# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Yunyin Niu' _publ_contact_author_email niuyy@zzu.edu.cn _publ_section_title ; External Template-Assisted Self-Assembly: Design and Synthesis of the [MoOS3Cu3]3- based supramolecular polymeric clusters ; loop_ _publ_author_name 'Hong-Mei Wang' 'Yunyin Niu' 'Zhen-Hua Zhang' 'Wei Hong' 'Yu Zhu' # Attachment '- cif2.cif' data_b _database_code_depnum_ccdc_archive 'CCDC 845162' #TrackingRef '- cif2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H20 Cu3 I Mo N5 O S3' _chemical_formula_sum 'C50 H40 Cu6 I2 Mo2 N10 O2 S6' _chemical_formula_weight 1832.20 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 Monoclinic _symmetry_space_group_name_H-M C2/c 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 21.186(5) _cell_length_b 21.293(5) _cell_length_c 17.947(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.459(18) _cell_angle_gamma 90.00 _cell_volume 8045(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 8223 _cell_measurement_theta_min 2.71 _cell_measurement_theta_max 24.40 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.513 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3544 _exptl_absorpt_coefficient_mu 2.814 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3761 _exptl_absorpt_correction_T_max 0.5149 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 46399 _diffrn_reflns_av_R_equivalents 0.0903 _diffrn_reflns_av_sigmaI/netI 0.0547 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 25.50 _reflns_number_total 7363 _reflns_number_gt 4785 _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^)+(0.1800P)^2^+8.1002P] 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 7363 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1096 _refine_ls_R_factor_gt 0.0818 _refine_ls_wR_factor_ref 0.2739 _refine_ls_wR_factor_gt 0.2246 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/su_max 0.002 _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 Mo1 Mo 0.21421(3) 1.01881(3) 0.49530(3) 0.0399(3) Uani 1 1 d . . . I1 I 0.38208(5) 0.86426(4) 0.57039(5) 0.0977(4) Uani 1 1 d . . . S1 S 0.21534(11) 0.94813(9) 0.58949(12) 0.0488(5) Uani 1 1 d . . . S2 S 0.24031(11) 1.11506(9) 0.54490(11) 0.0473(5) Uani 1 1 d . . . S3 S 0.29021(11) 0.99017(9) 0.42382(11) 0.0456(5) Uani 1 1 d . . . O1 O 0.1414(3) 1.0203(3) 0.4443(4) 0.0631(17) Uani 1 1 d . . . Cu1 Cu 0.28509(5) 0.91277(5) 0.51250(5) 0.0484(3) Uani 1 1 d . . . Cu2 Cu 0.23751(5) 1.04542(5) 0.64081(5) 0.0452(3) Uani 1 1 d . . . Cu3 Cu 0.31772(5) 1.08807(4) 0.47253(5) 0.0447(3) Uani 1 1 d . . . N1 N 0.2412(4) 0.8397(3) 0.4394(3) 0.0480(17) Uani 1 1 d . . . N2 N 0.1814(4) 0.6469(3) 0.1192(4) 0.0520(17) Uani 1 1 d . . . N3 N 0.1530(3) 1.0590(3) 0.6900(4) 0.0485(16) Uani 1 1 d . . . N4 N 0.3123(3) 1.0526(3) 0.7193(4) 0.0487(16) Uani 1 1 d . . . N5 N 0.5924(4) 1.0856(3) 0.9717(4) 0.0491(17) Uani 1 1 d . . . C1 C 0.1929(4) 0.8504(4) 0.3909(5) 0.054(2) Uani 1 1 d . . . H1 H 0.1688 0.8859 0.3983 0.065 Uiso 1 1 calc R . . C2 C 0.1736(5) 0.8138(4) 0.3289(5) 0.056(2) Uani 1 1 d . . . H2 H 0.1379 0.8243 0.2964 0.067 Uiso 1 1 calc R . . C3 C 0.2098(4) 0.7599(4) 0.3162(5) 0.051(2) Uani 1 1 d . . . C4 C 0.2626(5) 0.7474(5) 0.3693(5) 0.062(2) Uani 1 1 d . . . H4 H 0.2877 0.7121 0.3642 0.074 Uiso 1 1 calc R . . C5 C 0.2765(5) 0.7878(4) 0.4284(5) 0.057(2) Uani 1 1 d . . . H5 H 0.3117 0.7793 0.4626 0.068 Uiso 1 1 calc R . . C6 C 0.1726(6) 0.7090(4) 0.1162(5) 0.069(3) Uani 1 1 d . . . H6 H 0.1606 0.7275 0.0698 0.082 Uiso 1 1 calc R . . C7 C 0.1805(6) 0.7474(5) 0.1797(6) 0.073(3) Uani 1 1 d . . . H7 H 0.1757 0.7907 0.1750 0.088 Uiso 1 1 calc R . . C8 C 0.1952(4) 0.7212(4) 0.2481(4) 0.048(2) Uani 1 1 d . . . C9 C 0.2034(6) 0.6564(4) 0.2505(5) 0.068(3) Uani 1 1 d . . . H9 H 0.2144 0.6367 0.2964 0.082 Uiso 1 1 calc R . . C10 C 0.1958(6) 0.6219(4) 0.1875(6) 0.066(3) Uani 1 1 d . . . H10 H 0.2008 0.5786 0.1915 0.079 Uiso 1 1 calc R . . C11 C 0.1001(5) 1.0799(5) 0.6464(5) 0.062(3) Uani 1 1 d . . . H11 H 0.1049 1.0961 0.5992 0.075 Uiso 1 1 calc R . . C12 C 0.0438(4) 1.0783(5) 0.6672(5) 0.057(2) Uani 1 1 d . . . H12 H 0.0098 1.0931 0.6346 0.069 Uiso 1 1 calc R . . C13 C 0.0324(4) 1.0549(4) 0.7377(4) 0.0442(18) Uani 1 1 d . . . C14 C 0.0843(4) 1.0344(4) 0.7830(4) 0.0482(19) Uani 1 1 d . . . H14 H 0.0801 1.0194 0.8309 0.058 Uiso 1 1 calc R . . C15 C 0.1438(5) 1.0360(5) 0.7565(5) 0.055(2) Uani 1 1 d . . . H15 H 0.1786 1.0203 0.7870 0.066 Uiso 1 1 calc R . . C16 C 0.3204(5) 1.1025(4) 0.7664(5) 0.052(2) Uani 1 1 d . . . H16 H 0.2890 1.1332 0.7641 0.062 Uiso 1 1 calc R . . C17 C 0.3732(4) 1.1095(4) 0.8173(5) 0.052(2) Uani 1 1 d . . . H17 H 0.3761 1.1436 0.8499 0.062 Uiso 1 1 calc R . . C18 C 0.4213(4) 1.0667(4) 0.8205(5) 0.0453(18) Uani 1 1 d . . . C19 C 0.4112(5) 1.0151(5) 0.7729(6) 0.064(3) Uani 1 1 d . . . H19 H 0.4405 0.9824 0.7770 0.076 Uiso 1 1 calc R . . C20 C 0.3610(4) 1.0113(4) 0.7220(5) 0.051(2) Uani 1 1 d . . . H20 H 0.3592 0.9790 0.6868 0.061 Uiso 1 1 calc R . . C21 C 0.5681(5) 1.0294(4) 0.9491(6) 0.061(2) Uani 1 1 d . . . H21 H 0.5896 0.9934 0.9671 0.073 Uiso 1 1 calc R . . C22 C 0.5148(5) 1.0224(4) 0.9023(6) 0.064(3) Uani 1 1 d . . . H22 H 0.5018 0.9822 0.8871 0.077 Uiso 1 1 calc R . . C23 C 0.4790(4) 1.0729(4) 0.8760(5) 0.049(2) Uani 1 1 d . . . C24 C 0.5027(5) 1.1320(4) 0.8998(6) 0.067(3) Uani 1 1 d . . . H24 H 0.4812 1.1685 0.8839 0.080 Uiso 1 1 calc R . . C25 C 0.5587(6) 1.1347(5) 0.9476(7) 0.080(4) Uani 1 1 d . . . H25 H 0.5735 1.1741 0.9636 0.096 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 0.0439(5) 0.0351(4) 0.0380(4) -0.0030(2) -0.0081(3) -0.0002(3) I1 0.1061(8) 0.0750(6) 0.1062(7) 0.0047(4) -0.0135(6) 0.0050(4) S1 0.0584(14) 0.0395(10) 0.0480(11) 0.0003(8) 0.0039(10) -0.0043(9) S2 0.0571(13) 0.0363(9) 0.0468(11) -0.0040(8) -0.0014(9) 0.0007(9) S3 0.0568(13) 0.0370(9) 0.0416(10) -0.0043(8) -0.0002(9) 0.0010(9) O1 0.051(4) 0.068(4) 0.064(4) -0.008(3) -0.018(3) -0.005(3) Cu1 0.0615(7) 0.0351(5) 0.0469(6) -0.0026(4) -0.0019(5) 0.0028(4) Cu2 0.0445(6) 0.0476(6) 0.0413(6) -0.0051(4) -0.0045(4) 0.0011(4) Cu3 0.0492(6) 0.0387(5) 0.0438(6) 0.0050(4) -0.0053(4) -0.0003(4) N1 0.077(5) 0.037(3) 0.028(3) -0.004(3) -0.004(3) -0.006(3) N2 0.065(5) 0.040(4) 0.049(4) -0.006(3) -0.004(3) 0.002(3) N3 0.042(4) 0.056(4) 0.045(4) -0.001(3) -0.006(3) 0.006(3) N4 0.044(4) 0.051(4) 0.048(4) -0.007(3) -0.005(3) 0.003(3) N5 0.055(4) 0.047(4) 0.043(4) -0.006(3) -0.007(3) 0.007(3) C1 0.061(6) 0.034(4) 0.064(5) -0.014(4) -0.006(4) 0.007(4) C2 0.066(6) 0.034(4) 0.064(5) -0.008(4) -0.008(4) -0.002(4) C3 0.066(6) 0.030(4) 0.054(5) -0.004(3) -0.002(4) -0.017(4) C4 0.077(7) 0.047(5) 0.062(6) -0.009(4) 0.005(5) 0.002(5) C5 0.074(6) 0.030(4) 0.062(5) -0.008(4) -0.014(5) -0.001(4) C6 0.130(10) 0.034(4) 0.037(4) -0.006(3) -0.012(5) 0.011(5) C7 0.090(8) 0.048(5) 0.075(7) -0.002(5) -0.020(6) 0.009(5) C8 0.072(6) 0.039(4) 0.033(4) 0.004(3) 0.003(4) 0.000(4) C9 0.127(10) 0.032(4) 0.045(5) -0.005(4) 0.002(5) 0.007(5) C10 0.097(8) 0.032(4) 0.066(6) -0.004(4) -0.005(5) -0.006(5) C11 0.047(6) 0.091(7) 0.048(5) 0.016(5) 0.004(4) 0.009(5) C12 0.043(5) 0.085(7) 0.041(4) 0.014(4) -0.011(4) 0.017(4) C13 0.050(5) 0.046(4) 0.037(4) 0.001(3) 0.004(3) 0.009(4) C14 0.047(5) 0.059(5) 0.036(4) 0.007(4) -0.011(4) 0.001(4) C15 0.059(6) 0.065(5) 0.038(4) 0.010(4) -0.006(4) 0.001(4) C16 0.056(5) 0.052(5) 0.045(4) -0.006(4) -0.005(4) 0.010(4) C17 0.050(5) 0.039(4) 0.063(5) -0.018(4) -0.009(4) -0.004(4) C18 0.044(5) 0.039(4) 0.048(4) -0.007(3) -0.012(4) -0.005(3) C19 0.062(6) 0.056(5) 0.072(6) -0.012(5) 0.003(5) 0.013(4) C20 0.048(5) 0.051(5) 0.050(5) -0.021(4) -0.013(4) 0.003(4) C21 0.059(6) 0.038(4) 0.082(7) -0.014(4) -0.005(5) 0.005(4) C22 0.066(6) 0.046(5) 0.074(6) -0.007(4) -0.017(5) 0.005(4) C23 0.047(5) 0.043(4) 0.052(5) -0.006(4) -0.020(4) -0.010(4) C24 0.068(6) 0.031(4) 0.094(7) -0.020(4) -0.018(5) -0.001(4) C25 0.083(8) 0.042(5) 0.103(8) -0.016(5) -0.046(6) 0.009(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 O1 1.704(6) . ? Mo1 S3 2.253(2) . ? Mo1 S1 2.261(2) . ? Mo1 S2 2.278(2) . ? Mo1 Cu2 2.6636(13) . ? Mo1 Cu1 2.7099(13) . ? Mo1 Cu3 2.7116(13) . ? I1 Cu1 2.4266(15) . ? S1 Cu1 2.263(2) . ? S1 Cu2 2.294(2) . ? S2 Cu3 2.277(2) . ? S2 Cu2 2.278(2) . ? S3 Cu1 2.302(2) . ? S3 Cu3 2.310(2) . ? Cu1 N1 2.175(6) . ? Cu2 N4 2.003(7) . ? Cu2 N3 2.104(7) . ? Cu3 N5 2.050(7) 2_656 ? Cu3 N2 2.070(7) 4 ? N1 C1 1.287(11) . ? N1 C5 1.362(11) . ? N2 C6 1.336(11) . ? N2 C10 1.340(12) . ? N2 Cu3 2.070(7) 4_545 ? N3 C15 1.324(11) . ? N3 C11 1.367(12) . ? N4 C20 1.353(11) . ? N4 C16 1.358(11) . ? N5 C25 1.311(12) . ? N5 C21 1.347(11) . ? N5 Cu3 2.050(7) 2_656 ? C1 C2 1.383(12) . ? C1 H1 0.9300 . ? C2 C3 1.412(13) . ? C2 H2 0.9300 . ? C3 C4 1.410(13) . ? C3 C8 1.478(11) . ? C4 C5 1.372(13) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.397(14) . ? C6 H6 0.9300 . ? C7 C8 1.352(13) . ? C7 H7 0.9300 . ? C8 C9 1.390(12) . ? C9 C10 1.343(13) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.288(13) . ? C11 H11 0.9300 . ? C12 C13 1.406(12) . ? C12 H12 0.9300 . ? C13 C14 1.363(11) . ? C13 C13 1.490(17) 2_556 ? C14 C15 1.398(13) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.369(13) . ? C16 H16 0.9300 . ? C17 C18 1.364(12) . ? C17 H17 0.9300 . ? C18 C19 1.395(12) . ? C18 C23 1.493(11) . ? C19 C20 1.325(13) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.338(14) . ? C21 H21 0.9300 . ? C22 C23 1.368(13) . ? C22 H22 0.9300 . ? C23 C24 1.403(11) . ? C24 C25 1.385(14) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? 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 O1 Mo1 S3 111.2(2) . . ? O1 Mo1 S1 110.3(3) . . ? S3 Mo1 S1 107.30(8) . . ? O1 Mo1 S2 111.0(2) . . ? S3 Mo1 S2 107.97(8) . . ? S1 Mo1 S2 108.97(8) . . ? O1 Mo1 Cu2 125.4(2) . . ? S3 Mo1 Cu2 123.39(6) . . ? S1 Mo1 Cu2 54.79(6) . . ? S2 Mo1 Cu2 54.22(6) . . ? O1 Mo1 Cu1 122.2(2) . . ? S3 Mo1 Cu1 54.33(6) . . ? S1 Mo1 Cu1 53.22(6) . . ? S2 Mo1 Cu1 126.74(7) . . ? Cu2 Mo1 Cu1 91.51(4) . . ? O1 Mo1 Cu3 127.5(2) . . ? S3 Mo1 Cu3 54.51(6) . . ? S1 Mo1 Cu3 122.27(7) . . ? S2 Mo1 Cu3 53.46(6) . . ? Cu2 Mo1 Cu3 88.18(4) . . ? Cu1 Mo1 Cu3 91.32(4) . . ? Mo1 S1 Cu1 73.60(7) . . ? Mo1 S1 Cu2 71.56(7) . . ? Cu1 S1 Cu2 115.30(10) . . ? Cu3 S2 Mo1 73.07(7) . . ? Cu3 S2 Cu2 110.38(9) . . ? Mo1 S2 Cu2 71.56(7) . . ? Mo1 S3 Cu1 73.01(7) . . ? Mo1 S3 Cu3 72.92(7) . . ? Cu1 S3 Cu3 114.45(9) . . ? N1 Cu1 S1 110.0(2) . . ? N1 Cu1 S3 98.32(18) . . ? S1 Cu1 S3 105.59(8) . . ? N1 Cu1 I1 103.8(2) . . ? S1 Cu1 I1 117.38(8) . . ? S3 Cu1 I1 119.82(8) . . ? N1 Cu1 Mo1 109.5(2) . . ? S1 Cu1 Mo1 53.18(6) . . ? S3 Cu1 Mo1 52.66(6) . . ? I1 Cu1 Mo1 146.62(5) . . ? N4 Cu2 N3 109.7(3) . . ? N4 Cu2 S2 113.3(2) . . ? N3 Cu2 S2 108.9(2) . . ? N4 Cu2 S1 117.5(2) . . ? N3 Cu2 S1 98.5(2) . . ? S2 Cu2 S1 107.81(8) . . ? N4 Cu2 Mo1 138.6(2) . . ? N3 Cu2 Mo1 111.59(19) . . ? S2 Cu2 Mo1 54.21(6) . . ? S1 Cu2 Mo1 53.65(6) . . ? N5 Cu3 N2 108.3(3) 2_656 4 ? N5 Cu3 S2 114.6(2) 2_656 . ? N2 Cu3 S2 111.8(2) 4 . ? N5 Cu3 S3 110.0(2) 2_656 . ? N2 Cu3 S3 105.6(2) 4 . ? S2 Cu3 S3 106.04(9) . . ? N5 Cu3 Mo1 129.42(19) 2_656 . ? N2 Cu3 Mo1 121.9(2) 4 . ? S2 Cu3 Mo1 53.47(6) . . ? S3 Cu3 Mo1 52.57(6) . . ? C1 N1 C5 116.9(7) . . ? C1 N1 Cu1 122.4(5) . . ? C5 N1 Cu1 117.7(6) . . ? C6 N2 C10 116.5(7) . . ? C6 N2 Cu3 125.5(6) . 4_545 ? C10 N2 Cu3 117.8(6) . 4_545 ? C15 N3 C11 116.3(8) . . ? C15 N3 Cu2 123.0(6) . . ? C11 N3 Cu2 119.1(6) . . ? C20 N4 C16 116.4(7) . . ? C20 N4 Cu2 121.0(5) . . ? C16 N4 Cu2 122.2(6) . . ? C25 N5 C21 115.7(8) . . ? C25 N5 Cu3 125.6(7) . 2_656 ? C21 N5 Cu3 118.2(6) . 