 N5 C21 91.3(10) . . . . ? S4 Cu4 N5 C21 -145.6(9) 2_575 . . . ? S3 Cu4 N5 C21 -30.1(10) . . . . ? W2 Cu4 N5 C21 -86.3(9) . . . . ? N5 Cu4 N6 C26 126.1(9) . . . . ? S4 Cu4 N6 C26 4.9(10) 2_575 . . . ? S3 Cu4 N6 C26 -118.6(9) . . . . ? W2 Cu4 N6 C26 -57.0(11) . . . . ? N5 Cu4 N6 C30 -59.7(10) . . . . ? S4 Cu4 N6 C30 179.1(8) 2_575 . . . ? S3 Cu4 N6 C30 55.6(10) . . . . ? W2 Cu4 N6 C30 117.2(9) . . . . ? C5 N1 C1 C2 -4.2(18) . . . . ? Cu1 N1 C1 C2 179.6(9) . . . . ? N1 C1 C2 C3 5(2) . . . . ? C1 C2 C3 C4 -5(2) . . . . ? C2 C3 C4 C5 5(3) . . . . ? C1 N1 C5 C4 4(2) . . . . ? Cu1 N1 C5 C4 179.9(11) . . . . ? C3 C4 C5 N1 -4(2) . . . . ? C10 N2 C6 C7 -2.0(19) . . . . ? Cu1 N2 C6 C7 177.8(11) . . . . ? N2 C6 C7 C8 2(3) . . . . ? C6 C7 C8 C9 0(3) . . . . ? C7 C8 C9 C10 -1(3) . . . . ? C6 N2 C10 C9 1(2) . . . . ? Cu1 N2 C10 C9 -179.0(12) . . . . ? C8 C9 C10 N2 1(3) . . . . ? C15 N3 C11 C12 3.1(19) . . . . ? Cu2 N3 C11 C12 176.1(11) . . . . ? N3 C11 C12 C13 0(2) . . . . ? C11 C12 C13 C14 -5(3) . . . . ? C12 C13 C14 C15 6(3) . . . . ? C11 N3 C15 C14 -2(2) . . . . ? Cu2 N3 C15 C14 -174.7(13) . . . . ? C13 C14 C15 N3 -3(3) . . . . ? C20 N4 C16 C17 1.5(19) . . . . ? Cu3 N4 C16 C17 -178.5(12) . . . . ? N4 C16 C17 C18 -6(2) . . . . ? C16 C17 C18 C19 7(3) . . . . ? C17 C18 C19 C20 -4(3) . . . . ? C16 N4 C20 C19 2(2) . . . . ? Cu3 N4 C20 C19 -178.0(12) . . . . ? C18 C19 C20 N4 -1(2) . . . . ? C25 N5 C21 C22 -4(2) . . . . ? Cu4 N5 C21 C22 177.7(10) . . . . ? N5 C21 C22 C23 3(3) . . . . ? C21 C22 C23 C24 -1(3) . . . . ? C22 C23 C24 C25 1(3) . . . . ? C21 N5 C25 C24 4(2) . . . . ? Cu4 N5 C25 C24 -178.2(10) . . . . ? C23 C24 C25 N5 -2(3) . . . . ? C30 N6 C26 C27 7.5(19) . . . . ? Cu4 N6 C26 C27 -178.0(12) . . . . ? N6 C26 C27 C28 -8(3) . . . . ? C26 C27 C28 C29 4(3) . . . . ? C27 C28 C29 C30 0(3) . . . . ? C26 N6 C30 C29 -3(2) . . . . ? Cu4 N6 C30 C29 -177.9(13) . . . . ? C28 C29 C30 N6 0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.911 _refine_diff_density_min -0.662 _refine_diff_density_rms 0.099 #======END # CLUSTER 4 data_cluster_4 _database_code_CSD 156624 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H30 Br2 Cu4 Mo N6 S4' _chemical_formula_weight 1112.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'F d d 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 22.54960(10) _cell_length_b 22.7445(3) _cell_length_c 30.2498(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 15514.5(3) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6288 _cell_measurement_theta_min 1.44 _cell_measurement_theta_max 28.36 _exptl_crystal_description block _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.906 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8704 _exptl_absorpt_coefficient_mu 4.778 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3282 _exptl_absorpt_correction_T_max 0.3480 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Siemens SMART CCD area detector diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26474 _diffrn_reflns_av_R_equivalents 0.0457 _diffrn_reflns_av_sigmaI/netI 0.0544 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 28.30 _reflns_number_total 9414 _reflns_number_gt 6425 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1996a)' _computing_cell_refinement 'SAINT (Siemens, 1996b)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXTL (Sheldrick, 1997)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material ; SHELXTL, PARST (Nardelli, 1995) and PLATON (Spek, 1990) ; _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^)+(0.0239P)^2^+116.9016P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.051(12) _refine_ls_number_reflns 9414 _refine_ls_number_parameters 425 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0827 _refine_ls_R_factor_gt 0.0479 _refine_ls_wR_factor_ref 0.1099 _refine_ls_wR_factor_gt 0.0966 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.116 _refine_ls_shift/su_mean 0.010 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 Mo1 Mo 0.0000 0.5000 0.34607(3) 0.0419(2) Uani 1 2 d S . . Mo2 Mo 0.0000 1.0000 0.33640(3) 0.0501(3) Uani 1 2 d S . . Br1 Br 0.17527(4) 0.42762(4) 0.40676(4) 0.0765(3) Uani 1 1 d . . . Br2 Br 0.07186(5) 0.82876(4) 0.39786(3) 0.0751(3) Uani 1 1 d . . . Cu1 Cu 0.07255(5) 0.59294(4) 0.34512(3) 0.0588(2) Uani 1 1 d . . . Cu2 Cu 0.09691(4) 0.42961(4) 0.35004(3) 0.0590(3) Uani 1 1 d . . . Cu3 Cu 0.07228(5) 0.90586(4) 0.34088(4) 0.0646(3) Uani 1 1 d . . . Cu4 Cu 0.09319(5) 1.07178(5) 0.33350(4) 0.0692(3) Uani 1 1 d . . . S1 S 0.08177(10) 0.50912(9) 0.30468(7) 0.0544(5) Uani 1 1 d . . . S2 S -0.00921(9) 0.58053(10) 0.38771(7) 0.0558(5) Uani 1 1 d . . . S3 S 0.08071(11) 0.99290(10) 0.37884(8) 0.0627(6) Uani 1 1 d . . . S4 S -0.00805(10) 0.91912(12) 0.29451(8) 0.0671(6) Uani 1 1 d . . . N1 N 0.0746(4) 0.6621(3) 0.2988(2) 0.070(2) Uani 1 1 d . . . N2 N 0.1438(3) 0.6193(3) 0.3825(2) 0.0615(18) Uani 1 1 d . . . N3 N 0.1239(3) 0.3645(3) 0.3064(2) 0.0654(18) Uani 1 1 d . . . N4 N 0.1402(3) 0.8798(3) 0.2995(3) 0.073(2) Uani 1 1 d . . . N5 N 0.1655(3) 1.0539(4) 0.2939(2) 0.077(2) Uani 1 1 d . . . N6 N 0.1219(3) 1.1458(3) 0.3629(3) 0.072(2) Uani 1 1 d . . . C1 C 0.1017(4) 0.6527(4) 0.2596(3) 0.065(2) Uani 1 1 d . . . H1A H 0.1175 0.6159 0.2532 0.078 Uiso 1 1 calc R . . C2 C 0.1063(5) 0.6969(5) 0.2292(3) 0.086(3) Uani 1 1 d . . . H2A H 0.1273 0.6905 0.2031 0.103 Uiso 1 1 calc R . . C3 C 0.0808(6) 0.7495(5) 0.2366(4) 0.106(4) Uani 1 1 d . . . H3A H 0.0821 0.7791 0.2154 0.127 Uiso 1 1 calc R . . C4 C 0.0529(7) 0.7585(4) 0.2760(5) 0.125(5) Uani 1 1 d . . . H4A H 0.0353 0.7945 0.2822 0.149 Uiso 1 1 calc R . . C5 C 0.0512(6) 0.7144(4) 0.3058(4) 0.108(4) Uani 1 1 d . . . H5A H 0.0325 0.7213 0.3327 0.130 Uiso 1 1 calc R . . C6 C 0.1908(4) 0.5861(4) 0.3864(3) 0.079(3) Uani 1 1 d . . . H6A H 0.1908 0.5495 0.3727 0.095 Uiso 1 1 calc R . . C7 C 0.2409(5) 0.6030(7) 0.4101(5) 0.137(5) Uani 1 1 d . . . H7A H 0.2740 0.5788 0.4122 0.164 Uiso 1 1 calc R . . C8 C 0.2392(7) 0.6567(7) 0.4301(7) 0.155(8) Uani 1 1 d . . . H8A H 0.2722 0.6700 0.4455 0.186 Uiso 1 1 calc R . . C9 C 0.1896(7) 0.6913(6) 0.4278(6) 0.145(6) Uani 1 1 d . . . H9A H 0.1877 0.7270 0.4426 0.174 Uiso 1 1 calc R . . C10 C 0.1420(5) 0.6712(4) 0.4023(4) 0.102(3) Uani 1 1 d . . . H10A H 0.1085 0.6947 0.3992 0.122 Uiso 1 1 calc R . . C11 C 0.0864(5) 0.3395(5) 0.2778(3) 0.096(4) Uani 1 1 d . . . H11A H 0.0463 0.3493 0.2784 0.115 Uiso 1 1 calc R . . C12 C 0.1074(8) 0.2988(6) 0.2470(4) 0.130(5) Uani 1 1 d . . . H12A H 0.0812 0.2831 0.2263 0.155 Uiso 1 1 calc R . . C13 C 0.1626(7) 0.2821(6) 0.2464(5) 0.124(5) Uani 1 1 d . . . H13A H 0.1750 0.2513 0.2285 0.149 Uiso 1 1 calc R . . C14 C 0.2018(8) 0.3115(6) 0.2731(6) 0.155(7) Uani 1 1 d . . . H14A H 0.2424 0.3051 0.2706 0.186 Uiso 1 1 calc R . . C15 C 0.1792(5) 0.3513(5) 0.3041(5) 0.112(4) Uani 1 1 d . . . H15A H 0.2054 0.3690 0.3238 0.134 Uiso 1 1 calc R . . C16 C 0.1845(4) 0.8449(5) 0.3130(4) 0.092(3) Uani 1 1 d . . . H16A H 0.1845 0.8311 0.3419 0.110 Uiso 1 1 calc R . . C17 C 0.2299(5) 0.8291(6) 0.2852(5) 0.114(4) Uani 