2_656 ? N1 C1 C2 125.8(8) . . ? N1 C1 H1 117.1 . . ? C2 C1 H1 117.1 . . ? C1 C2 C3 118.1(9) . . ? C1 C2 H2 120.9 . . ? C3 C2 H2 120.9 . . ? C4 C3 C2 116.6(8) . . ? C4 C3 C8 122.0(8) . . ? C2 C3 C8 121.3(8) . . ? C5 C4 C3 119.3(9) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? N1 C5 C4 123.2(9) . . ? N1 C5 H5 118.4 . . ? C4 C5 H5 118.4 . . ? N2 C6 C7 122.9(9) . . ? N2 C6 H6 118.6 . . ? C7 C6 H6 118.6 . . ? C8 C7 C6 119.5(9) . . ? C8 C7 H7 120.2 . . ? C6 C7 H7 120.2 . . ? C7 C8 C9 117.0(8) . . ? C7 C8 C3 121.8(8) . . ? C9 C8 C3 120.8(7) . . ? C10 C9 C8 120.9(9) . . ? C10 C9 H9 119.6 . . ? C8 C9 H9 119.6 . . ? N2 C10 C9 123.1(8) . . ? N2 C10 H10 118.4 . . ? C9 C10 H10 118.4 . . ? C12 C11 N3 123.4(8) . . ? C12 C11 H11 118.3 . . ? N3 C11 H11 118.3 . . ? C11 C12 C13 121.9(8) . . ? C11 C12 H12 119.1 . . ? C13 C12 H12 119.1 . . ? C14 C13 C12 116.2(8) . . ? C14 C13 C13 122.1(8) . 2_556 ? C12 C13 C13 121.6(9) . 2_556 ? C13 C14 C15 119.1(8) . . ? C13 C14 H14 120.4 . . ? C15 C14 H14 120.4 . . ? N3 C15 C14 123.0(8) . . ? N3 C15 H15 118.5 . . ? C14 C15 H15 118.5 . . ? N4 C16 C17 122.5(8) . . ? N4 C16 H16 118.8 . . ? C17 C16 H16 118.8 . . ? C18 C17 C16 120.5(8) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C17 C18 C19 116.0(8) . . ? C17 C18 C23 121.5(7) . . ? C19 C18 C23 122.4(8) . . ? C20 C19 C18 121.8(9) . . ? C20 C19 H19 119.1 . . ? C18 C19 H19 119.1 . . ? C19 C20 N4 122.4(8) . . ? C19 C20 H20 118.8 . . ? N4 C20 H20 118.8 . . ? C22 C21 N5 123.7(9) . . ? C22 C21 H21 118.1 . . ? N5 C21 H21 118.1 . . ? C21 C22 C23 121.6(9) . . ? C21 C22 H22 119.2 . . ? C23 C22 H22 119.2 . . ? C22 C23 C24 115.8(8) . . ? C22 C23 C18 122.8(8) . . ? C24 C23 C18 121.3(8) . . ? C25 C24 C23 118.6(9) . . ? C25 C24 H24 120.7 . . ? C23 C24 H24 120.7 . . ? N5 C25 C24 124.6(9) . . ? N5 C25 H25 117.7 . . ? C24 C25 H25 117.7 . . ? 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 O1 Mo1 S1 Cu1 115.7(3) . . . . ? S3 Mo1 S1 Cu1 -5.53(9) . . . . ? S2 Mo1 S1 Cu1 -122.19(8) . . . . ? Cu2 Mo1 S1 Cu1 -124.59(9) . . . . ? Cu3 Mo1 S1 Cu1 -64.04(8) . . . . ? O1 Mo1 S1 Cu2 -119.7(3) . . . . ? S3 Mo1 S1 Cu2 119.06(8) . . . . ? S2 Mo1 S1 Cu2 2.40(9) . . . . ? Cu1 Mo1 S1 Cu2 124.59(9) . . . . ? Cu3 Mo1 S1 Cu2 60.56(8) . . . . ? O1 Mo1 S2 Cu3 -121.7(3) . . . . ? S3 Mo1 S2 Cu3 0.38(8) . . . . ? S1 Mo1 S2 Cu3 116.61(8) . . . . ? Cu2 Mo1 S2 Cu3 119.03(8) . . . . ? Cu1 Mo1 S2 Cu3 58.85(8) . . . . ? O1 Mo1 S2 Cu2 119.2(3) . . . . ? S3 Mo1 S2 Cu2 -118.65(8) . . . . ? S1 Mo1 S2 Cu2 -2.42(9) . . . . ? Cu1 Mo1 S2 Cu2 -60.18(9) . . . . ? Cu3 Mo1 S2 Cu2 -119.03(8) . . . . ? O1 Mo1 S3 Cu1 -115.2(3) . . . . ? S1 Mo1 S3 Cu1 5.45(8) . . . . ? S2 Mo1 S3 Cu1 122.77(8) . . . . ? Cu2 Mo1 S3 Cu1 64.26(7) . . . . ? Cu3 Mo1 S3 Cu1 123.14(8) . . . . ? O1 Mo1 S3 Cu3 121.7(3) . . . . ? S1 Mo1 S3 Cu3 -117.69(8) . . . . ? S2 Mo1 S3 Cu3 -0.37(8) . . . . ? Cu2 Mo1 S3 Cu3 -58.88(7) . . . . ? Cu1 Mo1 S3 Cu3 -123.14(8) . . . . ? Mo1 S1 Cu1 N1 -99.80(19) . . . . ? Cu2 S1 Cu1 N1 -159.6(2) . . . . ? Mo1 S1 Cu1 S3 5.37(8) . . . . ? Cu2 S1 Cu1 S3 -54.38(12) . . . . ? Mo1 S1 Cu1 I1 141.91(6) . . . . ? Cu2 S1 Cu1 I1 82.16(11) . . . . ? Cu2 S1 Cu1 Mo1 -59.75(8) . . . . ? Mo1 S3 Cu1 N1 108.2(2) . . . . ? Cu3 S3 Cu1 N1 169.7(2) . . . . ? Mo1 S3 Cu1 S1 -5.40(8) . . . . ? Cu3 S3 Cu1 S1 56.15(13) . . . . ? Mo1 S3 Cu1 I1 -140.66(6) . . . . ? Cu3 S3 Cu1 I1 -79.11(11) . . . . ? Cu3 S3 Cu1 Mo1 61.55(8) . . . . ? O1 Mo1 Cu1 N1 8.6(4) . . . . ? S3 Mo1 Cu1 N1 -85.6(2) . . . . ? S1 Mo1 Cu1 N1 100.9(2) . . . . ? S2 Mo1 Cu1 N1 -172.1(2) . . . . ? Cu2 Mo1 Cu1 N1 143.19(19) . . . . ? Cu3 Mo1 Cu1 N1 -128.60(19) . . . . ? O1 Mo1 Cu1 S1 -92.3(3) . . . . ? S3 Mo1 Cu1 S1 173.50(10) . . . . ? S2 Mo1 Cu1 S1 87.04(11) . . . . ? Cu2 Mo1 Cu1 S1 42.29(8) . . . . ? Cu3 Mo1 Cu1 S1 130.50(8) . . . . ? O1 Mo1 Cu1 S3 94.2(3) . . . . ? S1 Mo1 Cu1 S3 -173.50(10) . . . . ? S2 Mo1 Cu1 S3 -86.45(10) . . . . ? Cu2 Mo1 Cu1 S3 -131.21(7) . . . . ? Cu3 Mo1 Cu1 S3 -43.00(7) . . . . ? O1 Mo1 Cu1 I1 -177.0(3) . . . . ? S3 Mo1 Cu1 I1 88.78(12) . . . . ? S1 Mo1 Cu1 I1 -84.71(12) . . . . ? S2 Mo1 Cu1 I1 2.33(14) . . . . ? Cu2 Mo1 Cu1 I1 -42.42(10) . . . . ? Cu3 Mo1 Cu1 I1 45.79(10) . . . . ? Cu3 S2 Cu2 N4 71.0(2) . . . . ? Mo1 S2 Cu2 N4 134.1(2) . . . . ? Cu3 S2 Cu2 N3 -166.7(2) . . . . ? Mo1 S2 Cu2 N3 -103.5(2) . . . . ? Cu3 S2 Cu2 S1 -60.81(12) . . . . ? Mo1 S2 Cu2 S1 2.37(9) . . . . ? Cu3 S2 Cu2 Mo1 -63.17(7) . . . . ? Mo1 S1 Cu2 N4 -131.9(2) . . . . ? Cu1 S1 Cu2 N4 -71.0(3) . . . . ? Mo1 S1 Cu2 N3 110.6(2) . . . . ? Cu1 S1 Cu2 N3 171.5(2) . . . . ? Mo1 S1 Cu2 S2 -2.38(9) . . . . ? Cu1 S1 Cu2 S2 58.49(13) . . . . ? Cu1 S1 Cu2 Mo1 60.87(8) . . . . ? O1 Mo1 Cu2 N4 -177.2(4) . . . . ? S3 Mo1 Cu2 N4 3.4(3) . . . . ? S1 Mo1 Cu2 N4 91.8(3) . . . . ? S2 Mo1 Cu2 N4 -85.4(3) . . . . ? Cu1 Mo1 Cu2 N4 50.5(3) . . . . ? Cu3 Mo1 Cu2 N4 -40.8(3) . . . . ? O1 Mo1 Cu2 N3 6.5(4) . . . . ? S3 Mo1 Cu2 N3 -172.9(2) . . . . ? S1 Mo1 Cu2 N3 -84.6(2) . . . . ? S2 Mo1 Cu2 N3 98.2(2) . . . . ? Cu1 Mo1 Cu2 N3 -125.8(2) . . . . ? Cu3 Mo1 Cu2 N3 142.9(2) . . . . ? O1 Mo1 Cu2 S2 -91.7(3) . . . . ? S3 Mo1 Cu2 S2 88.87(10) . . . . ? S1 Mo1 Cu2 S2 177.20(11) . . . . ? Cu1 Mo1 Cu2 S2 135.93(8) . . . . ? Cu3 Mo1 Cu2 S2 44.66(8) . . . . ? O1 Mo1 Cu2 S1 91.1(3) . . . . ? S3 Mo1 Cu2 S1 -88.33(10) . . . . ? S2 Mo1 Cu2 S1 -177.20(11) . . . . ? Cu1 Mo1 Cu2 S1 -41.27(8) . . . . ? Cu3 Mo1 Cu2 S1 -132.55(8) . . . . ? Mo1 S2 Cu3 N5 -122.0(2) . . . 2_656 ? Cu2 S2 Cu3 N5 -59.7(2) . . . 2_656 ? Mo1 S2 Cu3 N2 114.3(2) . . . 4 ? Cu2 S2 Cu3 N2 176.5(2) . . . 4 ? Mo1 S2 Cu3 S3 -0.36(8) . . . . ? Cu2 S2 Cu3 S3 61.88(11) . . . . ? Cu2 S2 Cu3 Mo1 62.24(7) . . . . ? Mo1 S3 Cu3 N5 124.9(2) . . . 2_656 ? Cu1 S3 Cu3 N5 63.3(2) . . . 2_656 ? Mo1 S3 Cu3 N2 -118.5(2) . . . 4 ? Cu1 S3 Cu3 N2 179.9(2) . . . 4 ? Mo1 S3 Cu3 S2 0.37(8) . . . . ? Cu1 S3 Cu3 S2 -61.24(12) . . . . ? Cu1 S3 Cu3 Mo1 -61.61(8) . . . . ? O1 Mo1 Cu3 N5 -176.7(4) . . . 2_656 ? S3 Mo1 Cu3 N5 -86.0(3) . . . 2_656 ? S1 Mo1 Cu3 N5 3.0(3) . . . 2_656 ? S2 Mo1 Cu3 N5 93.6(3) . . . 2_656 ? Cu2 Mo1 Cu3 N5 48.4(3) . . . 2_656 ? Cu1 Mo1 Cu3 N5 -43.1(3) . . . 2_656 ? O1 Mo1 Cu3 N2 -5.1(4) . . . 4 ? S3 Mo1 Cu3 N2 85.6(3) . . . 4 ? S1 Mo1 Cu3 N2 174.6(2) . . . 4 ? S2 Mo1 Cu3 N2 -94.8(3) . . . 4 ? Cu2 Mo1 Cu3 N2 -140.0(2) . . . 4 ? Cu1 Mo1 Cu3 N2 128.5(2) . . . 4 ? O1 Mo1 Cu3 S2 89.7(3) . . . . ? S3 Mo1 Cu3 S2 -179.56(10) . . . . ? S1 Mo1 Cu3 S2 -90.60(10) . . . . ? Cu2 Mo1 Cu3 S2 -45.21(7) . . . . ? Cu1 Mo1 Cu3 S2 -136.68(7) . . . . ? O1 Mo1 Cu3 S3 -90.7(3) . . . . ? S1 Mo1 Cu3 S3 88.96(10) . . . . ? S2 Mo1 Cu3 S3 179.56(10) . . . . ? Cu2 Mo1 Cu3 S3 134.35(7) . . . . ? Cu1 Mo1 Cu3 S3 42.88(7) . . . . ? S1 Cu1 N1 C1 63.5(7) . . . . ? S3 Cu1 N1 C1 -46.5(7) . . . . ? I1 Cu1 N1 C1 -170.1(7) . . . . ? Mo1 Cu1 N1 C1 6.7(8) . . . . ? S1 Cu1 N1 C5 -136.8(6) . . . . ? S3 Cu1 N1 C5 113.2(6) . . . . ? I1 Cu1 N1 C5 -10.4(6) . . . . ? Mo1 Cu1 N1 C5 166.4(6) . . . . ? N4 Cu2 N3 C15 -39.9(8) . . . . ? S2 Cu2 N3 C15 -164.4(7) . . . . ? S1 Cu2 N3 C15 83.4(7) . . . . ? Mo1 Cu2 N3 C15 137.5(7) . . . . ? N4 Cu2 N3 C11 155.1(7) . . . . ? S2 Cu2 N3 C11 30.5(8) . . . . ? S1 Cu2 N3 C11 -81.7(7) . . . . ? Mo1 Cu2 N3 C11 -27.5(8) . . . . ? N3 Cu2 N4 C20 136.2(7) . . . . ? S2 Cu2 N4 C20 -101.9(7) . . . . ? S1 Cu2 N4 C20 25.0(8) . . . . ? Mo1 Cu2 N4 C20 -40.2(9) . . . . ? N3 Cu2 N4 C16 -51.6(7) . . . . ? S2 Cu2 N4 C16 70.3(7) . . . . ? S1 Cu2 N4 C16 -162.9(6) . . . . ? Mo1 Cu2 N4 C16 132.0(6) . . . . ? C5 N1 C1 C2 0.1(14) . . . . ? Cu1 N1 C1 C2 159.9(8) . . . . ? N1 C1 C2 C3 -0.4(15) . . . . ? C1 C2 C3 C4 0.9(13) . . . . ? C1 C2 C3 C8 -175.1(8) . . . . ? C2 C3 C4 C5 -1.0(13) . . . . ? C8 C3 C4 C5 174.9(9) . . . . ? C1 N1 C5 C4 -0.2(14) . . . . ? Cu1 N1 C5 C4 -161.1(8) . . . . ? C3 C4 C5 N1 0.7(15) . . . . ? C10 N2 C6 C7 2.9(17) . . . . ? Cu3 N2 C6 C7 -171.6(9) 4_545 . . . ? N2 C6 C7 C8 -2.8(18) . . . . ? C6 C7 C8 C9 1.8(16) . . . . ? C6 C7 C8 C3 174.4(10) . . . . ? C4 C3 C8 C7 -133.4(11) . . . . ? C2 C3 C8 C7 42.4(14) . . . . ? C4 C3 C8 C9 38.9(14) . . . . ? C2 C3 C8 C9 -145.3(10) . . . . ? C7 C8 C9 C10 -1.2(17) . . . . ? C3 C8 C9 C10 -173.9(10) . . . . ? C6 N2 C10 C9 -2.3(16) . . . . ? Cu3 N2 C10 C9 172.7(9) 4_545 . . . ? C8 C9 C10 N2 1.5(18) . . . . ? C15 N3 C11 C12 0.4(16) . . . . ? Cu2 N3 C11 C12 166.4(9) . . . . ? N3 C11 C12 C13 0.3(17) . . . . ? C11 C12 C13 C14 0.4(15) . . . . ? C11 C12 C13 C13 178.2(9) . . . 2_556 ? C12 C13 C14 C15 -1.8(13) . . . . ? C13 C13 C14 C15 -179.6(7) 2_556 . . . ? C11 N3 C15 C14 -1.8(14) . . . . ? Cu2 N3 C15 C14 -167.3(7) . . . . ? C13 C14 C15 N3 2.6(14) . . . . ? C20 N4 C16 C17 -3.7(13) . . . . ? Cu2 N4 C16 C17 -176.2(7) . . . . ? N4 C16 C17 C18 2.4(14) . . . . ? C16 C17 C18 C19 -3.9(14) . . . . ? C16 C17 C18 C23 -179.3(8) . . . . ? C17 C18 C19 C20 7.2(15) . . . . ? C23 C18 C19 C20 -177.5(9) . . . . ? C18 C19 C20 N4 -9.0(16) . . . . ? C16 N4 C20 C19 7.0(14) . . . . ? Cu2 N4 C20 C19 179.6(8) . . . . ? C25 N5 C21 C22 3.1(16) . . . . ? Cu3 N5 C21 C22 -168.9(9) 2_656 . . . ? N5 C21 C22 C23 -3.0(18) . . . . ? C21 C22 C23 C24 1.6(16) . . . . ? C21 C22 C23 C18 176.5(10) . . . . ? C17 C18 C23 C22 153.1(10) . . . . ? C19 C18 C23 C22 -22.0(15) . . . . ? C17 C18 C23 C24 -32.3(14) . . . . ? C19 C18 C23 C24 152.6(10) . . . . ? C22 C23 C24 C25 -0.7(16) . . . . ? C18 C23 C24 C25 -175.7(10) . . . . ? C21 N5 C25 C24 -2.2(18) . . . . ? Cu3 N5 C25 C24 169.1(10) 2_656 . . . ? C23 C24 C25 N5 1(2) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 2.226 _refine_diff_density_min -2.645 _refine_diff_density_rms 0.228 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 -0.005 1415.6 79.3 2 0.500 0.500 -0.033 1414.5 79.5 _platon_squeeze_details ; ? ; # Attachment '- cif 1.cif' data_nyy0303 _database_code_depnum_ccdc_archive 'CCDC 845163' #TrackingRef '- cif 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ;2(C25 H20 Cu3 I Mo N5 O S3), 4(C1.50 H3.50 N0.50 O0.50), C3 N O ; _chemical_formula_sum 'C62 H68 Cu6 I2 Mo2 N14 O6 S6' _chemical_formula_weight 2124.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c 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 21.2500(10) _cell_length_b 21.2819(8) _cell_length_c 18.1026(7) _cell_angle_alpha 90.00 _cell_angle_beta 96.336(4) _cell_angle_gamma 90.00 _cell_volume 8136.7(6) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 5493 _cell_measurement_theta_min 2.9591 _cell_measurement_theta_max 26.3147 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.734 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4184 _exptl_absorpt_coefficient_mu 2.800 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4872 _exptl_absorpt_correction_T_max 0.5412 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _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 'Xcalibur, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18816 _diffrn_reflns_av_R_equivalents 0.0375 _diffrn_reflns_av_sigmaI/netI 0.0549 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 26.37 _reflns_number_total 8301 _reflns_number_gt 6169 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0583P)^2^+21.1802P] 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 8301 _refine_ls_number_parameters 410 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0750 _refine_ls_R_factor_gt 0.0511 _refine_ls_wR_factor_ref 0.1324 _refine_ls_wR_factor_gt 0.1197 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.050 _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 I1 I 0.38714(3) -0.14045(2) 0.07014(3) 0.06080(16) Uani 1 1 d . . . Mo1 Mo 0.21525(2) 0.01756(2) -0.00410(2) 0.03117(13) Uani 1 1 d . . . Cu1 Cu 0.31835(4) 0.08788(3) -0.02574(4) 0.03625(18) Uani 1 1 d . . . Cu2 Cu 0.28544(4) -0.08913(3) 0.01048(4) 0.0405(2) Uani 1 1 d . . . Cu3 Cu 0.23805(3) 0.04295(3) 0.14125(3) 0.03706(18) Uani 1 1 d . . . S1 S 0.29158(8) -0.00967(6) -0.07495(7) 0.0370(3) Uani 1 1 d . . . S2 S 0.24047(8) 0.11328(6) 0.04642(7) 0.0372(3) Uani 1 1 d . . . S3 S 0.21661(8) -0.05378(7) 0.08904(8) 