1 1 d . . . H17A H 0.2610 0.8061 0.2956 0.137 Uiso 1 1 calc R . . C18 C 0.2290(7) 0.8474(7) 0.2425(5) 0.126(5) Uani 1 1 d . . . H18A H 0.2585 0.8353 0.2231 0.152 Uiso 1 1 calc R . . C19 C 0.1862(6) 0.8824(7) 0.2288(4) 0.110(4) Uani 1 1 d . . . H19A H 0.1851 0.8951 0.1996 0.132 Uiso 1 1 calc R . . C20 C 0.1445(5) 0.8992(5) 0.2574(3) 0.085(3) Uani 1 1 d . . . H20A H 0.1164 0.9262 0.2477 0.102 Uiso 1 1 calc R . . C21 C 0.2092(4) 1.0201(5) 0.3044(4) 0.093(3) Uani 1 1 d . . . H21A H 0.2080 1.0049 0.3329 0.111 Uiso 1 1 calc R . . C22 C 0.2558(5) 1.0040(7) 0.2802(5) 0.106(4) Uani 1 1 d . . . H22A H 0.2840 0.9789 0.2922 0.127 Uiso 1 1 calc R . . C23 C 0.2622(8) 1.0231(9) 0.2399(7) 0.153(7) Uani 1 1 d . . . H23A H 0.2942 1.0120 0.2224 0.184 Uiso 1 1 calc R . . C24 C 0.2184(11) 1.0613(8) 0.2246(5) 0.166(8) Uani 1 1 d . . . H24A H 0.2208 1.0763 0.1961 0.199 Uiso 1 1 calc R . . C25 C 0.1694(6) 1.0779(5) 0.2525(3) 0.107(4) Uani 1 1 d . . . H25A H 0.1409 1.1043 0.2426 0.128 Uiso 1 1 calc R . . C26 C 0.0894(5) 1.1950(4) 0.3616(4) 0.097(3) Uani 1 1 d . . . H26A H 0.0529 1.1946 0.3473 0.116 Uiso 1 1 calc R . . C27 C 0.1088(6) 1.2456(5) 0.3808(6) 0.143(6) Uani 1 1 d . . . H27A H 0.0865 1.2797 0.3770 0.172 Uiso 1 1 calc R . . C28 C 0.1581(7) 1.2485(6) 0.4048(7) 0.163(7) Uani 1 1 d . . . H28A H 0.1707 1.2840 0.4169 0.195 Uiso 1 1 calc R . . C29 C 0.1918(5) 1.1950(5) 0.4116(7) 0.141(6) Uani 1 1 d . . . H29A H 0.2241 1.1926 0.4306 0.169 Uiso 1 1 calc R . . C30 C 0.1716(4) 1.1485(5) 0.3875(4) 0.097(4) Uani 1 1 d . . . H30A H 0.1948 1.1147 0.3881 0.117 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 Mo1 0.0441(5) 0.0361(5) 0.0455(5) 0.000 0.000 0.0017(3) Mo2 0.0551(6) 0.0415(5) 0.0538(6) 0.000 0.000 0.0066(4) Br1 0.0682(5) 0.0708(6) 0.0905(7) -0.0067(5) -0.0139(5) 0.0142(4) Br2 0.0945(6) 0.0493(5) 0.0816(6) 0.0084(4) 0.0201(5) 0.0047(4) Cu1 0.0634(6) 0.0452(5) 0.0678(6) -0.0056(5) 0.0037(6) -0.0080(4) Cu2 0.0556(6) 0.0470(6) 0.0745(7) 0.0023(5) 0.0070(5) 0.0100(4) Cu3 0.0646(6) 0.0497(6) 0.0797(7) -0.0006(5) 0.0064(6) 0.0120(5) Cu4 0.0620(7) 0.0541(6) 0.0915(9) 0.0142(6) -0.0085(6) 0.0024(5) S1 0.0609(14) 0.0410(11) 0.0613(12) 0.0000(9) 0.0136(10) 0.0012(9) S2 0.0511(12) 0.0531(13) 0.0630(12) -0.0162(10) -0.0019(10) 0.0023(9) S3 0.0752(16) 0.0451(12) 0.0677(14) 0.0077(9) -0.0142(12) 0.0055(10) S4 0.0602(14) 0.0665(16) 0.0744(15) -0.0201(12) 0.0042(12) 0.0075(11) N1 0.101(6) 0.053(4) 0.055(4) -0.002(3) 0.001(4) -0.003(4) N2 0.060(4) 0.053(4) 0.071(5) -0.007(4) -0.001(3) -0.014(4) N3 0.073(5) 0.049(4) 0.074(4) -0.003(3) 0.009(4) 0.012(3) N4 0.067(5) 0.063(5) 0.089(5) 0.000(4) 0.007(4) -0.004(4) N5 0.075(5) 0.082(6) 0.073(5) 0.036(4) 0.003(4) -0.012(4) N6 0.065(4) 0.052(4) 0.100(5) 0.019(4) -0.005(4) 0.002(3) C1 0.084(6) 0.058(5) 0.053(4) 0.005(4) 0.009(4) -0.003(4) C2 0.100(8) 0.078(7) 0.080(6) 0.006(5) 0.019(6) 0.004(6) C3 0.153(11) 0.065(7) 0.100(8) 0.022(6) -0.013(8) -0.031(7) C4 0.190(14) 0.034(5) 0.150(12) -0.015(6) 0.030(10) -0.002(6) C5 0.184(13) 0.053(6) 0.088(7) -0.007(5) 0.054(7) 0.006(7) C6 0.097(7) 0.062(6) 0.078(6) 0.002(4) -0.010(5) -0.008(5) C7 0.099(9) 0.115(12) 0.196(14) 0.044(10) -0.077(10) -0.015(7) C8 0.117(11) 0.095(11) 0.25(2) 0.047(12) -0.104(12) -0.042(9) C9 0.159(14) 0.076(9) 0.201(16) -0.013(9) -0.049(12) -0.029(9) C10 0.097(7) 0.058(6) 0.150(10) -0.010(6) -0.036(8) -0.022(5) C11 0.114(9) 0.119(9) 0.053(5) -0.022(5) -0.013(5) 0.040(7) C12 0.206(17) 0.104(10) 0.079(8) -0.028(7) -0.045(9) 0.040(10) C13 0.132(12) 0.084(9) 0.157(13) -0.045(9) 