0.0404(4) Uani 1 1 d . . . O1 O 0.1427(2) 0.0188(2) -0.0549(2) 0.0572(13) Uani 1 1 d . . . O2 O 0.4401(5) 0.2898(5) -0.0092(6) 0.167(4) Uiso 1 1 d . . . O3 O 0.0742(11) 0.2351(10) -0.3092(12) 0.178(8) Uiso 0.50 1 d P . . O4 O -0.0142(15) 0.2006(14) 0.1947(14) 0.238(12) Uiso 0.50 1 d P . . N8 N 0.0000 0.2842(7) 0.2500 0.115(4) Uiso 1 2 d SD . . N1 N 0.3182(3) 0.1474(2) -0.1170(2) 0.0431(13) Uani 1 1 d . . . N2 N 0.2568(3) 0.3384(2) -0.4360(2) 0.0409(12) Uani 1 1 d . . . N3 N 0.3124(2) 0.0514(2) 0.2192(2) 0.0377(11) Uani 1 1 d . . . N4 N 0.5930(2) 0.0859(2) 0.4687(3) 0.0392(12) Uani 1 1 d . . . N5 N 0.1532(2) 0.0556(2) 0.1903(2) 0.0400(12) Uani 1 1 d . . . N6 N 0.5178(6) 0.3544(5) 0.0268(5) 0.123(3) Uiso 1 1 d . . . N7 N 0.1192(7) 0.1999(6) -0.1956(7) 0.072(4) Uiso 0.50 1 d PD . . C1 C 0.3269(4) 0.2092(3) -0.1138(3) 0.059(2) Uani 1 1 d . . . H1 H 0.3391 0.2273 -0.0677 0.070 Uiso 1 1 calc R . . C2 C 0.3188(4) 0.2479(3) -0.1753(3) 0.060(2) Uani 1 1 d . . . H2 H 0.3245 0.2910 -0.1699 0.072 Uiso 1 1 calc R . . C3 C 0.3021(3) 0.2224(3) -0.2450(3) 0.0438(15) Uani 1 1 d . . . C4 C 0.2939(4) 0.1574(3) -0.2482(3) 0.057(2) Uani 1 1 d . . . H4 H 0.2830 0.1377 -0.2937 0.069 Uiso 1 1 calc R . . C5 C 0.3020(4) 0.1225(3) -0.1842(3) 0.057(2) Uani 1 1 d . . . H5 H 0.2958 0.0793 -0.1877 0.069 Uiso 1 1 calc R . . C6 C 0.3067(3) 0.3504(3) -0.3868(3) 0.0443(15) Uani 1 1 d . . . H6 H 0.3313 0.3854 -0.3947 0.053 Uiso 1 1 calc R . . C7 C 0.3238(3) 0.3139(3) -0.3249(3) 0.0487(17) Uani 1 1 d . . . H7 H 0.3588 0.3248 -0.2919 0.058 Uiso 1 1 calc R . . C8 C 0.2892(3) 0.2617(2) -0.3122(3) 0.0400(14) Uani 1 1 d . . . C9 C 0.2389(3) 0.2472(3) -0.3654(3) 0.0501(18) Uani 1 1 d . . . H9 H 0.2154 0.2109 -0.3605 0.060 Uiso 1 1 calc R . . C10 C 0.2240(3) 0.2861(3) -0.4247(3) 0.0459(16) Uani 1 1 d . . . H10 H 0.1896 0.2758 -0.4589 0.055 Uiso 1 1 calc R . . C11 C 0.3591(3) 0.0097(3) 0.2241(3) 0.0492(17) Uani 1 1 d . . . H11 H 0.3550 -0.0250 0.1926 0.059 Uiso 1 1 calc R . . C12 C 0.4133(3) 0.0145(3) 0.2731(4) 0.0516(17) Uani 1 1 d . . . H12 H 0.4440 -0.0167 0.2747 0.062 Uiso 1 1 calc R . . C13 C 0.4221(3) 0.0660(3) 0.3199(3) 0.0370(13) Uani 1 1 d . . . C14 C 0.3737(3) 0.1095(3) 0.3156(3) 0.0420(15) Uani 1 1 d . . . H14 H 0.3769 0.1447 0.3462 0.050 Uiso 1 1 calc R . . C15 C 0.3204(3) 0.1003(3) 0.2658(3) 0.0447(15) Uani 1 1 d . . . H15 H 0.2882 0.1300 0.2645 0.054 Uiso 1 1 calc R . . C16 C 0.5681(3) 0.0306(3) 0.4487(4) 0.059(2) Uani 1 1 d . . . H16 H 0.5896 -0.0051 0.4675 0.071 Uiso 1 1 calc R . . C17 C 0.5132(3) 0.0217(3) 0.4024(4) 0.059(2) Uani 1 1 d . . . H17 H 0.4984 -0.0187 0.3913 0.070 Uiso 1 1 calc R . . C18 C 0.4802(3) 0.0732(3) 0.3724(3) 0.0382(14) Uani 1 1 d . . . C19 C 0.5039(4) 0.1304(3) 0.3953(4) 0.065(2) Uani 1 1 d . . . H19 H 0.4827 0.1668 0.3783 0.078 Uiso 1 1 calc R . . C20 C 0.5586(4) 0.1349(3) 0.4429(4) 0.067(2) Uani 1 1 d . . . H20 H 0.5725 0.1748 0.4580 0.080 Uiso 1 1 calc R . . C21 C 0.1431(3) 0.0348(3) 0.2574(3) 0.0420(15) Uani 1 1 d . . . H21 H 0.1778 0.0205 0.2886 0.050 Uiso 1 1 calc R . . C22 C 0.0854(3) 0.0330(3) 0.2832(3) 0.0414(14) Uani 1 1 d . . . H22 H 0.0815 0.0186 0.3310 0.050 Uiso 1 1 calc R . . C23 C 0.0320(3) 0.0530(3) 0.2372(3) 0.0364(13) Uani 1 1 d . . . C24 C 0.0418(3) 0.0743(3) 0.1680(3) 0.0528(18) Uani 1 1 d . . . H24 H 0.0077 0.0878 0.1352 0.063 Uiso 1 1 calc R . . C25 C 0.1018(3) 0.0758(4) 0.1469(3) 0.0539(18) Uani 1 1 d . . . H25 H 0.1072 0.0916 0.1002 0.065 Uiso 1 1 calc R . . C26 C 0.5735(10) 0.3231(9) 0.0223(10) 0.211(8) Uiso 1 1 d . . . H26A H 0.5912 0.3105 0.0712 0.317 Uiso 1 1 calc R . . H26B H 0.6028 0.3503 0.0010 0.317 Uiso 1 1 calc R . . H26C H 0.5658 0.2866 -0.0085 0.317 Uiso 1 1 calc R . . C27 C 0.5219(8) 0.4175(7) 0.0547(8) 0.170(6) Uiso 1 1 d . . . H27A H 0.4803 0.4355 0.0517 0.255 Uiso 1 1 calc R . . H27B H 0.5479 0.4421 0.0255 0.255 Uiso 1 1 calc R . . H27C H 0.5404 0.4172 0.1055 0.255 Uiso 1 1 calc R . . C28 C 0.4553(13) 0.3399(12) 0.0159(12) 0.236(10) Uiso 1 1 d . . . H28 H 0.4249 0.3685 0.0279 0.283 Uiso 1 1 calc R . . C29 C 0.1554(13) 0.2171(13) -0.1280(12) 0.154(10) Uiso 0.50 1 d PD . . H29A H 0.1306 0.2106 -0.0873 0.230 Uiso 0.50 1 calc PR . . H29B H 0.1671 0.2606 -0.1300 0.230 Uiso 0.50 1 calc PR . . H29C H 0.1929 0.1917 -0.1208 0.230 Uiso 0.50 1 calc PR . . C30 C 0.1193(12) 0.1362(8) -0.2081(13) 0.123(8) Uiso 0.50 1 d PD . . H30A H 0.1422 0.1274 -0.2497 0.184 Uiso 0.50 1 calc PR . . H30B H 0.0765 0.1216 -0.2185 0.184 Uiso 0.50 1 calc PR . . H30C H 0.1393 0.1152 -0.1647 0.184 Uiso 0.50 1 calc PR . . C31 C 0.0985(14) 0.2427(16) -0.2394(14) 0.163(11) Uiso 0.50 1 d PD . . H31 H 0.1004 0.2836 -0.2210 0.196 Uiso 0.50 1 calc PR . . C32 C -0.0273(13) 0.3452(12) 0.2880(13) 0.278(12) Uiso 1 1 d . . . C33 C 0.0112(11) 0.2530(11) 0.1847(10) 0.109(7) Uiso 0.50 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.0606(3) 0.0496(3) 0.0678(3) 0.0011(2) -0.0125(2) 0.0079(2) Mo1 0.0316(3) 0.0338(3) 0.0264(2) -0.00314(18) -0.00465(19) 0.0005(2) Cu1 0.0381(4) 0.0390(4) 0.0304(3) 0.0039(3) -0.0020(3) -0.0005(3) Cu2 0.0520(5) 0.0338(4) 0.0347(4) -0.0021(3) 0.0001(3) 0.0041(3) Cu3 0.0326(4) 0.0478(4) 0.0297(3) -0.0049(3) -0.0013(3) 0.0005(3) S1 0.0500(10) 0.0343(7) 0.0268(6) -0.0014(5) 0.0050(6) 0.0024(7) S2 0.0440(9) 0.0326(7) 0.0348(7) -0.0038(6) 0.0032(6) 0.0030(6) S3 0.0492(10) 0.0370(8) 0.0354(7) 0.0002(6) 0.0065(7) -0.0032(7) O1 0.047(3) 0.072(3) 0.048(2) -0.008(2) -0.018(2) 0.005(2) N1 0.056(4) 0.038(3) 0.035(3) 0.007(2) 0.002(2) -0.004(2) N2 0.059(4) 0.032(2) 0.030(2) 0.0015(19) -0.003(2) 0.003(2) N3 0.031(3) 0.049(3) 0.033(2) -0.003(2) 0.001(2) 0.001(2) N4 0.037(3) 0.040(3) 0.039(3) -0.005(2) -0.005(2) 0.002(2) N5 0.036(3) 0.051(3) 0.034(3) -0.004(2) 0.004(2) 0.006(2) C1 0.099(6) 0.041(4) 0.032(3) 0.003(3) -0.007(3) -0.012(4) C2 0.099(6) 0.035(3) 0.042(4) 0.003(3) -0.004(4) -0.010(4) C3 0.058(4) 0.035(3) 0.037(3) 0.006(2) 0.000(3) 0.005(3) C4 0.109(7) 0.031(3) 0.031(3) 0.004(2) -0.001(3) 0.003(4) C5 0.103(7) 0.033(3) 0.035(3) 0.002(3) 0.002(4) 0.001(4) C6 0.054(4) 0.035(3) 0.043(3) 0.011(2) 0.003(3) -0.006(3) C7 0.061(5) 0.040(3) 0.042(3) 0.005(3) -0.006(3) 0.005(3) C8 0.059(4) 0.027(3) 0.034(3) 0.004(2) 0.006(3) 0.005(3) C9 0.073(5) 0.031(3) 0.043(3) 0.007(3) -0.007(3) -0.009(3) C10 0.060(5) 0.035(3) 0.042(3) 0.002(2) 0.000(3) -0.008(3) C11 0.043(4) 0.051(4) 0.050(4) -0.019(3) -0.013(3) 0.009(3) C12 0.041(4) 0.049(4) 0.060(4) -0.017(3) -0.015(3) 0.011(3) C13 0.031(3) 0.044(3) 0.035(3) 0.001(2) 0.002(2) -0.003(3) C14 0.040(4) 0.038(3) 0.046(3) -0.013(3) -0.006(3) 0.005(3) C15 0.034(4) 0.051(4) 0.048(3) -0.006(3) -0.002(3) 0.010(3) C16 0.054(5) 0.043(4) 0.072(5) -0.009(3) -0.025(4) 0.014(3) C17 0.051(5) 0.043(4) 0.075(5) -0.011(3) -0.026(4) -0.003(3) C18 0.031(3) 0.044(3) 0.038(3) -0.004(2) -0.004(2) 0.002(3) C19 0.048(5) 0.042(4) 0.097(6) 0.004(4) -0.033(4) 0.005(3) C20 0.066(6) 0.038(4) 0.087(5) -0.001(3) -0.032(4) -0.006(3) C21 0.039(4) 0.056(4) 0.028(3) 0.003(3) -0.006(3) 0.000(3) C22 0.036(4) 0.059(4) 0.029(3) 0.006(3) 0.002(2) -0.001(3) C23 0.030(3) 0.044(3) 0.034(3) -0.001(2) -0.001(2) 0.003(2) C24 0.030(4) 0.090(5) 0.038(3) 0.012(3) 0.002(3) 0.015(4) C25 0.039(4) 0.089(5) 0.034(3) 0.013(3) 0.005(3) 0.017(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 I1 Cu2 2.5524(9) . ? Mo1 O1 1.706(4) . ? Mo1 S1 2.2518(16) . ? Mo1 S3 2.2668(15) . ? Mo1 S2 2.2727(14) . ? Mo1 Cu3 2.6775(8) . ? Mo1 Cu2 2.7134(8) . ? Mo1 Cu1 2.7171(9) . ? Cu1 N4 2.046(5) 2_655 ? Cu1 N1 2.081(4) . ? Cu1 S2 2.2835(17) . ? Cu1 S1 2.3056(15) . ? Cu2 N2 2.176(4) 4_544 ? Cu2 S3 2.2774(18) . ? Cu2 S1 2.3049(15) . ? Cu3 N3 2.007(4) . ? Cu3 N5 2.112(5) . ? Cu3 S2 2.2825(16) . ? Cu3 S3 2.2899(16) . ? O2 C28 1.19(2) . ? O3 C31 1.32(3) . ? O4 C33 1.26(3) . ? N8 C33 1.398(15) . ? N8 C33 1.398(15) 2 ? N8 C32 1.61(3) 2 ? N8 C32 1.61(3) . ? N1 C1 1.329(7) . ? N1 C5 1.336(7) . ? N2 C6 1.332(8) . ? N2 C10 1.340(8) . ? N2 Cu2 2.176(4) 4_554 ? N3 C11 1.328(8) . ? N3 C15 1.338(7) . ? N4 C16 1.325(8) . ? N4 C20 1.328(8) . ? N4 Cu1 2.046(5) 2_655 ? N5 C21 1.332(7) . ? N5 C25 1.343(7) . ? N6 C28 1.36(2) . ? N6 C26 1.37(2) . ? N6 C27 1.435(15) . ? N7 C31 1.26(3) . ? N7 C30 1.374(15) . ? N7 C29 1.420(15) . ? C1 C2 1.381(8) . ? C1 H1 0.9300 . ? C2 C3 1.382(8) . ? C2 H2 0.9300 . ? C3 C4 1.396(8) . ? C3 C8 1.476(7) . ? C4 C5 1.371(8) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.380(8) . ? C6 H6 0.9300 . ? C7 C8 1.367(9) . ? C7 H7 0.9300 . ? C8 C9 1.390(8) . ? C9 C10 1.366(8) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.378(8) . ? C11 H11 0.9300 . ? C12 C13 1.384(8) . ? C12 H12 0.9300 . ? C13 C14 1.380(8) . ? C13 C18 1.482(8) . ? C14 C15 1.381(8) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.373(8) . ? C16 H16 0.9300 . ? C17 C18 1.380(8) . ? C17 H17 0.9300 . ? C18 C19 1.364(8) . ? C19 C20 1.371(9) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.361(9) . ? C21 H21 0.9300 . ? C22 C23 1.398(8) . ? C22 H22 0.9300 . ? C23 C24 1.370(8) . ? C23 C23 1.484(12) 2 ? C24 C25 1.370(9) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28 0.9300 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31 0.9300 . ? C32 C32 1.89(5) 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 O1 Mo1 S1 111.21(17) . . ? O1 Mo1 S3 110.35(17) . . ? S1 Mo1 S3 107.48(6) . . ? O1 Mo1 S2 111.24(16) . . ? S1 Mo1 S2 107.89(6) . . ? S3 Mo1 S2 108.54(5) . . ? O1 Mo1 Cu3 125.55(16) . . ? S1 Mo1 Cu3 123.24(4) . . ? S3 Mo1 Cu3 54.41(4) . . ? S2 Mo1 Cu3 54.17(4) . . ? O1 Mo1 Cu2 121.30(16) . . ? S1 Mo1 Cu2 54.36(4) . . ? S3 Mo1 Cu2 53.52(5) . . ? S2 Mo1 Cu2 127.46(4) . . ? Cu3 Mo1 Cu2 92.02(2) . . ? O1 Mo1 Cu1 127.51(17) . . ? S1 Mo1 Cu1 54.32(4) . . ? S3 Mo1 Cu1 122.13(5) . . ? S2 Mo1 Cu1 53.57(4) . . ? Cu3 Mo1 Cu1 88.24(2) . . ? Cu2 Mo1 Cu1 91.81(3) . . ? N4 Cu1 N1 109.5(2) 2_655 . ? N4 Cu1 S2 113.66(15) 2_655 . ? N1 Cu1 S2 111.88(16) . . ? N4 Cu1 S1 110.52(14) 2_655 . ? N1 Cu1 S1 105.22(14) . . ? S2 Cu1 S1 105.70(6) . . ? N4 Cu1 Mo1 128.91(13) 2_655 . ? N1 Cu1 Mo1 121.27(15) . . ? S2 Cu1 Mo1 53.21(4) . . ? S1 Cu1 Mo1 52.50(4) . . ? N2 Cu2 S3 111.84(16) 4_544 . ? N2 Cu2 S1 98.88(12) 4_544 . ? S3 Cu2 S1 105.34(6) . . ? N2 Cu2 I1 103.32(14) 4_544 . ? S3 Cu2 I1 116.70(5) . . ? S1 Cu2 I1 119.33(5) . . ? N2 Cu2 Mo1 110.40(14) 4_544 . ? S3 Cu2 Mo1 53.16(4) . . ? S1 Cu2 Mo1 52.56(4) . . ? I1 Cu2 Mo1 146.09(3) . . ? N3 Cu3 N5 109.59(19) . . ? N3 Cu3 S2 112.87(15) . . ? N5 Cu3 S2 108.87(14) . . ? N3 Cu3 S3 118.44(15) . . ? N5 Cu3 S3 98.51(14) . . ? S2 Cu3 S3 107.40(5) . . ? N3 Cu3 Mo1 138.77(14) . . ? N5 Cu3 Mo1 111.61(12) . . ? S2 Cu3 Mo1 53.83(4) . . ? S3 Cu3 Mo1 53.62(4) . . ? Mo1 S1 Cu2 73.08(5) . . ? Mo1 S1 Cu1 73.19(5) . . ? Cu2 S1 Cu1 115.54(6) . . ? Mo1 S2 Cu3 72.00(5) . . ? Mo1 S2 Cu1 73.22(5) . . ? Cu3 S2 Cu1 110.67(6) . . ? Mo1 S3 Cu2 73.32(5) . . ? Mo1 S3 Cu3 71.97(5) . . ? Cu2 S3 Cu3 116.26(7) . . ? C33 N8 C33 123(2) . 2 ? C33 N8 C32 85.4(13) . 2 ? C33 N8 C32 148.0(15) 2 2 ? C33 N8 C32 148.0(15) . . ? C33 N8 C32 85.4(13) 2 . ? C32 N8 C32 72.2(19) 2 . ? C1 N1 C5 116.9(5) . . ? C1 N1 Cu1 125.4(4) . . ? C5 N1 Cu1 117.3(4) . . ? C6 N2 C10 116.6(5) . . ? C6 N2 Cu2 121.3(4) . 4_554 ? C10 N2 Cu2 119.8(4) . 4_554 ? C11 N3 C15 115.8(5) . . ? C11 N3 Cu3 120.8(4) . . ? C15 N3 Cu3 123.3(4) . . ? C16 N4 C20 114.5(5) . . ? C16 N4 Cu1 118.2(4) . 2_655 ? C20 N4 Cu1 127.0(4) . 