0.031(10) 0.018(8) C14 0.137(13) 0.089(11) 0.24(2) -0.049(12) 0.043(13) 0.011(9) C15 0.078(7) 0.081(8) 0.176(12) -0.036(8) 0.022(8) -0.002(6) C16 0.075(6) 0.103(8) 0.098(7) 0.003(6) 0.010(6) 0.023(6) C17 0.071(7) 0.110(10) 0.161(12) -0.002(9) 0.034(8) 0.030(6) C18 0.105(11) 0.156(15) 0.119(11) -0.028(10) 0.058(9) -0.012(10) C19 0.087(8) 0.160(14) 0.085(7) -0.008(8) 0.006(7) -0.003(8) C20 0.091(7) 0.093(8) 0.070(6) 0.005(5) 0.026(5) 0.004(6) C21 0.045(5) 0.136(10) 0.098(7) 0.000(7) 0.002(5) 0.008(6) C22 0.081(7) 0.127(11) 0.109(9) -0.008(7) 0.024(7) -0.021(8) C23 0.143(15) 0.167(18) 0.149(15) -0.023(13) 0.068(12) -0.020(12) C24 0.28(3) 0.128(14) 0.093(10) 0.006(9) 0.083(14) -0.051(14) C25 0.159(12) 0.091(8) 0.070(7) 0.028(6) 0.002(7) -0.014(8) C26 0.088(7) 0.062(6) 0.141(9) 0.020(6) -0.001(6) 0.007(5) C27 0.122(11) 0.046(6) 0.261(19) 0.011(8) -0.017(12) -0.009(6) C28 0.110(11) 0.080(10) 0.30(2) 0.039(13) -0.052(13) -0.023(8) C29 0.053(6) 0.081(8) 0.29(2) -0.036(11) -0.008(9) -0.022(5) C30 0.060(6) 0.098(8) 0.133(10) -0.021(7) 0.002(6) -0.021(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 S2 2.233(2) . ? Mo1 S2 2.233(2) 2_565 ? Mo1 S1 2.238(2) . ? Mo1 S1 2.238(2) 2_565 ? Mo1 Cu1 2.6732(10) . ? Mo1 Cu1 2.6732(10) 2_565 ? Mo1 Cu2 2.7116(9) . ? Mo1 Cu2 2.7116(9) 2_565 ? Mo2 S3 2.233(2) . ? Mo2 S3 2.233(2) 2_575 ? Mo2 S4 2.241(2) . ? Mo2 S4 2.241(2) 2_575 ? Mo2 Cu4 2.6626(11) . ? Mo2 Cu4 2.6626(11) 2_575 ? Mo2 Cu3 2.6943(10) . ? Mo2 Cu3 2.6943(10) 2_575 ? Br1 Cu2 2.4634(13) . ? Br2 Cu3 2.4590(14) . ? Cu1 N2 2.054(7) . ? Cu1 N1 2.107(7) . ? Cu1 S2 2.267(2) . ? Cu1 S1 2.275(2) . ? Cu2 N3 2.076(7) . ? Cu2 S2 2.294(2) 2_565 ? Cu2 S1 2.296(2) . ? Cu3 N4 2.065(8) . ? Cu3 S3 2.297(2) . ? Cu3 S4 2.311(3) . ? Cu4 N6 2.011(8) . ? Cu4 N5 2.064(8) . ? Cu4 S4 2.263(2) 2_575 ? Cu4 S3 2.276(2) . ? S2 Cu2 2.294(2) 2_565 ? S4 Cu4 2.263(2) 2_575 ? N1 C5 1.319(12) . ? N1 C1 1.352(11) . ? N2 C6 1.307(11) . ? N2 C10 1.324(11) . ? N3 C15 1.286(12) . ? N3 C11 1.336(12) . ? N4 C16 1.340(12) . ? N4 C20 1.350(12) . ? N5 C21 1.288(12) . ? N5 C25 1.370(11) . ? N6 C26 1.337(11) . ? N6 C30 1.347(12) . ? C1 C2 1.365(12) . ? C2 C3 1.348(14) . ? C3 C4 1.362(16) . ? C4 C5 1.349(15) . ? C6 C7 1.391(14) . ? C7 C8 1.36(2) . ? C8 C9 1.370(19) . ? C9 C10 1.398(16) . ? C11 C12 1.398(15) . ? C12 C13 1.301(18) . ? C13 C14 1.37(2) . ? C14 C15 1.399(17) . ? C16 C17 1.372(14) . ? C17 C18 1.356(19) . ? C18 C19 1.318(19) . ? C19 C20 1.334(14) . ? C21 C22 1.331(14) . ? C22 C23 1.30(2) . ? C23 C24 1.39(2) . ? C24 C25 1.44(2) . ? C26 C27 1.363(16) . ? C27 C28 1.331(19) . ? C28 C29 1.450(17) . ? C29 C30 1.363(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S2 Mo1 S2 111.31(12) . 2_565 ? S2 Mo1 S1 108.43(8) . . ? S2 Mo1 S1 108.36(7) 2_565 . ? S2 Mo1 S1 108.36(7) . 2_565 ? S2 Mo1 S1 108.43(8) 2_565 2_565 ? S1 Mo1 S1 111.98(12) . 2_565 ? S2 Mo1 Cu1 54.14(6) . . ? S2 Mo1 Cu1 126.72(6) 2_565 . ? S1 Mo1 Cu1 54.31(6) . . ? S1 Mo1 Cu1 124.85(6) 2_565 . ? S2 Mo1 Cu1 126.72(6) . 2_565 ? S2 Mo1 Cu1 54.14(6) 2_565 2_565 ? S1 Mo1 Cu1 124.85(6) . 2_565 ? S1 Mo1 Cu1 54.31(6) 2_565 2_565 ? Cu1 Mo1 Cu1 178.76(6) . 2_565 ? S2 Mo1 Cu2 122.30(6) . . ? S2 Mo1 Cu2 54.25(6) 2_565 . ? S1 Mo1 Cu2 54.24(6) . . ? S1 Mo1 Cu2 129.34(6) 2_565 . ? Cu1 Mo1 Cu2 88.52(3) . . ? Cu1 Mo1 Cu2 91.54(3) 2_565 . ? S2 Mo1 Cu2 54.25(6) . 2_565 ? S2 Mo1 Cu2 122.30(6) 2_565 2_565 ? S1 Mo1 Cu2 129.34(6) . 2_565 ? S1 Mo1 Cu2 54.24(6) 2_565 2_565 ? Cu1 Mo1 Cu2 91.54(3) . 2_565 ? Cu1 Mo1 Cu2 88.52(3) 2_565 2_565 ? Cu2 Mo1 Cu2 174.92(6) . 2_565 ? S3 Mo2 S3 109.82(14) . 2_575 ? S3 Mo2 S4 109.38(9) . . ? S3 Mo2 S4 108.56(8) 2_575 . ? S3 Mo2 S4 108.56(8) . 2_575 ? S3 Mo2 S4 109.38(9) 2_575 2_575 ? S4 Mo2 S4 111.13(15) . 2_575 ? S3 Mo2 Cu4 54.55(6) . . ? S3 Mo2 Cu4 128.16(7) 2_575 . ? S4 Mo2 Cu4 123.27(7) . . ? S4 Mo2 Cu4 54.13(6) 2_575 . ? S3 Mo2 Cu4 128.16(7) . 2_575 ? S3 Mo2 Cu4 54.55(6) 2_575 2_575 ? S4 Mo2 Cu4 54.13(6) . 2_575 ? S4 Mo2 Cu4 123.27(7) 2_575 2_575 ? Cu4 Mo2 Cu4 176.22(7) . 2_575 ? S3 Mo2 Cu3 54.59(6) . . ? S3 Mo2 Cu3 121.44(7) 2_575 . ? S4 Mo2 Cu3 54.91(7) . . ? S4 Mo2 Cu3 129.18(7) 2_575 . ? Cu4 Mo2 Cu3 90.66(3) . . ? Cu4 Mo2 Cu3 89.53(3) 2_575 . ? S3 Mo2 Cu3 121.44(7) . 2_575 ? S3 Mo2 Cu3 54.59(6) 2_575 2_575 ? S4 Mo2 Cu3 129.18(7) . 2_575 ? S4 Mo2 Cu3 54.91(7) 2_575 2_575 ? Cu4 Mo2 Cu3 89.53(3) . 2_575 ? Cu4 Mo2 Cu3 90.66(3) 2_575 2_575 ? Cu3 Mo2 Cu3 174.24(6) . 2_575 ? N2 Cu1 N1 97.6(3) . . ? N2 Cu1 S2 111.0(2) . . ? N1 Cu1 S2 119.2(2) . . ? N2 Cu1 S1 118.0(2) . . ? N1 Cu1 S1 105.4(2) . . ? S2 Cu1 S1 106.00(8) . . ? N2 Cu1 Mo1 134.7(2) . . ? N1 Cu1 Mo1 127.6(2) . . ? S2 Cu1 Mo1 52.96(6) . . ? S1 Cu1 Mo1 53.05(6) . . ? N3 Cu2 S2 119.8(2) . 2_565 ? N3 Cu2 S1 103.0(2) . . ? S2 Cu2 S1 104.35(8) 2_565 . ? N3 Cu2 Br1 102.7(2) . . ? S2 Cu2 Br1 105.70(7) 2_565 . ? S1 Cu2 Br1 122.51(7) . . ? N3 Cu2 Mo1 129.0(2) . . ? S2 Cu2 Mo1 52.17(6) 2_565 . ? S1 Cu2 Mo1 52.31(6) . . ? Br1 Cu2 Mo1 128.30(5) . . ? N4 Cu3 S3 119.3(2) . . ? N4 Cu3 S4 104.5(2) . . ? S3 Cu3 S4 104.83(9) . . ? N4 Cu3 Br2 102.9(2) . . ? S3 Cu3 Br2 105.34(7) . . ? S4 Cu3 Br2 121.04(9) . . ? N4 Cu3 Mo2 130.2(2) . . ? S3 Cu3 Mo2 52.42(6) . . ? S4 Cu3 Mo2 52.52(7) . . ? Br2 Cu3 Mo2 126.84(5) . . ? N6 Cu4 N5 99.6(3) . . ? N6 Cu4 S4 115.3(2) . 2_575 ? N5 Cu4 S4 112.7(2) . 2_575 ? N6 Cu4 S3 115.7(2) . . ? N5 Cu4 S3 107.0(2) . . ? S4 Cu4 S3 106.34(10) 2_575 . ? N6 Cu4 Mo2 138.8(2) . . ? N5 Cu4 Mo2 121.5(2) . . ? S4 Cu4 Mo2 53.39(7) 2_575 . ? S3 Cu4 Mo2 53.07(7) . . ? Mo1 S1 Cu1 72.64(7) . . ? Mo1 S1 Cu2 73.45(7) . . ? Cu1 S1 Cu2 110.64(10) . . ? Mo1 S2 Cu1 72.89(7) . . ? Mo1 S2 Cu2 73.59(7) . 2_565 ? Cu1 S2 Cu2 115.55(10) . 2_565 ? Mo2 S3 Cu4 72.38(7) . . ? Mo2 S3 Cu3 72.98(8) . . ? Cu4 S3 Cu3 112.86(11) . . ? Mo2 S4 Cu4 72.48(7) . 2_575 ? Mo2 S4 Cu3 72.57(8) . . ? Cu4 S4 Cu3 111.14(11) 2_575 . ? C5 N1 C1 117.6(8) . . ? C5 N1 Cu1 123.9(6) . . ? C1 N1 Cu1 118.4(6) . . ? C6 N2 C10 119.8(8) . . ? C6 N2 Cu1 121.1(6) . . ? C10 N2 Cu1 119.1(7) . . ? C15 N3 C11 118.7(9) . . ? C15 N3 Cu2 119.0(8) . . ? C11 N3 Cu2 121.9(6) . . ? C16 N4 C20 115.3(9) . . ? C16 N4 Cu3 122.5(7) . . ? C20 N4 Cu3 122.1(7) . . ? C21 N5 C25 114.4(10) . . ? C21 N5 Cu4 125.4(6) . . ? C25 N5 Cu4 120.2(8) . . ? C26 N6 C30 115.8(9) . . ? C26 N6 Cu4 120.7(7) . . ? C30 N6 Cu4 123.3(7) . . ? N1 C1 C2 120.6(9) . . ? C3 C2 C1 120.6(10) . . ? C2 C3 C4 118.4(10) . . ? C5 C4 C3 119.1(11) . . ? N1 C5 C4 123.5(10) . . ? N2 C6 C7 123.1(10) . . ? C8 C7 C6 116.9(12) . . ? C7 C8 C9 121.0(12) . . ? C8 C9 C10 117.8(13) . . ? N2 C10 C9 121.2(11) . . ? N3 C11 C12 119.9(11) . . ? C13 C12 C11 121.8(13) . . ? C12 C13 C14 117.9(13) . . ? C13 C14 C15 118.4(15) . . ? N3 C15 C14 122.7(13) . . ? N4 C16 C17 121.6(11) . . ? C18 C17 C16 119.5(12) . . ? C19 C18 C17 119.7(12) . . ? C18 C19 C20 119.0(12) . . ? C19 C20 N4 124.6(11) . . ? N5 C21 C22 129.2(12) . . ? C23 C22 C21 120.7(15) . . ? C22 C23 C24 116.0(15) . . ? C23 C24 C25 120.9(14) . . ? N5 C25 C24 118.7(13) . . ? N6 C26 C27 121.2(11) . . ? C28 C27 C26 122.9(12) . . ? C27 C28 C29 118.3(14) . . ? C30 C29 C28 113.6(14) . . ? N6 C30 C29 127.5(12) . . ? 