2_655 ? C21 N5 C25 115.8(5) . . ? C21 N5 Cu3 124.8(4) . . ? C25 N5 Cu3 118.2(4) . . ? C28 N6 C26 136.1(17) . . ? C28 N6 C27 106.5(16) . . ? C26 N6 C27 117.1(14) . . ? C31 N7 C30 128(2) . . ? C31 N7 C29 118.5(19) . . ? C30 N7 C29 112.7(17) . . ? N1 C1 C2 123.4(5) . . ? N1 C1 H1 118.3 . . ? C2 C1 H1 118.3 . . ? C1 C2 C3 120.0(6) . . ? C1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? C2 C3 C4 116.4(5) . . ? C2 C3 C8 122.4(5) . . ? C4 C3 C8 121.0(5) . . ? C5 C4 C3 119.9(5) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? N1 C5 C4 123.4(6) . . ? N1 C5 H5 118.3 . . ? C4 C5 H5 118.3 . . ? N2 C6 C7 123.6(6) . . ? N2 C6 H6 118.2 . . ? C7 C6 H6 118.2 . . ? C8 C7 C6 119.7(6) . . ? C8 C7 H7 120.1 . . ? C6 C7 H7 120.1 . . ? C7 C8 C9 116.8(5) . . ? C7 C8 C3 122.9(5) . . ? C9 C8 C3 120.2(5) . . ? C10 C9 C8 120.3(6) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? N2 C10 C9 122.9(6) . . ? N2 C10 H10 118.5 . . ? C9 C10 H10 118.5 . . ? N3 C11 C12 124.0(6) . . ? N3 C11 H11 118.0 . . ? C12 C11 H11 118.0 . . ? C11 C12 C13 120.0(6) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C14 C13 C12 116.6(5) . . ? C14 C13 C18 122.0(5) . . ? C12 C13 C18 121.4(5) . . ? C13 C14 C15 119.6(5) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? N3 C15 C14 124.1(6) . . ? N3 C15 H15 118.0 . . ? C14 C15 H15 118.0 . . ? N4 C16 C17 125.1(6) . . ? N4 C16 H16 117.4 . . ? C17 C16 H16 117.4 . . ? C16 C17 C18 119.4(6) . . ? C16 C17 H17 120.3 . . ? C18 C17 H17 120.3 . . ? C19 C18 C17 115.8(5) . . ? C19 C18 C13 122.7(5) . . ? C17 C18 C13 121.4(5) . . ? C18 C19 C20 120.7(6) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? N4 C20 C19 124.2(6) . . ? N4 C20 H20 117.9 . . ? C19 C20 H20 117.9 . . ? N5 C21 C22 124.4(5) . . ? N5 C21 H21 117.8 . . ? C22 C21 H21 117.8 . . ? C21 C22 C23 119.3(5) . . ? C21 C22 H22 120.4 . . ? C23 C22 H22 120.4 . . ? C24 C23 C22 116.8(5) . . ? C24 C23 C23 121.6(6) . 2 ? C22 C23 C23 121.6(6) . 2 ? C23 C24 C25 120.2(5) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? N5 C25 C24 123.5(6) . . ? N5 C25 H25 118.2 . . ? C24 C25 H25 118.2 . . ? N6 C26 H26A 109.5 . . ? N6 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N6 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N6 C27 H27A 109.5 . . ? N6 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N6 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O2 C28 N6 119(2) . . ? O2 C28 H28 120.7 . . ? N6 C28 H28 120.7 . . ? N7 C29 H29A 109.5 . . ? N7 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N7 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N7 C30 H30A 109.5 . . ? N7 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? N7 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N7 C31 O3 126(3) . . ? N7 C31 H31 117.0 . . ? O3 C31 H31 117.0 . . ? N8 C32 C32 53.9(9) . 2 ? O4 C33 N8 101(2) . . ? 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 O1 Mo1 Cu1 N4 -177.6(3) . . . 2_655 ? S1 Mo1 Cu1 N4 -87.04(19) . . . 2_655 ? S3 Mo1 Cu1 N4 2.14(19) . . . 2_655 ? S2 Mo1 Cu1 N4 92.32(19) . . . 2_655 ? Cu3 Mo1 Cu1 N4 47.16(18) . . . 2_655 ? Cu2 Mo1 Cu1 N4 -44.81(18) . . . 2_655 ? O1 Mo1 Cu1 N1 -5.1(3) . . . . ? S1 Mo1 Cu1 N1 85.47(17) . . . . ? S3 Mo1 Cu1 N1 174.65(17) . . . . ? S2 Mo1 Cu1 N1 -95.17(17) . . . . ? Cu3 Mo1 Cu1 N1 -140.33(17) . . . . ? Cu2 Mo1 Cu1 N1 127.70(17) . . . . ? O1 Mo1 Cu1 S2 90.1(2) . . . . ? S1 Mo1 Cu1 S2 -179.36(6) . . . . ? S3 Mo1 Cu1 S2 -90.18(7) . . . . ? Cu3 Mo1 Cu1 S2 -45.16(5) . . . . ? Cu2 Mo1 Cu1 S2 -137.13(5) . . . . ? O1 Mo1 Cu1 S1 -90.6(2) . . . . ? S3 Mo1 Cu1 S1 89.18(7) . . . . ? S2 Mo1 Cu1 S1 179.36(6) . . . . ? Cu3 Mo1 Cu1 S1 134.20(5) . . . . ? Cu2 Mo1 Cu1 S1 42.23(5) . . . . ? O1 Mo1 Cu2 N2 9.3(2) . . . 4_544 ? S1 Mo1 Cu2 N2 -85.56(15) . . . 4_544 ? S3 Mo1 Cu2 N2 102.56(15) . . . 4_544 ? S2 Mo1 Cu2 N2 -171.37(15) . . . 4_544 ? Cu3 Mo1 Cu2 N2 143.93(15) . . . 4_544 ? Cu1 Mo1 Cu2 N2 -127.77(15) . . . 4_544 ? O1 Mo1 Cu2 S3 -93.2(2) . . . . ? S1 Mo1 Cu2 S3 171.88(7) . . . . ? S2 Mo1 Cu2 S3 86.08(7) . . . . ? Cu3 Mo1 Cu2 S3 41.38(5) . . . . ? Cu1 Mo1 Cu2 S3 129.68(5) . . . . ? O1 Mo1 Cu2 S1 94.9(2) . . . . ? S3 Mo1 Cu2 S1 -171.88(7) . . . . ? S2 Mo1 Cu2 S1 -85.81(7) . . . . ? Cu3 Mo1 Cu2 S1 -130.50(5) . . . . ? Cu1 Mo1 Cu2 S1 -42.20(5) . . . . ? O1 Mo1 Cu2 I1 -177.0(2) . . . . ? S1 Mo1 Cu2 I1 88.10(8) . . . . ? S3 Mo1 Cu2 I1 -83.78(8) . . . . ? S2 Mo1 Cu2 I1 2.29(9) . . . . ? Cu3 Mo1 Cu2 I1 -42.40(7) . . . . ? Cu1 Mo1 Cu2 I1 45.89(6) . . . . ? O1 Mo1 Cu3 N3 -175.9(3) . . . . ? S1 Mo1 Cu3 N3 4.8(2) . . . . ? S3 Mo1 Cu3 N3 93.3(2) . . . . ? S2 Mo1 Cu3 N3 -84.0(2) . . . . ? Cu2 Mo1 Cu3 N3 52.4(2) . . . . ? Cu1 Mo1 Cu3 N3 -39.3(2) . . . . ? O1 Mo1 Cu3 N5 6.2(2) . . . . ? S1 Mo1 Cu3 N5 -173.04(15) . . . . ? S3 Mo1 Cu3 N5 -84.59(16) . . . . ? S2 Mo1 Cu3 N5 98.12(16) . . . . ? Cu2 Mo1 Cu3 N5 -125.41(15) . . . . ? Cu1 Mo1 Cu3 N5 142.84(15) . . . . ? O1 Mo1 Cu3 S2 -91.9(2) . . . . ? S1 Mo1 Cu3 S2 88.85(7) . . . . ? S3 Mo1 Cu3 S2 177.29(8) . . . . ? Cu2 Mo1 Cu3 S2 136.48(6) . . . . ? Cu1 Mo1 Cu3 S2 44.72(5) . . . . ? O1 Mo1 Cu3 S3 90.8(2) . . . . ? S1 Mo1 Cu3 S3 -88.44(7) . . . . ? S2 Mo1 Cu3 S3 -177.29(8) . . . . ? Cu2 Mo1 Cu3 S3 -40.81(6) . . . . ? Cu1 Mo1 Cu3 S3 -132.56(6) . . . . ? O1 Mo1 S1 Cu2 -114.05(18) . . . . ? S3 Mo1 S1 Cu2 6.84(6) . . . . ? S2 Mo1 S1 Cu2 123.71(5) . . . . ? Cu3 Mo1 S1 Cu2 65.30(5) . . . . ? Cu1 Mo1 S1 Cu2 124.25(5) . . . . ? O1 Mo1 S1 Cu1 121.70(18) . . . . ? S3 Mo1 S1 Cu1 -117.41(5) . . . . ? S2 Mo1 S1 Cu1 -0.54(5) . . . . ? Cu3 Mo1 S1 Cu1 -58.95(5) . . . . ? Cu2 Mo1 S1 Cu1 -124.25(5) . . . . ? N2 Cu2 S1 Mo1 108.95(15) 4_544 . . . ? S3 Cu2 S1 Mo1 -6.73(6) . . . . ? I1 Cu2 S1 Mo1 -140.24(4) . . . . ? N2 Cu2 S1 Cu1 170.23(16) 4_544 . . . ? S3 Cu2 S1 Cu1 54.55(9) . . . . ? I1 Cu2 S1 Cu1 -78.96(8) . . . . ? Mo1 Cu2 S1 Cu1 61.28(6) . . . . ? N4 Cu1 S1 Mo1 123.93(15) 2_655 . . . ? N1 Cu1 S1 Mo1 -117.99(17) . . . . ? S2 Cu1 S1 Mo1 0.53(5) . . . . ? N4 Cu1 S1 Cu2 62.70(17) 2_655 . . . ? N1 Cu1 S1 Cu2 -179.22(17) . . . . ? S2 Cu1 S1 Cu2 -60.69(8) . . . . ? Mo1 Cu1 S1 Cu2 -61.23(6) . . . . ? O1 Mo1 S2 Cu3 119.26(18) . . . . ? S1 Mo1 S2 Cu3 -118.51(5) . . . . ? S3 Mo1 S2 Cu3 -2.33(7) . . . . ? Cu2 Mo1 S2 Cu3 -60.11(6) . . . . ? Cu1 Mo1 S2 Cu3 -119.05(5) . . . . ? O1 Mo1 S2 Cu1 -121.68(18) . . . . ? S1 Mo1 S2 Cu1 0.55(5) . . . . ? S3 Mo1 S2 Cu1 116.73(6) . . . . ? Cu3 Mo1 S2 Cu1 119.05(5) . . . . ? Cu2 Mo1 S2 Cu1 58.94(6) . . . . ? N3 Cu3 S2 Mo1 134.65(16) . . . . ? N5 Cu3 S2 Mo1 -103.43(14) . . . . ? S3 Cu3 S2 Mo1 2.29(7) . . . . ? N3 Cu3 S2 Cu1 71.20(16) . . . . ? N5 Cu3 S2 Cu1 -166.88(14) . . . . ? S3 Cu3 S2 Cu1 -61.16(8) . . . . ? Mo1 Cu3 S2 Cu1 -63.45(5) . . . . ? N4 Cu1 S2 Mo1 -121.91(14) 2_655 . . . ? N1 Cu1 S2 Mo1 113.47(15) . . . . ? S1 Cu1 S2 Mo1 -0.53(5) . . . . ? N4 Cu1 S2 Cu3 -59.22(16) 2_655 . . . ? N1 Cu1 S2 Cu3 176.17(15) . . . . ? S1 Cu1 S2 Cu3 62.17(7) . . . . ? Mo1 Cu1 S2 Cu3 62.70(5) . . . . ? O1 Mo1 S3 Cu2 114.51(17) . . . . ? S1 Mo1 S3 Cu2 -6.91(6) . . . . ? S2 Mo1 S3 Cu2 -123.36(6) . . . . ? Cu3 Mo1 S3 Cu2 -125.67(6) . . . . ? Cu1 Mo1 S3 Cu2 -65.29(5) . . . . ? O1 Mo1 S3 Cu3 -119.81(17) . . . . ? S1 Mo1 S3 Cu3 118.76(5) . . . . ? S2 Mo1 S3 Cu3 2.32(7) . . . . ? Cu2 Mo1 S3 Cu3 125.67(6) . . . . ? Cu1 Mo1 S3 Cu3 60.38(6) . . . . ? N2 Cu2 S3 Mo1 -99.72(13) 4_544 . . . ? S1 Cu2 S3 Mo1 6.68(6) . . . . ? I1 Cu2 S3 Mo1 141.63(4) . . . . ? N2 Cu2 S3 Cu3 -159.19(14) 4_544 . . . ? S1 Cu2 S3 Cu3 -52.79(8) . . . . ? I1 Cu2 S3 Cu3 82.16(7) . . . . ? Mo1 Cu2 S3 Cu3 -59.47(6) . . . . ? N3 Cu3 S3 Mo1 -131.55(16) . . . . ? N5 Cu3 S3 Mo1 110.63(13) . . . . ? S2 Cu3 S3 Mo1 -2.29(7) . . . . ? N3 Cu3 S3 Cu2 -71.36(18) . . . . ? N5 Cu3 S3 Cu2 170.83(14) . . . . ? S2 Cu3 S3 Cu2 57.90(9) . . . . ? Mo1 Cu3 S3 Cu2 60.19(6) . . . . ? N4 Cu1 N1 C1 -66.2(7) 2_655 . . . ? S2 Cu1 N1 C1 60.8(6) . . . . ? S1 Cu1 N1 C1 175.0(6) . . . . ? Mo1 Cu1 N1 C1 120.0(6) . . . . ? N4 Cu1 N1 C5 120.8(5) 2_655 . . . ? S2 Cu1 N1 C5 -112.3(5) . . . . ? S1 Cu1 N1 C5 2.0(6) . . . . ? Mo1 Cu1 N1 C5 -53.0(6) . . . . ? N5 Cu3 N3 C11 133.0(5) . . . . ? S2 Cu3 N3 C11 -105.5(5) . . . . ? S3 Cu3 N3 C11 21.2(6) . . . . ? Mo1 Cu3 N3 C11 -44.9(6) . . . . ? N5 Cu3 N3 C15 -51.3(5) . . . . ? S2 Cu3 N3 C15 70.2(5) . . . . ? S3 Cu3 N3 C15 -163.1(4) . . . . ? Mo1 Cu3 N3 C15 130.8(4) . . . . ? N3 Cu3 N5 C21 -38.0(5) . . . . ? S2 Cu3 N5 C21 -161.9(4) . . . . ? S3 Cu3 N5 C21 86.3(5) . . . . ? Mo1 Cu3 N5 C21 140.5(4) . . . . ? N3 Cu3 N5 C25 154.6(5) . . . . ? S2 Cu3 N5 C25 30.7(5) . . . . ? S3 Cu3 N5 C25 -81.1(5) . . . . ? Mo1 Cu3 N5 C25 -26.9(5) . . . . ? C5 N1 C1 C2 1.3(12) . . . . ? Cu1 N1 C1 C2 -171.8(6) . . . . ? N1 C1 C2 C3 -1.5(13) . . . . ? C1 C2 C3 C4 0.5(12) . . . . ? C1 C2 C3 C8 176.4(7) . . . . ? C2 C3 C4 C5 0.5(12) . . . . ? C8 C3 C4 C5 -175.5(7) . . . . ? C1 N1 C5 C4 -0.2(12) . . . . ? Cu1 N1 C5 C4 173.4(6) . . . . ? C3 C4 C5 N1 -0.7(13) . . . . ? C10 N2 C6 C7 -2.9(9) . . . . ? Cu2 N2 C6 C7 160.1(5) 4_554 . . . ? N2 C6 C7 C8 0.9(10) . . . . ? C6 C7 C8 C9 2.3(9) . . . . ? C6 C7 C8 C3 -176.2(6) . . . . ? C2 C3 C8 C7 39.7(10) . . . . ? C4 C3 C8 C7 -144.6(7) . . . . ? C2 C3 C8 C9 -138.7(7) . . . . ? C4 C3 C8 C9 37.0(10) . . . . ? C7 C8 C9 C10 -3.4(10) . . . . ? C3 C8 C9 C10 175.1(6) . . . . ? C6 N2 C10 C9 1.7(10) . . . . ? Cu2 N2 C10 C9 -161.6(5) 4_554 . . . ? C8 C9 C10 N2 1.5(11) . . . . ? C15 N3 C11 C12 -0.2(10) . . . . ? Cu3 N3 C11 C12 175.8(6) . . . . ? N3 C11 C12 C13 -1.4(11) . . . . ? C11 C12 C13 C14 1.7(10) . . . . ? C11 C12 C13 C18 -179.1(6) . . . . ? C12 C13 C14 C15 -0.6(9) . . . . ? C18 C13 C14 C15 -179.8(6) . . . . ? C11 N3 C15 C14 1.3(10) . . . . ? Cu3 N3 C15 C14 -174.6(5) . . . . ? C13 C14 C15 N3 -0.9(10) . . . . ? C20 N4 C16 C17 3.1(12) . . . . ? Cu1 N4 C16 C17 -171.1(7) 2_655 . . . ? N4 C16 C17 C18 0.8(13) . . . . ? C16 C17 C18 C19 -3.5(11) . . . . ? C16 C17 C18 C13 177.6(7) . . . . ? C14 C13 C18 C19 -29.5(10) . . . . ? C12 C13 C18 C19 151.3(7) . . . . ? C14 C13 C18 C17 149.3(7) . . . . ? C12 C13 C18 C17 -29.9(10) . . . . ? C17 C18 C19 C20 2.4(12) . . . . ? C13 C18 C19 C20 -178.7(7) . . . . ? C16 N4 C20 C19 -4.3(12) . . . . ? Cu1 N4 C20 C19 169.3(7) 2_655 . . . ? C18 C19 C20 N4 1.6(14) . . . . ? C25 N5 C21 C22 0.0(9) . . . . ? Cu3 N5 C21 C22 -167.6(5) . . . . ? N5 C21 C22 C23 1.2(10) . . . . ? C21 C22 C23 C24 -0.9(9) . . . . ? C21 C22 C23 C23 -179.1(4) . . . 2 ? C22 C23 C24 C25 -0.5(10) . . . . ? C23 C23 C24 C25 177.6(5) 2 . . . ? C21 N5 C25 C24 -1.6(10) . . . . ? Cu3 N5 C25 C24 167.0(6) . . . . ? C23 C24 C25 N5 1.8(12) . . . . ? C26 N6 C28 O2 -7(4) . . . . ? C27 N6 C28 O2 178.0(17) . . . . ? C30 N7 C31 O3 -3(5) . . . . ? C29 N7 C31 O3 167(3) . . . . ? C33 N8 C32 C32 -48(3) . . . 2 ? C33 N8 C32 C32 156.9(17) 2 . . 2 ? C33 N8 C33 O4 22.8(17) 2 . . . ? C32 N8 C33 O4 -172(2) 2 . . . ? C32 N8 C33 O4 -128(3) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.128 _refine_diff_density_min -0.778 _refine_diff_density_rms 0.118 # Attachment '- cif 4.cif' data_a _database_code_depnum_ccdc_archive 'CCDC 845164' #TrackingRef '- cif 4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H20 Cu3 Mo N6 O S4' _chemical_formula_sum 'C52 H40 Cu6 Mo2 N12 O2 S8' _chemical_formula_weight 1694.56 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' 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c 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 40.592(8) _cell_length_b 9.7008(19) _cell_length_c 24.750(5) _cell_angle_alpha 90.00 _cell_angle_beta 104.95(3) _cell_angle_gamma 90.00 _cell_volume 9416(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9672 _cell_measurement_theta_min 2.0770 _cell_measurement_theta_max 27.9644 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.195 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3352 _exptl_absorpt_coefficient_mu 1.795 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6829 _exptl_absorpt_correction_T_max 0.7382 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 45938 _diffrn_reflns_av_R_equivalents 0.0984 _diffrn_reflns_av_sigmaI/netI 0.0765 _diffrn_reflns_limit_h_min -48 _diffrn_reflns_limit_h_max 48 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8255 _reflns_number_gt 5787 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0646P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8255 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0946 _refine_ls_R_factor_gt 0.0606 _refine_ls_wR_factor_ref 0.1505 _refine_ls_wR_factor_gt 0.1363 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _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 Mo1 Mo 0.089453(13) 0.62042(5) -0.04004(2) 0.05041(17) Uani 1 1 d . . . Cu1 Cu 0.107264(18) 0.35931(7) -0.01049(3) 0.0531(2) Uani 1 1 d . . . Cu2 Cu 0.14483(2) 0.70933(8) 0.03819(3) 0.0604(2) Uani 1 1 d . . . Cu3 Cu 0.130736(19) 0.60501(7) -0.10828(3) 0.0535(2) Uani 1 1 d . . . S1 S 0.10733(4) 0.54037(16) 0.04854(7) 0.0615(4) Uani 1 1 d . . . S2 S 0.12630(4) 0.78624(14) -0.05145(7) 0.0587(4) Uani 1 1 d . . . S3 S 0.09214(4) 0.44444(15) -0.09939(7) 0.0532(4) Uani 1 1 d . . . S4 S 0.26091(6) 0.5800(2) 0.11125(11) 0.0973(7) Uani 1 1 d . . . O1 O 0.04885(11) 0.6835(5) -0.0526(2) 0.0871(16) Uani 1 1 d . . . N1 N 0.15273(12) 0.2559(5) 0.0121(2) 0.0539(13) Uani 1 1 d . . . N2 N 0.31942(12) -0.0245(5) 0.0830(2) 0.0504(12) Uani 1 1 d . . . N3 N 0.07020(12) 0.2187(5) -0.0015(2) 0.0583(14) Uani 1 1 d . . . N4 N 0.13819(15) 0.8749(5) 0.0912(2) 0.0646(14) Uani 1 1 d . . . N5 N 0.13125(14) 1.3185(5) 0.3150(2) 0.0618(14) Uani 1 1 d . . . N6 N 0.19489(14) 0.6738(6) 0.0695(2) 0.0640(14) Uani 1 1 d . . . C1 C 0.16014(16) 0.1430(6) -0.0120(3) 0.0700(19) Uani 1 1 d . . . H1 H 0.1427 0.1020 -0.0391 0.084 Uiso 1 1 calc R . . C2 C 0.19176(15) 0.0813(7) 0.0001(3) 0.0623(17) Uani 1 1 d . . . H2 H 0.1952 0.0017 -0.0187 0.075 Uiso 1 1 calc R . . C3 C 0.21830(15) 0.1387(6) 0.0404(2) 0.0499(14) Uani 1 1 d . . . C4 C 0.20978(17) 0.2524(7) 0.0685(3) 0.0722(19) Uani 1 1 d . . . H4 H 0.2261 0.2907 0.0982 0.087 Uiso 1 1 calc R . . C5 C 0.17807(18) 0.3080(7) 0.0531(3) 0.072(2) Uani 1 1 d . . . H5 H 0.1736 0.3861 0.0718 0.087 Uiso 1 1 calc R . . C6 C 0.29270(17) -0.1002(6) 0.0580(3) 0.0617(17) Uani 1 1 d . . . H6 H 0.2967 -0.1908 0.0491 0.074 Uiso 1 1 calc R . . C7 C 0.25983(15) -0.0552(7) 0.0445(3) 0.0638(17) Uani 1 1 d . . . H7 H 0.2422 -0.1146 0.0277 0.077 Uiso 1 1 calc R . . C8 C 0.25294(15) 0.0805(6) 0.0560(2) 0.0494(14) Uani 1 1 d . . . C9 C 0.28136(16) 0.1636(6) 0.0811(3) 0.0651(18) Uani 1 1 d . . . H9 H 0.2785 0.2557 0.0895 0.078 Uiso 1 1 calc R . . C10 C 0.31334(16) 0.1050(6) 0.0930(3) 0.0691(19) Uani 1 1 d . . . H10 H 0.3319 0.1608 0.1093 0.083 Uiso 1 1 calc R . . C11 C 0.06498(19) 0.0962(8) -0.0255(4) 0.099(3) Uani 1 1 d . . . H11 H 0.0811 0.0662 -0.0437 0.119 Uiso 1 1 calc R . . C12 C 0.03878(17) 0.0103(6) -0.0265(4) 0.087(3) Uani 1 1 d . . . H12 H 0.0369 -0.0726 -0.0459 0.105 Uiso 1 1 calc R . . C13 C 0.01564(16) 0.0452(6) 0.0006(3) 0.0618(18) Uani 1 1 d . . . C14 C 0.0210(2) 0.1629(9) 0.0305(5) 0.135(5) Uani 1 1 d . . . H14 H 0.0068 0.1863 0.0531 0.163 Uiso 1 1 calc R . . C15 C 0.0479(2) 0.2494(9) 0.0277(4) 0.128(4) Uani 1 1 d . . . H15 H 0.0504 0.3324 0.0471 0.154 Uiso 1 1 calc R . . C16 C 0.1093(2) 0.9020(8) 0.1035(3) 0.082(2) Uani 1 1 d . . . H16 H 0.0900 0.8546 0.0840 0.098 Uiso 1 1 calc R . . C17 C 0.10565(18) 0.9962(7) 0.1433(3) 0.072(2) Uani 1 1 d . . . H17 H 0.0845 1.0115 0.1501 0.086 Uiso 1 1 calc R . . C18 C 0.13428(18) 1.0678(6) 0.1731(3) 0.0586(16) Uani 1 1 d . . . C19 C 0.1643(2) 1.0420(8) 0.1598(3) 0.080(2) Uani 1 1 d . . . H19 H 0.1840 1.0899 0.1776 0.096 Uiso 1 1 calc R . . C20 C 0.1652(2) 0.9442(8) 0.1198(3) 0.083(2) Uani 1 1 d . . . H20 H 0.1861 0.9258 0.1123 0.100 Uiso 1 1 calc R . . C21 C 0.1046(2) 1.3046(8) 0.2719(3) 0.085(2) Uani 1 1 d . . . H21 H 0.0846 1.3484 0.2738 0.102 Uiso 1 1 calc R . . C22 C 0.10397(19) 1.2311(8) 0.2247(3) 0.089(2) Uani 1 1 d . . . H22 H 0.0842 1.2288 0.1956 0.106 Uiso 1 1 calc R . . C23 C 0.13302(18) 1.1589(7) 0.2197(3) 0.0641(17) Uani 1 1 d . . . C24 C 0.1609(2) 1.1751(11) 0.2636(4) 0.121(4) Uani 1 1 d . . . H24 H 0.1811 1.1298 0.2633 0.145 Uiso 1 1 calc R . . C25 C 0.1597(2) 1.2599(10) 0.3098(4) 0.114(3) Uani 1 1 d . . . H25 H 0.1798 1.2749 0.3375 0.136 Uiso 1 1 calc R . . C26 C 0.2219(2) 0.6333(7) 0.0866(3) 0.071(2) 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 Mo1 0.0444(3) 0.0389(3) 0.0715(4) -0.0064(2) 0.0214(3) -0.0010(2) Cu1 0.0495(4) 0.0424(4) 0.0715(5) -0.0016(4) 0.0229(4) -0.0068(3) Cu2 0.0667(5) 0.0551(5) 0.0610(5) -0.0118(4) 0.0197(4) -0.0119(4) Cu3 0.0559(5) 0.0534(4) 0.0527(5) 0.0023(3) 0.0169(4) -0.0055(3) S1 0.0753(11) 0.0505(9) 0.0699(11) -0.0062(8) 0.0389(9) -0.0104(8) S2 0.0700(11) 0.0384(8) 0.0695(11) 0.0004(7) 0.0215(9) -0.0066(7) S3 0.0526(9) 0.0458(8) 0.0606(10) -0.0059(7) 0.0137(8) -0.0081(7) S4 0.0708(13) 0.0958(15) 0.1133(18) 0.0027(13) 0.0017(12) -0.0030(11) O1 0.055(3) 0.070(3) 0.138(5) -0.015(3) 0.028(3) 0.014(2) N1 0.054(3) 0.039(3) 0.075(4) 0.008(3) 0.029(3) 0.004(2) N2 0.047(3) 0.045(3) 0.055(3) 0.001(2) 0.007(2) -0.006(2) N3 0.050(3) 0.037(3) 0.095(4) -0.009(3) 0.033(3) -0.003(2) N4 0.073(4) 0.056(3) 0.072(4) -0.007(3) 0.032(3) -0.009(3) N5 0.062(4) 0.067(3) 0.053(3) -0.013(3) 0.010(3) 0.009(3) N6 0.052(3) 0.077(4) 0.068(4) 0.003(3) 0.025(3) -0.004(3) C1 0.049(4) 0.055(4) 0.100(6) -0.020(4) 0.009(4) -0.015(3) C2 0.046(4) 0.057(4) 0.084(5) -0.013(4) 0.017(3) 0.000(3) C3 0.052(4) 0.045(3) 0.055(4) 0.003(3) 0.018(3) -0.003(3) C4 0.052(4) 0.061(4) 0.093(5) -0.016(4) 0.000(4) -0.002(3) C5 0.062(4) 0.058(4) 0.092(5) -0.020(4) 0.012(4) 0.003(3) C6 0.063(4) 0.054(4) 0.067(4) -0.008(3) 0.014(3) -0.008(3) C7 0.044(4) 0.064(4) 0.078(5) -0.004(4) 0.006(3) -0.010(3) C8 0.052(4) 0.041(3) 0.054(4) 0.004(3) 0.012(3) -0.001(3) C9 0.054(4) 0.048(3) 0.087(5) -0.002(3) 0.005(4) -0.006(3) C10 0.051(4) 0.051(4) 0.097(5) -0.013(4) 0.004(4) -0.022(3) C11 0.072(5) 0.079(5) 0.167(9) -0.042(6) 0.070(6) -0.006(4) C12 0.067(5) 0.045(4) 0.174(8) -0.037(4) 0.074(5) -0.022(3) C13 0.070(4) 0.030(3) 0.099(5) 0.008(3) 0.048(4) -0.006(3) C14 0.120(8) 0.095(6) 0.242(13) -0.079(7) 0.138(9) -0.061(6) C15 0.116(7) 0.083(6) 0.220(12) -0.075(7) 0.107(8) -0.053(5) C16 0.074(5) 0.096(6) 0.070(5) -0.021(4) 0.009(4) -0.005(4) C17 0.066(4) 0.073(5) 0.072(5) -0.033(4) 0.011(4) 0.000(4) C18 0.072(4) 0.054(4) 0.051(4) -0.001(3) 0.017(3) -0.003(3) C19 0.091(6) 0.086(5) 0.075(5) -0.042(4) 0.043(4) -0.038(4) C20 0.080(5) 0.083(5) 0.104(6) -0.036(5) 0.057(5) -0.031(4) C21 0.074(5) 0.097(6) 0.079(5) -0.018(5) 0.013(4) 0.037(4) C22 0.077(5) 0.108(6) 0.062(5) -0.031(4) -0.014(4) 0.017(5) C23 0.066(4) 0.065(4) 0.061(4) -0.013(3) 0.016(4) -0.001(3) C24 0.067(5) 0.196(10) 0.092(6) -0.068(7) 0.005(5) 0.043(6) C25 0.063(5) 0.173(9) 0.096(6) -0.073(6) 0.004(4) 0.022(5) C26 0.082(5) 0.075(5) 0.055(4) 0.001(4) 0.015(4) -0.022(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 Mo1 O1 1.710(4) . ? Mo1 S1 2.2618(19) . ? Mo1 S2 2.2632(16) . ? Mo1 S3 2.2730(16) . ? Mo1 Cu3 2.6726(11) . ? Mo1 Cu1 2.6834(10) . ? Mo1 Cu2 2.7020(13) . ? Cu1 N1 2.048(5) . ? Cu1 N3 2.085(4) . ? Cu1 S3 2.2811(18) . ? Cu1 S1 2.2842(18) . ? Cu2 N6 2.009(6) . ? Cu2 N4 2.135(5) . ? Cu2 S2 2.277(2) . ? Cu2 S1 2.2958(17) . ? Cu3 N5 2.043(5) 6_575 ? Cu3 N2 2.107(5) 7 ? Cu3 S3 2.2599(16) . ? Cu3 S2 2.2875(17) . ? S4 C26 1.628(9) . ? N1 C1 1.318(7) . ? N1 C5 1.342(8) . ? N2 C10 1.317(7) . ? N2 C6 1.324(7) . ? N2 Cu3 2.107(5) 7 ? N3 C11 1.322(8) . ? N3 C15 1.328(8) . ? N4 C16 1.311(8) . ? N4 C20 1.324(8) . ? N5 C21 1.316(8) . ? N5 C25 1.325(8) . ? N5 Cu3 2.043(5) 6_576 ? N6 C26 1.138(8) . ? C1 C2 1.377(8) . ? C1 H1 0.9300 . ? C2 C3 1.382(8) . ? C2 H2 0.9300 . ? C3 C4 1.395(8) . ? C3 C8 1.471(8) . ? C4 C5 1.356(9) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.361(8) . ? C6 H6 0.9300 . ? C7 C8 1.390(8) . ? C7 H7 0.9300 . ? C8 C9 1.414(8) . ? C9 C10 1.377(8) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.346(9) . ? C11 H11 0.9300 . ? C12 C13 1.331(8) . ? C12 H12 0.9300 . ? C13 C14 1.348(9) . ? C13 C13 1.537(11) 5 ? C14 C15 1.393(9) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.379(9) . ? C16 H16 0.9300 . ? C17 C18 1.391(8) . ? C17 H17 0.9300 . ? C18 C19 1.367(9) . ? C18 C23 1.463(8) . ? C19 C20 1.379(9) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.364(9) . ? C21 H21 0.9300 . ? C22 C23 1.404(9) . ? C22 H22 0.9300 . ? C23 C24 1.362(10) . ? C24 C25 1.420(10) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? 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 O1 Mo1 S1 110.7(2) . . ? O1 Mo1 S2 111.09(17) . . ? S1 Mo1 S2 107.93(7) . . ? O1 Mo1 S3 110.84(17) . . ? S1 Mo1 S3 108.16(6) . . ? S2 Mo1 S3 108.05(6) . . ? O1 Mo1 Cu3 129.56(19) . . ? S1 Mo1 Cu3 119.78(5) . . ? S2 Mo1 Cu3 54.46(5) . . ? S3 Mo1 Cu3 53.65(4) . . ? O1 Mo1 Cu1 124.53(16) . . ? S1 Mo1 Cu1 54.21(4) . . ? S2 Mo1 Cu1 124.38(5) . . ? S3 Mo1 Cu1 54.04(5) . . ? Cu3 Mo1 Cu1 87.17(3) . . ? O1 Mo1 Cu2 126.95(17) . . ? S1 Mo1 Cu2 54.22(5) . . ? S2 Mo1 Cu2 53.71(5) . . ? S3 Mo1 Cu2 122.22(5) . . ? Cu3 Mo1 Cu2 85.95(3) . . ? Cu1 Mo1 Cu2 89.43(3) . . ? N1 Cu1 N3 105.94(18) . . ? N1 Cu1 S3 116.14(15) . . ? N3 Cu1 S3 108.51(16) . . ? N1 Cu1 S1 110.46(16) . . ? N3 Cu1 S1 108.46(14) . . ? S3 Cu1 S1 107.11(6) . . ? N1 Cu1 Mo1 134.23(13) . . ? N3 Cu1 Mo1 119.70(13) . . ? S3 Cu1 Mo1 53.76(4) . . ? S1 Cu1 Mo1 53.44(5) . . ? N6 Cu2 N4 99.7(2) . . ? N6 Cu2 S2 118.60(16) . . ? N4 Cu2 S2 106.88(16) . . ? N6 Cu2 S1 117.93(17) . . ? N4 Cu2 S1 106.01(15) . . ? S2 Cu2 S1 106.30(7) . . ? N6 Cu2 Mo1 142.47(16) . . ? N4 Cu2 Mo1 117.84(16) . . ? S2 Cu2 Mo1 53.24(5) . . ? S1 Cu2 Mo1 53.06(5) . . ? N5 Cu3 N2 99.8(2) 6_575 7 ? N5 Cu3 S3 120.94(16) 6_575 . ? N2 Cu3 S3 110.64(13) 7 . ? N5 Cu3 S2 108.27(16) 6_575 . ? N2 Cu3 S2 108.91(14) 7 . ? S3 Cu3 S2 107.66(6) . . ? N5 Cu3 Mo1 136.48(16) 6_575 . ? N2 Cu3 Mo1 122.94(13) 7 . ? S3 Cu3 Mo1 54.10(4) . . ? S2 Cu3 Mo1 53.61(4) . . ? Mo1 S1 Cu1 72.35(6) . . ? Mo1 S1 Cu2 72.72(6) . . ? Cu1 S1 Cu2 111.65(7) . . ? Mo1 S2 Cu2 73.05(6) . . ? Mo1 S2 Cu3 71.93(5) . . ? Cu2 S2 Cu3 106.78(7) . . ? Cu3 S3 Mo1 72.25(5) . . ? Cu3 S3 Cu1 108.81(7) . . ? Mo1 S3 Cu1 72.21(5) . . ? C1 N1 C5 115.7(5) . . ? C1 N1 Cu1 125.3(5) . . ? C5 N1 Cu1 118.9(4) . . ? C10 N2 C6 116.5(5) . . ? C10 N2 Cu3 120.7(4) . 7 ? C6 N2 Cu3 122.8(4) . 7 ? C11 N3 C15 113.2(6) . . ? C11 N3 Cu1 125.2(4) . . ? C15 N3 Cu1 121.5(4) . . ? C16 N4 C20 116.2(6) . . ? C16 N4 Cu2 123.8(5) . . ? C20 N4 Cu2 119.4(5) . . ? C21 N5 C25 115.6(6) . . ? C21 N5 Cu3 126.0(5) . 6_576 ? C25 N5 Cu3 117.7(5) . 6_576 ? C26 N6 Cu2 169.7(6) . . ? N1 C1 C2 124.9(6) . . ? N1 C1 H1 117.6 . . ? C2 C1 H1 117.6 . . ? C1 C2 C3 119.4(6) . . ? C1 C2 H2 120.3 . . ? C3 C2 H2 120.3 . . ? C2 C3 C4 115.5(6) . . ? C2 C3 C8 123.3(5) . . ? C4 C3 C8 121.0(5) . . ? C5 C4 C3 120.9(6) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? N1 C5 C4 123.4(6) . . ? N1 C5 H5 118.3 . . ? C4 C5 H5 118.3 . . ? N2 C6 C7 124.8(6) . . ? N2 C6 H6 117.6 . . ? C7 C6 H6 117.6 . . ? C6 C7 C8 119.3(6) . . ? C6 C7 H7 120.3 . . ? C8 C7 H7 120.3 . . ? C7 C8 C9 116.5(6) . . ? C7 C8 C3 122.6(5) . . ? C9 C8 C3 120.8(5) . . ? C10 C9 C8 118.4(6) . . ? C10 C9 H9 120.8 . . ? C8 C9 H9 120.8 . . ? N2 C10 C9 124.5(6) . . ? N2 C10 H10 117.8 . . ? C9 C10 H10 117.8 . . ? N3 C11 C12 126.8(6) . . ? N3 C11 H11 116.6 . . ? C12 C11 H11 116.6 . . ? C13 C12 C11 119.4(6) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C12 C13 C14 117.2(6) . . ? C12 C13 C13 122.2(7) . 5 ? C14 C13 C13 120.6(7) . 5 ? C13 C14 C15 120.1(7) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? N3 C15 C14 123.0(7) . . ? N3 C15 H15 118.5 . . ? C14 C15 H15 118.5 . . ? N4 C16 C17 124.4(7) . . ? N4 C16 H16 117.8 . . ? C17 C16 H16 117.8 . . ? C16 C17 C18 118.7(7) . . ? C16 C17 H17 120.6 . . ? C18 C17 H17 120.6 . . ? C19 C18 C17 117.2(6) . . ? C19 C18 C23 121.0(6) . . ? C17 C18 C23 121.7(6) . . ? C18 C19 C20 119.2(6) . . ? C18 C19 H19 120.4 . . ? C20 C19 H19 120.4 . . ? N4 C20 C19 124.2(7) . . ? N4 C20 H20 117.9 . . ? C19 C20 H20 117.9 . . ? N5 C21 C22 125.4(6) . . ? N5 C21 H21 117.3 . . ? C22 C21 H21 117.3 . . ? C21 C22 C23 120.3(6) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C24 C23 C22 114.6(6) . . ? C24 C23 C18 120.5(6) . . ? C22 C23 C18 124.8(6) . . ? C23 C24 C25 121.1(7) . . ? C23 C24 H24 119.5 . . ? C25 C24 H24 119.5 . . ? N5 C25 C24 122.6(7) . . ? N5 C25 H25 118.7 . . ? C24 C25 H25 118.7 . . ? N6 C26 S4 178.3(7) . . ? 