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 S2 Mo1 Cu1 N2 83.5(3) . . . . ? S2 Mo1 Cu1 N2 -7.7(3) 2_565 . . . ? S1 Mo1 Cu1 N2 -94.7(3) . . . . ? S1 Mo1 Cu1 N2 171.8(3) 2_565 . . . ? Cu1 Mo1 Cu1 N2 -141.8(3) 2_565 . . . ? Cu2 Mo1 Cu1 N2 -49.2(3) . . . . ? Cu2 Mo1 Cu1 N2 125.7(3) 2_565 . . . ? S2 Mo1 Cu1 N1 -101.0(3) . . . . ? S2 Mo1 Cu1 N1 167.8(3) 2_565 . . . ? S1 Mo1 Cu1 N1 80.8(3) . . . . ? S1 Mo1 Cu1 N1 -12.7(3) 2_565 . . . ? Cu1 Mo1 Cu1 N1 33.7(3) 2_565 . . . ? Cu2 Mo1 Cu1 N1 126.3(3) . . . . ? Cu2 Mo1 Cu1 N1 -58.8(3) 2_565 . . . ? S2 Mo1 Cu1 S2 -91.16(15) 2_565 . . . ? S1 Mo1 Cu1 S2 -178.18(11) . . . . ? S1 Mo1 Cu1 S2 88.30(10) 2_565 . . . ? Cu1 Mo1 Cu1 S2 134.74(7) 2_565 . . . ? Cu2 Mo1 Cu1 S2 -132.70(8) . . . . ? Cu2 Mo1 Cu1 S2 42.22(8) 2_565 . . . ? S2 Mo1 Cu1 S1 178.18(11) . . . . ? S2 Mo1 Cu1 S1 87.02(10) 2_565 . . . ? S1 Mo1 Cu1 S1 -93.52(15) 2_565 . . . ? Cu1 Mo1 Cu1 S1 -47.08(7) 2_565 . . . ? Cu2 Mo1 Cu1 S1 45.48(7) . . . . ? Cu2 Mo1 Cu1 S1 -139.60(8) 2_565 . . . ? S2 Mo1 Cu2 N3 -165.3(3) . . . . ? S2 Mo1 Cu2 N3 100.4(3) 2_565 . . . ? S1 Mo1 Cu2 N3 -75.0(3) . . . . ? S1 Mo1 Cu2 N3 15.4(3) 2_565 . . . ? Cu1 Mo1 Cu2 N3 -120.5(3) . . . . ? Cu1 Mo1 Cu2 N3 58.2(3) 2_565 . . . ? Cu2 Mo1 Cu2 N3 148.8(3) 2_565 . . . ? S2 Mo1 Cu2 S2 94.28(15) . . . 2_565 ? S1 Mo1 Cu2 S2 -175.39(11) . . . 2_565 ? S1 Mo1 Cu2 S2 -85.04(11) 2_565 . . 2_565 ? Cu1 Mo1 Cu2 S2 139.08(8) . . . 2_565 ? Cu1 Mo1 Cu2 S2 -42.15(8) 2_565 . . 2_565 ? Cu2 Mo1 Cu2 S2 48.40(8) 2_565 . . 2_565 ? S2 Mo1 Cu2 S1 -90.33(10) . . . . ? S2 Mo1 Cu2 S1 175.39(11) 2_565 . . . ? S1 Mo1 Cu2 S1 90.35(15) 2_565 . . . ? Cu1 Mo1 Cu2 S1 -45.52(7) . . . . ? Cu1 Mo1 Cu2 S1 133.24(8) 2_565 . . . ? Cu2 Mo1 Cu2 S1 -136.21(7) 2_565 . . . ? S2 Mo1 Cu2 Br1 14.47(10) . . . . ? S2 Mo1 Cu2 Br1 -79.81(9) 2_565 . . . ? S1 Mo1 Cu2 Br1 104.79(9) . . . . ? S1 Mo1 Cu2 Br1 -164.86(9) 2_565 . . . ? Cu1 Mo1 Cu2 Br1 59.27(6) . . . . ? Cu1 Mo1 Cu2 Br1 -121.97(6) 2_565 . . . ? Cu2 Mo1 Cu2 Br1 -31.42(6) 2_565 . . . ? S3 Mo2 Cu3 N4 -99.1(3) . . . . ? S3 Mo2 Cu3 N4 167.9(3) 2_575 . . . ? S4 Mo2 Cu3 N4 76.4(3) . . . . ? S4 Mo2 Cu3 N4 -13.4(3) 2_575 . . . ? Cu4 Mo2 Cu3 N4 -55.1(3) . . . . ? Cu4 Mo2 Cu3 N4 121.1(3) 2_575 . . . ? Cu3 Mo2 Cu3 N4 -147.0(3) 2_575 . . . ? S3 Mo2 Cu3 S3 -93.04(16) 2_575 . . . ? S4 Mo2 Cu3 S3 175.44(12) . . . . ? S4 Mo2 Cu3 S3 85.68(12) 2_575 . . . ? Cu4 Mo2 Cu3 S3 43.96(8) . . . . ? Cu4 Mo2 Cu3 S3 -139.82(9) 2_575 . . . ? Cu3 Mo2 Cu3 S3 -47.90(8) 2_575 . . . ? S3 Mo2 Cu3 S4 -175.44(12) . . . . ? S3 Mo2 Cu3 S4 91.52(11) 2_575 . . . ? S4 Mo2 Cu3 S4 -89.76(17) 2_575 . . . ? Cu4 Mo2 Cu3 S4 -131.48(9) . . . . ? Cu4 Mo2 Cu3 S4 44.74(8) 2_575 . . . ? Cu3 Mo2 Cu3 S4 136.66(8) 2_575 . . . ? S3 Mo2 Cu3 Br2 80.83(10) . . . . ? S3 Mo2 Cu3 Br2 -12.21(11) 2_575 . . . ? S4 Mo2 Cu3 Br2 -103.73(10) . . . . ? S4 Mo2 Cu3 Br2 166.50(10) 2_575 . . . ? Cu4 Mo2 Cu3 Br2 124.79(7) . . . . ? Cu4 Mo2 Cu3 Br2 -58.99(7) 2_575 . . . ? Cu3 Mo2 Cu3 Br2 32.93(6) 2_575 . . . ? S3 Mo2 Cu4 N6 -88.0(3) . . . . ? S3 Mo2 Cu4 N6 0.3(3) 2_575 . . . ? S4 Mo2 Cu4 N6 -179.1(3) . . . . ? S4 Mo2 Cu4 N6 87.6(3) 2_575 . . . ? Cu4 Mo2 Cu4 N6 135.2(3) 2_575 . . . ? Cu3 Mo2 Cu4 N6 -132.0(3) . . . . ? Cu3 Mo2 Cu4 N6 42.3(3) 2_575 . . . ? S3 Mo2 Cu4 N5 88.2(2) . . . . ? S3 Mo2 Cu4 N5 176.4(2) 2_575 . . . ? S4 Mo2 Cu4 N5 -3.0(3) . . . . ? S4 Mo2 Cu4 N5 -96.3(3) 2_575 . . . ? Cu4 Mo2 Cu4 N5 -48.7(2) 2_575 . . . ? Cu3 Mo2 Cu4 N5 44.2(2) . . . . ? Cu3 Mo2 Cu4 N5 -141.6(2) 2_575 . . . ? S3 Mo2 Cu4 S4 -175.55(12) . . . 