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 O1 Mo1 Cu1 N1 -175.2(3) . . . . ? S1 Mo1 Cu1 N1 -83.4(2) . . . . ? S2 Mo1 Cu1 N1 4.7(2) . . . . ? S3 Mo1 Cu1 N1 92.8(2) . . . . ? Cu3 Mo1 Cu1 N1 47.0(2) . . . . ? Cu2 Mo1 Cu1 N1 -39.0(2) . . . . ? O1 Mo1 Cu1 N3 -0.1(3) . . . . ? S1 Mo1 Cu1 N3 91.76(19) . . . . ? S2 Mo1 Cu1 N3 179.85(18) . . . . ? S3 Mo1 Cu1 N3 -92.02(19) . . . . ? Cu3 Mo1 Cu1 N3 -137.80(18) . . . . ? Cu2 Mo1 Cu1 N3 136.23(18) . . . . ? O1 Mo1 Cu1 S3 92.0(2) . . . . ? S1 Mo1 Cu1 S3 -176.22(7) . . . . ? S2 Mo1 Cu1 S3 -88.14(8) . . . . ? Cu3 Mo1 Cu1 S3 -45.78(5) . . . . ? Cu2 Mo1 Cu1 S3 -131.75(6) . . . . ? O1 Mo1 Cu1 S1 -91.8(2) . . . . ? S2 Mo1 Cu1 S1 88.08(8) . . . . ? S3 Mo1 Cu1 S1 176.22(7) . . . . ? Cu3 Mo1 Cu1 S1 130.44(6) . . . . ? Cu2 Mo1 Cu1 S1 44.47(6) . . . . ? O1 Mo1 Cu2 N6 179.2(3) . . . . ? S1 Mo1 Cu2 N6 89.0(3) . . . . ? S2 Mo1 Cu2 N6 -90.5(3) . . . . ? S3 Mo1 Cu2 N6 -1.0(3) . . . . ? Cu3 Mo1 Cu2 N6 -42.6(3) . . . . ? Cu1 Mo1 Cu2 N6 44.6(3) . . . . ? O1 Mo1 Cu2 N4 0.5(3) . . . . ? S1 Mo1 Cu2 N4 -89.61(17) . . . . ? S2 Mo1 Cu2 N4 90.88(17) . . . . ? S3 Mo1 Cu2 N4 -179.60(16) . . . . ? Cu3 Mo1 Cu2 N4 138.73(16) . . . . ? Cu1 Mo1 Cu2 N4 -134.06(16) . . . . ? O1 Mo1 Cu2 S2 -90.4(2) . . . . ? S1 Mo1 Cu2 S2 179.52(7) . . . . ? S3 Mo1 Cu2 S2 89.52(7) . . . . ? Cu3 Mo1 Cu2 S2 47.85(5) . . . . ? Cu1 Mo1 Cu2 S2 135.06(6) . . . . ? O1 Mo1 Cu2 S1 90.1(2) . . . . ? S2 Mo1 Cu2 S1 -179.52(7) . . . . ? S3 Mo1 Cu2 S1 -90.00(7) . . . . ? Cu3 Mo1 Cu2 S1 -131.66(6) . . . . ? Cu1 Mo1 Cu2 S1 -44.46(5) . . . . ? O1 Mo1 Cu3 N5 11.2(3) . . . 6_575 ? S1 Mo1 Cu3 N5 -169.4(2) . . . 6_575 ? S2 Mo1 Cu3 N5 -77.9(2) . . . 6_575 ? S3 Mo1 Cu3 N5 99.2(2) . . . 6_575 ? Cu1 Mo1 Cu3 N5 145.3(2) . . . 6_575 ? Cu2 Mo1 Cu3 N5 -125.1(2) . . . 6_575 ? O1 Mo1 Cu3 N2 179.2(3) . . . 7 ? S1 Mo1 Cu3 N2 -1.41(16) . . . 7 ? S2 Mo1 Cu3 N2 90.14(16) . . . 7 ? S3 Mo1 Cu3 N2 -92.83(16) . . . 7 ? Cu1 Mo1 Cu3 N2 -46.76(15) . . . 7 ? Cu2 Mo1 Cu3 N2 42.88(15) . . . 7 ? O1 Mo1 Cu3 S3 -88.0(2) . . . . ? S1 Mo1 Cu3 S3 91.42(7) . . . . ? S2 Mo1 Cu3 S3 -177.03(8) . . . . ? Cu1 Mo1 Cu3 S3 46.07(6) . . . . ? Cu2 Mo1 Cu3 S3 135.71(6) . . . . ? O1 Mo1 Cu3 S2 89.1(2) . . . . ? S1 Mo1 Cu3 S2 -91.55(8) . . . . ? S3 Mo1 Cu3 S2 177.03(8) . . . . ? Cu1 Mo1 Cu3 S2 -136.89(6) . . . . ? Cu2 Mo1 Cu3 S2 -47.26(6) . . . . ? O1 Mo1 S1 Cu1 118.36(17) . . . . ? S2 Mo1 S1 Cu1 -119.89(6) . . . . ? S3 Mo1 S1 Cu1 -3.22(6) . . . . ? Cu3 Mo1 S1 Cu1 -61.14(6) . . . . ? Cu2 Mo1 S1 Cu1 -120.30(6) . . . . ? O1 Mo1 S1 Cu2 -121.34(17) . . . . ? S2 Mo1 S1 Cu2 0.41(6) . . . . ? S3 Mo1 S1 Cu2 117.08(6) . . . . ? Cu3 Mo1 S1 Cu2 59.16(6) . . . . ? Cu1 Mo1 S1 Cu2 120.30(6) . . . . ? N1 Cu1 S1 Mo1 130.56(14) . . . . ? N3 Cu1 S1 Mo1 -113.75(16) . . . . ? S3 Cu1 S1 Mo1 3.19(6) . . . . ? N1 Cu1 S1 Cu2 68.06(16) . . . . ? N3 Cu1 S1 Cu2 -176.25(16) . . . . ? S3 Cu1 S1 Cu2 -59.31(10) . . . . ? Mo1 Cu1 S1 Cu2 -62.50(7) . . . . ? N6 Cu2 S1 Mo1 -136.42(18) . . . . ? N4 Cu2 S1 Mo1 113.09(17) . . . . ? S2 Cu2 S1 Mo1 -0.40(6) . . . . ? N6 Cu2 S1 Cu1 -74.1(2) . . . . ? N4 Cu2 S1 Cu1 175.37(18) . . . . ? S2 Cu2 S1 Cu1 61.88(9) . . . . ? Mo1 Cu2 S1 Cu1 62.28(7) . . . . ? O1 Mo1 S2 Cu2 121.1(2) . . . . ? S1 Mo1 S2 Cu2 -0.41(6) . . . . ? S3 Mo1 S2 Cu2 -117.15(6) . . . . ? Cu3 Mo1 S2 Cu2 -114.64(6) . . . . ? Cu1 Mo1 S2 Cu2 -58.85(6) . . . . ? O1 Mo1 S2 Cu3 -124.3(2) . . . . ? S1 Mo1 S2 Cu3 114.23(6) . . . . ? S3 Mo1 S2 Cu3 -2.51(7) . . . . ? Cu1 Mo1 S2 Cu3 55.79(7) . . . . ? Cu2 Mo1 S2 Cu3 114.64(6) . . . . ? N6 Cu2 S2 Mo1 136.07(19) . . . . ? N4 Cu2 S2 Mo1 -112.49(16) . . . . ? S1 Cu2 S2 Mo1 0.40(6) . . . . ? N6 Cu2 S2 Cu3 71.6(2) . . . . ? N4 Cu2 S2 Cu3 -176.99(16) . . . . ? S1 Cu2 S2 Cu3 -64.09(8) . . . . ? Mo1 Cu2 S2 Cu3 -64.49(5) . . . . ? N5 Cu3 S2 Mo1 134.85(16) 6_575 . . . ? N2 Cu3 S2 Mo1 -117.48(14) 7 . . . ? S3 Cu3 S2 Mo1 2.52(7) . . . . ? N5 Cu3 S2 Cu2 -159.90(17) 6_575 . . . ? N2 Cu3 S2 Cu2 -52.24(15) 7 . . . ? S3 Cu3 S2 Cu2 67.77(9) . . . . ? Mo1 Cu3 S2 Cu2 65.25(6) . . . . ? N5 Cu3 S3 Mo1 -127.57(19) 6_575 . . . ? N2 Cu3 S3 Mo1 116.40(15) 7 . . . ? S2 Cu3 S3 Mo1 -2.51(7) . . . . ? N5 Cu3 S3 Cu1 169.04(18) 6_575 . . . ? N2 Cu3 S3 Cu1 53.02(16) 7 . . . ? S2 Cu3 S3 Cu1 -65.89(8) . . . . ? Mo1 Cu3 S3 Cu1 -63.38(6) . . . . ? O1 Mo1 S3 Cu3 124.5(2) . . . . ? S1 Mo1 S3 Cu3 -114.05(6) . . . . ? S2 Mo1 S3 Cu3 2.54(7) . . . . ? Cu1 Mo1 S3 Cu3 -117.28(6) . . . . ? Cu2 Mo1 S3 Cu3 -55.42(6) . . . . ? O1 Mo1 S3 Cu1 -118.2(2) . . . . ? S1 Mo1 S3 Cu1 3.23(6) . . . . ? S2 Mo1 S3 Cu1 119.82(6) . . . . ? Cu3 Mo1 S3 Cu1 117.28(6) . . . . ? Cu2 Mo1 S3 Cu1 61.86(6) . . . . ? N1 Cu1 S3 Cu3 -63.72(17) . . . . ? N3 Cu1 S3 Cu3 177.14(14) . . . . ? S1 Cu1 S3 Cu3 60.24(8) . . . . ? Mo1 Cu1 S3 Cu3 63.42(5) . . . . ? N1 Cu1 S3 Mo1 -127.13(16) . . . . ? N3 Cu1 S3 Mo1 113.72(14) . . . . ? S1 Cu1 S3 Mo1 -3.18(6) . . . . ? N3 Cu1 N1 C1 59.5(5) . . . . ? S3 Cu1 N1 C1 -61.1(5) . . . . ? S1 Cu1 N1 C1 176.7(5) . . . . ? Mo1 Cu1 N1 C1 -124.9(5) . . . . ? N3 Cu1 N1 C5 -123.7(5) . . . . ? S3 Cu1 N1 C5 115.8(5) . . . . ? S1 Cu1 N1 C5 -6.4(5) . . . . ? Mo1 Cu1 N1 C5 52.0(6) . . . . ? N1 Cu1 N3 C11 -55.3(7) . . . . ? S3 Cu1 N3 C11 70.1(7) . . . . ? S1 Cu1 N3 C11 -173.9(6) . . . . ? Mo1 Cu1 N3 C11 128.3(6) . . . . ? N1 Cu1 N3 C15 128.4(7) . . . . ? S3 Cu1 N3 C15 -106.2(7) . . . . ? S1 Cu1 N3 C15 9.8(7) . . . . ? Mo1 Cu1 N3 C15 -48.0(8) . . . . ? N6 Cu2 N4 C16 -152.6(6) . . . . ? S2 Cu2 N4 C16 83.4(6) . . . . ? S1 Cu2 N4 C16 -29.7(6) . . . . ? Mo1 Cu2 N4 C16 26.5(6) . . . . ? N6 Cu2 N4 C20 17.9(6) . . . . ? S2 Cu2 N4 C20 -106.1(6) . . . . ? S1 Cu2 N4 C20 140.8(5) . . . . ? Mo1 Cu2 N4 C20 -162.9(5) . . . . ? N4 Cu2 N6 C26 136(3) . . . . ? S2 Cu2 N6 C26 -108(3) . . . . ? S1 Cu2 N6 C26 22(3) . . . . ? Mo1 Cu2 N6 C26 -43(3) . . . . ? C5 N1 C1 C2 -3.2(10) . . . . ? Cu1 N1 C1 C2 173.7(5) . . . . ? N1 C1 C2 C3 0.3(11) . . . . ? C1 C2 C3 C4 4.1(9) . . . . ? C1 C2 C3 C8 -179.8(6) . . . . ? C2 C3 C4 C5 -5.5(10) . . . . ? C8 C3 C4 C5 178.3(6) . . . . ? C1 N1 C5 C4 1.7(10) . . . . ? Cu1 N1 C5 C4 -175.4(6) . . . . ? C3 C4 C5 N1 2.7(11) . . . . ? C10 N2 C6 C7 -2.9(10) . . . . ? Cu3 N2 C6 C7 175.3(5) 7 . . . ? N2 C6 C7 C8 1.5(10) . . . . ? C6 C7 C8 C9 0.5(9) . . . . ? C6 C7 C8 C3 177.3(6) . . . . ? C2 C3 C8 C7 -19.4(9) . . . . ? C4 C3 C8 C7 156.5(6) . . . . ? C2 C3 C8 C9 157.3(6) . . . . ? C4 C3 C8 C9 -26.8(9) . . . . ? C7 C8 C9 C10 -0.8(9) . . . . ? C3 C8 C9 C10 -177.7(6) . . . . ? C6 N2 C10 C9 2.4(10) . . . . ? Cu3 N2 C10 C9 -175.8(5) 7 . . . ? C8 C9 C10 N2 -0.6(11) . . . . ? C15 N3 C11 C12 5.6(14) . . . . ? Cu1 N3 C11 C12 -171.0(8) . . . . ? N3 C11 C12 C13 -2.6(15) . . . . ? C11 C12 C13 C14 -3.8(14) . . . . ? C11 C12 C13 C13 177.6(9) . . . 5 ? C12 C13 C14 C15 6.6(16) . . . . ? C13 C13 C14 C15 -174.9(10) 5 . . . ? C11 N3 C15 C14 -2.5(15) . . . . ? Cu1 N3 C15 C14 174.3(9) . . . . ? C13 C14 C15 N3 -3.5(18) . . . . ? C20 N4 C16 C17 0.1(11) . . . . ? Cu2 N4 C16 C17 170.9(6) . . . . ? N4 C16 C17 C18 -0.3(12) . . . . ? C16 C17 C18 C19 1.5(10) . . . . ? C16 C17 C18 C23 -173.8(7) . . . . ? C17 C18 C19 C20 -2.4(11) . . . . ? C23 C18 C19 C20 173.0(7) . . . . ? C16 N4 C20 C19 -1.1(12) . . . . ? Cu2 N4 C20 C19 -172.3(6) . . . . ? C18 C19 C20 N4 2.3(13) . . . . ? C25 N5 C21 C22 2.9(13) . . . . ? Cu3 N5 C21 C22 -167.3(6) 6_576 . . . ? N5 C21 C22 C23 1.9(14) . . . . ? C21 C22 C23 C24 -3.0(12) . . . . ? C21 C22 C23 C18 174.6(7) . . . . ? C19 C18 C23 C24 -27.0(11) . . . . ? C17 C18 C23 C24 148.2(8) . . . . ? C19 C18 C23 C22 155.6(8) . . . . ? C17 C18 C23 C22 -29.2(11) . . . . ? C22 C23 C24 C25 -0.5(14) . . . . ? C18 C23 C24 C25 -178.1(9) . . . . ? C21 N5 C25 C24 -6.5(14) . . . . ? Cu3 N5 C25 C24 164.5(8) 6_576 . . . ? C23 C24 C25 N5 5.5(17) . . . . ? Cu2 N6 C26 S4 178(100) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.444 _refine_diff_density_min -0.374 _refine_diff_density_rms 0.090 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.014 -0.349 0.118 4181.4 1822.3 _platon_squeeze_details ; ? ; # Attachment '- cif 3.cif' data_zzuli20110113c _database_code_depnum_ccdc_archive 'CCDC 845165' #TrackingRef '- cif 3.cif' _audit_creation_date 2011-03-20 _audit_creation_method ; Olex2 1.1 (compiled 2011.02.15 svn.r1672, GUI svn.r3494) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety '2(C25 H20 Br Cu3 Mo N5 O S3), 4(C3 H7 N O), 2(C1.5 N0.5 O0.5)' _chemical_formula_sum 'C65 H68 Br2 Cu6 Mo2 N15 O7 S6' _chemical_formula_weight 2096.64 _chemical_melting_point ? _chemical_oxdiff_formula 'Cu C H O N Mo Br' _chemical_oxdiff_usercomment NYY-12.001 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' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_H-M_alt 'C 1 2/c 1' _space_group_name_Hall '-C 2yc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y, -z+1/2' 3 'x+1/2, y+1/2, z' 4 '-x+1/2, y+1/2, -z+1/2' 5 '-x, -y, -z' 6 'x, -y, z-1/2' 7 '-x+1/2, -y+1/2, -z' 8 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.263(2) _cell_length_b 21.2870(18) _cell_length_c 18.0287(17) _cell_angle_alpha 90.00 _cell_angle_beta 96.213(10) _cell_angle_gamma 90.00 _cell_volume 8112.2(13) _cell_formula_units_Z 4 _cell_measurement_reflns_used 6228 _cell_measurement_temperature 291.15 _cell_measurement_theta_max 26.3122 _cell_measurement_theta_min 2.9655 _exptl_absorpt_coefficient_mu 3.037 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.63007 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.717 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 4172 _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.21 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0588 _diffrn_reflns_av_unetI/netI 0.0653 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 28647 _diffrn_reflns_theta_full 26.37 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_min 2.97 _diffrn_ambient_temperature 291.15 _diffrn_detector_area_resol_mean 16.2542 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -50.00 44.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 18.4204 -37.0000 60.0000 94 #__ type_ start__ end____ width___ exp.time_ 2 omega -6.00 90.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 18.4204 37.0000 -120.0000 96 #__ type_ start__ end____ width___ exp.time_ 3 omega -10.00 88.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 18.4204 77.0000 -30.0000 98 #__ type_ start__ end____ width___ exp.time_ 4 omega -85.00 -59.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - -19.0454 142.0000 122.0000 26 #__ type_ start__ end____ width___ exp.time_ 5 omega -82.00 -56.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - -19.0454 -77.0000 -60.0000 26 #__ type_ start__ end____ width___ exp.time_ 6 omega -17.00 8.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - -19.0454 -77.0000 -60.0000 25 #__ type_ start__ end____ width___ exp.time_ 7 omega -46.00 -18.