2_575 ? S3 Mo2 Cu4 S4 -87.28(13) 2_575 . . 2_575 ? S4 Mo2 Cu4 S4 93.31(17) . . . 2_575 ? Cu4 Mo2 Cu4 S4 47.60(9) 2_575 . . 2_575 ? Cu3 Mo2 Cu4 S4 140.46(10) . . . 2_575 ? Cu3 Mo2 Cu4 S4 -45.29(9) 2_575 . . 2_575 ? S3 Mo2 Cu4 S3 88.27(16) 2_575 . . . ? S4 Mo2 Cu4 S3 -91.14(12) . . . . ? S4 Mo2 Cu4 S3 175.55(12) 2_575 . . . ? Cu4 Mo2 Cu4 S3 -136.85(8) 2_575 . . . ? Cu3 Mo2 Cu4 S3 -43.99(8) . . . . ? Cu3 Mo2 Cu4 S3 130.25(9) 2_575 . . . ? S2 Mo1 S1 Cu1 -1.56(9) . . . . ? S2 Mo1 S1 Cu1 -122.50(8) 2_565 . . . ? S1 Mo1 S1 Cu1 117.95(7) 2_565 . . . ? Cu1 Mo1 S1 Cu1 178.90(5) 2_565 . . . ? Cu2 Mo1 S1 Cu1 -118.56(8) . . . . ? Cu2 Mo1 S1 Cu1 56.90(9) 2_565 . . . ? S2 Mo1 S1 Cu2 117.01(8) . . . . ? S2 Mo1 S1 Cu2 -3.94(9) 2_565 . . . ? S1 Mo1 S1 Cu2 -123.49(7) 2_565 . . . ? Cu1 Mo1 S1 Cu2 118.56(8) . . . . ? Cu1 Mo1 S1 Cu2 -62.54(8) 2_565 . . . ? Cu2 Mo1 S1 Cu2 175.46(5) 2_565 . . . ? N2 Cu1 S1 Mo1 126.6(2) . . . . ? N1 Cu1 S1 Mo1 -125.8(2) . . . . ? S2 Cu1 S1 Mo1 1.51(9) . . . . ? N2 Cu1 S1 Cu2 62.5(2) . . . . ? N1 Cu1 S1 Cu2 170.1(2) . . . . ? S2 Cu1 S1 Cu2 -62.60(11) . . . . ? Mo1 Cu1 S1 Cu2 -64.11(8) . . . . ? N3 Cu2 S1 Mo1 129.6(2) . . . . ? S2 Cu2 S1 Mo1 3.75(9) 2_565 . . . ? Br1 Cu2 S1 Mo1 -115.87(7) . . . . ? N3 Cu2 S1 Cu1 -166.8(2) . . . . ? S2 Cu2 S1 Cu1 67.36(11) 2_565 . . . ? Br1 Cu2 S1 Cu1 -52.26(11) . . . . ? Mo1 Cu2 S1 Cu1 63.61(8) . . . . ? S2 Mo1 S2 Cu1 120.66(7) 2_565 . . . ? S1 Mo1 S2 Cu1 1.56(9) . . . . ? S1 Mo1 S2 Cu1 -120.20(8) 2_565 . . . ? Cu1 Mo1 S2 Cu1 -178.90(5) 2_565 . . . ? Cu2 Mo1 S2 Cu1 60.36(8) . . . . ? Cu2 Mo1 S2 Cu1 -124.13(9) 2_565 . . . ? S2 Mo1 S2 Cu2 -115.21(7) 2_565 . . 2_565 ? S1 Mo1 S2 Cu2 125.69(8) . . . 2_565 ? S1 Mo1 S2 Cu2 3.94(9) 2_565 . . 2_565 ? Cu1 Mo1 S2 Cu2 124.13(9) . . . 2_565 ? Cu1 Mo1 S2 Cu2 -54.77(9) 2_565 . . 2_565 ? Cu2 Mo1 S2 Cu2 -175.51(5) . . . 2_565 ? N2 Cu1 S2 Mo1 -130.8(2) . . . . ? N1 Cu1 S2 Mo1 117.0(2) . . . . ? S1 Cu1 S2 Mo1 -1.51(9) . . . . ? N2 Cu1 S2 Cu2 167.5(2) . . . 2_565 ? N1 Cu1 S2 Cu2 55.4(2) . . . 2_565 ? S1 Cu1 S2 Cu2 -63.17(12) . . . 2_565 ? Mo1 Cu1 S2 Cu2 -61.65(8) . . . 2_565 ? S3 Mo2 S3 Cu4 -123.35(8) 2_575 . . . ? S4 Mo2 S3 Cu4 117.61(9) . . . . ? S4 Mo2 S3 Cu4 -3.81(10) 2_575 . . . ? Cu4 Mo2 S3 Cu4 176.71(6) 2_575 . . . ? Cu3 Mo2 S3 Cu4 121.56(9) . . . . ? Cu3 Mo2 S3 Cu4 -63.45(9) 2_575 . . . ? S3 Mo2 S3 Cu3 115.09(7) 2_575 . . . ? S4 Mo2 S3 Cu3 -3.95(10) . . . . ? S4 Mo2 S3 Cu3 -125.37(9) 2_575 . . . ? Cu4 Mo2 S3 Cu3 -121.56(9) . . . . ? Cu4 Mo2 S3 Cu3 55.15(10) 2_575 . . . ? Cu3 Mo2 S3 Cu3 174.99(5) 2_575 . . . ? N6 Cu4 S3 Mo2 133.1(2) . . . . ? N5 Cu4 S3 Mo2 -117.0(2) . . . . ? S4 Cu4 S3 Mo2 3.73(10) 2_575 . . . ? N6 Cu4 S3 Cu3 -164.7(2) . . . . ? N5 Cu4 S3 Cu3 -54.8(3) . . . . ? S4 Cu4 S3 Cu3 65.88(13) 2_575 . . . ? Mo2 Cu4 S3 Cu3 62.15(9) . . . . ? N4 Cu3 S3 Mo2 120.2(3) . . . . ? S4 Cu3 S3 Mo2 3.74(10) . . . . ? Br2 Cu3 S3 Mo2 -124.99(6) . . . . ? N4 Cu3 S3 Cu4 58.4(3) . . . . ? S4 Cu3 S3 Cu4 -58.06(13) . . . . ? Br2 Cu3 S3 Cu4 173.21(9) . . . . ? Mo2 Cu3 S3 Cu4 -61.80(8) . . . . ? S3 Mo2 S4 Cu4 123.64(9) . . . 2_575 ? S3 Mo2 S4 Cu4 3.83(10) 2_575 . . 2_575 ? S4 Mo2 S4 Cu4 -116.51(8) 2_575 . . 2_575 ? Cu4 Mo2 S4 Cu4 -176.66(6) . . . 2_575 ? Cu3 Mo2 S4 Cu4 119.71(10) . . . 2_575 ? Cu3 Mo2 S4 Cu4 -55.19(11) 2_575 . . 2_575 ? S3 Mo2 S4 Cu3 3.94(10) . . . . ? S3 Mo2 S4 Cu3 -115.88(9) 2_575 . . . ? S4 Mo2 S4 Cu3 123.79(8) 2_575 . . . ? Cu4 Mo2 S4 Cu3 63.63(9) . . . . ? Cu4 Mo2 S4 Cu3 -119.71(10) 2_575 . . . ? Cu3 Mo2 S4 Cu3 -174.90(6) 2_575 . . . ? N4 Cu3 S4 Mo2 -130.0(2) . . . . ? S3 Cu3 S4 Mo2 -3.74(10) . . . . ? Br2 Cu3 S4 Mo2 114.86(8) . . . . ? N4 Cu3 S4 Cu4 167.4(2) . . . 