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - -19.0454 77.0000 60.0000 28 ; _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0013928000 _diffrn_orient_matrix_UB_12 0.0028041000 _diffrn_orient_matrix_UB_13 0.0389327000 _diffrn_orient_matrix_UB_21 -0.0015663000 _diffrn_orient_matrix_UB_22 -0.0331578000 _diffrn_orient_matrix_UB_23 0.0030843000 _diffrn_orient_matrix_UB_31 0.0334859000 _diffrn_orient_matrix_UB_32 -0.0014496000 _diffrn_orient_matrix_UB_33 0.0062336000 _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_source 'Enhance (Mo) X-ray Source' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 5500 _reflns_number_total 8279 _reflns_odcompleteness_completeness 99.79 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'A short history of SHELX (Sheldrick, 2007)' _refine_diff_density_max 0.943 _refine_diff_density_min -0.595 _refine_diff_density_rms 0.109 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 435 _refine_ls_number_reflns 8279 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0895 _refine_ls_R_factor_gt 0.0502 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0715P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1197 _refine_ls_wR_factor_ref 0.1412 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.28600(2) 0.51890(2) 0.50471(2) 0.03621(14) Uani 1 1 d . . . Br1 Br 0.11849(3) 0.36440(3) 0.43013(4) 0.0606(2) Uani 1 1 d . . . Cu1 Cu 0.26256(3) 0.54561(3) 0.35905(4) 0.04187(19) Uani 1 1 d . . . Cu2 Cu 0.18244(3) 0.58808(3) 0.52769(4) 0.04132(19) Uani 1 1 d . . . Cu3 Cu 0.21503(3) 0.41305(3) 0.48751(4) 0.0451(2) Uani 1 1 d . . . S1 S 0.28450(7) 0.44841(7) 0.41019(8) 0.0449(4) Uani 1 1 d . . . S2 S 0.25978(7) 0.61510(6) 0.45492(8) 0.0424(3) Uani 1 1 d . . . S3 S 0.21006(7) 0.49048(6) 0.57581(8) 0.0416(3) Uani 1 1 d . . . O1 O 0.35803(18) 0.5206(2) 0.5554(2) 0.0589(12) Uani 1 1 d . . . O2 O 0.5593(5) 0.2862(4) 0.5070(6) 0.170(4) Uani 1 1 d . . . O3 O 0.4256(9) 0.7302(9) 0.8102(13) 0.339(9) Uiso 1 1 d . . . O4 O 0.4854(11) 0.2911(12) 0.6988(13) 0.235(10) Uiso 0.50 1 d P . . N1 N 0.1882(2) 0.5534(2) 0.2803(3) 0.0426(11) Uani 1 1 d . . . N2 N -0.0926(2) 0.5848(2) 0.0288(3) 0.0461(12) Uani 1 1 d . . . N3 N 0.3473(2) 0.5590(2) 0.3100(3) 0.0446(11) Uani 1 1 d . . . N4 N 0.1811(2) 0.6472(2) 0.6197(3) 0.0445(11) Uani 1 1 d . . . N5 N 0.2428(2) 0.8390(2) 0.9399(2) 0.0453(11) Uani 1 1 d . . . N6 N 0.4812(4) 0.3567(5) 0.4709(5) 0.118(3) Uani 1 1 d . . . N7 N 0.3789(6) 0.7011(7) 0.6962(8) 0.171(4) Uiso 1 1 d . . . N8 N 0.5000 0.2108(6) 0.7500 0.106(3) Uiso 1 2 d S . . C1 C 0.1407(3) 0.5120(3) 0.2760(3) 0.0530(16) Uani 1 1 d . . . H1 H 0.1446 0.4777 0.3080 0.064 Uiso 1 1 calc R . . C2 C 0.0865(3) 0.5167(3) 0.2275(4) 0.0534(16) Uani 1 1 d . . . H2 H 0.0553 0.4861 0.2275 0.064 Uiso 1 1 calc R . . C3 C 0.0783(2) 0.5667(3) 0.1787(3) 0.0405(13) Uani 1 1 d . . . C4 C 0.1276(2) 0.6102(3) 0.1809(3) 0.0446(14) Uani 1 1 d . . . H4 H 0.1252 0.6443 0.1485 0.054 Uiso 1 1 calc R . . C5 C 0.1801(2) 0.6015(3) 0.2322(3) 0.0479(15) Uani 1 1 d . . . H5 H 0.2123 0.6312 0.2334 0.058 Uiso 1 1 calc R . . C6 C -0.0696(3) 0.5293(3) 0.0510(4) 0.0578(18) Uani 1 1 d . . . H6 H -0.0918 0.4935 0.0340 0.069 Uiso 1 1 calc R . . C7 C -0.0142(3) 0.5216(3) 0.0982(4) 0.0586(18) Uani 1 1 d . . . H7 H -0.0002 0.4814 0.1120 0.070 Uiso 1 1 calc R . . C8 C 0.0202(3) 0.5733(3) 0.1247(3) 0.0444(14) Uani 1 1 d . . . C9 C -0.0027(3) 0.6304(3) 0.0990(4) 0.070(2) Uani 1 1 d . . . H9 H 0.0196 0.6668 0.1131 0.084 Uiso 1 1 calc R . . C10 C -0.0581(3) 0.6343(3) 0.0528(4) 0.071(2) Uani 1 1 d . . . H10 H -0.0725 0.6740 0.0373 0.085 Uiso 1 1 calc R . . C11 C 0.3564(2) 0.5362(3) 0.2427(3) 0.0450(14) Uani 1 1 d . . . H11 H 0.3219 0.5212 0.2118 0.054 Uiso 1 1 calc R . . C12 C 0.4157(2) 0.5344(3) 0.2180(3) 0.0466(14) Uani 1 1 d . . . H12 H 0.4202 0.5187 0.1707 0.056 Uiso 1 1 calc R . . C13 C 0.4679(2) 0.5555(3) 0.2624(3) 0.0400(13) Uani 1 1 d . . . C14 C 0.4584(3) 0.5774(3) 0.3326(3) 0.0542(17) Uani 1 1 d . . . H14 H 0.4925 0.5905 0.3656 0.065 Uiso 1 1 calc R . . C15 C 0.3979(3) 0.5795(3) 0.3530(3) 0.0578(17) Uani 1 1 d . . . H15 H 0.3921 0.5962 0.3995 0.069 Uiso 1 1 calc R . . C16 C 0.1713(3) 0.7089(3) 0.6164(3) 0.0599(18) Uani 1 1 d . . . H16 H 0.1583 0.7271 0.5703 0.072 Uiso 1 1 calc R . . C17 C 0.1797(3) 0.7472(3) 0.6792(4) 0.0606(17) Uani 1 1 d . . . H17 H 0.1743 0.7904 0.6741 0.073 Uiso 1 1 calc R . . C18 C 0.1959(3) 0.7220(3) 0.7487(3) 0.0456(14) Uani 1 1 d . . . C19 C 0.2036(3) 0.6565(3) 0.7515(3) 0.0626(19) Uani 1 1 d . . . H19 H 0.2137 0.6365 0.7971 0.075 Uiso 1 1 calc R . . C20 C 0.1962(3) 0.6225(3) 0.6874(3) 0.0581(17) Uani 1 1 d . . . H20 H 0.2020 0.5793 0.6908 0.070 Uiso 1 1 calc R . . C21 C 0.1923(3) 0.8508(3) 0.8911(3) 0.0518(15) Uani 1 1 d . . . H21 H 0.1681 0.8861 0.8990 0.062 Uiso 1 1 calc R . . C22 C 0.1737(3) 0.8134(3) 0.8288(4) 0.0531(16) Uani 1 1 d . . . H22 H 0.1382 0.8236 0.7962 0.064 Uiso 1 1 calc R . . C23 C 0.2094(3) 0.7610(2) 0.8171(3) 0.0404(13) Uani 1 1 d . . . C24 C 0.2607(3) 0.7475(3) 0.8690(3) 0.0553(16) Uani 1 1 d . . . H24 H 0.2848 0.7117 0.8638 0.066 Uiso 1 1 calc R . . C25 C 0.2757(3) 0.7876(3) 0.9285(3) 0.0531(16) Uani 1 1 d . . . H25 H 0.3107 0.7782 0.9623 0.064 Uiso 1 1 calc R . . C26 C 0.5418(8) 0.3378(7) 0.4835(7) 0.150(5) Uani 1 1 d . . . H26 H 0.5729 0.3664 0.4734 0.180 Uiso 1 1 calc R . . C27 C 0.4283(7) 0.3225(8) 0.4759(10) 0.214(8) Uani 1 1 d . . . H27A H 0.4103 0.3107 0.4267 0.321 Uiso 1 1 calc R . . H27B H 0.3983 0.3472 0.4994 0.321 Uiso 1 1 calc R . . H27C H 0.4388 0.2855 0.5049 0.321 Uiso 1 1 calc R . . C28 C 0.4729(7) 0.4197(7) 0.4443(10) 0.191(7) Uani 1 1 d . . . H28A H 0.5134 0.4375 0.4376 0.286 Uiso 1 1 calc R . . H28B H 0.4531 0.4443 0.4800 0.286 Uiso 1 1 calc R . . H28C H 0.4466 0.4197 0.3975 0.286 Uiso 1 1 calc R . . C29 C 0.3830(9) 0.6367(11) 0.7153(12) 0.268(10) Uiso 1 1 d . . . H29A H 0.3608 0.6292 0.7581 0.401 Uiso 1 1 calc R . . H29B H 0.4267 0.6252 0.7267 0.401 Uiso 1 1 calc R . . H29C H 0.3644 0.6119 0.6741 0.401 Uiso 1 1 calc R . . C30 C 0.3465(11) 0.7231(11) 0.6303(15) 0.303(12) Uiso 1 1 d . . . H30A H 0.3739 0.7218 0.5913 0.454 Uiso 1 1 calc R . . H30B H 0.3332 0.7656 0.6372 0.454 Uiso 1 1 calc R . . H30C H 0.3101 0.6972 0.6168 0.454 Uiso 1 1 calc R . . C31 C 0.4051(14) 0.7478(19) 0.738(2) 0.366(16) Uiso 1 1 d . . . H31 H 0.4093 0.7884 0.7196 0.439 Uiso 1 1 calc R . . C32 C 0.5021(8) 0.2382(9) 0.6813(10) 0.089(5) Uiso 0.50 1 d P . . C33 C 0.4802(12) 0.1470(11) 0.7809(13) 0.287(11) Uiso 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 Mo1 0.0364(3) 0.0394(3) 0.0316(3) 0.0031(2) -0.0024(2) 0.0003(2) Br1 0.0613(4) 0.0504(4) 0.0668(4) -0.0047(3) -0.0083(3) -0.0047(3) Cu1 0.0382(4) 0.0518(4) 0.0350(4) 0.0049(3) 0.0009(3) -0.0005(3) Cu2 0.0434(4) 0.0437(4) 0.0360(4) -0.0036(3) 0.0004(3) 0.0013(3) Cu3 0.0560(4) 0.0385(4) 0.0404(4) 0.0025(3) 0.0037(3) -0.0032(3) S1 0.0536(8) 0.0418(8) 0.0405(8) 0.0003(7) 0.0101(7) 0.0038(7) S2 0.0498(8) 0.0369(7) 0.0406(8) 0.0039(6) 0.0045(7) -0.0020(6) S3 0.0537(8) 0.0382(7) 0.0335(7) 0.0009(6) 0.0075(6) -0.0025(6) O1 0.050(2) 0.067(3) 0.055(3) 0.010(2) -0.016(2) -0.001(2) O2 0.219(9) 0.096(6) 0.189(9) 0.039(6) -0.006(7) 0.015(6) N1 0.037(2) 0.050(3) 0.041(3) 0.007(2) 0.004(2) 0.000(2) N2 0.044(3) 0.045(3) 0.046(3) 0.003(2) -0.006(2) -0.004(2) N3 0.037(2) 0.060(3) 0.038(3) -0.001(2) 0.007(2) -0.003(2) N4 0.056(3) 0.037(3) 0.041(3) -0.008(2) 0.006(2) 0.002(2) N5 0.061(3) 0.039(3) 0.035(3) -0.004(2) 0.005(2) 0.000(2) N6 0.082(5) 0.139(9) 0.128(7) -0.016(6) -0.002(5) 0.027(6) C1 0.049(3) 0.056(4) 0.051(4) 0.015(3) -0.007(3) -0.013(3) C2 0.042(3) 0.055(4) 0.060(4) 0.014(3) -0.005(3) -0.011(3) C3 0.033(3) 0.047(3) 0.041(3) 0.005(3) 0.002(2) 0.001(2) C4 0.042(3) 0.043(3) 0.047(3) 0.009(3) -0.001(3) -0.002(3) C5 0.032(3) 0.051(3) 0.059(4) 0.006(3) -0.005(3) -0.009(3) C6 0.049(3) 0.046(4) 0.073(5) 0.011(3) -0.015(3) -0.006(3) C7 0.052(3) 0.047(4) 0.071(5) 0.015(3) -0.016(3) -0.001(3) C8 0.043(3) 0.043(3) 0.045(3) 0.003(3) -0.002(3) 0.002(3) C9 0.063(4) 0.043(4) 0.096(6) 0.006(4) -0.031(4) -0.007(3) C10 0.061(4) 0.047(4) 0.097(6) 0.005(4) -0.028(4) -0.007(3) C11 0.036(3) 0.060(4) 0.038(3) 0.000(3) 0.000(3) -0.007(3) C12 0.039(3) 0.062(4) 0.038(3) -0.009(3) 0.001(3) -0.003(3) C13 0.038(3) 0.044(3) 0.037(3) 0.006(3) 0.003(3) -0.002(2) C14 0.039(3) 0.090(5) 0.034(3) -0.009(3) 0.002(3) -0.013(3) C15 0.049(4) 0.082(5) 0.044(4) -0.011(3) 0.012(3) -0.017(3) C16 0.093(5) 0.053(4) 0.031(3) 0.001(3) -0.007(3) 0.012(3) C17 0.090(5) 0.039(3) 0.051(4) -0.003(3) -0.001(4) 0.008(3) C18 0.057(3) 0.044(3) 0.036(3) -0.003(3) 0.006(3) -0.001(3) C19 0.113(6) 0.037(3) 0.037(3) -0.004(3) 0.005(4) -0.002(3) C20 0.095(5) 0.039(3) 0.039(3) -0.004(3) 0.004(3) 0.001(3) C21 0.062(4) 0.040(3) 0.052(4) -0.010(3) 0.002(3) -0.001(3) C22 0.061(4) 0.047(4) 0.050(4) -0.006(3) -0.002(3) -0.006(3) C23 0.061(3) 0.027(3) 0.034(3) 0.000(2) 0.012(3) -0.010(3) C24 0.078(4) 0.043(3) 0.044(4) -0.003(3) 0.006(3) 0.006(3) C25 0.072(4) 0.044(3) 0.042(3) -0.006(3) -0.001(3) 0.005(3) C26 0.184(15) 0.127(11) 0.136(11) -0.027(10) 0.005(10) -0.026(11) C27 0.162(13) 0.206(16) 0.29(2) -0.003(15) 0.086(14) -0.072(12) C28 0.185(13) 0.132(12) 0.248(19) 0.007(12) -0.017(12) 0.048(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 Cu1 2.6804(8) . ? Mo1 Cu2 2.7180(8) . ? Mo1 Cu3 2.7109(8) . ? Mo1 S1 2.2681(15) . ? Mo1 S2 2.2808(14) . ? Mo1 S3 2.2504(15) . ? Mo1 O1 1.697(4) . ? Br1 Cu3 2.4283(9) . ? Cu1 S1 2.2926(16) . ? Cu1 S2 2.2806(16) . ? Cu1 N1 2.015(4) . ? Cu1 N3 2.110(5) . ? Cu2 S2 2.2855(17) . ? Cu2 S3 2.3031(15) . ? Cu2 N2 2.066(4) 2 ? Cu2 N4 2.085(4) . ? Cu3 S1 2.2666(17) . ? Cu3 S3 2.3018(15) . ? Cu3 N5 2.179(4) 4_546 ? O2 C26 1.220(15) . ? O3 C31 1.39(3) . ? O4 C32 1.23(3) . ? N1 C1 1.336(7) . ? N1 C5 1.341(7) . ? N2 Cu2 2.066(4) 2 ? N2 C6 1.326(7) . ? N2 C10 1.329(7) . ? N3 C11 1.339(7) . ? N3 C15 1.330(7) . ? N4 C16 1.331(7) . ? N4 C20 1.334(7) . ? N5 Cu3 2.179(4) 4_556 ? N5 C21 1.336(7) . ? N5 C25 1.326(7) . ? N6 C26 1.346(15) . ? N6 C27 1.349(14) . ? N6 C28 1.430(14) . ? N7 C29 1.41(2) . ? N7 C30 1.39(2) . ? N7 C31 1.33(3) . ? N8 C32 1.374(18) 2_656 ? N8 C32 1.374(18) . ? N8 C33 1.54(2) 2_656 ? N8 C33 1.54(2) . ? C1 H1 0.9300 . ? C1 C2 1.372(7) . ? C2 H2 0.9300 . ? C2 C3 1.381(8) . ? C3 C4 1.395(7) . ? C3 C8 1.495(7) . ? C4 H4 0.9300 . ? C4 C5 1.383(7) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C6 C7 1.386(8) . ? C7 H7 0.9300 . ? C7 C8 1.380(8) . ? C8 C9 1.370(8) . ? C9 H9 0.9300 . ? C9 C10 1.370(8) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C11 C12 1.382(8) . ? C12 H12 0.9300 . ? C12 C13 1.372(7) . ? C13 C13 1.482(10) 2_655 ? C13 C14 1.384(8) . ? C14 H14 0.9300 . ? C14 C15 1.377(8) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C16 C17 1.392(8) . ? C17 H17 0.9300 . ? C17 C18 1.372(8) . ? C18 C19 1.404(8) . ? C18 C23 1.489(7) . ? C19 H19 0.9300 . ? C19 C20 1.358(8) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C21 C22 1.399(8) . ? C22 H22 0.9300 . ? C22 C23 1.378(8) . ? C23 C24 1.389(7) . ? C24 H24 0.9300 . ? C24 C25 1.381(8) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31 0.9300 . ? C33 C33 1.47(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 Cu1 Mo1 Cu2 88.08(2) . . ? Cu1 Mo1 Cu3 91.27(2) . . ? Cu3 Mo1 Cu2 91.01(3) . . ? S1 Mo1 Cu1 54.43(4) . . ? S1 Mo1 Cu2 121.82(4) . . ? S1 Mo1 Cu3 53.26(4) . . ? S1 Mo1 S2 108.38(5) . . ? S2 Mo1 Cu1 54.01(4) . . ? S2 Mo1 Cu2 53.55(4) . . ? S2 Mo1 Cu3 126.29(4) . . ? S3 Mo1 Cu1 123.11(4) . . ? S3 Mo1 Cu2 54.25(4) . . ? S3 Mo1 Cu3 54.33(4) . . ? S3 Mo1 S1 107.31(5) . . ? S3 Mo1 S2 107.80(5) . . ? O1 Mo1 Cu1 125.74(15) . . ? O1 Mo1 Cu2 127.26(16) . . ? O1 Mo1 Cu3 122.57(14) . . ? O1 Mo1 S1 110.92(16) . . ? O1 Mo1 S2 111.13(15) . . ? O1 Mo1 S3 111.15(16) . . ? S1 Cu1 Mo1 53.58(4) . . ? S2 Cu1 Mo1 54.01(4) . . ? S2 Cu1 S1 107.54(6) . . ? N1 Cu1 Mo1 139.15(14) . . ? N1 Cu1 S1 117.90(14) . . ? N1 Cu1 S2 113.44(14) . . ? N1 Cu1 N3 109.51(18) . . ? N3 Cu1 Mo1 111.28(12) . . ? N3 Cu1 S1 98.33(14) . . ? N3 Cu1 S2 108.87(14) . . ? S2 Cu2 Mo1 53.39(4) . . ? S2 Cu2 S3 105.86(6) . . ? S3 Cu2 Mo1 52.47(4) . . ? N2 Cu2 Mo1 128.89(13) 2 . ? N2 Cu2 S2 114.19(15) 2 . ? N2 Cu2 S3 109.88(14) 2 . ? N2 Cu2 N4 108.69(18) 2 . ? N4 Cu2 Mo1 121.98(13) . . ? N4 Cu2 S2 112.20(14) . . ? N4 Cu2 S3 105.63(14) . . ? Br1 Cu3 Mo1 146.89(3) . . ? S1 Cu3 Mo1 53.31(4) . . ? S1 Cu3 Br1 117.18(5) . . ? S1 Cu3 S3 105.62(6) . . ? S3 Cu3 Mo1 52.58(4) . . ? S3 Cu3 Br1 120.00(5) . . ? N5 Cu3 Mo1 110.17(13) 4_546 . ? N5 Cu3 Br1 102.78(13) 4_546 . ? N5 Cu3 S1 110.88(14) 4_546 . ? N5 Cu3 S3 98.59(13) 4_546 . ? Mo1 S1 Cu1 71.99(5) . . ? Cu3 S1 Mo1 73.43(5) . . ? Cu3 S1 Cu1 115.42(7) . . ? Mo1 S2 Cu2 73.06(5) . . ? Cu1 S2 Mo1 71.98(5) . . ? Cu1 S2 Cu2 110.55(6) . . ? Mo1 S3 Cu2 73.28(5) . . ? Mo1 S3 Cu3 73.09(5) . . ? Cu3 S3 Cu2 114.48(6) . . ? C1 N1 Cu1 121.2(4) . . ? C1 N1 C5 115.0(5) . . ? C5 N1 Cu1 123.6(4) . . ? C6 N2 Cu2 118.0(4) . 