2_575 ? S3 Cu3 S4 Cu4 -66.37(13) . . . 2_575 ? Br2 Cu3 S4 Cu4 52.23(14) . . . 2_575 ? Mo2 Cu3 S4 Cu4 -62.63(9) . . . 2_575 ? N2 Cu1 N1 C5 -82.1(10) . . . . ? S2 Cu1 N1 C5 37.2(10) . . . . ? S1 Cu1 N1 C5 156.0(9) . . . . ? Mo1 Cu1 N1 C5 101.1(9) . . . . ? N2 Cu1 N1 C1 97.4(7) . . . . ? S2 Cu1 N1 C1 -143.3(6) . . . . ? S1 Cu1 N1 C1 -24.5(7) . . . . ? Mo1 Cu1 N1 C1 -79.4(7) . . . . ? N1 Cu1 N2 C6 -118.5(7) . . . . ? S2 Cu1 N2 C6 116.1(7) . . . . ? S1 Cu1 N2 C6 -6.5(8) . . . . ? Mo1 Cu1 N2 C6 58.0(8) . . . . ? N1 Cu1 N2 C10 60.4(8) . . . . ? S2 Cu1 N2 C10 -65.0(8) . . . . ? S1 Cu1 N2 C10 172.4(7) . . . . ? Mo1 Cu1 N2 C10 -123.2(8) . . . . ? S2 Cu2 N3 C15 -142.2(8) 2_565 . . . ? S1 Cu2 N3 C15 102.6(9) . . . . ? Br1 Cu2 N3 C15 -25.5(9) . . . . ? Mo1 Cu2 N3 C15 154.3(8) . . . . ? S2 Cu2 N3 C11 44.0(8) 2_565 . . . ? S1 Cu2 N3 C11 -71.2(8) . . . . ? Br1 Cu2 N3 C11 160.6(8) . . . . ? Mo1 Cu2 N3 C11 -19.5(9) . . . . ? S3 Cu3 N4 C16 92.5(8) . . . . ? S4 Cu3 N4 C16 -150.9(8) . . . . ? Br2 Cu3 N4 C16 -23.6(8) . . . . ? Mo2 Cu3 N4 C16 156.3(7) . . . . ? S3 Cu3 N4 C20 -84.1(8) . . . . ? S4 Cu3 N4 C20 32.6(8) . . . . ? Br2 Cu3 N4 C20 159.8(7) . . . . ? Mo2 Cu3 N4 C20 -20.2(9) . . . . ? N6 Cu4 N5 C21 93.4(9) . . . . ? S4 Cu4 N5 C21 -143.9(9) 2_575 . . . ? S3 Cu4 N5 C21 -27.4(10) . . . . ? Mo2 Cu4 N5 C21 -84.0(9) . . . . ? N6 Cu4 N5 C25 -87.7(8) . . . . ? S4 Cu4 N5 C25 35.0(8) 2_575 . . . ? S3 Cu4 N5 C25 151.5(7) . . . . ? Mo2 Cu4 N5 C25 94.9(8) . . . . ? N5 Cu4 N6 C26 125.8(8) . . . . ? S4 Cu4 N6 C26 4.9(8) 2_575 . . . ? S3 Cu4 N6 C26 -120.0(7) . . . . ? Mo2 Cu4 N6 C26 -57.6(9) . . . . ? N5 Cu4 N6 C30 -59.3(8) . . . . ? S4 Cu4 N6 C30 179.8(7) 2_575 . . . ? S3 Cu4 N6 C30 54.9(8) . . . . ? Mo2 Cu4 N6 C30 117.3(7) . . . . ? C5 N1 C1 C2 2.2(15) . . . . ? Cu1 N1 C1 C2 -177.3(7) . . . . ? N1 C1 C2 C3 -4.0(16) . . . . ? C1 C2 C3 C4 3.2(19) . . . . ? C2 C3 C4 C5 -1(2) . . . . ? C1 N1 C5 C4 0.2(19) . . . . ? Cu1 N1 C5 C4 179.7(11) . . . . ? C3 C4 C5 N1 -1(2) . . . . ? C10 N2 C6 C7 -1.2(16) . . . . ? Cu1 N2 C6 C7 177.6(9) . . . . ? N2 C6 C7 C8 1(2) . . . . ? C6 C7 C8 C9 2(3) . . . . ? C7 C8 C9 C10 -3(3) . . . . ? C6 N2 C10 C9 -0.5(17) . . . . ? Cu1 N2 C10 C9 -179.3(10) . . . . ? C8 C9 C10 N2 3(2) . . . . ? C15 N3 C11 C12 1.8(17) . . . . ? Cu2 N3 C11 C12 175.6(9) . . . . ? N3 C11 C12 C13 3(2) . . . . ? C11 C12 C13 C14 -9(3) . . . . ? C12 C13 C14 C15 10(3) . . . . ? C11 N3 C15 C14 -0.6(19) . . . . ? Cu2 N3 C15 C14 -174.6(11) . . . . ? C13 C14 C15 N3 -5(2) . . . . ? C20 N4 C16 C17 -1.8(16) . . . . ? Cu3 N4 C16 C17 -178.6(9) . . . . ? N4 C16 C17 C18 -2(2) . . . . ? C16 C17 C18 C19 3(2) . . . . ? C17 C18 C19 C20 0(2) . . . . ? C18 C19 C20 N4 -5(2) . . . . ? C16 N4 C20 C19 5.5(16) . . . . ? Cu3 N4 C20 C19 -177.7(9) . . . . ? C25 N5 C21 C22 -2.6(18) . . . . ? Cu4 N5 C21 C22 176.3(10) . . . . ? N5 C21 C22 C23 1(2) . . . . ? C21 C22 C23 C24 1(3) . . . . ? C22 C23 C24 C25 0(3) . . . . ? C21 N5 C25 C24 3.2(16) . . . . ? Cu4 N5 C25 C24 -175.8(10) . . . . ? C23 C24 C25 N5 -2(2) . . . . ? C30 N6 C26 C27 5.7(16) . . . . ? Cu4 N6 C26 C27 -179.0(10) . . . . ? N6 C26 C27 C28 -5(2) . . . . ? C26 C27 C28 C29 -2(3) . . . . ? C27 C28 C29 C30 7(3) . . . . ? C26 N6 C30 C29 1.2(18) . . . . ? Cu4 N6 C30 C29 -174.0(12) . . . . ? C28 C29 C30 N6 -8(2) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.815 _refine_diff_density_min -0.418 _refine_diff_density_rms 0.086 #======END