2 ? C6 N2 C10 115.9(5) . . ? C10 N2 Cu2 125.6(4) . 2 ? C11 N3 Cu1 123.0(4) . . ? C15 N3 Cu1 118.2(4) . . ? C15 N3 C11 117.4(5) . . ? C16 N4 Cu2 125.1(4) . . ? C16 N4 C20 116.8(5) . . ? C20 N4 Cu2 117.9(4) . . ? C21 N5 Cu3 120.5(4) . 4_556 ? C25 N5 Cu3 120.0(4) . 4_556 ? C25 N5 C21 117.0(5) . . ? C26 N6 C27 128.2(13) . . ? C26 N6 C28 114.7(12) . . ? C27 N6 C28 117.0(11) . . ? C30 N7 C29 123.3(18) . . ? C31 N7 C29 125(2) . . ? C31 N7 C30 111(2) . . ? C32 N8 C32 129.7(19) 2_656 . ? C32 N8 C33 137.4(14) 2_656 2_656 ? C32 N8 C33 90.7(12) . 2_656 ? C32 N8 C33 90.7(12) 2_656 . ? C32 N8 C33 137.4(14) . . ? C33 N8 C33 56.8(17) 2_656 . ? N1 C1 H1 117.7 . . ? N1 C1 C2 124.6(5) . . ? C2 C1 H1 117.7 . . ? C1 C2 H2 120.0 . . ? C1 C2 C3 120.0(5) . . ? C3 C2 H2 120.0 . . ? C2 C3 C4 116.8(5) . . ? C2 C3 C8 121.7(5) . . ? C4 C3 C8 121.4(5) . . ? C3 C4 H4 120.6 . . ? C5 C4 C3 118.7(5) . . ? C5 C4 H4 120.6 . . ? N1 C5 C4 124.8(5) . . ? N1 C5 H5 117.6 . . ? C4 C5 H5 117.6 . . ? N2 C6 H6 118.2 . . ? N2 C6 C7 123.5(6) . . ? C7 C6 H6 118.2 . . ? C6 C7 H7 119.9 . . ? C8 C7 C6 120.1(5) . . ? C8 C7 H7 119.9 . . ? C7 C8 C3 121.4(5) . . ? C9 C8 C3 122.8(5) . . ? C9 C8 C7 115.8(5) . . ? C8 C9 H9 119.7 . . ? C10 C9 C8 120.7(6) . . ? C10 C9 H9 119.7 . . ? N2 C10 C9 123.9(6) . . ? N2 C10 H10 118.0 . . ? C9 C10 H10 118.0 . . ? N3 C11 H11 119.0 . . ? N3 C11 C12 121.9(5) . . ? C12 C11 H11 119.0 . . ? C11 C12 H12 119.6 . . ? C13 C12 C11 120.8(5) . . ? C13 C12 H12 119.6 . . ? C12 C13 C13 122.6(6) . 2_655 ? C12 C13 C14 117.0(5) . . ? C14 C13 C13 120.4(5) . 2_655 ? C13 C14 H14 120.4 . . ? C15 C14 C13 119.2(5) . . ? C15 C14 H14 120.4 . . ? N3 C15 C14 123.6(6) . . ? N3 C15 H15 118.2 . . ? C14 C15 H15 118.2 . . ? N4 C16 H16 118.8 . . ? N4 C16 C17 122.4(6) . . ? C17 C16 H16 118.8 . . ? C16 C17 H17 119.6 . . ? C18 C17 C16 120.7(6) . . ? C18 C17 H17 119.6 . . ? C17 C18 C19 116.1(5) . . ? C17 C18 C23 123.0(5) . . ? C19 C18 C23 120.8(5) . . ? C18 C19 H19 120.2 . . ? C20 C19 C18 119.7(6) . . ? C20 C19 H19 120.2 . . ? N4 C20 C19 124.3(6) . . ? N4 C20 H20 117.9 . . ? C19 C20 H20 117.9 . . ? N5 C21 H21 118.0 . . ? N5 C21 C22 124.0(6) . . ? C22 C21 H21 118.0 . . ? C21 C22 H22 120.9 . . ? C23 C22 C21 118.1(5) . . ? C23 C22 H22 120.9 . . ? C22 C23 C18 121.2(5) . . ? C22 C23 C24 118.0(5) . . ? C24 C23 C18 120.7(5) . . ? C23 C24 H24 120.2 . . ? C25 C24 C23 119.6(6) . . ? C25 C24 H24 120.2 . . ? N5 C25 C24 123.3(6) . . ? N5 C25 H25 118.4 . . ? C24 C25 H25 118.4 . . ? O2 C26 N6 125.3(14) . . ? O2 C26 H26 117.4 . . ? N6 C26 H26 117.4 . . ? N6 C27 H27A 109.5 . . ? N6 C27 H27B 109.5 . . ? N6 C27 H27C 109.5 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N6 C28 H28A 109.5 . . ? N6 C28 H28B 109.5 . . ? N6 C28 H28C 109.5 . . ? H28A C28 H28B 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N7 C29 H29A 109.5 . . ? N7 C29 H29B 109.5 . . ? N7 C29 H29C 109.5 . . ? H29A C29 H29B 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N7 C30 H30A 109.5 . . ? N7 C30 H30B 109.5 . . ? N7 C30 H30C 109.5 . . ? H30A C30 H30B 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O3 C31 H31 123.3 . . ? N7 C31 O3 113(3) . . ? N7 C31 H31 123.3 . . ? O4 C32 N8 96.9(19) . . ? C33 C33 N8 61.6(9) 2_656 . ? 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 Mo1 Cu1 S1 Cu3 60.88(6) . . . . ? Mo1 Cu1 S2 Cu2 -63.30(5) . . . . ? Mo1 Cu1 N1 C1 -42.1(6) . . . . ? Mo1 Cu1 N1 C5 133.4(4) . . . . ? Mo1 Cu1 N3 C11 138.2(4) . . . . ? Mo1 Cu1 N3 C15 -27.8(5) . . . . ? Mo1 Cu2 S2 Cu1 62.64(5) . . . . ? Mo1 Cu2 S3 Cu3 -61.94(6) . . . . ? Mo1 Cu2 N4 C16 120.2(5) . . . . ? Mo1 Cu2 N4 C20 -54.1(5) . . . . ? Mo1 Cu3 S1 Cu1 -60.09(6) . . . . ? Mo1 Cu3 S3 Cu2 62.05(5) . . . . ? Br1 Cu3 S1 Mo1 142.34(4) . . . . ? Br1 Cu3 S1 Cu1 82.25(7) . . . . ? Br1 Cu3 S3 Mo1 -140.90(4) . . . . ? Br1 Cu3 S3 Cu2 -78.86(7) . . . . ? Cu1 Mo1 Cu2 S2 -45.07(5) . . . . ? Cu1 Mo1 Cu2 S3 134.23(5) . . . . ? Cu1 Mo1 Cu2 N2 48.18(18) . . . 2 ? Cu1 Mo1 Cu2 N4 -140.30(16) . . . . ? Cu1 Mo1 Cu3 Br1 -42.23(7) . . . . ? Cu1 Mo1 Cu3 S1 42.05(5) . . . . ? Cu1 Mo1 Cu3 S3 -131.05(5) . . . . ? Cu1 Mo1 Cu3 N5 143.57(14) . . . 4_546 ? Cu1 Mo1 S1 Cu3 -124.59(5) . . . . ? Cu1 Mo1 S2 Cu2 119.02(5) . . . . ? Cu1 Mo1 S3 Cu2 -58.75(5) . . . . ? Cu1 Mo1 S3 Cu3 64.17(5) . . . . ? Cu1 N1 C1 C2 175.2(5) . . . . ? Cu1 N1 C5 C4 -175.5(5) . . . . ? Cu1 N3 C11 C12 -166.8(4) . . . . ? Cu1 N3 C15 C14 165.5(5) . . . . ? Cu2 Mo1 Cu1 S1 -132.26(5) . . . . ? Cu2 Mo1 Cu1 S2 44.73(5) . . . . ? Cu2 Mo1 Cu1 N1 -40.2(2) . . . . ? Cu2 Mo1 Cu1 N3 143.13(15) . . . . ? Cu2 Mo1 Cu3 Br1 45.88(7) . . . . ? Cu2 Mo1 Cu3 S1 130.15(5) . . . . ? Cu2 Mo1 Cu3 S3 -42.95(5) . . . . ? Cu2 Mo1 Cu3 N5 -128.32(14) . . . 4_546 ? Cu2 Mo1 S1 Cu1 60.52(5) . . . . ? Cu2 Mo1 S1 Cu3 -64.07(5) . . . . ? Cu2 Mo1 S2 Cu1 -119.02(5) . . . . ? Cu2 Mo1 S3 Cu3 122.92(5) . . . . ? Cu2 N2 C6 C7 -170.5(5) 2 . . . ? Cu2 N2 C10 C9 170.4(6) 2 . . . ? Cu2 N4 C16 C17 -170.7(5) . . . . ? Cu2 N4 C20 C19 173.0(6) . . . . ? Cu3 Mo1 Cu1 S1 -41.29(5) . . . . ? Cu3 Mo1 Cu1 S2 135.70(5) . . . . ? Cu3 Mo1 Cu1 N1 50.8(2) . . . . ? Cu3 Mo1 Cu1 N3 -125.90(15) . . . . ? Cu3 Mo1 Cu2 S2 -136.30(5) . . . . ? Cu3 Mo1 Cu2 S3 43.00(5) . . . . ? Cu3 Mo1 Cu2 N2 -43.05(18) . . . 2 ? Cu3 Mo1 Cu2 N4 128.47(16) . . . . ? Cu3 Mo1 S1 Cu1 124.59(5) . . . . ? Cu3 Mo1 S2 Cu1 -60.03(6) . . . . ? Cu3 Mo1 S2 Cu2 58.99(6) . . . . ? Cu3 Mo1 S3 Cu2 -122.92(5) . . . . ? Cu3 N5 C21 C22 160.4(5) 4_556 . . . ? Cu3 N5 C25 C24 -161.1(5) 4_556 . . . ? S1 Mo1 Cu1 S2 176.99(7) . . . . ? S1 Mo1 Cu1 N1 92.0(2) . . . . ? S1 Mo1 Cu1 N3 -84.61(15) . . . . ? S1 Mo1 Cu2 S2 -90.17(7) . . . . ? S1 Mo1 Cu2 S3 89.13(7) . . . . ? S1 Mo1 Cu2 N2 3.08(19) . . . 2 ? S1 Mo1 Cu2 N4 174.59(16) . . . . ? S1 Mo1 Cu3 Br1 -84.28(8) . . . . ? S1 Mo1 Cu3 S3 -173.10(7) . . . . ? S1 Mo1 Cu3 N5 101.52(15) . . . 4_546 ? S1 Mo1 S2 Cu1 -2.58(6) . . . . ? S1 Mo1 S2 Cu2 116.44(5) . . . . ? S1 Mo1 S3 Cu2 -117.14(5) . . . . ? S1 Mo1 S3 Cu3 5.79(5) . . . . ? S1 Cu1 S2 Mo1 2.54(6) . . . . ? S1 Cu1 S2 Cu2 -60.77(7) . . . . ? S1 Cu1 N1 C1 23.4(5) . . . . ? S1 Cu1 N1 C5 -161.1(4) . . . . ? S1 Cu1 N3 C11 84.1(4) . . . . ? S1 Cu1 N3 C15 -81.8(5) . . . . ? S1 Cu3 S3 Mo1 -5.74(5) . . . . ? S1 Cu3 S3 Cu2 56.31(8) . . . . ? S2 Mo1 Cu1 S1 -176.99(7) . . . . ? S2 Mo1 Cu1 N1 -84.9(2) . . . . ? S2 Mo1 Cu1 N3 98.40(15) . . . . ? S2 Mo1 Cu2 S3 179.30(6) . . . . ? S2 Mo1 Cu2 N2 93.25(18) . . . 2 ? S2 Mo1 Cu2 N4 -95.23(16) . . . . ? S2 Mo1 Cu3 Br1 2.29(10) . . . . ? S2 Mo1 Cu3 S1 86.56(7) . . . . ? S2 Mo1 Cu3 S3 -86.54(7) . . . . ? S2 Mo1 Cu3 N5 -171.91(14) . . . 4_546 ? S2 Mo1 S1 Cu1 2.56(6) . . . . ? S2 Mo1 S1 Cu3 -122.03(5) . . . . ? S2 Mo1 S3 Cu2 -0.59(5) . . . . ? S2 Mo1 S3 Cu3 122.33(5) . . . . ? S2 Cu1 S1 Mo1 -2.55(6) . . . . ? S2 Cu1 S1 Cu3 58.33(8) . . . . ? S2 Cu1 N1 C1 -103.6(5) . . . . ? S2 Cu1 N1 C5 71.9(5) . . . . ? S2 Cu1 N3 C11 -164.0(4) . . . . ? S2 Cu1 N3 C15 30.0(5) . . . . ? S2 Cu2 S3 Mo1 0.58(5) . . . . ? S2 Cu2 S3 Cu3 -61.35(8) . . . . ? S2 Cu2 N4 C16 60.5(5) . . . . ? S2 Cu2 N4 C20 -113.8(4) . . . . ? S3 Mo1 Cu1 S1 -88.30(7) . . . . ? S3 Mo1 Cu1 S2 88.70(7) . . . . ? S3 Mo1 Cu1 N1 3.8(2) . . . . ? S3 Mo1 Cu1 N3 -172.90(15) . . . . ? S3 Mo1 Cu2 S2 -179.30(6) . . . . ? S3 Mo1 Cu2 N2 -86.05(18) . . . 2 ? S3 Mo1 Cu2 N4 85.47(17) . . . . ? S3 Mo1 Cu3 Br1 88.83(8) . . . . ? S3 Mo1 Cu3 S1 173.10(7) . . . . ? S3 Mo1 Cu3 N5 -85.37(15) . . . 4_546 ? S3 Mo1 S1 Cu1 118.72(5) . . . . ? S3 Mo1 S1 Cu3 -5.87(6) . . . . ? S3 Mo1 S2 Cu1 -118.42(5) . . . . ? S3 Mo1 S2 Cu2 0.60(5) . . . . ? S3 Cu2 S2 Mo1 -0.58(5) . . . . ? S3 Cu2 S2 Cu1 62.06(7) . . . . ? S3 Cu2 N4 C16 175.3(5) . . . . ? S3 Cu2 N4 C20 1.1(5) . . . . ? S3 Cu3 S1 Mo1 5.68(5) . . . . ? S3 Cu3 S1 Cu1 -54.41(8) . . . . ? O1 Mo1 Cu1 S1 91.50(19) . . . . ? O1 Mo1 Cu1 S2 -91.51(19) . . . . ? O1 Mo1 Cu1 N1 -176.5(3) . . . . ? O1 Mo1 Cu1 N3 6.9(2) . . . . ? O1 Mo1 Cu2 S2 90.08(19) . . . . ? O1 Mo1 Cu2 S3 -90.62(19) . . . . ? O1 Mo1 Cu2 N2 -176.7(3) . . . 2 ? O1 Mo1 Cu2 N4 -5.2(2) . . . . ? O1 Mo1 Cu3 Br1 -177.25(19) . . . . ? O1 Mo1 Cu3 S1 -92.98(19) . . . . ? O1 Mo1 Cu3 S3 93.92(19) . . . . ? O1 Mo1 Cu3 N5 8.5(2) . . . 4_546 ? O1 Mo1 S1 Cu1 -119.70(16) . . . . ? O1 Mo1 S1 Cu3 115.71(16) . . . . ? O1 Mo1 S2 Cu1 119.55(17) . . . . ? O1 Mo1 S2 Cu2 -121.43(17) . . . . ? O1 Mo1 S3 Cu2 121.43(16) . . . . ? O1 Mo1 S3 Cu3 -115.65(16) . . . . ? N1 Cu1 S1 Mo1 -132.30(16) . . . . ? N1 Cu1 S1 Cu3 -71.42(17) . . . . ? N1 Cu1 S2 Mo1 134.75(15) . . . . ? N1 Cu1 S2 Cu2 71.45(16) . . . . ? N1 Cu1 N3 C11 -39.5(5) . . . . ? N1 Cu1 N3 C15 154.5(4) . . . . ? N1 C1 C2 C3 0.0(10) . . . . ? N2 Cu2 S2 Mo1 -121.58(14) 2 . . . ? N2 Cu2 S2 Cu1 -58.94(15) 2 . . . ? N2 Cu2 S3 Mo1 124.34(15) 2 . . . ? N2 Cu2 S3 Cu3 62.40(16) 2 . . . ? N2 Cu2 N4 C16 -66.8(5) 2 . . . ? N2 Cu2 N4 C20 119.0(5) 2 . . . ? N2 C6 C7 C8 0.0(11) . . . . ? N3 Cu1 S1 Mo1 110.34(13) . . . . ? N3 Cu1 S1 Cu3 171.23(14) . . . . ? N3 Cu1 S2 Mo1 -103.05(14) . . . . ? N3 Cu1 S2 Cu2 -166.35(14) . . . . ? N3 Cu1 N1 C1 134.6(5) . . . . ? N3 Cu1 N1 C5 -49.9(5) . . . . ? N3 C11 C12 C13 0.8(9) . . . . ? N4 Cu2 S2 Mo1 114.17(14) . . . . ? N4 Cu2 S2 Cu1 176.80(14) . . . . ? N4 Cu2 S3 Mo1 -118.59(14) . . . . ? N4 Cu2 S3 Cu3 179.47(14) . . . . ? N4 C16 C17 C18 -3.1(11) . . . . ? N5 Cu3 S1 Mo1 -100.14(13) 4_546 . . . ? N5 Cu3 S1 Cu1 -160.23(14) 4_546 . . . ? N5 Cu3 S3 Mo1 108.88(14) 4_546 . . . ? N5 Cu3 S3 Cu2 170.92(14) 4_546 . . . ? N5 C21 C22 C23 0.2(10) . . . . ? C1 N1 C5 C4 0.2(9) . . . . ? C1 C2 C3 C4 1.2(9) . . . . ? C1 C2 C3 C8 179.5(6) . . . . ? C2 C3 C4 C5 -1.6(9) . . . . ? C2 C3 C8 C7 -27.4(9) . . . . ? C2 C3 C8 C9 151.8(7) . . . . ? C3 C4 C5 N1 0.9(9) . . . . ? C3 C8 C9 C10 -176.2(7) . . . . ? C4 C3 C8 C7 150.9(6) . . . . ? C4 C3 C8 C9 -29.9(10) . . . . ? C5 N1 C1 C2 -0.7(9) . . . . ? C6 N2 C10 C9 -1.4(11) . . . . ? C6 C7 C8 C3 176.8(6) . . . . ? C6 C7 C8 C9 -2.5(10) . . . . ? C7 C8 C9 C10 3.0(11) . . . . ? C8 C3 C4 C5 -179.9(5) . . . . ? C8 C9 C10 N2 -1.2(13) . . . . ? C10 N2 C6 C7 2.0(10) . . . . ? C11 N3 C15 C14 -1.2(9) . . . . ? C11 C12 C13 C13 -178.9(4) . . . 2_655 ? C11 C12 C13 C14 1.0(9) . . . . ? C12 C13 C14 C15 -2.8(9) . . . . ? C13 C13 C14 C15 177.1(5) 2_655 . . . ? C13 C14 C15 N3 3.1(10) . . . . ? C15 N3 C11 C12 -0.7(9) . . . . ? C16 N4 C20 C19 -1.7(10) . . . . ? C16 C17 C18 C19 0.5(10) . . . . ? C16 C17 C18 C23 176.1(6) . . . . ? C17 C18 C19 C20 1.3(10) . . . . ? C17 C18 C23 C22 40.2(9) . . . . ? C17 C18 C23 C24 -136.1(7) . . . . ? C18 C19 C20 N4 -0.7(11) . . . . ? C18 C23 C24 C25 174.1(6) . . . . ? C19 C18 C23 C22 -144.3(6) . . . . ? C19 C18 C23 C24 39.4(8) . . . . ? C20 N4 C16 C17 3.6(10) . . . . ? C21 N5 C25 C24 1.0(9) . . . . ? C21 C22 C23 C18 -174.6(5) . . . . ? C21 C22 C23 C24 1.8(9) . . . . ? C22 C23 C24 C25 -2.4(9) . . . . ? C23 C18 C19 C20 -174.5(6) . . . . ? C23 C24 C25 N5 1.0(10) . . . . ? C25 N5 C21 C22 -1.6(9) . . . . ? C27 N6 C26 O2 -5(2) . . . . ? C28 N6 C26 O2 179.1(13) . . . . ? C29 N7 C31 O3 -14(4) . . . . ? C30 N7 C31 O3 166(2) . . . . ? C32 N8 C32 O4 -16.2(13) 2_656 . . . ? C32 N8 C33 C33 -150.7(19) 2_656 . . 2_656 ? C32 N8 C33 C33 46(3) . . . 2_656 ? C33 N8 C32 O4 178.7(18) 2_656 . . . ? C33 N8 C32 O4 141.5(19) . . . . ?